水引发L-丙交酯开环聚合工艺研究

doi:10.13475/j.fzxb.20200303905

摘要/Abstract

摘要：

针对L-丙交酯本体开环聚合中富羟基水的存在导致产物聚乳酸相对分子质量偏低的问题,选用辛酸亚锡为催化剂,研究了L-丙交酯重结晶次数、精制L-丙交酯干燥时间及聚合前反应釜内真空干燥时间3项关键水分控制工艺对聚乳酸相对分子质量的影响。借助核磁共振仪、红外光谱仪、差示扫描量热仪和热重分析仪表征并分析了聚乳酸的化学结构和热力学性能。结果表明:增加L-丙交酯重结晶次数,延长精制L-丙交酯干燥时间以及延长聚合前反应釜内真空干燥时间,均不同程度上有助于提高聚乳酸的黏均分子量;与低黏均分子量聚乳酸相比,高黏均分子量的聚乳酸熔点提高至175 ℃,有较好的热稳定性。

关键词: L-丙交酯, 开环聚合, 黏均分子量, 引发剂, 热稳定性, 聚乳酸聚合工艺

Abstract:

The presence of hydroxyl-rich water in the bulk ring-opening polymerization of L-lactide (LLA) leads to lower molecular weight of obtained poly(L-lactide) (PLLA). In order to solve this problem, several moisture controlling technologies including purification of LLA monomer, drying of refined LLA and vacuum drying in the reactor before polymerization were investigated for their effects on the molecular weight of PLLA using stannous (Ⅱ) ethylhexanoate (Sn(Oct)₂) as the catalyst. Nuclear magnetic resonance spectrometer, Fourier transform infrared spectrometer, differential scanning calorimeter and thermogravimetric analysis were used to analyze the chemical structure and thermodynamic properties of PLLA. The results show that increasing purification times of LLA, extending drying time of refined LLA and extending the vacuum drying time in the reactor before polymerization all contribute to the increase of viscosity average molecular weight of PLLA. Compared with low viscosity average molecular weight PLLA, the high viscosity average molecular weight PLLA has a higher melting point of 175 ℃ and better thermal stability.

Key words: L-lactide, ring-opening polymerization, viscosity average molecular weight, initiator, thermal stability, poly(L-lactide) polymerization process

中图分类号:

O631.5

温馨, 张须臻, 李勇, 黄文健, 卢晨. 水引发L-丙交酯开环聚合工艺研究[J]. 纺织学报, 2020, 41(12): 21-25.

WEN Xin, ZHANG Xuzhen, LI Yong, HUANG Wenjian, LU Chen. Study on water-initiated ring-opening polymerization technology of L-lactide[J]. Journal of Textile Research, 2020, 41(12): 21-25.

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