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Prepn process of poly (ether-ketone-ketone) as high performance polymer

A polymer material, polyether ketone ketone technology, applied in the field of preparation of polyether ketone ketone high-performance thermal property polymer materials, can solve the problem of reducing material performance, polyether ketone ketone is difficult to obtain polymers, and limits application research And other issues

Inactive Publication Date: 2007-06-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polyether ketone ketone prepared by this method is difficult to obtain a linear high molecular weight polymer. There are six reactive sites in diphenyl ether, so that a branched cross-linking reaction occurs when the polymerization reaction is carried out. In order to avoid this For the occurrence of crosslinking reaction, many researchers have carried out in-depth and meticulous research work. Although it has avoided the subsequent occurrence to a certain extent, it will inevitably occur during branching. For this reason, Dupont Company adopted copolymerization when developing PEKK for commercialization. The way of reducing the performance of the material to a certain extent, thus limiting the application research of the material to a certain extent

Method used

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  • Prepn process of poly (ether-ketone-ketone) as high performance polymer
  • Prepn process of poly (ether-ketone-ketone) as high performance polymer
  • Prepn process of poly (ether-ketone-ketone) as high performance polymer

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Experimental program
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Effect test

Embodiment 1

[0036] Preparation of KOH solution: 280g (5mol) KOH was added to 500ml H 2 In a beaker or other container of O, dissolve to obtain an aqueous KOH solution; then 322g (1mol) two-1,4-(4-fluorobenzoyl)-benzene (purchased in the market) and the prepared KOH solution are added to the container Add 1000ml H 2 0 and 1500ml DMSO, stirred and heated to reflux, the speed of stirring was controlled at 100-2000 rev / min, the temperature of heated to reflux was 100 degrees, kept the reflux temperature for 6h, the reaction solution was cooled to 25 degrees, vacuum filtered by Buchner funnel, The degree of vacuum is 18 mm Hg; slowly add concentrated hydrochloric acid to the filtrate, the concentration of concentrated hydrochloric acid is 36%, the rate of addition is controlled within 10ml / min, to ensure that the temperature of the system does not exceed 30 degrees, when the pH of the system reaches 7 , stop adding hydrochloric acid, white precipitate is obtained in the solution; vacuum filtr...

Embodiment 2

[0038] Add 560gKOH to the 1000mlH 2 O container was dissolved to obtain a KOH solution. This solution was added to the reaction vessel according to the method described in Example 1, stirred and heated to reflux, and the reflux temperature was maintained for 8 hours, and the reaction solution was cooled and filtered; hydrochloric acid was slowly added to the filtrate to adjust the pH to 7, and suction filtered. A white (or light yellow precipitate) was obtained, which was repeatedly washed with water until pH = 7 and dried to obtain the monomeric bis-1,4-(4-hydroxybenzoyl)-benzene with a yield of 85%.

Embodiment 3

[0040] The method is the same as example 1, 400gNaOH is added to 1000mlH 2 O container was dissolved to obtain NaOH solution. Change the solvent, add 1000ml H 2 0 and 1000ml sulfolane, stir and heat to reflux, keep the reflux temperature for 8h, cool and filter the reaction solution; slowly add concentrated hydrochloric acid to the filtrate to adjust the pH to 7, filter with suction to obtain white (or light yellow precipitate), repeat with water Wash the precipitate (or use hot water) to pH = 7, and dry to obtain the monomeric bis-1,4-(4-hydroxybenzoyl)-benzene with a yield of 83%.

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Abstract

The present invention belongs to the field of polymer material, and is especially the preparation process of poly(ether-ketone-ketone) prepared through polymerizing bisphenol and bifluoric monomer. The preparation process includes adding bis-(4-hydroxybenzoyl)-benzene, bis-1, 4-(4-fluorobenzoyl)-benzene or bis-1, 3-(4- fluorobenzoyl)-benzene, Na2CO3 as salt-forming agent and diphenyl sulfone as solid solvent into flask with mechanical stirrer, thermometer and nitrogen duct; introducing high purity nitrogen, heating to 100-130 deg.c and stirring to melting solid matter completely; heating slowly to react; pouring the reaction product into water to separating out white solid; crushing, washing with acetone and water for several times, drying at 80-150 deg.c for 10-20 hr to obtain polymer in the yield over 90 %.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of a polyether ketone ketone type high-performance thermal property polymer material obtained by polymerization of bisphenol and bisfluoromonomers. Background technique [0002] With the development of science and technology, people have higher and higher requirements on the heat resistance level of materials, and general engineering plastics can no longer meet the requirements in some high-tech fields. In order to adapt to the development of cutting-edge technology, since the 1960s, the development of high-performance engineering plastics has been very rapid. Polyaryletherketone (PEEK), which was first successfully developed by the British ICI company, is a fully aromatic semi-crystalline polymer with excellent heat resistance, radiation resistance, insulation and aging resistance. The excellent physical and mechanical properties, thermal proper...

Claims

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Application Information

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IPC IPC(8): C08G65/40
Inventor 周宏伟陈春海党国栋
Owner JILIN UNIV
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