Method for purifying polyetherketoneketone crude product

A technology for crude polyether ketone ketone and polyether ketone ketone, which is applied in the field of purifying crude polyether ketone ketone, can solve the problems of complicated and tedious purification process of polyether ketone ketone, generating a large amount of waste liquid, high equipment requirements, etc., and achieving production efficiency High, improved color, simple operation effect

Active Publication Date: 2016-10-26
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the post-treatment purification process of polyether ketone ketone prepared by the electrophilic reaction route is mostly complicated and cumbersome, and a large amount of solvent is used for each treatment, and it often needs repeated washing for a long time, and sometimes high temperature and high pressure purification methods are required , high requirements on equipment, a large amount of waste liquid will be generated after washing, resulting in large investment, low efficiency, and great impact on the environment, thus limiting its further development and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 37.8g of crude polyether ketone ketone with a particle size range of 0.04-1mm into a 1000ml three-neck glass bottle, add 189ml of ethyl formate, heat and stir, adjust the pH to 4, make it swell, and then add 2.5% sodium gluconate 378g of aqueous solution; stirred at reflux temperature for 3 hours, then suction filtered after cooling down; the primary purified polyether ketone ketone was washed 3 times with 200ml of water at room temperature, suction filtered, and dried in a double-cone drier at 120°C for 4 hours. Then dry at negative pressure -0.13MPa for 1 hour, no organic solvent remains after testing, and the catalyst metal ion residue in polyether ketone ketone is 57ppm.

Embodiment 2

[0026] Put 23.56g of crude polyether ketone ketone with a particle size range of 0.5-1.5mm into a 1000ml three-necked glass bottle, add 353.5ml of methyl formate, heat and stir, adjust the pH to 5, make it swell, and then add 4% gluconic acid Sodium aqueous solution 294.5g; Stir at reflux temperature for 5 hours, then filter with suction after cooling down; wash the primary purified polyether ketone ketone with 150ml of water at room temperature for 3 times, filter with suction, and dry in a double-cone drier at 100°C for 6 hours Afterwards, it was dried under a negative pressure of -0.1MPa for 2 hours. It was detected that there was no organic solvent residue, and the catalyst metal ion residue in polyetherketoneketone was 62ppm.

Embodiment 3

[0028] Put 20 g of crude polyether ketone ketone with a particle size range of 1-2.15 mm into a 1000 ml three-necked glass bottle, add 400 ml of propyl formate, heat and stir, adjust the pH to 4, make it swell, and then add 5% sodium gluconate 300g aqueous solution; stir for 5 hours at reflux temperature, and suction filter after cooling down; wash the primary purified polyether ketone ketone with 100ml water at room temperature for 3 times, suction filter, and dry in a double-cone dryer at 110°C for 5 hours at normal pressure, then Negative pressure -0.12MPa dried for 1.5h, no organic solvent residue was detected, and catalyst metal ion residue in polyether ketone ketone was 38ppm.

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Abstract

The invention belongs to the technical field of high polymer materials and particularly relates to a method for purifying a polyetherketoneketone crude product. The method comprises the following steps: adding the polyetherketoneketone crude product into an organic solvent, carrying out heating reflux, and regulating the pH value of the polyetherketoneketone crude product with dilute sulphuric acid, so as to obtain a mixed solution, wherein the organic solvent is one or more of HCOOR smaller than C6; adding a sodium gluconate water solution into the mixed solution, further carrying out stir reflux, cooling, and filtering, so as to obtain a primary polyetherketoneketone purified product; washing the primary polyetherketoneketone purified product with water at the room temperature, carrying out suction filtration, and drying, so as to obtain the polyetherketoneketone purified product. The method has the characteristics of simple operation process, high production efficiency, good product quality, strong operability and the like and is applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a method for purifying crude polyetherketoneketone. Background technique [0002] Polyether ketone ketone is a kind of high-performance thermoplastic engineering plastics. Its excellent heat resistance, rigidity, mechanical properties and wear resistance are widely used in national defense, aerospace, electronic information, automobile manufacturing, petrochemical, medical and health, Household appliances, automobile manufacturing fields. [0003] At present, the preparation of polyether ketone ketone is divided into nucleophilic substitution reaction method and electrophilic substitution reaction method. The former has expensive raw materials and complicated process; the latter has low raw material price and relatively simple process. In the electrophilic substitution reaction method, when polyether ketone ketone is synthesized by polycondensation, anhydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/46
CPCC08G65/46C08G2650/40
Inventor 张聪聪张泰铭王荣海孙庆民李光辉王军黄桂青李云龙
Owner SHANDONG KAISHENG NEW MATERIALS
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