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Method for preparing chitosan-polylactic acid grafted copolymer

A technology of graft copolymer and polylactic acid, which is applied in the field of chitosan-polylactic acid graft copolymer and its preparation, can solve the problems of complex process and difficult control of product structure, and achieve the goal of overcoming acidic environment, eliminating bacteria and Effect of sterility response, slow degradation rate

Inactive Publication Date: 2003-05-21
TIANJIN UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another method for the copolymerization of chitosan and polylactic acid is to first hydroxylate chitosan ether, and then carry out graft copolymerization with lactide, [Zhou Changren, Li Lihua. Chinese patent, application number: 01114656.7], the process of this method Complex, difficult to control product structure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Dehydrate a certain amount of 88% L-lactic acid aqueous solution at 150°C, react for 2 hours under normal pressure, and gradually reduce the pressure to 1.3×10 4 React for 2h under Pa, and finally in 4×10 3 React under the pressure of Pa for 4h to obtain viscous L-lactic acid oligomer [OLLA].

[0016] Add 230g of L-lactic acid oligomer to a 250ml three-necked bottle, and add 0.4% SnCl of 1-lactic acid oligomer at the same time 2 2H 2 O and SnCl 2 2H 2 O equimolar p-toluenesulfonic acid. Turn on stirring, heat the mixture to 180°C, and gradually reduce the pressure to 1.06×10 3 Pa, reaction 4h.

[0017] After the reaction, the product was dissolved in 300ml of chloroform, and then precipitated with 1500ml of ether under strong mechanical stirring. After filtering under reduced pressure, it was dried in a vacuum oven at room temperature for 12 hours to finally obtain a white fibrous solid product with a yield of 92%, and the obtained polylactic acid had a molecular...

Embodiment 2

[0022] Dehydrate a certain amount of 88% L-lactic acid aqueous solution at 150°C, react for 2 hours under normal pressure, and gradually reduce the pressure to 1.3×10 4 React for 2h under Pa, and finally in 4×10 3 Under the pressure of Pa, the reaction was carried out for 4 hours to obtain a viscous L-lactic acid oligomer. The product was dissolved in 300 ml of acetone and then precipitated with 1500 ml of water under vigorous mechanical stirring. After filtering under reduced pressure, it was dried in a vacuum oven at room temperature for 12 hours to finally obtain a white powdery solid product with a yield of 97%, and the obtained polylactic acid had a molecular weight of 900.

[0023] The lactic acid oligomers obtained above were subjected to esterification and oxidation reactions in the same manner as in Example 1, and the yields of the esterification reactions were 85% and 90%.

[0024] The hydroformylated polylactic acid and chitosan were grafted according to the metho...

Embodiment 3

[0026] Polylactic acid was synthesized according to the method described in Example 1. The esterification reaction was carried out according to the method of Example 1, but the dihydric alcohol used was 1,4-butanediol, and the reaction was carried out for 4 hours, and the yield of the esterification product was 89.6%.

[0027] The oxidation reaction process of the esterification product was the same as in Example 1, and the yield of the hydroformylation product was 92%.

[0028] The hydroformylated polylactic acid and chitosan were grafted according to the method described in Example 1 to obtain a light yellow powdery solid with a yield of 98%.

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Abstract

The preparation method of chitosan-polylactic acid graft copolymer includes the following steps: utilziing melt condensation reaction to obtain polylactic acid with lower molecular weight, and utilizing esterification and oxidation reaction to convert the hydroxyl group of polylactic acid into aldehyde group, and making the hydroformylated polylactic acid react with chitosan so as to obtain the invented product with good working property, high hydrophilic property and good biological compatibility.

Description

technical field [0001] The invention relates to a biodegradable medical material, in particular to a chitosan-polylactic acid graft copolymer and a preparation method thereof. Background technique [0002] As a synthetic and molecular material with good biocompatibility and degradability, polylactic acid has been widely used in the field of biomedicine. However, due to the strong acidity of lactic acid, the initial product of polylactic acid degradation, its local accumulation will have a certain stimulating effect on the tissue. When it is implanted in the animal body, there are obvious capillary congestion and inflammatory cell infiltration, especially around the material. occur. [0003] Chitosan derivatives themselves have some physiological activities. It has free amino groups and is weakly alkaline. It can effectively adjust the pH value of the human body, prevent acidification, and improve the activity and phagocytosis of macrophages. It...

Claims

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Application Information

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IPC IPC(8): C08G81/00
Inventor 姚康德姚芳莲刘畅陈炜
Owner TIANJIN UNIV
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