Auxiliary-addition-free polyphenylene sulfide resin industrial synthetic process

A technology of polyphenylene sulfide resin and additives, which is applied in the field of polymer material resin synthesis, can solve the problems such as the introduction of the process of mixing sodium hydrosulfide, and achieve the effects of shortening the synthesis time, increasing the reaction speed, and reducing the cost

Active Publication Date: 2014-05-28
周洪
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As far as the existing polyphenylene sulfide synthesis technology is concerned, the synthesis of polyphenylene sulfide resin without any additives generally uses sodium hydrosulfide and p-dichlorobenzene (P-DCB) as raw materials, although the US Phillips company and Japan The polyphenylene sulfide resin produced by the polyphenylene sulfide resin production company has basically not changed much in the raw materials, so that the polyphenylene sulfide resin can achieve the purpose of low chlorine by adding auxiliary materials, but it has not been mixed. Mixed sodium hydrosulfide specific process introduction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] at 33m 3 In a 316L stainless steel autoclave, the molar ratio of sodium hydrosulfide (NaHS): p-dichlorobenzene (abbreviation: p-DCB): N-methyl-2-pyrrolidone (NMP): sodium hydroxide (NaOH) is 0.93: 1.00:1.98: 1.18; industrial synthesis process includes:

[0033] 1) In the sodium hydrosulfide dehydration treatment stage, sodium hydrosulfide crystals are added to a 316L stainless steel reactor, and heated to 80-90°C, and an oxygen-free deionized water is used to prepare a 33%wt sodium hydrosulfide aqueous solution, and then the sulfur The sodium hydride solution is input into a pipeline filter with a heat preservation temperature of 80-90°C for mechanical impurity treatment. The filter element of the filter element is a pure titanium metal filter with a pore size of 0.0001um and a flow rate of 33m 3 / h, then the sodium hydrosulfide solution processed by the pipeline filter is input to the next stage 316L stainless steel reactor for use, wherein the stirring intensity is 6...

Embodiment 2

[0044] at 33m 3 In a 316L stainless steel autoclave, the molar ratio of sodium hydrosulfide (NaHS): p-dichlorobenzene (p-DCB): NMP: NaOH is 1.15: 1.28: 2.98: 1.48; the industrial synthesis process includes:

[0045] 1) In the sodium hydrosulfide dehydration treatment stage, sodium hydrosulfide pentahydrate crystals are added to a 316L stainless steel reactor, and heated to 90°C, and an oxygen-free deionized water is used to prepare a 66%wt sodium hydrosulfide aqueous solution, and then the sulfur The sodium hydride solution is input into a pipeline filter with a heat preservation temperature of 90°C for mechanical impurity treatment. The filter element of the filter element is a pure titanium metal filter with a pore size of 0.0001um and a flow rate of 66m 3 / h, then the sodium hydrosulfide solution processed by the pipeline filter is input to the next stage 316L stainless steel reactor for use, wherein the stirring intensity is 800rmp, and the purity of sodium hydrosulfide is...

Embodiment 3

[0056] Sodium hydrosulfide (NaHS): p-dichlorobenzene (abbreviation: p-DCB): NMP: NaOH molar ratio is 1.03:1.08:2.16: 1.23; industrial synthesis process includes:

[0057] 1) In the sodium hydrosulfide dehydration treatment stage, sodium hydrosulfide crystals are added to a 316L stainless steel reactor, and heated to 88°C, and an oxygen-free deionized water is used to prepare a 48%wt sodium hydrosulfide aqueous solution, and then the sodium hydrosulfide The solution is input into a pipeline filter with a heat preservation temperature of 88°C for mechanical impurity treatment. The filter element of the filter element is a pure titanium metal filter with a pore size of 0.0001um and a flow rate of 48m 3 / h, then the sodium hydrosulfide solution that is processed through the pipeline filter is input to the next stage 316L stainless steel reactor for use, wherein the stirring intensity is 743rmp, and the purity of sodium hydrosulfide is a solid of 98.4%wt;

[0058] 2) Add the sodium...

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Abstract

The invention discloses auxiliary-addition-free polyphenylene sulfide resin industrial synthetic process. The formula of raw materials required in the auxiliary-addition-free polyphenylene sulfide resin industrial synthetic process is as follows: the mole ratio of sodium sulfide to sodium hydroxide to santochlor to N-methyl-2-pyrrolidinone is 0.93-1.15 to 1.00-1.28 to 1.98-2.98 to 1.18 to 1.48. The industrial synthetic process mainly comprises the following steps: firstly, in a sodium hydrosulfide dehydration treatment stage, a pipeline filter is adopted to filtrate a sodium hydrosulfide solution to treat mechanical impurities in the solution, then a sodium hydroxide solution with the concentration 84 mol percent is added in the formula for chemical treatment on the sodium hydrosulfide; secondly, in the condensation polymerization stage, anaerobic deionized water is added to further appropriately adjust the molecular weight and molecular weight distribution coefficient of synthesized polyphenylene sulfide resin; thirdly, deionized water is adopted for repeatedly scrubbing for 3 to 6 times, and finally, the target product of the auxiliary-addition-free polyphenylene sulfide resin industrial synthetic process provided by the invention is obtained. The resin in the obtained product of the auxiliary-addition-free polyphenylene sulfide resin industrial synthetic process is low in polydispersity index and high in oxygen index, and has an excellent electrical insulation property.

Description

technical field [0001] The invention belongs to the synthesis of polymer material resin, especially the field of polyphenylene sulfide resin 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 po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0213C08G75/0259
Inventor 陈逊
Owner 周洪
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