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Method for synthesizing high-molecular weight polyphenylene sulfide by controlling water content

A high molecular weight, polyphenylene sulfide technology, applied in the field of polyphenylene sulfide synthesis, can solve the problems of uncontrollable reaction process, many impurities, and difficult separation of products, and achieves the effect of reducing dehydration time, reducing impurity content, and reducing investment.

Active Publication Date: 2019-10-01
四川中科兴业高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is: in order to solve the problem that the reaction process cannot be controlled during the polymerization process of the existing polyphenylene sulfide synthesis process, and there are many impurities in the reactor and the products are not easy to separate. Thioether method

Method used

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  • Method for synthesizing high-molecular weight polyphenylene sulfide by controlling water content
  • Method for synthesizing high-molecular weight polyphenylene sulfide by controlling water content

Examples

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Effect test

Embodiment 1

[0026] This example provides a method for controlling the water content to synthesize high molecular weight polyphenylene sulfide

[0027] In the 316L stainless steel autoclave of 5L, the molar ratio of each component participating in the reaction is:

[0028] Sodium sulfide: sodium hydroxide: p-dichlorobenzene: N-methylpyrrolidone: distilled water = 1:0.15:1.28:3.5:0.

[0029] The overall process of preparing polyphenylene sulfide is:

[0030] 1) Sodium sulfide dehydration: Add N-methylpyrrolidone into the reaction kettle, then put sodium sulfide and sodium hydroxide into the reaction kettle in turn, pass in nitrogen protection, start stirring, and keep the temperature of the system at 0.8~2℃ / Min heating rate from room temperature to 150 ~ 203 ℃, stop dehydration after 10 minutes at constant temperature;

[0031] 2) Dissolution of p-dichlorobenzene: put p-dichlorobenzene into a p-dichlorobenzene dissolution kettle, add N-methylpyrrolidone, pass through nitrogen protection,...

Embodiment 2

[0037] This example provides a method for synthesizing high molecular weight polyphenylene sulfide by controlling the water content.

[0038] In the 316L stainless steel autoclave of 5L, the molar ratio of each component participating in the reaction is:

[0039] Sodium sulfide: sodium hydroxide: p-chlorobenzene: N-methylpyrrolidone: distilled water = 1:0.15:1.28:3.5:2.

[0040] The operation in Example 1 was repeated, wherein in step 3) prepolymerization, p-dichlorobenzene was analyzed and detected by gas chromatography, and the conversion rate of p-dichlorobenzene was 75%.

Embodiment 3

[0042] This example provides a method for synthesizing high molecular weight polyphenylene sulfide by controlling the water content.

[0043] In the 316L stainless steel autoclave of 5L, the molar ratio of each component participating in the reaction is:

[0044]Sodium sulfide: sodium hydroxide: p-dichlorobenzene: N-methylpyrrolidone: distilled water=1:0.15:1.28:3.5:4.

[0045] The operation in Example 1 was repeated, wherein in step 3) prepolymerization, p-dichlorobenzene was analyzed and detected by gas chromatography, and the conversion rate of p-dichlorobenzene was 83.5%.

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Abstract

The invention discloses a method for synthesizing high-molecular weight polyphenylene sulfide by controlling water content, and relates to the technical field of synthesizing of polyphenylene sulfide,which solves the problem of failure in controlling of physical property of the obtained polyphenylene sulfide in the polymerizing process of the existing polyphenylene sulfide synthesizing technologyand the problems of higher content of impurities and difficulty in separation of products in the reaction kettle. The method comprises the following steps of using sodium sulfide, sodium hydroxide, paradichlorobenzene and water as the raw materials, and condensing to synthesize high-molecular weight polyphenylene sulfide resin in an N-methyl pyrrolidone solvent; sending the dissolved paradichlorobenzene solution into the reaction kettle in the pre-polymerizing process; feeding nitrogen gas for protecting, stirring, and maintaining the system temperature at 150 to 240 DEG C; when the temperature of the reaction kettle is constant, uniformly and slowly adding distilled water into the reaction kettle, closing a valve of a high-pressure dripping device after the adding of the distilled wateris finished, reacting for 1 to 6h, and re-polymerizing after the pre-polymerizing is finished. The method has the advantage that the different amounts of water are added in the pre-polymerizing and polymerizing stages, so as to controllably synthesize the polyphenylene sulfide products with different molecular weights.

Description

technical field [0001] The invention relates to the technical field of polyphenylene sulfide synthesis, in particular to a method for synthesizing high molecular weight polyphenylene sulfide by controlling water content. Background technique [0002] Polyphenylene sulfide is a special engineering resin industrialized by Phillips in the 1960s. It has the characteristics of high temperature resistance, radiation protection, self-flammability, high strength and high modulus, and is widely used in automobiles, environmental protection, military industry, and aerospace. and other fields. At present, most domestic and foreign manufacturers continue to use the polymerization process developed by Phillips to produce polyphenylene sulfide. During the synthesis process, catalytic promoters are usually used to increase the synthesis efficiency. The catalytic promoters used include lithium chloride , sodium carbonate and other inorganic salts, or sodium acetate, lithium acetate, sodium...

Claims

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Application Information

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IPC IPC(8): C08G75/0254C08G75/0209
CPCC08G75/0254C08G75/0209
Inventor 刘洪余雷范永志姜希猛陈俊陈云
Owner 四川中科兴业高新材料有限公司
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