Process for producing polyphenyl thioether
A technology of polyphenylene sulfide and polyphenylene sulfide resin, which is applied in the production process of polyphenylene sulfide to achieve the effects of overall temperature stability, reduced loss, and overcoming large investment
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Embodiment 1
[0040] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.
[0041] (3) In the reactor, first add p-dichlorobenzene in anhydrous sodium sulfide at a molar ratio of 1:1, then add 450ml of NMP and 30g of lithium chloride according to 1mol of the mixture, and react for 3 to 4 hours at a temperature of 210°C. After 1 hour, react at 250° C. for 1 to 2 hours until the reaction is complete, then stop the reaction to obtain a mixture of polyphenylene sulfide and sodium chloride.
[0042] (4) Put the mixture obtained in step (3) into a filter for separation to obtain a polyphenylene sulfide resin and a mixed solution.
[0043] (5) Put the polyphenylene sulfide resin obtained in step (4) into a stirred tank with a steam heating jacket at a temperature of 85-95°C, and perform conventional washing: extract the solvent with desalted water and wash the soluble inorgani...
Embodiment 2
[0054] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.
[0055] (3) In the reactor, first add p-dichlorobenzene in anhydrous sodium sulfide at a molar ratio of 1:1, then add 550ml of NMP and 40g of lithium chloride respectively according to 1mol of the mixture, and react at a temperature of 220°C for 3 to 4 After 1 hour, react at 260° C. for 1 to 2 hours until the reaction is complete, then stop the reaction to obtain a mixture of polyphenylene sulfide and sodium chloride.
[0056] (4) Put the mixture obtained in step (3) into a filter for separation to obtain a polyphenylene sulfide resin and a mixed solution.
[0057] (5) performing conventional washing, acid washing, alkaline washing, rinsing, and clear water washing on the polyphenylene sulfide resin obtained in the step (4) in sequence to obtain a purified polyphenylene sulfide resin;
[0058] (...
Embodiment 3
[0064] (2) the mixed steam in step (1) is separated solvent NMP by rectifier rectification, and all the other vapors are then cooled to dehydration cooling liquid by rectifier.
[0065] (3) In anhydrous sodium sulfide, first add p-dichlorobenzene in a molar ratio of 1:1, then add 600ml of N-methylpyrrolidone and 50g of lithium chloride respectively according to 1mol of the mixture, and react at 230°C for 3 to 4 After 1 hour, react at 270° C. for 1 to 2 hours until the reaction is complete, then stop the reaction to obtain a mixture of polyphenylene sulfide and sodium chloride.
[0066] (4) separating the mixture obtained in the step (3) to obtain a polyphenylene sulfide resin and a mixed solution;
[0067] (5) performing conventional washing, acid washing, alkaline washing, rinsing, and clear water washing on the polyphenylene sulfide resin obtained in the step (4) in sequence to obtain a purified polyphenylene sulfide resin;
[0068] (6) After mixing the mixed liquid obtaine...
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