Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for refining crude product of polyether ketone ketone by using hydrochloric acid solution of oxalic acid

A hydrochloric acid aqueous solution, polyether ketone ketone technology, applied in the field of refining polymer materials, can solve the problems of increasing the amount of organic solvents, high safety risks, environmental pollution, etc., achieve obvious economic and environmental advantages, improve product quality, and reduce production costs Effect

Active Publication Date: 2016-10-26
SHANDONG KAISHENG NEW MATERIALS
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Traditional methods generally use solvents such as hydrochloric acid, chlorinated alkanes, and alcohols to remove residual metal ion impurities through repeated washing. The process is cumbersome, the treatment efficiency is low, the toxicity is high, the safety risk is high, and the environment is seriously polluted, which is not conducive to product quality stability and scale. production, and the high production cost seriously affects the large-scale application and promotion of polyether ketone ketone
CN200410081436 uses organic solvents and surfactants for purification, which increases the amount of organic solvents and increases production costs; US20050004340 uses high-temperature and high-pressure purification methods, which improves the use requirements of equipment; CN200910009128 uses acid purification methods, a large number of Acid solution brings difficulties to the biochemical treatment of post-production wastewater

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

[0027] Get 20g polyether ketone ketone crude product (Al 3+ Content 4200ppm), the particle size range is 1 ~ 2mm, add in 1000ml reaction vessel, add the aqueous solution 400g of the dimethyl sulfoxide that mass concentration is 5% afterwards, raise temperature and stir and reflux for 2 hours; then add 10% of 400g of hydrochloric acid aqueous solution of oxalic acid, reflux and stir for 6 hours, cool down to 23°C and filter to obtain the primary product of polyether ketone ketone; the primary product was washed with 600g of water under reflux for 3 times, then filtered and dried to obtain pure white polyether ketone ketone , detected by ICP, its Al 3+ The content is 36ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

[0028] The preparation method of the hydrochloric acid aqueous solution of oxalic acid is that oxalic acid is added into the hydrochloric acid aqueous solution whose mass concentration is 5%, to obtain the hydrochl...

Embodiment 2

[0032] Get 20g polyether ketone ketone crude product (Al 3+ Content 4200ppm), the particle size range is 0.5 ~ 1.5mm, put it into a 1000ml reaction vessel, and then add 300g of an aqueous solution of dimethyl sulfoxide with a mass concentration of 2%, raise the temperature and stir and reflux for 3 hours; then add 5% 300g of hydrochloric acid aqueous solution of oxalic acid, reflux and stir for 5 hours, cool down to 25°C and filter to obtain the primary product of polyether ketone ketone; the primary product was washed 4 times with 500g of water under reflux, then filtered and dried to obtain pure white polyether ketone ketone Products, detected by ICP, its Al 3+ The content is 49ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

[0033] The preparation method of the hydrochloric acid aqueous solution of oxalic acid is that oxalic acid is added in the hydrochloric acid aqueous solution that mass concentration is 8%, obtains the ...

Embodiment 3

[0035] Get 20g polyether ketone ketone crude product (Al 3+ Content 4200ppm), particle size range is 0.1 ~ 1mm, put into 1000ml reaction vessel, then add 200g of aqueous solution of dimethyl sulfoxide with a mass concentration of 1%, raise the temperature and stir and reflux for 4 hours; then add 8% of 200g of hydrochloric acid aqueous solution of oxalic acid, reflux and stir for 4 hours, cool down to 20°C and filter to obtain the primary product of polyether ketone ketone; the primary product was washed with 400g of water under reflux for 5 times, then filtered and dried to obtain pure white polyether ketone ketone , detected by ICP, its Al 3+ The content is 42ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

[0036] The preparation method of the hydrochloric acid aqueous solution of oxalic acid is that oxalic acid is added in the hydrochloric acid aqueous solution whose mass concentration is 10%, to obtain the hydrochloric ac...

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

No PUM Login to View More

Abstract

The invention relates to a high polymer material refining method, and in particular relates to a method for refining a crude product of polyether ketone ketone by using a hydrochloric acid solution of oxalic acid. The method comprises the following steps: firstly, refluxing and stirring a certain amount of the crude product of polyether ketone ketone in a dimethyl sulfoxide solution; subsequently adding the hydrochloric acid solution of oxalic acid, refluxing and stirring, cooling, and filtering; and refluxing and washing with water, filtering, and drying, thereby obtaining a pure product of polyether ketone ketone. By virtue of the swelling property of polyether ketone ketone in the dimethyl sulfoxide solution, molecular chains of polyether ketone ketone by which catalyst impurities are tightly wrapped can be expanded, then impurity ions can be diffused into organic phase, and meanwhile, metal ions can be continuously captured by virtue of the metal-chelating property of oxalic acid, so that Al<3+> in the crude product of polyether ketone ketone can be effectively removed.

Description

technical field [0001] The invention relates to a method for refining polymer materials, in particular to a method for refining crude polyether ketone ketone by using an aqueous hydrochloric acid solution of oxalic acid. Background technique [0002] Polyether ketone ketone (PEKK) is a high-performance semi-crystalline thermoplastic polymer, which belongs to the family of polyarylether ketone special polymer materials. Radiation and flame retardancy have broad application prospects in the fields of national defense, aerospace, electronic information, automobile manufacturing, petrochemical, medical and health, and household appliances. [0003] The electrophilic substitution reaction route to synthesize PEKK usually uses the Friedel-Crafts reaction catalyst AlCl 3 Synthesis, the reaction process requires a large amount of catalysts, due to the entanglement of macromolecular chains, some catalysts are firmly wrapped in the polymer, and catalysts inevitably remain in the poly...

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
IPC IPC(8): C08G65/46
CPCC08G65/46C08G2650/40
Inventor 李光辉贾远超张泰铭孙庆民王荣海薛居强黄桂青李云龙
Owner SHANDONG KAISHENG NEW MATERIALS
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products