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
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[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...
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[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...
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