Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Purification method of para-dichlorobenzene for high polymerization degree polyphenylene sulfide synthesis

A technology for p-dichlorobenzene and polyphenylene sulfide, which is applied in the field of purifying p-dichlorobenzene for synthesizing high-degree-of-polymerization polyphenylene sulfide, can solve the problems of decreased performance of PPS resin, unfavorable synthesis of PPS resin, and the like, and achieves easy operation. Effect

Active Publication Date: 2013-04-03
CHINA PETROLEUM & CHEM CORP
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The research results show that monochlorobenzene and o-dichlorobenzene in p-dichlorobenzene are the important reasons for the premature end-capping of PPS, and the existence of monochlorobenzene and o-dichlorobenzene is not conducive to the synthesis of higher molecular weight PPS resin
Secondly, the low-molecular-weight PPS generated by the end-capping of monochlorobenzene and o-dichlorobenzene is difficult to separate from the resin, resulting in a decrease in the performance of the PPS resin. Therefore, it is necessary to purify p-dichlorobenzene in order to synthesize a PPS resin with good performance.

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
  • Purification method of para-dichlorobenzene for high polymerization degree polyphenylene sulfide synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Melt p-dichlorobenzene, then add 0.2-1% concentrated sulfuric acid or fuming sulfuric acid with moles of p-dichlorobenzene to the molten p-dichlorobenzene, sulfonate at 40-100°C for 10-30 minutes, then distill off monochlorobenzene and part of o-dichlorobenzene to obtain high-purity p-dichlorobenzene A1 suitable for the synthesis of polymer PPS resin.

Embodiment 2

[0034] Melt p-dichlorobenzene, then add 0.2-1% concentrated nitric acid with moles of p-dichlorobenzene to the molten p-dichlorobenzene, nitrate at 80-120°C for 10-30 minutes, distill off monochlorobenzene and some ortho-dichlorobenzene to obtain high-purity p-dichlorobenzene A2 suitable for the synthesis of polymer PPS resins.

Embodiment 3

[0036] Melt p-dichlorobenzene, then add 0.2-1% concentrated nitric acid and an appropriate amount of concentrated sulfuric acid to the p-dichlorobenzene molten liquid, nitrate at 80-120°C for 10-30 minutes, and distill off a Chlorobenzene and part of ortho-dichlorobenzene to obtain high-purity p-dichlorobenzene A3 suitable for the synthesis of polymer PPS resin.

[0037] The purification effect was verified by the performance characterization after the synthesis of PPS.

[0038] The synthesis method is: add 1.5mol of untreated industrial grade p-dichlorobenzene A0 and purified p-dichlorobenzene A1, A2, A3 into the kettle, add 1.53mol of sodium sulfide, 0.9L of N-methylpyrrolidone, anhydrous Trisodium phosphate 40g, the air in the nitrogen replacement still, and inject the nitrogen of 0.8MP in the autoclave. Reaction at low temperature 160-220°C for 2 hours, high temperature at 250-280°C for 3-4 hours, continuous addition of p-dichlorobenzene at 250-280°C for 0.5-1 hour, addin...

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

PropertyMeasurementUnit
decomposition temperatureaaaaaaaaaa
Login to View More

Abstract

The present invention discloses a purification method of para-dichlorobenzene for high polymerization degree polyphenylene sulfide synthesis, wherein the purified para-dichlorobenzene is applicable for synthesis of high molecular weight polyphenylene sulfide (PPS). Usually the para-dichlorobenzene contains monochlorobenzene and o-dichlorobenzene, and the presence of the monochlorobenzene and the o-dichlorobenzene causes end capping of a polymer in advance, such that polymerization degree increase is not easily achieved. According to the method, an appropriate amount of at least one of a sulfonating agent and a nitrating agent is introduced to sulfonate or nitrate the extreme small amount of the monochlorobenzene and the o-dichlorobenzene, and a distillation method is adopted to obtain the purified para-dichlorobenzene. The method has characteristics of simpleness, easy performing and convenient operation, wherein the obtained product can completely meet high molecular weight PPS synthesis.

Description

technical field [0001] The invention belongs to a method for purifying p-dichlorobenzene. In particular, it relates to a method for purifying p-dichlorobenzene for synthesizing polyphenylene sulfide with a high degree of polymerization. Background technique [0002] Polyphenylene sulfide, referred to as PPS, is a thermoplastic resin whose molecular main chain is composed of p-phenylene and sulfur atoms. It is known as polycarbonate (PC), polyester (PET), polyoxymethylene (POM), nylon (PA) and polyphenylene oxide (PPO), the sixth largest general-purpose engineering plastic, and one of the eight major aerospace materials. PPS has a higher melting point of 280-290°C, a higher decomposition temperature of 400°C, a symmetrical molecular structure, good electrical properties, no water absorption, non-polarity and easy crystallization. PPS has excellent radiation resistance, corrosion resistance, high temperature resistance, electrical properties, and balanced mechanical properti...

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): C07C25/08C07C17/395C07C17/383
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 Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com