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Preparation method for high-flowability polyaryletherketone terpolymer containing side groups

A aryl ether ketone terpolymer, high fluidity technology, applied in the field of preparation of high fluidity polyarylether ketone terpolymer, can solve problems such as poor fluidity, polyether ether ketone resin high temperature viscosity, etc., to achieve Effects of reducing melt viscosity, increasing flexibility, and enhancing fluidity

Active Publication Date: 2019-11-12
NINGXIA QINGYAN POLYMER MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of polyaryletherketone terpolymer containing side groups in order to solve the problems of polyetheretherketone resin with high viscosity at high temperature and poor fluidity. The present invention uses phenylethylresorcinol and 4,4-dihydroxydiphenyl ether as polymerization raw materials, in order to introduce side groups and ether bonds in the polymer

Method used

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  • Preparation method for high-flowability polyaryletherketone terpolymer containing side groups

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preparation example Construction

[0018] A preparation method of polyaryletherketone terpolymer containing side groups, using 4,4-difluorobenzophenone, 4,4-dihydroxydiphenyl ether, phenylethyl resorcinol as raw materials, Using sulfolane as a solvent, hydroquinone as a molecular weight regulator, potassium bicarbonate as a catalyst, and benzoyl chloride as an end-capping agent, the nucleophilic polycondensation reaction is carried out. The specific preparation process includes the following steps:

[0019] (1) Sulfolane, 4,4-difluorobenzophenone and potassium bicarbonate are added to the reactor, and nitrogen is introduced to remove oxygen;

[0020] (2) Add 4,4-dihydroxydiphenyl ether and phenethyl resorcinol into the reaction system according to a certain ratio, so that the solid content of the system is between 25-40%;

[0021] (3) Pour the solvent xylene into the reaction system and start stirring, heat up to 110-130°C for 0.5-2 hours, continue to heat up to 150-160°C for 1-3 hours, and then continue to hea...

Embodiment 1

[0030] Add 110.1g (0.505mol) of 4,4-difluorobenzophenone and 634.2g of sulfolane into a four-necked reaction flask equipped with a thermometer, nitrogen pipe, condensing reflux separator, and stirrer, and add 102.5g (1.025 mol) potassium bicarbonate and 63.4g xylene, the air in the bottle was evacuated by nitrogen gas, and then 80.8 (0.4mol) 4,4-dihydroxydiphenyl ether and 21.4 (mol) phenylethylresorcinol were added, Stir and heat to 80°C, and continue to slowly raise the temperature after it is completely dissolved. When the temperature rises to 110°C, the system starts to remove water and react at a constant temperature for 2 hours. Continue to raise the temperature to 150°C, the system starts to azeotrope, xylene begins to reflux in the water separator, continue to keep constant temperature for 3 hours to remove xylene, and wait for xylene to evaporate completely. Continue to slowly raise the temperature to 180°C, keep the constant temperature reaction for 5 hours, the visc...

Embodiment 2

[0032] Add 114.4g (0.525mol) of 4,4-difluorobenzophenone and 507g of sulfolane into a four-necked reaction flask equipped with a thermometer, nitrogen pipe, condensing reflux separator, and stirrer, and add 105g (1.05mol) Potassium bicarbonate and 76.1g xylene, the air in the bottle is emptied by nitrogen gas, then add 70.7 (0.35mol) 4,4-dihydroxydiphenyl ether and 32.1 (0.15mol) phenylethyl resorcinol, stir And heat it to 80°C, and continue to slowly raise the temperature after it is completely dissolved. When the temperature rises to 120°C, the system starts to remove water and react at a constant temperature for 1.5h. Continue to raise the temperature to 155°C, the system starts to azeotrope, xylene begins to reflux in the water separator, continue to keep constant temperature for 2 hours to remove xylene, and wait for xylene to evaporate completely. Continue to slowly raise the temperature to 190°C, keep the constant temperature reaction for 4 hours, the viscosity of the s...

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Abstract

The invention provides a preparation method for a high-flowability polyaryletherketone terpolymer containing side groups. The preparation method uses 4,4-difluorobenzophenone, 4,4-dihydroxydiphenyl ether and phenethyl resorcinol as raw materials, sulfolane as a solvent, hydroquinone as a molecular weight regulator, potassium bicarbonate as a catalyst and benzoyl chloride as an end-capping reagent.According to the invention, phenethyl resorcinol and 4,4-dihydroxydiphenyl ether are used as the raw materials; the introduction of a phenethyl group increases the branched chain of the polymer, andincreases steric hindrance and intermolecular distance to decrease intermolecular force; the introduction of an ether bond increases the flexibility and flowability of the polymer; phenol is oxidizedinto benzoquinone in an alkaline environment, and potassium bicarbonate used as the catalyst is beneficial for inhibiting the oxidation of phenol; and the benzoyl chloride is used for terminating a phenoxy-potassium end group structure in the polymer so as to lower the possibility continued reaction or branched crosslinking of the polymer at a high temperature, which is beneficial for improving the flowability and stability of the produced polymer.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a side group-containing high-fluidity polyaryletherketone terpolymer. Background technique [0002] Polyaryletherketone is a class of crystalline polymers in which phenylene rings are linked by oxygen bridges (ether bonds) and carbonyl groups (ketones). Many different polymers can be formed according to the connection sequence and ratio of ether bond, ketone group and benzene ring in the molecular chain. There are mainly polyether ether ketone (PEEK), polyether ketone (PEK), polyether ketone ketone (PEKK) and polyetherether ketone ketone (PEEKK), among which polyetherether ketone is the most important product. Polyetheretherketone (PEEK) is a linear aromatic polymer compound. The main chain of its macromolecule contains a large number of aromatic rings and polar ketone groups, which endow the polymer with heat resistance and mechani...

Claims

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Application Information

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IPC IPC(8): C08G65/40
CPCC08G65/4012C08G65/4087C08G65/4093C08G2650/04C08G2650/40
Inventor 胡求学闫茹张奇张东宝
Owner NINGXIA QINGYAN POLYMER MATERIALS CO LTD
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