Chem.
Mater. 1999, 11, 3302-3308
Mesoporous Sieves With Unified Hybrid Inorganic/Organic Frameworks
Brian J. Melde, Brian T. Holland, Christopher F. Blanford, and Andreas Stein*
Department of Chemistry, University of Minnesota, Minneapolis, MN 55455
Abstract
Mesoporous materials have been synthesized that are composed of hybrid frameworks in which inorganic and organic components have a fixed stoichiometry and are covalently bonded. The creation of UOFMN (Unified Organically Functionalized Mesoporous Networks) materials incorporates concepts employed in the synthesis of MCM-41 mesoporous silicates, making use of a quaternary ammonium cationic surfactant and a double trialkoxysilyl precursor such as bis(triethoxysilyl)ethane (BTSE) or bis(triethoxysilyl)ethylene (BTSEY). The cetyltrimethylammonium (CTA+) surfactant is removed by extraction with acid, resulting in a high surface area porous organosilicate framework in which Si atoms are bridged by ethane (from BTSE) or ethylene (BTSEY) groups. The channels are worm-like and uniform in diameter. UOFMN materials are more hydrothermally stable than MCM-41 and have thicker pore walls. Ethylene groups in products made with BTSEY can be brominated, the brominated product itself being reactive as a bromine source. The UOFMN products were characterized by XRD, N2 adsorption, solid-state 29Si and 13C NMR, and TEM.