Synthesis method of ternary copolymer containing PEEK and poly(ether ether ketone ketone)s using sulfolane as solvent

A technology of polyether ether ketone ketone terpolymer and fluorine-terminated polyether ether ketone, which is applied in the field of polymer materials and can solve the problems of long process, large consumption, and increased production costs

Active Publication Date: 2006-12-27
长春吉大特塑工程研究有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this way, due to the long process and the consumption of a large amount of acetone and ethanol, the production cost will undoubtedly be greatly increased; t

Method used

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  • Synthesis method of ternary copolymer containing PEEK and poly(ether ether ketone ketone)s using sulfolane as solvent
  • Synthesis method of ternary copolymer containing PEEK and poly(ether ether ketone ketone)s using sulfolane as solvent
  • Synthesis method of ternary copolymer containing PEEK and poly(ether ether ketone ketone)s using sulfolane as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a three-necked reaction flask equipped with a thermometer, a nitrogen pipe, a condensing water separator, and a stirrer, 490 g of refined sulfolane was firstly added, and then 0.98 g (0.00303 mol) of 4,4'-difluorotriphenylene was added in sequence. 65.45g (0.29997mol) 4,4'-difluorobenzophenone 33.03g (0.30mol) hydroquinone The obtained polymer was 87.48 g with a solid content of 15.15%. After adding 74g xylene (15% of the solvent), stir and heat (put the reaction flask into the corresponding electric heating mantle), when it is completely dissolved and when the temperature rises to 80°C, add 25.73g (0.153mol, excess 2 %)K 2 CO 3 and 16.2g (0.153mol, 2% excess) Na 2 CO 3 , and then continue to heat up, when the temperature rises to 150 ° C, the system begins to azeotrope, xylene and water are condensed in the water separator, the upper layer of xylene is refluxed, and the lower layer of water is continuously released. When the water is recovered to the theoret...

Embodiment 2

[0022] Change the proportioning ratio of Example 1, after adding 490g sulfolane in sequence, add 19.53g (0.0606mol) 4,4'-difluorotribenzodione, 52.89g (0.2424mol) 4,4'-difluorodiphenyl Ketone, 33.03g (0.30mol) hydroquinone, the subsequent feeding amount, feeding sequence, reaction conditions and post-treatment refining are completely the same as those in Example 1, then the fluorine with x=0.2 as shown in formula (3-1) is obtained Terminated polyether ether ketone and polyether ether ketone ketone terpolymer, measured by DSC:

[0023] Tg=148℃

[0024] Tm=340℃

Embodiment 3

[0026] Change the proportioning ratio of Example 1, after adding 490g sulfolane in sequence, add 39.05g (0.1212mol) 4,4'-difluorotribenzodione, 39.67g (0.1818mol) 4,4'-difluorodiphenyl Ketone, 33.03g (0.30mol) hydroquinone, the subsequent feeding amount, feeding sequence, reaction conditions and post-treatment purification are completely the same as those in Example 1, then the fluorine with x=0.4 shown in formula (3-1) is obtained Terminated polyether ether ketone and polyether ether ketone ketone terpolymer, measured by DSC:

[0027] Tg=152℃

[0028] Tm=347℃

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Abstract

The invention relates to a method for preparing polyetheretherketone and polyetheretherketone terpolymer by using sulfolane. It comprises following steps: the mole number of 4, 4'- difluoro diphenyl ketone and 4, 4'- difluoro triphen dione is more than that of eldopaque by 0.1-1%, the mle number of 4, 4'- difluoro triphen dione is 1-4% of that of total fluorin and acetone, the solid content in reaction system is 15-30%; filling dimethylbenzene with its mass being 10-20% of that of organic solvent, stirring, heating, adding mixed salt of alkali metal carbonate when monomer is totally dissolved and the temperature is between 75 to 85 Deg. C, reacting at constant temperature 230-260 Deg. C for 1-3 hours, stopping reaction, pouring product into cold water, cooling and disintegrating and filtering, boiling solid product with deionized water for several times, drying refined powder material in baking box, and getting said final product.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a method for preparing polyether ether ketone and polyether ether ketone ketone terpolymer by using polar solvent, especially sulfolane. Background technique [0002] Polyaryletherketone polymers have a series of excellent comprehensive properties such as high temperature resistance, high strength and radiation resistance. Its earliest commercialized variety is the well-known polyetheretherketone (PEEK) resin that was first introduced to the market by the British ICI company in 1981. In the patent of its preparation method, it is clear that it is a high temperature solvent diphenyl sulfone. Because its polymer reaction temperature is above 300°C, other solvents cannot be adapted. All subsequent patents on polyaryl ether ketones use this solvent. In the related patents we obtained in the past (for example, the preparation of 97101168.0 polyaryl ether ketone copolyme...

Claims

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Application Information

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IPC IPC(8): C08G8/02C08G65/40
Inventor 吴忠文姜振华范曙光任殿福王兴武周福贵赵东辉陈凤勤王贵宾
Owner 长春吉大特塑工程研究有限公司
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