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Preparation method for polyetheretherketone

A technology of polyether ether ketone and difluorobenzophenone, which is applied in the field of preparation of special functional engineering resins, can solve problems such as strong water absorption of potassium carbonate, small molecular weight, and impact on industrial production, and reduce the introduction of impurities and reaction conditions Mild, raw material reduction effect

Active Publication Date: 2008-07-09
JILIN ZHONGYAN HIGH PERFORMANCE PLASTIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the existing PEEK preparation technology, no matter in terms of product quality or process maturity, the process of preparing PEEK by polycondensation of dihydric phenol and difluorobenzophenone still has a great advantage, but from the published experimental results. Look, most of them use K 2 CO 3 / Na 2 CO 3 or K 2 CO 3 / Na 2 CO 3 / SrCO 3 The mixed salt system is used as a condensing agent, and is based on K 2 CO 3 It is the main composite condensing agent, but the problems of this composite condensing agent are: potassium carbonate has strong water absorption, and it is difficult to crush and sieve, resulting in high impurity content in the product; one-time feeding cannot well control the polyetheretherketone product. Viscosity, which affects the batch stability of the product, but also has a certain impact on industrial production
In the condensation reaction, diphenol needs to form corresponding sodium phenate or potassium phenate with sodium carbonate or potassium carbonate at first, wherein the activity of potassium phenate is higher than that of sodium phenate, so it undergoes polycondensation with difluorobenzophenone It is easy to form PEEK products with larger molecular weight during the reaction, but in the later stage of the reaction, due to the high viscosity of the system, the probability of molecular collisions decreases, the molecular weight is difficult to increase to a large enough size, and the molecular weight distribution is also very wide; when sodium carbonate is used alone as the condensation agent, Due to its low activity, it is difficult to continue the reaction when the molecular weight increases to a certain extent. Therefore, it is usually impossible to prepare high-molecular-weight PEEK products, and only PEEK products with smaller molecular weights can be formed.

Method used

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  • Preparation method for polyetheretherketone

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Vacuumize the reactor equipped with mechanical stirrer, thermometer and condenser, and then fill it with high-purity nitrogen. After three times, the air in the system will be completely replaced with nitrogen. Phenylsulfone, after heating until it dissolves, add 172.2 grams of 4,4'-difluorobenzophenone (0.79 moles) to dissolve it, add 72.6 grams of biphenol (0.39 moles) to dissolve it, and add 42.9 grams of terephthalate Phenol (0.39 moles) was used to dissolve it, and the previously dried Na 2 CO 3 After crushing and sieving, accurately weigh 95.4 grams (0.9 moles) of powder and immediately add it to the reaction system, stir for 30 minutes to make it salt with diphenol and dissolve, quickly raise the temperature of the system to 190°C, and react for 30 minutes , raise the system temperature to 300°C within 10 minutes, react for 1 hour, rapidly raise the temperature to 325°C, and immediately add 1.1 grams of hydroquinone (0.01 mole) as a chain extender, increase the ...

Embodiment 2

[0020] Under the same reaction conditions as in Example 1, the mol ratio of hydroquinone and biquinone was 1: 2 when charging for the first time, and other conditions did not change, that is, when charging for the first time, hydroquinone was 28.6 grams (0.26 moles), biphenol is 96.7 grams (0.52 moles), and the experimental results are shown in Table 1.

Embodiment 3

[0022] Under the same reaction conditions as in Example 1, the mol ratio of hydroquinone and biquinone was changed to 1: 3 when charging for the first time, and other conditions did not change, that is, hydroquinone was added when charging for the first time. It is 20.9 grams (0.19 moles), and biphenol is 110 grams (0.57 moles). The experimental results are shown in Table 1.

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Abstract

The invention relates to a process for preparing polyetheretherketone products, which is characterized in that the process comprises adopting Na2CO3 to be condensating agent, leading 4, 4'- difluorobenzophenone, hydroquinone and diresorcinol to have polymerization reaction, improving the reaction temperature after producing the relative prepolymer, and secondly adding hydroquinone to be chain extender to react for a period of time to prepare polyetheretherketone products with high viscosity.

Description

technical field [0001] The invention relates to a method for preparing a special functional engineering resin, more specifically a method for preparing polyether ether ketone. Background technique [0002] Polyetheretherketone (PEEK) is an aromatic linear polymer. It not only has good processing performance, but also has excellent high temperature resistance. Its load heat distortion temperature is as high as 315°C, and its continuous use temperature can reach 260°C. , At the same time, this polymer also has many excellent properties such as good wear resistance, chemical resistance, flame retardancy, hydrolysis resistance, and radiation resistance. In view of this, in addition to the application in national defense and military, PEEK is also widely used in many fields such as aerospace, automobile manufacturing, electronic appliances, medical treatment and food. [0003] From a structural point of view, PEEK is a polymer composed of ether bonds and ketone groups connecting...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/02
CPCC08G65/40C08G65/4093
Inventor 发明人请求不公开姓名
Owner JILIN ZHONGYAN HIGH PERFORMANCE PLASTIC
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