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Preparation method of organic acid salt catalytic polyarylene sulfide

An organic acid salt catalyzed polyarylene sulfide and polyarylene sulfide technology, which is applied in the field of polyarylene sulfide preparation, can solve the problems of difficult catalyst recovery, low solvent recovery rate, and many reaction by-products, and achieve easy processing, Effect of high glass transition temperature and low product cost

Active Publication Date: 2013-06-26
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In industrialized production, the current main method of polyarylene sulfide production is: using a composite catalytic system to carry out solution polycondensation of sodium sulfide and dihalogenated aromatic compounds under high temperature and high pressure, such as Philips company using sodium sulfide and p-dichlorobenzene in nitrogen Prepared by pressure reaction in polar solvent NMP (US33544129), this method consumes a lot of energy and costs high
Chinese patent CN1143652A reports that in a polar solvent, sulfur is used as a raw material to pressurize and synthesize tough polyphenylene sulfide resin. The reaction process requires the use of a reducing agent, the process is relatively complicated, there are many reaction by-products, and the product is not easy to purify; CN1793202A Deyang Technology Co., Ltd. Co., Ltd. uses sodium sulfide and p-dichlorobenzene as raw materials to use a composite catalytic system to pressurize synthetic fiber-grade polyphenylene sulfide resin, but the catalyst it uses is a composite catalytic system, including catalytic promoters and catalysts, making its products more difficult Purification, catalyst recovery is difficult, and the solvent recovery rate is low, making its production cost higher

Method used

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  • Preparation method of organic acid salt catalytic polyarylene sulfide
  • Preparation method of organic acid salt catalytic polyarylene sulfide
  • Preparation method of organic acid salt catalytic polyarylene sulfide

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Experimental program
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Effect test

Embodiment 1

[0031] 30g calcium adipate, 10g sodium carbonate, 500g N-methylpyrrolidone and 240g Na 2 S·9H 2 O was added to the autoclave, and under the protection of nitrogen, the dehydration reaction was carried out at a temperature of 200°C for 2 hours to obtain the dehydrated Na 2 S solution, to be the above Na 2 When the temperature of the S solution drops to 190°C, add 147g of p-dichlorobenzene, react at a temperature of 200°C for 6h, then keep at a temperature of 230°C for 3h, cool down to 140°C, filter the reaction solution, and filter the polyphenylene sulfide ( PPS) was poured into water, the crude product was separated, the crude product was washed, dried, purified with deionized water and acetone, and dried at a temperature of 120°C and a vacuum of 0.095 MPa for 1 hour to obtain polyphenylene sulfide resin (PPS). Its yield is 93%, intrinsic viscosity number [η]=0.32, solvent recovery rate is 93%, and melt index is 56g / 10min. For infrared characterization see figure 1 Shown,...

Embodiment 2

[0033] 50g of zinc p-ethylbenzenesulfonate, 20g of potassium formate, 400g of N,N-dimethylpropenyl urea and 166g of Na 2 S·5H 2 O was added to the autoclave, and under the protection of nitrogen, the dehydration reaction was carried out at a temperature of 190°C for 1 hour to obtain the dehydrated Na 2 S solution, to be the above Na 2 When the temperature of the S solution drops to 180°C, add 218g of 4,4'-difluorobenzophenone, react at a temperature of 240°C for 3h, then keep at a temperature of 280°C for 0.5h, cool down to 120°C, filter the reaction solution, and Pour the finished polyphenylene sulfide ketone (PPSK) into water, separate the crude product, wash the crude product, dry it, purify it with deionized water and acetone, and dry it at a temperature of 110°C and a vacuum of 0.09 MPa for 5 hours to obtain polyphenylene sulfide Etherketone resin (PPSK). The yield was 92%, the intrinsic viscosity [η]=0.52, and the solvent recovery was 95%. For infrared characterizati...

Embodiment 3

[0035] 5 g tin p-sulfosalicylate, 0.1 g potassium hydroxide, 400 g 2,4-dimethylsulfolane and 130 g Na 2 S·3H 2 O was added to the autoclave, and under the protection of nitrogen, the dehydration reaction was carried out at a temperature of 190°C for 1.5h to obtain the dehydrated Na 2 S solution, to be the above Na 2 When the temperature of the S solution drops to 180°C, add 287g of 4,4'-dichlorodiphenyl sulfone, react at a temperature of 220°C for 3 hours, then keep at a temperature of 230°C for 1 hour, cool down to 110°C, and filter the reaction solution. Pour polyphenylene sulfide sulfone (PPSS) into water, separate the crude product, wash the crude product, dry it, purify it with deionized water and acetone, and dry it for 8 hours at a temperature of 110°C and a vacuum of 0.085 MPa to obtain polyphenylene sulfide sulfone Resin (PPSS). Its yield is 92%, intrinsic viscosity number [η]=0.61, and solvent recovery rate is 90%. For infrared characterization see figure 1 Show...

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Abstract

The invention discloses a preparation method of organic acid salt catalytic polyarylene sulfide. The preparation method is characterized by comprising the following steps of: adding 1-50 parts of catalyst, 0.1-20 parts of alkali or strong alkali and weak acid salt, 100-500 parts of organic solvent and 130-140 parts of Na2S.xH2O into a reaction kettle, carrying out dehydration reaction for 0.5-2h at 150-200 DEG C under the protection of nitrogen to obtain a dehydrated Na2S solution, when the temperature of the Na2S solution is reduced to 150-190 DEG C, adding 114-287 parts of dihalogenated aromatic compound, reacting for 0.5-6h at 160-240 DEG C, maintaining the temperature for 0.5-6h at 190 DEG C to 280 DEG C, reducing temperature to 80-140 DEG C, filtering reaction liquid, pouring a filtered reaction product into water, separating a polymer crude product, washing the crude product, purifying by using deionized water and acetone after drying, and drying for 1-10h at 100-120 DEG C under vacuum of 0.08-0.095Mpa, thus obtaining the polyarylene sulfide resin.

Description

technical field [0001] The invention relates to a preparation method of polyarylene sulfide, which belongs to the field of polymer synthesis. Background technique [0002] Polyarylene sulfide such as polyphenylene sulfide, polyphenylene sulfide ketone, and polyphenylene sulfide sulfone are widely used in automobiles, aerospace and aviation due to their high temperature resistance, corrosion resistance, excellent electrical properties, mechanical properties and dimensional stability and electronic technology. In industrialized production, the current main method of polyarylene sulfide production is: using a composite catalytic system to carry out solution polycondensation of sodium sulfide and dihalogenated aromatic compounds under high temperature and high pressure, such as Philips company using sodium sulfide and p-dichlorobenzene in nitrogen It is prepared by pressure reaction in polar solvent NMP (US33544129). This method consumes a lot of energy and costs high. Chinese...

Claims

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Application Information

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IPC IPC(8): C08G75/02C08G75/0213C08G75/0236C08G75/024C08G75/0254C08G75/0281
Inventor 张刚杨杰李东升李志敏王孝军龙盛如严永刚
Owner SICHUAN UNIV
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