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Method for preparing aliphatic polyester (urethane urea-amine)

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

Active Publication Date: 2013-06-12
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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+20mL1,3-dioxane+0.005mol glycerol+0.01mol ZnEt 2 , at CO 2 Added under protection, evacuated to 20Pa at 80°C, filled with CO 2 Treat for 2h, charge with CO 2 10 times, and cooled to the autoclave at room temperature, at the same time, 80mL 2-methylaziridine and 50mL 1,3-dioxane were added to the autoclave, and the pressure of carbon dioxide in the autoclave reached 5.0 MPa. The polymerization reaction 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, and 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. Diethyl ether was slowly added dropwise to the mixture with stirring until...

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+5mL1,3-dioxane+0.00125mol glycerol+0.0025mol ZnEt 2 , at CO 2 Added under protection, evacuated 40Pa at 80°C, filled with CO 2 Treat for 2h, charge with CO 2 10 times, and cooled to room temperature in the autoclave, at the same time, 20mL 2-methylaziridine, 50mL N, N-dimethylacetamide were added to the autoclave, and the carbon dioxide pressure in the autoclave was rapidly reduced by the carbon dioxide pressure regulator. Reach 5.0MPa. The polymerization reaction temperature was 80° C., the reaction time was 10 h, and the stirring speed was 500 rpm. Aftertreatment is the same as embodiment 1, obtains 24g polymkeric substance, and catalyst efficiency is 1.9 * 10 5 g / mol yttrium trichloroacetate. Elemental analysis result is similar to embodiment 1, obtains polymer alternate structure (urethane content) content 84%, carbon d...

Embodiment 3

[0043] From 0.01mol ZnEt 2 Configured and aged rare earth three-way catalyst, the three-way catalyst includes: 0.0005mol neodymium trichloroacetate+20mL1,3-dioxane+0.005mol glycerol+0.01mol ZnEt 2 , at CO 2 Added under protection, evacuated 35Pa at 80°C, filled with CO 2 Treat for 2h, charge with CO 2 10 times, and cooled to the autoclave at room temperature, at the same time, 80mL 2-methylaziridine and 50mL 1,3-dioxane were added to the autoclave, and the pressure of carbon dioxide in the autoclave reached 4.5 MPa. The polymerization reaction temperature was 80° C., the reaction time was 8 hours, and the stirring speed was 500 rpm. The aftertreatment is the same as in Example 1, and the 95g polymer is obtained, and the catalyst efficiency is 1.9×10 5 g / mol neodymium trichloroacetate. Elemental analysis result is similar to embodiment 1, obtains polymer alternate structure (urethane content) content 83%, carbon dioxide fixation rate is 39.1wt%, aziridine compound transfo...

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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 preparation method of aliphatic poly(urethane-amine). Background technique [0002] Carbon dioxide is a recognized greenhouse gas, and its greenhouse effect has constituted increasingly serious environmental pollution. Therefore, reducing carbon dioxide emissions has become a focus of attention of countries all over the world. But on the other hand, carbon dioxide is an inexhaustible C1 raw material. One of the main directions of using carbon dioxide is to synthesize polymer materials from it. Carbon dioxide copolymers (aliphatic poly(urethane-amines)) with urethane and amine units can be synthesized from carbon dioxide and aziridine compounds. Due to the presence of urethane and amine linkages in the main chain, the polymer exhibits thermoresponsive behavior in aqueous solution. The polymer is well soluble in water below the critical solubility temperature (LCST), ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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