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Method for simultaneously preparing octogen and hexogen

A technology of Octogen and Hexogen, which is applied to the field of simultaneous preparation of Octogen and Hexogen, can solve the problems of low yield and achieve the effects of high yield, good safety and low pollution

Inactive Publication Date: 2010-10-20
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the 1970s, researchers used small molecules to synthesize polynitrotetraazacyclooctane, 1,3,5,7-tetramethate-1,3,5,7-tetraazacyclones HMX intermediates such as octane and 1,3,5,7-tetraacetyl-1,3,5,7-tetraazacyclooctane (TAT), but the yields are all low
(Lukasavage W J. Process for the preparation of 1, 3, 5, 7-tetranitro-1, 3, 5, 7-tetraazacyc looctane [P]: EP, 0547735, 1993-06-23.) However, with acetonitrile and three Polyoxymethylene is a raw material, concentrated sulfuric acid is a catalyst, condensation is prepared TAT and TRAT mixture, and the method that TAT and TRAT mixture is carried out nitration to prepare HMX and RDX, there is no bibliographical information yet at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] 1) Add 48ml of acetonitrile and 800μl of concentrated sulfuric acid into the three-necked flask, and drop the acetonitrile solution of paraformaldehyde into the three-necked flask at a rate of 10ml / min at 80°C, react for 10min, and then rapidly cool down to 0°C, Acetonitrile was removed by distillation to obtain 104.70 g of a mixture of TAT and TRAT, with a total yield of 98.31%, wherein the mass fraction of TAT was 31.23%;

[0032] 2) At room temperature, in a 1000ml beaker, add 1000g concentration of 99% concentrated nitric acid, stir, slowly add 140g P 2 o 5 , the temperature is 35°C, and the reaction solution A is obtained;

[0033] 3) Divide 100 g of the mixture of TAT and TRAT obtained in step 1) into 4 equal parts and add it to the reaction solution in step 2) in batches, stir at a temperature of 40°C, and stir for 1 hour, then let it stand at room temperature for 8 days to react , to obtain reaction solution B;

[0034] 4) Pour the reaction solution B obtaine...

Embodiment 2

[0038] 1) Add 48ml of acetonitrile and 800μl of concentrated sulfuric acid into the three-necked flask, and drop the acetonitrile solution of paraformaldehyde into the three-necked flask at a rate of 10ml / min at 80°C, react for 10min, and then rapidly cool down to 0°C, Acetonitrile was removed by distillation to obtain 104.70 g of a mixture of TAT and TRAT, with a total yield of 98.31%, wherein the mass fraction of TAT was 31.23%;

[0039] 2) Add 150ml of ethyl acetate to the mixture of TAT and TRAT obtained in step 1), stir to separate out the solid, filter, the filter cake is white powdery solid TAT33.60g, the purity is 96.2%, and the yield is 30.29%; in the filtrate 150ml of water was added, crystals were precipitated, and 69.91g of white crystal TRAT was obtained by suction filtration, with a purity of 99.3% and a yield of 65.63%; the total yield of TAT and TRAT was 97.18%;

[0040] 3) at room temperature, in a 1000ml beaker, add 336g concentration of 99% concentrated nitr...

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PUM

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Abstract

The invention relates to a method for simultaneously preparing octogen and hexogen, and belongs to the field of applied chemistry. The method comprises the following steps of: condensing acetonitrile and trioxymethylene serving as raw materials in the presence of a catalyst concentrated sulfuric acid to obtain a mixture of TAT and TRAT; and nitrating the mixture of TAT and TRAT in the presence of nitrating agents, namely concentrated nitric acid and phosphorus pentoxide to obtain a mixture of HMX and RDX, purifying the HMX and the RDX by adopting a DMF complex separation method, and purifying the RDX by adopting an anti-solvent phase separation method; or separating the mixture of TAT and TRAT and then nitrating to obtain the HMX and the RDX. The method has the advantages of simple and readily available raw materials, high yield, low cost, mild nitrating condition, easy temperature control, high safety and small pollution; and the simultaneously obtained HMX and RDX nitro-amine dynamite at one time can be directly used for preparing dynamite formulas without separation.

Description

technical field [0001] The invention relates to a method for simultaneously preparing octogen and rdoxogen, belonging to the field of applied chemistry, in particular to a method for simultaneously preparing and separating octogen (HMX) and rdexogen (RDX) by using a small molecule synthesis method method. Background technique [0002] Octojin (HMX), scientific name 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane, is the highest energy level and the best comprehensive performance that has been used at home and abroad. Good elemental dynamite. RDX, the scientific name is 1,3,5-trinitro-1,3,5-triazacyclohexane, its explosive energy is second only to Octogen, and it is one of the most important elemental high explosives in contemporary times. one. There are many ways to manufacture RDX, including direct nitrification method, Bachmann method, K method, E method, W method and R salt oxidation method, etc. The most commonly used in industry are direct nitrification method and Bac...

Claims

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Application Information

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IPC IPC(8): C07D257/02C07D251/06C06B25/34
Inventor 王鹏孟子晖李杰敏娄忠良徐志斌
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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