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Method for preparing lactide-propylene oxide-CO2 terpolymer by using rare earth three-way catalyst

A ternary catalyst and terpolymer technology, applied in the field of polymers, can solve the problems of unfavorable industrial production, long polymerization reaction time, etc.

Active Publication Date: 2013-08-14
中科应化(长春)科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, the polymerization time of the method of above-mentioned report is long, is unfavorable for industrialized production

Method used

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  • Method for preparing lactide-propylene oxide-CO2 terpolymer by using rare earth three-way catalyst
  • Method for preparing lactide-propylene oxide-CO2 terpolymer by using rare earth three-way catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of Rare Earth Three-way Catalyst

[0037] Evacuate a 50mL two-neck bottle under reduced pressure at 80°C to 20-40Pa, replace it with high-purity argon every 20 minutes, and replace it 5 times in total, and then cool it to room temperature under the protection of high-purity argon;

[0038] Under the protection of high-purity argon, add 0.0005mol Y (CCl 3 COO) 3 , and then add 20mL 1,3-dioxane and 0.005mol glycerol in turn, until the Y(CCl in the two-necked bottle 3 COO) 3 After it is completely dissolved, add 0.01mol of diethyl zinc dropwise into the bottle. During the process of adding diethyl zinc, the reaction temperature in the bottle is controlled at 20-25°C. After the reaction gas is released, the two-necked bottle is sealed and placed in a constant temperature water bath oscillator for aging to obtain a white suspension liquid, that is, a rare earth three-way catalyst. The aging conditions are: the temperature of the constant temperature water bath...

Embodiment 2

[0040] Evacuate the reactor at 80°C to 20-40Pa, fill it with CO 2 Treated for 2 hours, filled with CO 2 6 times, then cooled to room temperature; the rare earth three-way catalyst (0.0005mol yttrium trichloroacetate, 20mL1, 3-dioxane, 0.005mol glycerol, 0.01mol ZnEt 2 ) at CO 2 Put it into the reaction kettle under protection, and inject 100 mL of propylene oxide dissolved with 2.06 g of recrystallized lactide into the reaction kettle at the same time. The molar ratio of lactide to propylene oxide is 0.01431:1.431;

[0041] Put the reaction kettle into an adjustable constant temperature heating bath, quickly pass the carbon dioxide pressure regulator to make the carbon dioxide pressure in the kettle reach 4.0MPa under the condition of a stirring rate of 500rpm, the polymerization reaction temperature is 70°C, and the reaction time is 10 hours;

[0042] After the polymerization reaction is over, cool the reactor to room temperature with a cold water bath at a temperature of 1...

Embodiment 3

[0045] Evacuate the reactor at 80°C to 20-40Pa, fill it with CO 2 Treated for 2 hours, filled with CO 2 6 times, then cooled to room temperature; the rare earth three-way catalyst (0.0005mol yttrium trichloroacetate, 20mL 1,3-dioxane, 0.005mol glycerol, 0.01mol ZnEt 2 ) at CO 2 Put it into the reaction kettle under protection, and inject 100 mL of propylene oxide dissolved with 4.12 g of recrystallized lactide into the reaction kettle at the same time. The molar ratio of lactide to propylene oxide is 0.02862:1.431;

[0046] Put the reaction kettle into an adjustable constant temperature heating bath, quickly pass the carbon dioxide pressure regulator to make the carbon dioxide pressure in the kettle reach 4.0MPa under the condition of a stirring rate of 500rpm, the polymerization reaction temperature is 70°C, and the reaction time is 10 hours;

[0047] After the polymerization reaction is over, cool the reactor to room temperature with a cold water bath at a temperature of 1...

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Abstract

The invention discloses a method for preparing lactide-propylene oxide-CO2 terpolymer by using a rare earth three-way catalyst. The method comprises the following steps of: adding the rare earth three-way catalyst, lactide, propylene oxide and CO2 into a reaction kettle, and performing polymerization on the lactide, the propylene oxide and the CO2 under the action of the rare earth three-way catalyst to obtain the lactide-propylene oxide-CO2 terpolymer, wherein the rare earth three-way catalyst consists of trichloroacetic acid yttrium, diethyl zinc, glycerol and 1,3-dioxolane; a molar ratio of the trichloroacetic acid yttrium to the diethyl zinc to the glycerol is 1:20:10; and the concentration of the diethyl zinc in the 1,3-dioxolane is 0.5*10<-3>mol / ml. Compared with the prior art, the method has the advantages that: the polymerization of the lactide, the propylene oxide and the CO2 is catalyzed by the rare earth three-way catalyst, so the polymerization time is short; and the prepared terpolymer has the ether block content of less than 2 percent, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of polymers, more specifically, to a method for preparing lactide-propylene oxide-CO with a rare earth three-way catalyst 2 Terpolymer method. Background technique [0002] Polypropylene carbonate (PPC) is an alternating copolymer of carbon dioxide and propylene oxide. It is an environmentally friendly polymer material with excellent gas barrier properties, good biocompatibility and biodegradability. However, the glass transition temperature of polypropylene carbonate is low (T g =35~41℃), poor thermal stability and narrow thermal processing window (130~140℃), thus seriously affecting its processing performance and application range. [0003] At present, adopting physical blending modification to modify the self local defects of PPC is a common method to improve the performance of PPC. The Chinese patent literature with publication number CN1058408 has reported a modification method of aliphatic polycarbon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/64C08G63/87C08G63/84C08G63/83
Inventor 顾林赵晓江王献红王佛松
Owner 中科应化(长春)科技有限公司
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