Institut für Physikalische Chemie, Universität Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart, Germany.
J Chromatogr A. 2010 May 14;1217(20):3362-74. doi: 10.1016/j.chroma.2010.03.005. Epub 2010 Mar 10.
Surface modification offers a great opportunity to adjust both the pore diameter and surface properties of MCM-41 type organic-inorganic hybrid materials which result in materials of improved hydrothermal and mechanical stability. Therefore, MCM-41 silica, surface modified with organic ligands, are promising systems with engineered properties and attractive for advanced applications. In the present study, after optimization of the reaction conditions highly ordered MCM-41 silica spheres with uniform mesopores were prepared by the pseudomorphic transformation route. The effect of functionality and alkyl chain length of the alkyl ligands during surface modification was probed by using butyl and octylsilanes with two different functionalities. Due to steric hindrance, the longer chains are assumed to bind only on the outer silica surface and near the entrance of the pores, while the shorter chains are also able to bind to the interior mesopore walls. The resulting materials were comprehensively characterized before and after surface modification using nitrogen sorption techniques, XRD, SEM, solid-state NMR spectroscopy and FTIR spectroscopy. From chromatographic test measurements it was found that the separation power primarily depends on surface coverage and alkyl chain length. On the basis of the present data, surface modified mesoporous silica of MCM-41 type are very promising candidates for future chromatographic applications.
表面修饰为调整 MCM-41 型有机-无机杂化材料的孔径和表面性质提供了极好的机会,从而得到热稳定性和机械稳定性得到提高的材料。因此,用有机配体表面修饰的 MCM-41 硅具有工程特性,在先进应用中具有吸引力,是一种很有前途的体系。在本研究中,通过调整反应条件,采用拟晶转化途径制备了具有均匀介孔的高度有序 MCM-41 硅球。通过使用两种不同功能的丁基和辛基硅烷,研究了烷基配体的功能和烷基链长度在表面修饰过程中的影响。由于空间位阻,较长的链仅假定结合在二氧化硅外表面和孔入口附近,而较短的链也能够结合到介孔壁内。在表面修饰前后,使用氮气吸附技术、XRD、SEM、固态 NMR 光谱和 FTIR 光谱对材料进行了全面的表征。从色谱测试结果发现,分离能力主要取决于表面覆盖率和烷基链长度。根据目前的数据,MCM-41 型表面修饰介孔硅是未来色谱应用的非常有前途的候选材料。