Method for synthesizing low-color high-purity fiber-grade polyphenylene sulfide resin

A polyphenylene sulfide resin, polyphenylene sulfide technology, applied in the direction of one-component synthetic polymer rayon, fiber chemical characteristics, textiles and papermaking, etc., can solve the problem of poor processing stability and limited polyphenylene sulfide chain growth , polyphenylene sulfide resin color depth and other problems

Active Publication Date: 2013-05-01
CHINA PETROLEUM & CHEM CORP
View PDF2 Cites 29 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Aiming at the deficiencies in the prior art, the present invention proposes a method for preparing high-performance polyphenylene sulfide, which solves the problem of limited polyphenylene sulfide chain growth, and at the same time solves the problem of deep color and poor processing stability of polyphenylene sulfide resin The problem

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for synthesizing low-color high-purity fiber-grade polyphenylene sulfide resin
  • Method for synthesizing low-color high-purity fiber-grade polyphenylene sulfide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The feed is: anhydrous sodium sulfide / p-dichlorobenzene / N-methylpyrrolidone / anhydrous trisodium phosphate=1.52-1.6mol / 1.5mol / 0.5-1.2L / 40g, the air in the autoclave is replaced with nitrogen, and the Inject 0.6-0.1MP nitrogen. Low temperature 160-230°C for 2-4 hours, high temperature 240-280°C for 3-6 hours, 250-300°C feeding for 1-2 hours, 250-300°C for 0.5-2 hours of p-dichlorobenzene capping. Stirring speed 50-150R / Min. After the reaction was completed, it was filtered and washed to obtain a white powder. The white powder is measured by high-temperature gel chromatography to obtain an average molecular weight Mw of 4.4-5.2×10 4 gmol -1 , molecular distribution index 2.4-3.01. The white powder is fused and granulated into milky white granules, and the product yield is 96-98%.

Embodiment 2

[0038] The feeding material is: anhydrous sodium sulfide / p-dichlorobenzene / N-methylpyrrolidone / anhydrous trisodium phosphate=1.5mol / 1.5mol / 0.5-1.2L / 40g, nitrogen replaces the air in the autoclave, and injects into the autoclave 0.6-1MP nitrogen. Low temperature 160-230°C for 2-3 hours, high temperature 240-280°C for 3-6 hours, 250-300°C feeding for 0.5-2 hours, 250-300°C for 0.5-2 hours to end-block dichlorobenzene. Stirring speed 50-150R / Min. After the reaction was completed, it was filtered and washed to obtain a white powder. The white powder is measured by high-temperature gel chromatography to obtain an average molecular weight Mw of 3.0-3.2×10 4 gmol -1 , molecular distribution index 2.3-2.5. The white powder is fused and granulated into milky white granules, and the product yield is 96-97%.

Embodiment 3

[0040] The feed is: anhydrous sodium sulfide / p-dichlorobenzene / N-methylpyrrolidone / anhydrous trisodium phosphate=1.52-1.6mol / 1.5mol / 0.5-1.2L / 40g, the air in the autoclave is replaced with nitrogen, and the Inject 0.5-1MP nitrogen. Low temperature 160-230°C for 2-3 hours, high temperature 240-280°C for 2-6 hours, 250-300°C feeding 1,2,4-trichlorobenzene for 0.5-4 hours, 250-300°C 1,2, 4-Trichlorobenzene capped for 0.5-4 hours. Stirring speed 50-150R / Min. After the reaction was completed, it was filtered and washed to obtain a white powder. The white powder is measured by high-temperature gel chromatography to obtain an average molecular weight Mw of 3.7-4.8×10 4 gmol -1 , molecular distribution index 2.2-2.5. The white powder is fused and granulated into milky white granules, and the product yield is 96-97%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for synthesizing low-color high-purity fiber-grade polyphenylene sulfide resin. According to the invention, sodium sulfide and p-dichlorobenzene are adopted as raw materials; N-methyl pyrrolidone, N,N-dimethyl acetamide, and the like are adopted as solvents; under the existence of a basic salt, through a four-step method comprising pre-polymerization, polymerization, chain extension and end-capping, the high-purity low-color fiber-grade polyphenylene sulfide resin is synthesized. By adjusting process parameters, polyphenylene sulfide average molecular weight and distribution index can be effectively controlled. Also, purification process can be simplified, and metal ion embedding can be reduced. Resin slice color is reduced, resin processing stability is improved, and resin performance is improved.

Description

technical field [0001] The invention belongs to the technical field of material synthesis and relates to a preparation method of fiber-grade high-purity polyphenylene sulfide. Specifically, it is a method for synthesizing high-performance polyphenylene sulfide resin, that is, a method for synthesizing low-color and high-purity fiber-grade polyphenylene sulfide resin. Background technique [0002] Polyphenylene sulfide, the full name is polyphenylene sulfide, the English name is Polyphenylene sulfide, referred to as PPS. The molecular structure of PPS is relatively simple. The main chain is composed of p-phenylene and sulfur atoms. Its chemical structural formula is: [0003] [0004] The rigid benzene ring structure is connected by flexible thioether bonds, so that PPS has excellent heat resistance, flame retardancy, corrosion resistance and balanced mechanical and electrical properties. The lone electron pair on the sulfur atom makes PPS have good compatibility with in...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02D01F6/76C08G75/0254
Inventor 李振环孙绪江程博闻马志忠张春林
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap