CN106905533A - 一种利用高内相乳液模版法制备表面β‑环糊精修饰的多孔吸附材料的方法 - Google Patents

一种利用高内相乳液模版法制备表面β‑环糊精修饰的多孔吸附材料的方法 Download PDF

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CN106905533A
CN106905533A CN201710101610.4A CN201710101610A CN106905533A CN 106905533 A CN106905533 A CN 106905533A CN 201710101610 A CN201710101610 A CN 201710101610A CN 106905533 A CN106905533 A CN 106905533A
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袁伟忠
陈相南
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Abstract

本发明属于高分子材料、环境功能材料制备领域，具体涉及一种利用高内相乳液模版法制备表面β‑环糊精修饰的多孔吸附材料的方法。制备方法是利用非离子表面活性剂来稳定高内相乳液，以水为分散相，甲基丙烯酸缩水甘油酯单体、交联剂二乙烯基苯、致孔剂甲苯为连续相，在引发剂存在下，通过高内相乳液模版法制得多孔泡沫材料；通过表面修饰在泡沫材料表面引入β‑环糊精，最终得到表面β‑环糊精修饰的多孔泡沫材料。本发明所得到的产品不仅含有丰富的孔道结构和功能基团，表面的β‑环糊精结构，能有效吸附水中微量有机物吸，如2,4‑二氯苯酚、2‑萘酚、双酚A、双酚S等芳香烃，而且具有可重复使用效能。

Description

一种利用高内相乳液模版法制备表面β-环糊精修饰的多孔吸 附材料的方法
技术领域
本发明属于高分子材料和环境功能材料制备领域，具体涉及一种利用高内相乳液模版法制备表面β-环糊精修饰的多孔吸附材料的方法。
背景技术
高内相乳液模版法因其制备所得多孔材料具有低密度和高度多孔性，可相对方便地加工与化学改性。与其它制备多孔材料的方法相比，该法具有可精确控制孔及通道直径的大小和分布的优点而成为制备聚合物多孔材料最为有效的方法之一。该种方法适合被用作制备吸附材料，所制备材料不尽吸附效率高且可回收利用，同时通过孔壁改性可使材料具有良好的选择吸附性。
Song Yang等人(S. Yang, C. Nie, et al. European Polymer Journal, 2014,57, 127-136)将甲基丙烯酸缩水甘油酯引入将高内相乳液聚合体系，利用二乙烯基苯为交联剂，以三聚甘油单硬脂酸酯为乳化剂，成功合成了聚甲基丙烯酸缩水甘油酯-二乙烯基苯高内相乳液固体块，并利用二乙胺在表面引入了氨基，为其表面功能化提供了新的思路。
β-环糊精是一种天然的，可持续生产的，无毒、可生物降解葡萄糖大环，并且具有“内腔疏水, 外壁亲水”的特殊结构和性质，已成为构筑各种功能材料的优良结构单元，特别是吸附材料的构建以及对环境污染物的吸附性能测试(YKang, J YYuan, et al. J. Mater. Chem., 2011, 21, 3704–3710)。β-环糊精吸附环境污染物，主要是借助β-环糊精单元对环境污染物分子的包结络合作用，将环境污染物包结富集，还具有增强载体在水相中分散的作用，从而促进吸附过程的进行(A Alsbaiee, et al. Nature.,2015,529)。
利用乙二胺胺化改性的β-环糊精作为单体，将多孔泡沫表面改性，引入β-环糊精基团，可以实现选择性吸附的效果。
利用高内相乳液制备多孔材料结构的优势，结合酯化反应，在多孔泡沫表面引入大量β-环糊精，合成产物不仅含有丰富的孔道结构和功能集团，表面的β-环糊精修饰能有效吸附微量环境污染物，如2,4-二氯苯酚、2-萘酚、双酚A、双酚S等芳香烃，而且具有可重复使用效能，在环境功能材料具有广泛的应用前景。
发明内容
本发明的目的在于提供一种利用高内相乳液模版法制备表面β-环糊精修饰的多孔吸附材料的方法。
本发明的目的是将β-环糊精作为支链引入到高内相乳液聚合物表面上，使所获得的产物同时具有低密度、高度多孔性、良好的选择吸附性、高吸附效率及可重复利用性。本发明用甲基丙烯酸缩水甘油酯／二乙烯基苯高内相乳液模版法体系，采用乙二胺的酯化反应方法，制备β-环糊精表面修饰的多孔泡沫材料。
本发明提出的表面糖基修饰的多孔泡沫材料的制备方法，具体步骤如下：
(1)利用乳化剂A来稳定高内相乳液，甲基丙烯酸缩水甘油酯单体、交联剂二乙烯基苯、致孔剂甲苯为连续相，其中甲基丙烯酸缩水甘油酯、二乙烯基苯、乳化剂A、甲苯四种物质的质量比为1:(0.5~1.5):(1~1.5):(1~2)，以水为分散相，水相占乳液整体的质量百分数为75%～90%，以水为分散相，过硫酸钾引发下，反应温度为50-80℃，反应12-48小时，通过高内相乳液模版法制得多孔泡沫材料；通过乙醇洗涤，经索氏提取10-48小时，真空干燥，得到基体为甲基丙烯酸缩水甘油酯-二乙烯基苯的白色多孔泡沫；
(2)将步骤(1)得到基体为甲基丙烯酸缩水甘油酯-二乙烯基苯的白色多孔泡沫物块加入溶剂B中，然后加入乙二胺胺化改性的β-环糊精，加入量按所设计的分子量及其性能确定，反应温度为50-90℃，反应12-48小时；所得产物分别以N,N-二甲基甲酰胺和乙醇为洗液，经索氏提取10-48小时，真空干燥，即得到所需产物。
本发明中，所述乳化剂A为司班80、三聚甘油单硬脂酸酯中的一种或几种。
本发明中，所述溶剂B为四氢呋喃、N,N-二甲基甲酰胺、N,N-二乙基甲酰胺或N,N-二甲基乙酰胺中的一种或几种。
本发明的优点在于：原料来源广泛，所用的甲基丙烯酸缩水甘油酯单体、二乙烯基苯、溶剂、乳化剂、催化剂等均可工业化生产，乙二胺胺化改性的β-环糊精较易合成，整个制备过程方法简单易行。高内相乳液模版法可精确控制孔及通道直径的大小和分布。所合成的表面β-环糊精修饰的多孔泡沫材料同时具有低密度、高度多孔性，能有效吸附水中微量有机物吸，如2,4-二氯苯酚、2-萘酚、双酚A、双酚S等芳香烃，而且具有可重复使用效能。
附图说明
图1：本发明中制备的表面β-环糊精修饰的多孔泡沫的结构示意图。
图2：本发明中制备的表面β-环糊精修饰的多孔泡沫材料的扫描电子显微镜照片。
具体实施方式
以下实施例是对本发明的进一步说明，而不是限制本发明的范围。
该表面糖基修饰的多孔泡沫结构形貌用傅里叶变换红外光谱仪（FTIR）和扫描电子显微镜（SEM）测定。
实施例1
将Span80 0.4g、甲基丙烯酸缩水甘油酯单体0.4g、交联剂二乙烯基苯0.6g、致孔剂甲苯1.0 g混合，向其中逐滴滴加过硫酸钾溶液13.6 ml，反应温度为50℃，反应48小时，通过高内相乳液模版法制得多孔泡沫材料；取产物物块0.3g加入N,N-二甲基甲酰胺中，然后加入乙二胺胺化改性的β-环糊精2.0g，反应温度为60℃，反应24小时；所得产物分别以N,N-二甲基甲酰胺、水和乙醇为洗液，经索氏提取24小时，真空干燥，即得到所需产物。
实施例2
将Span80 0.6 g、甲基丙烯酸缩水甘油酯单体0.6 g、交联剂二乙烯基苯0.4 g、致孔剂甲苯0.8 g混合，向其中逐滴滴加过硫酸钾溶液13.6 ml，反应温度为60℃，反应24小时，通过高内相乳液模版法制得多孔泡沫材料；取产物物块0.3 g加入N,N-二甲基乙酰胺中，然后加入乙二胺胺化改性的β-环糊精2.5 g，反应温度为70℃，反应12小时；所得产物分别以N,N-二甲基乙酰胺、水和乙醇为洗液，经索氏提取24小时，真空干燥，即得到所需产物。
实施例3
将乳化剂三聚甘油单硬脂酸酯 0.6 g、甲基丙烯酸缩水甘油酯单体0.5 g、交联剂二乙烯基苯0.5 g、致孔剂甲苯1.0g混合，向其中逐滴滴加过硫酸钾溶液13.6 ml，反应温度为70℃，反应36小时，通过高内相乳液模版法制得多孔泡沫材料；取产物物块0.3 g加入四氢呋喃中，然后加入乙二胺胺化改性的β-环糊精2.0 g，反应温度为50℃，反应36小时；所得产物分别以四氢呋喃、水和乙醇为洗液，经索氏提取24小时，真空干燥，即得到所需产物。

Claims (3)

1.一种利用高内相乳液模版法制备表面β-环糊精修饰的多孔吸附材料的方法，其特征在于具体步骤如下：
(1)利用乳化剂A来稳定高内相乳液，甲基丙烯酸缩水甘油酯单体、交联剂二乙烯基苯、致孔剂甲苯为连续相，其中甲基丙烯酸缩水甘油酯、二乙烯基苯、乳化剂A、甲苯四种物质的质量比为1:(0.5~1.5):(1~1.5):(1~2)，以水为分散相，水相占乳液整体的质量百分数为75%～90%，以水为分散相，过硫酸钾引发下，反应温度为50-80℃，反应12-48小时，通过高内相乳液模版法制得多孔泡沫材料；通过乙醇洗涤，经索氏提取10-48小时，真空干燥，得到基体为甲基丙烯酸缩水甘油酯-二乙烯基苯的白色多孔泡沫；
(2)将步骤(1)得到基体为甲基丙烯酸缩水甘油酯-二乙烯基苯的白色多孔泡沫物块加入溶剂B中，然后加入乙二胺胺化改性的β-环糊精，加入量按所设计的分子量及其性能确定，反应温度为50-90℃，反应12-48小时；所得产物分别以N,N-二甲基甲酰胺和乙醇为洗液，经索氏提取10-48小时，真空干燥，即得到所需产物。
2.根据权利要求1所述的一种利用高内相乳液模版法制备表面β-环糊精修饰的多孔吸附材料的方法，其特征是所述乳化剂A为司班80、三聚甘油单硬脂酸酯中的一种或几种。
3.根据权利要求1所述的一种利用高内相乳液模版法制备表面β-环糊精修饰的多孔吸附材料的方法，其特征是所述溶剂B为四氢呋喃、N,N-二甲基甲酰胺、N,N-二乙基甲酰胺或N,N-二甲基乙酰胺中的一种或几种。
CN201710101610.4A 2017-02-24 2017-02-24 一种利用高内相乳液模版法制备表面β‑环糊精修饰的多孔吸附材料的方法 Pending CN106905533A (zh)

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