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Purification method of N-methyl pyrrolidone for high polymerization degree polyphenylene sulfide synthesis

A technology of methylpyrrolidone and polyphenylene sulfide, which is applied in the field of purification of N-methylpyrrolidone for the synthesis of polyphenylene sulfide with a high degree of polymerization, can solve problems such as unfavorable polymerization and unfavorable PPS chain growth, and achieve easy operation Effect

Inactive Publication Date: 2013-04-03
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reason is that NMP contains hydroxyl and amino compounds, and the active hydrogen and S in hydroxyl and amino 2- Has a strong electrostatic attraction, which is not conducive to Na 2 S and P-DCB aggregation
Secondly, hydroxyl and amino compounds can also react with chlorobenzene at the end of the PPS chain, causing the PPS to be blocked in advance, which is not conducive to the growth of the PPS chain

Method used

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  • Purification method of N-methyl pyrrolidone for high polymerization degree polyphenylene sulfide synthesis

Examples

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Effect test

Embodiment 1

[0029] Add appropriate amount of dehydroxy compound reagent such as Na or K and deaminated compound reagent such as CaCl to NMP 2 Or ZnCl 2 The suspension is reacted at 80-120°C for 5 minutes to 5 hours, and purified NMP is obtained by distillation under reduced pressure, and the performance of NMP is verified by polymerization reaction. The feed is: sodium sulfide / p-dichlorobenzene / NMP / anhydrous trisodium phosphate =1.53mol / 1.5mol / 0.9L / 40g, nitrogen replaces the air in the autoclave, and 0.8MP nitrogen is injected into the autoclave. Reaction at low temperature 160-220°C for 2 hours, reaction at high temperature 250-270°C for 3-4 hours, 250-280°C feeding for 1 hour, 250-280°C p-dichlorobenzene capping for 0.5-1 hour. After the reaction, it was filtered and washed to obtain a white powder. The Mw of the white powder measured by high temperature gel chromatography is 4.2-5.2×10 4 g mol -1 , Molecular distribution index 2.4-3.0.

Embodiment 2

[0031] Add an appropriate amount of anhydrous high-valent metal salt such as AlCl to NMP 3 Or FeCl 3 , The suspension is reacted at a certain temperature of 80-100°C for 5 minutes to 5 hours, and purified NMP is obtained by distillation under reduced pressure. The performance of NMP is verified by polymerization reaction. The feed is: sodium sulfide / p-dichlorobenzene / NMP / trisodium phosphate anhydrous=1.53mol / 1.5mol / 0.9L / 40g, nitrogen replaces the air in the autoclave, and 0.8 is injected into the autoclave MP's nitrogen. React at a low temperature of 160-220°C for 2 hours, at a high temperature of 250-270°C for 3-4 hours, add p-dichlorobenzene at 250-280°C for 1 hour, and block p-dichlorobenzene at 250-280°C for 0.5-1 hours. After the reaction, it was filtered and washed to obtain a white powder. The Mw of white powder measured by high temperature gel chromatography is 3.2-4.1×10 4 g mol -1 , Molecular distribution index 2.2-3.0. The white powder is melted and granulated into...

Embodiment 3

[0033] Add CaH to NMP first 2 After adding TiCl 4 The suspension is reacted at a certain temperature of 80-100°C for 5 minutes to 5 hours, and purified NMP is obtained by distillation under reduced pressure. The performance of NMP is verified by polymerization reaction. The feed is: sodium sulfide / p-dichlorobenzene / NMP / trisodium phosphate anhydrous=1.53mol / 1.5mol / 0.9L / 40g, nitrogen replaces the air in the autoclave, and 0.8 is injected into the autoclave MP's nitrogen. React at a low temperature of 160-220°C for 2 hours, at a high temperature of 250-270°C for 3-4 hours, add p-dichlorobenzene at 250-280°C for 1 hour, and block p-dichlorobenzene at 250-280°C for 0.5-1 hours. After the reaction, it was filtered and washed to obtain a white powder. The white powder Mw measured by high temperature gel chromatography is 3.3-4.8×10 4 g mol -1 , Molecular distribution index 2.0-2.8. The white powder is melted and granulated into milky white particles.

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Abstract

The present invention discloses a purification method of N-methyl pyrrolidone for high polymerization degree polyphenylene sulfide synthesis, wherein NMP purified by the method is suitable for synthesis of high molecular weight PPS (polyphenylene sulfide), and an active metal, a metal hydride, an organic metal compound, an anhydrous salt of a metal and an anhydrous high valence metal compound are adopted to separately or simultaneously remove a small amount of a hydroxy compound and a small amount of an amino compound from the NMP solution so as to promote high molecular weight PPS synthesis. The purification method has characteristics of simpleness, easy performing and convenient operation, wherein the obtained product completely meet the high molecular weight PPS synthesis.

Description

Technical field [0001] The present invention belongs to a method involving the purification of NMP (N-methylpyrrolidone). In particular, it relates to a purification method of N-methylpyrrolidone for synthesizing high polymerization degree polyphenylene sulfide. Background technique [0002] PPS has a high melting point of 280~290℃, a high decomposition temperature of 400℃, a symmetrical molecular structure, good electrical properties, no water absorption, no polarity and easy crystallization. PPS has excellent radiation resistance, corrosion resistance, high temperature resistance, electrical properties, and balanced mechanical properties and flame retardant properties. PPS has a wide range of uses, mainly used in high-tech fields such as environmental protection, automobiles, textiles, military industry, electronics and electrical appliances, machinery industry, and aerospace. It is regarded as one of the key materials necessary for the development of high-tech in the United S...

Claims

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Application Information

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IPC IPC(8): C07D207/267C08G75/02C08G75/0254
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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