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A kind of preparation method of polyphenylene sulfide ketone and product thereof

A technology of polyphenylene sulfide ketone and sodium sulfide, which is applied in the field of polymer engineering, can solve the problems of unreachable physical and mechanical performance indicators, difficult post-processing of products, or serious side reactions, etc., to achieve stable dehydration effect and improve uniformity. and the degree of polymerization of the product, the effect of reducing the production of oligomers

Active Publication Date: 2022-07-01
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at present, there is no mature polyphenylene sulfide ketone product available for industrial use. The main problems are that the degree of polymerization of the product is low, or the side reaction is serious, which leads to difficulties in the post-processing of the product, and the physical and mechanical properties of the product cannot reach the relevant The application requirements of the field affect its normal use

Method used

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  • A kind of preparation method of polyphenylene sulfide ketone and product thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 8Kg of technical-grade 5-hydrate crystalline sodium sulfide (according to the main content, take this as quantitative benchmark 1), and weigh technical-grade 4,4'-dichlorodicarbonate according to the molar ratio of active ingredients 1:0.96:0.60:7:0.06 Benzophenone, catalyst potassium carbonate, solvent N-methylpyrrolidone, caustic soda. One quarter of the total amount of solvent N-methylpyrrolidone is used in the dehydration process, and three quarters is used in the polymerization process.

[0033] Crystallized sodium sulfide was evaporated and dehydrated to 195°C, then filled with nitrogen and cooled to 155°C, the first-stage polymerization temperature was 155°C, the time was 120 minutes, and the stirring speed was 90rpm; the second-stage polymerization temperature was 275°C, the time was 120 minutes, and the stirring speed was 120rpm.

[0034] After the polymerization reaction, the reaction mass was cooled to 165° C., separated, washed and dried to obtain 8.25...

Embodiment 2

[0037] Weigh 8Kg of technical-grade 9-hydrate crystalline sodium sulfide (according to the main content, take this as quantitative benchmark 1), and weigh technical-grade 4,4'-dichlorodicarbonate according to the molar ratio of active ingredients 1:0.95:0.65:8:0.08 Benzophenone, catalyst potassium carbonate, solvent N-methylpyrrolidone, caustic soda. One quarter of the total amount of solvent N-methylpyrrolidone is used in the dehydration process, and three quarters is used in the polymerization process.

[0038] Crystallized sodium sulfide was evaporated and dehydrated to 195°C, then filled with nitrogen and cooled to 155°C, the first-stage polymerization temperature was 155°C, the time was 120 minutes, the stirring speed was 90rpm, the second-stage polymerization temperature was 275°C, the time was 120 minutes, and the stirring speed was 120rpm.

[0039] After the polymerization reaction was completed, the reaction mass was cooled to 165° C., separated, washed and dried to o...

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Abstract

The invention discloses a preparation method of polyphenylene sulfide ketone and a product thereof, comprising: adding crystalline sodium sulfide, solvent N-methyl pyrrolidone (NMP) and caustic soda into a dehydration reaction vessel, and dehydration at temperature under the protection of nitrogen , adjusted to a polymerization temperature after dehydration. 4,4'-dichlorobenzophenone (DCBP), catalyst potassium carbonate are added in the polymerization reactor, under nitrogen atmosphere, stir, be warmed up to the first section of reaction temperature and seal, then the dehydration product is slowly added to the reactor. In the polymerization reactor, a stage of polymerization is carried out. After the first-stage polymerization reaction is completed, the temperature is raised to the second-stage polymerization reaction temperature to prepare polyphenylene sulfide ketone. The polyphenylene sulfide ketone prepared by the invention has high molecular weight, easy separation of reaction by-products, good product comprehensive performance and high yield.

Description

technical field [0001] The invention belongs to the technical field of polymer engineering, and specifically relates to a preparation method of polyphenylene sulfide ketone and a product thereof. Background technique [0002] Polyphenylene sulfide ketone is a special organic polymer compound with high heat resistance, corrosion resistance and thermoplasticity. Its melting point can be as high as 350 ℃. It is a special engineering plastic required by many special industrial fields. [0003] Regarding the polymerization route and method of polyphenylene sulfide ketone, literature reports mainly include alkali metal vulcanization method, halogenated thiophenol self-polycondensation method, sulfur solution method and phosgene method. However, at present, there is no mature polyphenylene sulfide ketone product available for industrial use. The main problems are that the product has a low degree of polymerization or serious side reactions, which lead to difficulties in the post-pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/10C08G75/0254
CPCC08G75/10C08G75/0254
Inventor 杨永彬刘建容
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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