低取代羟丙基纤维素的制备工艺优化探析

谈友丹 庄利欢 王文聪 王鸿博

摘要： 文章采用液相法制备低取代羟丙基纤维素（L-HPC），设计L9（34）正交实验以浊度值为间接判定指标讨论并确立了制备L-HPC的最佳碱化温度、碱化时间、碱化质量分数和醚化温度，通过气相色谱（GC）、FT-IR、XRD和偏光显微镜表征了不同醚化程度L-HPC的结构和性能。结果表明，在固定醚化剂环氧丙烷（PO）与纤维素质量比为17的情况下，碱化温度20 ℃、碱化时间2 h、碱化质量分数20%、醚化温度85 ℃时可以制备得到在碱液中溶解性能相对最优的L-HPC。此外，纤维素经醚化改性后部分羟基基团成功被羟丙基基团取代得到L-HPC，易溶于弱碱，随着醚化程度的加深，L-HPC在碱液中的溶解性提高，但结晶度有所下降，L-HPC膜的力学性能提高。

关键词： 低取代羟丙基纤维素（L-HPC）;液相法;正交;溶解性;醚化程度;力学性能

中图分类号： TS102.52

文献标志码： A

文章编号： 10017003（2021）07003207

引用页码： 071106

DOI： 10.3969/j.issn.1001-7003.2021.07.006（篇序）

Research on the optimizing preparation technology of L-HPC

TAN Youdan， ZHUANG Lihuan， WANG Wencong， WANG Hongbo

（a.College of Textile Science and Engineering; b.Education Ministry Key Laboratory of Science & Technology for Eco-Textiles，Jiangnan University， Wuxi 214122， China）

Abstract： Using liquid phase method， the paper has prepared thelow-substituted hydroxypropyl cellulose（L-HPC）. The optimum alkalinization temperature， alkalinization time， alkalinization concentration and etherification temperature for the preparation of L-HPC were discussed and established by using turbidity value as indirect determination index in an designed L9（34） orthogonal experiment. The structure and properties of L-HPC with different etherification degrees were characterized by gas chromatography（GC）， FT-IR， XRD and polarizing microscope. The results have shown that under the condition that the mass ratio of propylene oxide（PO） to cellulose was 1.7， and when the etherifying agent was fixed， the alkaline temperature was 20 ℃， the alkaline time was 2 h， the alkaline concentration was 20%， and the etherifying temperature was 85 ℃， L-HPC with optimal solubility in the alkaline solution could be prepared. In addition， after the cellulose was modified by etherification， some hydroxyl groups were successfully replaced by hydroxypropyl groups to obtain L-HPC， which was easily soluble in weak base. With the deepening of etherification， the solubility of L-HPC in alkali liquor increased， but the crystallinity decreased， and the mechanical properties of L-HPC membrane were improved.

Key words： low-substituted hydroxypropyl cellulose（L-HPC）; liquid phase method; orthogonal; solubility; etherification degree; mechanical property

收稿日期： 20201221;

修回日期： 20210624

基金項目： 国家自然科学基金项目（51703085）;江苏省自然科学基金项目（BK20170189）;中国博士后科学基金项目（2019M651574）;江苏省博士后科研资助计划项目（2018K108C）

作者简介： 谈友丹（1995），女，硕士研究生，研究方向为功能纺织材料。通信作者：王文聪，副教授，wencong828@hotmail.com。

羟丙基纤维素（Hydroxypropyl Cellulose，HPC）是纤维素与环氧丙烷（Propylene Oxide，PO）或氯代丙醇进行醚化反应后得到的一种非离子型纤维素醚[1]。区分高取代羟丙基纤维素（H-HPC）和低取代羟丙基纤维素（L-HPC）的依据就是其羟丙氧基含量的不同[2]。H-HPC（羟丙氧基含量≥20%）具有良好的悬浮、黏结、乳化、热塑等性能，广泛地应用于食品、建筑和智能材料等领域[3]。L-HPC（羟丙氧基含……