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

A technology of p-dichlorobenzene and polyphenylene sulfide, which is applied in the field of purification of p-dichlorobenzene for the synthesis of polyphenylene sulfide with a high degree of polymerization, can solve the problems of PPS resin performance degradation and unfavorable PPS resin synthesis, and achieve easy operation Effect

Active Publication Date: 2015-04-22
CHINA PETROLEUM & CHEM CORP
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  • 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

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  • 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...

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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

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Application Information

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Patent Type & Authority Patents(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
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