Preparation method of polyphenylsulfone resin
The technology of polyphenylsulfone and resin is applied in the field of preparation of polyphenylsulfone resin, which can solve the problems of complicated polyphenylsulfone resin polymerization process and high product cost, and achieve the effects of preventing oxidation, improving product performance and improving product quality.
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[0019] The invention provides a kind of preparation method of polyphenylsulfone resin, comprises the following steps:
[0020] The aromatic dihydroxy compound, the bis-(halogenated aryl) sulfone compound, the catalyst and the organic solvent are mixed and dehydrated by blowing off with a protective gas to obtain a dehydrated product;
[0021] The dehydrated product is subjected to a polymerization reaction to obtain a polyphenylsulfone resin; the polymerization reaction is a gradient temperature rise process, the temperature at which the polymerization reaction begins to heat up is 90-120°C, and the final temperature of the polymerization reaction is 250-270°C , the time of the polymerization reaction is 5-8 hours, the heating rate of each gradient heating is independently 1-3°C / min, the temperature difference of each gradient heating is independently 15-30°C, and each gradient heating reaches the end of the heating The last holding time is independently 0.5-1h.
[0022] The ...
Embodiment 1
[0037] (1) Under nitrogen protection, add 1 weight part of 4,4'-difluorodiphenyl sulfone and 1 weight part of biphenol into 300 weight parts of N-methylpyrrolidone, and stir evenly. After complete dissolution, 0.3 parts by weight of catalyst lithium formate is added for preliminary dehydration, and after dehydration, the next stage of polymerization reaction is carried out, and nitrogen gas is used to take away moisture during the dehydration process.
[0038] (2) Polymerization is carried out by temperature control and temperature rise several times under stirring conditions, and the polymer product is finally obtained. The polymer product is discharged in cold water, and then crushed and cut. The obtained product with uniform particles is desalinated and washed with an alcohol solvent. Then use pure water to remove the alcohol solvent in the product, and finally the product is vacuum dried at 90°C for 17 hours.
[0039] Polymerization adopts a pressurized method, each holdin...
Embodiment 2
[0041](1) Under the protection of argon, 1 weight part of 4,4'-difluorodiphenyl sulfone and 3 weight parts of biphenol were added to 700 weight parts of N-methylpyrrolidone, and stirred evenly. After complete dissolution, 0.9 parts by weight of catalyst lithium formate is added for preliminary dehydration, and after the dehydration is completed, the next stage of polymerization reaction is carried out, and argon gas is used to take away moisture during the dehydration process.
[0042] (2) Polymerization is carried out by temperature control and temperature rise several times under stirring conditions, and finally a polymerized product is obtained, and the polymerized product is discharged in cold water, and then crushed and cut, and the obtained product with uniform particles is desalinated and washed with an alcohol solvent, Then use pure water to remove the alcohol solvent in the product, and finally the product is vacuum dried at 150°C for 7 hours.
[0043] Polymerization ...
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