Halogen-free catalytic polyphenylene sulfide and preparation method thereof

A technology of polyphenylene sulfide and sodium sulfide, which is applied in the field of organic matter processing, and can solve problems such as secondary pollution, threats to health, and the environment

Inactive Publication Date: 2016-07-20
四川中科兴业高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogen may be used in the preparation of polyphenylene sulfide, but the combustion of halogen-containing organic waste will cause secondary pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A halogen-free catalytic polyphenylene sulfide is prepared from hydrogen sulfide, sodium hydroxide, dichlorobenzene, caprolactam, 6-aminocaproic acid, N-methylpyrrolidone, glycerol and antioxidants.

[0028] The preparation method of the halogen-free catalytic polyphenylene sulfide includes the following steps:

[0029] (1) Preparation of sodium sulfide

[0030] The hydrogen sulfide was passed into the reactor containing the sodium hydroxide solution with a concentration of 380 g / mL.

[0031] (2) Vacuum dehydration

[0032] The solution obtained by the reaction (1) is naturally volatilized to obtain sodium sulfide with crystal water, and the sodium sulfide with crystal water is put into the polymerization kettle, sealed and then evacuated, the vacuum degree is 0.096MPa, and then in the nitrogen gas It is heated and dehydrated under protection. The heating and dehydration is heating in sections. The temperature of the first section is 80°C and the time is 1.0h, and the temperatur...

Embodiment 2

[0044] A halogen-free catalytic polyphenylene sulfide is prepared from hydrogen sulfide, sodium hydroxide, dichlorobenzene, caprolactam, 6-aminocaproic acid, N-methylpyrrolidone, glycerol and antioxidants.

[0045] The preparation method of the halogen-free catalytic polyphenylene sulfide includes the following steps:

[0046] (1) Preparation of sodium sulfide

[0047] Pass hydrogen sulfide into a reactor containing a sodium hydroxide solution with a concentration of 400 g / mL.

[0048] (2) Vacuum dehydration

[0049] The solution obtained by the reaction (1) is naturally volatilized to obtain sodium sulfide with crystal water, and the sodium sulfide with crystal water is put into the polymerization kettle, sealed and then evacuated, the vacuum degree is 0.098MPa, and then it is protected by nitrogen It is heated and dehydrated under heating and dehydration is segmented heating. The temperature of the first stage is 82.5℃ and the time is 1.5h, and the temperature of the second stage is ...

Embodiment 3

[0061] A halogen-free catalytic polyphenylene sulfide is prepared from hydrogen sulfide, sodium hydroxide, dichlorobenzene, caprolactam, 6-aminocaproic acid, N-methylpyrrolidone, glycerol and antioxidants.

[0062] The preparation method of the halogen-free catalytic polyphenylene sulfide includes the following steps:

[0063] (1) Preparation of sodium sulfide

[0064] Pass hydrogen sulfide into a reactor containing a sodium hydroxide solution with a concentration of 420g / mL;

[0065] (2) Vacuum dehydration

[0066] The solution obtained by the reaction (1) is naturally volatilized to obtain sodium sulfide with crystal water, and the sodium sulfide with crystal water is put into the polymerization kettle, sealed and then evacuated, the vacuum degree is 0.1MPa, and then it is protected by nitrogen It is heated and dehydrated under heating and dehydration is heating in sections. The temperature of the first section is 85°C and the time is 2.0h, and the temperature of the second section i...

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PUM

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Abstract

The invention discloses halogen-free catalytic polyphenylene sulfide and a preparation method thereof. Concentration of a sodium hydroxide solution in a reaction kettle is 400 g/mL, at the moment, sodium hydroxide has maximum absorbing rate on hydrogen sulfide, and yield of sodium sulfide is highest. Vacuum degree in a polymerization kettle is 0.098 MPa. Dewatered sodium sulfide obtained at the vacuum degree is loose, free of melting and boiling and wall sticking and conducive to subsequent reaction. Sectional heating is adopted, so that conversion of sodium sulfide in the heating process can be prevented, and vacuum dewatering time can be shortened. Polycondensation is performed in two steps to enable further reaction of active end group of oligomer and enable further growth of molecular chains.4, 4'-dihydroxybiphenyl is added into polycondensation, so that the polyphenylene sulfide is enabled to be oxidation-resistant. Therefore, by adopting the preparation method, the halogen-free catalytic polyphenylene sulfide is high in quality, little in pollution, great in market potential and promising in prospect.

Description

Technical field [0001] The invention belongs to the field of organic processing. More specifically, the invention relates to a halogen-free catalytic polyphenylene sulfide and a preparation method thereof. Background technique [0002] Polyphenylene sulfide (PPS for short) has excellent flame retardancy, heat resistance, chemical resistance, electrical insulation properties and good mechanical properties. Its usage ranks sixth in the field of engineering plastics. Special engineering plastics with excellent performance. Polyphenylene sulfide is widely used in automobiles, electronic appliances, machinery industry, petrochemical, military industry, aerospace and other fields. Polyphenylene sulfide is a high-performance fiber with high temperature resistance, chemical corrosion resistance and good flame retardancy. It can be used in high-temperature flue dust removal, fire-fighting insulation clothing, etc. It is one of the high-performance fibers that have developed rapidly in re...

Claims

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Application Information

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IPC IPC(8): C08G75/0222C08G75/0254
CPCC08G75/0222C08G75/0254
Inventor 刘洪陈培龙陈显坊
Owner 四川中科兴业高新材料有限公司
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