Synthesis-auxiliary-free polyphenylene sulfide resin industrial synthetic process

A technology of polyphenylene sulfide resin and auxiliary agent is applied in the field of polymer material resin synthesis to achieve the effects of improving production efficiency, reducing cost and improving reaction speed.

Active Publication Date: 2014-05-28
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

[0005] As far as the development of the existing polyphenylene sulfide synthesis technology is concerned, the synthesis of polyphenylene sulfide resin without adding any synthetic additives is the future of polyphenylene sulfide synthesis technology The development direction is generally to use sodium sulfide, sodium hydroxide and p-dichlorobenzene (P-DCB) as raw materials, although the American Phillips company and Japan's polyphenylene sulfide resin production company without any synthetic additives produce The polyphenylene sulfide resin without adding

Method used

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  • Synthesis-auxiliary-free polyphenylene sulfide resin industrial synthetic process

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Experimental program
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Effect test

Embodiment 1

[0032] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): Sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): The molar ratio of NMP is 0.98: 0.30:1.00:2.30; the industrial synthesis process includes:

[0033] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is 33rmp, sodium sulfide is dissolved in anaerobic water to form a transparent solution containing sodium sulfide with a concentration of 18%wt. Sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 38%wt. Sodium sulfide and sodium hydroxide are added in a 316L stainless steel reactor with a molar ratio of 0.98:0.20, and heated to 130°C to make Sodium sulfide and sodium hydroxide are fully mixed and dissolved to form an aqueous solution of sodium sulfide and sodium hydroxide, and then the mixed solution containing sodi...

Embodiment 2

[0040] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): Sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): N-methylpyrrolidone (NMP) with a molar ratio of 1.18: 0.30: 1.28: 3.80; the industrial synthesis process includes:

[0041] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is within 66rmp, sodium sulfide is dissolved in anaerobic water to form a transparent solution containing sodium sulfide with a concentration of 38%wt. Sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 88%wt. Sodium sulfide and sodium hydroxide are added in a 316L stainless steel reaction kettle with a molar ratio of 1.18:0.20, and heated to 130°C to make Sodium sulfide and sodium hydroxide are fully mixed and dissolved to form an aqueous solution of sodium sulfide and sodium hydroxide, and ...

Embodiment 3

[0049] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): NMP molar ratio is 1.01:0.14:1.06:2.68; industrial synthesis process includes:

[0050] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is 33-66rmp, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 18-38%wt The transparent solution of sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 38~88%wt. Sodium sulfide and sodium hydroxide are added in the 316L stainless steel reaction kettle with the molar ratio of 1.01:0.10, and Heating to 121°C to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing sodium sulfi...

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Abstract

The invention discloses a synthesis-auxiliary-free polyphenylene sulfide resin industrial synthetic process. The formula of raw materials required in the synthesis-auxiliary-free polyphenylene sulfide resin industrial synthetic process is as follows: the mole ratio of sodium sulfide to sodium hydroxide to santochlor to N-methylpyrrolidinone is 0.98-1.18 to 0.01-0.30 to 1.00-1.28 to 2.30 to 3.80. The industrial synthetic process comprises the following steps: firstly, a pipeline filter is adopted to filtrate a sodium sulfide solution and a sodium hydroxide solution to treat the mechanical impurities in the solutions; secondly, a sodium hydroxide solution with the concentration of 60 mol percent is added in the formula for chemical treatment on the sodium sulfide solution; thirdly, in a condensation polymerization stage, 0.01-0.03 mol of sodium sulfide and 0.01-0.03 mol of dichlorobenzene are added to adjust the molecular weight and molecular weight distribution coefficient and adjust the content of covalent chlorine below 120 ppm, and finally the target product of the synthesis-auxiliary-free polyphenylene sulfide resin industrial synthetic process is obtained. According to the synthesis-auxiliary-free polyphenylene sulfide resin industrial synthetic process provided by the invention, the halogen in the obtained product is low in total content and polydispersity index, molecular weight distribution is narrow and oxygen index is high, the electrical insulation property is excellent, and the product adopted through the process can be used as packaging materials of electronic devices as well as industrial and civilian products, and particularly clad materials for wires and cables.

Description

technical field [0001] The invention belongs to the field of polymer material resin synthesis, especially the production of polyphenylene sulfide resin without adding any synthesis auxiliary agent. 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 that chemical substances such as mercapto and mercapto metal salts are used to synthesize polyphenylene sulfide resins. After the synthesis, the polyphenylene sulfide resins are treated to reduce the content of chlorine in the polyphenylene sulfide resins. In the future, the polyphenylene sulfide resin will be applied to the field of electronic components through mo...

Claims

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Application Information

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IPC IPC(8): C08G75/02C08G75/0213C08G75/0254
Inventor 陈逊
Owner 德阳科吉高新材料有限责任公司
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