High-purity glycolide preparation method

A glycolide, high-purity technology, applied in the field of preparation of high-purity glycolide, can solve the problems of low lactide yield, high cost, low purity, etc., and achieve the effect of less by-products and short reaction time

Active Publication Date: 2019-11-29
SHANDONG GUYUCHUN BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Usually glycolide is synthesized by using low-molecular-weight polyglycolic acid as an intermediate through pyrolysis. The glycolide synthesized by this method contains impurities such as water, glycolic acid and glycolic acid oligomers, and the purity is not high. Multiple purifications are required, which leads to low lactide yield and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A preparation method of high-purity glycolide, comprising steps as follows:

[0038] Weigh 500g of glycolic acid, pour it into a three-necked flask equipped with a thermometer, a condensation device and a stirrer, heat slowly to boiling, decompress and dehydrate at a pressure of 0.04~0.06MPa, add 4g of zinc oxide (glycolic acid Its mass ratio is 125), keep the dehydration under reduced pressure for 2 hours, and the pressure is 0.06-0.09MPa, so that glycolic acid can be polycondensed into glycolic acid oligomers. The pressure is 1500Pa~0.1MPa, and the crude glycolide is collected by the three-stage cooling collection system. The product is a yellow solid, and the crude product yield is 92%. The crude product is dissolved in methanol, cooled, filtered, recrystallized with methanol three times, and dried in vacuum The finished product is obtained when the weight is constant, the yield is 78%, and the purity of glycolide is 99.92% after inspection.

Embodiment 2

[0040] A preparation method of high-purity glycolide, comprising steps as follows:

[0041] Weigh 500g of glycolic acid, pour it into a three-necked flask equipped with a thermometer, condensing device and stirrer, slowly heat to boiling, decompress and dehydrate at a pressure of 0.04~0.06MPa, add 2g of antimony trioxide ( The ratio of glycolic acid to its mass is 250), keep dehydration under reduced pressure for 6 hours, and the pressure is 0.06-0.09MPa, so that glycolic acid can be polycondensed into glycolic acid oligomers. , the distillation pressure is 1500Pa~0.1MPa, the crude glycolide is collected by a three-stage cooling collection system, the product is a yellow solid, and the yield of the crude product is 94%. Recrystallize three times, vacuum dry to constant weight to get the finished product, the yield is 77%, and the purity of glycolide is 99.95% after inspection.

Embodiment 3

[0043] A preparation method of high-purity glycolide, comprising steps as follows:

[0044] Weigh 500g of glycolic acid, pour it into a three-neck flask equipped with a thermometer, a condensation device and a stirrer, heat slowly to boiling, decompress and dehydrate at a pressure of 0.05~0.06MPa, add 5g of alumina (glycolic acid) when the temperature rises to 150°C Its mass ratio is 100), keep the dehydration under reduced pressure for 7 hours, and the pressure is 0.07-0.09MPa, so that glycolic acid can be polycondensed into glycolic acid oligomers. The pressure is 1500Pa~0.1MPa, and the crude glycolide is collected by the three-stage cooling collection system. The product is a yellow solid, and the crude product yield is 90%. The crude product is dissolved in methanol, cooled, filtered, recrystallized with methanol three times, and dried in vacuum The finished product is obtained when the weight is constant, the yield is 76%, and the purity of glycolide is 99.93%.

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Abstract

The invention provides a high-purity glycolide preparation method, which comprises: preparing a polyglycolide (PGA) oligomer through pressure reducing dehydration, carrying out high-temperature cracking distillation to obtain crude glycolide, and finally purifying to obtain the polymer-grade high-purity glycolide. According to the present invention, the method has characteristics of low reaction conditions, rapid reaction, short reaction time and high purity of the purified glycolide, and can meet the requirements in polymerization of high-molecular-weight polyglycolide.

Description

technical field [0001] The invention relates to a method for preparing high-purity glycolide, which belongs to the technical field of organic polymers. Background technique [0002] Polyglycolide (PGA) is a biodegradable polymer material. It is non-toxic, non-irritating, has excellent biocompatibility, can be biodegraded and absorbed, has high strength, good plasticity, and is easy to process and shape. In recent years, polyglycolide and polyglycolide copolymers have been widely used in the fields of biomedical materials such as surgical sutures, drug controlled release, and artificial tissues. [0003] At present, the methods for synthesizing polyglycolide mainly include direct polycondensation method and glycolide ring-opening polymerization method. The direct polycondensation method uses glycolic acid for direct dehydration polycondensation, and generally only oligomers with relative molecular weights of tens to thousands can be obtained. , it is difficult to meet the pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 赵春华苏红清袁文博陈儒浩李建
Owner SHANDONG GUYUCHUN BIOTECHNOLOGY CO LTD
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