Polyphenylene sulfide resin synthesis process

A technology for polyphenylene sulfide resin and synthesis process is applied in the field of synthesis technology of polyphenylene sulfide resin, which can solve the problem of irregular polyphenylene sulfide resin particles, fine polyphenylene sulfide resin particles, and polyphenylene sulfide resin molding. Difficulties and other problems, to achieve the effect of omitting the treatment process, improving the particle forming rate, and reducing soluble by-products

Active Publication Date: 2019-03-29
德阳科吉高新材料有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In Chinese patent application 201610033529.2, a co-solvent using sodium acetate as a synthetic polyphenylene sulfide resin is introduced. After the polyphenylene sulfide resin is synthesized, it is affected by the shape of the sodium acetate crystal, making the polyphenylene sulfide resin relatively difficult to form. more difficult
[0006] In Chinese patent application 201410087155.3, an industrial synthesis process of polyphenylene sulfide resin without adding any additives is introduced, in which sodium hydrosulfide, sodium hydroxide and p-dichlorobenzene are used as raw materials, and N-methyl- 2-Pyrrolidone is used as a solvent, and polyphenylene sulfide resin is synthesized by polycondensation without adding any synthetic additives. Due to the influence of the amount of solvent in the polymerization reaction system, the synthesized polyphenylene sulfide resin particles are very irregular, and at the same time The presence of polyphenylene sulfide resin particles is very small, which is not conducive to later purification and washing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The synthesis process of polyphenylene sulfide resin:

[0031] (1) Under the condition of nitrogen protection, add sodium hydrogen sulfide and oxygen-free deionized water into one reaction kettle to form an aqueous solution containing 45%wt of sodium hydrogen sulfide, and in another reaction kettle, under the condition of nitrogen protection Next, add sodium hydroxide and oxygen-free deionized water to form an aqueous solution containing 45%wt of sodium hydroxide, then heat the materials in the two reactors to 80°C, and use an alkali-resistant pump to input the aqueous sodium hydroxide solution into the container. In a reaction kettle with sodium hydrosulfide dissolved in water, when the material temperature reaches 120°C, under this temperature condition, after 30 minutes of heat preservation to generate sodium sulfide, N-methylpyrrolidone is added to make Na 2 The molar ratio of S:NMP is 1.0:3.8, the temperature of the material in the reactor is raised to 200°C at a t...

Embodiment 2

[0039] The synthesis process of polyphenylene sulfide resin:

[0040] (1) Under the condition of nitrogen protection, add sodium hydrogen sulfide and oxygen-free deionized water into one reaction kettle to form an aqueous solution containing 60%wt of sodium hydrogen sulfide, and in another reaction kettle, under the condition of nitrogen protection Next, add sodium hydroxide and oxygen-free deionized water to form an aqueous solution containing 60%wt of sodium hydroxide, then heat the materials in the two reactors to 100°C, and use an alkali-resistant pump to input the aqueous solution of sodium hydroxide into the container. In a reaction kettle with sodium hydrosulfide dissolved in water, when the temperature of the material reaches 130°C, under this temperature condition, after 18 minutes of heat preservation to generate sodium sulfide, N-methylpyrrolidone is added to make Na 2 The molar ratio of S:NMP is 1.0:5.8, the temperature of the material in the reactor is raised to 2...

Embodiment 3

[0048] The synthesis process of polyphenylene sulfide resin:

[0049] (1) Under the condition of nitrogen protection, add sodium hydrogen sulfide and oxygen-free deionized water into one reaction kettle to form an aqueous solution containing 48%wt of sodium hydrogen sulfide, and in another reaction kettle, under the condition of nitrogen protection Next, add sodium hydroxide and oxygen-free deionized water to form an aqueous solution containing 52%wt of sodium hydroxide, then heat the materials in the two reactors to 83°C, and use an alkali-resistant pump to input the aqueous sodium hydroxide solution into the container. In a reaction kettle with sodium hydrosulfide dissolved in water, when the temperature of the material reaches 123°C, under this temperature condition, after 21 minutes of heat preservation to generate sodium sulfide, N-methylpyrrolidone is added to make Na2 The molar ratio of S:NMP is 1.0:4.3, and the temperature of the material in the reactor is raised to 203...

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Abstract

The invention discloses a polyphenylene sulfide resin synthesis process, which aims to obtain a resin synthesis method with good particle formation, high product yield, high solvent recovery rate, andreduced corrosion degree of a polymerization reaction device. The method adopts sodium sulfhydrate containing sodium crystallization, sodium hydroxide, and p-dichlorobenzene as raw materials, and takes N-methylpyrrolidone as a solvent, and a condensation polymerization reaction is carried out in a synthesis system, after the low temperature and high temperature polycondensation is completed, acetate, NMP and an aqueous solution are added by a high-pressure pump, then the materials are insulated at a high temperature, cooled, and filtered, and a filter cake is purified by a NMP solvent, repeatedly washed with deionized water and filtered, and the filter cake is dried to obtain the polyphenylene sulfide resin. The polyphenylene sulfide resin synthesized by the invention is widely used in the fields of aerospace, electronic machinery, petrochemical, food, light industry, thermal power generation, cement industry, steel manufacturing, environmental protection, textile industry and the like.

Description

technical field [0001] The invention relates to the field of synthesis of resin materials, in particular to a synthesis process of polyphenylene sulfide resin. Background technique [0002] Linear high-molecular-weight polyphenylene sulfide (PPS) is widely used in aerospace, electronic machinery, petrochemical, food, light industry and other industrial technology fields due to its good chemical and physical properties. attention. US Patent No. 4910294, European Patent No. EP0256757, and U.S. Patent No. 4794164 all describe the process of synthesizing PPS in two steps, but they do not involve the method of adding materials. Domestic industrial synthesis process about PPS, only see the synthesis process and process condition control method announced by Chinese patent CN971073570, in the process of its polymerization reaction, almost all adopt a one-time feeding method, this method must reduce the temperature in the kettle to When the temperature is below 160°C, open the kett...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0259C08G75/0281C08G75/0209
CPCC08G75/0209C08G75/0259C08G75/0281
Inventor 陈逊
Owner 德阳科吉高新材料有限责任公司
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