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Method for synthesizing low-chloride polyphenylene sulfide resin

A technology of polyphenylene sulfide resin and synthesis method, which is applied in the field of polymer material resin synthesis and production, and can solve problems such as unseen process introduction

Active Publication Date: 2010-03-10
德阳科吉高新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] As far as the existing polyphenylene sulfide synthesis technology is concerned, the synthesis of polyphenylene sulfide resin generally uses sodium sulfide and p-dichlorobenzene (P-DCB) as raw materials, although the American Phillips company and Japanese polyphenylene sulfide r

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the autoclave, 12 kilograms of N-methyl-2-pyrrolidone (NMP) is a solvent, and sodium sulfide (Na 2 S.3H 2(0) 4.2 kilograms, 0.01 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, while stirring, heat up, rise to 203 ℃ dehydration with the time of 2 hours, add p-dichlorobenzene 4.6 kilograms, NMP 2 kg, react at a temperature of 200°C for 3 hours, extract the solvent NMP with ethanol several times, then wash the prepolymer repeatedly with deionized water, and dry it under vacuum at 110°C for 3 hours, then add N-methyl-2 -Pyrrolidone solvent, make the polyphenylene sulfide resin content of pre-polymerization be 20%, then add 2,5-dimethyl p-aminochlorobenzene 0.025 kilograms (0.5% mol) in solvent system, cool down after polymerization reaction 2 hours After reaching 185°C, add 0.2 kg (3.0% mol) of 2,5-dimethyl-p-chlorobenzoate, then heat up to 250°C for 1 hour, then cool to 200°C and add the deionizing agent mixture ethylene...

Embodiment 2

[0027] In the autoclave, 12 kilograms of N-methyl-2 pyrrolidone (NMP) is a solvent, and sodium sulfide (Na 2 S.3H 2 (O) 4.2 kilograms, 0.02 kilograms of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, while stirring, while heating up, rise to 203 ℃ dehydration with the time of 2 hours, add 4.6 kilograms of p-dichlorobenzene, NMP 2 kg, at a temperature of 200 ° C for 3 hours, under the conditions of this temperature, add 0.03 kg (0.6% mol) of 2,5-dimethyl-p-aminochlorobenzene, cool to 185 ° C after 2 hours of polymerization, and use ethanol The solvent NMP was extracted for many times, and then the prepolymer was repeatedly washed with deionized water, and dried under vacuum at 110°C for 3 hours, and then N-methyl-2-pyrrolidone solvent was added to make the prepolymerized polyphenylene sulfide The resin content is 30%, then add 0.22 kg (3.3% mol) of 2,5-dimethyl p-chlorobenzoate to the solvent system, then heat up to 250 ° C for 1 hour, cool...

example 3

[0029] In the autoclave, 12 kilograms of N-methyl-2 pyrrolidone (NMP) is a solvent, and sodium sulfide (Na 2 S.3H 2 (O) 4.2 kilograms, 0.013 kilograms of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, while stirring, heat up, rise to 203 ℃ dehydration with the time of 2 hours, add 4.6 kilograms of p-dichlorobenzene, NMP 2 1 kg, at a temperature of 200 ° C for 3 hours, under the conditions of this temperature, add 0.03 kg (0.5% mol) of 2,5-dimethyl-p-nitrochlorobenzene, cool to 185 ° C after the polymerization reaction for 2 hours, use The solvent NMP was extracted by ethanol for many times, and then the prepolymer was repeatedly washed with deionized water, and dried under vacuum at 110°C for 3 hours, and then N-methyl-2-pyrrolidone solvent was added to make the prepolymerized polyphenylene sulfide The content of ether resin is 22%, then add 0.239 kg (3.0% mol) of 2,5-dimethyl-p-chlorobenzenesulfonate to the solvent system, heat up to 250°...

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Abstract

The invention discloses a method for synthesizing low-chloride polyphenylene sulfide resin, comprising the following steps: taking sodium sulfide and p-dichlorobenzene with the molar ratio of 1:1 as raw materials, N-methyl-2-pyrrolidone as a solvent, and carrying out polycondensation to generate the polyphenylene sulfide resin under the action of alkali metal cosolvent. The synthesizing process mainly comprises the following steps: adding adjuvant lithium aluminum hydride in the dewatering phase of sodium sulfide; adding molecular weight regulator and deionizer in the polycondensation stage; and adopting an extraction process in the resin recovery stage. The product obtained in the invention has low content of halogen element, relative low polydispersion coefficient, very narrow molecularweight distribution, high oxygen index and other excellent performance indexes, can be used as products such as injection moulds, extrusion moulds, fibers, films and the like, can be widely used in the fields such as machinery, chemical industry, electrical and electronic products, military project, aerospace and the like, and is particularly applied to electrical and electronic field with very excellent electrical insulation property.

Description

technical field [0001] The invention belongs to the field of polymer material resin synthesis production. Background technique [0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardancy, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from all over the world have been working hard to find it. [0003] In U.S. Patent No: 4761468, it is described to use chemical substances such as mercapto and mercapto metal salts to treat the polyphenylene sulfide resin after the polyphenylene sulfide resin is synthesized, thereby reducing the content of chlorine in the polyphenylene sulfide resin. Later, polyphenylene sulfide resin is applied to the field of electronic components through modification, and its main purpose is to improve the insulation performance of polyphenylene sulfide materials. [0004] As far...

Claims

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Application Information

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IPC IPC(8): C08G75/02C08G75/0254
Inventor 陈逊
Owner 德阳科吉高新材料有限责任公司
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