Polymerization process for fiber-grade polyphenyl thioether production process

A technology of polyphenylene sulfide and polymerization technology, applied in the field of polymerization technology, can solve the problems of increasing industrial production cost, reducing solvent recovery efficiency, difficult to control molecular weight, etc., and achieves the effects of reducing energy consumption, easy process control, and reducing reaction time

Inactive Publication Date: 2009-07-08
JIANGSU XINZHONG INVESTMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the polymerization process in the above production process are: long reaction time, difficult to control the molecular weight, and the increase of the high temperature time period will intensify the hydrolysis of the solvent, reduce the efficiency of solvent recovery, and increase the cost of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] 180L stainless steel reaction kettle, add solvent NMP40.0kg, aqueous sodium sulfide 23.40kg, catalyst 3.00kg, heat up and dehydrate; after dehydration, add 60.0kg solvent NMP into the reaction kettle, add p-dichlorobenzene 22.15kg after the temperature is stable, Turn on the heating device, start from 170°C at an average heating rate of 0.4°C / min to 285°C to stop the polymerization reaction, cool down and discharge the material, and enter the post-processing stage; during the polymerization process, the pressure is finally raised from 0MPa to 0.8MPa, and the process is stable and automatic It takes about 6.5 hours from the feeding to the end of feeding, including 30 minutes of feeding, 2 hours of dehydration, and 4 hours of polymerization. The product PPS is a white granular dense solid with a molecular weight of 5.5×10 4 about.

Embodiment 2

[0012] 180L stainless steel reaction kettle, add solvent NMP40.0kg, aqueous sodium sulfide 23.40kg, catalyst 3.00kg, heat up and dehydrate; after dehydration, add 60.0kg solvent NMP into the reaction kettle, add p-dichlorobenzene 22.35kg after the temperature is stable, Turn on the heating device, start from 175°C at an average heating rate of 0.3°C / min to 272°C to stop the reaction, cool down and discharge the material, and enter the post-processing stage; during the polymerization process, the pressure rises from 0MPa to 0.75MPa, the process is stable, and the material is fed automatically A total of 7.5 hours from the start to the end of the discharge, including feeding for 30 minutes, dehydration for 2 hours, and polymerization for 5 hours, the product PPS is a white granular solid with a molecular weight of 6.0×10 4 about.

Embodiment 3

[0014] 180L stainless steel reaction kettle, add 28.0kg of solvent NMP, 15.60kg of aqueous sodium sulfide, and 1.50kg of catalyst, heat up and dehydrate; The heating device starts from 185°C at an average heating rate of 0.3°C / min to 275°C to stop the reaction, cools down and discharges the material, and enters the post-processing stage; during the polymerization process, the pressure rises from 0MPa to 0.65MPa, and the process is stable. A total of 7.5 hours until the end of feeding, wherein feeding 30 minutes, dehydration 2 hours, polymerization 5 hours, the product PPS is a white granular dense solid, the molecular weight of 6.0 × 10 through preliminary determination 4 about.

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Abstract

The invention discloses a polymerization process during the production of fiber-grade polyphenylene sulfide with simple operation, easily controlled reaction condition, ideal repeatability, short reaction time and reasonable energy consumption. The polymerization process is characterized in that during polymerization reaction of raw materials in a reaction kettle, a continuous heating-up mode is adopted for the reaction kettle and the heating-up speed is controlled between 0.3 and 0.6 DEG C per minute; when the reaction kettle is heated up from a range between 165 and 185 DEG C to another range between 245 and 295 DEG C, the polymerization reaction is finished. PPS products prepared by the method have stable quality and excellent performance and can meet the requirements of fiber-grade PPS resin.

Description

technical field [0001] The present invention relates to the production process of producing fiber-grade polyphenylene sulfide with p-dichlorobenzene and sodium sulfide as main raw materials, in particular to the polymerization process in the production process. Background technique [0002] Polyphenylene sulfide (PPS for short) is a new type of high-performance thermoplastic resin with excellent thermal stability, chemical stability, corrosion resistance and electrical properties. It has a wide range of applications in industry, food, etc., and has a broad market prospect. At present, there are mainly two types of polyphenylene sulfide resin products: linear type and cross-linked type. Only linear polyphenylene sulfide resin with high molecular weight and high purity can be used as PPS fiber raw material. The synthesis research of PPS has a history of many years, and a variety of synthesis methods have been developed, but there is only one method for realizing large-scale i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02D01F6/76C08G75/0254
Inventor 陈松张建新丁元尹航胡晓霞
Owner JIANGSU XINZHONG INVESTMENT
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