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Crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups and preparation method

A technology of polyether ether ketone ketone resin and polyetherether ketone ketone, which is applied in the field of polymer materials, can solve the problems of poor resin solubility and limited application, and achieve high heat resistance, diverse radiation resistance, and high tensile deformation rate Effect

Active Publication Date: 2020-09-25
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it is precisely because it has a rigid main chain and can be arranged regularly that the solubility of the corresponding resin is extremely poor. At present, it can only be dissolved in concentrated sulfuric acid.
Therefore, the above-mentioned classic polyarylether materials can only be used to prepare reinforcing fibers by melt extrusion, and the high melt viscosity greatly limits the corresponding applications.

Method used

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  • Crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups and preparation method
  • Crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups and preparation method
  • Crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under nitrogen protection, add 0.01mol of mixed bisphenol with a 9:1 molar ratio of phenolphthalein and 4,4'-dihydroxybiphenyl to a three-necked flask with a stirrer, a nitrogen inlet and a condenser, where n / ( The ratio of n+m) is 0.9, the dihalogen monomer 1,3-bis(4'-fluorobenzoyl)benzene is 0.01mol, and potassium carbonate with 1 times the total molar amount of the mixed bisphenol monomer is used as a catalyst, and an appropriate amount is used. The toluene is used as a water-carrying agent, and an appropriate amount of sulfolane is used as a solvent. The temperature was kept at 110°C for 1 hour, after which the toluene was distilled off, and the temperature was raised to 175°C for 4.5 hours. After the final post-treatment, a novel crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups is obtained. The crystallinity of the corresponding resin was 2%, and the number-average relative molecular weight was 30,000. The thermal te...

Embodiment 2

[0022] According to the same operation procedure as Example 1, under nitrogen protection, in a three-necked flask with a stirrer, a nitrogen inlet and a condenser, a mixed biphenyl with a molar ratio of phenolphthalein and 4,4'-dihydroxybiphenyl of 5:5 was added. Phenol 0.01mol, the ratio of n / (n+m) in the structural formula is 0.5, the dihalogen monomer 1,3-bis(4'-fluorobenzoyl)benzene is 0.01mol, and the total molar amount of mixed bisphenol monomers is 1.2 Use potassium carbonate as a catalyst, an appropriate amount of toluene as a water-carrying agent, and an appropriate amount of sulfolane as a solvent. The temperature was kept at 120°C for 2 hours, then the toluene was distilled off, and the temperature was raised to 200°C for 6 hours. After the final post-treatment, a novel crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups is obtained. The crystallinity of the corresponding resin was 20%, and the number-average relative mol...

Embodiment 3

[0024] According to the same operation procedure as Example 1, under nitrogen protection conditions, in a three-necked flask with a stirrer, a nitrogen inlet and a condenser, a mixed biphenyl with a molar ratio of phenolphthalein and 4,4'-dihydroxybiphenyl of 1:9 was added. Phenol 0.01mol, the ratio of n / (n+m) in the structural formula is 0.1, the dihalogen monomer 1,3-bis(4'-fluorobenzoyl)benzene is 0.01mol, and the total molar amount of mixed bisphenol monomers is 1.4 Use potassium carbonate as a catalyst, an appropriate amount of toluene as a water-carrying agent, and an appropriate amount of sulfolane as a solvent. The temperature was kept at 130°C for 3 hours, then the toluene was evaporated, and the temperature was raised to 240°C for 10 hours. After final post-treatment, a novel crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups is obtained. The crystallinity of the corresponding resin is 40%, and the number-average relative...

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Abstract

The invention provides a novel crystallizable polyether ether ketone resin capable of dissolving side groups containing phthalein and a preparation method thereof, and belongs to the technical field of polymer materials. Under nitrogen protection conditions, mixed bisphenol and a dihalogen monomer of the equimolar ratio are used as a synthetic monomer, toluene or xylene is used as a water-carryingagent, potassium carbonate and / or sodium carbonate 1-1.4 times the total molar amount of a bisphenol monomer is used as a catalyst, and sulfolane or dimethyl sulfoxide is used as a solvent for the reaction. Synthesis is performed at 240 DEG C for 4.5-10 hours. The crystallinity of the resin is 2-40%, and the number average relative molecular weight is more than 30,000. The thermal tensile deformation rate of the resin at 250 DEG C is 0-400%, and the resin can be dissolved in 1,1',2,2'-tetrachloroethane and / or p-chlorophenol. The polyether ether ketone resin has the advantages of strong crystallization capacity, high molecular mass, good tensile performance, strong molecular orientation capability and excellent solubility.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a novel crystallizable and soluble polyether ether ketone ketone resin containing phthalein side groups and a preparation method. Background technique [0002] Polyetherketone resins containing phthalein side groups have the characteristics of high tensile strength, high heat resistance, good wear resistance, and good solubility. Polyetherketone resins containing phthalein side groups can be used to manufacture various structural parts and products by thermoforming methods such as injection and extrusion. Used in aerospace, vehicles, ships, electronic appliances, nuclear energy, precision handling, petrochemical, environmental engineering and other fields. High temperature resistant special insulating paints and coatings can also be prepared by dissolving processing. Due to the characteristics of chemical structure, it can also be used as an ideal material for membrane ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40
CPCC08G65/405
Inventor 宾月珍董大林唐萍
Owner DALIAN UNIV OF TECH