Polyphenylene sulfide resin production process

A technology of polyphenylene sulfide resin and production process, which is applied in the field of production process of polyphenylene sulfide resin, and can solve the problem of irregular polyphenylene sulfide resin particles, small polyphenylene sulfide resin particles, and polyphenylene sulfide resin molding Difficulties and other problems, to achieve the effect of improving particle forming rate, improving purity and improving performance characteristics

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

AI Technical Summary

Problems solved by technology

[0005] In Chinese patent 201610033529.2, sodium acetate is introduced as a co-solvent for the synthesis of polyphenylene sulfide resin. Due to the influence of the crystal shape of sodium acetate after the synthesis of polyphenylene sulfide resin, the molding of polyphenylene sulfide resin is relatively difficult. difficulty
[0006] In Chinese patent 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 condensation polymerization without adding any synthetic auxiliary agent. Due to the influence of the amount of solvent in the polymerization reaction system, the synthesized polyphenylene sulfide resin particles are very irregular, and there are still Polyphenylene sulfide resin particles are 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 production process of polyphenylene sulfide resin:

[0031] (1) Add sodium sulfide and N-methylpyrrolidone containing 5 crystal waters into the dehydration kettle, of which Na 2 The molar ratio of S:NMP is 1.0:1.8. Under the condition of feeding nitrogen, the temperature in the reactor is raised to 210°C at a rate of 1°C / min, and the dehydration time is 300min;

[0032] (2) In the dehydration system, after adding p-dichlorobenzene, add a certain amount of NMP solvent, so that the Na in the polymerization system 2 S:p-DCB:H 2 The molar ratio of O:NMP is 1.0:0.98:1.6:3.8. Nitrogen is introduced into the synthesis system, and the air in the polymerization system is replaced to seal the polymerization reaction system, and then the polymerization system is heated up. When the temperature rises to the low temperature stage At this stage, the temperature is 210°C and the pressure is 3kg / cm 2 , time 210min, when the low-temperature stage heat preservation is over, the te...

Embodiment 2

[0042] (1) Add sodium sulfide and N-methylpyrrolidone containing 5 crystal waters into the dehydration kettle, of which Na 2 The molar ratio of S:NMP is 1.0:3.8, under the condition of feeding nitrogen, the temperature in the reactor is raised to 214°C at a speed of 3°C / min, and the dehydration time is 240min;

[0043] (2) After adding p-dichlorobenzene in the dehydration system, add a certain amount of NMP solvent, so that the Na in the polymerization system 2 S:p-DCB:H 2 The molar ratio of O:NMP is 1.0:1.08:1.9:4.8. Nitrogen is introduced into the synthesis system, and the air in the polymerization system is replaced to seal the polymerization reaction system, and then the polymerization system is heated up. When the temperature rises to the low temperature stage At this stage, the temperature is 220°C and the pressure is 6kg / cm 2 , time 180min, when the low-temperature stage heat preservation is over, the temperature rises to the high-temperature polymerization stage at a...

Embodiment 3

[0053] (1) Add sodium sulfide and N-methylpyrrolidone containing 5 crystal waters into the dehydration kettle, of which Na 2 The molar ratio of S:NMP is 1.0:2.1. Under the condition of feeding nitrogen, the temperature in the reactor is raised to 211°C at a rate of 1.5°C / min, and the dehydration time is 255min;

[0054] (2) Add p-dichlorobenzene in the dehydration system and add a certain amount of NMP solvent so that Na in the polymerization system 2 S:p-DCB:H 2 The molar ratio of O:NMP is 1.0:1.0:1.63:4.1. Nitrogen is introduced into the synthesis system, and the air in the polymerization system is replaced to seal the polymerization reaction system, and then the polymerization system is heated up. When the temperature rises to the low temperature stage At this stage, the temperature is 212°C and the pressure is 3.5kg / cm 2 , time 191min, when the low-temperature stage heat preservation is over, the temperature rises to the high-temperature polymerization stage at a rate of...

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Abstract

The invention discloses a polyphenylene sulfide resin production process, which aims to a resin production method with good particle formation, high product yield, high solvent recovery rate, and reduced corrosion degree of a polymerization reaction device. The process adopts sodium sulfide containing a certain crystal water and p-dichlorobenzene as raw materials, and takes N-methylpyrrolidone asa solvent to synthesize the polyphenylene sulfide resin, and before a dehydration process, sodium sulfide and NMP raw materials are added to a dehydration system, a synthesis system is heated and dehydrated, after the dehydration is completed, p-dichlorobenzene and sodium sulfide are added in the synthesis system to carry out a condensation polymerization reaction 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 resin material synthesis, in particular to a production 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. countries' 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 production process about PPS, only see the production 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, ope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0254C08G75/0209C08G75/0281
CPCC08G75/0209C08G75/0254C08G75/0281
Inventor 陈逊
Owner 德阳科吉高新材料有限责任公司
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