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A kind of preparation method of polyethylene tetrazole

A polyvinyl tetrazole and polyacrylonitrile technology, which is applied in the field of preparation of polyvinyl tetrazole, can solve the problems of large investment scale, harsh conditions, complex synthesis process equipment, etc., and achieves the promotion of mass transfer and heat transfer, and mild reaction conditions. , the effect of simple process

Active Publication Date: 2018-06-12
中国船舶集团有限公司第七一八研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Described in U.S. Patent No. 7,776,169 is to take polyacrylonitrile and sodium azide as raw material, take zinc bromide as catalyst, the method for synthesizing polyethylene tetrazole by high pressure method in the aqueous solution containing surfactant, this method does not use organic solvent , to avoid the potential safety hazards and possible damage to the environment in the storage, use and recycling of organic solvents, but the synthesis process equipment is complex, the process requires high temperature and high pressure, harsh conditions, and a large investment scale

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add a mixed solution of 100mL DMF and 50mL distilled water into a three-necked flask, and then successively add 10.6g polyacrylonitrile, 21.4g ammonium chloride, 15.6g sodium azide, mix well, heat to 120℃, and react for 7h under stirring. There was no precipitation during the reaction; after cooling, the mixed solution was poured into a 1000 mL beaker, and then 500 mL of 0.5 mol / L hydrochloric acid aqueous solution was added to the beaker, and stirred until the white precipitate was completely precipitated; the precipitated precipitate It was washed 3 times with distilled water, and then placed in a drying oven at 120° C. to dry for 24 hours to obtain 19.68 g of polyvinyltetrazole.

[0014] Dissolve 0.243g of polyethylenetetrazole prepared in this implementation into 25mL DMF solution, then add thymol blue ethanol solution as an indicator, titrate with 0.5mol / L sodium hydroxide solution, until the solution turns from light yellow The titration is stopped in light blue, the...

Embodiment 2

[0016] Add a mixed solution of 100mL DMF and 25mL distilled water into a three-necked flask, and then successively add 10.6g polyacrylonitrile, 21.4g ammonium chloride, 15.6g sodium azide, mix well, heat to 150℃, and react for 7h under stirring. No precipitation precipitated during the reaction; after cooling the mixed solution, pour it into a 1000 mL beaker, and then add 400 mL of a 0.7mol / L hydrochloric acid aqueous solution to the beaker, and stir until the white precipitate is completely precipitated; the precipitated precipitate It was washed 3 times with distilled water, and then placed in a drying oven at 120° C. for drying for 24 hours to obtain 21.47 g of polyvinyltetrazole.

[0017] Dissolve 0.192g of polyethylenetetrazole prepared in this implementation into 25mL DMF solution, then add thymol blue ethanol solution as an indicator, titrate with 0.5mol / L sodium hydroxide solution, until the solution turns from light yellow The titration is stopped in light blue, the volu...

Embodiment 3

[0019] Add a mixed solution of 100mL DMF and 75mL distilled water into a three-necked flask, then successively add 10.6g polyacrylonitrile, 21.4g ammonium chloride, 15.6g sodium azide, mix well, heat to 105℃, and react for 7h under stirring. No precipitation precipitated during the reaction; after cooling, the mixed solution was poured into a 2000mL beaker, and then 800mL hydrochloric acid aqueous solution with a concentration of 0.3mol / L was added to the beaker and stirred until the white precipitate was completely precipitated; the precipitated precipitate It was washed 3 times with distilled water, and then placed in a drying oven at 120° C. to dry for 24 hours to obtain 21.11 g of polyvinyltetrazole.

[0020] Dissolve 0.214g of polyethylenetetrazole prepared in this implementation into 25mL DMF solution, add thymol blue ethanol solution as an indicator, and titrate with 0.5mol / L sodium hydroxide solution until the solution turns from light yellow The titration is stopped in l...

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PUM

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Abstract

The invention relates to a preparation method of polyethylene tetrazole and belongs to the technical field of polymer synthesis. The method comprises steps as follows: polyacrylonitrile, ammonium chloride and sodium azide are added to a mixed solution of water and DMF (dimethyl formamide) sequentially, and then, the mixture is heated to 100-150 DEG C and subjected to a reflux reaction for 4-7 hours under the stirring condition; a diluted hydrochloric acid solution is added to the reacted mixed solution and stirred until white precipitates are completely separated out, the precipitates separated out are washed with water and dried, and polyethylene tetrazole is obtained. According to the method, the phenomenon that a middle product has jelly precipitation in the preparation process is avoided, uniform stirring is facilitated, and mass transferring and heat transferring in the reaction process are promoted; the method adopts a simple process, the reaction conditions are mild, and the product yield is high.

Description

Technical field [0001] The invention relates to a preparation method of polyvinyltetrazole and belongs to the technical field of polymer synthesis. Background technique [0002] Polyethylenetetrazole is a high-energy binder with high nitrogen content, low sensitivity and good stability. It has a wide range of effects in the fields of gas generating agents, rocket propellants, pyrotechnics and so on. At present, the main preparation method of polyvinyltetrazole is the [3+2] cyclization reaction method of polyacrylonitrile and azide, which has the advantages of high ring-forming efficiency and high product yield. The article "Resultful synthesis of polyvinyltetrazole from polyacrylonitrile" published by Li Xingui and others in "reactive&functional polymers" describes the use of polyacrylonitrile, sodium azide and ammonium chloride as raw materials, and N,N-dimethylformamide (DMF) It is a method for solvent synthesis of polyvinyltetrazole, but this method is accompanied by the phen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F20/44C08F8/48
CPCC08F8/48C08F20/44
Inventor 李栋梁尹燕华马丽娥
Owner 中国船舶集团有限公司第七一八研究所
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