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Synthesis method of ternary copolymer containing PEDEK and PEEK using sulfolane as solvent

A polyether ether ketone terpolymer, biphenyl polyether ether ketone technology, applied in the field of polymer materials, can solve the problems of unsafe hidden danger, increase production cost, large consumption and the like

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

AI Technical Summary

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; the second is that a large amount of acetone and ethanol used are flammable and explosive dangerous chemicals. There are also unavoidable hidden dangers in the

Method used

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  • Synthesis method of ternary copolymer containing PEDEK and PEEK using sulfolane as solvent
  • Synthesis method of ternary copolymer containing PEDEK and PEEK using sulfolane as solvent
  • Synthesis method of ternary copolymer containing PEDEK and PEEK using sulfolane as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First add 490g of sulfolane to a three-necked reaction flask equipped with a thermometer, a nitrogen pipe, a condensing water separator, and a stirrer, and then add 66.11g (0.303mol) of 4,4'-difluorobenzophenone in sequence 0.558g (0.003mol) biphenol 32.70g (0.297mol) hydroquinone About 86 g of polymer were obtained with a solids content (calculated on polymer content excluding by-product salts) of about 15%. After adding 74g xylene (15% of solvent) again, stir, heat (reaction flask is put into corresponding electric heating mantle), treat that it all dissolves and when temperature rises to 80 ℃, add 25.73g (0.153mol, excess 2 %) K 2 CO 3 and 16.2g (0.153mol, excess 2%) Na 2 CO 3 , and then continue to heat up, when the temperature rises to 150 ° C, the system starts to azeotrope, xylene and water condense in the water separator, the upper layer of xylene refluxes, and the lower layer of water is continuously released. When the water is recovered to the theoreti...

Embodiment 2

[0023] Change the batching ratio of Example 1, after adding 490g sulfolane, add 66.11g (0.303mol) 4,4'-difluorobenzophenone, 11.17g (0.06mol) biphenol, 26.43g (0.24mol) ) Hydroquinone, the charging amount, charging sequence and reaction conditions and aftertreatment refining thereafter are all with embodiment 1. Then obtain the polyether ether ketone and polyether ether ketone terpolymer containing the biphenyl structure of the fluorine end group shown in formula (2-1) x=0.2, record with DSC:

[0024] Tg=149℃

[0025] Tm = 298°C

Embodiment 3

[0027] Change the batching ratio of embodiment 1, after adding 490g sulfolane, add 66.11g (0.303mol) 4,4'-difluorobenzophenone, 22.33g (0.120mol) biphenyldiphenol, 19.82g (0.180mol) ) Hydroquinone, the charging amount, charging sequence and reaction conditions and aftertreatment refining thereafter are all with embodiment 1. Then obtain the polyether ether ketone and polyether ether ketone terpolymer containing the biphenyl structure of the fluorine end group shown in formula (2-1) x=0.4, record with DSC:

[0028] Tg=155℃

[0029] Tm = 302°C

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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 is more than that of eldopaque and diphenol by 0.1-1%, 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 macromolecular materials, and in particular relates to a method for preparing biphenyl-containing polyetheretherketone and polyetheretherketone terpolymer by using a polar solvent, especially sulfolane as a solvent. 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 polyether ether ketone (PEEK) resin that was first introduced to the market by the British ICl company in 1981. The patent of its preparation method clearly refers to the high-temperature solvent diphenyl sulfone. Because its polymer reaction temperature is above 300°C, other solvents cannot adapt. All of the patents on polyaryletherketone that were applied for later used this solvent. We have also used this traditional high-temperature solvent in the related pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/02C08G65/40
Inventor 吴忠文王贵宾王兴武周福贵范曙光任殿福赵东辉陈凤勤姜振华
Owner 长春吉大特塑工程研究有限公司
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