Synthesis of polyether-ether-ketone resin with sulfolane as solvent

A technology of polyether ether ketone resin and sulfolane is applied in the field of sulfolane to prepare polyether ether ketone resin, which can solve the problems of high consumption, long process and unsafe hidden danger.

Active Publication Date: 2006-08-16
PANJIN ZHONGRUN SUPER ENG PLASTICS
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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; 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 of polyether-ether-ketone resin with sulfolane as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] First add 490g of refined sulfolane to a three-necked reaction flask equipped with a thermometer, nitrogen pipe, condensing water separator, and stirrer, and then add 67.11g (0.303mol, 1% excess relative to the amount of hydroquinone 0.30mol) , namely 0.30mol+0.30mol×1%=0.303mol) of 4,4'-difluorobenzophenone ( 33.03g (0.30mol) of hydroquinone (Available polymer 86.4g, solid content is 15%). After adding 74g xylene (15% of solvent) again, stir, heat (reaction bottle 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 theoretical amount, the uppe...

Embodiment 2

[0024] As in Example 1, add 490g sulfolane in the same reactor, then add 65.46g (0.30mol) 4,4'-difluorobenzophenone in sequence 33.36g (0.303mol) hydroquinone Thereafter, the order of addition, the amount of addition and the temperature rise reaction are completely the same as in Example 1. Only after 1.5 hours of constant temperature reaction, add 1.195g (0.006mol) of monofluoroketone The reaction was continued for 0.5 hours to stop the reaction. Subsequent refining and drying steps are completely the same as in Example 1.

[0025] Finally obtain the phenyl-terminated polyether ether ketone shown in (1-2) formula, record with DSC:

[0026] Tg=143℃

[0027] Tm = 334°C

[0028] The result of the thermostability measurement of product is:

[0029] Heating at 400°C for 5 minutes: MI = 18.6g / 10 minutes

[0030] Heating at 400°C for 30 minutes: MI = 16.9g / 10 minutes

[0031] 9% lower than the two. Compared with the 17% reduction in Exampl...

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Abstract

Synthesis of poly ether-ether-ketone resin as sulfolane as solvent is carried out by adding into 4,4,-difluoro-benzophenone and hydroquinone related to excessive dihydroxy-benzene 0.1~1%( or insufficient 0.1~1% ) successively, agitating, heating to 75~85 degrees C, adding into K2CO3 and Na2CO3 mixed salt, constant-temperature reacting at 230~260 degrees C for 1~3hrs, putting the reactant into cool water, cooling, freezing, crushing, filtering, boiling the solid product by non-ionic water repeatedly, removing solvent and by-product and drying the refined materials in oven to obtain final product. It can acquire poly ether-ether-ketone resin with two different hydroxyl terminal groups.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a method for preparing polyetheretherketone resin by using a 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 species is the well-known polyether ether ketone (PEEK) resin that was first introduced to the market by the British ICI 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. Among the relevant patents we have obtained in the past (such as 97101168.0 Synthesis of high-viscosity polyetheretherketone resin containing biphe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/02
CPCC08G65/4012C08G65/46
Inventor 吴忠文赵东辉
Owner PANJIN ZHONGRUN SUPER ENG PLASTICS
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