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Method for preparing aliphatic polyester (urethane urea-amine)

An aliphatic and urethane technology, applied in the field of polymer material synthesis, can solve the problem that the conversion rate is only 35%

Active Publication Date: 2012-03-28
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, Osamu Ihata and others have studied the copolymerization of 2-methylaziridine and carbon dioxide under supercritical carbon dioxide. It is reported that the content of urethane can be 62% and the fixation rate of carbon dioxide is 32wt at 100°C and 22MPa for 24 hours. % of aliphatic poly(urethane-amine) copolymers, but the conversion rate of 2-methylaziridine compounds is only 35% (Angew.Chem.Int.Ed.43,717,2004; Macromolecules, 38,6429, 2005)

Method used

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  • Method for preparing aliphatic polyester (urethane urea-amine)
  • Method for preparing aliphatic polyester (urethane urea-amine)

Examples

Experimental program
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Effect test

Embodiment 1

[0039] From 0.01mol ZnEt 2 Configured and aged rare earth three-way catalyst, the three-way catalyst includes: 0.0005mol yttrium trichloroacetate+20mL 1,3-dioxolane+0.005mol glycerol+0.01mol ZnEt 2 , In CO 2 Add under protection, evacuate at 80℃ to pressure of 20Pa, charge CO 2 Treat for 2h, charge CO 2 10 times, and cooled to room temperature in the autoclave, while adding 80mL 2-methylaziridine, 50mL 1,3-dioxolane into the autoclave, and quickly pass the carbon dioxide pressure regulator to make the carbon dioxide pressure in the autoclave reach 5.0MPa. The polymerization temperature was 70°C, the reaction time was 12 hours, and the stirring speed was 500 rpm. After the polymerization, the autoclave was cooled to room temperature, the residual carbon dioxide in the autoclave was slowly removed, and 100 mL of 5% hydrochloric acid / ethanol solution (V / V) was added to terminate the polymerization and eliminate the catalyst. Ether was slowly added dropwise to the mixture with stir...

Embodiment 2

[0041] From 0.0025mol ZnEt 2 Configured and aged rare earth three-way catalyst, the three-way catalyst includes: 0.000125mol yttrium trichloroacetate+5mL 1,3-dioxolane+0.00125mol glycerol+0.0025mol ZnEt 2 , In CO 2 Add under protection, evacuate 40Pa at 80℃, charge CO 2 Treat for 2h, charge CO 2 10 times, and cooled to room temperature in the autoclave, while adding 20mL 2-methylaziridine, 50mL N,N-dimethylacetamide into the autoclave, quickly through the carbon dioxide pressure regulator to make the pressure of carbon dioxide in the autoclave It reaches 5.0MPa. The polymerization temperature was 80°C, the reaction time was 10 hours, and the stirring speed was 500 rpm. The post-treatment is the same as in Example 1, to obtain 24 g of polymer, and the catalyst efficiency is 1.9×10 5 g / mol Yttrium trichloroacetate. The elemental analysis results were similar to those of Example 1. The polymer alternating structure (urethane content) content was 84%, the carbon dioxide fixation ra...

Embodiment 3

[0043] From 0.01mol ZnEt 2 A rare earth three-way catalyst configured and aged, the three-way catalyst comprising: 0.0005mol neodymium trichloroacetate+20mL 1,3-dioxolane+0.005mol glycerol+0.01mol ZnEt 2 , In CO 2 Add under protection, evacuate 35Pa at 80℃, charge CO 2 Treat for 2h, charge CO 2 10 times, and cooled to room temperature in the autoclave, while adding 80mL 2-methylaziridine, 50mL 1,3-dioxolane into the autoclave, and quickly pass the carbon dioxide pressure regulator to make the carbon dioxide pressure in the autoclave reach 4.5MPa. The polymerization temperature was 80°C, the reaction time was 8 hours, and the stirring speed was 500 rpm. The post-treatment is the same as in Example 1, to obtain 95 g of polymer, and the catalyst efficiency is 1.9×10 5 g / mol neodymium trichloroacetate. The elemental analysis results were similar to those of Example 1. The content of the polymer alternating structure (urethane content) was 83%, the carbon dioxide fixation rate was 3...

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Abstract

The invention discloses a method for preparing aliphatic polyester (urethane urea-amine). The method comprises: subjecting an aziridine compound and CO2 in the presence of a rare earth ternary catalyst to obtain the aliphatic polyester (urethane urea-amine) which consists of a rare earth carboxylic acid compound, glycerol, diethylzinc and 1,3-dioxolane, wherein the molar ratio of the rare earth carboxylic acid compound to glycerol to diethylzinc is (0.85-1.15):(8.5-11.5):(17-23). The conversion rate of the aliphatic polyester (urethane urea-amine) prepared by the method is more than 80 percent, the molecular weight of the copolymer is 3*10<3> to 4*10<4>, the urethane urea content is more than 80 percent, and the carbon dioxide immobilization rate is more than 38 weight percent.

Description

Technical field [0001] The invention relates to the field of polymer material synthesis, in particular to a method for preparing aliphatic poly(urethane-amine). Background technique [0002] Carbon dioxide is a recognized greenhouse gas, and the greenhouse effect that it produces has constituted increasingly serious environmental pollution. Therefore, reducing carbon dioxide emissions has become a hot spot in the world. But on the other hand, carbon dioxide is an inexhaustible and inexhaustible C1 raw material. One of the main directions of using carbon dioxide is to synthesize polymer materials with it as a raw material. Carbon dioxide copolymers (aliphatic poly(urethane-amine)) with urethane and amine units can be synthesized using carbon dioxide and aziridine compounds as raw materials. Due to the presence of urethane and amine bonds in the main chain, the polymer exhibits thermal response behavior in aqueous solutions. The polymer can dissolve well in water below the criti...

Claims

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Application Information

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IPC IPC(8): C08G71/04
Inventor 顾林王献红赵晓江王佛松
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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