Polyether ketone ketone crude product purification technology

A technology of crude polyether ketone ketone and polyether ketone ketone, which is applied in the field of purification process of crude polyether ketone ketone, can solve the problems of polyether ketone ketone viscosity decrease, product structure change, molecular weight decrease, etc. Energy saving, environmental protection, and low toxicity

Inactive Publication Date: 2016-11-23
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

[0023] 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.

[0024] Add the primary purified product to 1000ml of aqueous solution with a pH of 8 adjusted by ammonia water, under the irradiation of ultraviolet light with a wavelength of 280nm, pass through ozone at a rate of 1L / h and reflux for 3 hours, cool down, and filter to obtain the secondary purified product .

[0025] 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 32ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 2

[0027] 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.

[0028] Add the primary purified product to 750ml of aqueous solution with a pH of 9 adjusted with ammonia water, under the irradiation of ultraviolet light with a wavelength of 290nm, pass through ozone at a rate of 0.5L / h and reflux for 4 hours, cool down, filter, and obtain secondary purification Taste.

[0029] 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 20ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 3

[0031] 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.

[0032] Add the primary purified product to 500ml of aqueous solution with a pH of 10 adjusted with ammonia water, and under the irradiation of ultraviolet light with a wavelength of 320nm, pass through ozone at a rate of 0.1L / h and reflux for 5 hours, cool down, filter, and obtain secondary purification Taste.

[0033] 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 45ppm, 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 polyether ketone ketone crude product purification technology. The technology comprises the steps of adding a polyether ketone ketone crude product to ethydiaminedhephen acetic aqueous solution, and conducting reflux, cooling and filtration to obtain a primary purified product; adding the primary purified product to an alkaline aqueous solution, introducing ozone for reflux under UV-irradiation, and conducting cooling and filtration to obtain a secondary purified product; conducting reflux and washing on the secondary purified product with water, and conducting filtration and drying to obtain a polyether ketone ketone purified product. The content of Al3+ in the polyether ketone ketone crude product can be reduced to be below 50 ppm, the consumption of ethydiaminedhephen acetic is low, cost is low, the technology is energy-efficient and environment-friendly, product quality is effectively improved, and production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a purification 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, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/46C08G65/40
CPCC08G65/46C08G65/4012C08G2650/40
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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