Unlock instant, AI-driven research and patent intelligence for your innovation.

Technology for purifying poly(ether-ketone-ketone) crude product by using amino tris(methylene phosphonic acid)

A technology of aminotrimethylene phosphonic acid and crude polyether ketone ketone, which is applied in the field of polymer materials, can solve the problems of polyether ketone ketone viscosity decrease, product structure change, molecular weight decrease, etc., and achieve low cost, energy saving and environmental protection of the process, less toxic effect

Active Publication Date: 2016-10-12
SHANDONG KAISHENG NEW MATERIALS
View PDF1 Cites 1 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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 an aqueous solution of aminotrimethylene phosphonic 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.

[0024] Add the primary purified product to 1000ml of aqueous solution with a pH of 8 adjusted by ammonia water, under the action of ultraviolet light with a wavelength of 280nm and 20KHZ ultrasonic waves, pass through ozone at a rate of 1L / h and reflux for 3 hours, cool down and filter to obtain the following Grade Purity.

[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 23ppm, 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 an aqueous solution of aminotrimethylenephosphonic acid with a mass concentration of 10% was added thereto, stirred at reflux at 100°C for 8 hours, cooled and filtered to obtain a primary purified product.

[0028] The primary purified product was added to 750ml of aqueous solution with a pH of 9 adjusted by ammonia water, and under the action of ultraviolet light with a wavelength of 290nm and 20KHZ ultrasonic waves, ozone was refluxed at a rate of 0.5L / h for 4 hours, cooled and filtered to obtain Secondary purification.

[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 18ppm, 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 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.

[0032] 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 ultraviolet light with a wavelength of 320nm and 20KHZ ultrasonic waves, ozone was refluxed at a rate of 0.1L / h for 5 hours, cooled and filtered to obtain Secondary purification.

[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 28ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle diameteraaaaaaaaaa
Login to View More

Abstract

The invention belongs to the technical field of high polymer materials and particularly relates to a technology for purifying a poly(ether-ketone-ketone) crude product by using amino tris(methylene phosphonic acid). The technology comprises the following steps: adding the poly(ether-ketone-ketone) crude product into an aqueous solution of amino tris(methylene phosphonic acid), and performing reflux, cooling and filtration to obtain a primary purified product; adding the primary purified product into an alkaline aqueous solution; under the effect of ultraviolet irradiation and ultrasonic waves, introducing ozone and performing reflux, cooling and filtration to obtain a secondary purified product; performing reflux and washing of the secondary purified product by using water; and filtering and drying to obtain a poly(ether-ketone-ketone) pure product. In the invention, the content of Al<3+> in the poly(ether-ketone-ketone) crude product can be reduced to 30ppm or below while the dosage of the amino tris(methylene phosphonic acid) is small, the cost is low, the technology has energy-saving and environment-friendly effects, the product quality is effectively improved, and the production cost is reduced.

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 aminotrimethylene phosphonic acid. 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 r...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/46C08G65/40
CPCC08G65/46C08G65/4012C08G2650/40
Inventor 薛居强王荣海王军孙庆民李光辉张泰铭黄桂青李文娟
Owner SHANDONG KAISHENG NEW MATERIALS