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5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole and synthetic method

A trinitromethyl, synthesis method technology, applied in the field of synthesis and preparation of energetic materials, can solve the problems of low energy and complicated nitration steps, and achieve the effect of simple nitration steps, easy separation, and mild reaction conditions

Active Publication Date: 2017-05-10
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Above-mentioned route directly adopts triazole diacetate ethyl ester to carry out nitration, can only obtain the gem-dinitro triazole with low energy, simultaneously their nitration steps are comparatively complicated: first add the concentrated sulfuric acid, then the concentrated nitric acid and 60% Add fuming sulfuric acid to the reaction system in turn

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  • 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole and synthetic method
  • 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole and synthetic method
  • 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole and synthetic method

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1, Preparation of 5,5'-bis(trinitromethyl)-3,3'-H,H'-linked-1,2,4-triazole

[0033] At room temperature, add 17.9g (58mmol) of ethyl bi-1,2,4-triazole-5,5'-diacetate to 90mL of 5mol / L sodium hydroxide solution, react at room temperature for 1h, then cool down to 0°C, slowly add 37% mass fraction of concentrated hydrochloric acid to the solution, adjust the pH value to 3-4, filter out the precipitate, and wash with a small amount of cold water to obtain bi-1,2,4-triazole-5 ,5'-Diacetic acid hydrate 12.6g, yield 75.4%. -10°C, slowly add 2g (7mmol) bi-1,2,4-triazole-5,5'-diacetic acid hydrate into 20mL 96% mass fraction of fuming nitric acid, stir at this temperature until dissolved, then Slowly add 30mL of 98% concentrated sulfuric acid dropwise below 0°C, return to 25°C and react for 18h after dropping, pour into 200g of crushed ice to quench, filter out the solid, wash with water, and vacuum dry to obtain 0.84g of white solid , yield 27.9%.

[0034] Dissolve ...

Embodiment 2

[0036] Example 2, Preparation of 5,5'-bis(trinitromethyl)-3,3'-H,H'-linked-1,2,4-triazole

[0037] The preparation method of bi-1,2,4-triazole-5,5'-diacetic acid hydrate is the same as that in Example 1. -10°C, slowly add 2g (7mmol) bi-1,2,4-triazole-5,5'-diacetic acid hydrate into 15mL 96% mass fraction of fuming nitric acid, stir at this temperature until dissolved, then Slowly add 30mL of 98% concentrated sulfuric acid dropwise below 0°C, return to 25°C and react for 12h after dropping, pour into 200g of crushed ice to quench, filter out the solid, wash with water, and vacuum dry to obtain 0.89g of white solid, The yield is 29.6%.

Embodiment 3

[0038] Example 3, Preparation of 5,5'-bis(trinitromethyl)-3,3'-H,H'-linked-1,2,4-triazole

[0039] The preparation method of bi-1,2,4-triazole-5,5'-diacetic acid hydrate is the same as that in Example 1. -10°C, slowly add 3g (10mmol) of bi-1,2,4-triazole-5,5'-diacetic acid hydrate into 23mL of 96% mass fraction fuming nitric acid, stir at this temperature until dissolved, then Slowly add 50mL of 98% concentrated sulfuric acid dropwise below 0°C, return to 25°C and react for 16h after dropping, pour into 300g of crushed ice to quench, filter out the solid, wash with water, and vacuum dry to obtain 1.66g of white solid, The yield is 36.6%.

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Abstract

The invention discloses 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole, an energetic ionic salt and a synthetic method thereof. The synthetic method comprises the following steps: adding di-1,2,4-triazole-5,5'-ethyl diacetate into an alkaline solution for reaction, and then performing acidification to obtain a di-1,2,4-triazole-5,5'-diacetate hydrate; and then adding the di-1,2,4-triazole-5,5'-diacetate hydrate into a certain proportion of fuming nitric acid / concentrated sulfuric acid to perform nitration, performing quenching in ice water, and performing filtration to obtain 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole. The synthetic method further comprises a reaction step for salt formation. The invention determines and discloses the 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole and an energetic ionic salt thereof for the first time. Moreover, the nitration step of the 5,5'-di(trinitromethyl)-3,3'-H,H'-di-1,2,4-triazole provided by the invention is relatively simple, the reaction conditions of the ionic salt are mild, and products are easy to separate.

Description

technical field [0001] The invention relates to an azole material and a preparation method thereof, in particular to 5,5'-bis(trinitromethyl)-3,3'-H,H'-bi-1,2,4-triazole, The energy-containing ion salt and its synthesis method belong to the technical field of synthesis and preparation of energy-containing materials. Background technique [0002] Azole high-energy explosives have attracted extensive attention in the field of energetic materials in recent years due to their high nitrogen content and thermal stability. Among them, bi-1,2,4-triazole molecules are coplanar and intramolecularly conjugated, and have good physical and chemical stability, and are often used as the basic skeleton in the synthesis of energetic compounds. In terms of structural modification in the synthesis of explosives, from C-nitro / amino, N-nitro / amino, N-nitroamine to gem-dinitro, the derivation of detonating groups is also constantly broadening our knowledge. The introduction of higher-energy ene...

Claims

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Application Information

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IPC IPC(8): C07D249/08C06B25/34
CPCC06B25/34C07D249/08
Inventor 马卿卢欢唱廖龙渝范桂娟顾昊
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS