化工进展

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熔融/固相缩聚法制备聚乙醇酸甲酯的工艺条件优化

王泽云,崔爱军,陆卫良,陈 群,何明阳   

  1. 常州大学江苏省精细石油化工重点实验室,常州 213164
  • 出版日期:2012-12-05 发布日期:2012-12-05

Optimization on the synthesis process of polymethyl glycolate via melt/solid polycondensation

WANG Zeyun,CUI Aijun,LU Weiliang,CHEN Qun,HE Mingyang   

  1. Key Lab of Fine Petrochemical Engineering Changzhou University,Changzhou 213164,Jiangsu,China
  • Online:2012-12-05 Published:2012-12-05

摘要: 以乙醇酸甲酯为原料,先通过熔融缩聚法得到低聚物,然后进行固相缩聚法制备出高分子量的聚乙醇酸甲酯(PMG)。考察了工艺过程中催化剂的种类和用量、反应温度以及反应时间对PMG分子量的影响。并通过正交试验得到较优的合成条件为:催化剂二水合氯化亚锡的质量分数为0.5%,压力70 Pa,反应温度180 ℃,反应时间100 h,合成的PMG的特性黏度可达0.802 dL/g。采用傅里叶红外光谱(FT-IR)表征了PMG基团的特征吸收峰,差示扫描量热仪(DSC)表征了PMG的玻璃化温度、结晶温度和熔点。

关键词: 聚乙醇酸甲酯, 固相缩聚, 生物可降解材料, 正交试验

Abstract: Polymethyl glycolate (PMG) with high molecular weight was synthesized via melt/solid polycondensation with methyl glycolate as the starting material. By an orthogonal test, different catalysts, the amount of catalyst, reaction temperature, time and other factors were examined in the polymerization, and the optimal condition of the melt/solid polycondensation synthesis of high molecular weight ploymethyl glycolate was obtained as follows:reaction temperature 180℃,0.5% tin(Ⅱ) chloride dihydrate, 70 Pa , reaction time 100h. The intrinsic viscosity of PMG can reach 0.802 dL/g. The typical absorption peaks of PMG in Fourier transform infrared (FT-IR) spectra were measured, and the glass transition temperature, crystallization temperature and melting point were determined by differential scanning calorimetry (DSC).

Key words: ploymethyl glycolate, solid polycondensation, biodegradable materials, orthogonal test

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