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Catalyst for synthesizing polyketone by copolymerization of carbon monooxide and phenyl ethylene

A carbon monoxide and styrene technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of low catalytic activity and relative molecular mass, and achieve relative The effect of high molecular mass, good catalytic activity and high yield

Inactive Publication Date: 2008-11-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently used ligand is 2,2'-bipyridine. This catalytic system is used in the process of copolymerization of carbon monoxide and styrene to form polyketones. The catalytic activity and relative molecular weight are not high.

Method used

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  • Catalyst for synthesizing polyketone by copolymerization of carbon monooxide and phenyl ethylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add the distilled 4-picoline and palladium-carbon catalyst in the ratio of 40:1 (g / g) to a 250mL three-necked flask in turn, stir, and heat in an oil bath after mixing evenly. Reflux at 160°C for 72h, stop the reaction, and filter after cooling. The filtrate was collected, and the resulting filtrate was distilled under reduced pressure until a white solid was precipitated. After collecting the solid, recrystallize it with ethyl acetate to obtain 4,4'-dimethyl-2,2'-bipyridyl crystals with a melting point of 171-172°C.

[0021] Under magnetic stirring, 9.7 mmol of Na 2 Cr 2 o 7 Slowly added to concentrated sulfuric acid, and after stirring for 30 min, 4.3 mmol of 4,4'-dimethyl-2,2'-bipyridine was further added thereto. Orange-yellow flocs were formed immediately in the solution, and the stirring was continued, the flocs gradually turned dark green, and the reaction stopped after 30 minutes. The mixture was poured into 100 mL of ice-water mixture, and a pale yellow pr...

Embodiment 2

[0028] Embodiment 2 (for comparison)

[0029] Under the same conditions as in Example 1, a copolymer of carbon monoxide and styrene was prepared. The difference is that the bidentate ligand was changed from 4,4'-dicarboxylate-2,2'-bipyridine to 2,2'-bipyridine, and 4.68 g of copolymerized product was obtained with a catalytic activity of 881.6 gSTCO / gPd h. Relative molecular mass M n =4182, M w =6039, M w / M n = 1.444.

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Abstract

The invention relates to a catalyst used for synthesizing polyketone by copolymerization of carbon monoxide and cinnamene and a method for synthesizing the same. The catalyst comprises palladium acetate, para-benzoquinone, paratoluenesulfonic acid, fluoboric acid or a mixture of the palladium acetate, the para-benzoquinone, the paratoluenesulfonic acid and the fluoboric acid and 4, 4'-dicarboxylic acid carbethoxyl group-2,2'- dipyridyl. In the invention, carbon monoxide and cinnamene are taken as materials, and absolute methanol is taken as a solvent, and under the conditions of a temperature of between 20 and 80 DEG C and a pressure of between 0.1 and 10Mpa and in the presence of the catalyst, the materials undergo the polymerization reaction for 1 to 3 hours. The catalyst provided by the invention has the advantages of good activity, high yield of the polyketone and high relative molecular mass of the synthesized polyketone; under the condition of the same use level of the main catalyst palladium acetate, the addition of the 4, 4'-dicarboxylic acid carbethoxyl group-2, 2'- dipyridyl can not only improve the activity of the catalyst by 1 to 3 times, but also improve the relative molecular mass of the polyketone by 1 to 2 times.

Description

technical field [0001] The invention relates to a catalyst for synthesizing polyketones, in particular to a catalyst for preparing polyketones by copolymerizing carbon monoxide and styrene with 4,4'-dicarboxylate-2,2'-bipyridine. Background technique [0002] Polyketone is a linear and strictly alternating copolymer prepared by the copolymerization reaction of carbon monoxide (CO) and α-olefin. It has good mechanical properties, solvent resistance, and non-toxic properties. The raw material CO comes from a wide range of sources, reducing the cost compared to most materials synthesized from petroleum. More importantly, the carbonyl group on the main chain of polyketone endows it with unique photodegradation or biodegradation properties, which can slowly degrade into alkenes and CO 2 And other small molecules, which is of great significance in environmental protection and medical health. In addition, the carbonyl group of polyketone is relatively active, and can be used as a...

Claims

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Application Information

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IPC IPC(8): C08G67/02B01J31/18
Inventor 郭锦棠赵海洋冯亚凯李鹏
Owner TIANJIN UNIV
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