Page 105 - 《精细化工》2020年第6期

第 37 卷第 6 期 精 细 化 工 Vol.37, No.6
202 0 年 6 月 FINE CHEMICALS June 2020

功能材料
微波辅助制备 β-环糊精纳米海绵

*
乔宗梅，张阳倩，张毅民
（天津大学 绿色合成与转化教育部重点实验室，天津大学 化工学院，天津 300350）

摘要：利用微波辐射法制备了 β-环糊精纳米海绵（NSCD）。以 β-环糊精（β-CD）为单体，碳酸二苯酯（DPC）
为交联剂，以反应时间、反应温度和物料比为自变量，产物收率为响应指标，通过响应曲面法建立 Box-Behnken
模型对工艺优化及预测，得到最优反应条件为：反应时间 87 min，反应温度 90 ℃，物料物质的量比 n（β-CD）∶
n（DPC）= 1∶7.75，在该条件下产物实际收率为 68.92%。利用 FTIR、DSC、PXRD、SEM 和 BET 等方法对产
–1
物进行了表征。FTIR 结果显示，在 1757 cm 处出现新的羰基特征峰，表明 β-CD 与 DPC 交联成功；DSC 测得
分解温度在 260 ℃左右；PXRD 和 SEM 表明，微波法得到的产物其结晶度比传统加热法产物的结晶度更高；
BET 分析表明，随着物料 β-CD 与 DPC 物质的量比减小，产物比表面积增加，孔径减小。优化后的工艺方法相
较于传统方法反应时间缩短至原来的 1/4，收率提高约 20%。
关键词：β-环糊精；纳米海绵；碳酸二苯酯；响应曲面；微波辐射；功能材料
中图分类号：TQ317 文献标识码：A 文章编号：1003-5214 (2020) 06-1171-07

Microwave-assisted synthesis of β-cyclodextrin nanosponges

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QIAO Zongmei, ZHANG Yangqian, ZHANG Yimin
（Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and
Technology, Tianjin University, Tianjin 300350, China）

Abstract: β-cyclodextrin nanosponge (NSCD) was synthesized by microwave irradiation method. The
Box-Behnken design of response surface methodology was used to evaluate the interactive effects of
temperature, reaction time, n (β-CD)∶n (DPC) on the yield of NSCD. The optimum reaction conditions
were obtained as follows: the reaction time was 87 min, reaction temperature was 90 ℃，n (β-CD)∶
n (DPC)=1∶7.75. Under these reaction conditions, the yield of product was 68.92%. The products were
characterized by FTIR, DSC, PXRD, SEM and BET. FTIR suggested that the characteristic peak of
–1
carbonyl appeared at 1757 cm , indicating that β-CD and DPC were successfully crosslinked. The thermal
degradation temperature of NSCD was about 260 ℃. PXRD results showed that the obtained NSCD
prepared by microwave-assisted method had higher crystallinity than that prepared by conventional heating
method, consistent with SEM results. The BET analysis results revealed that the specific surface area of
product was increased with the increase of molar ratio of β-CD to DPC, while the pore size showed an
opposite change tendency. Compared with that of the traditional method, the reaction time of the optimized
process was shortened to 1/4 of the original one, and the yield was increased by 20%.
Key words: β-cyclodextrin; nanosponges; diphenyl carbonate; response surface; microwave irradiation;
functional materials

β-CD 具有外亲水内疏水的空腔结构，可以与一 物，但是对亲水性和大分子化合物的包合存在一定
[1]
系列空腔大小相匹配的亲脂性极性分子形成包合 局限性 。

收稿日期：2019-12-17; 定用日期：2020-03-12; DOI: 10.13550/j.jxhg.20191173
作者简介：乔宗梅（1993—），女，硕士生，E-mail：1749827520@qq.com。联系人：张毅民（1961—），男，副教授，E-mail：
zhangym@tju.edu.cn。