Environment-friendly economical polyarylether and preparation method thereof

An economical technology of polyarylether, which is applied in the field of environmentally friendly and economical polyarylether and its preparation, can solve the problems of difficult ultra-large-scale industrial scale-up, low catalyst recovery rate, high production cost, etc., and reduce energy consumption , Reduce the frequency of solvent recovery, the effect of high molecular weight

Active Publication Date: 2016-09-28
安徽旭云商务咨询有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main process and method in the industrial production of polyarylethers: using additives, sulfides or oxygen-containing compounds and dihalogenated aromatic compounds for high temperature and high pressure solution polycondensation in polar organic solvents, after the reaction, the used additives and extreme Rectification and recovery of non-toxic organic solvents for subsequent recycling, this method requires a lot of heat in the process of rectification and purification of solvents, high energy consumption and high cost, and the separation and recovery of catalysts involved also have similar problems, namely energy consumption At the same time, due to the high solubility of the catalyst in the solvent, the recovery rate of the catalyst is not high, which leads to the high production cost of polyarylether products for a long time, and it is difficult for large-scale industrial scale-up

Method used

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  • Environment-friendly economical polyarylether and preparation method thereof
  • Environment-friendly economical polyarylether and preparation method thereof
  • Environment-friendly economical polyarylether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]1kg of lithium acetate, 0.1kg of sodium hydroxide, 500kg of the reaction filtrate (mixed solution of hexamethylphosphoric triamide and catalyst) used in the last preparation of polyphenylene sulfide and 130kg of sodium sulfide with a water content of 40% were added to the reaction In the kettle, under the protection of nitrogen, dehydrate at a temperature of 200°C for 2 hours to obtain a dehydrated reaction solution. When the temperature of the above solution drops to 160°C, add 147kg of p-dichlorobenzene and react at a temperature of 230°C for 3 hours. Keep at ℃ for 1h, cool down to 90℃, filter the reaction solution, add 0.1kg18-crown-6 to the filtered liquid to precipitate the dissolved metal salt in the filtrate, and then remove the precipitated precipitate by filtration to obtain the second filtration Liquid, add 0.1kg polyferric chloride in the filtrate for the second time to precipitate the oligomers in the filtrate, separate the oligomers and the liquid by centrifu...

Embodiment 2

[0045] Add 0.2kg sodium tartrate, 5kg potassium hydroxide, 1200kg of the reaction filtrate (N-cyclohexylpyrrolidone and catalyst mixed solution) and 82.4kg of sodium hydrosulfide with a water content of 32% after the polyphenylene sulfide ketone was prepared last time In the reaction kettle, under the protection of nitrogen, dehydration reaction was carried out at a temperature of 185°C for 1.5h to obtain a dehydrated reaction solution. When the temperature of the above solution dropped to 160°C, 218kg of 4,4'-difluorobenzophenone was added to the React at a temperature of 205°C for 2 hours, keep at a temperature of 270°C for 3 hours, cool down to 100°C, filter the reaction solution, add 0.1kg of polyvinyl alcohol to the filtered liquid to precipitate the dissolved metal salt in the filtrate, and then remove the precipitate Remove by filtration, obtain the filtrate for the second time, add 0.2kg ammonium polyphosphate in the filtrate for the second time to precipitate the oligo...

Embodiment 3

[0047] With 0.5kg lithium phosphate, 12kg magnesium hydroxide, the reaction filtrate (N-methyl caprolactam and catalyst mixed solution) and the sodium sulfide 130kg of 40% that 1800kg prepare semiaromatic polyphenylene sulfide amide last time use Put it into the reaction kettle, and under the protection of nitrogen, dehydrate at a temperature of 195°C for 2 hours to obtain a dehydrated reaction solution. When the temperature of the above solution drops to 120°C, add 360kg of 1,6-bis(4-fluorobenzoyl) Hexamethylenediamine, react at a temperature of 200°C for 2h, keep at a temperature of 235°C for 6h, cool down to 90°C, filter the reaction solution, add 0.5kg polydopamine to the filtered liquid to precipitate the dissolved metal salt in the filtrate, and then Remove the precipitated precipitate by filtration to obtain the second filtrate, add 0.1kg polyacrylamide to the second filtrate to precipitate oligomers in the filtrate, and separate the precipitated oligomers and liquid by ...

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Abstract

The invention discloses an environment-friendly economical polyarylether and a preparation method thereof. The method is characterized by comprising the following steps: adding 0-5 parts of catalyst, 0.1-100 parts of alkali, 1000-3000 parts of solvent and 56-250 parts of sulfide or oxygen-containing compound into a reaction kettle, carrying out dehydration reaction at 150-230 DEG C in a nitrogen protective atmosphere for 0.5-2 hours to obtain a dehydrated reaction solution, cooling the solution to 80-160 DEG C, adding 114-467 parts of dihalogenated aromatic compound, reacting at 160-260 DEG C for 0.5-6 hours, keeping at the temperature of 180-280 DEG C for 0.5-10 hours, cooling to 50-100 DEG C, filtering the reaction solution, adding 0.1-5 parts of chelator into the filtrate to remove metal salts so as to obtain a secondary filtrate, adding 0.1-2 parts of flocculant into the filtrate, and centrifugating the precipitated low polymer and liquid to obtain a tertiary centrifugate; and washing the solid resin with desalted water 4-8 times (600-1000 parts each time) to remove impurities in the product, and drying at 80-120 DEG C under the vacuum degree of 0.03-0.095MPa for 1-10 hours, thereby obtaining the purified polyarylether resin.

Description

technical field [0001] The invention relates to an environment-friendly and economical polyarylether and a preparation method thereof, belonging to the field of polymer synthesis. Background technique [0002] Polyarylene ether mainly includes polyethersulfone (PES), polyether ether ketone (PEEK), polyarylether amide (PAEA), polyphenylene sulfide (PPS), polyphenylene sulfide ketone (PASK), polyarylene sulfide sulfone (PASS), polyarylene sulfide amide (PASA), polyarylene ether sulfide (PAES), because of its high temperature resistance, corrosion resistance, excellent electrical properties, mechanical properties and dimensional stability, are widely used in automobiles, aerospace and electronic technology. The main process and method in the industrial production of polyarylether: using auxiliary agents, sulfides or oxygen-containing compounds and dihalogenated aromatic compounds for high-temperature and high-pressure solution polycondensation in polar organic solvents, after ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0254C08G75/0259C08G75/025C08G65/40
CPCC08G65/4006C08G65/4025C08G75/0254C08G75/0259C08G75/0272
Inventor 张刚杨杰任浩浩王孝军龙盛如严永刚
Owner 安徽旭云商务咨询有限公司
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