Process for producing high-purity polyphenylene sulfide resin

A polyphenylene sulfide resin, high-purity technology, applied in the field of polyphenylene sulfide high-tech material synthesis, can solve problems such as exhaust pressure relief, reaction failure, material ratio imbalance, etc.

Inactive Publication Date: 2016-06-29
何展潮
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When feeding in this method, the temperature in the kettle must be lowered to below 160°C, and then the kettle is opened to feed, otherwise, p-dichlorobenzene p-DCB, one of the materials participating in the PPS polymerization reaction, will cause a change in the material ratio due to vaporization escape; Reheating the reaction after adding materials not only affects the success rate of the reaction, but also consumes a lot of energy; the exothermic reaction generated by the synthesis of PPS causes vaporized materials to be produced in the kettle, which increases the pressure of the

Method used

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  • Process for producing high-purity polyphenylene sulfide resin
  • Process for producing high-purity polyphenylene sulfide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the reactor, add sodium sulfide containing 1 water of crystallization, oxygen-free deionized water, lithium chloride, N-methylpyrrolidone, wherein Na 2 S:H 2 The molar ratio of O:LiCl:NMP is 1.0:13.0:0.88:1.8. Under the condition of feeding nitrogen, the temperature in the reactor is raised to 204°C at a rate of 1°C / min, and the dehydration time is 180min. When the dehydration rate is above 160°C, the dehydration rate is controlled within the range of 6000ml / min; when the dehydration is completed, the Na in the dehydration system 2 S:H 2 O:LiCl:NMP molar ratio becomes 1.0:.8:0.88:1.8; 2 S:p-DCB:H 2 The molar ratio of O:LiCl:NMP is 1.0:0.96:1.8:0.88:1.8; Nitrogen gas is passed 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 to raise the temperature. When rising to the low temperature stage, the temperature in this stage is controlled at 180°C an...

Embodiment 2

[0024] In the reactor, add sodium sulfide containing 3 crystal waters, anaerobic deionized water, lithium chloride, N-methylpyrrolidone, wherein Na 2 S:H 2 The molar ratio of O:LiCl:NMP is 1.0:9.0:0.28:6.8. Under the condition of feeding nitrogen, the temperature in the reactor is raised to 210°C at a speed of 3°C / min, and the dehydration time is 150min. When the dehydration rate is above 160°C, the dehydration rate is controlled within the range of 8000ml / min; when the dehydration is completed, the Na in the dehydration system 2 S:H 2 O:LiCl:NMP molar ratio becomes 1.0:1.0:0.28:5.8; 2 S:p-DCB:H 2 The molar ratio of O:LiCl:NMP is 1.0:1.28:1.0:0.28:5.8; Nitrogen is passed 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 to raise the temperature. When rising to the low temperature stage, the temperature in this stage is controlled at 200°C and the pressure ...

Embodiment 3

[0027] In the reactor, add sodium sulfide containing 1.5 crystal waters, anaerobic deionized water, lithium chloride, N-methylpyrrolidone, wherein Na 2 S:H 2 The molar ratio of O:LiCl:NMP is 1.0:11.0:0.43:2.8. Under the condition of feeding nitrogen, the temperature in the reactor is raised to 206°C at a rate of 1-3°C / min, and the dehydration time is 155min. When the temperature rises above 160°C, the dehydration rate is controlled within the range of 6369ml / min; when the dehydration is completed, the Na in the dehydration system 2 S:H 2 O:LiCl:NMP molar ratio becomes 1.0:1.3:0.43:2.8; 2 S:p-DCB:H 2 The molar ratio of O:LiCl:NMP is 1.0:1.08:1.3:0.43:2.8; Nitrogen is passed 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 to raise the temperature. When rising to the low temperature stage, the temperature in this stage is controlled at 186°C and the pressur...

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Abstract

The invention discloses a process for synthesizing high-purity polyphenylene sulfide resin. The high-purity polyphenylene sulfide resin is made of p-dichlorobenzene and sodium sulfide with certain crystal water, lithium chloride is used as a solubilizing assistant, and N-methyl-2-pyrrolidone is used as a solvent, so that the high-purity polyphenylene sulfide resin can be synthesized. The process includes that chemical raw materials such as oxygen-free deionized water, the sodium sulfide, the lithium chloride and the NMP (N-methyl-2-pyrrolidone) need to be added in a dehydration system before dehydration technological procedures are carried out, and then the p-dichlorobenzene is added into a synthesis system after heating dehydration is completely carried out on the synthesis system, so that condensation polymerization can be carried out. The process has the advantage that the high-purity polyphenylene sulfide resin synthesized and produced by the aid of the process can be widely applied to the fields of aerospace, electronic machinery, petrochemical engineering, foods, light industry, thermal power generation, cement industry, iron and steel manufacture, environmental protection, textile industry and the like.

Description

technical field [0001] The invention belongs to the field of polyphenylene sulfide high-tech material synthesis Background technique [0002] Linear high-molecular-weight polyphenylene sulfide (PPS) is widely used in aerospace, electronic machinery, petrochemical, food, light industry and other industrial technical fields because of 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. As for the industrial synthesis process of PPS in China, only the synthesis process and its process condition control method announced by Chinese patent CN971073570, almost all adopt a one-time feeding method in the process of its polymerization reaction. When feeding in this method, the temperature in the kettle must be lowered to below 160°C, and then the kettle is opened to feed, othe...

Claims

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Application Information

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IPC IPC(8): C08G75/0209C08G75/0254C08G75/0281
CPCC08G75/0209C08G75/0254C08G75/0281
Inventor 何展潮杨刚蔡洛川
Owner 何展潮
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