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Preparation method of polyether-ether-ketone

A technology of polyether ether ketone and difluorobenzophenone, which is applied in the field of polymer material preparation, can solve problems such as unfavorable reaction and carbon dioxide is not conducive to the environment, and achieve the effects of shortening reaction time, easy control of reaction temperature and high purity

Inactive Publication Date: 2017-02-22
枣阳市华威硅氟材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of them use 4,4'-difluorobenzophenone and hydroquinone as raw materials to prepare polyether ether ketone by solution polycondensation reaction in the presence of a large amount of sodium carbonate. The reaction temperature often exceeds 320 ° C, and the excess Carbonate is not only not conducive to the reaction, but the reaction produces a large amount of carbon dioxide and is not conducive to the environment

Method used

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Examples

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preparation example Construction

[0020] The invention discloses a preparation method of polyether ether ketone, comprising the following steps:

[0021] Step 1: In the reaction kettle equipped with a stirrer, thermometer, reflux condenser and nitrogen pipe, feed nitrogen, then add solvent to stir and heat up to 140-160 ° C, and then add hydroquinone and sodium hydroxide Stir continuously with potassium carbonate, after all dissolve, add 4,4'-difluorobenzophenone and water-carrying agent, continue to stir and react, take out the water generated by the reaction, continue to heat up to release the water-carrying agent, and then Continue to heat up to 220-260°C, react for 2-4h;

[0022] Step 2: Continue stirring to raise the temperature to 300-310°C, add 3,4-difluorobenzophenone or 3-chloro-4-fluorobenzophenone, and then react for 10-20 minutes to obtain polymerized mucus;

[0023] Step 3: Pour the polymerized mucus into deionized water quickly, and stir quickly to obtain crude polyether ether ketone particles, ...

Embodiment 1

[0032] In the reaction kettle equipped with a stirrer, thermometer, reflux condenser and nitrogen pipe, feed nitrogen, then add 65.4g diphenyl sulfone to stir and raise the temperature to 140°C, and then add 11.2g hydroquinone, 6.2g Sodium hydroxide and 6.9g of potassium carbonate were continuously stirred. After they were completely dissolved, 21.8g of 4,4'-difluorobenzophenone and 150ml of toluene were added, and the reaction was continuously stirred. Toluene, then continue to heat up to 220°C, react for 2.5h; continue to stir and heat up to 300°C, add 0.3g 3,4'difluorobenzophenone, and then react for 15min to obtain polymerized slime; quickly pour the polymerized slime into deionized water, and stirred rapidly to obtain the crude polyether ether ketone particles, filtered and crushed, wrapped in a degreased filter paper bag, put into the extraction tube of the extractor, added hot methanol, kept the pressure in the range of 0.3Mpa, heated to boiling, and kept the temperature...

Embodiment 2

[0034] In the reaction kettle equipped with a stirrer, thermometer, reflux condenser and nitrogen pipe, nitrogen was introduced, then 36.0g of sulfolane was added to stir and the temperature was raised to 160°C, and then 11.0g of hydroquinone and 6.0g of hydrogen peroxide were added. Sodium and 13.8g Potassium Carbonate >Continue to stir, after all dissolved, add 24.0g 4,4'-difluorobenzophenone and 150ml xylene, continue to stir the reaction, take out the water generated by the reaction, continue to heat up Release xylene, continue to heat up to 240°C, and react for 3 hours; continue to stir and heat up to 310°C, add 0.25g of 3-chloro-4-fluorobenzophenone, and then react for 20min to obtain polymerized mucus; quickly pour the polymerized mucus into In deionized water, stir rapidly to obtain crude polyether ether ketone particles, filter and pulverize them, wrap them in a degreased filter paper bag, put them into the extraction tube of the extractor, add hot methanol, keep the p...

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PUM

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Abstract

The invention provides a preparation method of polyether-ether-ketone. The method comprises the following steps that in a reaction kettle, nitrogen is introduced, then, a solvent is added for stirring and heating, hydroquinone, sodium hydroxide and potassium carbonate are added to continue to be stirred, then, 4,4'-difluorobenzophenone and a water-carrying agent are added, after water generated by the reaction is completely carried out, continuous heating is performed to discharge the water-carrying agent, stirring and heating are performed continuously, 3,4-difluorobenzophenone or 3-chlorin-4-fluorinated diphenyl ketones is added, and a reaction is performed to obtain a polymerized mucus; the polymerized mucus is poured into deionized water, rapid stirring is performed to obtain crude polyether-ether-ketone particles, filtering and smashing are performed, and after extraction and washing are performed inside an extractor, vacuum drying is performed to obtain the polyether-ether-ketone. According to the method, the reaction time is shortened, discharge of carbon dioxide is reduced, the subsection charging mode is adopted, the reaction temperature is easier to control, energy conservation and consumption reduction are promoted, and an end-capping agent is added before the polymerization reaction is ended, so that the thermal stability of the polyether-ether-ketone is improved.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, and in particular relates to a preparation method of polyether ether ketone. Background technique [0002] Polyetheretherketone is an aromatic linear polymer material with physical and chemical properties such as high temperature resistance and chemical corrosion resistance, and is widely used in many fields. Most of them use 4,4'-difluorobenzophenone and hydroquinone as raw materials to prepare polyether ether ketone by solution polycondensation reaction in the presence of a large amount of sodium carbonate. The reaction temperature often exceeds 320 ° C, and the excess Carbonate is not only not conducive to the reaction, but the reaction produces a large amount of carbon dioxide and is not conducive to the environment. In addition, if no capping monomer is added to the reaction end, then polyetheretherketone is fluorine-terminated or phenol-terminated. In order to further improve th...

Claims

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Application Information

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IPC IPC(8): C08G8/02
CPCC08G8/02
Inventor 文建强
Owner 枣阳市华威硅氟材料有限公司