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A kind of ultrasonic cleaning and purification method of polyphenylene sulfide

A purification method, polyphenylene sulfide technology, applied in the field of ultrasonic cleaning and purification of polyphenylene sulfide, can solve the problems of large product loss and cumbersome separation steps, and achieve simple operation, narrow molecular weight distribution, and good separation and purification effect Effect

Active Publication Date: 2020-04-14
广东南粤精工精密组件有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the separation steps are cumbersome and the product loss is large
[0004] In summary, the current technology still lacks a method that can efficiently separate the crude product of polyphenylene sulfide

Method used

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  • A kind of ultrasonic cleaning and purification method of polyphenylene sulfide
  • A kind of ultrasonic cleaning and purification method of polyphenylene sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Separation of crude polyphenylene sulfide to obtain separation product A1

[0025] (1) Ultrasonic high-frequency pre-cleaning: Add 3.5 kg of crude polyphenylene sulfide to an ultrasonic cleaning tank filled with 10 liters of N-methylpyrrolidone solvent and 0.001 liter of hexamethylphosphoric triamide solvent for cleaning. The ultrasonic temperature is 200KHz, and the ultrasonic temperature is 200°C. After cleaning for 120 minutes, the solid-liquid separation is carried out by rotary evaporation to obtain the pretreated solid;

[0026] (2) Ultrasonic low-frequency cleaning and purification: put the pretreated solid obtained in step (1) into an ultrasonic cleaning tank equipped with 10 liters of deionized water, the ultrasonic frequency is 20KHz, the ultrasonic temperature is 60°C, and it is cleaned for 240 minutes. , carrying out solid-liquid separation by vacuum filtration to obtain a purified solid;

[0027] (3) Vacuum-dry the purified solid obtained in step...

Embodiment 2

[0028] Example 2 Separation of crude polyphenylene sulfide to obtain separation product A2

[0029] (1) Ultrasonic high-frequency pre-cleaning: Add 3.5 kg of crude polyphenylene sulfide to an ultrasonic cleaning tank filled with 10 liters of N-methylpyrrolidone solvent and 0.005 liter of hexamethylphosphoric triamide solvent for cleaning. The ultrasonic temperature is 200KHz, and the ultrasonic temperature is 200°C. After cleaning for 120 minutes, the solid-liquid separation is carried out by rotary evaporation to obtain the pretreated solid;

[0030] (2) Ultrasonic low-frequency cleaning and purification: put the pretreated solid obtained in step (1) into an ultrasonic cleaning tank equipped with 10 liters of deionized water, the ultrasonic frequency is 20KHz, the ultrasonic temperature is 60°C, and it is cleaned for 240 minutes. , carrying out solid-liquid separation by vacuum filtration to obtain a purified solid;

[0031] (3) Vacuum-dry the purified solid obtained in step...

Embodiment 3

[0032] Example 3 Separation of crude polyphenylene sulfide to obtain isolated product A3

[0033] (1) Ultrasonic high-frequency pre-cleaning: Add 3.5 kg of crude polyphenylene sulfide into an ultrasonic cleaning tank filled with 10 liters of N-methylpyrrolidone solvent and 0.01 liter of hexamethylphosphoric triamide solvent for cleaning. The ultrasonic temperature is 200KHz, and the ultrasonic temperature is 200°C. After cleaning for 120 minutes, the solid-liquid separation is carried out by rotary evaporation to obtain the pretreated solid;

[0034] (2) Ultrasonic low-frequency cleaning and purification: put the pretreated solid obtained in step (1) into an ultrasonic cleaning tank equipped with 10 liters of deionized water, the ultrasonic frequency is 20KHz, the ultrasonic temperature is 60°C, and it is cleaned for 240 minutes. , carrying out solid-liquid separation by vacuum filtration to obtain a purified solid;

[0035] (3) Vacuum drying the purified solid obtained in st...

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Abstract

The invention discloses an ultrasonic cleaning and purifying method of polyphenylene sulfide. The method comprises steps as follows: ultrasonic high-frequency pre-cleaning, ultrasonic low-frequency cleaning and purification and vacuum drying. A reasonable high-frequency ultrasonic and low-frequency ultrasonic combined method is adopted, a mixture of an N-methyl pyrrolidone solvent and a hexamethylphosphoramide solvent serves as a high-frequency ultrasonic separation solvent, a crude product of polyphenylene sulfide can be effectively separated, the finished product obtained through separationhas narrow molecular weight distribution and good separation and purification effects, and the method is simple to operate and favorable for large-scale industrial application.

Description

technical field [0001] The invention relates to the field of polyphenylene sulfide purification, in particular to an ultrasonic cleaning and purification method of polyphenylene sulfide. Background technique [0002] Polyphenylene sulfide is widely used in the production of films, fibers and electronic components, such as capacitors, resistors, transistors, diodes, coils, varistors, integrated circuits and large-scale integrated circuits. Sodium sulfide and p-dichlorobenzene are polymerized into crude polyphenylene sulfide by high temperature and high compression in N-methylpyrrolidone solvent. The crude product contains catalyst, small molecular oligomers and a large amount of sodium chloride. The presence of inorganic ionic impurities reduces the electrical insulation performance of polyphenylene sulfide, and it will corrode semiconductors during use, resulting in leakage accidents. The presence of oligomers reduces the strength of the material, and polyphenylene sulfide ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/0281
CPCC08G75/0281
Inventor 杨伟明叶维雪张德明周鸿文
Owner 广东南粤精工精密组件有限公司
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