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Method for preparing poly (lactic-co-glycolic acid)

A technology of polylactide and lactide, which is applied in the field of synthesis of medical absorbable copolymer polylactide, can solve the problem of expensive monitoring devices, no mention of copolymer thermal stability and molecular weight distribution, product heat Poor stability and other problems, to achieve the effect of broad copolymerization temperature and copolymerization time, highly controllable fine structure, and good processing thermal stability

Active Publication Date: 2008-02-20
HUIZHOU HUAYANG MEDICAL EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high catalyst consumption, low catalytic activity, poor product thermal stability, and large molecular weight degradation during melt processing.
[0011] Chinese patent (application number 200410025458.9, publication number CN1712426) adopts supercritical carbon dioxide fluid as reaction medium, uses metal, metal oxide or metal salt as initiator, and takes lactide and glycolide mixture as raw material to prepare copolymer PLGA, There are also problems such as poor thermal stability caused by high catalyst content, and large molecular weight degradation during melt processing.
[0013] Chinese patent (application number 200580008598.8, publication number CN1934161) uses strongly acidic ion exchange resins to catalyze the copolymerization of lactide and glycolide. This method also has the problems of high catalyst consumption and low product molecular weight.
The monitoring device of this method is extremely expensive, and the reaction cost is high, which is not conducive to the promotion of the technology. In addition, it does not mention the thermal stability and molecular weight distribution of the copolymer.

Method used

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  • Method for preparing poly (lactic-co-glycolic acid)
  • Method for preparing poly (lactic-co-glycolic acid)
  • Method for preparing poly (lactic-co-glycolic acid)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0137] Embodiment 1: Preparation of 90 / 10 glycolide / L-lactide copolymer

[0138] Catalyst preparation: The molar ratio of stannous octoate / benzyl alcohol / tri-p-hydroxyphenylphosphine is 1 / 15.0 / 1.5, with stannous octoate as the nominal name, toluene as the solvent, and a catalyst solution with a concentration of 0.012 mol / liter .

[0139] Accurately weigh 2088 grams of glycolide with a melting range of 82.0 to 82.5°C and 288 grams of L-lactide with a melting range of 95.5 to 96.1°C, add them to the reaction vessel, and then add 8.33ml of the prepared catalyst solution, that is, single The molar ratio of body / catalyst was 200,000.

[0140]At room temperature, absolute vacuum pressure ≤ 0.1mmHg, vacuumize for 24 hours to remove toluene solvent. Fill with high-purity nitrogen (99.999%) to keep the pressure at 0.035-0.050MPa. Raise the temperature to 98.0-105°C, stir for 1 hour, then raise the temperature to 205°C at a heating rate of 13-15°C / 10 minutes, and react for 15 hours. ...

Embodiment 2

[0158] Embodiment two: preparation 90 / 10 glycolide / L-lactide copolymer

[0159] Catalyst preparation: The molar ratio of triethylaluminum / dodecyl alcohol / 2,4,6-collidine is 1 / 10.0 / 2.5, with triethylaluminum as the nominal, toluene as the solvent, and the prepared concentration 0.0048 mol / L catalyst solution.

[0160] Accurately weigh 1044 grams of glycolide (melting range: 82.0-82.5°C) and 144 grams of L-lactide (melting range: 95.5-96.1°C) into the reaction vessel, then add 20.83ml of the prepared catalyst solution, The monomer / catalyst molar ratio was 100,000. At room temperature, absolute vacuum pressure ≤ 0.1mmHg, vacuumize for 24 hours to remove toluene solvent. Fill with high-purity nitrogen (99.999%) to keep the pressure at 0.035-0.050MPa. Raise the temperature to 98.0-105°C, stir for 1 hour, then raise the temperature to 185°C at 13-15°C / 10 minutes, and react for 12 hours. Stop the reaction, cool to room temperature, take out the material, crush it, and put the cru...

Embodiment 3

[0168] Embodiment three: prepare the copolymer of 15 / 85 glycolide / DL-lactide

[0169] Catalyst preparation: according to the molar ratio of lanthanum isopropoxide / benzyl alcohol / triisobutylphosphine as 1.0 / 15.0 / 1.0, with lanthanum isopropoxide as the nominal and toluene as the solvent, prepare a catalyst solution with a concentration of 0.01 mol / liter .

[0170] Accurately weigh 52.2 grams of glycolide (melting range: 82.0-82.5°C) and 367.2 grams of DL-lactide (melting range: 123.4-124.1°C) into the reaction vessel, then add 6.0ml of the prepared catalyst solution, The monomer / catalyst molar ratio was 50,000. At room temperature, absolute vacuum pressure ≤ 0.1mmHg, vacuumize for 24 hours to remove toluene solvent. Fill with high-purity nitrogen (99.999%) to keep the pressure at 0.035-0.050MPa. Raise the temperature to 128.0-135.0°C, stir for 1 hour, then raise the temperature to 165°C at 13-15°C / 10 minutes, and react for 15 hours. Stop the reaction, cool to room temperatur...

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Abstract

The invention provides a preparation method of a lactic and glycolic acid. The method comprises a catalyst containing three compounds of a catalytic induction system. The catalyst catalyzes and induces ring cleavage copolymerization between diglycolide and lactide to synthesize lactic and glycolic acid. The monomer to catalyst (mol ratio) is at 20,000 to 500,000 and the reaction temperature is 100 to 220 DEG C for 1 to 200 hours with inert gas protection or in vacuum. The invention has the advantages of high transformation ration, low catalyst contents of products, high molecular weight, narrow molecular weight disposition, good heat stability, small degradation of high temperature molten, good uniformity of materials, and is provided with excellent biological degradability and biological compatibleness. The lactic and glycolic acid prepared by the invention can be widely used for surgical operation suture, internal fixation of fracture, tissue repair, plastic surgery, anti-organic conglutination, medical slow release, organic engineering, etc.

Description

technical field [0001] The present invention relates to a synthetic method of polyester polymer material, in particular to a synthetic method of medical absorbable copolymer polylactide Background technique [0002] Polyglycolide, which is prepared by ring-opening copolymerization of glycolide and lactide (L-lactide or / and DL-lactide) monomers, not only has good biodegradability, biocompatibility, It is widely used in the field of biomedical materials such as surgical sutures, internal fixation of fractures, tissue repair, plastic surgery, anti-tissue adhesion, drug sustained release, tissue engineering, etc. [0003] There are currently two ways for the copolymerization of polylactide, one is to use glycolic acid (glycolic acid), lactic acid CH 3 The direct polycondensation method of CH(OH)COOH as the raw material, the molecular weight of the copolymer obtained by this method is low, and the application is greatly limited; the second is to make glycolic acid and lactic aci...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/85
Inventor 潘高峰孟永刚
Owner HUIZHOU HUAYANG MEDICAL EQUIP
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