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Process for purifying polyether ketone ketone crude product by chelating agent

A technology of polyether ketone ketone crude product and polyether ketone ketone, which is applied in the field of purification of polyether ketone ketone crude product, can solve the problems of polyether ketone ketone viscosity decrease, product structure change, molecular weight decrease, etc., and achieve low cost and process energy saving Environmentally friendly and less toxic

Active Publication Date: 2018-07-13
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrophilic substitution reaction method generally adopts the Friedel-Crafts reaction synthesis with anhydrous aluminum chloride as a catalyst. The crude polyether ketone ketone synthesized has relatively high residual aluminum ions, which reduces the viscosity and molecular weight of the polyether ketone ketone. Changes in product structure lead to more side reactions when using subsequent processed polymers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 500 g of ethylenediamine di-o-phenylacetic acid aqueous solution with a mass concentration of 20% was added thereto, refluxed and stirred at 100° C. for 6 hours, cooled, and filtered to obtain a primary purified product.

[0023] The primary purified product was added to 1000ml of aqueous solution with pH 8 adjusted with ammonia water, and under the action of 20KHZ ultrasonic waves, ozone was refluxed at a rate of 1L / h for 3 hours, the temperature was lowered, and the secondary purified product was obtained by filtration.

[0024] The secondary purified product was added to 1000g of water, washed by reflux, filtered and dried to obtain pure white polyether ketone ketone. As detected by ICP, its Al 3+ The content is 23ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 2

[0026] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 750 g of ethylenediamine di-o-phenylacetic acid aqueous solution with a mass concentration of 10% was added thereto, refluxed and stirred at 100° C. for 8 hours, cooled, and filtered to obtain a primary purified product.

[0027] The primary purified product was added to 750ml of aqueous solution with pH 9 adjusted with ammonia water, under the action of 20KHZ ultrasonic waves, ozone was refluxed at a rate of 0.5L / h for 4 hours, the temperature was lowered, and the secondary purified product was obtained by filtration.

[0028] The secondary purified product was added to 1250 g of water, washed by reflux, filtered and dried to obtain pure white polyether ketone ketone. As detected by ICP, its Al 3+ The content is 32ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 3

[0030] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 1000 g of ethylenediamine di-o-phenylacetic acid aqueous solution with a mass concentration of 1% was added thereto, refluxed and stirred at 100° C. for 10 hours, cooled, and filtered to obtain a primary purified product.

[0031] The primary purified product was added to 500ml of aqueous solution with a pH of 10 adjusted by ammonia water, and under the action of 20KHZ ultrasonic waves, ozone was refluxed at a rate of 0.1L / h for 5 hours, the temperature was lowered, and the secondary purified product was obtained by filtration.

[0032] The secondary purified product was added to 1500g of water, washed by reflux, filtered and dried to obtain pure white polyether ketone ketone. As detected by ICP, its Al 3+ The content is 41ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

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Abstract

The invention belongs to the technical field of high polymer materials, and in particular relates to a process for purifying a crude product of polyether ether ketone ketone by using a chelating agent. The process comprises the following steps: adding the crude product of polyether ether ketone ketone into an ethanediamine di-o-phenyl acetic acid solution, refluxing, cooling, and filtering so as to obtain a primary purified product; adding the primary purified product into an alkali solution, introducing ozone to reflux under the action of ultrasonic waves, cooling, and filtering so as to obtain a secondary purified product; refluxing and washing the secondary purified product by using water, filtering, and drying, thereby obtaining a purified product of polyether ether ketone ketone. By adopting the process, the content of Al<3+> of the crude product of polyether ether ketone ketone can be reduced to be less than or equal to 50ppm, moreover, a small amount of ethanediamine di-o-phenyl acetic acid is used, the cost is low, the process has energy-saving and environment-friendly effects, the product quality is effectively improved, and the production cost is lowered.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a process for purifying crude polyether ketone ketone by using a chelating agent. Background technique [0002] Polyether ketone ketone (PEKK) is a high-performance special engineering plastic with high temperature resistance, radiation resistance, acid and alkali resistance, and good flame retardancy. It plays an important role in the fields of aerospace, electronic communications, national defense and military technology products, etc. . [0003] Polyether ketone ketone is a product developed by DuPont Company of the United States, and its preparation method is divided into two types: nucleophilic substitution and electrophilic substitution. The electrophilic substitution reaction method generally adopts the Friedel-Crafts reaction synthesis with anhydrous aluminum chloride as a catalyst. The crude polyether ketone ketone synthesized has relatively high r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/46
CPCC08G65/46
Inventor 薛居强李光辉孙庆民王荣海王军张泰铭黄桂青李云龙
Owner SHANDONG KAISHENG NEW MATERIALS