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Porous polyaryletherketone microsphere and preparation method thereof

A technology of porous microspheres and polyaryletherketone, which is applied in the field of porous materials, can solve the problems of subsequent application influence, residual porogen, complicated process, etc., and achieve the effects of improving purity, simple preparation process and low energy consumption.

Active Publication Date: 2019-11-19
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since porogens need to be used in the preparation process, and porogens need to be removed from the final product, the porous microspheres obtained by this method have more or less porogen residues, which will have a certain impact on subsequent applications. influences
Moreover, the existing preparation process often uses crosslinking agents, stirring, heating and other conditions, not only the process is complicated, but also the energy consumption is high

Method used

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  • Porous polyaryletherketone microsphere and preparation method thereof
  • Porous polyaryletherketone microsphere and preparation method thereof
  • Porous polyaryletherketone microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Quickly weigh 0.500 g of 1,3,5-benzenetricarboxylic acid chloride and 0.481 g of diphenyl ether into a 250 mL three-necked flask, and then add 100 mL of dichloromethane. Quickly weigh 5.359g of titanium tetrachloride and add it into a three-necked flask, and shake it with a shaker for about 1min. After standing at room temperature for 72 hours, the orange-red transparent liquid gradually became turbid and precipitated out. The reaction mixture was placed in a centrifuge tube for separation under the conditions of 10000 rpm and 1 min. The obtained solid was washed with dichloromethane and centrifuged three times, and the solid in the centrifuge tube was put into a drying oven to dry overnight to finally obtain a dark yellow solid powder, namely polyaryletherketone porous microspheres.

Embodiment 2

[0036] Quickly weigh 0.700 g of 1,3,5-benzenetricarboxylic acid chloride and 0.481 g of diphenyl ether into a 250 mL three-necked flask, and then add 100 mL of chloroform. Quickly weigh 5.359g of titanium tetrachloride and add it into a three-necked flask, and shake it with a shaker for about 1min. After standing at room temperature for 12 hours, the orange-red transparent liquid gradually became turbid and precipitated out. The reaction mixture was placed in a centrifuge tube for separation under the conditions of 10000 rpm and 1 min. The obtained solid was washed with acetone and centrifuged three times, and the solid in the centrifuge tube was put into a drying oven to dry overnight, and finally dark yellow solid powder was obtained, namely polyaryletherketone porous microspheres.

Embodiment 3

[0038] Quickly weigh 0.800 g of 1,3,5-benzenetricarbonyl chloride and 0.481 g of diphenyl ether into a 250 mL three-necked flask, and then add 100 mL of dimethyl sulfoxide. Quickly weigh 5.359g of titanium tetrachloride and add it into a three-necked flask, and shake it with a shaker for about 1min. After standing at room temperature for 24 hours, the transparent liquid gradually became cloudy and precipitated out. The reaction mixture was placed in a centrifuge tube for separation under the conditions of 10000 rpm and 1 min. The obtained solid was washed with acetone and centrifuged three times, and the solid in the centrifuge tube was put into a drying oven to dry overnight, and finally dark yellow solid powder was obtained, namely polyaryletherketone porous microspheres.

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Abstract

The invention relates to a porous polyaryletherketone microsphere and a preparation method thereof. 1,3,5-trichlorobenzoylchloride and diphenyl ether which are used as raw materials undergo precipitation polymerization by a Friedel-Crafts acylation reaction with dichloromethane as a solvent and titanium tetrachloride as a catalyst in order to synthesize polyaryletherketone. Results of characterization of the polyaryletherketone by scanning electron microscopy, thermogravimetry and infrared spectroscopy show that the polyaryletherketone material exhibits a regular spherical structure, is insoluble in most organic solvents, has a large number of irregular pores inside, and has great applications in the fields of catalyst supports and adsorption separation.

Description

technical field [0001] The invention relates to a polyaryletherketone porous microsphere and a preparation method thereof, belonging to the technical field of porous materials. Background technique [0002] Porous polymer microspheres are polymer spherical particles with a porous structure prepared by polymer synthesis. This kind of material has the characteristics of various preparation methods, easy modification, and adjustable pore size, and has a wide range of applications in chromatography packing, catalyst carrier, biological analysis, composite materials, etc. Suspension polymerization is the main method for preparing porous microspheres. Firstly, a porogen is added to the monomer for suspension polymerization, and then the porogen is removed after the polymerization. The space originally occupied by the porogen is retained, so that the microspheres have porous structure. Yang Shujing and others used a mixed solution of dibutyl phthalate (DBP) and toluene as a porog...

Claims

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Application Information

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IPC IPC(8): C08G61/12
CPCC08G61/127C08G2261/12C08G2261/3442C08G2261/45
Inventor 杨鹏飞张志良白锋王永清
Owner QILU UNIV OF TECH
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