Green high-purity polyarylether and preparation method thereof

A high-purity polyarylether technology, applied in the production of bulk chemicals, can solve problems such as dark color, impure resin, and long process flow

Active Publication Date: 2020-05-05
成都锦颜科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the main production method of polyarylether is: using auxiliary agent, nucleophile (such as diphenol compound or sulfide), dihalogenated aromatic compound and polar solvent as raw materials, carrying out solution polycondensation, and reacting the reaction mixture For solid-liquid separation, the crude resin product is purified by water washing, the process is long, and the water consumption in this process is large, and the subsequent solvent is generally recovered by distillation and separation, resulting in high energy consumption in the subsequent solvent recovery process , and the purity of the recovered solvent is not high; the solvent wrapped in the resin has high volatile content, and the resin is impure, which will make the resin processed into products dark in color, produce cells or defects, and affect the overall performance of the final

Method used

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  • Green high-purity polyarylether and preparation method thereof
  • Green high-purity polyarylether and preparation method thereof
  • Green high-purity polyarylether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 10kg lithium hydroxide, 20kg potassium acetate, 500kg 1,3-dimethyl-2-imidazolinone and 178kg hydrous sodium sulfide were dehydrated at 220°C for 0.5h under the protection of nitrogen to obtain a dehydrated reaction solution , when the temperature of the above solution drops to 180°C, add 114kg of p-difluorobenzene, react at a temperature of 230°C for 1h, then keep at a temperature of 280°C for 10h, cool down to 200°C, perform a high-temperature filtration, and recover the part in the reaction slurry solvent, and transported to the solvent recovery tank; continue to cool the reactor to 160 ° C, close all inlet and outlet valves in the reactor, open the supercritical extraction agent feed valve, switch the reactor mode to the extraction tank mode, and feed the extraction tank respectively Add 500kg of supercritical extractant trifluoromethane three times each time, extract the remaining reaction solvent at a temperature of 30°C and a pressure of 5MPa, and then send the ext...

Embodiment 2

[0060] 100kg of sodium carbonate, 120kg of sodium alginate, 1000kg of hexamethylphosphoric triamide and 186kg of biphenyldiphenol were dehydrated at a temperature of 210°C for 1 hour under the protection of nitrogen to obtain a dehydrated reaction solution. When the temperature reaches 120°C, add 254kg of 4,4'-difluorodiphenyl sulfone, react at 240°C for 1 hour, then keep at 270°C for 8 hours, cool down to 220°C, perform a high-temperature closed flash evaporation, and recover the part in the reaction slurry solvent, and transported to the solvent recovery tank; continue to cool the reactor to 130 ° C, close all inlet and outlet valves in the reactor, open the supercritical extraction agent feed valve, switch the reactor mode to the extraction tank mode, and feed the Add 800kg of supercritical extractant sulfur hexafluoride in 5 times each time, extract the remaining reaction solvent at a temperature of 50°C and a pressure of 4MPa, and then send the extracted mixed supercritica...

Embodiment 3

[0063] 200kg of potassium bicarbonate, 80kg of sodium adipate, 2000kg of N-cyclohexylpyrrolidone and 127kg of aqueous sodium hydrosulfide were dehydrated at a temperature of 180°C for 3 hours under the protection of nitrogen to obtain a dehydrated reaction solution. When the temperature reaches 160°C, add 287kg of 4,4'-dichlorodiphenylsulfone, react at a temperature of 190°C for 6 hours, then keep at a temperature of 230°C for 6 hours, cool down to 210°C, perform a high-temperature closed flash evaporation, and recover the reaction slurry part of the solvent, and sent to the solvent recovery tank; continue to cool the reactor to 30 ° C, close all the inlet and outlet valves in the reactor, open the supercritical extraction agent feed valve, switch the reactor mode to the extraction tank mode, respectively The kettle is divided into 6 times, each time adding 500kg of supercritical extractant carbon dioxide, and the remaining reaction solvent is extracted at a temperature of 32°C...

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Abstract

The invention relates to a green high-purity polyarylether and a preparation method thereof, and belongs to the field of polymer synthesis. A initial raw material of the green high-purity polyarylether is composed of the following components in parts by weight: 56 to 324 parts of a diphenol compound or a sulfide, 114 to 577 parts of a dihalogenated aromatic compound, 400 to 5000 parts of a solvent, 0.1 to 300 parts of an auxiliary agent, 500 to 5000 parts of a supercritical extraction agent and 300 to 3000 parts of an auxiliary agent leaching agent; the green high-purity polyarylether is prepared by the following preparation method: 1) carrying out dehydration reaction; 2) recovering the solvent for the first time through high-temperature filtration or high-temperature closed flash evaporation; 3) carrying out supercritical extraction to recovery the solvent; and 4) carrying out auxiliary agent recovery and separation. The purity of the obtained polyarylether is more than or equal to 99.9%, the whiteness is more than or equal to 75, the impurity content is less than or equal to 20 ppm, the complete recycling of the solvent and the auxiliary agent is achieved in the whole preparation process, and the method is green and environmentally friendly.

Description

technical field [0001] The invention relates to a green, high-purity polyarylether and a preparation method thereof, belonging to the field of polymer synthesis. Background technique [0002] Polyarylene ether mainly includes polyarylene sulfide such as polyphenylene sulfide, polyphenylene sulfide ester, polyphenylene sulfide ketone, polyphenylene sulfide sulfone, polyphenylene sulfide amide, polyphenylene ether sulfide, polyphenylene sulfide acyl Imine; polyphenylene oxide, polyether sulfone, polyether ketone, polyether ether ketone, polyether ether ketone ketone, polyaryletheramide, polyaryletherimide, due to its corrosion resistance, high temperature and excellent electrical properties, Mechanical properties and dimensional stability are widely used in aerospace and electronic technology. Among them, the main production method of polyarylether is: using auxiliary agent, nucleophile (such as diphenol compound or sulfide), dihalogenated aromatic compound and polar solvent ...

Claims

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Application Information

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IPC IPC(8): C08G65/40C08G65/46
CPCC08G65/4006C08G65/40C08G65/4056C08G65/4068C08G65/4037C08G65/46Y02P20/54
Inventor 宋颖琦其他发明人请求不公开姓名
Owner 成都锦颜科技有限公司
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