The Azeotropic Polycondensation-depolymerization Method for Efficient Synthesis of Glycolide

WEN Liang; YIN Tian; XUE Ya-qi; MA Jian-gong

doi:10.14028/j.cnki.1003-3726.2023.04.005

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The Azeotropic Polycondensation-depolymerization Method for Efficient Synthesis of Glycolide

更新时间：2023-02-18

- The Azeotropic Polycondensation-depolymerization Method for Efficient Synthesis of Glycolide
- Polymer Bulletin Vol. 36, Issue 4, Pages: 459-465(2023)
- 作者机构：
  
  1.中国神华煤制油化工有限公司，北京　100011
  2.先进能源材料化学教育部重点实验室新能源转化与存储交叉科学中心　南开大学化学学院，天津　300071
- 作者简介：
- 基金信息：
- DOI：10.14028/j.cnki.1003-3726.2023.04.005
  CLC：
- Published：20 April 2023，
  
  Received：12 July 2022，
  
  Revised：17 September 2022，
扫描看全文
WEN Liang, YIN Tian, XUE Ya-qi, MA Jian-gong. The Azeotropic Polycondensation-depolymerization Method for Efficient Synthesis of Glycolide. [J]. Polymer Bulletin 36(4):459-465(2023)
DOI：

WEN Liang, YIN Tian, XUE Ya-qi, MA Jian-gong. The Azeotropic Polycondensation-depolymerization Method for Efficient Synthesis of Glycolide. [J]. Polymer Bulletin 36(4):459-465(2023) DOI： 10.14028/j.cnki.1003-3726.2023.04.005.

摘要

乙交酯是聚羟基乙酸的单体，乙交酯的合成直接影响聚羟基乙酸的合成。一般用羟基乙酸（酯）制备乙交酯，但是，制备乙交酯的缩聚过程需要真空高温的条件，消耗大量的能量。共沸缩聚-解聚法制备乙交酯的缩聚过程，具有条件温和、无催化剂、溶剂可回收的优点。羟基乙酸通过共沸缩聚-解聚法得到乙交酯。用X-射线粉末衍射、红外分析、差热分析等方法对聚羟基乙酸低聚物进行了表征。结果表明:羟基乙酸制备的聚羟基乙酸低聚物是一种半结晶聚合物，聚羟基乙酸低聚物解聚得到产率为81.26%和纯度为89.29%的乙交酯，并且解聚反应残渣可以重复利用来制备乙交酯。

Abstract

Glycolide is used to synthesize polyglycolic acid

which is highly demanded due to the promising mechanical property

biocompatibility and especially biodegradability for sustainable developement. The synthesis of polyglycolic acid is therefore significantly affected by the glycolide. Glycolide is generally prepared from glycolic acid (ester). However

the polycondensation of glycolic acid (ester) requires high energy consumption including vacuum and high temperature. Herein

we report a azeotropic polycondensationdepolymerization method for the synthesis of glycolide

enabling the polycondensation of glycolic acid into polyglycolic acid oligomers under mild conditions with recoverable solvent and no catalyst

which are subsequently depolymerized into glycolide finally. Polyglycolic acid oligomers was comprehensively characterized as a kind of semi-crystalline polymers with the number average molecular weight of 1900 g/mol and the crystallinity of 33.1% by X-ray powder diffraction

Fourier transform infrared spectroscopy

differential scanning calorimetry and other methods. The glycolide product is obtained from the depolymerization polyglycolic acid oligomers with a yield of 81.26% and a purity of 89.29%. Furthermore

the depolymerization reaction residues of polyglycolide acid oligomers can be reused to produce more glycolide. Our method provides a green way for the production of glycolide and polyglycolic acid oligomers

and should contribute to the sustainable development and energy-saving of polyglycolic acid in the areas of material

industry and environment

关键词

羟基乙酸聚羟基乙酸低聚物乙交酯缩聚解聚

Keywords

Glycolic acidPolyglycolic acid oligomersGlycolidePolycondensationDepolymerization

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