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Process for synthesizing polyphenylene sulfide resin

A polyphenylene sulfide resin and process technology, applied in the field of synthesizing polyphenylene sulfide resin, can solve the problems of many by-products, affecting product yield, etc., and achieve the effects of small fluctuation of product quality and reduction of production cost

Active Publication Date: 2014-08-20
JIANGSU GELANDE INVESTMENT DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] After a lot of experiments and painstaking research, the applicant found that the use of sodium 4-methylaminobutyrate as an intermediate can indeed promote the synthesis of polyphenylene sulfide resin, but too much sodium 4-methylaminobutyrate The existence of will make the by-products increase and affect the yield of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Select 1.003mol aqueous sodium hydrosulfide crystal as the sulfur source, add it to a 1L reactor, and add 1.00mol sodium hydroxide solid;

[0022] Step 2: Introduce nitrogen into the reaction kettle, gradually heat the above mixture, after the temperature rises to 120°C, start stirring, control the rotation speed at 300rpm, then raise the temperature to 170±3°C for dehydration, collect the dehydration liquid, and prevent the dehydration process The tail gas is absorbed with sodium hydroxide solution until no droplet is observed within one minute at the eluate collection port;

[0023] Step 3: Add 0.15 mol of pre-prepared and pulverized 4-methylaminobutyrate sodium, 1.01 mol of p-dichlorobenzene, 3.3 mol of N-methyl-2-pyrrolidone into the reactor, and use nitrogen gas to Replace the air that may be introduced into the reactor during the feeding process;

[0024] Step 4: Raise the temperature of the reactor to 220±8°C, control the rotation speed of the stirring p...

Embodiment 2

[0029] Step 1: Select 1.003mol hydrous sodium sulfide crystals as the sulfur source, and add it to a 1L reactor;

[0030] Step 2: Introduce nitrogen into the reaction kettle, gradually heat the above mixture, after the temperature rises to 120°C, start stirring, control the rotation speed at 200rpm, and then raise the temperature to 175±3°C for dehydration, collect the dehydration liquid, and prevent the dehydration process The tail gas is absorbed with sodium hydroxide solution until no droplet is observed within one minute at the eluate collection port;

[0031] Step 3: Add 0.25 mol of pre-prepared and pulverized 4-methylaminobutyrate sodium, 1.01 mol of p-dichlorobenzene, 3.5 mol of N-methyl-2-pyrrolidone into the reactor, and use nitrogen gas to Replace the air that may be introduced into the reactor during the feeding process;

[0032] Step 4: Raise the temperature of the reactor to 220±8°C, control the rotation speed of the stirring paddle at 600rpm, keep it warm for 1h...

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PUM

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Abstract

The invention relates to a process for synthesizing polyphenylene sulfide resin. The process comprises the following steps of: firstly blending sulfur source with sodium hydroxide or liquid alkali in a reaction kettle, carrying out temperature rising and dehydration in atmosphere of nitrogen, then adding 0.05-0.25 mol of sodium 4-methylamino butyrate relative to 1 mol of the sulfur source, adding p-dichlorobenzene and N-methyl-2-pyrrolidone, rising the temperature and carrying out polymerization, after finishing the polymerization, carrying out temperature lowering and decompression on the reaction kettle, screening and filtering reaction products, and carrying out washing and oven drying on granular resins. The process is adopted to synthesize the polyphenylene sulfide resin, not only the yield of the polyphenylene sulfide resin is improved, but also the production cost is lowered, and the stability of the product quality is improved.

Description

technical field [0001] The invention relates to a process for synthesizing polyphenylene sulfide resin, which belongs to the field of polymer material synthesis. Background technique [0002] Since the Philips Petroleum Company of the United States began to industrialize the production of polyphenylene sulfide resin in the 1970s, the excellent chemical corrosion resistance, high temperature resistance, radiation resistance and high flame retardancy of this engineering plastic have become more and more popular. draw people's attention. There are a lot of literature reports around the synthesis process and application performance of this product, but there is no accurate conclusion on the mechanism of the synthesis process of polyphenylene sulfide resin. [0003] Since Philips Petroleum Company discovered that the solvent commonly used for the synthesis of polyphenylene sulfide resin - N-methyl-2-pyrrolidone can be hydrolyzed under alkaline conditions to generate sodium 4-met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/02C08G75/0254C08G75/0259
Inventor 郑渊博
Owner JIANGSU GELANDE INVESTMENT DEV