megalomania
April 26th, 2002, 02:54 PM
I am thinking we need to have some better information about RDX synthesis as there seems to be some disagreement as to how it can be most efficiently done. To that end I have rounded up some references on RDX synthesis for the past few decades. If someone who involves themselves in greater detail than I can give in RDX synthesis, please review this list of references and I will get what is asked for. These are from 1993-2002
Bibliographic Information
Nitric acid decomposition of waste composite propellants for recovery of nitramine components. Warner, Kirstin F.; Cannizzo, Louis F.; Hajik, Robert M.; Johnston, Harold E. (Cordant Technologies Inc., USA). U.S. Pat. Appl. Publ. (2002), 9 pp. CODEN: USXXCO US 20020028971 A1 20020307 Patent written in English. Application: US 2001-784475 20010215. Priority: US 2000-188182 20000310. CAN 136:219170 AN 2002:172521 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 2002028971 A1 20020307 US 2001-784475 20010215
Priority Application Information
US 2000-188182P 20000310
Abstract
Nitramines are recovered from waste or unwanted composite nitramine aluminized propellants by: (1) treating the waste propellant with aq. nitric acid (below 55 wt.% HNO3), at a 4-6:1 wt. ratio of HNO3 to waste propellant, to digest the binder into soln. while neither solvating nor solvolyzing into soln. all or most of the nitramine, (2) adding a mineral acid other than nitric acid to the soln. and digesting a portion of the aluminum, and (3) recovering the nitramine. Suitable mineral acids other than nitric acid are selected from hydrochloric acid, perchloric acid, sulfuric acid, phosphoric acid, hydrobromic acid, and hydroiodic acid. Suitable nitramines that can be recovered include RDX, HMX, TEX, 4,10-dinitro-4,10-diaza-2,6,8,12-tetraoxatetracyclo[5.5.0.05,9.0.3,11] dodecane, and CL-20 (HNIW). Treatment of the energetic material can be carried out without the use of volatile org. solvents.
Bibliographic Information
Formation of energetic materials using supercritical fluids. Teipel, Ulrich; Krober, Hartmut; Krause, Horst H. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Propellants, Explosives, Pyrotechnics (2001), 26(4), 168-173. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 136:104697 AN 2001:829487 CAPLUS (Copyright 2002 ACS)
Abstract
A new field of applications of compressed gases is the formation of solid particles with well-defined properties, e.g. the particle size, the particle size distribution, the particle shape, the sp. surface area and free of solvent inclusions. It is possible to process moderately solids like energetic materials which are difficult to comminute due to their sensitivity to mech. or thermal stress. The characteristics of compressed gases allow to vary the morphol. of solid particles in a wide range. A pilot plant is presented, which has been built to prep. fine particles by the rapid expansion of supercrit. solns. (RESS process) and pptn. by a compressed fluid antisolvent (PCA process). The micronization of different energetic materials by the RESS and PCA processes is investigated.
Bibliographic Information
Process for co-manufacturing RDX high explosive and TNT-free emulsified explosive. Bao, Guangyi; Bao, Cuoli. (Peop. Rep. China). Faming Zhuanli Shenqing Gongkai Shuomingshu (2001), 4 pp. CODEN: CNXXEV CN 1293177 A 20010502 Patent written in Chinese. Application: CN 2000-131348 20001102. CAN 135:320150 AN 2001:813474 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
CN 1293177 A 20010502 CN 2000-131348 20001102
Abstract
The process comprises reacting of 10-12 wt. parts HNO3 with 1 wt. part hexamine at below 20° to obtain RDX, charging a mixt. contg. ammonium nitrate and ammonium sulfonate in an amt. of 8-12 wt. parts to the reactant, reacting the mixt. at 70-80°, neutralizing the byproduct (nitrate, H2O, etc.) with CaCO3, Ca(OH)2 or CaO to obtain the aq. phase of TNT-free emulsified explosive, and then reacting with oily phase to obtain TNT-free emulsified explosive.
Bibliographic Information
Study on preparation of ultrafine particle of explosive using technology of direct dilution. Sima, Tianlong; Yan, Jisheng. Gansu Yinguang Chemical industrial Complex, Baiyin, Peop. Rep. China. Huozhayao Xuebao (2001), 24(4), 46-47. CODEN: HUXUFP Journal written in Chinese. CAN 136:234276 AN 2001:804744 CAPLUS (Copyright 2002 ACS)
Abstract
Ultrafine particle of explosive is prepd. by using direct diln. technol. The fundamental principle of the method is introduced. The particle size and distribution of size of ultrafine PETN and RDX are tested.
Bibliographic Information
Study on high-energy LOVA propellant. Liao, Xin; Huang, Zhenya; Yang, Wenbao; Wang, Zeshan. Xi'an Modern Chemistry Research Institute, Xi'an, Peop. Rep. China. Huozhayao Xuebao (2001), 24(4), 8-9, 30. CODEN: HUXUFP Journal written in Chinese. CAN 136:249804 AN 2001:804730 CAPLUS (Copyright 2002 ACS)
Abstract
The formulation of a LOVA propellant was detd. by using RDX as the main energetic compn. with inert and energetic complex binders, complex plasticizers and combustion modifiers. The closed bomb tests showed that the designed formula of the LOVA propellant had the characteristic of high energy and low erosion. The solvent-extrusion process was demonstrated practicable for this type of LOVA propellant formula.
Bibliographic Information
Supercritical fluid technology: a new process on formation of energetic materials. Krober, H.; Reinhard, W.; Teipel, U. Fraunhofer Institut fur Chemische Technologie (ICT), Pfinztal, Germany. International Annual Conference of ICT (2001), 32nd(Energetic Materials), 48/1-48/13. CODEN: IACIEQ ISSN: 0722-4087. Journal written in English. CAN 135:346528 AN 2001:605072 CAPLUS (Copyright 2002 ACS)
Abstract
A novel process for purifn. of energetic solids was developed using compressed inert supercrit. gases (esp. CO2), in which the material can be comminuted to solid particles with well-defined properties (e.g., particle size, size distribution, shape, and sp. surface area) and no fluid inclusions. The particle morphol. can be varied by varying the characteristics of the compressed gases. The RESS (Rapid Expansion of Supercrit. Solns.) uses a loaded supercrit. fluid that is expanded through a nozzle to create a high supersatn. in the jet, in which rapid crystal nucleation and growth occurs. Solids which are insol. in a compressed gas can be processed by using the PCA process (pptn. with a compressed antisolvent). In this process, a soln. consisting of an org. solvent that is completely miscible with the compressed gas, and a solid material dissolved in this solvent is sprayed through a nozzle into a high-pressure vessel filled with a compressed gas. A pilot plant was thus built to prep. fine particles of certain solid explosives (e.g., HNS, TNT, RDX, etc.).
Bibliographic Information
Raman spectroscopy investigation of the effects of precipitation of precursor powders by antisolvents. Case study of RDX powders precipitation. Marlange, L.; Begue, G.; Petitet, J. P.; Jacob, G. Laboratoire D'Ingenierie des Materiaux et des Hautes Pressions, Institut Galilee - Universite Paris XIII, Villetaneuse, Fr. Recents Progres en Genie des Procedes (2001), 15(77, Science et Technologie des Poudres), 61-66. CODEN: RPGPEX ISSN: 1166-7478. Journal written in French. CAN 136:8599 AN 2001:599690 CAPLUS (Copyright 2002 ACS)
Abstract
Based on Raman spectroscopic results, the effect of a CO2 antisolvent (at densities 0.01-0.25 g/cm3) on the precursors of the powders obtained by pptn. was discussed for different solvents (e.g., acetone, Et acetate, or toluene) depending on the solvent swelling capacity. Three results were obsd. in the rapid pptn. of RDX from acetone soln. using crit. CO2 antisolvent: (1) the observable appearance of the ppt. is localized just beyond the max. obsd. Raman intensity, (2) the morphol. of the powder is different at a low pressure or under crit. conditions for CO2, and (3) the appearance of the pptd. powder at low pressure is reversible.
Bibliographic Information
Separation of nitramine and nitroaromatic explosives by capillary liquid chromatography. Goodpaster, John V.; McGuffin, Victoria L. Department of Chemistry, Michigan State University, East Lansing, MI, USA. Journal of Liquid Chromatography & Related Technologies (2001), 24(13), 1965-1978. CODEN: JLCTFC ISSN: 1082-6076. Journal written in English. CAN 135:244590 AN 2001:557131 CAPLUS (Copyright 2002 ACS)
Abstract
This study outlines the successful sepn. of nitrated explosives by using high efficiency capillary liq. chromatog. Careful optimization of sepn. conditions such as mobile phase compn. and temp. was performed by using a window diagram, as well as a more global criterion, the chromatog. resoln. statistic. These efforts resulted in complete baseline resoln. of all 14 components of a std. mixt. of explosives, which has not previously been achieved by using conventional liq. chromatog. This method was then applied to the detn. of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazine (HMX), and 2,4,6-trinitrotoluene (2,4,6-TNT) in com.-grade and military-grade explosive samples. As a result, the countries of manuf. of two RDX samples were deduced based on the presence or absence of reaction byproducts.
Bibliographic Information
Explosive properties of reactive mixtures formed during manufacturing of explosives. Buczkowski, Daniel; Gucma, Miroslaw; Pagowski, Witold. Institute of Industrial Organic Chemistry, Warsaw, Pol. Editor(s): Zeman, Svatopluk. New Trends in Research of Energetic Materials, Proceedings of the Seminar, 4th, Pardubice, Czech Republic, Apr. 11-12, 2001 (2001), 29-33. Publisher: University of Pardubice, Pardubice, Czech Rep CODEN: 69BKIC Conference written in English. CAN 135:228922 AN 2001:476831 CAPLUS (Copyright 2002 ACS)
Abstract
Explosive properties of mixts. formed in manuf. of PETN and RDX are presented. Deposits of PETN and RDX in nitric acid filling voids between crystals have detonation abilities similar to typical brisant explosives. Such deposits are formed if mixing is stopped. Soln. of RDX and slurry of PETN in nitric acid have weaker explosive properties, but are dangerous from the point of view of explosion. A problem of minimizing the possibility of damage of mixing equipment or electricity loss must be anticipated during designing producing plants for the manuf. of explosives.
Bibliographic Information
The sensitivity of explosives. McCrone, Walter C. McCrone Associates, Inc., Chicago, IL, USA. Microscope (2001), 49(1), 47-48. CODEN: MICRAD ISSN: 0026-282X. Journal written in English. CAN 135:109344 AN 2001:363793 CAPLUS (Copyright 2002 ACS)
Abstract
The sensitivity of HMX (e.g., as a byproduct of the manuf. of RDX) posses 4 known polymorphs, and, in one form (designated HMX 1, in the bipyramidal polymorph) is relatively insensitive. Phys. deformation (e.g., induced by rapid crystn.) results in a marked increase in sensitivity of HMX 1. HMX in general is subject to crystal strain if crystd. rapidly or ground to finer crystals, which can increase sensitivity, make the total batch have variable sensitivity, and can cause occasional unexpected explosions. This effect of crystal strain on sensitivity was also obsd. for TNT and lead azide, although no quant. relationship was examd.
Bibliographic Information
Study on the crystal size control of RDX. Liu, Han-bin; Yeh, Tsao-fa; Hu, Cheng-ching; Shieh, Chow-yang; Wang, Shan-guang. Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Ta-hsi, Taoyuan, Taiwan. Huoyao Jishu (2001), 17(1), 41-51. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 135:7561 AN 2001:312660 CAPLUS (Copyright 2002 ACS)
Abstract
RDX is probably the most important high brisance explosive and has wide applications. The performances of explosive depend on the crystal size distribution of RDX. The crystal size control is studied by using the characteristic of RDX dissoln. in concd. nitric acid. Based on the process flow conditions of RDX prodn. in the 203rd Arsenal Combined Service Force, the temp., concn. and residence time are selected as control parameters to conduct the expts. Thus it provides the better conditions of product and enables to obtain higher yield of target crystal size with the redn. of the quantity of outside target range of RDX.
Bibliographic Information
Study of the optimal reactor design in the manufacture process of RDX. Luo, Kuo-ming; Lin, Sheann-huei; Chang, Jih-guang; Chu, Kuang-shing. Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Ta-hsi, Taoyuan, Taiwan. Huoyao Jishu (2001), 17(1), 21-32. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 135:7560 AN 2001:312659 CAPLUS (Copyright 2002 ACS)
Abstract
The RDX is produced by the chem. reaction of Hexamine and nitric acid in three CSTRs of vol. of 112.5 L. A correlation is given for the calcn. of the reaction rate. To det. the optimal reactor design. The reaction temp. and fractional conversion are added to det. the optimum reactor design. The highest yield of the RDX is obtained at const. feeding ratio and const. reaction temp. range. The results enable to improve the RDX prodn. at optimum reaction temp. and flow rate.
Bibliographic Information
Preparation of nanometer RDX in situ by solvent substitution effect in reverse micelles. Liu, Dabin; Xu, Dong; Zhao, Baochang; Peng, Jinhua; Gao, Yaolin; Fan, Qinwen. Nanjing University Science Technology, Nanjing, Peop. Rep. China. Proceedings of the International Pyrotechnics Seminar (1999), 26th 269-275. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 134:313266 AN 2001:294122 CAPLUS (Copyright 2002 ACS)
Abstract
A new method to prep. ultrafine explosive through solvent substitution effect in reverse micelles was introduced. The max. soly. of DMF, DMSO, and its RDX soln. in NaAOT-isooctane reverse micelles were detd. The cylinder model RDX crystallites with their diam. of 70-100 nm were prepd. in situ in the NaAOT-isooctane reverse micelle system.
Bibliographic Information
Manufacture of finely dispersed explosives by crystallization from supercritical fluids. Teipel, Ulrich; Krause, Horst; Krober, Hartmut; Forter-Barth, Ulrich. (Fraunhofer-Gesellschaft zur Forderung der Angewandten Forschung e.V., Germany). Eur. Pat. Appl. (2001), 13 pp. CODEN: EPXXDW EP 1090894 A1 20010411 Designated States R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO. Patent written in German. Application: EP 2000-121747 20001005. Priority: DE 99-19948133 19991006. CAN 134:282927 AN 2001:261086 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
EP 1090894 A1 20010411 EP 2000-121747 20001005
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
Priority Application Information
DE 1999-19948133 19991006
Abstract
An explosive is dissolved in an org. solvent, a supercrit. fluid, which is miscible or partially miscible with the solvent and in which the explosive is insol. or slightly sol., is injected in the form of a jet flow into the soln., the solvent is collected during crystn. of the explosive particles from the supercrit. fluid, and the explosive particles are sepd. after expansion into a subcrit. state. Preferably, the soln. is injected into the supercrit. fluid by means of a complex nozzle or at least 1 nozzle channel of the complex nozzle, and the supercrit. fluid is fed by means of another nozzle channel.
Bibliographic Information
Effect of entropy on the formation of circular nitramine. Fang, Yi; Yongping, Pan. Nanjing, Peop. Rep. China. Proceedings of the International Pyrotechnics Seminar (1999), 26th 578-582. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 134:268397 AN 2001:115917 CAPLUS (Copyright 2002 ACS)
Abstract
Linear nitramines of TDA, BSX and ACAN were used to compose RDX directly in the soln. of ammonium nitrate - nitric acid. The reaction mechanism is discussed. Eight-member ring nitramine was composed difficultly. The effect of entropy was an important factor.
Bibliographic Information
Synthesis and nitration of condensation products of sulfamates with aliphatic amines and formaldehyde. Tartakovsky, V. A.; Ermakov, A. S.; Sigai, N. V.; Vinogradov, D. B. N. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, Moscow, Russia. Russian Chemical Bulletin (Translation of Izvestiya Akademii Nauk, Seriya Khimicheskaya) (2000), 49(6), 1082-1085. CODEN: RCBUEY ISSN: 1066-5285. Journal written in English. CAN 134:4920 AN 2000:700624 CAPLUS (Copyright 2002 ACS)
Abstract
A method for the synthesis of 5-alkyl-1,3-dinitro-1,3,5-triazacyclohexanes and linear polynitramines was proposed. It includes the reaction of aliph. amines with sulfamates and formaldehyde and nitration of the reaction products. The yield and compn. of nitramino derivs. depend on the conditions of the condensation and nitration.
Bibliographic Information
Crystallization of explosives and high-energy oxidizers in presence of ultrasound. Veltmans, Wilhelmina H. m.; Wierckx, Franciscus J. m. (Aerospace Propulsion Products B.V., Neth.). Eur. Pat. Appl. (2000), 13 pp. CODEN: EPXXDW EP 1033357 A1 20000906 Designated States R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO. Patent written in English. Application: EP 99-200592 19990302. CAN 133:195590 AN 2000:626476 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
EP 1033357 A1 20000906 EP 1999-200592 19990302
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
NO 2000001017 A 20000904 NO 2000-1017 20000229
Priority Application Information
EP 1999-200592 19990302
Abstract
Cryst. energetic materials with improved stability and/or decreased sensitivity are prepd. by crystn. with stirring at 15-75° in the presence of ultrasound with frequency 10-100 kHz and amplitudes of 0.4-10 m. The energetic materials that can be prepd. in this manner are explosives and high-energy oxidizers, esp. hydrazinium nitroformate, CL-20, ADN, AP, RDX, HMX, and PETN.
Bibliographic Information
Simple method for labeled conjugate production using N-hydroxysuccinimide and phase changes to control the reaction. Morseman, John P.; Zeng, Xiangfei. (Martek Biosciences Corporation, USA). PCT Int. Appl. (2000), 35 pp. CODEN: PIXXD2 WO 0043784 A1 20000727 Designated States W: AE, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CR, CU, CZ, DE, DK, DM, EE, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, TZ, UA, UG, US, UZ, VN, YU, ZA, ZW, AM, AZ, BY, KG, KZ, MD, RU, TJ, TM. Designated States RW: AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE, BF, BJ, CF, CG, CI, CM, GA, ML, MR, NE, SN, TD, TG. Patent written in English. Application: WO 2000-US1350 20000121. Priority: US 99-116689 19990122. CAN 133:101746 AN 2000:513898 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
WO 2000043784 A1 20000727 WO 2000-US1350 20000121
W: AE, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CR, CU, CZ, DE, DK, DM, EE, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, TZ, UA, UG, US, UZ, VN, YU, ZA, ZW, AM, AZ, BY, KG, KZ, MD, RU, TJ, TM
RW: GH, GM, KE, LS, MW, SD, SL, SZ, TZ, UG, ZW, AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE, BF, BJ, CF, CG, CI, CM, GA, GN, GW, ML, MR, NE, SN, TD, TG
EP 1145007 A1 20011017 EP 2000-903358 20000121
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
Priority Application Information
US 1999-116689P 19990122
WO 2000-US1350 20000121
Abstract
The present invention relates to methods for coupling labels to particular target moieties. The coupling reactions of the present invention use temporal spacing of the reactants through phase change (i.e. by rapid freezing) to control the initiation and termination of reaction. This process results in a simplified and improved method for linking labels to specific binding moieties using N-hydroxysuccinimide chem. The present invention further relates to kits comprising all necessary components to easily and rapidly make protein conjugates. Phycoerythrin was conjugated to streptavidin via EDAC/sulfo-NHS from a freeze dried reagent where D-(+)-trehalose was used.
Bibliographic Information
Application of solid-phase microextraction to the recovery of explosives and ignitable liquid residues from forensic specimens. Furton, K. G.; Almirall, J. R.; Bi, M.; Wang, J.; Wu, L. Department of Chemistry and International Forensic Research Institute, Florida International University, Miami, FL, USA. Journal of Chromatography, A (2000), 885(1+2), 419-432. CODEN: JCRAEY ISSN: 0021-9673. Journal written in English. CAN 133:203913 AN 2000:436513 CAPLUS (Copyright 2002 ACS)
Abstract
Solid-phase microextn. (SPME) was applied to the anal. of ignitable liqs. and explosive residues and the relative effects of controllable variables were studied. Variables discussed include fiber chem., adsorption and desorption temps., extn. and desorption times, fiber sampling placement (direct, headspace, and partial headspace) and matrix effects, including water content. SPME is shown to be an inexpensive, rapid and sensitive method for the anal. of ignitable liqs. and high explosives residues from solid debris samples and from aq. samples. Explosives are readily detected at parts per trillion concns. and ignitable liqs. are reproducibly detected at levels below those using conventional methods.
Bibliographic Information
Preparation of Grade III RDX by crystallization in nitric acid. Ye, Ling; Wang, Jian-long; Ye, Yu-peng. Capital University of Medical Science, Beijing, Peop. Rep. China. Hanneng Cailiao (2000), 8(1), 46-48. CODEN: HACAFQ ISSN: 1006-9941. Journal written in Chinese. CAN 132:349813 AN 2000:372246 CAPLUS (Copyright 2002 ACS)
Abstract
The prepn. of RDX of grade III is controlled by the nucleation temp., the interval of heat preservation, and the rate of stepwise diln. with water during the crystn. process in nitric acid. The exptl. results show that reducing the acidity and controlling the granularity of the final product are keys to the technol. for crystn. of RDX in strong acid medium.
Bibliographic Information
Recovering nitroamines from energetic pyrotechnic materials and reformulation of by-products. Phillips, Randall S.; Cain, Andrew W.; Schilling, Thomas J.; Miks, Michael W. (TPL, Inc., USA). U.S. (2000), 5 pp. CODEN: USXXAM US 6063960 A 20000516 Patent written in English. Application: US 98-212050 19981215. Priority: US 97-69492 19971215. CAN 132:323300 AN 2000:323256 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 6063960 A 20000516 US 1998-212050 19981215
Priority Application Information
US 1997-69492P 19971215
Abstract
A method for recovering nitroamines from energetic pyrotechnic materials yielding usable byproducts and no waste comprises solubilizing an energetic pyrotechnic material (such as surplus energetic material plastic binder) in a nitric acid soln., (b) removing an effluent from the soln. to leave a nitroamine (such as cyclotetramethylene tetranitramine), (c) neutralizing the effluent with a base, (d) removing liq. content from the effluent to yield a compd. salt, (e) rinsing the nitroamine and (f) desensitizing the nitroamine.
Bibliographic Information
Supercritical fluid extraction of triple-base and LOVA gun propellants. Morris, Jeffrey B. U. S. Army Research Laboratory AMSRL-WM-BD, Aberdeen Proving Ground, MD, USA. CPIA Publication (1999), 687(JANNAF 28th Propellant Development & Characterization and 17th Safety & Environmental Protection Subcommittee Joint Meeting, Vol. 1, 1999), 331-340. CODEN: CPPUDT ISSN: 0272-5118. Journal written in English. CAN 132:267179 AN 2000:256920 CAPLUS (Copyright 2002 ACS)
Abstract
Two supercrit. fluid extn. (SFE) studies are carried out on low-vulnerability ammunition (LOVA) and triple-base gun propellants. The extn. of RDX from ground LOVA gun propellant is carried out using dynamic SFE conditions with acetonitrile and dimethylsulfoxide modifiers for carbon dioxide (CO2). The results of this study are compared to the previous work on static SFE of bulk LOVA propellant. The extn. of nitroglycerin (NG) from M30 gun propellant is investigated with unmodified CO2, using both bulk and ground propellant. In addn., the soly. of NG is also measured under isothermal conditions at 40°. For both types of propellants, substantial matrix effects are encountered for the extn. of RDX or NG from the bulk propellant sample.
Bibliographic Information
Preparation of ultra-fine explosive HMX and RDX using high-speed impinging streams. Zhang, Xiaoning; Xu, Gengguang; Wang, Tingzeng. Department of Engineeing Safty, Beijing Institute of Technology, Beijing, Peop. Rep. China. Beijing Ligong Daxue Xuebao (1999), 19(5), 646-650. CODEN: BLXUEV ISSN: 1001-0645. Journal written in Chinese. CAN 132:51962 AN 1999:815237 CAPLUS (Copyright 2002 ACS)
Abstract
A method for prepg. ultra-fine HMX and RDX and their technol. factors affecting the prepn. are described. High-speed impinging streams of suspending liq. were used. The particles of HMX and RDX can be crushed into sub-micron effectively by high-speed impinging streams method. The effective particle diam. is 612.2 nm and the particle size distribution is 236.5.apprx.1286.0 nm. The pressures and times of processing are the main factors that affect the particle sizes and particle size distribution. The most important factor affecting the degree of crush is the pressure. The times of processing affect the mean particle diam. and the particle size distribution, not the crushing lower limit.
Bibliographic Information
Method for the recovery of secondary explosives from 2,4,6-trinitrotoluene-containing explosive compositions. Spencer, Arthur F.; Hartline, David F. (United States Dept. of the Air Force, USA). U.S. (1999), 4 pp. CODEN: USXXAM US 5977354 A 19991102 Patent written in English. Application: US 98-211491 19981215. CAN 131:288483 AN 1999:705051 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5977354 A 19991102 US 1998-211491 19981215
Abstract
Secondary explosive materials, particularly nitramines, are recovered from an explosive compn. contg. a mixt. of 2,4,6-trinitrotoluene (I) and at least one secondary explosive(s) by heating the explosive compn. to melt the I (preferably using steam), sep. collecting and recovering the melted I, treating the sepd. secondary explosive (e.g., octahydro-1,3,5,7-tetranitro-1,3,5,7-Tetrazocine; i.e., HMX) with a material which is a solvent for I and a nonsolvent for the secondary explosive (e.g., toluene) to dissolve the TNT, removing the nonsolvent from the secondary explosive, and recovering the secondary explosive.
Bibliographic Information
A molecular modeling study of the solvent effect on the RDX crystal morphology. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft University of Technology, Delft, Neth. International Symposium on Industrial Crystallization, 14th, Cambridge, United Kingdom, Sept. 12-16, 1999 (1999), 1973-1984. Publisher: Institution of Chemical Engineers, Rugby, UK CODEN: 68IRAJ Conference written in English. CAN 132:37699 AN 1999:704681 CAPLUS (Copyright 2002 ACS)
Abstract
The choice of solvent has a large effect on the crystal morphol. of RDX explosive. Mol. dynamics simulations of a solvent layer of g-butyrolactone upon the {200} and {210} RDX crystal surfaces were performed to obtain a better understanding of the behavior of solvent mols. near a crystal surface. The av. potential energy of the solvent mols. near the surfaces was higher than in the solvent bulk. The surface induces a potential energy change in the solvent layer. This surface-induced potential energy change might be an adequate solvent effect parameter to use in the prediction of the morphol. importance of a crystal surface. From the calcd. surface-induced potential energy changes, it follows that the {210} face is morphol. more important than the {200} surface. This agreed well with the obsd. exptl. RDX morphol. grown in the solvent g-butyrolactone.
Bibliographic Information
Antisolvent crystallization of the explosive compound RDX. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft University of Technology, Delft, Neth. International Symposium on Industrial Crystallization, 14th, Cambridge, United Kingdom, Sept. 12-16, 1999 (1999), 1960-1972. Publisher: Institution of Chemical Engineers, Rugby, UK CODEN: 68IRAJ Conference written in English. CAN 132:37698 AN 1999:704678 CAPLUS (Copyright 2002 ACS)
Abstract
RDX crystals were produced by antisolvent crystn. with either acetone or g-butyrolactone as the solvent and water as the antisolvent. Prodn. rates up to 38 g/L-h with acetone and 96 g/L-h with g-butyrolactone were achieved at a residence time of .apprx.30 min. The single crystals have a rather large av. size for such an antisolvent crystn. process. Attrition of the larger crystals reduces the quality of the crystals. In addn. to unagglomerated single crystals, the product contained a considerable amt. of agglomerated crystals.
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Preparation of ultra-fine nitroamine explosives by using high-speed impinging stream. Zhang, Xiao-Ning; Xu, Geng-Guang; Wang, Ting-Zeng. Beijing Institute of Technology, Beijing, Peop. Rep. China. Hanneng Cailiao (1999), 7(3), 97-99,102. CODEN: HACAFQ ISSN: 1006-9941. Journal written in Chinese. CAN 131:339045 AN 1999:689401 CAPLUS (Copyright 2002 ACS)
Abstract
The sub-micron ultra-fine particles of nitroamine explosives (HMX and RDX) were prepd. by using high-speed impinging stream. The fundamental principle and characteristic of this method were analyzed. The granularity and shape of the ultra-fine explosive particles obtained were tested with laser-sedimentograph and scanning electronic microscope.
Bibliographic Information
Crystallization and characterization of energetic materials. Van der Heijden, A. E. D. M. TNO Prins Maurits Laboratory, Research Group Pyrotechnics and Energetic Materials, Rijswijk, Neth. Current Topics in Crystal Growth Research (1998), 4 99-114. CODEN: CTCRFJ Journal; General Review written in English. CAN 131:259565 AN 1999:646019 CAPLUS (Copyright 2002 ACS)
Abstract
A review, with 85 refs., of the general aspects of crystn. of energetic materials, esp. explosives and oxidizers, driven by the need to develop less-sensitive materials. Topics discussed include soly., nucleation and crystal growth mechanisms, layer growth, rough growth, crystn. techniques (e.g., melt, cooling, evaporative, pptn., drowning out, supercrit., and quasi-emulsion crystn.), prediction of crystal shape, plastic explosives, formation of inclusions and dislocations, examples of crystn. of energetic materials, polymorphism, crystal size distribution, particle shape, crystal perfection, purity, thermal stability, and hazard properties of crystd. explosives. Compds. discussed include ammonium nitrate, TNT, RDX, HMX, hydrazinium nitroformate, hexanitrostilbene, HNIW, and NTO.
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Fluid extraction with supercritical carbon dioxide for recovery of TNT from high explosives. Morris, Jeffrey B. (United States Dept. of the Army, USA). U.S. (1999), 10 pp. CODEN: USXXAM US 5953679 A 19990914 Patent written in English. Application: US 97-840779 19970416. CAN 131:186997 AN 1999:582734 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5953679 A 19990914 US 1997-840779 19970416
Abstract
TNT is recovered from high explosives contg. TNT by supercrit. fluid extn. with CO2 at a temp. above the m.p. of TNT, preferably at .apprx.85° and .apprx.37.4 MPa. The TNT can be recovered from such TNT-contg. explosives as Compn. B, Compn. B3, Cyclotol, Octol, Tritonal, and Torpex, in which a warhead to be decommissioned is held in an inverted position, and supercrit. CO2 is led through channels in the warhead. RDX can often be recovered as a CO2-insol. fraction.
Bibliographic Information
Solubility Determination of TNT and Wax and Their Fractionation from an Explosive Material Using a Supercritical Fluid. Ashraf-Khorassani, Mehdi; Taylor, Larry T. Department of Chemistry, Virginia Polytechnic Institute and State University, Blacksburg, VA, USA. Journal of Chemical and Engineering Data (1999), 44(6), 1254-1258. CODEN: JCEAAX ISSN: 0021-9568. Journal written in English. CAN 131:301221 AN 1999:574255 CAPLUS (Copyright 2002 ACS)
Abstract
The solubilities of 2,4,6-trinitrotoluene (TNT) and wax were measured in supercrit. carbon dioxide (CO2) under nine static conditions of pressure (13.8, 25.0, and 37.9 MPa) and temp. (35, 50, and 70°). The concns. of each component were detd. off-line via UV (TNT) and evaporative light scattering (wax) detection. The soly. of TNT was an order of magnitude higher than that of wax. Gas chromatog. assay of the wax ext. revealed that only the lower mol. wt. components dissolved. Fractionation of the TNT and wax from an explosive material (Compn. B, contg. 59.5 wt.% RDX and 39.5 wt.% TNT) was attempted by making incremental increases in CO2 d. Although TNT and wax could be easily isolated from RDX, attempts to sep. TNT from wax were not totally successful. More specifically, the initial fractions contained lower mol. wt. wax components in addn. to major amts. of TNT. Since the percentage of TNT was .apprx.50 times the amt. of wax, later fractions were 100% TNT, although most of the TNT was removed at the lower densities.
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Recovery of acetic acid from spent liquor of cyclotetramethylene tetranitramine plant. Rajopadhye, M. V.; Hima, P. R.; Syal, R. K. Materials Research Laboratory, Pune, India. Chemical Engineering World (1999), 34(5), 81-86. CODEN: CEWOF5 Journal written in English. CAN 131:189044 AN 1999:520590 CAPLUS (Copyright 2002 ACS)
Abstract
A technol. for wastewater treatment and recovery of acetic acid from the effluent of the explosive cyclotetramethylene tetranitramine (HMX) plant was developed. At pH 2.8, HNO3, present in the spent liquor, is completely neutralized. The dild. acetic acid is recovered (greater than 85%) in a single-stage distn. under reduced pressure. The residues contg. all impurities including the explosives RDX/HMX are sepd. by cooling and filtration. Diln. of the residues with water enhances the pptn. of the explosives. From the safety point of view and for efficient recovery, spent liquors with higher acid concn. must be dild. to acetic acid concns. of .apprx.25-30% by water addn. prior to distn. A pilot plant with a capacity of 2000 L/day effluent is in operation.
Bibliographic Information
Recycling of nitramines at Bofors Explosives AB. Sjoberg, Per. Bofors Explosives AB, Karlskoga, Swed. Editor(s): Johansson, Stig R. Proceedings of the International Disposal Conference, 1st, Lund, Swed., Nov. 12-13, 1997 (1999), Meeting Date 1997, 133-136. Publisher: Sektionen foer Detonik och Foerbraenning, Combustion Institute, Billdal, Swed CODEN: 67YNAC Conference written in English. CAN 131:161104 AN 1999:502652 CAPLUS (Copyright 2002 ACS)
Abstract
Bofors Explosives has reclaimed 50 tonnes of nitramines from destroyed ammunition. The process was developed and is patented by Bofors Explosives. All worked-up nitramines have been reused in com. applications where otherwise freshly synthesized nitramines would have been used. The work-up process produces nitramine which is pure and chem. and phys. indistinguishable from freshly synthesized ones. The operation could be scaled up considerably if the recycled nitramines are accepted by the military for use in new ammunition. The military require freshly synthesized nitramines.
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Study on preparation of ultrafine particle of explosive by high-speed impinging stream technology. Zhang, Xiaoning; Wang, Weimin; Xu, Gengguang. Department of Mechanical and Electronic Engineerig, Beijing Institute of Technology, Beijing, Peop. Rep. China. Huozhayao Xuebao (1999), 22(3), 1-3. CODEN: HUXUFP Journal written in Chinese. CAN 131:172278 AN 1999:464551 CAPLUS (Copyright 2002 ACS)
Abstract
The prepn. of sub-micron ultrafine particle of explosive by high-speed impinging stream technol. was studied. The particle sizes of ultrafine HMX and RDX were detd.
Bibliographic Information
Mannich condensation reactivity of DPT nitrolysis fragments. Zhang, Yuejun; Zhou, Weilian; Wen, Jinquan. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1997), 23rd 999-1007. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 130:298956 AN 1999:154372 CAPLUS (Copyright 2002 ACS)
Abstract
The two kinds of different nitrogen atoms of amino groups in DPT (dinitropentamethylenetetramine) mol. had been labeled with 15N atoms, resp., in order to distinguish Mannich reactivity of fragments formed in DPT nitrolysis process. The nitrolysis fragments produced in DPT nitrolysis process could condense with urea or nitrourea to form product Keto-RDX. With the aid of mass spectrum isotope anal., the isotope distribution and abundance of 15N tracer atoms in product Keto-RDX and reactant DPT could be detd. The research results showed: nitrogen atoms of the trimethylene amino groups in DPT mol. appeared 100% in the 4 position in product Keto-RDX mol., but nitrogen atoms of the nitroamino groups in DPT mol. disappeared completely in the product Keto-RDX mol.
Bibliographic Information
Studies on the mechanism of synthesizing Keto-RDX in direct preparation method. Zhang, Yuejun. School of Chemical Engineering, Nanjing University of Science and Technology (NUST), Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1997), 23rd 987-998. CODEN: PPYSD7 ISSN: 0270-1898. Journal; General Review written in English. CAN 130:298931 AN 1999:154371 CAPLUS (Copyright 2002 ACS)
Abstract
A review with 19 refs. of the recent progresses of mechanistic researches of synthesizing Keto-RDX in direct prepn. method using urotropine and urea as reactants were systematically described in this paper. The evidences of reaction forms of urotropine and urea in the reaction to form resultant Keto-RDX were presented in several aspects: the active intermediates, the relationships between intermediate structures and reactivities, and the 15N trace atoms, etc.. The nitrolysis fragments N,N-dimethylolamines and their imine cations formed during the urotropine nitrolysis process were active intermediates from urotropine. And the product of nitrating urea or nitrourea, N,N'-dinitrourea also was an active intermediate. Keto-RDX was synthesized via Mannich condensation of the above active intermediates in strong acidic media.
Bibliographic Information
Missile system reclamation and recycling. Melvin, William S.; Freeman, Charles W.; Wright, Jeffrey S. U.S. Army Aviation and Missile Command (AMCOM) Missile Research, Development, and Engineering Center Propulsion and Structures Directorate, AMSAM-RD-PS-R, Redstone Arsenal, AL, USA. CPIA Publ. (1998), 674(Vol. 1, 1998 JANNAF Propellant Development & Characterization Subcommittee and Safety & Environmental Protection Subcommittee Joint Meeting, Vol. 1), 411-421. CODEN: CPPUDT ISSN: 0272-5118. Journal written in English. CAN 130:200413 AN 1999:80588 CAPLUS (Copyright 2002 ACS)
Abstract
This report describes the implementation, testing, and evaluation of environmentally friendly procedures and processes for complete missile system demilitarization and recycling of recovered ingredients and hardware components. Redstone Arsenal facilities and AMCOM developed technologies to support these efforts. The vast majority of the Army missile systems are full up rounds. The demilitarization approach addresses the entire missile system. Loaded rocket motors and cases are considered a subset of the total missile system. Warheads, rocket motors, guidance and control packages, shipping containers, and launch tubes will all be recycled. In contrast to missile system destruction approaches, where neither products nor assocd. values are recovered, this Army initiative includes both military and com. market reuse options for deriving max. product values of reclaimed ingredients and components. The AMCOM liq. ammonia-based, ingredient extn. and reclamation process for rocket propellant recycling has been integrated into a Missile System Recycling Facility at Redstone Arsenal. This propellant reclamation technol. has successfully completed full scale, class 1.3 MLRS and class 1.1 Hellfire rocket motor recycling demonstrations. The fully operational AMCOM pilot plant validated the closed-loop reclamation process by efficiently extg. and recovering 100% of the ammonium perchlorate (AP) and aluminum/binder from the MLRS propellant. This pilot facility fully achieved its design requirements. Test demonstrations confirmed the operational capability to process greater than 200 lb of AP composite propellant from a full scale MLRS rocket motor in a single batch. Pilot demonstrations have validated its operational capability by the processing of 100 lb batches of nitrate ester plasticized, HMX/RDX nitramine propellant from Hellfire rocket motors. Complete missile system recycling demonstrations using 60 TOW missiles are in progress. Pilot demonstration efforts have confirmed that strategically valuable fuel and oxidizer ingredients (such as HMX, RDX, AP, aluminum/rubber binder) can be safely and efficiently recovered from Army tactical rocket motors. The AMCOM missile system recycling technol. is directly applicable to the vast majority of rocket motors in the Army, other DoD, and foreign missile inventories. With emphasis on reclamation instead of destruction, the liq. ammonia process is a near-optimal soln. for environmentally sound rocket motor disposition.
Bibliographic Information
A fiber optic biosensor for multianalyte detection: importance of preventing fluorophore aggregation. Bakaltcheva, Irina B.; Shriver-Lake, Lisa C.; Ligler, Frances S. Geo-Centers, Incorporated, Rockville, MD, USA. Sens. Actuators, B (1998), B51(1-3), 46-51. CODEN: SABCEB ISSN: 0925-4005. Journal written in English. CAN 130:211443 AN 1998:815678 CAPLUS (Copyright 2002 ACS)
Abstract
Individual assays for the detection of the explosives RDX and TNT with a fiber-optic biosensor were developed. In order to develop an assay for simultaneous detection of RDX and TNT, a mixt. of the fluorescent-labeled analogs Cy5-EDA-RDH (hapten) and Cy5-EDA-TNB used in the individual assays was passed over the sensor that used anti-RDX and anti-TNT fiber probes connected in series. There was an increased total fluorophore concn. in the mixt., which resulted in a significant increase in the normalized signal compared to that produced by a single fluorophore. Aggregation of the amphiphilic fluorophores in the mixt. on the surface of the fiber optic probe was a possible reason for the obsd. effect. The use of nonionic (Tween 20) and ionic detergents (deoxycholic acid) to block aggregate formation and to allow detn. of RDX and TNT was examd. Use of the ionic detergent deoxycholic acid can help prevent fluorophore aggregation.
Bibliographic Information
Recovery/reuse of energetics from military munitions. Burch, Dan; Griggs, John; Johnson, Mike; Sims, Keith. Naval Surface Warfare Center, Crane Division (Code 4073), Crane, IN, USA. Proc. Int. Pyrotech. Semin. (1998), 24th 101-112. CODEN: PPYSD7 ISSN: 0270-1898. Journal; General Review written in English. CAN 129:278152 AN 1998:574325 CAPLUS (Copyright 2002 ACS)
Abstract
A review, with 8 refs., of methods for recovery and reuse of propellants and explosives from military munitions. Disassembly technol. using an abrasive waterjet was developed by the University of Missouri-Rolla (UMR) which can cut through projectiles and other munition items. Testing was performed using an abrasive slurry waterjet to cut the tracers and fuses off of Navy 40mm projectiles in order to reclaim the TNT. In addn., UMR has developed high-pressure water technol. to remove explosives and high-energy propellants from projectiles, warheads, and rocket motors. Other removal technologies being explored are microwave melt out and induction heating. Several projects are underway to process the reclaimed explosive from the waterjet washout process and other removal processes. This includes the mech. reprocessing of the PBXN-106 into two sep. explosive products, a dimensional stone mining explosive, boosters for insensitive blasting agents, high-purity HMX from reclaimed LX-14 and Trident I rocket motor formulations, and RDX from PBXN-106 and Compn. A3. Possible com. products manufd. from recovered military explosives included sporting powder, oil-gas well perforation charges, and fertilizer from reclaimed nitrocellulose-based gun propellants. Other projects currently being explored at the lab/bench scale include catalytic hydrotreating technol. to convert Explosive D (ammonium picrate) contained in Navy projectile to higher value products and the recovery of magnesium from illumination and decoy flares for reuse in the military or for com. applications.
Bibliographic Information
Process safety management on spray system to produce ultrafine RDX powder. Hong, Yaw-Shun; Huang, Chen-Chia; Chang, Fang-Mo; Luo, Shen-Kay; Chen, Sun-I. Department of Applied Chemistry, Chung Cheng Institute of Technology, Taoyuan, Taiwan. Huoyao Jishu (1997), 13(2), 37-47. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 129:97364 AN 1998:393643 CAPLUS (Copyright 2002 ACS)
Abstract
Spraying is an useful fabrication technique to obtain ultrafine powd. RDX. A process safety management program for the process involved mech. integrity information, std. operation procedures, safety systems, and maintenance and emergency planning. Following the management procedure, it was possible to reduce manufg. hazards.
Bibliographic Information
Recrystallization technology of powdered RDX. Wang, Jianlong; Xu, Chunyan. North China Institute of Technology, Taiyuan, Peop. Rep. China. Huabei Gongxueyuan Xuebao (1997), 18(3), 262-265. CODEN: HUGXFH ISSN: 1006-5431. Journal written in Chinese. CAN 129:83380 AN 1998:365791 CAPLUS (Copyright 2002 ACS)
Abstract
The technol. of producing powd. RDX by recrystn. was studied, with emphasis on the factors that affect the quality of the product.
Bibliographic Information
Recovery and reuse of rocket propellants. Melvin, William S.; Starling, Jarel P. U.S. Army Missile Command, Research, Development, and Engineering Center, Propulsion Directorate, Redstone Arsenal, AL, USA. NASA Conf. Publ. (1997), 3349(Second Aerospace Environmental Technology Conference, 1996), 193-201. CODEN: NACPDX ISSN: 0191-7811. Journal written in English. CAN 128:296643 AN 1998:300290 CAPLUS (Copyright 2002 ACS)
Abstract
An ongoing process development effort by the U.S. Army Missile Command (MICOM) to support environmentally safe rocket motor demilitarization demonstrations was discussed. This process is used to recover oxidizer and fuel ingredients from tactical and strategic class 1.1 and 1.3 solid propellants for recycle/reuse. The closed-loop demilitarization method uses liq. anhyd. ammonia as the processing solvent for ingredient extn. and recovery. A pilot-plant facility was designed and constructed in Magna, Utah, to demonstrate this technol. using Multiple Launch Rocket System (MLRS) and Chaparral tactical solid rocket motors. In July 1996, the pilot plant successfully completed full-scale MLRS propellant testing in a batch process mode at rates approaching 90 kg/h. Process descriptions of the integrated Class 1.1/1.3 rocket motor demilitarization system involving propellant removal, ingredient extn., binder sepn., oxidizer recovery, and solvent regeneration were provided. Test results demonstrating the ability of energetic products recovered by this process to be recycled into other products, and future work plans in support of this program also, were included.
Bibliographic Information
Recovering of components from plastic bonded propellants. Bohn, Manfred A.; Schweppe, Rainer; Weisweiler, Werner. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 175-185. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:219125 AN 1998:219158 CAPLUS (Copyright 2002 ACS)
Abstract
In order to recover the components of so-called "plastic-bonded propellants" (e.g., cryst. energetic materials bonded in a chem. three-dimensional crosslinked polyurethane matrix), the polyurethane matrix is broken solvolytically with water and alk. water (0.05 N-0.5 N NaOH) at 130-170°. Using a model rocket propellant, consisting of a polyether polyol mixt. (Lupranol 1000/2021) cured with Desmodur T80 and filled with 60 wt.% ammonium perchlorate (AP), 84-90% of the polyether polyol component was recovered, and 98% of the AP content subsequently detd. in the aq. hydrolyzate. The polyether polyols were nearly unchanged at 170° for 2 h, as shown by the molar mass distributions (detd. by gel permeation chromatog.). The solid gun propellant KHP (86 wt.% RDX-14 wt.% GAP-Desmodur N100 binder) was solvolyzed at 130, 150, and 170° with pure water and with 0.05 N NaOH for 10, 30, and 60 min. RDX was recovered in high yields and high purity. Under similar hydrolytic conditions, GAP did not behave in the same way as the Lupranol polyether polyols. The molar mass distribution of GPA was broadened and its azide content reduced, as detd. via IR absorption of the asym. N3 stretching vibration, and by differential scanning calorimetry, in both cases in relation to the azide content of the unreacted GAP. Neither the GAP-N100 binder or GAP were recoverable. Under these conditions, the N3 group decompd., yielding a nitrene functionality which formed solvolytically not scissionable C-N bonds by intermol. insertion reactions. The main gaseous reaction products in the solvolysis of KHP were N2, and N2O, with a little CO2, O2, and CO, and small amts. of NH3 and HCHO. The following ionic decompn. products were obsd.: NO2-, NO3-, HCOO- and NH4+.
Bibliographic Information
Value added products from reclamation of military munitions. Burch, D.; Johnson, M.; Sims, K. Crane Division (Code 4073), Naval Surface Warfare Center, Crane, IN, USA. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 159-163. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:219168 AN 1998:219156 CAPLUS (Copyright 2002 ACS)
Abstract
The Department of Defense has a backlog of excess, obsolete and unserviceable munitions for disposal. For many of these munition items the only method of disposal is open burning/open detonation (OB/OD) which destroys valuable resources which can be reclaimed and converted to useful products. The Crane Division, Naval Surface Warfare Center (NAVSURFWARCENDIV Crane) in support of the Navy's Ordnance Reclamation Program and the Joint Service Large Rocket Motor Disposal Program has been developing technol. for the removal and reclamation of the energetics from munitions. The University of Missouri-Rolla has demonstrated the use of high pressure waterjet technol. for removal of PBX explosives from projectiles and warheads. Development work is nearing completion for demonstrating the capability to remove Class 1.1 propellant from strategic rocket motors using high pressure waterjets. Current projects are under way focusing on resource recovery and recycling (R3) of the reclaimed energetics while minimizing disposal. The current reclamation projects include reformulation of the explosives and Class 1.1 propellants into com. blasting agents, reuse of Navy gun propellant for various applications including agriculture and oil-gas well stimulation. Other projects include the recovery of RDX/HMX from Class 1.1 explosives and propellants and the conversion of Explosive D into higher value products. Lab/bench scale testing has been completed on many of these processes, and for some pilot scale demonstrations have been or are scheduled to be completed during 1997.
Bibliographic Information
Solubility and phase behavior of PEP binders in supercritical carbon dioxide. Dinoia, Todd P.; Mchugh, Mark A.; Cocchiaro, James E.; Morris, Jeffrey B. Department of Chemical Engineering, The Johns Hopkins University, Baltimore, MD, USA. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 151-158. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:232440 AN 1998:219155 CAPLUS (Copyright 2002 ACS)
Abstract
Soly. and phase behavior data up to 300° and pressures to 3000 bars were presented for various propellant, explosive, and pyrotechnic (PEP) binder polymers in supercrit. CO2 with and without modifiers. The binder polymers investigated were polyethylene (PE), oxidized PE, poly(urethane), cellulose acetate butyrate (CAB), poly(vinylidene fluoride-co-hexafluoropropylene) with .apprx.20 mol% hexafluoropropylene (Fluorel and Viton), and poly(chlorotrifluoroethylene-co-vinylidene fluoride) with 24 mol% (Kel-F 800) and 69 mol% (Kel-F 3700) vinylidene fluoride. CO2 has the characteristics of a weak polar solvent which does not dissolve polyethylene although it is can dissolve low-mol.-wt. nonpolar waxes. However, CO2 is not polar enough to dissolve very polar polymers, such as oxidized PE, polyurethane, Kel-F 3700, and CAB (cellulose acetate butyrate). Moderately polar poly(vinylidene fluoride-co-hexafluoropropylene) and Kel-F 800 are sol. in CO2. The soly. of these two copolymers can be further enhanced using acetone as a modifier with CO2. Addnl., oxidized PE is sol. in CO2 with acetone and ethanol as modifiers, but temps. .gtorsim.200° are needed. The fact that many of these polymers are sol. in neat CO2 suggests the potential for a substantial impact upon environmentally sound processing technologies for polymer-based PEP materials.
Bibliographic Information
A study on the preparation of superfine RDX. Gou, Ruijun; Zhang, Jinglin; Han, Baocheng. North China Institute of Technology, Taiyuan, Peop. Rep. China. Editor(s): Feng, Changgen; Ou, Yuxiang; Zeng, Qingxuan. Theory Pract. Energ. Mater., [Proc. Int. Autumn Semin. Propellants, Explos. Pyrotech.], 2nd (1997), 37-40. Publisher: Publishing House of Ordnance Industry, Beijing, Peop. Rep. China CODEN: 65OYAF Conference written in English. CAN 128:142781 AN 1998:84547 CAPLUS (Copyright 2002 ACS)
Abstract
A process parameter study on prepn. of superfine cyclotrimethylenetrinitramine (RDX) was conducted using solvent-nonsolvent type of recrystn. Change in the process conditions caused significant changes in the particle size distribution, sp. surface area, bulk d. and residual solvent content. The particle size of RDX can be in the range of 2.apprx.0.1 mm by controlling the process conditions.
Bibliographic Information
Demilitarization facility for the environmental and acquisition life cycle analysis of explosives and munitions systems. Jeffers, Scott R.; Corley, John. Energetic Materials Branch (WL/MNME), Eglin AFB, FL, USA. Proceedings - International Symposium on Energetic Materials Technology, Phoenix, 1995 (1995), 337-341. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117024 AN 1998:63032 CAPLUS (Copyright 2002 ACS)
Abstract
As part of an environmental life-cycle anal. of the munitions design, manuf., and disposal, an aggressive pilot-scale demilitarization program was developed to recover, recycle, reuse, or dispose of explosives and munitions. Technologies developed at the facility will transition to industry or government agencies tasked to execute demil of prodn. weapons systems. The concurrent development of advanced energetic materials for munitions applications and recovery/treatment/disposal technologies for these materials was essential if they are to be incorporated into inventory systems. The technologies used in this program are: (1) high-pressure water washout for removal of the bulk explosive from the munition containers, (2) high-pressure water maceration for size redn. of bulk material for further processing and for the recovery of water-sol. materials, (3) hydrolysis to remove remaining explosive residues from the sides of the munition allowing for container recovery and reuse, (4) molten salt destruction for an environmentally compatible way to completely destroy and dispose of the unrecoverable materials, (5) and non-thermal discharge plasma processing as a supplement to molten salt destruction for controlling any acid gas formation.
Bibliographic Information
Hazards analysis of an integral Class 1.1/1.3 rocket motor demilitarization and ingredient recovery system using ammonia. Stevens, P. M.; Reed, M. H.; Losee, L. A.; Graul, E. R.; Mitchell, D. H. Global Environmental Solutions (Alliant Techsystems), Magna, UT, USA. Proc. - Int. Symp. Energ. Mater. Technol. (1995), 326-336. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117007 AN 1998:63027 CAPLUS (Copyright 2002 ACS)
Abstract
Research efforts conducted at the bench-scale have demonstrated the U.S. Army Missile Command (MICOM) near-crit. fluid technol. (using liq. anhyd. NH3) as a viable method of demilitarizing solid rocket motors for recovery of waste rocket propellants. This method was used to recover valuable ingredients, such as HMX, RDX, ammonium perchlorate, and aluminum/binder crumb from tactical and strategic Class 1.1 and 1.3 solid propellants. Ongoing hazards anal. efforts were reported. Hazards anal. testing has characterized the sensitivity of propellants, process streams, and extd. materials. Hazards anal. techniques, such as logic diagrams, and failure modes and effects anal., have identified credible hazards in the equipment design and pilot plant operations. These potential hazards were tracked by a closed loop system and were mitigated by design features or operating controls. Major hazards identified included: (1) shock initiation of ammonium perchlorate-ammonia solns. and undissolved BTTN, (2) ammonia jet impingement heating, (3) reaction of NH3 with nitroglycerin in Class 1.1 propellants, (4) spills and leaks of ammonia with hazard to operators, (5) instability of byproduct ammonium nitrite, (6) oxygen depletion by N2 displacement, (7) startup-shutdown-sampling-maintenance operation, and (8) abnormal situations and contingency plans.
Bibliographic Information
Crystallization of energetic materials; the effect on stability, sensitivity and processing properties. Meulenbrugge, Jan; van der Steen, Albert; van der Heyden, Antoine. TNO Prins Maurits Lab., Rijswijk, Neth. Proc. - Int. Symp. Energ. Mater. Technol. (1995), 297-302. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117022 AN 1998:60343 CAPLUS (Copyright 2002 ACS)
Abstract
Results were presented from expts. on crystn. of HNF (hydrazinium nitroformate) and RDX, and the effect of crystn. on the properties of these materials. Control of the crystn. process for HNF will improve the particle shape, the stability and the processability. Other parameters, like sensitivity, are much more reproducible and the control over the particle size will be improved. For RDX esp., the processability and the sensitivity to shock were improved when the particles are made spherical or treated in another way. Photographs of the crystals were presented as well as the properties of the various batches.
Bibliographic Information
Preparation and characterization of an AN-containing IMX. Zhang, Yian; Zhao, Shengxiang; Wu, Zhixing; Zhang, Chengwei. Xian Modern Chem. Res. Inst., Xian, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 75-80. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:265104 AN 1997:588770 CAPLUS (Copyright 2002 ACS)
Abstract
An intermol. explosive (IMX) mixt., XR-30, composed of phase-stabilized ammonium nitrate, ethylenediamine dinitrate, RDX, and a melt-casting agent, was prepd. conventionally, with filling d. greater than 98% theor. max. d. The formulation is a eutectic composite explosive. Its impact sensitivity, H50, is 68.5 cm, with a friction sensitivity 4% probability to reaction. The max. detonation velocity and pressure calcd. with N-M-Q method were 8.22 km/s and 28.9 GPa, resp.
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Synthesis of 2,4,6-trinitro-2,4,6-triazacyclohexanone (keto-RDX) from DPT and PHX. Zhang, Yuejun; Xie, Chunping. School Chem. Engineering, Nanjing Univ. Sci. & Technology, Nanjing, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 63-69. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:250216 AN 1997:588757 CAPLUS (Copyright 2002 ACS)
Abstract
A method was given for synthesis of 2,4,6-trinitro-2,4,6-triazacyclohexanone (Keto-RDX) from 1,5-methylene-3,7-dinitro-1,3,5,7-tetraazacyclononane (I) [DPT], and urea (or nitrourea) in several kinds of nitrating reagents. Primary investigations were carried out for the reaction forms of nitrolysis fragments I and 1,7-diacetoxy-2,4,6-trinitro-2,4,6-triazacycloheptane (II), and on the mechanism of forming byproduct. The nitrolysis fragments N,N-dihydroxymethylamines [RN(CH2OH)2, N is not NO2] that were not directly substituted by nitro groups condensed with urea or nitrourea to form keto-RDX, whereas N,N-dihydroxymethylnitroamine [O2NN(CH2OH)2] did not. Using I as a reactant, the yield of Keto-RDX was 69% (one mole keto-RDX per mol reactant); the byproducts were HMX, RDX, and smaller mol. fragments. Using II, no keto-RDX product and no cyclonitroamine byproducts were obtained.
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Technical research to class 5 RDX crystal in nitric acid system. TianLong, Si Ma; Jie, Zhao Yong. Dep. Technique, Yinguang Chem. Corp., Baiying City, Gansu, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 54-62. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:250215 AN 1997:588746 CAPLUS (Copyright 2002 ACS)
Abstract
An improved process for producing RDX by direct oxidn. of hexamethylenetetramine was theor. based on the soln. chem. performance. Using this method, RDX can be made in one step, with a quality that complies with class 5 requirements of USA Military Std. USA-R-398C. By controlling the diln. process, the RDX has a granularity of .gtorsim.85% less than 10 mm.
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Evaluation of leaving groups in nitramine synthesis. An experimental and theoretical (AM1) study. Piacenza, G.; Jacob, G.; Girard, A.; Graindorge, H.; Gallo, R. Fac. Sciences Saint-Jerome, Marseille, Fr. Int. Annu. Conf. ICT (1997), 28th(Combustion and Detonation), 124.1-124.12. CODEN: IACIEQ ISSN: 0722-4087. Journal written in English. CAN 127:190355 AN 1997:522194 CAPLUS (Copyright 2002 ACS)
Abstract
An exptl. study of nitrolysis was conducted with 12 selected leaving groups located at the N atoms of hexahydro-s-triazine (a reasonably transposable mol. structure) using 7 nitrating media. Yields and limiting side reactions are given and discussed. A theor. study by semi-empirical quantum mech. calcn. (AM1) is made on this substitution reaction by NO2+ with a series of electrophilic leaving groups, the same as studied exptl. The nature, geometry, and energy of intermediates and of transition states are calcd. These results give a classification of leaving-group ability which is in good agreement with exptl. results. They allow a selection of leaving groups for nitrolysis and design of more efficient synthetic methods for prepg. high energy nitramines.
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Crystallization technology of Grade 5 RDX. Wang, Janlong; Ye, Yupeng. North China Inst. Tech., Taiyuan, Peop. Rep. China. Huozhayao (1997), 20(2), 14-15. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 127:68122 AN 1997:354693 CAPLUS (Copyright 2002 ACS)
Abstract
A technol. of producing Grade 5 RDX by crystn. was studied.
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Study on the nitrolysis of hexamethylenetetramine by NMR spectrometry. Part 2. Some new evidence of the intermediate of HOCH2NHNO2 as a possible precursor to RDX. Fang, Zhi Jie; Chen, Li; Wang, Shao Fang; Chen, Ju; Li, Fu Ping. Institute Chemical Engineering, University Science Technology, Nanjing, Peop. Rep. China. Propellants, Explos., Pyrotech. (1997), 22(2), 78-80. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 127:83507 AN 1997:332267 CAPLUS (Copyright 2002 ACS)
Abstract
The RDX yield from nitrolysis of hexamethylenetetramine (HA) together with methylenedinitramine (MDNA) in 90% HNO3 was greater than 100%. MDNA decompd. completely in 90% HNO3, forming O(CH2ONO2)2, whereas in HNO3-NH4NO3 system, the decompd. fragments of MDNA condensed to form RDX. Based on a comparison of the exptl. results to the 1H-NMR spectra obtained by following the decompn. reaction of MDNA with HNO3, the intermediate, HOCH2NHNO2, was postulated as one of the possible precursors to RDX both in Hale and in K process.
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Improvement of combustion property of double base propellant with N,N'-dinitropiperazine. Pan, Wenda; Chang, Jingxiang. Xi'an Modern Chemistry Research Inst., Xi'an, Peop. Rep. China. Guti Huojian Jishu (1997), 20(1), 36-40. CODEN: GHJIFL ISSN: 1006-2793. Journal written in Chinese. CAN 126:253075 AN 1997:244968 CAPLUS (Copyright 2002 ACS)
Abstract
This paper presents the formulation and prepn. method of the double base propellant contg. N,N'-dinitropiperazine (DNP) and investigates the effects of DNP on the energy and combustion properties of the double base propellant. Results show that DNP can decrease burning temp. of double base propellant and increase sp. vol., but its specific impulse is almost const. or has a little decrease. DNP can significantly decrease the burning rate and pressure exponent of the double base propellant.
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Preparation of RDX of different particle-size by recrystallization in nitric acid solution. Rui, Jiuhou; Liu, Yuhai; Wu, Siaoqing. North China Inst. Technol., Taiyuan, Peop. Rep. China. Baopo Qicai (1997), 26(1), 10-13. CODEN: BAQIEJ ISSN: 1001-8352. Journal written in Chinese. CAN 126:279788 AN 1997:219443 CAPLUS (Copyright 2002 ACS)
Abstract
A method of prepn. of RDX crystals of different particle size distribution by recrystn. in aq. HNO3 was suggested. The relationship between RDX crystal nucleation, crystal fault formation, and the amt. of included acid in RDX crystals was discussed. Special attention was paid to the process conditions which affected the granularity, shape, and the amt. of included acid in RDX crystals (e.g., the crystn. temp., stirring speed, and the diln. rate). RDX crystals could be prepd. with less than 0.02% included acid.
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Supercritical fluid extraction of polar nitrogen containing-substances. Niehaus, M.; Teipel, U.; Bunte, G.; Krause, H.; Weisweiler, W. Fraunhofer Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Process Technol. Proc. (1996), 12(High Pressure Chemical Engineering), 345-350. CODEN: PTPREM ISSN: 0921-8610. Journal written in English. CAN 126:187773 AN 1997:79413 CAPLUS (Copyright 2002 ACS)
Abstract
Dynamic fluid extn. with supercrit. CO2 was investigated for the purifn. and prepn. of fine particles of polar nitrogen-contg. compds. (e.g., typical explosives and energetic compds. such as PETN, nitroguanidine, RDX, and 3-nitro-1,2,4-triazole). The two processes examd. were: (1) rapid expansion of supercrit. solns. (RESS), and (2) the gas-antisolvent (GAS) process. All explosives except nitroguanidine could be extd., although for RDX and 3-nitro-1,2,4-triazole, modifiers were necessary. The results demonstrated the high capacity of modified supercrit. CO2 as a solvent in RESS and GAS processes. Suitable modifiers must be examd. empirically.
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New Method for preparation of ultrafine RDX crystals. Rui, Jiuhou; Wang, Zeshan; Liu, Yuhai; Shi, Jie. School of Chemical Engineering, NUST, Nanjing, Peop. Rep. China. Nanjing Ligong Daxue Xuebao (1996), 20(5), 385-388. CODEN: NLIXET ISSN: 1005-9830. Journal written in Chinese. CAN 125:333433 AN 1996:686435 CAPLUS (Copyright 2002 ACS)
Abstract
A new method for the direct prepn. of ultrafine RDX crystals was described, in which RDX is dissolved in 98% HNO3 and then treated with water at 0-50°, during which fine and ultrapure RDX crystals ppt. Using the solvent (98% HNO3)-non-solvent (H2O) pptn. technique, 50 g-scale expts. were conducted. Depending on the crystn. condition chosen, ultrafine RDX crystals of 5 to .apprx.7 mm median particle diam. were prepd. Special emphasis was paid to the study of the process conditions affecting the granularity of the ultrafine RDX crystals (e.g., the crystn. temp., stirring speed, concn. of the soln. and the amt. of diln. water).
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New method for preparing submicron explosives - microemulsion method. Liu, Zhijian; Fan, Shijun. Xi'an Modern Chemistry Research Institute, Xi'an, Peop. Rep. China. Huozhayao (1996), 19(4), 12-13. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 125:252227 AN 1996:621954 CAPLUS (Copyright 2002 ACS)
Abstract
This paper presents, for the fabrication of ultrafine particle explosives, a novel method, the microemulsion method which yields 1.02-0.42 mm-particle explosives. In this paper, the theor. basis of the method and a physicochem. model for the ultrafine particle formation are elucidated, and also four basic compns. for microemulsion explosives are given.
Bibliographic Information
New method for improving the particle size of RDX. Zhang, Nanjiang. Huahei Inst. Technol., Taiyuan, Peop. Rep. China. Huozhayao (1996), 19(3), 23-24. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 125:252221 AN 1996:558168 CAPLUS (Copyright 2002 ACS)
Abstract
In the manufg. of RDX, crystal grain size of RDX is improved (increased) by adding to the crystn. soln. the surfactant dodecyl sodium sulfate.
Bibliographic Information
Extraction of explosives by supercritical fluids. Niehaus, M.; Teipel, U.; Krause, H.; Bunte, G. Fraunhofer Institut Chemische Technologie (ICT), Pfinztal, Germany. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 128.1-128.16. CODEN: IACIEQ Journal written in German. CAN 125:200039 AN 1996:514603 CAPLUS (Copyright 2002 ACS)
Abstract
The soly. parameters of explosives in supercrit. carbon dioxide are important for evaluation of novel techniques in manuf. and also in quant. anal. Efforts have been made to use the unique possibilities that supercrit. carbon dioxide offers, such as nontoxicity and therefore redn. of environmental pollution or low-temp. processing resulting in addnl. process safety. Also, the performance of explosives improves because of the minimization of contamination caused by conventional org. solvents with low vapor pressure. Supercrit. fluid extn. of the explosives pentaerythrityl tetranitrate (PETN), nitroguanidine (NIGU), RDX, and 3-Nitro-1,3,4-triazole (NTO) has been done in the dynamic mode with pure and modified carbon dioxide. All explosives except nitroguanidine have been extd., although for RDX and NTO use of modifiers proved to be necessary. Effective modifiers must be chosen empirically. The results show the high potential of supercrit. fluids as substitutes for org. solvents.
Bibliographic Information
Bench-scale cooling crystallization of RDX. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft Univ. of Technology, Delft, Neth. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 126.1-126.11. CODEN: IACIEQ Journal written in English. CAN 125:225933 AN 1996:514601 CAPLUS (Copyright 2002 ACS)
Abstract
Crystals of the explosive RDX were produced by bench-scale batch cooling crystn. and on the lab. scale using three solvents: (1) cyclohexanone, (2) cyclohexanone satd. (3 wt.%) water, and (3) g-butyrolactone. The morphol. of the RDX crystals was strongly dependent on the solvent and independent of the prodn. scale. Crystn. from cyclohexanone gaves block-like RDX crystals with large macrosteps, indicating blockage of growth. When crystn. takes place from cyclohexanone satd. with water, the macrostep formation seems to be eliminated. Comparison of the crystals growing from stagnant solns. and from the bench-scale expts. showed that the turbulence in the crystallizer, that leads to crystal collisions, has a large neg. influence on the formation of crystal inclusions, esp. at high solid loadings.
Bibliographic Information
Study on the nitrolysis of hexamethylenetetramine by NMR-spectrometry. IV. A novel mechanism of the formation of RDX from HA. Fang, Zhijie; Wang, Shaofang; Li, Fuping. Inst. Chemical Eng., Nanjing Univ. Sci. Technology, Jiangsu, Peop. Rep. China. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 89.1-89.7. CODEN: IACIEQ Journal written in English. CAN 125:172518 AN 1996:514567 CAPLUS (Copyright 2002 ACS)
Abstract
The mechanisms of the nitrolysis of hexamethylenetetramine (hexamine or HA) with nitric acid and with the mist. of nitric acid and ammonium nitrate to form 1,3,5-trinitro-1,3,5-triazacyclhexane (hexogen or RDX) were studied by NMR tracing. It was found that HA immediately disappeared, while RDX was formed gradually, which indicates the formation of some intermediates in the HA nitrolysis to give RDX. The chem. shift of the peaks in the 1H and 13C NMR tracing spectra disagreed with the possible cyclic-structure intermediates proposed by G. F. Wright (1969) and co-workers. Comparison of the 13C NMR spectra showed that the nitrolysis fragments in K process can be used to form RDX. Based on the results, structures of intermediates were proposed. All the evidences mentioned above suggested a novel mechanism of the formation of RDX form HA, i.e., the nitrolysis of HA first gives some open-chain methylenenitramine intermediates, and the condensation of the latter gives RDX under certain conditions.
Bibliographic Information
New nitration and nitrolysis procedures in the synthesis of energetic materials. Pagoria, Philip F.; Mitchell, Alexander R.; Schmidt, Robert D.; Coon, Clifford L.; Jessop, Edward S. Energetic mater. Cent., Lawrence Livermore Natl. Lab., Livermore, CA, USA. ACS Symp. Ser. (1996), 623(Nitration), 151-164. CODEN: ACSMC8 ISSN: 0097-6156. Journal written in English. CAN 125:37462 AN 1996:288534 CAPLUS (Copyright 2002 ACS)
Abstract
The development of new nitrolysis and nitration reagents are essential to the research and development of energetic materials. In this paper we describe the development of two new nitrolysis reagents, trifluoromethanesulfonic anhydride/HNO3/N2O5 and trifluoroacetic anhydride/HNO3/N2O5, which were uniquely successful in the nitrolysis of secondary amide groups to yield several new, bicyclic nitramines. An alternative method for the synthesis of secondary nitramines by the mild nitrolysis of N-tert-butoxycarbonyl (N-BOC) derivs. The attempted synthesis of 18O-labeled 2,4,6-trinitroltoluene using trifluoromethanesulfonic acid and NaN18O3 at elevated temps. resulted in incorporation of only two 18O atoms per TNT mol., indicating substantial oxygen exchange.
Bibliographic Information
A facile pressing technique for the preparation of small calibre dual role explosive charge. Kumar, A. S.; Samudre, S. S.; Waghmare, N. G.; Gharia, J. S. Explosives Res. and Development Laboratory, Pune, India. Propellants, Explos., Pyrotech. (1996), 21(2), 106-110. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 124:320938 AN 1996:286536 CAPLUS (Copyright 2002 ACS)
Abstract
Small-caliber shaped charges were prepd. by pressing of RDX-wax compns. The shaped-charge performance was considerably influenced by the d. gradient which is an inherent drawback assocd. with pressing. A new method, double-action pressing, was developed which overcomes this problem and is amenable for large-scale prodn. Properties of the charges prepd. by the different methods, esp. with respect to the d. gradient and performance against targets, were presented and discussed. The penetration performance was increased by 8-10% with explosives prepd. by the double-action pressing technique.
Bibliographic Information
Manufacture of HMX with high yield using byproducts from DPT nitrolysis. Xi, Meihong; Deng, Ning. Nanjing Univ. Sci. and Technol., Nanjing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 280-283. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347528 AN 1996:285175 CAPLUS (Copyright 2002 ACS)
Abstract
In the step-wise nitrolysis of DPT and hexamine (HA), the condensation of nitrolyzed segments of HA and linear nitramines produced in nitrolysis of DPT can increase in yield of HMX to 60% (counted by DPT) and yield of RDX to 75% (counted by HA). The presence of condensation is conformed in the nitrolysis of HA.
Bibliographic Information
Methods for the production of fine particle explosives. Ji, Liguo; Jiao, Qingjie; Cai, Ruijiao. Beijing Institute Technology, Beijing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 170-174. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347523 AN 1996:285153 CAPLUS (Copyright 2002 ACS)
Abstract
A ultrasonic generator and a sprayer are used in the prodn. of fine cryst. explosive. The cavity effect of ultrasonic is used to crush explosive particles while substituting stirring app. The recryst. process of explosive is controlled by the sprayer. The mechanism of ultrasonic and spraying jet is discussed. Fine particles of PETN and RDX having medium diams. less than 10 mm are manufd. in the process.
Bibliographic Information
Conformation of intermediate HOCH2NHNO2 from nitrolysis of hexamethylentetramine as possible precursor for RDX formation by NMR spectrometry study. Fang, Zhijie; Chen, Li; Wang, Shaofang; Chen, Ju; Li, Fuping. Institute Chemical Engineering, Nanjing University Science and Technology, Nanjing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 121-123. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347522 AN 1996:285144 CAPLUS (Copyright 2002 ACS)
Abstract
RDX manufd. from nitrolysis of hexamine together with methylenedinitramine (MDNA) in 90% nitric acid is reported. MDNA decompd. completely in 90% nitric acid, forming O(CH2ONO2)2, while in HNO3-NH4NO3 system the decompd. fragments of MDNA condensed into RDX. On the basis of the comparison of the exptl. results to the 1H NMR spectra obtained by following the decompn. reaction of MDNA with nitric acid, the intermediate, HOCH2NHNO2, was postulated as one of the possible precursors to RDX both in Hale and in K process.
Bibliographic Information
Detecting genotoxic activity in industrial effluents using the SOS Chromotest microplate assay. Legault, Richard; Blaise, C.; Trottier, S.; White, P. A. Cent. Saint-Laurent, Environment Canada, Montreal, Can. Environ. Toxicol. Water Qual. (1996), 11(2), 151-65. CODEN: ETWQEZ ISSN: 1053-4725. Journal written in English. CAN 124:335056 AN 1996:271876 CAPLUS (Copyright 2002 ACS)
Abstract
The SOS Chromotest, a cost-effective short-term bacterial genotoxicity screening assay, was performed to appraise its capacity for detecting the presence of sol. genotoxic activity in industrial effluent samples (org. and inorg. chem. plants, metallurgical plants, pulp and paper mills, municipal wastewater treatment plants). An optimized methodol., based on criteria taking into account b-galactosidase activity (the indicator of SOS gene induction), alk. phosphatase activity (the indicator of cytotoxicity), and two genotoxicity measurement end points (min. genotoxic concn. and max. induction factor), was employed to generate reliable results that overcame the potential interferences inherent to complex wastewaters. Of 48 effluent samples tested, 37 (77%) elicited a significant induction of the Escherichia coli PQ37 SOS response. Effluents from inorg. chem. plants and pulp and paper mills displayed the most potent responses, with and without metabolizing enzymes (S9 mix). In general, chem. data available for some wastewaters supported SOS Chromotest pos. responses. The genotoxic activity of whole effluents subjected to a 5-day aeration treatment was as high as that of native (un-aerated) samples, suggesting that sol. genotoxicants are relatively recalcitrant to oxidn., although redns. in genotoxic activity did occur. This study indicates that the SOS Chromotest is sufficiently sensitive to screen for the presence of sol. DNA-damaging agents in a wide variety of un-concd. wastewater samples.
Bibliographic Information
Relationship between crystallization and acidity for RDX. Lu, Yuexian; Chang, Zhihong. North China Inst. Technol., Taiyuan, Peop. Rep. China. Huozhayao (1996), 19(1), 15-18. CODEN: HUOZFT Journal written in Chinese. CAN 124:293627 AN 1996:254833 CAPLUS (Copyright 2002 ACS)
Abstract
Based on the technol. of RDX prepn. by nitrolysis of hexamethylenetetramine (HA), the effect of each factor in crystn. on the acidity of the product was investigated. By controlling the crystn. point and each factor in crystn., the acidity of large-grain product can be reduced such that the RDX product conforms to the appropriate American Military stds.
Bibliographic Information
Crystal growth of energetic materials during high acceleration. Lanzerotti, M. Y. D.; Autera, J.; Borne, L.; Sharma, J. ARDEC, U.S. Army, Picatinny Arsenal, NJ, USA. Mater. Res. Soc. Symp. Proc. (1996), 418(Decomposition, Combustion, and Detonation Chemistry of Energetic Materials), 73-8. CODEN: MRSPDH ISSN: 0272-9172. Journal written in English. CAN 124:206434 AN 1996:176813 CAPLUS (Copyright 2002 ACS)
Abstract
Studies of the growth of crystals of energetic materials under conditions of high acceleration in an ultracentrifuge were reported. When a satd. soln. is accelerated in an ultracentrifuge, the solute mols. move individually through the solvent mols. to form a crystal at the outer edge of the tube if the solute is more dense than the solvent. Since there is no evapn. or temp. variation, convection currents caused by simultaneous movement of solvent and solute are minimized and crystal defects are potentially minimized. Crystal growth is thus controlled by the g-level of the acceleration. In addn., soln. inclusions and bubbles migrate out of the satd. soln. as a result of the pressure gradient induced by the g-force. Results were presented for TNT, RDX, and TNAZ grown at high g from various solns.
Bibliographic Information
Granularity and spheroidization of RDX. Rui, Jiuhou; Ye, Yupeng; Liu, Yuhai; Gu, Jianliang. Sch. Chem. Eng., NUST, Nanjing, Peop. Rep. China. Nanjing Ligong Daxue Xuebao (1995), 19(6), 497-500. CODEN: NLIXET ISSN: 1005-9830. Journal written in Chinese. CAN 124:150101 AN 1996:63600 CAPLUS (Copyright 2002 ACS)
Abstract
A method was described for the direct prepn. of ball-grain RDX that afforded different particle size distributions. HNO3(98%) was reacted with a second acid to form a soln. of RDX in HNO3; the ball-grain RDX with different particle size distributions were then prepd. directly by making use of the technique of solvent/nonsolvent pptn. Expts. with scales of 50 g yield were carried out in the lab. The six classes of ball-grain RDX prepd. directly the acids met the American military specification qualities of the products. Special attention was paid to factors which affect the granularity and spheroidization of RDX (e.g., crystn. temp., stirer speed, and diln. rate).
Bibliographic Information
Recovery of ingredients from plastic-bonded propellants. Bohn, M. A.; Schweppe, R.; Weisweiler, W. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Int. Annu. Conf. ICT (1995), 26th(Pyrotechnics), 44/1-44/32. CODEN: IACIEQ Journal written in German. CAN 124:33073 AN 1995:866216 CAPLUS (Copyright 2002 ACS)
Abstract
The possibility of recovery of energetic ingredients and binders from urethane-bonded propellants was examd. in a process based on high-temp. hydrolysis/solvolysis at 130-170° in pure water and alk. (0.05-0.5 N NaOH) medium. Ammonium perchlorate could be 98% recovered from the aq. soln. from hydrolysis of a 40:60 polyetherdiol-based urethane (prepd. from Lupranol 1000, Lupranol 2021, and TDI); the polyetherpolyol component was 84-90% recoverable and did not show any structural or mol. wt. changes after hydrolysis at 170° for 2 h. Treatment of a second propellant (contg. 86 wt.% RDX and 14 wt.% glycidyl azide-Desmodur N100 copolymer) at 130, 150, and 179° in pure water and 0.05 N NaOH for 10, 30, and 60 min resulted in high recovery of RDX but the GAP-derived urethane was recovered with a significant loss of azide groups. In this case, the azide group reacted to form N2 and nitrenes which formed non-reactive carbon-nitrogen bonds through intermol. insertion reactions, in addn. to nitrogen-contg. gaseous products and aq. ions.
Bibliographic Information
Process and apparatus for producing ultrafine explosive particles. (du Pont de Nemours, E. I., and Co., USA). Israeli (1995), 24 pp. CODEN: ISXXAQ IL 100231 A1 19950124 Patent written in English. Application: IL 91-100231 19911203. CAN 123:117652 AN 1995:743038 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
IL 100231 A1 19950124 IL 1991-100231 19911203
Abstract
An app. for producing ultrafine explosive particles comprises (1) means for injecting a soln. of a crystallizable explosive compns. and a nonsolvent soln. for mixing with the explosive compn. soln., (2) nozzles being adapted for moving the explosive compn. and nonsolvent solns., (3) venturi means communicating with nozzle means, and (4) explosive particle collection means connected with venturi means. The app. further comprises an auxiliary inlet means coaxial with and surrounding the explosive compns. and the nonsolvent soln. inlet means. The nozzle means include first and second continuous orifices. The ultrafine granular explosives which when incorporated into a binder system have the ability to propagate in thin sheets and have very low impact and very high propagation sensitivities.
Bibliographic Information
Method for making explosive charges by filtering liquid explosive. Vlassov, D. A. St. Petersburg Technological Inst., Russia. Hanneng Cailiao (1993), 1(1), 27-30. CODEN: HACAFQ Journal written in English. CAN 123:117600 AN 1995:695221 CAPLUS (Copyright 2002 ACS)
Abstract
A relatively safe method was developed for manuf. of explosive charges contg. a solid cryst. explosive and a liq. thermoplastic or thermosetting (i.e., polymg.) material (typically cryst. RDX and molten TNT). The technique involved filling of shells; calcns. were presented to calc. the porosity of RDX and the vol. of molten TNT that is necessary to fill the pores. The method was esp suitable for manuf. of rocket fuel compns. contg. solid oxidizer, metals, and liq. polymeric binder.
Bibliographic Information
Study on the nitrolysis of hexamethylenetetramine by NMR spectrometry. Fang, Zhijie; Chen, Li; Wang, Shaofang; Chen, Ju; Li, Fuping. Inst. Chemical Engineering, Nanjing Univ. Science and Technol., Nanjing, Jiangsu, Peop. Rep. China. Propellants, Explos., Pyrotech. (1995), 20(2), 83-6. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 122:294747 AN 1995:550727 CAPLUS (Copyright 2002 ACS)
Abstract
The nitrolysis of hexamethylenetetramine (HA) and 1,3,5-trioxane was studied by NMR spectrometry. The structure of the nitrolysis products of the trioxane could be monomethylenedinitrate, dioxymethylenenitronitrate and trioxymethylenenitronitrate, of structures O2N(OCH2)nONO2 (n = 1,2,3). A comparison of the 1H and 13C spectra of the nitrolysis mixt. of HA with the nitrolysis products of trioxane proved that in the nitrolysis mixt. of HA, the methylene group which cannot be used to form 1,3,5-triazacyclohexane (RDX) appears in O2N(OCH2)ONO2 and not in CH2(ONO2)2.
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Separation of RDX and HMX by recrystallization using supercritical fluids as anti-solvent. Gallagher, Paula M.; Krukonis, Val J.; Coffey, Michael P. (Phasex Corp., USA). U.S. (1995), 20 pp. CODEN: USXXAM US 5389263 A 19950214 Patent written in English. Application: US 92-886603 19920520. CAN 122:269545 AN 1995:420719 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5389263 A 19950214 US 1992-886603 19920520
Abstract
Materials that are ordinarily difficult-to-comminute such as a mixt. of RDX and HMX are sepd. by dissolving in a common liq. solvent to form a soln., adding to the soln. a supercrit. fluid to induce pptn. of one component of the components of the solid mixt. resulting in a pptd. component, and collecting the pptd. component. The process shows effective at sepg. HMX and RDX to obtain a ppt. of RDX which is essentially free of HMX.
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Recrystallization process of RDX and cobalt chloride using anti-solvent methods. Krukonis, Val J.; Gallagher, P. M.; Coffey, M. P. (Phasex Corp., USA). U.S. (1994), 21 pp. Cont.-in-part of U.S. Ser. No. 421,978, abandoned. CODEN: USXXAM US 5360478 A 19941101 Patent written in English. Application: US 91-723245 19910628. Priority: US 89-421978 19891016. CAN 122:34594 AN 1995:229370 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5360478 A 19941101 US 1991-723245 19910628
Priority Application Information
US 1989-421978 19891016
Abstract
In recrystg. solid RDX from systems comprising a solute which is the eventual material recrystd. and a liq. which is a suitable solvent for the solute, a gaseous component which is sol. within the solvent is added into the system to cause the solvent to approach or attain a supersatd. state and solute material to ppt. By control of process parameters such as pressure, temp., time, and rate, rate of injection of gas, the properties of the material recrystd. can be influenced.
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Rapid near-IR measurements of explosives. Eisenreich, N.; Kull, H.; Hertz, J. Fraunhofer-Institut fur Chemische Technologie, Pfinztal, Germany. Int. Annu. Conf. ICT (1994), 25TH(ENERGETIC MATERIALS-ANALYSIS, CHARACTERIZATION AND TEST TECHNIQUES), 86/1-86/7. CODEN: IACIEQ Journal; General Review written in German. CAN 122:13139 AN 1995:192723 CAPLUS (Copyright 2002 ACS)
Abstract
A review, with 6 refs., of the use of rapid near-IR (NIR) spectroscopy for online evaluation of explosives (esp. during manuf. and processing). Topics discussed include rapid NIR spectrometry with acoustooptical filters and the NIR spectra of energetic materials. Spectra given were nitromethane, GAP, TAGN (triaminoguanidine nitrate), TNT, RDX, HMX, ammonium nitrate, and ammonium perchlorate.
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Explosive property and mechanical characteristics of the trial PBX consisting of RDX and HTPB. Sato, Junichi; Shinkai, Masanori; Ito, Takeshi. Dep. Chem., Natl. Def. Acad., Yokosuka, Japan. Kayaku Gakkaishi (1994), 55(3), 89-95. CODEN: KAGAEA Journal written in English. CAN 121:160342 AN 1994:560342 CAPLUS (Copyright 2002 ACS)
Abstract
The prepn. of PBX (plastic-bonded explosive), consisting of RDX and hydroxy-terminated polybutadiene (HTPB) binder, was attempted. Various tests of explosive properties and mech. characteristics were carried out on the RDX-HTPB compn. as a trial PBX.
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Extraction of nitramine propellants using supercritical fluids. Morris, J.B.; McNesby, K.L.; Pesce-Rodriguez, R.A.; Schroeder, M.A.; Fifer, R.A. WT, U.S. Army Res. Lab., Aberdeen Proving Ground, MD, USA. Int. Annu. Conf. ICT (1993), 24th(Energetic Materials: Insensitivity and Environmental Awareness), 37-1/37-12. CODEN: IACIEQ Journal written in English. CAN 120:326901 AN 1994:326901 CAPLUS (Copyright 2002 ACS)
Abstract
The addn. of org. modifiers (co-solvents) for CO2-based supercrit. fluid extn. of an RDX-based LOVA composite gun propellant was examd. for the purpose of maximizing RDX recovery. Under supercrit. fluid extn. conditions (32° and 55 MPa for 45 min), MeCN displayed the greatest soly., or dissoln. rate enhancement, for RDX, with nitromethane a close second. When extg. solid gun propellant, solvent-modified CO2 fluid caused significant swelling of the propellant relative to the use of heat CO2. In addn. to RDX, the gun propellant contained cellulose acetate butyrate, nitrocellulose, plasticizer, and other additives.
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Design and calibration of pulsed vapor generators for TNT, RDX and PETN. Davies, J. P.; Blackwood, L. G.; Davis, S. G.; Goodrich, L. D.; Larson, R. A. Idaho Nat. Eng. Lab., Idaho Falls, ID, USA. Editor(s): Yinon, Jehuda. Adv. Anal. Detect. Explos., Proc. Int. Symp., 4th (1993), Meeting Date 1992, 513-32. Publisher: Kluwer, Dordrecht, Neth CODEN: 59MKAE Conference written in English. CAN 120:221786 AN 1994:221786 CAPLUS (Copyright 2002 ACS)
Abstract
Computer-controlled explosive vapor generators for TNT, RDX, and PETN were built and calibrated to support an independent validation and verification facility for Explosive detection systems for the Federal Aviation Administration (FAA). The generators were constructed using pure explosive suspended on quartz beads which were then loaded into a coiled stainless steel tube. A carrier gas (ultra-pure air) was passed through the coil to carry the explosive mols. The generators were capable of delivering a pulse of varying explosive mass through the control of coil temp., air flow rate, and pulse width. Preliminary calibrations were completed in the picogram-to-nanogram range using an ion mobility spectrometer as the calibrating instrument. The explosive vapor generators can be used as quant. vapor stds. to establish the lower detection limits for explosive detection systems systems.
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Process for preparation of RDX. Lukasavage, William J.; Nicolich, Steven; Slagg, Norman. (United States Dept. of the Army, USA). U.S. (1993), 4 pp. CODEN: USXXAM US 5250687 A 19931005 Patent written in English. Application: US 92-936375 19920828. CAN 119:271209 AN 1993:671209 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5250687 A 19931005 US 1992-936375 19920828
Abstract
The title process comprises repeated sequential addn. of NH4NO3/HNO3 and Ac2O to DAPT. This method, with continuous addn. of quantities of DAPT, provides near-quant. yields of RDX.
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Synthesis of carbon-14 labeled hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX). Horvath, Karoly; Alworth, William L. Dep. Chem., Tulane Univ., New Orleans, LA, USA. J. Labelled Compd. Radiopharm. (1993), 33(6), 467-71. CODEN: JLCRD4 ISSN: 0362-4803. Journal written in English. CAN 119:271112 AN 1993:671112 CAPLUS (Copyright 2002 ACS)
Abstract
14C-labeled hexahydro-1,3,5-trinitro-1,3,5-triazine was prepd by nitrolysis of hexahydro-1,3,5-tripropionyl-1,3,5-triazine (1) for bioenvironmental studies. 1 Was synthesized from paraformaldehyde and propionitrile by a modified method reported earlier.
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On the use of AM1 and PM3 methods on energetic compounds. De Paz, Jose Luis G.; Ciller, Juan. Dep. I+D, Union Espanola Explosivos, Madrid, Spain. Propellants, Explos., Pyrotech. (1993), 18(1), 33-40. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 118:237100 AN 1993:237100 CAPLUS (Copyright 2002 ACS)
Abstract
Stewart's new semi-empirical method MNDO-PM3 (PM3) was compared with the well-known Dewar's AM1 method in the study of the heats of formation and dipole moments of nitro-substituted compds., esp. for some energetic materials. The PM3 method had better performance than the AM1 method. Adjacent lone pair-lone pair repulsions were better described at the PM3 level; the known systematic correction of .apprx.-9 kcal/mol for each C-NO2 group of the AM1 method became +3.5 kcal/mol at the PM3 level. PM3 results for N-NO2 contg. compds. were directly comparable to exptl. gas phase data.
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Process and apparatus for producing ultrafine explosives. McGowan, Michael James. (du Pont de Nemours, E. I., and Co., USA). PCT Int. Appl. (1993), 26 pp. CODEN: PIXXD2 WO 9304018 A1 19930304 Designated States W: CA, NO. Designated States RW: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LU, NL, SE. Patent written in English. Application: WO 91-US5900 19910827. CAN 118:172045 AN 1993:172045 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
WO 9304018 A1 19930304 WO 1991-US5900 19910827
W: CA, NO
RW: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LU, NL, SE
EP 600881 A1 19940615 EP 1991-916893 19910827
EP 600881 B1 19960424
R: CH, DE, FR, GB, LI
WO 9304019 A1 19930304 WO 1991-US6748 19910924
W: CS, SU
Priority Application Information
WO 1991-US5900 19910827
Abstract
The process comprises prepg. a stream of a soln. of the explosive dissolved in a solvent and a stream of an inert nonsolvent, injecting the two streams through concentric orifices of a nozzle into a mixing chamber by injecting nonsolvent stream through the central orifice and explosive stream through the outer orifice, converging the streams in a mixing zone under turbulent conditions to entrap the explosive compn. in droplets of nonsolvent and to rapidly ppt. the explosive compn. as spheroidal particles, and recovering the particles from the solvent and nonsolvent materials.
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Explosive biodegradation in soil slurry batch reactors amended with exogenous microorganisms. Shen C F; Hawari J A; Paquet L; Ampleman G; Thiboutot S; Guiot S R Environmental Bioengineering Group, Biotechnology Research Institute, National Research Council, 6100 Royalmount Avenue, Montreal, Quebec H4P 2R2, Canada WATER SCIENCE AND TECHNOLOGY (2001), 43(3), 291-8. Journal code: DV8. ISSN:0273-1223. Journal; Article; (JOURNAL ARTICLE) written in English. DN 21274696 PubMed ID 11381919 AN 2001295394 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
The present study explores the feasibility of biotreatment of 2,4,6-trinitrotoluene (TNT) and hexahydro-1,3,5-trinitro- 1,3,5-triazine (RDX)-contaminated soils in slurry batch reactors. Radiorespirometric assays showed that anaerobic sludge was able to mineralize 59% RDX to CO2 although significant mineralization of TNT was not observed in all cases. TNT and RDX at concentrations higher than 50 and 100 mg/L respectively were inhibitory to methanogenesis (used as a bioindicator), however, methanogenesis recovered after TNT was transformed into less toxic triaminotoluene. Bioslurry batch reactors containing 40% of contaminated soil (2000 mg RDX and 1000 mg TNT/kg dry soil) were operated under various conditions. Both TNT and RDX were persistent to soil indigenous microbes. Degradation of both TNT and RDX was enhanced by the municipal sludge amendment, although degradation of RDX was only achieved under anaerobic conditions.
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Type I nitroreductases in soil enterobacteria reduce TNT (2,4,6,-trinitrotoluene) and RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine). Kitts C L; Green C E; Otley R A; Alvarez M A; Unkefer P J Environmental Biotechnology Institute, California Polytechnic State University, San Luis Obispo 93407, USA. ckitts@calpoly.edu CANADIAN JOURNAL OF MICROBIOLOGY (2000 Mar), 46(3), 278-82. Journal code: CJ3. ISSN:0008-4166. Journal; Article; (JOURNAL ARTICLE) written in English. DN 20211112 PubMed ID 10749541 AN 2000211112 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
Many enteric bacteria express a type I oxygen-insensitive nitroreductase, which reduces nitro groups on many different nitroaromatic compounds under aerobic conditions. Enzymatic reduction of nitramines was also documented in enteric bacteria under anaerobic conditions. This study indicates that nitramine reduction in enteric bacteria is carried out by the type I, or oxygen-insensitive nitroreductase, rather than a type II enzyme. The enteric bacterium Morganella morganii strain B2 with documented hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) nitroreductase activity, and Enterobacter cloacae strain 96-3 with documented 2,4,6-trinitrotoluene (TNT) nitroreductase activity, were used here to show that the explosives TNT and RDX were both reduced by a type I nitroreductase. Morganella morganii and E. cloacae exhibited RDX and TNT nitroreductase activities in whole cell assays. Type I nitroreductase, purified from E. cloacae, oxidized NADPH with TNT or RDX as substrate. When expression of the E. cloacae type I nitroreductase gene was induced in an Escherichia coli strain carrying a plasmid, a simultaneous increase in TNT and RDX nitroreductase activities was observed. In addition, neither TNT nor RDX nitroreductase activity was detected in nitrofurazone-resistant mutants of M. morganii. We conclude that a type I nitroreductase present in these two enteric bacteria was responsible for the nitroreduction of both types of explosive.
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Degradation of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) by Stenotrophomonas maltophilia PB1. Binks P R; Nicklin S; Bruce N C Institute of Biotechnology, University of Cambridge, United Kingdom APPLIED AND ENVIRONMENTAL MICROBIOLOGY (1995 Apr), 61(4), 1318-22. Journal code: 6K6. ISSN:0099-2240. Journal; Article; (JOURNAL ARTICLE) written in English. DN 95266812 PubMed ID 7747953 AN 95266812 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
A mixed microbial culture capable of metabolizing the explosive RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine) was obtained from soil enrichments under aerobic and nitrogen-limiting conditions. A bacterium, Stenotrophomonas maltophilia PB1, isolated from the culture used RDX as a sole source of nitrogen for growth. Three moles of nitrogen was used per mole of RDX, yielding a metabolite identified by mass spectroscopy and 1H nuclear magnetic resonance analysis as methylene-N-(hydroxymethyl)-hydroxylamine-N'-(hydroxymethyl)nitroamin e. The bacterium also used s-triazine as a sole source of nitrogen but not the structurally similar compounds octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine, cyanuric acid, and melamine. An inducible RDX-degrading activity was present in crude cell extracts.
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Isolation of three hexahydro-1,3,5-trinitro-1,3,5-triazine-degrading species of the family Enterobacteriaceae from nitramine explosive-contaminated soil. Kitts C L; Cunningham D P; Unkefer P J Los Alamos National Laboratory, New Mexico 87545 APPLIED AND ENVIRONMENTAL MICROBIOLOGY (1994 Dec), 60(12), 4608-11. Journal code: 6K6. ISSN:0099-2240. Journal; Article; (JOURNAL ARTICLE) written in English. DN 95110151 PubMed ID 7811097 AN 95110151 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
Three species of the family Enterobacteriaceae that biochemically reduced hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) were isolated from nitramine explosive-contaminated soil. Two isolates, identified as Morganella morganii and Providencia rettgeri, completely transformed both RDX and the nitroso-RDX reduction intermediates. The third isolate, identified as Citrobacter freundii, partially transformed RDX and generated high concentrations of nitroso-RDX intermediates. All three isolates produced 14CO2 from labeled RDX under O2-depleted culture conditions. While all three isolates transformed HMX, only M. morganii transformed HMX in the presence of RDX.
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Nitric acid decomposition of waste composite propellants for recovery of nitramine components. Warner, Kirstin F.; Cannizzo, Louis F.; Hajik, Robert M.; Johnston, Harold E. (Cordant Technologies Inc., USA). U.S. Pat. Appl. Publ. (2002), 9 pp. CODEN: USXXCO US 20020028971 A1 20020307 Patent written in English. Application: US 2001-784475 20010215. Priority: US 2000-188182 20000310. CAN 136:219170 AN 2002:172521 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 2002028971 A1 20020307 US 2001-784475 20010215
Priority Application Information
US 2000-188182P 20000310
Abstract
Nitramines are recovered from waste or unwanted composite nitramine aluminized propellants by: (1) treating the waste propellant with aq. nitric acid (below 55 wt.% HNO3), at a 4-6:1 wt. ratio of HNO3 to waste propellant, to digest the binder into soln. while neither solvating nor solvolyzing into soln. all or most of the nitramine, (2) adding a mineral acid other than nitric acid to the soln. and digesting a portion of the aluminum, and (3) recovering the nitramine. Suitable mineral acids other than nitric acid are selected from hydrochloric acid, perchloric acid, sulfuric acid, phosphoric acid, hydrobromic acid, and hydroiodic acid. Suitable nitramines that can be recovered include RDX, HMX, TEX, 4,10-dinitro-4,10-diaza-2,6,8,12-tetraoxatetracyclo[5.5.0.05,9.0.3,11] dodecane, and CL-20 (HNIW). Treatment of the energetic material can be carried out without the use of volatile org. solvents.
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Formation of energetic materials using supercritical fluids. Teipel, Ulrich; Krober, Hartmut; Krause, Horst H. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Propellants, Explosives, Pyrotechnics (2001), 26(4), 168-173. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 136:104697 AN 2001:829487 CAPLUS (Copyright 2002 ACS)
Abstract
A new field of applications of compressed gases is the formation of solid particles with well-defined properties, e.g. the particle size, the particle size distribution, the particle shape, the sp. surface area and free of solvent inclusions. It is possible to process moderately solids like energetic materials which are difficult to comminute due to their sensitivity to mech. or thermal stress. The characteristics of compressed gases allow to vary the morphol. of solid particles in a wide range. A pilot plant is presented, which has been built to prep. fine particles by the rapid expansion of supercrit. solns. (RESS process) and pptn. by a compressed fluid antisolvent (PCA process). The micronization of different energetic materials by the RESS and PCA processes is investigated.
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Process for co-manufacturing RDX high explosive and TNT-free emulsified explosive. Bao, Guangyi; Bao, Cuoli. (Peop. Rep. China). Faming Zhuanli Shenqing Gongkai Shuomingshu (2001), 4 pp. CODEN: CNXXEV CN 1293177 A 20010502 Patent written in Chinese. Application: CN 2000-131348 20001102. CAN 135:320150 AN 2001:813474 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
CN 1293177 A 20010502 CN 2000-131348 20001102
Abstract
The process comprises reacting of 10-12 wt. parts HNO3 with 1 wt. part hexamine at below 20° to obtain RDX, charging a mixt. contg. ammonium nitrate and ammonium sulfonate in an amt. of 8-12 wt. parts to the reactant, reacting the mixt. at 70-80°, neutralizing the byproduct (nitrate, H2O, etc.) with CaCO3, Ca(OH)2 or CaO to obtain the aq. phase of TNT-free emulsified explosive, and then reacting with oily phase to obtain TNT-free emulsified explosive.
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Study on preparation of ultrafine particle of explosive using technology of direct dilution. Sima, Tianlong; Yan, Jisheng. Gansu Yinguang Chemical industrial Complex, Baiyin, Peop. Rep. China. Huozhayao Xuebao (2001), 24(4), 46-47. CODEN: HUXUFP Journal written in Chinese. CAN 136:234276 AN 2001:804744 CAPLUS (Copyright 2002 ACS)
Abstract
Ultrafine particle of explosive is prepd. by using direct diln. technol. The fundamental principle of the method is introduced. The particle size and distribution of size of ultrafine PETN and RDX are tested.
Bibliographic Information
Study on high-energy LOVA propellant. Liao, Xin; Huang, Zhenya; Yang, Wenbao; Wang, Zeshan. Xi'an Modern Chemistry Research Institute, Xi'an, Peop. Rep. China. Huozhayao Xuebao (2001), 24(4), 8-9, 30. CODEN: HUXUFP Journal written in Chinese. CAN 136:249804 AN 2001:804730 CAPLUS (Copyright 2002 ACS)
Abstract
The formulation of a LOVA propellant was detd. by using RDX as the main energetic compn. with inert and energetic complex binders, complex plasticizers and combustion modifiers. The closed bomb tests showed that the designed formula of the LOVA propellant had the characteristic of high energy and low erosion. The solvent-extrusion process was demonstrated practicable for this type of LOVA propellant formula.
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Supercritical fluid technology: a new process on formation of energetic materials. Krober, H.; Reinhard, W.; Teipel, U. Fraunhofer Institut fur Chemische Technologie (ICT), Pfinztal, Germany. International Annual Conference of ICT (2001), 32nd(Energetic Materials), 48/1-48/13. CODEN: IACIEQ ISSN: 0722-4087. Journal written in English. CAN 135:346528 AN 2001:605072 CAPLUS (Copyright 2002 ACS)
Abstract
A novel process for purifn. of energetic solids was developed using compressed inert supercrit. gases (esp. CO2), in which the material can be comminuted to solid particles with well-defined properties (e.g., particle size, size distribution, shape, and sp. surface area) and no fluid inclusions. The particle morphol. can be varied by varying the characteristics of the compressed gases. The RESS (Rapid Expansion of Supercrit. Solns.) uses a loaded supercrit. fluid that is expanded through a nozzle to create a high supersatn. in the jet, in which rapid crystal nucleation and growth occurs. Solids which are insol. in a compressed gas can be processed by using the PCA process (pptn. with a compressed antisolvent). In this process, a soln. consisting of an org. solvent that is completely miscible with the compressed gas, and a solid material dissolved in this solvent is sprayed through a nozzle into a high-pressure vessel filled with a compressed gas. A pilot plant was thus built to prep. fine particles of certain solid explosives (e.g., HNS, TNT, RDX, etc.).
Bibliographic Information
Raman spectroscopy investigation of the effects of precipitation of precursor powders by antisolvents. Case study of RDX powders precipitation. Marlange, L.; Begue, G.; Petitet, J. P.; Jacob, G. Laboratoire D'Ingenierie des Materiaux et des Hautes Pressions, Institut Galilee - Universite Paris XIII, Villetaneuse, Fr. Recents Progres en Genie des Procedes (2001), 15(77, Science et Technologie des Poudres), 61-66. CODEN: RPGPEX ISSN: 1166-7478. Journal written in French. CAN 136:8599 AN 2001:599690 CAPLUS (Copyright 2002 ACS)
Abstract
Based on Raman spectroscopic results, the effect of a CO2 antisolvent (at densities 0.01-0.25 g/cm3) on the precursors of the powders obtained by pptn. was discussed for different solvents (e.g., acetone, Et acetate, or toluene) depending on the solvent swelling capacity. Three results were obsd. in the rapid pptn. of RDX from acetone soln. using crit. CO2 antisolvent: (1) the observable appearance of the ppt. is localized just beyond the max. obsd. Raman intensity, (2) the morphol. of the powder is different at a low pressure or under crit. conditions for CO2, and (3) the appearance of the pptd. powder at low pressure is reversible.
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Separation of nitramine and nitroaromatic explosives by capillary liquid chromatography. Goodpaster, John V.; McGuffin, Victoria L. Department of Chemistry, Michigan State University, East Lansing, MI, USA. Journal of Liquid Chromatography & Related Technologies (2001), 24(13), 1965-1978. CODEN: JLCTFC ISSN: 1082-6076. Journal written in English. CAN 135:244590 AN 2001:557131 CAPLUS (Copyright 2002 ACS)
Abstract
This study outlines the successful sepn. of nitrated explosives by using high efficiency capillary liq. chromatog. Careful optimization of sepn. conditions such as mobile phase compn. and temp. was performed by using a window diagram, as well as a more global criterion, the chromatog. resoln. statistic. These efforts resulted in complete baseline resoln. of all 14 components of a std. mixt. of explosives, which has not previously been achieved by using conventional liq. chromatog. This method was then applied to the detn. of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazine (HMX), and 2,4,6-trinitrotoluene (2,4,6-TNT) in com.-grade and military-grade explosive samples. As a result, the countries of manuf. of two RDX samples were deduced based on the presence or absence of reaction byproducts.
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Explosive properties of reactive mixtures formed during manufacturing of explosives. Buczkowski, Daniel; Gucma, Miroslaw; Pagowski, Witold. Institute of Industrial Organic Chemistry, Warsaw, Pol. Editor(s): Zeman, Svatopluk. New Trends in Research of Energetic Materials, Proceedings of the Seminar, 4th, Pardubice, Czech Republic, Apr. 11-12, 2001 (2001), 29-33. Publisher: University of Pardubice, Pardubice, Czech Rep CODEN: 69BKIC Conference written in English. CAN 135:228922 AN 2001:476831 CAPLUS (Copyright 2002 ACS)
Abstract
Explosive properties of mixts. formed in manuf. of PETN and RDX are presented. Deposits of PETN and RDX in nitric acid filling voids between crystals have detonation abilities similar to typical brisant explosives. Such deposits are formed if mixing is stopped. Soln. of RDX and slurry of PETN in nitric acid have weaker explosive properties, but are dangerous from the point of view of explosion. A problem of minimizing the possibility of damage of mixing equipment or electricity loss must be anticipated during designing producing plants for the manuf. of explosives.
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The sensitivity of explosives. McCrone, Walter C. McCrone Associates, Inc., Chicago, IL, USA. Microscope (2001), 49(1), 47-48. CODEN: MICRAD ISSN: 0026-282X. Journal written in English. CAN 135:109344 AN 2001:363793 CAPLUS (Copyright 2002 ACS)
Abstract
The sensitivity of HMX (e.g., as a byproduct of the manuf. of RDX) posses 4 known polymorphs, and, in one form (designated HMX 1, in the bipyramidal polymorph) is relatively insensitive. Phys. deformation (e.g., induced by rapid crystn.) results in a marked increase in sensitivity of HMX 1. HMX in general is subject to crystal strain if crystd. rapidly or ground to finer crystals, which can increase sensitivity, make the total batch have variable sensitivity, and can cause occasional unexpected explosions. This effect of crystal strain on sensitivity was also obsd. for TNT and lead azide, although no quant. relationship was examd.
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Study on the crystal size control of RDX. Liu, Han-bin; Yeh, Tsao-fa; Hu, Cheng-ching; Shieh, Chow-yang; Wang, Shan-guang. Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Ta-hsi, Taoyuan, Taiwan. Huoyao Jishu (2001), 17(1), 41-51. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 135:7561 AN 2001:312660 CAPLUS (Copyright 2002 ACS)
Abstract
RDX is probably the most important high brisance explosive and has wide applications. The performances of explosive depend on the crystal size distribution of RDX. The crystal size control is studied by using the characteristic of RDX dissoln. in concd. nitric acid. Based on the process flow conditions of RDX prodn. in the 203rd Arsenal Combined Service Force, the temp., concn. and residence time are selected as control parameters to conduct the expts. Thus it provides the better conditions of product and enables to obtain higher yield of target crystal size with the redn. of the quantity of outside target range of RDX.
Bibliographic Information
Study of the optimal reactor design in the manufacture process of RDX. Luo, Kuo-ming; Lin, Sheann-huei; Chang, Jih-guang; Chu, Kuang-shing. Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Ta-hsi, Taoyuan, Taiwan. Huoyao Jishu (2001), 17(1), 21-32. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 135:7560 AN 2001:312659 CAPLUS (Copyright 2002 ACS)
Abstract
The RDX is produced by the chem. reaction of Hexamine and nitric acid in three CSTRs of vol. of 112.5 L. A correlation is given for the calcn. of the reaction rate. To det. the optimal reactor design. The reaction temp. and fractional conversion are added to det. the optimum reactor design. The highest yield of the RDX is obtained at const. feeding ratio and const. reaction temp. range. The results enable to improve the RDX prodn. at optimum reaction temp. and flow rate.
Bibliographic Information
Preparation of nanometer RDX in situ by solvent substitution effect in reverse micelles. Liu, Dabin; Xu, Dong; Zhao, Baochang; Peng, Jinhua; Gao, Yaolin; Fan, Qinwen. Nanjing University Science Technology, Nanjing, Peop. Rep. China. Proceedings of the International Pyrotechnics Seminar (1999), 26th 269-275. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 134:313266 AN 2001:294122 CAPLUS (Copyright 2002 ACS)
Abstract
A new method to prep. ultrafine explosive through solvent substitution effect in reverse micelles was introduced. The max. soly. of DMF, DMSO, and its RDX soln. in NaAOT-isooctane reverse micelles were detd. The cylinder model RDX crystallites with their diam. of 70-100 nm were prepd. in situ in the NaAOT-isooctane reverse micelle system.
Bibliographic Information
Manufacture of finely dispersed explosives by crystallization from supercritical fluids. Teipel, Ulrich; Krause, Horst; Krober, Hartmut; Forter-Barth, Ulrich. (Fraunhofer-Gesellschaft zur Forderung der Angewandten Forschung e.V., Germany). Eur. Pat. Appl. (2001), 13 pp. CODEN: EPXXDW EP 1090894 A1 20010411 Designated States R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO. Patent written in German. Application: EP 2000-121747 20001005. Priority: DE 99-19948133 19991006. CAN 134:282927 AN 2001:261086 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
EP 1090894 A1 20010411 EP 2000-121747 20001005
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
Priority Application Information
DE 1999-19948133 19991006
Abstract
An explosive is dissolved in an org. solvent, a supercrit. fluid, which is miscible or partially miscible with the solvent and in which the explosive is insol. or slightly sol., is injected in the form of a jet flow into the soln., the solvent is collected during crystn. of the explosive particles from the supercrit. fluid, and the explosive particles are sepd. after expansion into a subcrit. state. Preferably, the soln. is injected into the supercrit. fluid by means of a complex nozzle or at least 1 nozzle channel of the complex nozzle, and the supercrit. fluid is fed by means of another nozzle channel.
Bibliographic Information
Effect of entropy on the formation of circular nitramine. Fang, Yi; Yongping, Pan. Nanjing, Peop. Rep. China. Proceedings of the International Pyrotechnics Seminar (1999), 26th 578-582. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 134:268397 AN 2001:115917 CAPLUS (Copyright 2002 ACS)
Abstract
Linear nitramines of TDA, BSX and ACAN were used to compose RDX directly in the soln. of ammonium nitrate - nitric acid. The reaction mechanism is discussed. Eight-member ring nitramine was composed difficultly. The effect of entropy was an important factor.
Bibliographic Information
Synthesis and nitration of condensation products of sulfamates with aliphatic amines and formaldehyde. Tartakovsky, V. A.; Ermakov, A. S.; Sigai, N. V.; Vinogradov, D. B. N. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, Moscow, Russia. Russian Chemical Bulletin (Translation of Izvestiya Akademii Nauk, Seriya Khimicheskaya) (2000), 49(6), 1082-1085. CODEN: RCBUEY ISSN: 1066-5285. Journal written in English. CAN 134:4920 AN 2000:700624 CAPLUS (Copyright 2002 ACS)
Abstract
A method for the synthesis of 5-alkyl-1,3-dinitro-1,3,5-triazacyclohexanes and linear polynitramines was proposed. It includes the reaction of aliph. amines with sulfamates and formaldehyde and nitration of the reaction products. The yield and compn. of nitramino derivs. depend on the conditions of the condensation and nitration.
Bibliographic Information
Crystallization of explosives and high-energy oxidizers in presence of ultrasound. Veltmans, Wilhelmina H. m.; Wierckx, Franciscus J. m. (Aerospace Propulsion Products B.V., Neth.). Eur. Pat. Appl. (2000), 13 pp. CODEN: EPXXDW EP 1033357 A1 20000906 Designated States R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO. Patent written in English. Application: EP 99-200592 19990302. CAN 133:195590 AN 2000:626476 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
EP 1033357 A1 20000906 EP 1999-200592 19990302
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
NO 2000001017 A 20000904 NO 2000-1017 20000229
Priority Application Information
EP 1999-200592 19990302
Abstract
Cryst. energetic materials with improved stability and/or decreased sensitivity are prepd. by crystn. with stirring at 15-75° in the presence of ultrasound with frequency 10-100 kHz and amplitudes of 0.4-10 m. The energetic materials that can be prepd. in this manner are explosives and high-energy oxidizers, esp. hydrazinium nitroformate, CL-20, ADN, AP, RDX, HMX, and PETN.
Bibliographic Information
Simple method for labeled conjugate production using N-hydroxysuccinimide and phase changes to control the reaction. Morseman, John P.; Zeng, Xiangfei. (Martek Biosciences Corporation, USA). PCT Int. Appl. (2000), 35 pp. CODEN: PIXXD2 WO 0043784 A1 20000727 Designated States W: AE, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CR, CU, CZ, DE, DK, DM, EE, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, TZ, UA, UG, US, UZ, VN, YU, ZA, ZW, AM, AZ, BY, KG, KZ, MD, RU, TJ, TM. Designated States RW: AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE, BF, BJ, CF, CG, CI, CM, GA, ML, MR, NE, SN, TD, TG. Patent written in English. Application: WO 2000-US1350 20000121. Priority: US 99-116689 19990122. CAN 133:101746 AN 2000:513898 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
WO 2000043784 A1 20000727 WO 2000-US1350 20000121
W: AE, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CR, CU, CZ, DE, DK, DM, EE, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, TZ, UA, UG, US, UZ, VN, YU, ZA, ZW, AM, AZ, BY, KG, KZ, MD, RU, TJ, TM
RW: GH, GM, KE, LS, MW, SD, SL, SZ, TZ, UG, ZW, AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE, BF, BJ, CF, CG, CI, CM, GA, GN, GW, ML, MR, NE, SN, TD, TG
EP 1145007 A1 20011017 EP 2000-903358 20000121
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
Priority Application Information
US 1999-116689P 19990122
WO 2000-US1350 20000121
Abstract
The present invention relates to methods for coupling labels to particular target moieties. The coupling reactions of the present invention use temporal spacing of the reactants through phase change (i.e. by rapid freezing) to control the initiation and termination of reaction. This process results in a simplified and improved method for linking labels to specific binding moieties using N-hydroxysuccinimide chem. The present invention further relates to kits comprising all necessary components to easily and rapidly make protein conjugates. Phycoerythrin was conjugated to streptavidin via EDAC/sulfo-NHS from a freeze dried reagent where D-(+)-trehalose was used.
Bibliographic Information
Application of solid-phase microextraction to the recovery of explosives and ignitable liquid residues from forensic specimens. Furton, K. G.; Almirall, J. R.; Bi, M.; Wang, J.; Wu, L. Department of Chemistry and International Forensic Research Institute, Florida International University, Miami, FL, USA. Journal of Chromatography, A (2000), 885(1+2), 419-432. CODEN: JCRAEY ISSN: 0021-9673. Journal written in English. CAN 133:203913 AN 2000:436513 CAPLUS (Copyright 2002 ACS)
Abstract
Solid-phase microextn. (SPME) was applied to the anal. of ignitable liqs. and explosive residues and the relative effects of controllable variables were studied. Variables discussed include fiber chem., adsorption and desorption temps., extn. and desorption times, fiber sampling placement (direct, headspace, and partial headspace) and matrix effects, including water content. SPME is shown to be an inexpensive, rapid and sensitive method for the anal. of ignitable liqs. and high explosives residues from solid debris samples and from aq. samples. Explosives are readily detected at parts per trillion concns. and ignitable liqs. are reproducibly detected at levels below those using conventional methods.
Bibliographic Information
Preparation of Grade III RDX by crystallization in nitric acid. Ye, Ling; Wang, Jian-long; Ye, Yu-peng. Capital University of Medical Science, Beijing, Peop. Rep. China. Hanneng Cailiao (2000), 8(1), 46-48. CODEN: HACAFQ ISSN: 1006-9941. Journal written in Chinese. CAN 132:349813 AN 2000:372246 CAPLUS (Copyright 2002 ACS)
Abstract
The prepn. of RDX of grade III is controlled by the nucleation temp., the interval of heat preservation, and the rate of stepwise diln. with water during the crystn. process in nitric acid. The exptl. results show that reducing the acidity and controlling the granularity of the final product are keys to the technol. for crystn. of RDX in strong acid medium.
Bibliographic Information
Recovering nitroamines from energetic pyrotechnic materials and reformulation of by-products. Phillips, Randall S.; Cain, Andrew W.; Schilling, Thomas J.; Miks, Michael W. (TPL, Inc., USA). U.S. (2000), 5 pp. CODEN: USXXAM US 6063960 A 20000516 Patent written in English. Application: US 98-212050 19981215. Priority: US 97-69492 19971215. CAN 132:323300 AN 2000:323256 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 6063960 A 20000516 US 1998-212050 19981215
Priority Application Information
US 1997-69492P 19971215
Abstract
A method for recovering nitroamines from energetic pyrotechnic materials yielding usable byproducts and no waste comprises solubilizing an energetic pyrotechnic material (such as surplus energetic material plastic binder) in a nitric acid soln., (b) removing an effluent from the soln. to leave a nitroamine (such as cyclotetramethylene tetranitramine), (c) neutralizing the effluent with a base, (d) removing liq. content from the effluent to yield a compd. salt, (e) rinsing the nitroamine and (f) desensitizing the nitroamine.
Bibliographic Information
Supercritical fluid extraction of triple-base and LOVA gun propellants. Morris, Jeffrey B. U. S. Army Research Laboratory AMSRL-WM-BD, Aberdeen Proving Ground, MD, USA. CPIA Publication (1999), 687(JANNAF 28th Propellant Development & Characterization and 17th Safety & Environmental Protection Subcommittee Joint Meeting, Vol. 1, 1999), 331-340. CODEN: CPPUDT ISSN: 0272-5118. Journal written in English. CAN 132:267179 AN 2000:256920 CAPLUS (Copyright 2002 ACS)
Abstract
Two supercrit. fluid extn. (SFE) studies are carried out on low-vulnerability ammunition (LOVA) and triple-base gun propellants. The extn. of RDX from ground LOVA gun propellant is carried out using dynamic SFE conditions with acetonitrile and dimethylsulfoxide modifiers for carbon dioxide (CO2). The results of this study are compared to the previous work on static SFE of bulk LOVA propellant. The extn. of nitroglycerin (NG) from M30 gun propellant is investigated with unmodified CO2, using both bulk and ground propellant. In addn., the soly. of NG is also measured under isothermal conditions at 40°. For both types of propellants, substantial matrix effects are encountered for the extn. of RDX or NG from the bulk propellant sample.
Bibliographic Information
Preparation of ultra-fine explosive HMX and RDX using high-speed impinging streams. Zhang, Xiaoning; Xu, Gengguang; Wang, Tingzeng. Department of Engineeing Safty, Beijing Institute of Technology, Beijing, Peop. Rep. China. Beijing Ligong Daxue Xuebao (1999), 19(5), 646-650. CODEN: BLXUEV ISSN: 1001-0645. Journal written in Chinese. CAN 132:51962 AN 1999:815237 CAPLUS (Copyright 2002 ACS)
Abstract
A method for prepg. ultra-fine HMX and RDX and their technol. factors affecting the prepn. are described. High-speed impinging streams of suspending liq. were used. The particles of HMX and RDX can be crushed into sub-micron effectively by high-speed impinging streams method. The effective particle diam. is 612.2 nm and the particle size distribution is 236.5.apprx.1286.0 nm. The pressures and times of processing are the main factors that affect the particle sizes and particle size distribution. The most important factor affecting the degree of crush is the pressure. The times of processing affect the mean particle diam. and the particle size distribution, not the crushing lower limit.
Bibliographic Information
Method for the recovery of secondary explosives from 2,4,6-trinitrotoluene-containing explosive compositions. Spencer, Arthur F.; Hartline, David F. (United States Dept. of the Air Force, USA). U.S. (1999), 4 pp. CODEN: USXXAM US 5977354 A 19991102 Patent written in English. Application: US 98-211491 19981215. CAN 131:288483 AN 1999:705051 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5977354 A 19991102 US 1998-211491 19981215
Abstract
Secondary explosive materials, particularly nitramines, are recovered from an explosive compn. contg. a mixt. of 2,4,6-trinitrotoluene (I) and at least one secondary explosive(s) by heating the explosive compn. to melt the I (preferably using steam), sep. collecting and recovering the melted I, treating the sepd. secondary explosive (e.g., octahydro-1,3,5,7-tetranitro-1,3,5,7-Tetrazocine; i.e., HMX) with a material which is a solvent for I and a nonsolvent for the secondary explosive (e.g., toluene) to dissolve the TNT, removing the nonsolvent from the secondary explosive, and recovering the secondary explosive.
Bibliographic Information
A molecular modeling study of the solvent effect on the RDX crystal morphology. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft University of Technology, Delft, Neth. International Symposium on Industrial Crystallization, 14th, Cambridge, United Kingdom, Sept. 12-16, 1999 (1999), 1973-1984. Publisher: Institution of Chemical Engineers, Rugby, UK CODEN: 68IRAJ Conference written in English. CAN 132:37699 AN 1999:704681 CAPLUS (Copyright 2002 ACS)
Abstract
The choice of solvent has a large effect on the crystal morphol. of RDX explosive. Mol. dynamics simulations of a solvent layer of g-butyrolactone upon the {200} and {210} RDX crystal surfaces were performed to obtain a better understanding of the behavior of solvent mols. near a crystal surface. The av. potential energy of the solvent mols. near the surfaces was higher than in the solvent bulk. The surface induces a potential energy change in the solvent layer. This surface-induced potential energy change might be an adequate solvent effect parameter to use in the prediction of the morphol. importance of a crystal surface. From the calcd. surface-induced potential energy changes, it follows that the {210} face is morphol. more important than the {200} surface. This agreed well with the obsd. exptl. RDX morphol. grown in the solvent g-butyrolactone.
Bibliographic Information
Antisolvent crystallization of the explosive compound RDX. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft University of Technology, Delft, Neth. International Symposium on Industrial Crystallization, 14th, Cambridge, United Kingdom, Sept. 12-16, 1999 (1999), 1960-1972. Publisher: Institution of Chemical Engineers, Rugby, UK CODEN: 68IRAJ Conference written in English. CAN 132:37698 AN 1999:704678 CAPLUS (Copyright 2002 ACS)
Abstract
RDX crystals were produced by antisolvent crystn. with either acetone or g-butyrolactone as the solvent and water as the antisolvent. Prodn. rates up to 38 g/L-h with acetone and 96 g/L-h with g-butyrolactone were achieved at a residence time of .apprx.30 min. The single crystals have a rather large av. size for such an antisolvent crystn. process. Attrition of the larger crystals reduces the quality of the crystals. In addn. to unagglomerated single crystals, the product contained a considerable amt. of agglomerated crystals.
Bibliographic Information
Preparation of ultra-fine nitroamine explosives by using high-speed impinging stream. Zhang, Xiao-Ning; Xu, Geng-Guang; Wang, Ting-Zeng. Beijing Institute of Technology, Beijing, Peop. Rep. China. Hanneng Cailiao (1999), 7(3), 97-99,102. CODEN: HACAFQ ISSN: 1006-9941. Journal written in Chinese. CAN 131:339045 AN 1999:689401 CAPLUS (Copyright 2002 ACS)
Abstract
The sub-micron ultra-fine particles of nitroamine explosives (HMX and RDX) were prepd. by using high-speed impinging stream. The fundamental principle and characteristic of this method were analyzed. The granularity and shape of the ultra-fine explosive particles obtained were tested with laser-sedimentograph and scanning electronic microscope.
Bibliographic Information
Crystallization and characterization of energetic materials. Van der Heijden, A. E. D. M. TNO Prins Maurits Laboratory, Research Group Pyrotechnics and Energetic Materials, Rijswijk, Neth. Current Topics in Crystal Growth Research (1998), 4 99-114. CODEN: CTCRFJ Journal; General Review written in English. CAN 131:259565 AN 1999:646019 CAPLUS (Copyright 2002 ACS)
Abstract
A review, with 85 refs., of the general aspects of crystn. of energetic materials, esp. explosives and oxidizers, driven by the need to develop less-sensitive materials. Topics discussed include soly., nucleation and crystal growth mechanisms, layer growth, rough growth, crystn. techniques (e.g., melt, cooling, evaporative, pptn., drowning out, supercrit., and quasi-emulsion crystn.), prediction of crystal shape, plastic explosives, formation of inclusions and dislocations, examples of crystn. of energetic materials, polymorphism, crystal size distribution, particle shape, crystal perfection, purity, thermal stability, and hazard properties of crystd. explosives. Compds. discussed include ammonium nitrate, TNT, RDX, HMX, hydrazinium nitroformate, hexanitrostilbene, HNIW, and NTO.
Bibliographic Information
Fluid extraction with supercritical carbon dioxide for recovery of TNT from high explosives. Morris, Jeffrey B. (United States Dept. of the Army, USA). U.S. (1999), 10 pp. CODEN: USXXAM US 5953679 A 19990914 Patent written in English. Application: US 97-840779 19970416. CAN 131:186997 AN 1999:582734 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5953679 A 19990914 US 1997-840779 19970416
Abstract
TNT is recovered from high explosives contg. TNT by supercrit. fluid extn. with CO2 at a temp. above the m.p. of TNT, preferably at .apprx.85° and .apprx.37.4 MPa. The TNT can be recovered from such TNT-contg. explosives as Compn. B, Compn. B3, Cyclotol, Octol, Tritonal, and Torpex, in which a warhead to be decommissioned is held in an inverted position, and supercrit. CO2 is led through channels in the warhead. RDX can often be recovered as a CO2-insol. fraction.
Bibliographic Information
Solubility Determination of TNT and Wax and Their Fractionation from an Explosive Material Using a Supercritical Fluid. Ashraf-Khorassani, Mehdi; Taylor, Larry T. Department of Chemistry, Virginia Polytechnic Institute and State University, Blacksburg, VA, USA. Journal of Chemical and Engineering Data (1999), 44(6), 1254-1258. CODEN: JCEAAX ISSN: 0021-9568. Journal written in English. CAN 131:301221 AN 1999:574255 CAPLUS (Copyright 2002 ACS)
Abstract
The solubilities of 2,4,6-trinitrotoluene (TNT) and wax were measured in supercrit. carbon dioxide (CO2) under nine static conditions of pressure (13.8, 25.0, and 37.9 MPa) and temp. (35, 50, and 70°). The concns. of each component were detd. off-line via UV (TNT) and evaporative light scattering (wax) detection. The soly. of TNT was an order of magnitude higher than that of wax. Gas chromatog. assay of the wax ext. revealed that only the lower mol. wt. components dissolved. Fractionation of the TNT and wax from an explosive material (Compn. B, contg. 59.5 wt.% RDX and 39.5 wt.% TNT) was attempted by making incremental increases in CO2 d. Although TNT and wax could be easily isolated from RDX, attempts to sep. TNT from wax were not totally successful. More specifically, the initial fractions contained lower mol. wt. wax components in addn. to major amts. of TNT. Since the percentage of TNT was .apprx.50 times the amt. of wax, later fractions were 100% TNT, although most of the TNT was removed at the lower densities.
Bibliographic Information
Recovery of acetic acid from spent liquor of cyclotetramethylene tetranitramine plant. Rajopadhye, M. V.; Hima, P. R.; Syal, R. K. Materials Research Laboratory, Pune, India. Chemical Engineering World (1999), 34(5), 81-86. CODEN: CEWOF5 Journal written in English. CAN 131:189044 AN 1999:520590 CAPLUS (Copyright 2002 ACS)
Abstract
A technol. for wastewater treatment and recovery of acetic acid from the effluent of the explosive cyclotetramethylene tetranitramine (HMX) plant was developed. At pH 2.8, HNO3, present in the spent liquor, is completely neutralized. The dild. acetic acid is recovered (greater than 85%) in a single-stage distn. under reduced pressure. The residues contg. all impurities including the explosives RDX/HMX are sepd. by cooling and filtration. Diln. of the residues with water enhances the pptn. of the explosives. From the safety point of view and for efficient recovery, spent liquors with higher acid concn. must be dild. to acetic acid concns. of .apprx.25-30% by water addn. prior to distn. A pilot plant with a capacity of 2000 L/day effluent is in operation.
Bibliographic Information
Recycling of nitramines at Bofors Explosives AB. Sjoberg, Per. Bofors Explosives AB, Karlskoga, Swed. Editor(s): Johansson, Stig R. Proceedings of the International Disposal Conference, 1st, Lund, Swed., Nov. 12-13, 1997 (1999), Meeting Date 1997, 133-136. Publisher: Sektionen foer Detonik och Foerbraenning, Combustion Institute, Billdal, Swed CODEN: 67YNAC Conference written in English. CAN 131:161104 AN 1999:502652 CAPLUS (Copyright 2002 ACS)
Abstract
Bofors Explosives has reclaimed 50 tonnes of nitramines from destroyed ammunition. The process was developed and is patented by Bofors Explosives. All worked-up nitramines have been reused in com. applications where otherwise freshly synthesized nitramines would have been used. The work-up process produces nitramine which is pure and chem. and phys. indistinguishable from freshly synthesized ones. The operation could be scaled up considerably if the recycled nitramines are accepted by the military for use in new ammunition. The military require freshly synthesized nitramines.
Bibliographic Information
Study on preparation of ultrafine particle of explosive by high-speed impinging stream technology. Zhang, Xiaoning; Wang, Weimin; Xu, Gengguang. Department of Mechanical and Electronic Engineerig, Beijing Institute of Technology, Beijing, Peop. Rep. China. Huozhayao Xuebao (1999), 22(3), 1-3. CODEN: HUXUFP Journal written in Chinese. CAN 131:172278 AN 1999:464551 CAPLUS (Copyright 2002 ACS)
Abstract
The prepn. of sub-micron ultrafine particle of explosive by high-speed impinging stream technol. was studied. The particle sizes of ultrafine HMX and RDX were detd.
Bibliographic Information
Mannich condensation reactivity of DPT nitrolysis fragments. Zhang, Yuejun; Zhou, Weilian; Wen, Jinquan. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1997), 23rd 999-1007. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 130:298956 AN 1999:154372 CAPLUS (Copyright 2002 ACS)
Abstract
The two kinds of different nitrogen atoms of amino groups in DPT (dinitropentamethylenetetramine) mol. had been labeled with 15N atoms, resp., in order to distinguish Mannich reactivity of fragments formed in DPT nitrolysis process. The nitrolysis fragments produced in DPT nitrolysis process could condense with urea or nitrourea to form product Keto-RDX. With the aid of mass spectrum isotope anal., the isotope distribution and abundance of 15N tracer atoms in product Keto-RDX and reactant DPT could be detd. The research results showed: nitrogen atoms of the trimethylene amino groups in DPT mol. appeared 100% in the 4 position in product Keto-RDX mol., but nitrogen atoms of the nitroamino groups in DPT mol. disappeared completely in the product Keto-RDX mol.
Bibliographic Information
Studies on the mechanism of synthesizing Keto-RDX in direct preparation method. Zhang, Yuejun. School of Chemical Engineering, Nanjing University of Science and Technology (NUST), Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1997), 23rd 987-998. CODEN: PPYSD7 ISSN: 0270-1898. Journal; General Review written in English. CAN 130:298931 AN 1999:154371 CAPLUS (Copyright 2002 ACS)
Abstract
A review with 19 refs. of the recent progresses of mechanistic researches of synthesizing Keto-RDX in direct prepn. method using urotropine and urea as reactants were systematically described in this paper. The evidences of reaction forms of urotropine and urea in the reaction to form resultant Keto-RDX were presented in several aspects: the active intermediates, the relationships between intermediate structures and reactivities, and the 15N trace atoms, etc.. The nitrolysis fragments N,N-dimethylolamines and their imine cations formed during the urotropine nitrolysis process were active intermediates from urotropine. And the product of nitrating urea or nitrourea, N,N'-dinitrourea also was an active intermediate. Keto-RDX was synthesized via Mannich condensation of the above active intermediates in strong acidic media.
Bibliographic Information
Missile system reclamation and recycling. Melvin, William S.; Freeman, Charles W.; Wright, Jeffrey S. U.S. Army Aviation and Missile Command (AMCOM) Missile Research, Development, and Engineering Center Propulsion and Structures Directorate, AMSAM-RD-PS-R, Redstone Arsenal, AL, USA. CPIA Publ. (1998), 674(Vol. 1, 1998 JANNAF Propellant Development & Characterization Subcommittee and Safety & Environmental Protection Subcommittee Joint Meeting, Vol. 1), 411-421. CODEN: CPPUDT ISSN: 0272-5118. Journal written in English. CAN 130:200413 AN 1999:80588 CAPLUS (Copyright 2002 ACS)
Abstract
This report describes the implementation, testing, and evaluation of environmentally friendly procedures and processes for complete missile system demilitarization and recycling of recovered ingredients and hardware components. Redstone Arsenal facilities and AMCOM developed technologies to support these efforts. The vast majority of the Army missile systems are full up rounds. The demilitarization approach addresses the entire missile system. Loaded rocket motors and cases are considered a subset of the total missile system. Warheads, rocket motors, guidance and control packages, shipping containers, and launch tubes will all be recycled. In contrast to missile system destruction approaches, where neither products nor assocd. values are recovered, this Army initiative includes both military and com. market reuse options for deriving max. product values of reclaimed ingredients and components. The AMCOM liq. ammonia-based, ingredient extn. and reclamation process for rocket propellant recycling has been integrated into a Missile System Recycling Facility at Redstone Arsenal. This propellant reclamation technol. has successfully completed full scale, class 1.3 MLRS and class 1.1 Hellfire rocket motor recycling demonstrations. The fully operational AMCOM pilot plant validated the closed-loop reclamation process by efficiently extg. and recovering 100% of the ammonium perchlorate (AP) and aluminum/binder from the MLRS propellant. This pilot facility fully achieved its design requirements. Test demonstrations confirmed the operational capability to process greater than 200 lb of AP composite propellant from a full scale MLRS rocket motor in a single batch. Pilot demonstrations have validated its operational capability by the processing of 100 lb batches of nitrate ester plasticized, HMX/RDX nitramine propellant from Hellfire rocket motors. Complete missile system recycling demonstrations using 60 TOW missiles are in progress. Pilot demonstration efforts have confirmed that strategically valuable fuel and oxidizer ingredients (such as HMX, RDX, AP, aluminum/rubber binder) can be safely and efficiently recovered from Army tactical rocket motors. The AMCOM missile system recycling technol. is directly applicable to the vast majority of rocket motors in the Army, other DoD, and foreign missile inventories. With emphasis on reclamation instead of destruction, the liq. ammonia process is a near-optimal soln. for environmentally sound rocket motor disposition.
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A fiber optic biosensor for multianalyte detection: importance of preventing fluorophore aggregation. Bakaltcheva, Irina B.; Shriver-Lake, Lisa C.; Ligler, Frances S. Geo-Centers, Incorporated, Rockville, MD, USA. Sens. Actuators, B (1998), B51(1-3), 46-51. CODEN: SABCEB ISSN: 0925-4005. Journal written in English. CAN 130:211443 AN 1998:815678 CAPLUS (Copyright 2002 ACS)
Abstract
Individual assays for the detection of the explosives RDX and TNT with a fiber-optic biosensor were developed. In order to develop an assay for simultaneous detection of RDX and TNT, a mixt. of the fluorescent-labeled analogs Cy5-EDA-RDH (hapten) and Cy5-EDA-TNB used in the individual assays was passed over the sensor that used anti-RDX and anti-TNT fiber probes connected in series. There was an increased total fluorophore concn. in the mixt., which resulted in a significant increase in the normalized signal compared to that produced by a single fluorophore. Aggregation of the amphiphilic fluorophores in the mixt. on the surface of the fiber optic probe was a possible reason for the obsd. effect. The use of nonionic (Tween 20) and ionic detergents (deoxycholic acid) to block aggregate formation and to allow detn. of RDX and TNT was examd. Use of the ionic detergent deoxycholic acid can help prevent fluorophore aggregation.
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Recovery/reuse of energetics from military munitions. Burch, Dan; Griggs, John; Johnson, Mike; Sims, Keith. Naval Surface Warfare Center, Crane Division (Code 4073), Crane, IN, USA. Proc. Int. Pyrotech. Semin. (1998), 24th 101-112. CODEN: PPYSD7 ISSN: 0270-1898. Journal; General Review written in English. CAN 129:278152 AN 1998:574325 CAPLUS (Copyright 2002 ACS)
Abstract
A review, with 8 refs., of methods for recovery and reuse of propellants and explosives from military munitions. Disassembly technol. using an abrasive waterjet was developed by the University of Missouri-Rolla (UMR) which can cut through projectiles and other munition items. Testing was performed using an abrasive slurry waterjet to cut the tracers and fuses off of Navy 40mm projectiles in order to reclaim the TNT. In addn., UMR has developed high-pressure water technol. to remove explosives and high-energy propellants from projectiles, warheads, and rocket motors. Other removal technologies being explored are microwave melt out and induction heating. Several projects are underway to process the reclaimed explosive from the waterjet washout process and other removal processes. This includes the mech. reprocessing of the PBXN-106 into two sep. explosive products, a dimensional stone mining explosive, boosters for insensitive blasting agents, high-purity HMX from reclaimed LX-14 and Trident I rocket motor formulations, and RDX from PBXN-106 and Compn. A3. Possible com. products manufd. from recovered military explosives included sporting powder, oil-gas well perforation charges, and fertilizer from reclaimed nitrocellulose-based gun propellants. Other projects currently being explored at the lab/bench scale include catalytic hydrotreating technol. to convert Explosive D (ammonium picrate) contained in Navy projectile to higher value products and the recovery of magnesium from illumination and decoy flares for reuse in the military or for com. applications.
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Process safety management on spray system to produce ultrafine RDX powder. Hong, Yaw-Shun; Huang, Chen-Chia; Chang, Fang-Mo; Luo, Shen-Kay; Chen, Sun-I. Department of Applied Chemistry, Chung Cheng Institute of Technology, Taoyuan, Taiwan. Huoyao Jishu (1997), 13(2), 37-47. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 129:97364 AN 1998:393643 CAPLUS (Copyright 2002 ACS)
Abstract
Spraying is an useful fabrication technique to obtain ultrafine powd. RDX. A process safety management program for the process involved mech. integrity information, std. operation procedures, safety systems, and maintenance and emergency planning. Following the management procedure, it was possible to reduce manufg. hazards.
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Recrystallization technology of powdered RDX. Wang, Jianlong; Xu, Chunyan. North China Institute of Technology, Taiyuan, Peop. Rep. China. Huabei Gongxueyuan Xuebao (1997), 18(3), 262-265. CODEN: HUGXFH ISSN: 1006-5431. Journal written in Chinese. CAN 129:83380 AN 1998:365791 CAPLUS (Copyright 2002 ACS)
Abstract
The technol. of producing powd. RDX by recrystn. was studied, with emphasis on the factors that affect the quality of the product.
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Recovery and reuse of rocket propellants. Melvin, William S.; Starling, Jarel P. U.S. Army Missile Command, Research, Development, and Engineering Center, Propulsion Directorate, Redstone Arsenal, AL, USA. NASA Conf. Publ. (1997), 3349(Second Aerospace Environmental Technology Conference, 1996), 193-201. CODEN: NACPDX ISSN: 0191-7811. Journal written in English. CAN 128:296643 AN 1998:300290 CAPLUS (Copyright 2002 ACS)
Abstract
An ongoing process development effort by the U.S. Army Missile Command (MICOM) to support environmentally safe rocket motor demilitarization demonstrations was discussed. This process is used to recover oxidizer and fuel ingredients from tactical and strategic class 1.1 and 1.3 solid propellants for recycle/reuse. The closed-loop demilitarization method uses liq. anhyd. ammonia as the processing solvent for ingredient extn. and recovery. A pilot-plant facility was designed and constructed in Magna, Utah, to demonstrate this technol. using Multiple Launch Rocket System (MLRS) and Chaparral tactical solid rocket motors. In July 1996, the pilot plant successfully completed full-scale MLRS propellant testing in a batch process mode at rates approaching 90 kg/h. Process descriptions of the integrated Class 1.1/1.3 rocket motor demilitarization system involving propellant removal, ingredient extn., binder sepn., oxidizer recovery, and solvent regeneration were provided. Test results demonstrating the ability of energetic products recovered by this process to be recycled into other products, and future work plans in support of this program also, were included.
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Recovering of components from plastic bonded propellants. Bohn, Manfred A.; Schweppe, Rainer; Weisweiler, Werner. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 175-185. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:219125 AN 1998:219158 CAPLUS (Copyright 2002 ACS)
Abstract
In order to recover the components of so-called "plastic-bonded propellants" (e.g., cryst. energetic materials bonded in a chem. three-dimensional crosslinked polyurethane matrix), the polyurethane matrix is broken solvolytically with water and alk. water (0.05 N-0.5 N NaOH) at 130-170°. Using a model rocket propellant, consisting of a polyether polyol mixt. (Lupranol 1000/2021) cured with Desmodur T80 and filled with 60 wt.% ammonium perchlorate (AP), 84-90% of the polyether polyol component was recovered, and 98% of the AP content subsequently detd. in the aq. hydrolyzate. The polyether polyols were nearly unchanged at 170° for 2 h, as shown by the molar mass distributions (detd. by gel permeation chromatog.). The solid gun propellant KHP (86 wt.% RDX-14 wt.% GAP-Desmodur N100 binder) was solvolyzed at 130, 150, and 170° with pure water and with 0.05 N NaOH for 10, 30, and 60 min. RDX was recovered in high yields and high purity. Under similar hydrolytic conditions, GAP did not behave in the same way as the Lupranol polyether polyols. The molar mass distribution of GPA was broadened and its azide content reduced, as detd. via IR absorption of the asym. N3 stretching vibration, and by differential scanning calorimetry, in both cases in relation to the azide content of the unreacted GAP. Neither the GAP-N100 binder or GAP were recoverable. Under these conditions, the N3 group decompd., yielding a nitrene functionality which formed solvolytically not scissionable C-N bonds by intermol. insertion reactions. The main gaseous reaction products in the solvolysis of KHP were N2, and N2O, with a little CO2, O2, and CO, and small amts. of NH3 and HCHO. The following ionic decompn. products were obsd.: NO2-, NO3-, HCOO- and NH4+.
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Value added products from reclamation of military munitions. Burch, D.; Johnson, M.; Sims, K. Crane Division (Code 4073), Naval Surface Warfare Center, Crane, IN, USA. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 159-163. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:219168 AN 1998:219156 CAPLUS (Copyright 2002 ACS)
Abstract
The Department of Defense has a backlog of excess, obsolete and unserviceable munitions for disposal. For many of these munition items the only method of disposal is open burning/open detonation (OB/OD) which destroys valuable resources which can be reclaimed and converted to useful products. The Crane Division, Naval Surface Warfare Center (NAVSURFWARCENDIV Crane) in support of the Navy's Ordnance Reclamation Program and the Joint Service Large Rocket Motor Disposal Program has been developing technol. for the removal and reclamation of the energetics from munitions. The University of Missouri-Rolla has demonstrated the use of high pressure waterjet technol. for removal of PBX explosives from projectiles and warheads. Development work is nearing completion for demonstrating the capability to remove Class 1.1 propellant from strategic rocket motors using high pressure waterjets. Current projects are under way focusing on resource recovery and recycling (R3) of the reclaimed energetics while minimizing disposal. The current reclamation projects include reformulation of the explosives and Class 1.1 propellants into com. blasting agents, reuse of Navy gun propellant for various applications including agriculture and oil-gas well stimulation. Other projects include the recovery of RDX/HMX from Class 1.1 explosives and propellants and the conversion of Explosive D into higher value products. Lab/bench scale testing has been completed on many of these processes, and for some pilot scale demonstrations have been or are scheduled to be completed during 1997.
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Solubility and phase behavior of PEP binders in supercritical carbon dioxide. Dinoia, Todd P.; Mchugh, Mark A.; Cocchiaro, James E.; Morris, Jeffrey B. Department of Chemical Engineering, The Johns Hopkins University, Baltimore, MD, USA. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 151-158. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:232440 AN 1998:219155 CAPLUS (Copyright 2002 ACS)
Abstract
Soly. and phase behavior data up to 300° and pressures to 3000 bars were presented for various propellant, explosive, and pyrotechnic (PEP) binder polymers in supercrit. CO2 with and without modifiers. The binder polymers investigated were polyethylene (PE), oxidized PE, poly(urethane), cellulose acetate butyrate (CAB), poly(vinylidene fluoride-co-hexafluoropropylene) with .apprx.20 mol% hexafluoropropylene (Fluorel and Viton), and poly(chlorotrifluoroethylene-co-vinylidene fluoride) with 24 mol% (Kel-F 800) and 69 mol% (Kel-F 3700) vinylidene fluoride. CO2 has the characteristics of a weak polar solvent which does not dissolve polyethylene although it is can dissolve low-mol.-wt. nonpolar waxes. However, CO2 is not polar enough to dissolve very polar polymers, such as oxidized PE, polyurethane, Kel-F 3700, and CAB (cellulose acetate butyrate). Moderately polar poly(vinylidene fluoride-co-hexafluoropropylene) and Kel-F 800 are sol. in CO2. The soly. of these two copolymers can be further enhanced using acetone as a modifier with CO2. Addnl., oxidized PE is sol. in CO2 with acetone and ethanol as modifiers, but temps. .gtorsim.200° are needed. The fact that many of these polymers are sol. in neat CO2 suggests the potential for a substantial impact upon environmentally sound processing technologies for polymer-based PEP materials.
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A study on the preparation of superfine RDX. Gou, Ruijun; Zhang, Jinglin; Han, Baocheng. North China Institute of Technology, Taiyuan, Peop. Rep. China. Editor(s): Feng, Changgen; Ou, Yuxiang; Zeng, Qingxuan. Theory Pract. Energ. Mater., [Proc. Int. Autumn Semin. Propellants, Explos. Pyrotech.], 2nd (1997), 37-40. Publisher: Publishing House of Ordnance Industry, Beijing, Peop. Rep. China CODEN: 65OYAF Conference written in English. CAN 128:142781 AN 1998:84547 CAPLUS (Copyright 2002 ACS)
Abstract
A process parameter study on prepn. of superfine cyclotrimethylenetrinitramine (RDX) was conducted using solvent-nonsolvent type of recrystn. Change in the process conditions caused significant changes in the particle size distribution, sp. surface area, bulk d. and residual solvent content. The particle size of RDX can be in the range of 2.apprx.0.1 mm by controlling the process conditions.
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Demilitarization facility for the environmental and acquisition life cycle analysis of explosives and munitions systems. Jeffers, Scott R.; Corley, John. Energetic Materials Branch (WL/MNME), Eglin AFB, FL, USA. Proceedings - International Symposium on Energetic Materials Technology, Phoenix, 1995 (1995), 337-341. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117024 AN 1998:63032 CAPLUS (Copyright 2002 ACS)
Abstract
As part of an environmental life-cycle anal. of the munitions design, manuf., and disposal, an aggressive pilot-scale demilitarization program was developed to recover, recycle, reuse, or dispose of explosives and munitions. Technologies developed at the facility will transition to industry or government agencies tasked to execute demil of prodn. weapons systems. The concurrent development of advanced energetic materials for munitions applications and recovery/treatment/disposal technologies for these materials was essential if they are to be incorporated into inventory systems. The technologies used in this program are: (1) high-pressure water washout for removal of the bulk explosive from the munition containers, (2) high-pressure water maceration for size redn. of bulk material for further processing and for the recovery of water-sol. materials, (3) hydrolysis to remove remaining explosive residues from the sides of the munition allowing for container recovery and reuse, (4) molten salt destruction for an environmentally compatible way to completely destroy and dispose of the unrecoverable materials, (5) and non-thermal discharge plasma processing as a supplement to molten salt destruction for controlling any acid gas formation.
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Hazards analysis of an integral Class 1.1/1.3 rocket motor demilitarization and ingredient recovery system using ammonia. Stevens, P. M.; Reed, M. H.; Losee, L. A.; Graul, E. R.; Mitchell, D. H. Global Environmental Solutions (Alliant Techsystems), Magna, UT, USA. Proc. - Int. Symp. Energ. Mater. Technol. (1995), 326-336. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117007 AN 1998:63027 CAPLUS (Copyright 2002 ACS)
Abstract
Research efforts conducted at the bench-scale have demonstrated the U.S. Army Missile Command (MICOM) near-crit. fluid technol. (using liq. anhyd. NH3) as a viable method of demilitarizing solid rocket motors for recovery of waste rocket propellants. This method was used to recover valuable ingredients, such as HMX, RDX, ammonium perchlorate, and aluminum/binder crumb from tactical and strategic Class 1.1 and 1.3 solid propellants. Ongoing hazards anal. efforts were reported. Hazards anal. testing has characterized the sensitivity of propellants, process streams, and extd. materials. Hazards anal. techniques, such as logic diagrams, and failure modes and effects anal., have identified credible hazards in the equipment design and pilot plant operations. These potential hazards were tracked by a closed loop system and were mitigated by design features or operating controls. Major hazards identified included: (1) shock initiation of ammonium perchlorate-ammonia solns. and undissolved BTTN, (2) ammonia jet impingement heating, (3) reaction of NH3 with nitroglycerin in Class 1.1 propellants, (4) spills and leaks of ammonia with hazard to operators, (5) instability of byproduct ammonium nitrite, (6) oxygen depletion by N2 displacement, (7) startup-shutdown-sampling-maintenance operation, and (8) abnormal situations and contingency plans.
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Crystallization of energetic materials; the effect on stability, sensitivity and processing properties. Meulenbrugge, Jan; van der Steen, Albert; van der Heyden, Antoine. TNO Prins Maurits Lab., Rijswijk, Neth. Proc. - Int. Symp. Energ. Mater. Technol. (1995), 297-302. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117022 AN 1998:60343 CAPLUS (Copyright 2002 ACS)
Abstract
Results were presented from expts. on crystn. of HNF (hydrazinium nitroformate) and RDX, and the effect of crystn. on the properties of these materials. Control of the crystn. process for HNF will improve the particle shape, the stability and the processability. Other parameters, like sensitivity, are much more reproducible and the control over the particle size will be improved. For RDX esp., the processability and the sensitivity to shock were improved when the particles are made spherical or treated in another way. Photographs of the crystals were presented as well as the properties of the various batches.
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Preparation and characterization of an AN-containing IMX. Zhang, Yian; Zhao, Shengxiang; Wu, Zhixing; Zhang, Chengwei. Xian Modern Chem. Res. Inst., Xian, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 75-80. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:265104 AN 1997:588770 CAPLUS (Copyright 2002 ACS)
Abstract
An intermol. explosive (IMX) mixt., XR-30, composed of phase-stabilized ammonium nitrate, ethylenediamine dinitrate, RDX, and a melt-casting agent, was prepd. conventionally, with filling d. greater than 98% theor. max. d. The formulation is a eutectic composite explosive. Its impact sensitivity, H50, is 68.5 cm, with a friction sensitivity 4% probability to reaction. The max. detonation velocity and pressure calcd. with N-M-Q method were 8.22 km/s and 28.9 GPa, resp.
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Synthesis of 2,4,6-trinitro-2,4,6-triazacyclohexanone (keto-RDX) from DPT and PHX. Zhang, Yuejun; Xie, Chunping. School Chem. Engineering, Nanjing Univ. Sci. & Technology, Nanjing, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 63-69. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:250216 AN 1997:588757 CAPLUS (Copyright 2002 ACS)
Abstract
A method was given for synthesis of 2,4,6-trinitro-2,4,6-triazacyclohexanone (Keto-RDX) from 1,5-methylene-3,7-dinitro-1,3,5,7-tetraazacyclononane (I) [DPT], and urea (or nitrourea) in several kinds of nitrating reagents. Primary investigations were carried out for the reaction forms of nitrolysis fragments I and 1,7-diacetoxy-2,4,6-trinitro-2,4,6-triazacycloheptane (II), and on the mechanism of forming byproduct. The nitrolysis fragments N,N-dihydroxymethylamines [RN(CH2OH)2, N is not NO2] that were not directly substituted by nitro groups condensed with urea or nitrourea to form keto-RDX, whereas N,N-dihydroxymethylnitroamine [O2NN(CH2OH)2] did not. Using I as a reactant, the yield of Keto-RDX was 69% (one mole keto-RDX per mol reactant); the byproducts were HMX, RDX, and smaller mol. fragments. Using II, no keto-RDX product and no cyclonitroamine byproducts were obtained.
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Technical research to class 5 RDX crystal in nitric acid system. TianLong, Si Ma; Jie, Zhao Yong. Dep. Technique, Yinguang Chem. Corp., Baiying City, Gansu, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 54-62. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:250215 AN 1997:588746 CAPLUS (Copyright 2002 ACS)
Abstract
An improved process for producing RDX by direct oxidn. of hexamethylenetetramine was theor. based on the soln. chem. performance. Using this method, RDX can be made in one step, with a quality that complies with class 5 requirements of USA Military Std. USA-R-398C. By controlling the diln. process, the RDX has a granularity of .gtorsim.85% less than 10 mm.
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Evaluation of leaving groups in nitramine synthesis. An experimental and theoretical (AM1) study. Piacenza, G.; Jacob, G.; Girard, A.; Graindorge, H.; Gallo, R. Fac. Sciences Saint-Jerome, Marseille, Fr. Int. Annu. Conf. ICT (1997), 28th(Combustion and Detonation), 124.1-124.12. CODEN: IACIEQ ISSN: 0722-4087. Journal written in English. CAN 127:190355 AN 1997:522194 CAPLUS (Copyright 2002 ACS)
Abstract
An exptl. study of nitrolysis was conducted with 12 selected leaving groups located at the N atoms of hexahydro-s-triazine (a reasonably transposable mol. structure) using 7 nitrating media. Yields and limiting side reactions are given and discussed. A theor. study by semi-empirical quantum mech. calcn. (AM1) is made on this substitution reaction by NO2+ with a series of electrophilic leaving groups, the same as studied exptl. The nature, geometry, and energy of intermediates and of transition states are calcd. These results give a classification of leaving-group ability which is in good agreement with exptl. results. They allow a selection of leaving groups for nitrolysis and design of more efficient synthetic methods for prepg. high energy nitramines.
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Crystallization technology of Grade 5 RDX. Wang, Janlong; Ye, Yupeng. North China Inst. Tech., Taiyuan, Peop. Rep. China. Huozhayao (1997), 20(2), 14-15. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 127:68122 AN 1997:354693 CAPLUS (Copyright 2002 ACS)
Abstract
A technol. of producing Grade 5 RDX by crystn. was studied.
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Study on the nitrolysis of hexamethylenetetramine by NMR spectrometry. Part 2. Some new evidence of the intermediate of HOCH2NHNO2 as a possible precursor to RDX. Fang, Zhi Jie; Chen, Li; Wang, Shao Fang; Chen, Ju; Li, Fu Ping. Institute Chemical Engineering, University Science Technology, Nanjing, Peop. Rep. China. Propellants, Explos., Pyrotech. (1997), 22(2), 78-80. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 127:83507 AN 1997:332267 CAPLUS (Copyright 2002 ACS)
Abstract
The RDX yield from nitrolysis of hexamethylenetetramine (HA) together with methylenedinitramine (MDNA) in 90% HNO3 was greater than 100%. MDNA decompd. completely in 90% HNO3, forming O(CH2ONO2)2, whereas in HNO3-NH4NO3 system, the decompd. fragments of MDNA condensed to form RDX. Based on a comparison of the exptl. results to the 1H-NMR spectra obtained by following the decompn. reaction of MDNA with HNO3, the intermediate, HOCH2NHNO2, was postulated as one of the possible precursors to RDX both in Hale and in K process.
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Improvement of combustion property of double base propellant with N,N'-dinitropiperazine. Pan, Wenda; Chang, Jingxiang. Xi'an Modern Chemistry Research Inst., Xi'an, Peop. Rep. China. Guti Huojian Jishu (1997), 20(1), 36-40. CODEN: GHJIFL ISSN: 1006-2793. Journal written in Chinese. CAN 126:253075 AN 1997:244968 CAPLUS (Copyright 2002 ACS)
Abstract
This paper presents the formulation and prepn. method of the double base propellant contg. N,N'-dinitropiperazine (DNP) and investigates the effects of DNP on the energy and combustion properties of the double base propellant. Results show that DNP can decrease burning temp. of double base propellant and increase sp. vol., but its specific impulse is almost const. or has a little decrease. DNP can significantly decrease the burning rate and pressure exponent of the double base propellant.
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Preparation of RDX of different particle-size by recrystallization in nitric acid solution. Rui, Jiuhou; Liu, Yuhai; Wu, Siaoqing. North China Inst. Technol., Taiyuan, Peop. Rep. China. Baopo Qicai (1997), 26(1), 10-13. CODEN: BAQIEJ ISSN: 1001-8352. Journal written in Chinese. CAN 126:279788 AN 1997:219443 CAPLUS (Copyright 2002 ACS)
Abstract
A method of prepn. of RDX crystals of different particle size distribution by recrystn. in aq. HNO3 was suggested. The relationship between RDX crystal nucleation, crystal fault formation, and the amt. of included acid in RDX crystals was discussed. Special attention was paid to the process conditions which affected the granularity, shape, and the amt. of included acid in RDX crystals (e.g., the crystn. temp., stirring speed, and the diln. rate). RDX crystals could be prepd. with less than 0.02% included acid.
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Supercritical fluid extraction of polar nitrogen containing-substances. Niehaus, M.; Teipel, U.; Bunte, G.; Krause, H.; Weisweiler, W. Fraunhofer Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Process Technol. Proc. (1996), 12(High Pressure Chemical Engineering), 345-350. CODEN: PTPREM ISSN: 0921-8610. Journal written in English. CAN 126:187773 AN 1997:79413 CAPLUS (Copyright 2002 ACS)
Abstract
Dynamic fluid extn. with supercrit. CO2 was investigated for the purifn. and prepn. of fine particles of polar nitrogen-contg. compds. (e.g., typical explosives and energetic compds. such as PETN, nitroguanidine, RDX, and 3-nitro-1,2,4-triazole). The two processes examd. were: (1) rapid expansion of supercrit. solns. (RESS), and (2) the gas-antisolvent (GAS) process. All explosives except nitroguanidine could be extd., although for RDX and 3-nitro-1,2,4-triazole, modifiers were necessary. The results demonstrated the high capacity of modified supercrit. CO2 as a solvent in RESS and GAS processes. Suitable modifiers must be examd. empirically.
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New Method for preparation of ultrafine RDX crystals. Rui, Jiuhou; Wang, Zeshan; Liu, Yuhai; Shi, Jie. School of Chemical Engineering, NUST, Nanjing, Peop. Rep. China. Nanjing Ligong Daxue Xuebao (1996), 20(5), 385-388. CODEN: NLIXET ISSN: 1005-9830. Journal written in Chinese. CAN 125:333433 AN 1996:686435 CAPLUS (Copyright 2002 ACS)
Abstract
A new method for the direct prepn. of ultrafine RDX crystals was described, in which RDX is dissolved in 98% HNO3 and then treated with water at 0-50°, during which fine and ultrapure RDX crystals ppt. Using the solvent (98% HNO3)-non-solvent (H2O) pptn. technique, 50 g-scale expts. were conducted. Depending on the crystn. condition chosen, ultrafine RDX crystals of 5 to .apprx.7 mm median particle diam. were prepd. Special emphasis was paid to the study of the process conditions affecting the granularity of the ultrafine RDX crystals (e.g., the crystn. temp., stirring speed, concn. of the soln. and the amt. of diln. water).
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New method for preparing submicron explosives - microemulsion method. Liu, Zhijian; Fan, Shijun. Xi'an Modern Chemistry Research Institute, Xi'an, Peop. Rep. China. Huozhayao (1996), 19(4), 12-13. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 125:252227 AN 1996:621954 CAPLUS (Copyright 2002 ACS)
Abstract
This paper presents, for the fabrication of ultrafine particle explosives, a novel method, the microemulsion method which yields 1.02-0.42 mm-particle explosives. In this paper, the theor. basis of the method and a physicochem. model for the ultrafine particle formation are elucidated, and also four basic compns. for microemulsion explosives are given.
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New method for improving the particle size of RDX. Zhang, Nanjiang. Huahei Inst. Technol., Taiyuan, Peop. Rep. China. Huozhayao (1996), 19(3), 23-24. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 125:252221 AN 1996:558168 CAPLUS (Copyright 2002 ACS)
Abstract
In the manufg. of RDX, crystal grain size of RDX is improved (increased) by adding to the crystn. soln. the surfactant dodecyl sodium sulfate.
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Extraction of explosives by supercritical fluids. Niehaus, M.; Teipel, U.; Krause, H.; Bunte, G. Fraunhofer Institut Chemische Technologie (ICT), Pfinztal, Germany. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 128.1-128.16. CODEN: IACIEQ Journal written in German. CAN 125:200039 AN 1996:514603 CAPLUS (Copyright 2002 ACS)
Abstract
The soly. parameters of explosives in supercrit. carbon dioxide are important for evaluation of novel techniques in manuf. and also in quant. anal. Efforts have been made to use the unique possibilities that supercrit. carbon dioxide offers, such as nontoxicity and therefore redn. of environmental pollution or low-temp. processing resulting in addnl. process safety. Also, the performance of explosives improves because of the minimization of contamination caused by conventional org. solvents with low vapor pressure. Supercrit. fluid extn. of the explosives pentaerythrityl tetranitrate (PETN), nitroguanidine (NIGU), RDX, and 3-Nitro-1,3,4-triazole (NTO) has been done in the dynamic mode with pure and modified carbon dioxide. All explosives except nitroguanidine have been extd., although for RDX and NTO use of modifiers proved to be necessary. Effective modifiers must be chosen empirically. The results show the high potential of supercrit. fluids as substitutes for org. solvents.
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Bench-scale cooling crystallization of RDX. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft Univ. of Technology, Delft, Neth. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 126.1-126.11. CODEN: IACIEQ Journal written in English. CAN 125:225933 AN 1996:514601 CAPLUS (Copyright 2002 ACS)
Abstract
Crystals of the explosive RDX were produced by bench-scale batch cooling crystn. and on the lab. scale using three solvents: (1) cyclohexanone, (2) cyclohexanone satd. (3 wt.%) water, and (3) g-butyrolactone. The morphol. of the RDX crystals was strongly dependent on the solvent and independent of the prodn. scale. Crystn. from cyclohexanone gaves block-like RDX crystals with large macrosteps, indicating blockage of growth. When crystn. takes place from cyclohexanone satd. with water, the macrostep formation seems to be eliminated. Comparison of the crystals growing from stagnant solns. and from the bench-scale expts. showed that the turbulence in the crystallizer, that leads to crystal collisions, has a large neg. influence on the formation of crystal inclusions, esp. at high solid loadings.
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Study on the nitrolysis of hexamethylenetetramine by NMR-spectrometry. IV. A novel mechanism of the formation of RDX from HA. Fang, Zhijie; Wang, Shaofang; Li, Fuping. Inst. Chemical Eng., Nanjing Univ. Sci. Technology, Jiangsu, Peop. Rep. China. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 89.1-89.7. CODEN: IACIEQ Journal written in English. CAN 125:172518 AN 1996:514567 CAPLUS (Copyright 2002 ACS)
Abstract
The mechanisms of the nitrolysis of hexamethylenetetramine (hexamine or HA) with nitric acid and with the mist. of nitric acid and ammonium nitrate to form 1,3,5-trinitro-1,3,5-triazacyclhexane (hexogen or RDX) were studied by NMR tracing. It was found that HA immediately disappeared, while RDX was formed gradually, which indicates the formation of some intermediates in the HA nitrolysis to give RDX. The chem. shift of the peaks in the 1H and 13C NMR tracing spectra disagreed with the possible cyclic-structure intermediates proposed by G. F. Wright (1969) and co-workers. Comparison of the 13C NMR spectra showed that the nitrolysis fragments in K process can be used to form RDX. Based on the results, structures of intermediates were proposed. All the evidences mentioned above suggested a novel mechanism of the formation of RDX form HA, i.e., the nitrolysis of HA first gives some open-chain methylenenitramine intermediates, and the condensation of the latter gives RDX under certain conditions.
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New nitration and nitrolysis procedures in the synthesis of energetic materials. Pagoria, Philip F.; Mitchell, Alexander R.; Schmidt, Robert D.; Coon, Clifford L.; Jessop, Edward S. Energetic mater. Cent., Lawrence Livermore Natl. Lab., Livermore, CA, USA. ACS Symp. Ser. (1996), 623(Nitration), 151-164. CODEN: ACSMC8 ISSN: 0097-6156. Journal written in English. CAN 125:37462 AN 1996:288534 CAPLUS (Copyright 2002 ACS)
Abstract
The development of new nitrolysis and nitration reagents are essential to the research and development of energetic materials. In this paper we describe the development of two new nitrolysis reagents, trifluoromethanesulfonic anhydride/HNO3/N2O5 and trifluoroacetic anhydride/HNO3/N2O5, which were uniquely successful in the nitrolysis of secondary amide groups to yield several new, bicyclic nitramines. An alternative method for the synthesis of secondary nitramines by the mild nitrolysis of N-tert-butoxycarbonyl (N-BOC) derivs. The attempted synthesis of 18O-labeled 2,4,6-trinitroltoluene using trifluoromethanesulfonic acid and NaN18O3 at elevated temps. resulted in incorporation of only two 18O atoms per TNT mol., indicating substantial oxygen exchange.
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A facile pressing technique for the preparation of small calibre dual role explosive charge. Kumar, A. S.; Samudre, S. S.; Waghmare, N. G.; Gharia, J. S. Explosives Res. and Development Laboratory, Pune, India. Propellants, Explos., Pyrotech. (1996), 21(2), 106-110. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 124:320938 AN 1996:286536 CAPLUS (Copyright 2002 ACS)
Abstract
Small-caliber shaped charges were prepd. by pressing of RDX-wax compns. The shaped-charge performance was considerably influenced by the d. gradient which is an inherent drawback assocd. with pressing. A new method, double-action pressing, was developed which overcomes this problem and is amenable for large-scale prodn. Properties of the charges prepd. by the different methods, esp. with respect to the d. gradient and performance against targets, were presented and discussed. The penetration performance was increased by 8-10% with explosives prepd. by the double-action pressing technique.
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Manufacture of HMX with high yield using byproducts from DPT nitrolysis. Xi, Meihong; Deng, Ning. Nanjing Univ. Sci. and Technol., Nanjing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 280-283. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347528 AN 1996:285175 CAPLUS (Copyright 2002 ACS)
Abstract
In the step-wise nitrolysis of DPT and hexamine (HA), the condensation of nitrolyzed segments of HA and linear nitramines produced in nitrolysis of DPT can increase in yield of HMX to 60% (counted by DPT) and yield of RDX to 75% (counted by HA). The presence of condensation is conformed in the nitrolysis of HA.
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Methods for the production of fine particle explosives. Ji, Liguo; Jiao, Qingjie; Cai, Ruijiao. Beijing Institute Technology, Beijing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 170-174. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347523 AN 1996:285153 CAPLUS (Copyright 2002 ACS)
Abstract
A ultrasonic generator and a sprayer are used in the prodn. of fine cryst. explosive. The cavity effect of ultrasonic is used to crush explosive particles while substituting stirring app. The recryst. process of explosive is controlled by the sprayer. The mechanism of ultrasonic and spraying jet is discussed. Fine particles of PETN and RDX having medium diams. less than 10 mm are manufd. in the process.
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Conformation of intermediate HOCH2NHNO2 from nitrolysis of hexamethylentetramine as possible precursor for RDX formation by NMR spectrometry study. Fang, Zhijie; Chen, Li; Wang, Shaofang; Chen, Ju; Li, Fuping. Institute Chemical Engineering, Nanjing University Science and Technology, Nanjing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 121-123. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347522 AN 1996:285144 CAPLUS (Copyright 2002 ACS)
Abstract
RDX manufd. from nitrolysis of hexamine together with methylenedinitramine (MDNA) in 90% nitric acid is reported. MDNA decompd. completely in 90% nitric acid, forming O(CH2ONO2)2, while in HNO3-NH4NO3 system the decompd. fragments of MDNA condensed into RDX. On the basis of the comparison of the exptl. results to the 1H NMR spectra obtained by following the decompn. reaction of MDNA with nitric acid, the intermediate, HOCH2NHNO2, was postulated as one of the possible precursors to RDX both in Hale and in K process.
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Detecting genotoxic activity in industrial effluents using the SOS Chromotest microplate assay. Legault, Richard; Blaise, C.; Trottier, S.; White, P. A. Cent. Saint-Laurent, Environment Canada, Montreal, Can. Environ. Toxicol. Water Qual. (1996), 11(2), 151-65. CODEN: ETWQEZ ISSN: 1053-4725. Journal written in English. CAN 124:335056 AN 1996:271876 CAPLUS (Copyright 2002 ACS)
Abstract
The SOS Chromotest, a cost-effective short-term bacterial genotoxicity screening assay, was performed to appraise its capacity for detecting the presence of sol. genotoxic activity in industrial effluent samples (org. and inorg. chem. plants, metallurgical plants, pulp and paper mills, municipal wastewater treatment plants). An optimized methodol., based on criteria taking into account b-galactosidase activity (the indicator of SOS gene induction), alk. phosphatase activity (the indicator of cytotoxicity), and two genotoxicity measurement end points (min. genotoxic concn. and max. induction factor), was employed to generate reliable results that overcame the potential interferences inherent to complex wastewaters. Of 48 effluent samples tested, 37 (77%) elicited a significant induction of the Escherichia coli PQ37 SOS response. Effluents from inorg. chem. plants and pulp and paper mills displayed the most potent responses, with and without metabolizing enzymes (S9 mix). In general, chem. data available for some wastewaters supported SOS Chromotest pos. responses. The genotoxic activity of whole effluents subjected to a 5-day aeration treatment was as high as that of native (un-aerated) samples, suggesting that sol. genotoxicants are relatively recalcitrant to oxidn., although redns. in genotoxic activity did occur. This study indicates that the SOS Chromotest is sufficiently sensitive to screen for the presence of sol. DNA-damaging agents in a wide variety of un-concd. wastewater samples.
Bibliographic Information
Relationship between crystallization and acidity for RDX. Lu, Yuexian; Chang, Zhihong. North China Inst. Technol., Taiyuan, Peop. Rep. China. Huozhayao (1996), 19(1), 15-18. CODEN: HUOZFT Journal written in Chinese. CAN 124:293627 AN 1996:254833 CAPLUS (Copyright 2002 ACS)
Abstract
Based on the technol. of RDX prepn. by nitrolysis of hexamethylenetetramine (HA), the effect of each factor in crystn. on the acidity of the product was investigated. By controlling the crystn. point and each factor in crystn., the acidity of large-grain product can be reduced such that the RDX product conforms to the appropriate American Military stds.
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Crystal growth of energetic materials during high acceleration. Lanzerotti, M. Y. D.; Autera, J.; Borne, L.; Sharma, J. ARDEC, U.S. Army, Picatinny Arsenal, NJ, USA. Mater. Res. Soc. Symp. Proc. (1996), 418(Decomposition, Combustion, and Detonation Chemistry of Energetic Materials), 73-8. CODEN: MRSPDH ISSN: 0272-9172. Journal written in English. CAN 124:206434 AN 1996:176813 CAPLUS (Copyright 2002 ACS)
Abstract
Studies of the growth of crystals of energetic materials under conditions of high acceleration in an ultracentrifuge were reported. When a satd. soln. is accelerated in an ultracentrifuge, the solute mols. move individually through the solvent mols. to form a crystal at the outer edge of the tube if the solute is more dense than the solvent. Since there is no evapn. or temp. variation, convection currents caused by simultaneous movement of solvent and solute are minimized and crystal defects are potentially minimized. Crystal growth is thus controlled by the g-level of the acceleration. In addn., soln. inclusions and bubbles migrate out of the satd. soln. as a result of the pressure gradient induced by the g-force. Results were presented for TNT, RDX, and TNAZ grown at high g from various solns.
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Granularity and spheroidization of RDX. Rui, Jiuhou; Ye, Yupeng; Liu, Yuhai; Gu, Jianliang. Sch. Chem. Eng., NUST, Nanjing, Peop. Rep. China. Nanjing Ligong Daxue Xuebao (1995), 19(6), 497-500. CODEN: NLIXET ISSN: 1005-9830. Journal written in Chinese. CAN 124:150101 AN 1996:63600 CAPLUS (Copyright 2002 ACS)
Abstract
A method was described for the direct prepn. of ball-grain RDX that afforded different particle size distributions. HNO3(98%) was reacted with a second acid to form a soln. of RDX in HNO3; the ball-grain RDX with different particle size distributions were then prepd. directly by making use of the technique of solvent/nonsolvent pptn. Expts. with scales of 50 g yield were carried out in the lab. The six classes of ball-grain RDX prepd. directly the acids met the American military specification qualities of the products. Special attention was paid to factors which affect the granularity and spheroidization of RDX (e.g., crystn. temp., stirer speed, and diln. rate).
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Recovery of ingredients from plastic-bonded propellants. Bohn, M. A.; Schweppe, R.; Weisweiler, W. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Int. Annu. Conf. ICT (1995), 26th(Pyrotechnics), 44/1-44/32. CODEN: IACIEQ Journal written in German. CAN 124:33073 AN 1995:866216 CAPLUS (Copyright 2002 ACS)
Abstract
The possibility of recovery of energetic ingredients and binders from urethane-bonded propellants was examd. in a process based on high-temp. hydrolysis/solvolysis at 130-170° in pure water and alk. (0.05-0.5 N NaOH) medium. Ammonium perchlorate could be 98% recovered from the aq. soln. from hydrolysis of a 40:60 polyetherdiol-based urethane (prepd. from Lupranol 1000, Lupranol 2021, and TDI); the polyetherpolyol component was 84-90% recoverable and did not show any structural or mol. wt. changes after hydrolysis at 170° for 2 h. Treatment of a second propellant (contg. 86 wt.% RDX and 14 wt.% glycidyl azide-Desmodur N100 copolymer) at 130, 150, and 179° in pure water and 0.05 N NaOH for 10, 30, and 60 min resulted in high recovery of RDX but the GAP-derived urethane was recovered with a significant loss of azide groups. In this case, the azide group reacted to form N2 and nitrenes which formed non-reactive carbon-nitrogen bonds through intermol. insertion reactions, in addn. to nitrogen-contg. gaseous products and aq. ions.
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Process and apparatus for producing ultrafine explosive particles. (du Pont de Nemours, E. I., and Co., USA). Israeli (1995), 24 pp. CODEN: ISXXAQ IL 100231 A1 19950124 Patent written in English. Application: IL 91-100231 19911203. CAN 123:117652 AN 1995:743038 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
IL 100231 A1 19950124 IL 1991-100231 19911203
Abstract
An app. for producing ultrafine explosive particles comprises (1) means for injecting a soln. of a crystallizable explosive compns. and a nonsolvent soln. for mixing with the explosive compn. soln., (2) nozzles being adapted for moving the explosive compn. and nonsolvent solns., (3) venturi means communicating with nozzle means, and (4) explosive particle collection means connected with venturi means. The app. further comprises an auxiliary inlet means coaxial with and surrounding the explosive compns. and the nonsolvent soln. inlet means. The nozzle means include first and second continuous orifices. The ultrafine granular explosives which when incorporated into a binder system have the ability to propagate in thin sheets and have very low impact and very high propagation sensitivities.
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Method for making explosive charges by filtering liquid explosive. Vlassov, D. A. St. Petersburg Technological Inst., Russia. Hanneng Cailiao (1993), 1(1), 27-30. CODEN: HACAFQ Journal written in English. CAN 123:117600 AN 1995:695221 CAPLUS (Copyright 2002 ACS)
Abstract
A relatively safe method was developed for manuf. of explosive charges contg. a solid cryst. explosive and a liq. thermoplastic or thermosetting (i.e., polymg.) material (typically cryst. RDX and molten TNT). The technique involved filling of shells; calcns. were presented to calc. the porosity of RDX and the vol. of molten TNT that is necessary to fill the pores. The method was esp suitable for manuf. of rocket fuel compns. contg. solid oxidizer, metals, and liq. polymeric binder.
Bibliographic Information
Study on the nitrolysis of hexamethylenetetramine by NMR spectrometry. Fang, Zhijie; Chen, Li; Wang, Shaofang; Chen, Ju; Li, Fuping. Inst. Chemical Engineering, Nanjing Univ. Science and Technol., Nanjing, Jiangsu, Peop. Rep. China. Propellants, Explos., Pyrotech. (1995), 20(2), 83-6. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 122:294747 AN 1995:550727 CAPLUS (Copyright 2002 ACS)
Abstract
The nitrolysis of hexamethylenetetramine (HA) and 1,3,5-trioxane was studied by NMR spectrometry. The structure of the nitrolysis products of the trioxane could be monomethylenedinitrate, dioxymethylenenitronitrate and trioxymethylenenitronitrate, of structures O2N(OCH2)nONO2 (n = 1,2,3). A comparison of the 1H and 13C spectra of the nitrolysis mixt. of HA with the nitrolysis products of trioxane proved that in the nitrolysis mixt. of HA, the methylene group which cannot be used to form 1,3,5-triazacyclohexane (RDX) appears in O2N(OCH2)ONO2 and not in CH2(ONO2)2.
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Separation of RDX and HMX by recrystallization using supercritical fluids as anti-solvent. Gallagher, Paula M.; Krukonis, Val J.; Coffey, Michael P. (Phasex Corp., USA). U.S. (1995), 20 pp. CODEN: USXXAM US 5389263 A 19950214 Patent written in English. Application: US 92-886603 19920520. CAN 122:269545 AN 1995:420719 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5389263 A 19950214 US 1992-886603 19920520
Abstract
Materials that are ordinarily difficult-to-comminute such as a mixt. of RDX and HMX are sepd. by dissolving in a common liq. solvent to form a soln., adding to the soln. a supercrit. fluid to induce pptn. of one component of the components of the solid mixt. resulting in a pptd. component, and collecting the pptd. component. The process shows effective at sepg. HMX and RDX to obtain a ppt. of RDX which is essentially free of HMX.
Bibliographic Information
Recrystallization process of RDX and cobalt chloride using anti-solvent methods. Krukonis, Val J.; Gallagher, P. M.; Coffey, M. P. (Phasex Corp., USA). U.S. (1994), 21 pp. Cont.-in-part of U.S. Ser. No. 421,978, abandoned. CODEN: USXXAM US 5360478 A 19941101 Patent written in English. Application: US 91-723245 19910628. Priority: US 89-421978 19891016. CAN 122:34594 AN 1995:229370 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5360478 A 19941101 US 1991-723245 19910628
Priority Application Information
US 1989-421978 19891016
Abstract
In recrystg. solid RDX from systems comprising a solute which is the eventual material recrystd. and a liq. which is a suitable solvent for the solute, a gaseous component which is sol. within the solvent is added into the system to cause the solvent to approach or attain a supersatd. state and solute material to ppt. By control of process parameters such as pressure, temp., time, and rate, rate of injection of gas, the properties of the material recrystd. can be influenced.
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Rapid near-IR measurements of explosives. Eisenreich, N.; Kull, H.; Hertz, J. Fraunhofer-Institut fur Chemische Technologie, Pfinztal, Germany. Int. Annu. Conf. ICT (1994), 25TH(ENERGETIC MATERIALS-ANALYSIS, CHARACTERIZATION AND TEST TECHNIQUES), 86/1-86/7. CODEN: IACIEQ Journal; General Review written in German. CAN 122:13139 AN 1995:192723 CAPLUS (Copyright 2002 ACS)
Abstract
A review, with 6 refs., of the use of rapid near-IR (NIR) spectroscopy for online evaluation of explosives (esp. during manuf. and processing). Topics discussed include rapid NIR spectrometry with acoustooptical filters and the NIR spectra of energetic materials. Spectra given were nitromethane, GAP, TAGN (triaminoguanidine nitrate), TNT, RDX, HMX, ammonium nitrate, and ammonium perchlorate.
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Explosive property and mechanical characteristics of the trial PBX consisting of RDX and HTPB. Sato, Junichi; Shinkai, Masanori; Ito, Takeshi. Dep. Chem., Natl. Def. Acad., Yokosuka, Japan. Kayaku Gakkaishi (1994), 55(3), 89-95. CODEN: KAGAEA Journal written in English. CAN 121:160342 AN 1994:560342 CAPLUS (Copyright 2002 ACS)
Abstract
The prepn. of PBX (plastic-bonded explosive), consisting of RDX and hydroxy-terminated polybutadiene (HTPB) binder, was attempted. Various tests of explosive properties and mech. characteristics were carried out on the RDX-HTPB compn. as a trial PBX.
Bibliographic Information
Extraction of nitramine propellants using supercritical fluids. Morris, J.B.; McNesby, K.L.; Pesce-Rodriguez, R.A.; Schroeder, M.A.; Fifer, R.A. WT, U.S. Army Res. Lab., Aberdeen Proving Ground, MD, USA. Int. Annu. Conf. ICT (1993), 24th(Energetic Materials: Insensitivity and Environmental Awareness), 37-1/37-12. CODEN: IACIEQ Journal written in English. CAN 120:326901 AN 1994:326901 CAPLUS (Copyright 2002 ACS)
Abstract
The addn. of org. modifiers (co-solvents) for CO2-based supercrit. fluid extn. of an RDX-based LOVA composite gun propellant was examd. for the purpose of maximizing RDX recovery. Under supercrit. fluid extn. conditions (32° and 55 MPa for 45 min), MeCN displayed the greatest soly., or dissoln. rate enhancement, for RDX, with nitromethane a close second. When extg. solid gun propellant, solvent-modified CO2 fluid caused significant swelling of the propellant relative to the use of heat CO2. In addn. to RDX, the gun propellant contained cellulose acetate butyrate, nitrocellulose, plasticizer, and other additives.
Bibliographic Information
Design and calibration of pulsed vapor generators for TNT, RDX and PETN. Davies, J. P.; Blackwood, L. G.; Davis, S. G.; Goodrich, L. D.; Larson, R. A. Idaho Nat. Eng. Lab., Idaho Falls, ID, USA. Editor(s): Yinon, Jehuda. Adv. Anal. Detect. Explos., Proc. Int. Symp., 4th (1993), Meeting Date 1992, 513-32. Publisher: Kluwer, Dordrecht, Neth CODEN: 59MKAE Conference written in English. CAN 120:221786 AN 1994:221786 CAPLUS (Copyright 2002 ACS)
Abstract
Computer-controlled explosive vapor generators for TNT, RDX, and PETN were built and calibrated to support an independent validation and verification facility for Explosive detection systems for the Federal Aviation Administration (FAA). The generators were constructed using pure explosive suspended on quartz beads which were then loaded into a coiled stainless steel tube. A carrier gas (ultra-pure air) was passed through the coil to carry the explosive mols. The generators were capable of delivering a pulse of varying explosive mass through the control of coil temp., air flow rate, and pulse width. Preliminary calibrations were completed in the picogram-to-nanogram range using an ion mobility spectrometer as the calibrating instrument. The explosive vapor generators can be used as quant. vapor stds. to establish the lower detection limits for explosive detection systems systems.
Bibliographic Information
Process for preparation of RDX. Lukasavage, William J.; Nicolich, Steven; Slagg, Norman. (United States Dept. of the Army, USA). U.S. (1993), 4 pp. CODEN: USXXAM US 5250687 A 19931005 Patent written in English. Application: US 92-936375 19920828. CAN 119:271209 AN 1993:671209 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
US 5250687 A 19931005 US 1992-936375 19920828
Abstract
The title process comprises repeated sequential addn. of NH4NO3/HNO3 and Ac2O to DAPT. This method, with continuous addn. of quantities of DAPT, provides near-quant. yields of RDX.
Bibliographic Information
Synthesis of carbon-14 labeled hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX). Horvath, Karoly; Alworth, William L. Dep. Chem., Tulane Univ., New Orleans, LA, USA. J. Labelled Compd. Radiopharm. (1993), 33(6), 467-71. CODEN: JLCRD4 ISSN: 0362-4803. Journal written in English. CAN 119:271112 AN 1993:671112 CAPLUS (Copyright 2002 ACS)
Abstract
14C-labeled hexahydro-1,3,5-trinitro-1,3,5-triazine was prepd by nitrolysis of hexahydro-1,3,5-tripropionyl-1,3,5-triazine (1) for bioenvironmental studies. 1 Was synthesized from paraformaldehyde and propionitrile by a modified method reported earlier.
Bibliographic Information
On the use of AM1 and PM3 methods on energetic compounds. De Paz, Jose Luis G.; Ciller, Juan. Dep. I+D, Union Espanola Explosivos, Madrid, Spain. Propellants, Explos., Pyrotech. (1993), 18(1), 33-40. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 118:237100 AN 1993:237100 CAPLUS (Copyright 2002 ACS)
Abstract
Stewart's new semi-empirical method MNDO-PM3 (PM3) was compared with the well-known Dewar's AM1 method in the study of the heats of formation and dipole moments of nitro-substituted compds., esp. for some energetic materials. The PM3 method had better performance than the AM1 method. Adjacent lone pair-lone pair repulsions were better described at the PM3 level; the known systematic correction of .apprx.-9 kcal/mol for each C-NO2 group of the AM1 method became +3.5 kcal/mol at the PM3 level. PM3 results for N-NO2 contg. compds. were directly comparable to exptl. gas phase data.
Bibliographic Information
Process and apparatus for producing ultrafine explosives. McGowan, Michael James. (du Pont de Nemours, E. I., and Co., USA). PCT Int. Appl. (1993), 26 pp. CODEN: PIXXD2 WO 9304018 A1 19930304 Designated States W: CA, NO. Designated States RW: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LU, NL, SE. Patent written in English. Application: WO 91-US5900 19910827. CAN 118:172045 AN 1993:172045 CAPLUS (Copyright 2002 ACS)
Patent Family Information
Patent No. Kind Date Application No. Date
WO 9304018 A1 19930304 WO 1991-US5900 19910827
W: CA, NO
RW: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LU, NL, SE
EP 600881 A1 19940615 EP 1991-916893 19910827
EP 600881 B1 19960424
R: CH, DE, FR, GB, LI
WO 9304019 A1 19930304 WO 1991-US6748 19910924
W: CS, SU
Priority Application Information
WO 1991-US5900 19910827
Abstract
The process comprises prepg. a stream of a soln. of the explosive dissolved in a solvent and a stream of an inert nonsolvent, injecting the two streams through concentric orifices of a nozzle into a mixing chamber by injecting nonsolvent stream through the central orifice and explosive stream through the outer orifice, converging the streams in a mixing zone under turbulent conditions to entrap the explosive compn. in droplets of nonsolvent and to rapidly ppt. the explosive compn. as spheroidal particles, and recovering the particles from the solvent and nonsolvent materials.
Bibliographic Information
Explosive biodegradation in soil slurry batch reactors amended with exogenous microorganisms. Shen C F; Hawari J A; Paquet L; Ampleman G; Thiboutot S; Guiot S R Environmental Bioengineering Group, Biotechnology Research Institute, National Research Council, 6100 Royalmount Avenue, Montreal, Quebec H4P 2R2, Canada WATER SCIENCE AND TECHNOLOGY (2001), 43(3), 291-8. Journal code: DV8. ISSN:0273-1223. Journal; Article; (JOURNAL ARTICLE) written in English. DN 21274696 PubMed ID 11381919 AN 2001295394 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
The present study explores the feasibility of biotreatment of 2,4,6-trinitrotoluene (TNT) and hexahydro-1,3,5-trinitro- 1,3,5-triazine (RDX)-contaminated soils in slurry batch reactors. Radiorespirometric assays showed that anaerobic sludge was able to mineralize 59% RDX to CO2 although significant mineralization of TNT was not observed in all cases. TNT and RDX at concentrations higher than 50 and 100 mg/L respectively were inhibitory to methanogenesis (used as a bioindicator), however, methanogenesis recovered after TNT was transformed into less toxic triaminotoluene. Bioslurry batch reactors containing 40% of contaminated soil (2000 mg RDX and 1000 mg TNT/kg dry soil) were operated under various conditions. Both TNT and RDX were persistent to soil indigenous microbes. Degradation of both TNT and RDX was enhanced by the municipal sludge amendment, although degradation of RDX was only achieved under anaerobic conditions.
Bibliographic Information
Type I nitroreductases in soil enterobacteria reduce TNT (2,4,6,-trinitrotoluene) and RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine). Kitts C L; Green C E; Otley R A; Alvarez M A; Unkefer P J Environmental Biotechnology Institute, California Polytechnic State University, San Luis Obispo 93407, USA. ckitts@calpoly.edu CANADIAN JOURNAL OF MICROBIOLOGY (2000 Mar), 46(3), 278-82. Journal code: CJ3. ISSN:0008-4166. Journal; Article; (JOURNAL ARTICLE) written in English. DN 20211112 PubMed ID 10749541 AN 2000211112 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
Many enteric bacteria express a type I oxygen-insensitive nitroreductase, which reduces nitro groups on many different nitroaromatic compounds under aerobic conditions. Enzymatic reduction of nitramines was also documented in enteric bacteria under anaerobic conditions. This study indicates that nitramine reduction in enteric bacteria is carried out by the type I, or oxygen-insensitive nitroreductase, rather than a type II enzyme. The enteric bacterium Morganella morganii strain B2 with documented hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) nitroreductase activity, and Enterobacter cloacae strain 96-3 with documented 2,4,6-trinitrotoluene (TNT) nitroreductase activity, were used here to show that the explosives TNT and RDX were both reduced by a type I nitroreductase. Morganella morganii and E. cloacae exhibited RDX and TNT nitroreductase activities in whole cell assays. Type I nitroreductase, purified from E. cloacae, oxidized NADPH with TNT or RDX as substrate. When expression of the E. cloacae type I nitroreductase gene was induced in an Escherichia coli strain carrying a plasmid, a simultaneous increase in TNT and RDX nitroreductase activities was observed. In addition, neither TNT nor RDX nitroreductase activity was detected in nitrofurazone-resistant mutants of M. morganii. We conclude that a type I nitroreductase present in these two enteric bacteria was responsible for the nitroreduction of both types of explosive.
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Degradation of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) by Stenotrophomonas maltophilia PB1. Binks P R; Nicklin S; Bruce N C Institute of Biotechnology, University of Cambridge, United Kingdom APPLIED AND ENVIRONMENTAL MICROBIOLOGY (1995 Apr), 61(4), 1318-22. Journal code: 6K6. ISSN:0099-2240. Journal; Article; (JOURNAL ARTICLE) written in English. DN 95266812 PubMed ID 7747953 AN 95266812 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
A mixed microbial culture capable of metabolizing the explosive RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine) was obtained from soil enrichments under aerobic and nitrogen-limiting conditions. A bacterium, Stenotrophomonas maltophilia PB1, isolated from the culture used RDX as a sole source of nitrogen for growth. Three moles of nitrogen was used per mole of RDX, yielding a metabolite identified by mass spectroscopy and 1H nuclear magnetic resonance analysis as methylene-N-(hydroxymethyl)-hydroxylamine-N'-(hydroxymethyl)nitroamin e. The bacterium also used s-triazine as a sole source of nitrogen but not the structurally similar compounds octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine, cyanuric acid, and melamine. An inducible RDX-degrading activity was present in crude cell extracts.
Bibliographic Information
Isolation of three hexahydro-1,3,5-trinitro-1,3,5-triazine-degrading species of the family Enterobacteriaceae from nitramine explosive-contaminated soil. Kitts C L; Cunningham D P; Unkefer P J Los Alamos National Laboratory, New Mexico 87545 APPLIED AND ENVIRONMENTAL MICROBIOLOGY (1994 Dec), 60(12), 4608-11. Journal code: 6K6. ISSN:0099-2240. Journal; Article; (JOURNAL ARTICLE) written in English. DN 95110151 PubMed ID 7811097 AN 95110151 MEDLINE (Copyright 2002 U.S. National Library of Medicine)
Abstract
Three species of the family Enterobacteriaceae that biochemically reduced hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) were isolated from nitramine explosive-contaminated soil. Two isolates, identified as Morganella morganii and Providencia rettgeri, completely transformed both RDX and the nitroso-RDX reduction intermediates. The third isolate, identified as Citrobacter freundii, partially transformed RDX and generated high concentrations of nitroso-RDX intermediates. All three isolates produced 14CO2 from labeled RDX under O2-depleted culture conditions. While all three isolates transformed HMX, only M. morganii transformed HMX in the presence of RDX.