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
View PDF7 Cites 21 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0030] Example 1

[0031] Mix 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 200℃ for 2h to obtain dehydrated Na 2 S solution, wait for the above Na 2 When the temperature of S solution drops to 190℃, add 147g of p-dichlorobenzene, react at 200℃ for 6h, then keep at 230℃ for 3h, and then cool to 140℃. Filter the reaction solution. The filtered polyphenylene sulfide ( PPS) is poured into water, the crude product is separated, the crude product is washed, dried and purified with deionized water and acetone, and dried at a temperature of 120°C and a vacuum of 0.095MPa for 1 hour to obtain polyphenylene sulfide resin (PPS). The yield was 93%, the intrinsic viscosity [η] = 0.32, the solvent recovery rate was 93%, and the melt index was 56 g / 10 min. Infrared characterization see figure 1 Shown, DSC analysis see figure 2 Shown: Its me...

Example Embodiment

[0032] Example 2

[0033] Mix 50g zinc p-ethylbenzene sulfonate, 20g potassium formate, 400g N,N-dimethyl allyl urea and 166g 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℃ for 1 hour to obtain dehydrated Na 2 S solution, wait for the above Na 2 When the temperature of the S solution drops to 180°C, add 218g of 4,4'-difluorobenzophenone, react at 240°C for 3h, then keep at 280°C for 0.5h, and cool to 120°C. Filter the reaction solution. The latter polyphenylene sulfide ketone (PPSK) is poured into water, the crude product is separated, the crude product is washed, dried, and then purified with deionized water and acetone. After drying at a temperature of 110°C and a vacuum of 0.09MPa for 5 hours, polyphenylene sulfide is obtained. Ether ketone resin (PPSK). The yield was 92%, the intrinsic viscosity [η] = 0.52, and the solvent recovery rate was 95%. Infrared characterization see fi...

Example Embodiment

[0034] Example 3

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Melt indexaaaaaaaaaa
Melt indexaaaaaaaaaa
Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products