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Refinement technique of polyetherketoneketone crude product

The technology of crude polyetherketone ketone and polyetherketoneketone is applied in the refining process field of crude polyetherketoneketone, and can solve the problems of viscosity decrease of polyetherketoneketone, product structure change, molecular weight decrease, etc. Energy saving, environmental protection and low toxicity

Inactive Publication Date: 2016-08-31
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

[0021] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 500 g of an aqueous solution of aminotrimethylenephosphonic acid 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.

[0022] The primary purified product was added to 1000 g of 10% hydrogen peroxide acetic acid solution, refluxed for 3 hours, cooled and filtered to obtain the secondary purified product.

[0023] 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 22ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 2

[0025] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 750 g of an aqueous solution of aminotrimethylene phosphonic acid 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.

[0026] The primary purified product was added to 750 g of 20% hydrogen peroxide acetic acid solution, refluxed for 4 hours, cooled, and filtered to obtain the secondary purified product.

[0027] 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 19ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 3

[0029] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 1000 g of an aqueous solution of amino trimethylene phosphonic acid 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.

[0030] The primary purified product was added to 500 g of 30% hydrogen peroxide acetic acid solution, refluxed for 5 hours, cooled, and filtered to obtain the secondary purified product.

[0031] 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 28ppm, 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 particularly relates to a refinement technique of a polyetherketoneketone crude product. The refinement technique comprises the following steps: adding the polyetherketoneketone crude product into an aminotrimethylene phosphonic acid water solution, refluxing, cooling and filtering to obtain a primary purified product; adding the primary purified product into a hydrogen peroxide-acetic acid solution, refluxing, cooling and filtering to obtain a secondary purified product; and washing the secondary purified product with water under reflux, filtering and drying to obtain the polyetherketoneketone pure product. The technique can lower the Al<3+> content in the polyetherketoneketone crude product to 30 ppm or below, has the advantages of low aminotrimethylene phosphonic acid consumption, low cost, energy saving and environment friendliness, effectively enhances the product quality, and lowers the production cost.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a refining process of crude polyether ketone ketone. 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 residual aluminum ions, which ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/46
CPCC08G65/46
Inventor 薛居强王军孙庆民王荣海李光辉张泰铭黄桂青李云龙
Owner SHANDONG KAISHENG NEW MATERIALS
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