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Preparation method of polyetheretherketone resin

A technology of polyetheretherketone resin and polyetheretherketone, which is applied in the field of preparation of polyetheretherketone resin, can solve the problems of low level, discontinuous process flow, and unclean polymer product purity, etc., and achieves high purity, Ensure purity and performance, overcome the effect of low purity of polymer products

Active Publication Date: 2017-10-24
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above-mentioned defects, the present invention provides a preparation method of polyetheretherketone resin, which overcomes the problem of discontinuous process flow caused by the need to pulverize the product in the production process of the existing polyetheretherketone resin, and also overcomes the traditional In the process, the inorganic salt particles wrapped in product particles are not cleaned cleanly, resulting in the problem of low purity of polymer products. This provides a new method for product precipitation and purification in the field of amorphous polymer production, and simplifies the production process.

Method used

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  • Preparation method of polyetheretherketone resin

Examples

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preparation example Construction

[0020] The invention provides a preparation method of polyether ether ketone resin, including polymerization reaction and precipitation and purification treatment of reaction products, wherein:

[0021] The raw materials and their molar ratios in polyether ether ketone polymerization are: 4,4′-difluorobenzophenone: hydroquinone: catalyst: diphenyl sulfone: dehydrating agent = 1: 1: 1.2: 4.1~4.5 ︰1.4~1.6;

[0022] The precipitation treatment of the reaction product is as follows: after the polymerization reaction is completed, the reaction temperature is lowered to 210-230 °C, and the stirring is accelerated to make the polyether ether ketone resin system uniformly precipitated. When the temperature in the reactor is stable, trimethylbenzene is added and stirred until the reaction system After uniformity, the reaction temperature is lowered to 90-110°C (preferably 100°C), so that all the polyether ether ketone resins are uniformly crystallized and precipitated, and the reaction...

Embodiment 1

[0044] The preparation of embodiment 1 polyetheretherketone resin

[0045] Taking a 200L polymerization kettle as an example, prepare raw materials according to the following quality: 4,4'-difluorobenzophenone (10.9Kg), hydroquinone (5.5Kg), potassium carbonate (4.96Kg), sodium carbonate (2.54 Kg), diphenylsulfone 46.8Kg), trimethylbenzene (9.3Kg).

[0046] Accurately weigh the above formula components respectively, add diphenyl sulfone and trimethylbenzene into a 200L polymerization kettle equipped with a water separator, agitator (frame-type paddle-type two-way stirring) and a heating device, and pass in an inert gas nitrogen protection , start stirring (frame stirring 30r / min, paddle stirring 60r / min), the jacket of the reactor is heated to 140°C, after 40 minutes all diphenyl sulfone is dissolved, and 4,4'-difluorobenzophenone is added in sequence and hydroquinone, continue to stir for 10 minutes to dissolve the monomer, add catalyst potassium carbonate and sodium carbona...

Embodiment 2

[0054] Refer to Example 1 for the specific method. The only difference from the example is that the reflux reaction time is extended by 30 minutes, and the polymerization reaction is extended by 30 minutes; the properties of the obtained polyether ether ketone resin are shown in Table 1.

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Abstract

The invention belongs to the technical field of high molecular materials, and particularly relates to a method for preparing polyether ether ketone. The method for preparing the polyether ether ketone includes the steps of a polymerization reaction; precipitation treatment of a reaction product, wherein after the polymerization reaction is finished, reaction temperature is reduced to 210-230 DEG C, stirring is accelerated to enable a polyether ether ketone system to be evenly polymerized, trimethylbenzene is added when the temperature in a reactor is stable, the reaction system is stirred to be even, and then the reaction temperature is reduced to 90-110 DEG C to enable all polyether ether ketone to be evenly crystallized and polymerized; purification treatment, wherein a dehydrating agent and diphenyl sulfone are sequentially recycled from white slurry obtained through precipitation treatment, and then the polyether ether ketone can be obtained through washing and drying. By means of the method, the problem that in the existing production process of the polyether ether ketone, as a product needs to be smashed, technological processes are discontinuous is solved, and meanwhile the problem that in a traditional technology, as inorganic salt particles wrapped by product particles can not be completely washed away, a high molecular product is not high in purity is solved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a preparation method of polyetheretherketone resin. Background technique [0002] At present, the synthesis technology of polyether ether ketone resin is relatively mature, and most manufacturers often use the method of gradually releasing the product from the polymerization kettle to cool after the synthesis reaction of polyether ether ketone resin, and then pulverize it to obtain powder for subsequent use. The solvent and by-product salts are recovered. Such a production process has the following disadvantages: one is that it is difficult to operate automatically, the site is polluted, and the product in the polymerization tank is likely to remain and affect the next batch production; the other is that the particle size of the powder obtained after crushing is difficult to be uniform, and the catalyst and by-products used for synthesis are still It is difficult to pu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/02
CPCC08G8/02
Inventor 钟家春曲忠先
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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