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Process for refining polyether ketone ketone crude product by adopting 2-hydroxysuccinic acid

A technology of hydroxysuccinic acid and polyether ketone ketone, which is applied in the field of refining polymer materials, can solve the problems of increasing the amount of organic solvents, environmental pollution, and high safety risks, and achieve obvious economic and environmental advantages, reduce production costs, and improve The effect of product quality

Inactive Publication Date: 2016-09-07
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional process generally uses solvents such as hydrochloric acid, chlorinated alkanes, and alcohols to remove residual metal ion impurities after 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

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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, put it into a 1000ml reaction vessel, and then add 400g of diphenyl sulfone dichloromethane solution with a mass concentration of 5%, raise the temperature to 45°C and stir and reflux for 2 hours; then add 400g of 10% aqueous solution of 2-hydroxysuccinic acid was stirred under reflux at 45°C for 6 hours, cooled to 23°C and filtered to obtain the primary product of polyether ketone ketone; the primary product was reflux washed with 600g of water for 3 times, then filtered and dried. Obtain white polyether ketone ketone pure product, detect through ICP, its Al 3+ The content is 34ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 2

[0031] Get 20g polyether ketone ketone crude product (Al 3+ Content 4200ppm), the particle size range is 0.5 ~ 1.5mm, add in 1000ml reaction vessel, then add 300g of diphenyl sulfone dichloromethane solution with a mass concentration of 2%, raise the temperature to 42°C and stir and reflux for 3 hours; Add 300g of 5% 2-hydroxysuccinic acid aqueous solution, reflux and stir at 42°C for 5 hours, cool to 25°C and filter to obtain the primary product of polyether ketone ketone; the primary product is washed with 500g of water for 4 times, then filtered and dried , to obtain pure white polyether ketone ketone, detected by ICP, its Al 3+ The content is 46ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

Embodiment 3

[0033] Get 20g polyether ketone ketone crude product (Al 3+ Content 4200ppm), the particle size range is 0.1 ~ 1mm, put it into a 1000ml reaction vessel, and then add 200g of diphenyl sulfone dichloromethane solution with a mass concentration of 1%, raise the temperature to 41°C and stir and reflux for 4 hours; then add 8% 2-hydroxysuccinic acid aqueous solution 200g, reflux and stir at 42°C for 4 hours, cool to 20°C and filter to obtain the primary product of polyether ketone ketone; the primary product was washed with 400g water reflux for 5 times, then filtered and dried, Obtain white polyether ketone ketone pure product, detect through ICP, its Al 3+ The content is 38ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.

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PUM

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Abstract

The invention relates to a refining process of high polymer materials, and in particular relates to a process for refining a polyether ketone ketone crude product by adopting 2-hydroxysuccinic acid. The refining process comprises the steps of: firstly, performing return flow agitation on a certain amount of the polyether ketone ketone crude product in a dichloromethane solution containing diphenyl sulfone; secondly, adding a 2-hydroxysuccinic acid aqueous solution, performing return flow agitation, and performing filtration after cooling; and finally, performing return flow washing by using water, and performing filtration and drying to obtain a polyether ketone ketone pure product. According to the process provided by the invention, diphenyl sulfone is added into dichloromethane to effectively promote the swelling capability of dichloromethane to ensure that polyether ketone ketone molecular chains closely wrapping catalyst impurities are propped open, and foreign ions are scattered into an organic phase; and meanwhile, the efficient metal chelating capability of 2-hydroxysuccinic acid is used to catch metal ions from the organic phase continuously, so that efficient removal of Al<3+> in the polyether ketone ketone crude product is realized.

Description

technical field [0001] The invention relates to a process for refining polymer materials, in particular to a process for refining crude polyether ketone ketone by using 2-hydroxysuccinic 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 polymer, and the higher Al 3+ T...

Claims

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Application Information

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IPC IPC(8): C08G65/46C08G65/40
CPCC08G65/46C08G65/4012C08G2650/40
Inventor 孙庆民张泰铭王荣海李光辉薛居强黄桂青王军贾远超
Owner SHANDONG KAISHENG NEW MATERIALS