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A kind of efficient synthetic method of polyphenylene sulfide resin

A technology of polyphenylene sulfide resin and synthesis method, which is applied in the field of organic polymer resin production, can solve the problems of uneven particle size of the final product, unstable resin melt index, low yield of polyphenylene sulfide resin, etc., and achieve product Good particle uniformity, avoiding scarring, and maintaining the effect of particle distribution

Active Publication Date: 2021-02-19
YIBIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned method prepares polyphenylene sulfide resin yield is lower, and some reason wherein comprises: in synthetic process, resin usually can appear obvious agglomeration phenomenon, further occurs a large amount of scarring phenomena, not only can lose more excellent products that reaction obtains , and during this process, the agglomerated or scarred resin will adhere to the reaction equipment, and even form a "barrel-shaped" agglomeration in severe cases to completely wrap some key parts of the reaction equipment, making it difficult to detach; and after the reaction, the resin melt index (MFR value ) is unstable, the particle size of the final product is not uniform, the quality control is unstable, etc.

Method used

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  • A kind of efficient synthetic method of polyphenylene sulfide resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of efficient synthetic method of polyphenylene sulfide resin, it comprises steps:

[0034] (1) Dissolve the sulfur source in NMP, and carry out dehydration treatment under the protection of an inert gas in the presence of a catalyst and an alkali to complete the intermediate and the remaining mixed solution separated by dehydration, and then add p-DCB to the intermediate Carry out polymerization reaction with NMP, obtain polyphenylene sulfide resin mixture slurry;

[0035] (2) After the above-mentioned polymerization reaction, the temperature of the material in the reaction vessel is 250°C, the pressure in the kettle is 0.9Mpa, and the stirring speed is 100rpm, and then the coil of the reaction vessel is opened to cool the heat transfer oil to cool down the above-mentioned polyphenylene sulfide resin mixture slurry, When the temperature in the kettle drops to 245°C, use a pump to add the remaining mixed liquid at room temperature under the condition of a stirring...

Embodiment 2

[0038] A kind of efficient synthetic method of polyphenylene sulfide resin, it comprises steps:

[0039] (1) Dissolve the sulfur source in NMP, and carry out dehydration treatment under the protection of an inert gas in the presence of a catalyst and an alkali to complete the intermediate and the remaining mixed solution separated by dehydration, and then add p-DCB to the intermediate Carry out polymerization reaction with NMP, obtain polyphenylene sulfide resin mixture slurry;

[0040](2) After the above-mentioned polymerization reaction, the temperature of the material in the reaction vessel is 265°C, the pressure in the kettle is 1.1Mpa, and the stirring speed is 80rpm, and then the coil cooling water of the reaction vessel is opened to cool down the above-mentioned polyphenylene sulfide resin mixture slurry. When the temperature in the kettle drops to 260°C, use a pump to add the remaining mixed solution at room temperature under the condition of a stirring speed of 80rpm,...

Embodiment 3

[0043] A kind of efficient synthetic method of polyphenylene sulfide resin, it comprises steps:

[0044] (1) Dissolve the sulfur source in NMP, and carry out dehydration treatment under the protection of an inert gas in the presence of a catalyst and an alkali to complete the intermediate and the remaining mixed solution separated by dehydration, and then add p-DCB to the intermediate Carry out polymerization reaction with NMP, obtain polyphenylene sulfide resin mixture slurry;

[0045] (2) After the above-mentioned polymerization reaction, the temperature of the material in the reaction vessel is 260°C, the pressure in the kettle is 1.0Mpa, and the stirring speed is 80rpm, and then the coil cooling water of the reaction vessel is opened to cool down the above-mentioned polyphenylene sulfide resin mixture slurry. When the temperature in the kettle drops to 250°C, then use a pump to add the remaining mixed liquid at room temperature under the condition of a stirring speed of 40...

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Abstract

The invention provides an efficient synthesis method of polyphenylene sulfide resin. The efficient synthesis method includes the steps of: (1) dissolving a sulfur source in NMP, performing dehydrationtreatment through inert gas protection with the presence of a catalyst and an alkali to obtain an intermediate and a residual mixed solution obtained after dehydration, and adding p-DCB and NMP intothe intermediate for polymerization reaction to obtain polyphenylene sulfide resin mixture paste; (2) initially cooling the polyphenylene sulfide resin mixture paste, adding the residual mixed solution in a normal temperature state while stirring, controlling the cooling temperature, stopping adding the residual mixed solution when the internal temperature and / or pressure of a kettle is lowered toa certain value, and completing stirring; (3) after secondary cooling, discharging the stirred mixture paste to complete synthesis. The efficient synthesis method has the advantages that the stability of the melt index (MFR value) of the PPS resin can be improved, and the synthesis yield of the product can be increased; during reaction, the resin is easily separated from equipment, and energy conservation and high efficiency are achieved.

Description

technical field [0001] The invention relates to the technical field of organic polymer resin production, in particular to a high-efficiency synthesis method of polyphenylene sulfide resin. [0002] technical background [0003] Polyphenylene sulfide (PolyPhenylene Sulfide, hereinafter referred to as PPS) is a high-performance thermoplastic resin, which not only has the advantages of chemical corrosion resistance, high temperature resistance, good flame retardancy, and non-toxicity, but also has good physical and mechanical properties and Dimensional stability, it has a very wide range of applications in the production of mechanical and electronic components, fibers, films, etc. [0004] At present, the mainstream industrial production method of PPS resin is the sodium sulfide method, and its general synthesis process is: dissolving the sulfur source (sodium sulfide trihydrate, sodium sulfide pentahydrate, sodium sulfide nonahydrate, sodium hydrosulfide, etc.) in NMP (nitrogen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/0209C08G75/0254C08G75/0259C08G75/0277
CPCC08G75/0209C08G75/0254C08G75/0259C08G75/0277
Inventor 唐国强陈仕全钟富生帅永康李林舒砚勤
Owner YIBIN UNIV
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