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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

Active Publication Date: 2011-07-13
DUNHUANG XIYU MINING & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the domestic units developing polyphenylene sulfide adopt the method of dehydration outside the kettle to prepare anhydrous sodium sulfide, and then mix with p-dichlorobenzene in the polar organic solvent hexamethylphosphoric triamide under normal pressure. Under such an immature process route of reaction, the production often encounters great difficulties in the refining of sodium sulfide. In addition, the reaction catalytic system is backward and the process control is difficult, resulting in low solvent recovery rate, high production cost, and product reproduction. Poor performance and low molecular weight, so these research and development and experiments have ended in failure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a process for producing polyphenyl thioether, comprising the following steps of:, mixing hydrogenous sodium sulfide, lithium chloride and N-methyl pyrrolidone in the weight ratio of (20-25): (2-6): (70-80), co-boiling the mixture and inert gases at 150-210 DEG C for distilling and dehydrating; separating solvent by refining; respectively adding santochlor, solvent and lithium chloride in anhydrous sodium sulfide, separating after complete reaction to obtain polyphenylene sulfide; compositely washing the polyphenylene sulfide to obtain pure polyphenylene sulfide; and reclaiming the lithium chloride by filtering, reclaiming the solvent and flashly evaporating dimethylbenzene solution in a two-period mode and cooling and crystallizing. The invention has the advantages of low cost, simple process, excellent performance of synthetic resin and high solvent recovering rate.

Description

technical field [0001] The invention relates to a production process of a polymer material, in particular to a process for producing polyphenylene sulfide. Background technique [0002] Polyphenylene sulfide is referred to as PPS, which has excellent thermal stability, short-term heat resistance and long-term continuous use thermal stability, as well as good corrosion resistance, adhesion and fluidity, while PPS has very low dielectric constant, inductance and dielectric loss factor, and has excellent insulation and dielectric properties in high temperature, high humidity and other environments. Therefore, as a special engineering plastic with excellent performance, it has been widely used in the fields of automobiles, electrical electronics and machinery. [0003] At present, there are many synthetic routes of polyphenylene sulfide, but there are only two routes that have been industrialized or have industrial value: one is the industrialized Phillips route (i.e. sodium s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/02C08G75/0213C08G75/0254C08G75/0281
Inventor 宋祥会周文胡原周华杨永红宋立旺宋丽
Owner DUNHUANG XIYU MINING & CHEM
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