以β-环糊精改性自组装的化合物为模板剂合成介孔分子筛及其表征

Synthesis and Characterization of Mesoporous Molecular Sieve on Template of Self-Assembled Modified β-Cyclodextrin

利用纯天然化合物β-环糊精的特殊结构,通过优化苯基修饰改性过程制备了单(6-氧-6-苯基)-β-环糊精,单(6-氧-6-苯基)-β-环糊精具有自组装能力形成超分子聚合物,以该超分子聚合物为模板剂合成了介孔分子筛;用X射线衍射、N2吸附-脱附、傅里叶变换红外光谱、热重与差热分析、固体硅核磁共振、扫描电子显微镜、透射电子显微镜等方法对产物进行了表征。表征结果显示,所合成的产物具有高度有序的六方介孔分子筛的结构特征,孔径约为2.13nm,比表面积达到260m2/g以上,完全符合螺旋柱状超分子聚合物的外径尺寸;螺旋柱状超分子聚合物的紧密堆积程度没有有机胺类模板剂大,相邻β-环糊精母体之间存在一定的空隙,产品在整体结构上还存在一定程度的缺陷。

Self-assembled supermolecular polymer composed ot mono-（6-oxygen-6-pnenyl ）-β- cyclodextrin was attempted to be used as a template for preparing a novel mesoporous molecular sieves. The product molecular sieves were synthesized from derivative of β-cyclodextrin by phenyl modification which possessed the ability of self-assembling and was used as template in preparation of new molecular sieve. The structure and properties of the product were characterized by means of powder XRD, N2 adsorption-desorption, FTIR, Si MAS NMR, TG-DTA, SEM and TEM. The product mainly shows hexagonal mesoporous structure, similar to MCM-41 molecular sieve. The pore diameter of the product is about 2. 13 nm. The specific surface area of the product is more than 260 m2/g. However the product is somewhat defective in monolithic structure, which may be due to that the compatibility of intermediate supermolecular polymer is not enough and slits still exist between adjacentβ-cyclodextrin mother-molecules.