A kind of preparation method of high-energy low-explosion temperature nitrocellulose

A nitrocellulose and explosion temperature technology, applied in organic chemistry and other directions, can solve the problems of large shooting smoke, endanger the safety of the environmental shooter, and low temperature, and achieve the effect of less smoke and flame, improving the probability of self-survival, and high safety.

Active Publication Date: 2019-06-25
CHANGSHU INSTITUTE OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The high-energy gunpowder ingredients urgently needed by contemporary weapons are mainly nitrocellulose (NC), nitroglycerin (NG), RDX, etc. These substances have high carbon content, and the combustion products have high explosion temperature, large average molar mass, There are many harmful gas components; when applied, there are defects such as short life of the weapon launching barrel due to severe ablation, large shooting smoke, endangering the environment and the safety of the shooter.
Tetrazole derivatives (TZD) have the advantages of high nitrogen content, small average molar mass of combustion products, low temperature and no pollution. As a high-energy propellant component, it is expected to significantly improve its existing defects; Gold and other components have poor compatibility and have not been applied and developed

Method used

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  • A kind of preparation method of high-energy low-explosion temperature nitrocellulose
  • A kind of preparation method of high-energy low-explosion temperature nitrocellulose
  • A kind of preparation method of high-energy low-explosion temperature nitrocellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1), the synthesis of dipotassium azobistetrazolium

[0034] A certain amount of KOH is made into a solution of 0.15-0.18mol / L, and then according to the ratio of the amount of substances, pentaaminotetrazole is added in a ratio of KOH: pentaaminotetrazole=(2.3-2.6):1, and then at 70 Stir at ℃~80℃ for 20~30min, then slowly add KMnO with a ratio of 0.7~0.85 to pentaaminotetrazole 4 , react for 4-5 hours, then add ethanol equal to the volume of KOH solution, boil for 2-3 minutes, filter while hot to obtain the filtrate, freeze and filter to obtain a yellow needle-like solid, dry to obtain dipotassium azobistetrazolium.

[0035] 2), the synthesis of ethyl azobistetrazolium diacetate

[0036] Dissolve the obtained dipotassium azobistetrazolium completely in methanol, and then add BrCH with a molar ratio of 3 to 3.2 to the dipotassium azobistetrazolium substance 2 COOC 2 h 5 , reacted for 12 hours, and then heated to reflux around 90-110°C. Take out and spin dry to obtai...

Embodiment 2

[0042] 1), the synthesis of N, N-two tetrazole potassium amines

[0043]Dissolve sodium dicyanamide and sodium azide in ethanol solution at a ratio of 1:1 according to the following formula, adjust the pH to 6-7 with HCI solution, react at 60°C for 12 hours, spin dry, wash with water, and dry by spin Get N, N-two tetrazolium amine.

[0044]

[0045] Then dissolve the prepared N,N-bistetrazole amine in ethanol, slowly add KMnO4 with a substance ratio of 1.8-2 to N,N-bistetrazole amine at 60°C, and react for 3-4 hours, Raise the temperature to 80°C and keep for 3-5 minutes, filter while hot to obtain the filtrate, freeze and filter to obtain a solid, and dry to obtain N,N-bistetrazole potassium amine.

[0046] 2), the synthesis of N, N two tetrazole ethyl diacetate

[0047] Dissolve the obtained N,N di-tetrazole potassium amine completely in methanol, and then add BrCH with a ratio of 3 to 3.2 to N,N di-tetrazole methyl amine 2 COOC 2 h 5 , reacted for 12 hours, and then...

Embodiment 3

[0053] 1) Synthesis of 5,1'-tetrazole-1-acetic acid:

[0054]

[0055] Aminotetrazoleacetic acid and sodium azide were reacted in a 1:1 mixed solution of triethyl orthoformate and acetic acid at 80°C for 12 hours according to the ratio of substances of 1:1, spin-dried, washed with water, and dried by filtration to obtain 5 , 1'-Bitrazol-1-acetic acid.

[0056] 2) Preparation of nitrocellulose grafted with 5,1'-tetrazole-1-acetic acid

[0057] Add the 5,1'-bitetrazol-1-acetic acid prepared in the previous step to the microcrystalline cellulose substance at a ratio of 1 / 4 to 1 / 3 to the N,N-dimethylacetamide dissolved The microcrystalline cellulose solution is added with anhydrous LiCl in an amount of 0.9 to 1 in a molar ratio to the microcrystalline cellulose substance, and after stirring at 60 to 70°C for 24 hours, then added in a molar ratio to the microcrystalline cellulose substance of 2 to 2.2 HNO3, after reacting for 6-7 hours, drop KOH until the solution is neutral, ...

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Abstract

The invention discloses a high-energy low-explosion-temperature nitrocellulose preparation method, which comprises the steps of adding azo bistetrazole diacetic acid or N,N-bistetrazole diacetic acid or 5,1'-bisterazole-1-acetic acid into a microcrystalline cellulose solution dissolved by N,N-dimethylacetamide; adding a catalyst of anhydrous LiCl and stirring for a certain time at 60 DEG C to 70 DEG C; adding a certain amount of nitric acid and reacting for a certain time; adjusting the solution to neutral and spin drying to obtain solid; washing with water and drying to obtain azo bistetrazole diacetic acid grafted nitrocellulose or N,N-bistetrazole diacetic acid grafted nitrocellulose or 5,1'-bisterazole-1-acetic acid grafted nitrocellulose. According to the high-energy low-explosion-temperature nitrocellulose preparation method disclosed by the invention, nitrocellulose can keep explosive energy, meanwhile explosion temperature of explosive, fuel gas average molar mass and explosive sensitivity are obviously reduced, service life of weapon is prolonged, and density of explosive is improved.

Description

technical field [0001] The invention relates to a preparation method of nitrocellulose, in particular to a preparation method of high energy and low explosion temperature nitrocellulose. Background technique [0002] The high-energy gunpowder ingredients urgently needed by contemporary weapons are mainly nitrocellulose (NC), nitroglycerin (NG), RDX, etc. These substances have high carbon content, and the combustion products have high explosion temperature, large average molar mass, There are many harmful gas components; when used, there are defects such as short life of the weapon launching barrel due to serious ablation, large shooting smoke, endangering the environment and the safety of the shooter. Tetrazole derivatives (TZD) have the advantages of high nitrogen content, small average molar mass of combustion products, low temperature and no pollution. As a high-energy propellant component, it is expected to significantly improve its existing defects; Gold and other comp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B5/02C07D257/06C07D257/04
CPCC07D257/04C07D257/06C08B5/02
Inventor 杨春海杨高文
Owner CHANGSHU INSTITUTE OF TECHNOLOGY
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