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Trinitramine triazol triazole, and energetic ionic salt and preparation thereof

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

Active Publication Date: 2019-10-29
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 triazol triazole, and energetic ionic salt and preparation thereof
  • Trinitramine triazol triazole, and energetic ionic salt and preparation thereof
  • Trinitramine triazol triazole, and energetic ionic salt and preparation thereof

Examples

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 synthesis field of energetic materials, in particular to 3,6,7-trinitramine[1,2,4]triazol[4,3-b][1,2,4]triazole, and an energetic ionic salt and preparation thereof. The compound has good application prospects in high energy explosives. 6 kinds of energetic ionic salts of the trinitramine triazol triazole have a high density after a test, and the density is between 1.65-1.89g / cm<3>. According to the energetic ionic salt, calculated by an EXPLO5 (v6.01) software, the theoretical detonation velocity is between 8519-9518m / s, and burst pressure is between 27.6-41.1 Gpa. A synthesis method of the energetic ionic salt is simple, a condition is mild, the yield is high, deionized water is mostly used as a reaction solvent, and 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 Applications(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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