Polyphenylene sulfide purifying method

A technology of polyphenylene sulfide and purification method, applied in the field of purification of polyphenylene sulfide, can solve the problems affecting the electrical insulation and mechanical strength of polyphenylene sulfide, and achieve high mechanical strength, strong electrical insulation and low content Effect

Active Publication Date: 2012-10-17
江苏新任环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the above purification method are: the purified polyphenylene sulfide still contains a large amount of inorganic ion impurities, oligomers and organic impurities, which seriously affect the electrical insulation and mechanical strength of polyphenylene sulfide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: A purification method of polyphenylene sulfide, comprising the following steps: (1) Acid-base neutralization: the product polyphenylene sulfide generated after the polymerization reaction is cooled to 100°C, hydrochloric acid is added, the pH is controlled to 3, and the mixture is stirred React for 25 minutes under stirring at a speed of 20 rpm; (2) solid-liquid separation: cool the reaction product obtained in step (1) to 75°C, and separate solid-liquid through a centrifuge to obtain polyphenylene sulfide solid; (3) solvent washing: in Add the organic solvent hexamethylphosphoric triamide to the obtained polyphenylene sulfide solid, control the temperature at 95° C., and wash under stirring for 10 minutes; (4) steam distillation and water washing: the polyphenylene sulfide obtained after washing in step (3) Phenyl sulfide is subjected to steam distillation under the condition of negative pressure -60KPa, and the organic solvent remaining in the solid parti...

Embodiment 2

[0013] Embodiment 2: A purification method of polyphenylene sulfide, comprising the following steps: (1) acid-base neutralization: the product polyphenylene sulfide generated after the polymerization reaction is cooled to 110°C, sulfuric acid is added, the pH is controlled to 3.5, and the mixture is stirred React for 30 minutes under stirring at a speed of 25 rpm; (2) solid-liquid separation: cool the reaction product obtained in step (1) to 80°C, and separate solid-liquid through a centrifuge to obtain polyphenylene sulfide solid; (3) solvent washing: in Add organic solvent N-methylpyrrolidone to the obtained polyphenylene sulfide solid, control the temperature at 100°C, and wash under stirring for 15 minutes; (4) steam distillation and water washing: the polyphenylene sulfide obtained after washing in step (3) Sulfur ether is steam distilled under the condition of negative pressure -70KPa, and the organic solvent remaining in the solid particles of polyphenylene sulfide is re...

Embodiment 3

[0014] Embodiment 3: A purification method of polyphenylene sulfide, comprising the following steps: (1) Acid-base neutralization: cooling the product polyphenylene sulfide generated after the polymerization reaction to 120°C, adding oxalic acid, controlling the pH to 4, and stirring React for 35 minutes under stirring at a speed of 30 rpm; (2) solid-liquid separation: cool the reaction product obtained in step (1) to 85°C, and separate the solid and liquid through a centrifuge to obtain a polyphenylene sulfide solid; (3) solvent washing: in Add the organic solvent hexamethylphosphoric triamide to the obtained polyphenylene sulfide solid, control the temperature at 105° C., and wash under stirring for 20 minutes; (4) steam distillation and water washing: the polyphenylene sulfide obtained after washing in step (3) Phenyl sulfide is subjected to steam distillation under the condition of negative pressure -80KPa, and the organic solvent remaining in the solid particles of polyphe...

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PUM

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Abstract

The invention discloses a polyphenylene sulfide purifying method. The method comprises the steps that: (1) acid-base neutralization is carried out, wherein a polymerization reaction product polyphenylene sulfide is cooled, an acid is added to polyphenylene sulfide, the pH of the mixture is controlled at 3-4, and a reaction is carried out while stirring; (2) solid-liquid separation is carried out, wherein a reaction product obtained in the step (1) is cooled and is subjected to solid-liquid separation, such that polyphenylene sulfide solid is obtained; (3) solvent washing is carried out, wherein an organic solvent is added to the obtained polyphenylene sulfide solid, and washing is carried out while stirring; (4) steam distillation and washing are carried out, wherein the polyphenylene sulfide obtained by washing in the step (3) is subjected to steam distillation under a negative-pressure condition, the residual organic solvent in the polyphenylene sulfide solid particles is recovered during the steam distillation process, and the polyphenylene sulfide is washed by using steam condensation water with a temperature of 75-85 DEG C when the content of the organic solvent is lower than 1%; and (5) drying and packaging are carried out, wherein qualified polyphenylene sulfide obtained in the step (4) is separated, dried, and packaged. Polyphenylene sulfide obtained with the method is advantaged in high electrical insulating property and high mechanical strength.

Description

technical field [0001] The invention relates to the production field of polyphenylene sulfide, in particular to a purification method of polyphenylene sulfide. Background technique [0002] Polyphenylene sulfide (PPS for short) has excellent thermal stability, good corrosion resistance, and excellent insulation and dielectric properties in high temperature and high humidity environments. Therefore, polyphenylene sulfide is widely used in fibers and electronic components. [0003] Polyphenylene sulfide is usually produced from sodium sulfide and p-dichlorobenzene. The polymerization reaction is completed at high temperature (usually around 300°C) and high pressure, and then purified and dried to obtain the finished product of polyphenylene sulfide. Since the directly produced polyphenylene sulfide contains a large amount of inorganic ion impurities, organic impurities and oligomers, which will affect the performance of subsequent polyphenylene sulfide, it must be effectively...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0281
Inventor 马建中唐峰夏海峰
Owner 江苏新任环保科技有限公司
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