第 48 卷第 2 期 Vol. 48 No. 2 2018 年 4 月 Apr 2018

所属栏目：功能材料 乙酰基封端烯丙醇聚醚的合成

万庆梅1，王胜利2，刘志湘1 （1.浙江皇马科技股份有限公司，浙江 上虞 312363；2.浙江绿科安化学有限公司，浙江 上虞 312359）

摘　要：以乙酸酐为封端剂，合成乙酰基封端烯丙醇聚醚，考察了乙酸酐和烯丙醇聚醚的物质的量比、反应温度、反应时间等条件对封端反应的影响。优化了反应条件：n（乙酸酐）∶n（烯丙醇聚醚）=1.5∶1.0，120～125℃回流反应3 h。真空脱酸脱除过量的乙酸酐和生成的乙酸，最后使用庚烷共沸脱除微量的乙酸和乙酸酐。优化条件下，乙酰基封端烯丙醇聚醚的封端率达95%以上，双键保护率达90%以上，酸值小于0.1 mg KOH·g-1。用红外光谱和凝胶色谱对反应产物进行了表征。

关键词：封端聚醚；烯丙醇聚醚；酯化封端

中图分类号：TQ328.3 TQ423　　文献标识码：A　　文章编号：1009-9212（2018）02-0059-03

Synthesis of Acetyl Capped Allyl Alcohol Polyether

WAN Qing-mei1, WANG Sheng-li2, LIU Zhi-xiang1 (1. Zhejiang Huangma Technology Co.,Ltd., Shangyu 312363, China; 2. Zhejiang Lükean Chemical Co., Ltd., Shangyu 312369, China)

Abstract：Using acetic anhydride as end-capping reagent, allyl alcohol polyether and acetic anhydride were reacted to obtain acetyl capped allyl alcohol polyether. Effects of factors including molar ratio of acetic anhydride and allyl alcohol polyether, reaction temperature, reaction time on the results of reaction were investigated. The optimal conditions were determined as: n(acetic anhydride)∶n(allyl alcohol polyether) equaled 1.5∶1.0; reaction temperature was of 120～125℃and reaction time was of 3 h. Excess acetic anhydride and acetic acid in the reaction were removed using vacuum pump and less acetic anhydride and acetic acid were distilled with heptane. The yield of end-capping reaction reached more than 95%. The retaining ratio of double bonds was more than 90% and the acid value was less than 0.1 mg KOH·g-1. The reaction products were characterized by the FTIR and GPC.

Key words：end capping polyether; allyl alcohol polyether; envelop-end of esterification

作者简介：万庆梅（1979-），女，山东德州人，高级工程师，硕士研究生，研究方向：表面活性剂的研究与开发（E-mail：wanqingmei@huangma.com）。

收稿日期：2018-04-22