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Synthetic method of deuterated hexogen

A synthetic method, RDX technology, applied in organic chemistry methods, organic chemistry, etc., can solve problems such as difficult structural analysis and low signal-to-noise ratio, and achieve high deuterium substitution rate, high yield, and high product purity.

Inactive Publication Date: 2018-06-01
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the sp on the methylene in the molecular structure of RDX 3 The influence of hydrogen atoms on the C-H bond, the non-correlated scattering of hydrogen to neutrons is very strong, resulting in a very low signal-to-noise ratio in the neutron scattering characterization results, making it difficult to achieve accurate structural analysis

Method used

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  • Synthetic method of deuterated hexogen
  • Synthetic method of deuterated hexogen
  • Synthetic method of deuterated hexogen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Under nitrogen protection, 20 mL of deionized water and 11.58 g of paraformaldehyde were added to a 100 mL two-neck round-bottom flask, and 60 mL of commercially available concentrated ammonia water was slowly added dropwise using a dropping funnel at room temperature. The addition time was 45 minutes, stirring rapidly while adding. After the addition, the reaction system was stirred and reacted at room temperature for 24 hours. After the reaction is completed, filter, wash the solid with the mother liquor and deionized water at 0°C, and dry in vacuum to obtain a white solid powder, which is perdeuterated urotropine.

[0035] 2) Add 5 mL of fuming nitric acid into a 50 mL dry and clean single-necked bottle, place it in an ice-water bath and stir for 20 minutes. Weigh 1.0 g of perdeuterated urotropine, and slowly add it to the reaction system in batches and several times under ice-water bath conditions. After the addition is completed in 30 minutes, the solution turn...

Embodiment 2

[0038] 1) Under the condition of nitrogen protection, add deionized water and commercially available deuterated formaldehyde solution into a two-necked round bottom flask, slowly add commercially available concentrated ammonia water dropwise at room temperature, and stir rapidly while adding. After the addition, the reaction system was stirred and reacted at room temperature for 24 hours. After the reaction is completed, filter, wash the solid with the mother liquor and deionized water at 0°C, and dry in vacuum to obtain a white solid powder, which is perdeuterated urotropine.

[0039]2) Add 5 mL of fuming nitric acid into a single-necked bottle, place it in an ice-water bath and stir for 20 minutes. Weigh 1.0 g of perdeuterated urotropine, and slowly add it to the reaction system in batches and several times under ice-water bath conditions. After the addition is completed in 30 minutes, the solution turns from light yellow to colorless and transparent. The ice-water bath con...

Embodiment 3-5

[0042] 1) Under the condition of nitrogen protection, add lysate (respectively: tetrahydrofuran, N, N-dimethylformamide, dimethyl sulfoxide) and commercially available deuterated For paraformaldehyde, slowly add commercially available concentrated ammonia water dropwise at room temperature, and stir rapidly while adding. After the addition, the reaction system was stirred and reacted at room temperature for 24 hours. After the reaction is completed, filter, wash the solid with the mother liquor and deionized water at 0°C, and dry in vacuum to obtain a white solid powder, which is perdeuterated urotropine.

[0043] 2) Add 5 mL of nitric acid (dilute nitric acid, concentrated nitric acid, and fuming nitric acid in Examples 3-5, respectively) into a single-necked bottle, place in an ice-water bath and stir for 20 minutes. Weigh 1.0 g of perdeuterated urotropine, and slowly add it to the reaction system in batches and several times under ice-water bath conditions. After the addit...

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Abstract

The invention relates to a synthetic method of deuterated hexogen, specifically to deuteration technology of hydrogen atoms which are located on non-active carbon-hydrogen bonds inside energetic material molecules. The synthetic method is characterized by reacting a deuterated formaldehyde substance with an ammonia substance to obtain deuterated urotropine which is an intermediate; and further performing nitrification to obtain deuterated hexogen which is the final product. The method is simple and efficient in steps, safe to operate, and is simple in purification. The prepared deuterated hexogen product is high in purity, high in deuteration rate, and suitable for fields of neutron scattering research, energetic material research and nuclear magnetism research.

Description

technical field [0001] The invention relates to a synthesis method of deuterated RDX, in particular to the deuterated technology of hydrogen atoms on inactive carbon-hydrogen bonds inside energetic material molecules. The deuterated RDX prepared by the invention has simple and efficient synthesis steps, safe operation and simple purification; the product has high purity and high deuteration rate, and is suitable for neutron scattering research, energetic material research, nuclear magnetic research and other fields. Background technique [0002] The molecule of RDX (Royal Demolition Explosive) is named 1,3,5-trinitrohexahydro-1,3,5-triazine, which is a high energy density element formed by substituting trinitrohexahydro-1,3,5-triazine explosives. RDX has a variety of crystal structures, and its performance and efficacy show obvious differences with different crystal structures. Under normal temperature and pressure conditions, α-type RDX (α-RDX) presents a white powder, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/06
CPCC07B2200/05C07D251/06
Inventor 邹林白亮飞李昊夏元华闫冠云孙光爱钱宇龚建李新喜杨海君胡文浩张春
Owner INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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