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Preparation method of melt-cast explosive 2, 3, 4-trifluoro-1, 5 dinitrobenzene

A technology of trifluoronitrobenzene and dinitrobenzene, which is applied in the field of compound preparation, can solve the problems of ammunition sensitivity, fragility and transportation impact, hazards to workers’ health and the environment, oil leakage of explosives, etc., and achieve superior performance, The effect of safe raw materials and simple equipment

Inactive Publication Date: 2019-03-08
XINYANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, not only the waste discharged during the production process of TNT is harmful to the health of workers and the environment, but also the phenomenon of oil leakage, shrinkage, cavity, brittleness and expansion in TNT explosives will affect the sensitivity, vulnerability and transportation of ammunition

Method used

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  • Preparation method of melt-cast explosive 2, 3, 4-trifluoro-1, 5 dinitrobenzene
  • Preparation method of melt-cast explosive 2, 3, 4-trifluoro-1, 5 dinitrobenzene

Examples

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Effect test

Embodiment 1

[0019] A preparation method for melting and casting explosive 2,3,4-trifluoro-1,5-dinitrobenzene (ZXC-16), comprising the following steps:

[0020] Under ice-water bath, weigh potassium nitrate 5.55g (55mmol, 1.1eq) and slowly add in the cold 50ml concentrated sulfuric acid (concentration of sulfuric acid is 95%), continue to stir until potassium nitrate dissolves completely after adding, then, slowly Add 8.85g (50mmol, 1.0eq) of 2,3,4-trifluoronitrobenzene. After the addition, continue stirring at room temperature until the reaction is complete (TLC detection).

[0021] After the reaction was complete, the reaction mixture was slowly poured into ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain a light yellow solid with a yield of 89.01%.

[0022] Its H NMR spectrum is 1 H NMR (600MHz, CDCl 3 -d 1 )δppm: 8.79m, 1H); 13 C NMR (125MHz, CDCl3-d1); δppm: 150.68-148.91(d), 143.10-141.33(d), 133.24, 118.07; 19 F NMR (...

Embodiment 2

[0024] A preparation method for melting and casting explosive 2,3,4-trifluoro-1,5-dinitrobenzene (ZXC-16), comprising the following steps:

[0025] Under ice-water bath, weigh ammonium nitrate 4.4g (55mmol, 1.1eq) and add slowly in cold 50ml concentrated sulfuric acid (concentration of sulfuric acid is 95%), after adding, continue to stir until potassium nitrate dissolves completely, then, slowly Add 8.85g (50mmol, 1.0eq) of 2,3,4-trifluoronitrobenzene. After the addition, continue stirring at room temperature until the reaction is complete (TLC detection).

[0026] After the reaction was complete, the reaction mixture was slowly poured into ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain a light yellow solid with a yield of 86.67%.

Embodiment 3

[0028] A preparation method for melting and casting explosive 2,3,4-trifluoro-1,5-dinitrobenzene (ZXC-16), comprising the following steps:

[0029] Under ice-water bath, weigh potassium nitrate 5.55g (55mmol, 1.1eq) and slowly add in cold 50ml concentrated sulfuric acid (concentration of sulfuric acid is 98%), after adding, continue to stir until potassium nitrate dissolves completely, then, slowly Add 8.85g (50mmol, 1.0eq) of 2,3,4-trifluoronitrobenzene. After the addition, continue stirring at room temperature until the reaction is complete (TLC detection).

[0030] After the reaction was complete, the reaction mixture was slowly poured into ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain a light yellow solid with a yield of 87.34%.

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Abstract

The invention belongs to the technical field of compound preparation, and discloses a preparation method of melt-cast explosive 2, 3, 4-trifluoro-1, 5 dinitrobenzene. The preparation method includes the steps: adding nitrate or nitric acid into 95-98% concentrated sulfuric acid in a low-temperature stirred manner; adding 2, 3, 4-trifluoronitrobenzene, and continuing to stirring mixture to completely react; pouring reacted mixture into ice water, separating out precipitates, and filtering, washing and drying the precipitates to obtain the 2, 3, 4-trifluoro-1, 5 dinitrobenzene. Comprised with TNT, the prepared 2, 3, 4-trifluoro-1, 5 dinitrobenzene has better detonation performance and higher density, materials used by the method are safe, devices needed by the method are simple, the methodis simple and easy, yield and purity are high, and the dinitrobenzene is easily purified and re-crystallized.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of fused-cast explosive 2,3,4-trifluoro-1,5-dinitrobenzene. Background technique [0002] Fusion-cast explosives refer to mixed explosives that can be cast in a molten state, and are currently the most widely used type of military mixed explosives, accounting for more than 90% of military mixed explosives. They can adapt to the charges of various shapes of chambers, and have good comprehensive performance. They are mostly used in mortars, grenades, shells, missile warheads and mine charges, and occupy an important position in military mixed explosives. Its carrier can be synthesized by nitrating nitrating agents such as nitric acid, fuming nitric acid and nitric acid-acetic anhydride. An ideal melt-cast explosive should have the following properties: (1) melting point of 70-120°C; (2) low vapor pressure (lower poisonous gas inhalatio...

Claims

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Application Information

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IPC IPC(8): C07C201/14C07C205/12
CPCC07C201/14C07C205/12
Inventor 姚磊张正张行程胡文祥
Owner XINYANG NORMAL UNIVERSITY
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