EDNA

[mav]

Excuse me under my bad English,
I am EDNA (ethylendinitramin) makes from ethylen urea (143 g ethylen glycol+ 550 g urea near 240 C and depolymerization) nitration 98 % HNO3 and hydrolysis by water ( 68 g ethylen urea + 325 g 98% HNO3; HNO3 with cool on 0 C and dose in mixture EM, near 45 C this temperature preserve cooling , let with into-react c. 5 mine. and dilute H2O in intensive cooling on 40-50 %, cool on 20 C and filter off) product with under intensive mixture bring into up small dues into 10 multiple quantity waters , (which contains 0,3 g CH3COONA on 100 ml)about temperatures 88-89 C. Get cool on 20 C and filter off: yield was c. 100 g


Found am instruction (http://www.geocities.com/spxors/)na preparation EDNA and non-believer to him

EDNA
prepare mixture from 100 g dichloretanu and 170 g 10% solution NH4OH. Mixture heat on water or oily bath into 100 C and near these temperatures let mixture react for the duration of 20 minutes. Then into solution add 210 g 60% HNO3 and let near these temperatures mixture react even 15 minutes. Then mixture cool on 20 C and filter off finished EDNA (c. 130 g). on account of production astable salt.
1) (CH2CI)(CH2Cl) + 2NH3 => (CH2(NH2))(CH2(NH2)) + 2HCl
2) (CH2(NH2))(CH2(NH2)) + 2HNO3 => (CH2(NH2))(CH2(NH2)) * 2HNO3
3) (CH2(NH2))(CH2(NH2)) * 2HNO3 =(t) => NO2NHC2H4NHNO2


It's her possibility so make?

[PHILOU Zrealone]

The first one look OK! But the second one is wrong for one part!
The frist one:
CH2OH-CH2OH + NH2-CO-NH2 ---> (CH2-NH)2C=O + (-NH-CO-NH-CH2-CH2-)n
Then making those react with HNO3 conc and H2SO4 conc ---> dinitrourea's like
(CH2-NH)2C=O +HNO3+H2SO4 --> (CH2-NNO2)2C=O +H2O +H2SO4
(-NH-CO-NH-CH2-CH2-)n +HNO3+ H2SO4 --> (-NNO2-CO-NNO2-CH2-CH2-)n

After hydrolysis
(CH2-NNO2)2C=O +2H2O --> (CH2-NHNO2)2+ H2CO3
(CH2-NHNO2)2 is of course O2NNH-CH2-CH2-NHNO2 EDNA (ethylene dinitramine)

(-NNO2-CO-NNO2-CH2-CH2-)n + H2O --> O2NNH-CH2-CH2-NHNO2 + H2CO3

The second one:
CH2Cl-CH2Cl + 2 NH3 --> ClNH3-CH2-CH2-NH3Cl
(possible)!
ClNH3-CH2-CH2-NH3Cl + 2HNO3 --> O3NNH3-CH2-CH2-NH3NO3 + 2HCl
(possible!)
Heating the last one is wishing for death and you will never get to the dinitramine by that way even with conc H2SO4 (what is strictly dangerous to do since nitramines are sensitive to H2SO4 and can runaway-explode-detonate!).

You will say that in the first case we have used H2SO4! Yes that's true but there it is possible to do so because nitrourea's are insensitive to H2SO4 reason why they pass via an urea derivative and they don't do directly the EDNA from diamino ethane!!!!


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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[VasiaPupkin]

Excuse me for my bad english.

Hello mav! I have a some questions for you. Why you have wrote temerature near 240 C? In my russians chemical encyclopedia and dictionary the boiling point of ethyleneglycol is 197.6 Ñ. And can I boil mixture, which consist from 1 mole ethyleneglycol per 1 mole of urea? Or it is impossible?
Also from that encyclopedia: "ethylenediaminedinitrate is decomposed to EDNA and water when heated" (I dont know exactly in what temperature)
I tryed to carry out the second method about year ago. In result - EDNA. But this method is very uncomfortable, espesially the first reaction. I used 25% ammonia solution with a great surplus. 1) ClCH2CH2Cl + 4NH3 =>H2NCH2CH2NH2 + 2NH4HCl. This reaction is provided by smell, espesially when heat. Ñancerogenic ethyleneimine is able to appear in some conditions. And I have tryed a "interphase" catalyse with benzylammonium salt (some kinds of cars shampoo). The speed of reaction was improved, and it could possible to carry out the process with 60 Ñ. I have to receive some EDNA with heat, but the second portions was overheated and burns.
But process is still uncomfortable. How do you think can I make EDNA by thermal decomposition of ethyleneurea nitrate (salt)? Did you made EDNA's lead salt? I heard its a primary explosive.

[simply RED]

I may try the second process with the CH2Cl-CH2Cl soon in very small quantities but i also doubt it will work.
How powerful is ethylene diamine dinitrate?

[PHILOU Zrealone]

Don't forget that the dichlorethane can react with ammonia but also with another aminoethan already formed...
CH2Cl-CH2Cl + NH3 ---> CH2Cl-CH2-NH3Cl
CH2Cl-CH2-NH3Cl + NH3 --> CH2Cl-CH2-NH2 + NH4Cl
CH2Cl-CH2-NH2+CH2Cl-CH2Cl --> ClNH2(CH2-CH2Cl)2

This is why an excess of NH3 has to be used!
I think it is more convenient to use urea as a starting material since there no gaseous NH3!
Why not dichloroethan and urea....



------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Mr Cool]

Philou, when you say, "why not dichloroethane and urea...?", is that a question, or are you suggesting that it will work?

[mav]

Hello Vasia, may I the send instruction on preparations EDNA from college script in png c. 800 kB is it only in Czech language, but whether is of Rusland so with translation wont'you be in a tight spot. Temperature with teak mixture urea + ethylenglykolu. Temperature with slowly increases from 140 on 240 c. Is necessary backward condenser.
Charge: 500g urea, 143 g ethylenglykolu = 100 g ethylenurea ( 50% yield).Cook with resin and compressive with depolymerization.

For pressureless depolymerization resin with takes urea : ethylenglykol 3-3,5 :1 (300-340g ethylenglykolu :100g urea)
I have productions ethylenmocoviny from ethylendiaminu and urea.

[VasiaPupkin]

Hello All ! Excuse me for my bad english.
Philou, I almost agree with you about reactions. It Really, this reactions could be if I used more quantity of dichlorethane. In result - in water soluble polymer.
I tryed many kind reaction (dichlorethane with urea too). But there is no good result - no reaction or very slow reaction even it catalysed. I think more perspective is to use an ethyleneglycol at homemade condition. (its more spread than dichlorethane. Its a main component of car engine's cooling liquid (I dont know its name on english http://theforum.virtualave.net/ubb/smilies/smile.gif. And dichlorethane much more toxic for liver when vaporised)

[VasiaPupkin]

Hi mav! Excuse me for my bad english too, but I dont know Czech language quite http://theforum.virtualave.net/ubb/smilies/frown.gif
Thanks for information. If you have ethylenediamine try to prepare EDNA with thermal decomposition of nitrate. Ok. I have guess just now. Right reaction is HOCH2CH2OH + 3(NH2)2CO => Ethyleneurea (or polymer product) + 4NH3 + 2CO2. There are many reactions with urea like this. You may send instruction on mail: (crvonline@fromru.com). But much better if insruction will be on russian or english http://theforum.virtualave.net/ubb/smilies/smile.gif Some I will try to realize. If you know russian, I can provide to you with adress of russian konference like this forum. I know the russian site which provided to you with information about EDNA from dichloroethane,(even first source of info) - You should not trust them much http://theforum.virtualave.net/ubb/smilies/smile.gif. They dont know chemistry correctly. And sign "?" was there.

[simply RED]

Excuse me, philow, but what is the structural formula of: ClNH2(CH2-CH2-Cl)2 ?
it sounds something like iprite? is the N- 5 valent?

[simply RED]

I tried the dichloroethane process but it didn't work. The dichloroethane didn't react with the ammonia(must it dissolve). I wait it to react for 20 mins on 100degrees Celsius (10%ammonia solution). No reaction, and then i put the nitric acid. I thought it will explode at this temp, but it didn't reat at all, after 15 mins still dichloroethane floating round the reaction liquid. Byt it will be innteresting to try termal decomposition of NH2-(CH2)2-NH2.2HNO3, i doubt it will work...

[VasiaPupkin]

Hello Simply Red! Did you really see what I said to mav? I said - Reciept from (www.geocities.com/spxors/) dont work. Because those guys dont know chemistry well. This reaction may be carryed out only with catalyst at home condition. A few days (maybe 1 week) in the room temperature. Or a few hours when heated to 60 C. I used 25% ammonia solution.
And only one toxic product maybe if bad proportion. ClCH2CH2Cl + 3NH3 => (CH2)2NH + 2 NH4Cl. Ethyleneimine very toxic and cancerous with skin contact and when vaporized. Its smells like ethylenediamine.
I have a question for all who knows. Do you know gas volume and achievment in Truzl's Pb bomb for PETN, RDX, HMX and especially for EDNA? I hope this info will be from advanced book.

[Mr Cool]

Not from an advanced book, but quite a reliable site (http://edetonator.hyperlink.cz/HOME1.htm):

Trauzl test:

RDX: 450 ml/10g
PETN: 500
HMX: 470
EDNA: ?

Gas volume:

RDX: 908 cm3/g
PETN: 790
HMX: 908 (I'm guessing)
EDNA: ?

Sorry, I could find no information on EDNA.

[wantsomfet]

EDNA: gas volume 908 l/kg, heat of explosion 1276 kcal/kg, velocity of detonation 7750 m/s @ 1,55 g/ccm
RDX: gas volume 910 l/kg, Trautzl: 450-520 ccm
HMX: Trautzl: 450 ccm*
PETN: gas volume 768 l/kg, heat of explosion 1530 kcal/kg, Trautzl: 500 ccm (sand) 560 ccm (water)

*there's not much about HMX in Urbanski...


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[This message has been edited by wantsomfet (edited July 05, 2001).]

[VasiaPupkin]

Thanks guys! I try to check info from my books. I thought a misprint was there. Because I saw info (like (www.faqs.org/faqs/sci/chem-faq/part3/)) which dont meet with my sources. But I really cannot find info about Trauzl for EDNA. But it probably some less than RDX's. And very interestly why gas volume so different for RDX and HMX (908 and 782). Chemistry for this explosives almost equally !?


[This message has been edited by VasiaPupkin (edited July 06, 2001).]

[cutefix]

There is a simple ternary explosive composition made by combining stoichiometric mixture of ethylenediamine,nitric acid,ammonia,and potassium hydroxide forming ethylenediaminedinitrate,ammonium nitrate,and potassium nitrate.The procedure is simple and looks interesting.check it at US Patent 4,419,155.

[PHILOU Zrealone]

I was only saying that urea is more convenient to use at home than ammonia and that it may work!Especially if you have to heat it!

I personaly doubt the only products to be ethyleneimine (CH2)2NH and diaminoethane (NH2-CH2-CH2-NH2) when mixing dichloroethane and ammonia solution.

For sure the glycol process is the best!

(ClCH2CH2)2NH2Cl is indeed near the structura of hyperite ClCH2CH2-S-CH2CH2Cl since it is ClCH2CH2-NH2Cl2-CH2CH2Cl

Nitrogen may look pentavalent but it is not the case actually when under the aminium form (salt of amine) N is linked to 4 atoms generating a + charge that has to be compensed by an anion...never seen in NH4Cl if I follow your logic N is linked to 4 H and 1 Cl what make it pentavalent but actually it is a salt and thus NH4(+) + Cl(-)
here I have written it like that but I should have had written NH3.HCl and ClCH2CH2-NH-CH2CH2Cl.HCl

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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[PHILOU Zrealone]

Thermal decomposition of EDAdinitrate salt can only result in an explosion-fire.

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[VasiaPupkin]

Hmmm. In my "Chemical encyclopedia" '98 is says that Dinitrate decomposes to EDNA and water when heated. But there's nothing about temperatures :-(

[cutefix]

I just have a second look with EDNA in volume 3 of the Urbanski book and saw the information about the synthesis of it from ethylene urea using mixed acids.
It is stated as
“ one part of ethylene urea to every ten parts of mixed acid mixture containing nitric acid 15.4% sulfuric acid 74 % and water 10.6%.”
Or simply as e.g 10 parts of ethylene urea to 100 parts of the mixed acids which means that for illustrative explanation, you only need for 10 units of the ethylene urea to 15 .4 units of HNO3 , 74 units of sulfuric acid and 10.6 units of water.
Now if we use a blend of water and nitric acid the resulting nitric acid concentration will be around 60% within the range of the common nitric acid which is 65-70& HNO3 concentration.
Even if there will be slight excess of nitric acid you will still get Ethylene dinitramine in the end of the synthesis.
The most important part is the acids are easily available and the raw material can be procured from chemical supply, free from suspicion
So roughly it will be 26% nitric acid and 74% sulfuric acid..
Then if you are using such mixed acid then for 10 units of ethylene urea you need 26 units of nitric acid and 74 units of sulfuric acid.
Pretty simple.
There is no need then to find the fuming nitric acids with concentration reaching more than 90%..
Now the synthesis of EDNA is straight forward

{CH2NH2}2CO + mixed acid( at 10degC) ={CH2NNO2)2CO
Now this intermediate dinitroethylene urea is not very stable and dropping it in boiling water and cooking it for some time will release the EDNA
{CH2NNO2}2CO + H2O(100 deg C) ={CH2NHNO2)2 + CO2

Now EDNA is a powerful explosive better than Tetryl the detonation velocity at a density of 1.53 is 7750 meters per second ;and as easily initiated as picric acid, then I wonder why nobody here is playing with these unique material?
BTW ethylene urea is not a restricted material but widely used industrial chemical.

[simply RED]

What about the toxicity of these materials?

[cutefix]

Materials, you mean the the ingredients?
Here you have sulfuric acid and nitric acid , then you have ethylene urea. As well as the unstable intermediate dinitiroethylene urea.
Most of the people here have played a lot with these strong acids which are already dangerous chemicals to handle..
It means that people here are matured enough to handle dangerous chemicals like a professional ,and any safety issues are already considered during their experiments.
BTW,I cannot find any toxicological details or MSDS of ethylene urea.
The related product ethylene thiourea is known decomposition product of carbamate insecticides during its degradation, through the release of sulfur that will be bound by tissues and can promote cancerous lesions but there was not comment about the effects of ethylene urea. Maybe if you have the Merck Index that will give some guide about this issue.
But I am certain that if anybody had access to the main ingredient, the guy will not think that its poisonous or not but will go on play with it.
The main product is an interesting material to play BOOM anyway....

[Myrol]

Today I made just for Fun some Ethylene Urea and it worked great :p .
I prepared two days ago a batch with 125g pure Ethyleneglycole and
250g Urea. It does absolutely nothing until the mix reached 150°C.
It was a faint straw-yellow solution wich started to give off
white fumes and a harsh smell of Ammonia. It looked like it boils,
but it didn't. I warmed it more and more until it reached 220°C.

I stopped the heating and let it cool down. It's VERY EASY to
make Ethylene urea, I think it should work even with Anti-freeze
and Urea-fertilizer. Im not sure about the solubilities. Is Ethylene urea
solubile in Water or Ethanole? I want to clean the stuff a little via
recristallization. After this I can make some EDNA.

I think, 16,5ml 67% Nitric Acid and 42ml 96% Sulfuric Acid
will nitrate 10g 2-Imidazolidone perfectly! Its the mix like
used in Industrial Nitrationplants. Has someone some
Polyformaldehyd handy? I think, if we heat Urea
and (CH2O)n together it CAN form some METHYLENE urea.
Should be a faster way to come MEDINA closer, huh?
P.s. EDNA has a Trautzl Test of 410ccm per 10g ;)