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Method for synthesizing polyphenylene sulfide copolymer containing heteroaromatics

A technology of polyphenylene sulfide and synthesis method, applied in the field of polymer material resin production, can solve problems such as unseen process introduction and the like

Active Publication Date: 2008-06-18
四川中科兴业高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] As far as the existing polyphenylene sulfide synthesis technology is concerned, the synthesis of polyphenylene sulfide resin generally uses sodium sulfide and p-dichlorobenzene (P-DCB) as raw materials, although the American Phillips company and Japanese polyphenylene sulfide resin The polyphenylene sulfide resin produced by the production company has basically not changed much in the raw materials, so the molecular structure of the polymer has not been changed, but there is no specific process introduction for the copolymer blended with other dihalogenated compounds

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In the autoclave, 12 kilograms of N-methyl-2 pyrrolidone (NMP) is a solvent, and sodium sulfide (Na 2 S.3H 2(0) 4.2 kilograms, 0.01 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, while stirring, heat up, rise to 203 ℃ dehydration with the time of 2 hours, add 2.49 kilograms of p-dichlorobenzene, NMP 2 kg, at a temperature of 200 ° C for 3 hours, then add 2.99 kg of 2-(4-chlorophenyl)-5-chlorobenzimidazole (abbreviated DCPBI), so that sodium sulfide and p-dichlorobenzene and 2- The molar ratio of (4-chlorophenyl)-5-chlorobenzimidazole is 1:0.6:0.4. When the temperature is 280°C, react for 4 hours, and under the condition of this temperature, add 0.036 kg of p-chloroaminobenzene, cool to 185°C after 2 hours of polymerization, add 0.046 kg of terephthalic acid, and then heat up to 250°C After treatment for 1 hour, cool to 200°C and add 0.008 kg of deionizing agent mixture ethylenediaminetetraacetic acid, and keep stirring ...

Embodiment 2

[0029] In the autoclave, add 12 kilograms of N-methyl-2 pyrrolidone (NMP), sodium sulfide (Na 2 S.3H 2 (0) 4.3 kilograms, 0.01 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, while stirring, heat up, rise to 190 ℃ dehydration with the time of 8 hours, add p-dichlorobenzene 3.66 kilograms, NMP 2 kg, at a temperature of 280 ° C for 1 hour, then add 0.75 kg of 2-(4-chlorophenyl)-5-chlorobenzimidazole, so that sodium sulfide and p-dichlorobenzene and 2-(4-chlorobenzene The molar ratio of (phenyl)-5-chlorobenzimidazole is 1:0.9:0.1. When the temperature is 280°C, react for 6 hours, and under the condition of this temperature, add 0.178 kg of p-chloroaminobenzene, cool to 185°C after 2 hours of polymerization, add 0.15 kg of terephthalic acid, and then heat up to 250°C After 1 hour of treatment, cool to 100°C, add 0.108 kg of deionizing agent mixture ethylenediaminetetraacetic acid, and keep stirring for 1 hour, filter at 100°C and c...

example 3

[0031] In the autoclave, add 12 kilograms of N-methyl-2 pyrrolidone (NMP), sodium sulfide (Na 2 S.3H 2 (0) 4.2 kilograms, 0.01 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, while stirring, heat up, rise to 203 ℃ dehydration with the time of 2 hours, add 2.49 kilograms of p-dichlorobenzene, NMP 2 kg, at a temperature of 200 ° C for 3 hours, then add 2.99 kg of 2-(4-chlorophenyl)-5-chlorobenzimidazole, so that sodium sulfide and p-dichlorobenzene and 2-(4-chlorobenzene The molar ratio of (phenyl)-5-chlorobenzimidazole is 1:0.6:0.4. When the temperature is 280°C, react for 4 hours, and under the condition of this temperature, add 0.178 kg of p-chloroaminobenzene, cool to 185°C after 2 hours of polymerization, add 0.15 kg of terephthalic acid and then heat up to 250°C After treatment for 1 hour, cool to 200°C and add 0.108 kg of deionizing agent mixture ethylenediaminetetraacetic acid, and keep stirring for 1 hour, cool to 100°C ...

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PUM

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Abstract

The present invention discloses a synthetic method of heteroaromatics polyphenyl sulfur ether. The present invention adopts sodium sulfide and paradichlorobenzene and 2-(4-chlorine phenyl group)-5-chlorine phenyl benzimidazole as raw materials and N-methyl-2 pyrrolidone as solvent for condensation and polymerization under the role of alkali metal lacquer solvent, so as to produce the polyphenyl sulfur ether resin. The mol ratio between sodium sulfide and paradichlorobenzene and 2-(4-chlorine phenyl group)-5-chlorine phenyl benzimidazole is 1:0.6-0.9:0.4-0.1. The sequential process mainly includes: in the process of sodium sulfide dehydration stage, assistant lithium aluminum hydride is added; in the condensation and polymerization stage, 2-(4-chlorine phenyl group)-5-chlorine phenyl benzimidazole is added. The product provided by the present invention with excellent indexes of relatively low dispersion coefficient and narrow molecular weight distribution and oxygen index can be made into paint, injection mold, fiber and membrane and be widely applied to the fields of machinery, chemicals, oil, electronic apparatus, war industry and airspace.

Description

technical field [0001] The invention belongs to the field of polymer material resin production. Background technique [0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardancy, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from all over the world have been working hard to find it. [0003] Chinese patent CN200510022437.6 discloses a process method of fiber-grade polyphenylene sulfide resin, using sodium sulfide and p-dichlorobenzene (P-DCB) as raw materials, polycondensation under the action of an alkali metal catalyst to produce polyphenylene sulfide (PPS) ) monomer, using the following process flow and conditions: adding additive sodium borohydride in the dehydration stage; adding nitrodichlorobenzene or p-chlorobenzylamine in the polycondensation stage; finally adding regulator adipic acid. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0213C08G75/0222C08G75/0227C08G75/0254
Inventor 陈逊
Owner 四川中科兴业高新材料有限公司
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