Preparation method and application of composite catalyst for synthesis of carbon dioxide copolymer

A technology of composite catalyst and carbon dioxide, which is applied in the field of preparation of composite catalysts for the synthesis of carbon dioxide copolymers, can solve the problems of low conversion rate of epoxy compounds, low catalytic efficiency of zinc carboxylate, high catalyst concentration, etc., to shorten the induction period and cost The effect of low cost and simple synthesis process

Inactive Publication Date: 2011-02-23
GUANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic efficiency of zinc carboxylate is low, requiring higher catalyst concentration and longer reaction time to carry out the reaction, and the conversion rate of epoxy compounds is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: the preparation of double metal cyanide / zinc carboxylate composite catalyst

[0021] Add 8.139g (100mmol) of zinc oxide and 12.947g (98mmol) of glutaric acid into a three-necked flask with a reflux condenser, then add 100mL of toluene, stir vigorously at 80°C for 4 hours, cool, and obtain glutaric acid by filtration Zinc acid, washed 3 times with acetone. The obtained zinc glutarate was vacuum-dried at 80° C. for 24 hours, and stored in a common desiccator.

[0022] Add 8.139g (100mmol) of zinc oxide and 14.322g (98mmol) of adipic acid into a three-necked flask with a reflux condenser, then add 100mL of toluene, stir vigorously at 80°C for 10 hours, cool, and obtain adipic acid by filtration Zinc acid, washed 3 times with acetone. The resulting zinc adipate was vacuum-dried at 80°C for 24 hours and stored in a common desiccator.

[0023] Weighing 5.452g (40mmol) zinc chloride is dissolved in 400mL water, under stirring, add the polyethylene glycol-polyp...

Embodiment 2

[0026] Embodiment 2: Utilize double metal cyanide / zinc carboxylate composite catalyst to synthesize carbon dioxide copolymer

[0027] Weigh 0.1g of the double metal cyanide / zinc glutarate composite catalyst prepared in Example 1 and add it to a 100mL autoclave. After drying in vacuum at 60°C for 24 hours, the reactor was cooled to room temperature, and 34.03g of epoxy Propane and filled with carbon dioxide to make the pressure inside the kettle reach 4.0MPa. After reacting at 60° C. for 8 hours at a stirring speed of 200 rpm, the reactor was cooled to room temperature, unreacted carbon dioxide was slowly released, and the product was taken out. The product was vacuum-dried at 50° C. for 8 hours, the product weighed 45.20 g, and the catalytic efficiency was 452 g polymer / g catalyst. The product was dissolved in dichloromethane, and 5 wt% HCl ethanol solution was added dropwise while stirring until clarified, precipitated with ethanol and washed until neutral, and dried in vacu...

Embodiment 3

[0028] Embodiment 3: Utilize double metal cyanide / zinc carboxylate composite catalyst to synthesize carbon dioxide copolymer

[0029] Weigh 0.1g of the double metal cyanide / zinc glutarate composite catalyst prepared in Example 1 and add it to a 100mL autoclave. After drying in vacuum at 60°C for 24 hours, the reactor was cooled to room temperature, and 39.01g of epoxy Propane and filled with carbon dioxide to make the pressure inside the kettle reach 4.0MPa. After reacting at 60° C. for 12 hours at a stirring speed of 200 rpm, the reactor was cooled to room temperature, unreacted carbon dioxide was slowly released, and the product was taken out. The product was vacuum-dried at 50° C. for 8 hours, the product weighed 55.38 g, and the catalytic efficiency was 553.8 g polymer / g catalyst. The product was dissolved in dichloromethane, and 5 wt% HCl ethanol solution was added dropwise while stirring until clarified, precipitated with ethanol and washed until neutral, and dried in v...

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Abstract

The invention discloses a preparation method and application of a composite catalyst for synthesis of carbon dioxide copolymer, in particular a novel composite catalyst for synthesis of the carbon dioxide copolymer, which is prepared by compounding double metal cyanide and zinc carboxylate according to a certain ratio. The double metal cyanide shortens the induction period of the zinc carboxylate and improves the conversion rate of epoxy compounds; the catalysis efficiency of the catalyst is more than 550g polymer/g catalyst; the molecular weight of the obtained polymer is 40,000 to 100,000; the content of carbonic ester chain element is over 68 percent; the carbon dioxide fixation rate reaches 30 percent; the conversion rate of epoxypropane reaches 95 percent; and the selectivity is over 99 percent. Compared with the single double metal cyanide or single zinc carboxylate, the composite catalyst has obvious advantages; the synthesis process is simple; and the composite catalyst is stable in air, has lower cost, and is particularly applied to industrial production of the carbon dioxide copolymer.

Description

technical field [0001] The invention relates to the field of polymer preparation, in particular to a preparation method and application of a composite catalyst for synthesizing carbon dioxide copolymers. Background technique [0002] Carbon dioxide is considered to be the most important greenhouse gas, making the "greenhouse effect" increasingly serious. Although carbon dioxide pollutes the atmosphere, it is also an abundant, cheap, non-toxic and recyclable carbon resource on the earth. Synthesizing carbon dioxide copolymers with carbon dioxide as a raw material can not only reduce the dependence of polymer materials on petroleum resources, but also turn carbon dioxide from waste into treasure, realize its resource utilization, reduce its impact on the environment and create value, and all The synthesized carbon dioxide copolymer has biodegradable properties and is an environmentally friendly material. [0003] Carbon dioxide itself is not active and requires catalyst acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34
Inventor 杨辉李秉正黄慨黄日波
Owner GUANGXI ACAD OF SCI
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