Trinitramine triazolotriazole and its energetic ion salt and its preparation

A technology of triazolo and trinitroamine, which is applied in the directions of nitrated acyclic/alicyclic/heterocyclic amine explosive compositions, organic chemistry, etc., to achieve the effects of high yield, simple synthesis method and mild conditions

Active Publication Date: 2021-05-04
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This is the first synthetic route of this compound, which has not been reported before

Method used

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  • Trinitramine triazolotriazole and its energetic ion salt and its preparation
  • Trinitramine triazolotriazole and its energetic ion salt and its preparation
  • Trinitramine triazolotriazole and its energetic ion salt and its preparation

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Experimental program
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Effect test

Embodiment 1 3

[0045] The synthesis of embodiment 1 trinitramine three and three (1)

[0046] Add 1.54g of 3,6,7-triamino[1,2,4]triazolo[4,3-b][1,2,4]triazole (10mmol) to 18g of oleum, and wait until the ultrasonic After dissolution, then slowly add 5 mL of fuming nitric acid while keeping the temperature not exceeding -5°C. Reaction for 4h, keeping the temperature at -5°C. It was then quenched with 30 g of crushed ice and filtered to obtain a yellow solid, which was dissolved in CaCl 2 Dry in medium to obtain the product (yield 78%).

[0047] In the present invention, the 3,6,7-triamino[1,2,4]triazolo[4,3-b][1,2,4]triazole is self-made in the laboratory, and the specific preparation method See also T.M. P.C. Schmid, S. Schnell and J. Stierstorfer, Chem. Eur. J., 2015, 21, 9219-9228.

[0048] Product structure identification:

[0049] Decomposition temperature: 89°C (DSC, the following refers to the melting point and decomposition temperature are the initial temperature).

[0050] NMR ...

Embodiment 2 3

[0055] The synthesis of embodiment 2 trinitramine three and three (1)

[0056] Add 1.54g of 3,6,7-triamino[1,2,4]triazolo[4,3-b][1,2,4]triazole (10mmol) into 14g of concentrated sulfuric acid, and wait until it is completely dissolved by ultrasonic Then, keep the temperature not exceeding -5°C, and slowly add 4 mL of anhydrous nitric acid. Reaction for 4h, keeping the temperature at -5°C. It was then quenched with 30 g of crushed ice and filtered to obtain a yellow solid, which was dissolved in CaCl 2 Dry in medium to obtain the product (yield 83%).

Embodiment 3 3

[0057] The synthesis of the double ammonium salt (2) of embodiment 3 trinitramine three three

[0058] Disperse 578 mg of trinitramine trisanetris (2 mmol) in 30 mL of water, add 272 mg of concentrated ammonia water (25% by mass) to it, keep the temperature at 70° C., and stir for 4 h. After cooling, concentrate, filter, and recrystallize in hot water to obtain a yellow solid product (yield 85%).

[0059] Product structure identification, density detection, detonation performance calculation and sensitivity test:

[0060] Melting point: 122°C. The decomposition temperature is 172°C.

[0061] NMR 1 H NMR ([D 6 ]DMSO, 100MHz, 25°C, TMS): δ=7.14(s)ppm. 13 C NMR ([D 6 ]DMSO, 600MHz, 25°C): δ=159.22, 145.64, 141.85ppm.

[0062] Infrared spectrum (KBr): 3599,3544,3451,3206,1644,1571,1527,1477,1422,1278,1239,1138,1064,1002,952,842,802,764,742,716,582cm -1 .

[0063] Elemental analysis: Molecular formula C 3 h 9 N 13 o 6 , Theoretical C, 11.15; H, 2.81; N, 56.34. Found C...

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Abstract

The invention relates to the field of energetic material synthesis, specifically 3,6,7-trinitramine[1,2,4]triazolo[4,3-b][1,2,4]triazole and its energetic materials Ionic salt and preparation, the compound in the present invention will have better application prospect in high-energy explosives. 6 kinds of energetic ion salts of trinitramine trihexamethylene, the tested density is relatively high, ranging from 1.65‑1.89 g / cm 3 . The theoretical detonation velocity calculated by EXPLO5 (v6.01) software of the energetic ion salt in the present invention is between 8519-9518 m / s, and the detonation pressure is between 27.6-41.1 GPa. The synthesis method of this kind of salt is simple, the condition is mild, the yield is high, and deionized water is mostly used as the reaction solvent, and the environment is friendly.

Description

technical field [0001] The invention relates to the field of energetic material synthesis, specifically 3,6,7-trinitramine[1,2,4]triazolo[4,3-b][1,2,4]triazole and its energetic materials Ionic salt and preparation, the compound in the present invention will have better application prospect in high-energy explosives. Background technique [0002] Different from the energy of traditional CHNO explosives from the oxidation of the carbon skeleton, most of the energy of nitrogen-rich heterocyclic energetic ionic salts comes from their ring tension and high positive enthalpy of formation, because they contain a large number of energetic N–N and C–N single / double bond. And its main decomposition product is nitrogen, which has little environmental pollution. [0003] In addition to the above advantages, nitrogen-rich fused-ring energetic ion salts, more importantly, compared with their monocyclic or bicyclic analogues, fused-ring compounds have a higher density, which is benefici...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04C06B25/34
CPCC06B25/34C07D487/04
Inventor 卞成明冯文静雷群英吴晓青
Owner ZHONGBEI UNIV
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