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ε-caprolactone and l-lactide copolymerization catalyst and copolymerization method

A technology of copolymerization catalyst and lactide, which is applied in the field of L-lactide and ε-caprolactone copolymerization catalyst and copolymerization, can solve the problems of poor permeability degradation speed, slow melting point degradation speed, etc., and achieve the effect of broadening the application range

Active Publication Date: 2019-05-17
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention uses metal zinc complexes to catalyze the copolymerization of caprolactone and lactide to obtain block copolymers and random copolymers with high molecular weight, improve the defects of single polymers in material properties, make their advantages and disadvantages complement each other, and make up for it. The shortcoming of polycaprolactone's low melting point, insufficient hardness and slow degradation rate, and the poor permeability of polylactide to drugs and too fast degradation rate, the synthesized biodegradable copolymer broadens the range of polymers. Application range

Method used

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  • ε-caprolactone and l-lactide copolymerization catalyst and copolymerization method
  • ε-caprolactone and l-lactide copolymerization catalyst and copolymerization method
  • ε-caprolactone and l-lactide copolymerization catalyst and copolymerization method

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Embodiment 1

[0030]

[0031] Under the protection of nitrogen, add 0.048mmol of catalyst 1 to the polymerizer, add 14.4mL of toluene, add ε-caprolactone (0.493g, 4.32mmol) into the polymerization system, react at 90°C for 1h, then add L-lactide (0.761g, 5.28mmol) was polymerized for 12h, then quenched by adding glacial acetic acid, and finally the copolymer was precipitated with methanol to form a PCL block PLLA copolymer. Dry in a vacuum oven for 24 hours. ε-caprolactone conversion: 96%, L-lactide conversion: 95%, M n = 18214 g / mol, molecular weight distribution PDI = 1.32. The melting points of the polymers are: 50.6°C and 166.1°C.

Embodiment 2

[0033]Under the protection of nitrogen, add 0.048mmol of catalyst 1 to the polymerizer, add 14.4mL of toluene, add ε-caprolactone (0.548g, 4.80mmol) into the polymerization system, react at 90°C for 1h, then add L-lactide (0.691g, 4.80mmol) was polymerized for 12h, then quenched by adding glacial acetic acid, and finally the copolymer was precipitated with methanol to form a PCL block PLLA copolymer. Dry in a vacuum oven for 24 hours. ε-caprolactone conversion: 97%, L-lactide conversion: 99%, M n = 19518 g / mol, molecular weight distribution PDI = 1.30. The melting points of the polymer are: 51.6°C and 164.2°C ( figure 1 ).

Embodiment 3

[0035] Under the protection of nitrogen, add 0.048mmol of catalyst 1 to the polymerizer, add 14.4mL of toluene, add ε-caprolactone (0.602g, 5.28mmol) into the polymerization system, react at 90°C for 1h, then add L-lactide (0.622g, 4.32mmol) was polymerized for 12h, then quenched by adding glacial acetic acid, and finally the copolymer was precipitated with methanol to form a PCL block PLLA copolymer. Dry in a vacuum oven for 24 hours. ε-caprolactone conversion: 97%, L-lactide conversion: 99%, M n = 19047 g / mol, molecular weight distribution PDI = 1.31. The melting points of the polymers are: 52.4°C and 163.7°C.

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Abstract

The invention discloses an epsilon-caprolactone and L-lactide copolymerizing catalyst and a copolymerizing method. The catalyst is a beta-pyridine enol zinc complex. The copolymerizing method comprises the following steps of firstly, adding a beta-pyridine enol zinc catalyst into a methylbenzene solvent; sequentially adding two monomers into a catalyzing system, and performing block copolymerizing reaction; or, simultaneously adding the two monomers into the reaction system according to different ratio, and performing irregular copolymerizing reaction, so as to obtain a block copolymer or an irregular copolymer. The epsilon-caprolactone and L-lactide copolymerizing catalyst and the copolymerizing method have the advantages that the monomer price is low; a zinc element is a necessary element of an organism, the toxicity and pollution are avoided, the catalytic activity is higher, and the polymerizing method is simple; the block copolymer and the irregular copolymer of L-lactide and epsilon-caprolactone with higher molecular weight can be obtained, the defect of a single polymer is overcome, and a synthesized biodegradable copolymerizing material can widen the application range of the polymer.

Description

technical field [0001] The invention relates to a L-lactide and ε-caprolactone copolymerization catalyst and a copolymerization method. Background technique [0002] Polymer polyester is a synthetic material widely used in film, fiber, clothing and other fields after polyolefin. [0003] Aliphatic polyester materials have been widely studied because of their good biocompatibility and degradability, and have been widely used in the field of biomedicine in recent years. Such as drug slow-release materials, implants in vivo, surgical sutures, orthopedic fixation and tissue repair materials, etc.; in addition, some progress has been made in the application of packaging industry, textile industry and agricultural industry. The good mechanical processing performance, easy degradation and environmental friendliness of polyester materials determine that it will become an important substitute for polyolefin materials in the future when petroleum resources are increasingly tight, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/83C08G63/08
CPCC08G63/08C08G63/823C08G63/83
Inventor 陈霞肖霞白建良
Owner SHANXI UNIV