Synthetic method of high-molecular-weight linear polyphenylene sulfide

A polyphenylene sulfide and synthesis method technology, applied in the field of synthesis of high molecular weight linear polyphenylene sulfide, can solve the problems of low yield, high toxicity of liquid bromine raw materials, cumbersome process routes, etc., and achieve high molecular weight and high purity , The effect of simplifying the synthesis process

Inactive Publication Date: 2019-04-12
TAIYUAN UNIV OF TECH
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  • Abstract
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  • Claims
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Problems solved by technology

[0011] The present invention aims at the disadvantages of the prior art, such as cumbersome process route for synthesizing polyphenylene sulfide with anisole as a raw material, low yield, high toxicity of liquid bromine raw material, etc., and provides a high-purity, high-molecular-weight linear polyphenylene sulfide synthesis method , the reaction system conditions are mild, the operation of the whole process is relatively stable, and it has industrial application prospects

Method used

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  • Synthetic method of high-molecular-weight linear polyphenylene sulfide
  • Synthetic method of high-molecular-weight linear polyphenylene sulfide
  • Synthetic method of high-molecular-weight linear polyphenylene sulfide

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Embodiment 1

[0032] Put 5.71g (0.046mol) of sulfide anisole, 4.36g (0.02mol) of diphenyl disulfide, and 10.81g (0.04mol) of potassium persulfate into the reaction bottle, and slowly add 6ml of it dropwise with a constant pressure dropping funnel Trifluoroacetic acid, continue to react at room temperature for 412 hours after the dropwise addition, the raw material diphenyl disulfide is consumed, add 300ml water to the system and stir for 30 minutes, extract three times with 50ml ethyl acetate, combine the organic phases, backwash with water, The organic phase was separated and dried with anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain a light yellow liquid. After column chromatography, 7.4 g of 4-(thiophenyl)sulfide anisole was obtained as a colorless transparent liquid with a yield of 81%. .

[0033] Put 4.64g (0.02mol) of 4-(thiophenyl)sulfide anisole and 20ml of acetonitrile into the reaction bottle, slowly add 16ml of hydrogen peroxide (30%) dropwis...

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Abstract

The invention discloses a synthetic method of high-molecular-weight linear polyphenylene sulfide. The synthesis method comprises the following steps: synthesizing 4-(thiophenyl)thioanisole by taking polyphenylene sulfide and diphenyl disulfide as raw materials, further synthesizing 4-(sulfophenyl)methyl phenyl sulfoxide through oxidation by using hydrogen peroxide, then carrying out a cationic polymerization reaction on the 4-(sulfophenyl)methyl phenyl sulfoxide under the action of trifluoromethanesulfonic acid to synthesize a polymethyl[4-(thiophenyl)-phenyl]sulfonium trifluoromethanesulfonate; and finally, removing methyl by a nucleophilic reagent pyridine to obtain the polyphenylene sulfide. The polyphenylene sulfide synthesized by the method is high in purity and high in molecular weight and is in linear, the reaction system is mild in condition, operation of the whole process is relatively stable, and the method has an industrial application prospect.

Description

technical field [0001] The invention relates to a method for synthesizing high-molecular weight linear polyphenylene sulfide, in particular to a method for synthesizing polyphenylene sulfide in four steps using anisole and diphenyl disulfide as raw materials. Background technique [0002] Polyphenylene sulfide is the largest special engineering plastic and one of the eight major aerospace materials. Because of its high temperature resistance, radiation resistance, corrosion resistance, wear resistance, flame retardancy, high modulus, high dimensional stability, excellent electrical properties, and good molding and processing properties, it is widely used in environmental protection, automobiles, electronics, petrochemicals, pharmaceuticals, etc. industry. Its structural formula is as follows: [0003] [0004] There are many synthetic methods for the synthesis of polyphenylene sulfide. [0005] The industrial production of PPS mainly adopts the sodium sulfide method. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0213C08G75/025C08G75/0281
CPCC08G75/0218C08G75/0272C08G75/0281
Inventor 卢建军刘烨葛超刘妙青王慧娟
Owner TAIYUAN UNIV OF TECH
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