Tert-butyl polyaryletherketone resin and preparation method thereof

The technology of tert-butyl polyaryl ether and tert-butyl aryl ether is applied in the field of tert-butyl polyaryl ether ketone resin and its preparation, and can solve the problems of high melting temperature and melt viscosity, difficult molding process, limited application and the like, Achieve the effects of excellent solubility and film-forming properties, good heat resistance, and low price

Inactive Publication Date: 2019-11-12
JIANGXI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Polyaryletherketone belongs to high temperature resistant thermoplastic polymer. Although its heat resistance is very good, its glass transition temperature (T g ) is still not high, and the operating temperature exceeds T g After that, the modulus drops more
At the same time, as a semi-crystalline polymer, PEK has high melting temperature and melt viscosity, and is insoluble in common solvents. The molding process is relatively difficult, which limits its application.

Method used

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  • Tert-butyl polyaryletherketone resin and preparation method thereof
  • Tert-butyl polyaryletherketone resin and preparation method thereof
  • Tert-butyl polyaryletherketone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Preparation of tert-butyl aryl ether monomer

[0048] Add 0.22mol o-tert-butylphenol, 50ml N-methylpyrrolidone, 0.22mol sodium hydroxide, and 80ml toluene to a three-necked flask equipped with a mechanical stirrer, reflux dehydration device, and nitrogen protection. Heating under reflux for dehydration, until the reaction is complete to remove the water, the temperature of the oil bath is raised to 160°C to distill the toluene. Cool slightly, add 0.1mol of 4,4-dichlorobenzophenone, and adjust the temperature of the oil bath to 190-200°C, and react for 5-6h. After the reaction was completed, the reactant was poured into water to precipitate a precipitate, filtered with suction, washed once with dilute sodium hydroxide solution, and washed once with cold and hot water to obtain a solid with a yield of 90%. The prepared monomers were recrystallized, dried and characterized for structure.

[0049] From figure 1 The H NMR spectrum is given. 1 H NMR (400MHz, CDCl 3 )δ 7....

Embodiment 2

[0051] Add 0.22mol o-tert-butylphenol, 50ml sulfolane, 0.22mol potassium carbonate, and 80ml toluene to a three-necked flask equipped with a mechanical stirrer, reflux dehydration device, and nitrogen protection, and heat the mixture under reflux dehydration at a temperature of 150°C in an oil bath. After the reaction was completed, the water was removed, and the temperature of the oil bath was raised to 160°C to distill off the toluene. Cool slightly, add 0.1mol of 4,4'-difluorobenzophenone, and adjust the temperature of the oil bath to 200°C, and react for 5-6h. After the reaction was completed, the reactant was poured into water to precipitate a precipitate, filtered with suction, washed once with dilute sodium hydroxide solution, and washed once with cold and hot water to obtain a solid with a yield of 95%. The prepared tert-butyl aryl ether monomer was recrystallized and dried to characterize the structure.

Embodiment 3

[0053] Add 0.22mol o-tert-butylphenol, 50ml N-methylpyrrolidone, 0.22mol potassium hydroxide, and 80ml toluene to a three-necked flask equipped with a mechanical stirrer, reflux dehydration device, and nitrogen protection. Heating under reflux for dehydration, until the reaction is complete to remove the water, the temperature of the oil bath is raised to 160°C to distill the toluene. Cool slightly, add 0.1mol of 1,4-bis(4-fluorobenzoyl)benzene, and adjust the temperature of the oil bath to 180-190°C, and react for 5-6h. After the reaction was completed, the reactant was poured into water to precipitate a precipitate, filtered with suction, washed once with dilute sodium hydroxide solution, and washed once with cold and hot water to obtain a solid with a yield of 96%. The prepared tert-butyl aryl ether monomer was recrystallized and dried to characterize the structure.

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Abstract

The invention relates to tert-butyl polyaryletherketone resin and a preparation method thereof. Specifically, aromatic dihalides such as 4,4'-difluorobenzophenone or 1,4-bis(4-fluorobenzoyl)benzene and o-tert-butylphenol are used as raw materials to prepare tert-butyl aryl ether monomers, and then the tert-butyl aryl ether monomers and acyl chloride monomers such as terephthaloyl chloride or isophthaloyl chloride are subjected to electrophilic substitution polycondensation reaction to prepare the polyaryletherketone resin with tert-butyl side groups. The tert-butyl polyaryletherketone resin prepared by the method has good heat resistance, solubility and film-forming property and excellent mechanical properties, and tert-butyl can be further functionalized, so that the tert-butyl polyaryletherketone resin has lower price than commercial polyaryletherketone resin and is wide in application field.

Description

technical field [0001] The invention relates to a tert-butyl polyaryletherketone resin and a preparation method thereof, specifically belonging to the technical field of polymer materials. Background technique [0002] Polyaryletherketone (PEK) is a kind of special polymer material with excellent mechanical properties, dimensional stability, high heat resistance, chemical corrosion resistance, solvent resistance, flame retardancy, radiation protection, etc. It is suitable for Special engineering plastics and high-performance composite material resin matrix have good applications in aerospace, electronic information, high-tech, advanced weapons and other fields, and have become a research hotspot of special polymer materials. [0003] Polyaryletherketone belongs to high temperature resistant thermoplastic polymer. Although its heat resistance is very good, its glass transition temperature (T g ) is still not high, and the operating temperature exceeds T g Afterwards, the mo...

Claims

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Application Information

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IPC IPC(8): C08G61/12
CPCC08G61/127C08G2261/124C08G2261/1412C08G2261/228C08G2261/312C08G2261/3442C08G2261/354C08G2261/592C08G2261/64
Inventor 刘勇军钟鸣宋琤盛寿日刘晓玲宋才生
Owner JIANGXI NORMAL UNIVERSITY
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