Supercharge Your Innovation With Domain-Expert AI Agents!

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: 2016-11-09
中国船舶集团有限公司第七一八研究所
View PDF8 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0014] 0.243g of the prepared polyethylene tetrazole is dissolved in 25mL of DMF solution, then add the ethanol solution of thymol blue as indicator, and titrate with the sodium hydroxide solution of 0.5mol / L until the solution turns from light yellow to Stop titration for light blue, the v...

Embodiment 2

[0016] Add the mixed solution of 100mL DMF and 25mL distilled water into the three-necked flask, then successively add 10.6g polyacrylonitrile, 21.4g ammonium chloride, 15.6g sodium azide, mix well, heat to 150°C, and react for 7h under stirring. There is no precipitation during the reaction process; the mixed solution after the reaction is cooled and then poured into a 1000mL beaker, and then 400mL of aqueous hydrochloric acid solution with a concentration of 0.7mol / L is added to the beaker, and stirred until the white precipitate is completely precipitated; Wash with distilled water for 3 times, and then dry in a drying oven at 120°C for 24 hours to obtain 21.47 g of polyethylene tetrazole.

[0017] 0.192g of the polyethylene tetrazole prepared by this implementation is dissolved in 25mL DMF solution, then the ethanol solution of thymol blue is added as indicator, and titrated with 0.5mol / L sodium hydroxide solution until the solution turns from light yellow to Stop titratio...

Embodiment 3

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

[0020] 0.214g of polyethylene tetrazole prepared by this implementation is dissolved in 25mL of DMF solution, and the ethanol solution of thymol blue is added as indicator, and titrated with 0.5mol / L sodium hydroxide solution until the solution turns from light yellow to Stop titration for li...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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 polyethylene tetrazole, which belongs to the technical field of polymer synthesis. Background technique [0002] Polyethylene tetrazole is a high-energy binder with high nitrogen content, low sensitivity, and good stability. It has a wide range of applications in the fields of gas generating agents, rocket propellants, and pyrotechnics. At present, the main preparation method of polyethylene tetrazole is the [3+2] ring-closing 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 et al. on "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 synthesizing polyethylene tetrazole with a solvent, but this method i...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com