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Preparation method of perdeuterated CL-20

A CL-20 and deuterated technology, which is applied in the field of preparation of fully deuterated CL-20, can solve the problems of not being able to meet production needs, increase production costs, and low product yields, and achieve increased yields, reduced production costs, The effect of high purity

Inactive Publication Date: 2020-07-31
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires the use of noble metal palladium as a catalyst in the hydrogenolysis of TADB, which increases the production cost
In addition, the products obtained by the above method are all non-deuterated CL-20. If the deuterated CL-20 is simply prepared by replacing its raw material with a deuterated raw material, the yield of the resulting product is low and cannot meet the requirements. Production needs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Place the three-necked flask containing 8.4 g of deuterated tert-butylamine in a high-precision medium-temperature circulating bath with a temperature of 23 ° C, start stirring, and, under stirring at a speed of 200 rpm, pour the constant pressure dropping funnel at a rate of 1 mL / min to the In the deuterated tert-butylamine, dropwise add the deuterated glyoxal solution whose mass fraction is 40%, wherein the quality of the deuterated glyoxal solution is 6.5g, continue to stir for 35 minutes after the dropwise addition, then add 33.6g to the mixed solution to remove Ionized water, after standing for 10 minutes, the mixture is suction filtered, and the precipitate on the filter paper is washed with deionized water during the suction filtration until the pH value of the filtrate is neutral, and then the filter residue is vacuum-dried at 25°C After drying in the oven for 8 hours, 7.3 g of deuterated N,N'-di-tert-butylethane-1,2-diimine was obtained;

[0021] Place the thre...

Embodiment 2

[0026] Place the three-necked flask containing 21.9 g of deuterated tert-butylamine in a high-precision medium-temperature circulating bath at a temperature of 24°C, start stirring, and, under stirring at a speed of 250 rpm, pass through a constant-pressure dropping funnel at a dropping rate of 1.5 mL / min Add dropwise a deuterated glyoxal solution with a mass fraction of 45% in deuterated tert-butylamine, wherein the quality of the deuterated glyoxal solution is 13.8 g, continue stirring for 40 minutes after the dropwise addition, and then add 109.4 g of the deuterated glyoxal solution to the mixed solution deionized water, after standing for 10 minutes, the mixture is suction filtered, and the precipitate on the filter paper is washed with deionized water during the suction filtration until the pH value of the filtrate is neutral, and then the filter residue is vacuum-filtered at 25°C Dry in a drying oven for 9 hours to obtain 17.6 g of deuterated N,N'-di-tert-butylethane-1,2-...

Embodiment 3

[0032] Place the three-necked flask containing 34.5 g of deuterated tert-butylamine in a high-precision medium-temperature circulating bath at a temperature of 24°C, start stirring, and, under stirring at a speed of 250 rpm, pass through a constant-pressure dropping funnel at a dropping rate of 1.5 mL / min In the deuterated tert-butylamine, it is 50% deuterated glyoxal solution that the mass fraction is added dropwise, wherein the quality of deuterated glyoxal solution is 17.6g, after the dropwise addition, continue to stir for 50 minutes, then add 207g to the mixed solution to remove Ionized water, after standing for 10 minutes, the mixture is suction filtered, and the precipitate on the filter paper is washed with deionized water during the suction filtration until the pH value of the filtrate is neutral, and then the filter residue is vacuum-dried at 27°C After drying in the oven for 10 hours, 25.4 g of deuterated N,N'-di-tert-butylethane-1,2-diimine was obtained;

[0033] P...

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Abstract

The invention relates to a preparation method of perdeuterated CL-20, and belongs to a synthesis technology of a deuterated energetic material. According to the method, deuterated N,N'-di-tert-butyl ethane-1,2-diimine and deuterated benzylamine are used as raw materials, deuterated acetic acid is used as a catalyst to synthesize an intermediate product that is deuterated hexabenzyl hexaazaisowurtzitane. Compared with a traditional method, the yield of the deuterated hexabenzyl hexaazaisowurtzitane is obviously increased; by adopting the deuterated hexaacetyl hexaazaisowurtzitane as a nitrification precursor for nitrification, the product does not contain impurities such as pentanitromonoformyl hexaazaisowurtzitane, and the obtained deuterated CL-20 is high in purity. Compared with common CL-20, the prepared perdeuterated CL-20 has better detonation performance and improved safety and better facilitates practical application.

Description

technical field [0001] The invention relates to a preparation method of fully deuterated CL-20, which belongs to the synthesis technology of deuterated energetic materials. Background technique [0002] Hexanitrohexaazaisowurtzitane, also known as CL-20, is a new type of high-energy-density explosive that has received widespread attention since it was first synthesized in 1987. CL-20 not only has excellent oxygen balance, but also has better detonation velocity, detonation pressure and density than the current military main explosive Octojin (HMX), and its energy output is 10% to 15% higher than that of HMX, but its mechanical sensitivity is higher than that of HMX. , The unsatisfactory safety seriously restricts the development and application of CL-20. [0003] The deuterium atom carries one more neutron than the hydrogen atom, and the carbon-deuterium bond formed by deuterium and carbon has a lower vibration frequency than the carbon-hydrogen bond, so it is more stable; ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22C06B25/34C07B59/00
CPCC06B25/34C07B59/002C07B2200/05C07D487/22
Inventor 刘吉平方祝青
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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