Preparation method of polylactic acid-polyethylene glycol block copolymer

A block copolymer and polyethylene glycol technology, which is applied in the preparation of polylactic acid-polyethylene glycol block copolymer and the preparation of polyester polyether copolymer, can solve toxicity, high toxicity, adverse effects, etc. question

Inactive Publication Date: 2004-08-04
BEIJING TIANRUNXING BIO TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

HansR.Kricheldorf etc. used stannous octoate as catalyst, at 150℃, N 2 Under protection, bulk polymerization makes poly-L-lactic acid-polyethylene glycol block copolymer (Makromol.Chem., 1993,194:175), but, tin catalyst all has certain toxicity, accumulates in human body A certain amount will bring adverse effects to the body; Xiong Chengdong et al reported using triisobutylaluminum as a catalyst, in N 2 Under protection, 60-220°C, triggers bulk or solution copolymerization of lactone or lactide and polyether diol (Chinese invention patent, 94111738.3); but the triisobutyl aluminum selected by this technology has certain toxicity, and solution polymerization The selected solvent is an aromatic hydrocarbon, which is highly toxic and requires particularly strict reaction conditions; Y.Li, T.Kissel adopt aluminum isopropoxide as a catalyst, and prepare polyester polyether copolymer ( J. Control. Release. 27 (1993) 247-257)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1: Add 47.5g of D, L-lactide, 2.5g of polyethylene glycol with a molecular weight of 6000 and 0.4g of calcium hydride in a 250ml reaction bottle. After 4 hours of vacuuming, the pressure in the bottle reaches -0.01Ma, and the bottle is sealed. The reaction bottle was immersed in an oil bath, heated to 140°C, reacted for 10 hours, cooled to stop the reaction, added acetone to dissolve, first precipitated with distilled water, then with absolute ethanol, and vacuum dried to obtain 41g of the product. The molecular weight of the polymer measured by GPC was 118,000, and the molecular weight distribution was 1.85.

Embodiment 2

[0012] Example 2: Add 45g of D, L-lactide, 5g of polyethylene glycol with a molecular weight of 3000 and 0.8g of calcium hydride in a 250ml reaction bottle. After 4 hours of vacuuming, the pressure in the bottle reaches -0.08Ma, and the reaction bottle is sealed , immersed in an oil bath, heated to 160°C, reacted for 8 hours, cooled to stop the reaction, added acetone to dissolve, first precipitated with distilled water, then precipitated with absolute ethanol, and obtained 41g of the product after vacuum drying. The polymer molecular weight measured by GPC was 58,000, and the molecular weight distribution was 1.55.

Embodiment 3

[0013] Example 3: Add 45g D, L-lactide, 5g polyethylene glycol with a molecular weight of 1000 and 0.3g calcium hydride in a 250ml reaction bottle, after vacuuming for 3.5 hours, the pressure in the bottle reaches -0.05Ma, and seal the reaction bottle , immersed in an oil bath, heated to 130°C, reacted for 11 hours, cooled to stop the reaction, added acetone to dissolve, first precipitated with distilled water, then precipitated with absolute ethanol, and obtained 34g of the product after vacuum drying. The molecular weight of the polymer measured by GPC was 11,000, and the molecular weight distribution was 1.95.

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Abstract

A process for preparing the polylactic acid-polyethanediol block copolymer is prepared through the copolymerizing reaction between polyethanediol and lactide at 130-160 deg.C under -0.08-0.01 MPa and existance of calcium hydride for 8-12 hr, adding acetone for dissolving, deposition in distilled water and then in absolute alcohol, and vacuum drying.

Description

technical field [0001] The invention relates to a preparation method of a polyester polyether copolymer, more precisely, the invention relates to a preparation method of a polylactic acid-polyethylene glycol block copolymer, which belongs to the field of biomedical polymer materials. Background technique [0002] In the past ten years, with the development of drug controlled release system and tissue engineering technology, biodegradable materials have been developed rapidly, and their application scope involves almost all non-permanent implant devices, including drug controlled release carriers, surgical sutures, etc. Sutures, internal fixation devices for fractures, artificial skin, surgical anti-adhesion membranes and tissue engineering, etc. The homopolymer of lactide, polylactic acid and its copolymer with glycolide, has good biocompatibility, non-toxic, biodegradable and can be metabolized by the body after fulfilling its purpose without leaving any Traces and other a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48
Inventor 杜丽娟吕卓
Owner BEIJING TIANRUNXING BIO TECH DEV
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