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

A technology of ternary catalyst and terpolymer, which is applied in the field of polymers and can solve problems such as unfavorable industrial production and long polymerization reaction time

Active Publication Date: 2012-01-25
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
  • 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-necked flask under reduced pressure at 80°C to 20-40Pa, replace it with high-purity argon every 20 minutes for 5 times, and then cool to room temperature under the protection of high-purity argon;

[0038] Under the protection of high-purity argon, 0.0005mol Y(CCl 3 COO) 3 , Then add 20mL 1,3-dioxolane and 0.005mol glycerol in turn, and wait for the Y(CCl 3 COO) 3 After all is dissolved, 0.01 mol of diethyl zinc is added dropwise to the bottle. During the process of adding diethyl zinc, the reaction temperature in the bottle is controlled at 20~25℃. After the addition of diethyl zinc is completed, there will be no more After the reaction gas is released, the two-necked bottle is sealed and placed in a constant temperature water bath shaker for aging to obtain a white suspension liquid that is a rare earth three-way catalyst. The aging conditions are: constant temperature water bath temperature of 60℃, m...

Embodiment 2

[0040] Evacuate the reactor at 80℃ to 20~40Pa, and charge CO 2 Treat for 2 hours, charge CO in total 2 6 times, and then cooled to room temperature; the rare earth ternary catalyst prepared in Example 1 (0.0005mol yttrium trichloroacetate, 20mL 1,3-dioxolane, 0.005mol glycerol, 0.01mol ZnEt 2 ) In CO 2 Add into the reactor under protection, and at the same time inject 100 mL of propylene oxide with 2.06 g of recrystallized lactide dissolved in the reactor, the molar ratio of lactide to propylene oxide is 0.01431:1.431;

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

[0042] After the polymerization reaction is over, the reactor is cooled to room temperature with a cold water bath at a temperature of 12-15...

Embodiment 3

[0045] Evacuate the reactor at 80℃ to 20~40Pa, and charge CO 2 Treat for 2 hours, charge CO in total 2 6 times, and then cooled to room temperature; the rare earth ternary catalyst prepared in Example 1 (0.0005mol yttrium trichloroacetate, 20mL 1,3-dioxolane, 0.005mol glycerol, 0.01mol ZnEt 2 ) In CO 2 Put it into the reactor under protection, and at the same time inject 100 mL of propylene oxide containing 4.12 g of recrystallized lactide into the reactor, the molar ratio of lactide to propylene oxide is 0.02862:1.431;

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

[0047] After the polymerization reaction is over, the reactor is cooled to room temperature with a cold water bath at a temperature of 12-1...

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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, and more specifically, to a preparation of lactide-propylene oxide-CO by using 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 relatively low (T g =35~41℃), poor thermal stability and narrow thermal processing window (130~140℃), which seriously affects its processing performance and application range. [0003] At present, the use of physical blending modification to modify the local defects of PPC is a common method to improve the performance of PPC. The Chinese patent document with publication number CN1058408 reports a modification method of aliphatic polycarbonate nit...

Claims

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Application Information

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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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