megalomania
June 21st, 2003, 11:43 AM
cutefix
Frequent Poster
Posts: 330
From: california
Registered: MAY 2001
posted 07-28-2001 03:01 AM
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This formula was obtained from a former classmate of mine who became an organic chemist.The actual yield that he got from it was only 190 grams of beta HMX:
Preparation and Purification of HMX
Prepare the following solutions:
Solution A-Dissolve 233 grams of ammonium nitrate in 218 grams of 99% Nitric acid.(Be sure to maintain the solution above 20C to prevent crystallization of ammonium nitrate).
Solution B-Dissolve 101 grams of hexamine in 165 grams of acetic acid.
Prepare acetic anhydride portions- a) 320 grams b) 480 grams
Method:
1) In a 6-10 liter flask,put in 785 grams of glacial acetic acid,13 grams of acetic anhydride and 17 grams of paraformaldehyde.This flask is equipped with a stirrer,thermometer,and 3-dropping funnels.Maintain temperature at 44 C(by means of a water bath).
2) The hexamine and acetic anhydride were added continuously and in proper proportions;That is ,add four portions of 66.5 gram of solution B and three portion of 64 grams acetic anhydride alternately(beginning and ending with solution B).Finally add the remaining 128 grams of acetic anhydride.These additions should be done within 15 minutes.Then let it stand for 15 minutes.
3) From the 480 grams of acetic anhydride,use 320 grams,to be added in four portions( of 80 grams each),alternately,with four portions of approx.68 grams(each) of solution A,then finally add the remaining 160 grams of acetic anhydride.The addition should be also done in within 15 minutes.Let it stand for about 60 minutes.
Purification:
1) Pour the reaction mixture into a 7-10 liter flask, equipped with a suitable reflux condenser.
2) Add 350 gram of hot water (75-90C) to the reaction mixture,and reflux for 30 minutes.Cool it to 20C by means of an ice bath and by adding about 2000grams of ice to the mixture.Precipitation will occur and this insoluble material will be filtered out and washed with three(400 gram portions of cold water).The product was then dried.
3) The yield of crude product was 200 grams, or 95% of the theoretical;the purity was above 90%,and the impurity was mostly RDX.
The resulting product is needle-like crystals(alpha –HMX). Convert to beta form by recrystallization from hot solvent like acetone,acetonitrile,or cyclohexanone.Use equal parts by weight of alpha HMX and the solvent.The resulting white crystals of Beta HMX melts at 278-279C and have a purity of 99% or more.
Frequent Poster
Posts: 330
From: california
Registered: MAY 2001
posted 07-28-2001 03:01 AM
--------------------------------------------------------------------------------
This formula was obtained from a former classmate of mine who became an organic chemist.The actual yield that he got from it was only 190 grams of beta HMX:
Preparation and Purification of HMX
Prepare the following solutions:
Solution A-Dissolve 233 grams of ammonium nitrate in 218 grams of 99% Nitric acid.(Be sure to maintain the solution above 20C to prevent crystallization of ammonium nitrate).
Solution B-Dissolve 101 grams of hexamine in 165 grams of acetic acid.
Prepare acetic anhydride portions- a) 320 grams b) 480 grams
Method:
1) In a 6-10 liter flask,put in 785 grams of glacial acetic acid,13 grams of acetic anhydride and 17 grams of paraformaldehyde.This flask is equipped with a stirrer,thermometer,and 3-dropping funnels.Maintain temperature at 44 C(by means of a water bath).
2) The hexamine and acetic anhydride were added continuously and in proper proportions;That is ,add four portions of 66.5 gram of solution B and three portion of 64 grams acetic anhydride alternately(beginning and ending with solution B).Finally add the remaining 128 grams of acetic anhydride.These additions should be done within 15 minutes.Then let it stand for 15 minutes.
3) From the 480 grams of acetic anhydride,use 320 grams,to be added in four portions( of 80 grams each),alternately,with four portions of approx.68 grams(each) of solution A,then finally add the remaining 160 grams of acetic anhydride.The addition should be also done in within 15 minutes.Let it stand for about 60 minutes.
Purification:
1) Pour the reaction mixture into a 7-10 liter flask, equipped with a suitable reflux condenser.
2) Add 350 gram of hot water (75-90C) to the reaction mixture,and reflux for 30 minutes.Cool it to 20C by means of an ice bath and by adding about 2000grams of ice to the mixture.Precipitation will occur and this insoluble material will be filtered out and washed with three(400 gram portions of cold water).The product was then dried.
3) The yield of crude product was 200 grams, or 95% of the theoretical;the purity was above 90%,and the impurity was mostly RDX.
The resulting product is needle-like crystals(alpha –HMX). Convert to beta form by recrystallization from hot solvent like acetone,acetonitrile,or cyclohexanone.Use equal parts by weight of alpha HMX and the solvent.The resulting white crystals of Beta HMX melts at 278-279C and have a purity of 99% or more.