Periodic Mesoporous Organosilicas PMOs with Different Organic Bridging Groups: Synthesis and Characterization
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Periodic Mesoporous Organosilicas PMOs with Different Organic Bridging Groups: Synthesis and Characterization Vivian Rebbin, Olaf Muth1 and Michael Fröba* Institute of Inorganic and Analytical Chemistry, Justus-Liebig-University, Heinrich-Buff-Ring 58, D-35392 Giessen, Germany, E-mail: [email protected] 1 Institute of Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg, Germany ABSTRACT We present results on new periodic mesoporous organosilicas synthesized with 1,4-bis(triethoxysilyl)benzene (BTEB), 1,2-bis(trimethoxysilyl)ethane (BTME) and bis[3-(trimethoxysilyl)propyl]amine (BTMPA). The materials show high inner surfaces up to 830 m2/g and pore diameters in the range of 2.7 to 3.7 nm depending on the structure directing agent used. In case of BTEB as precursor and triblock copolymer Pluronic P123 as structure directing agent exceptional thick pore walls were obtained (7.2 nm). Characterization was carried out by P-XRD, nitrogen physisorption analysis, thermoanalytical methods and IR spectroscopy.
INTRODUCTION In 1999, a new way was found to incorporate organic moieties into M41S silica materials [1-6]. For the first time bridged silsesquioxane precursors, e.g. 1,2-bis(trimethoxysilyl)ethane, were used as silica source in the synthesis of highly ordered hybrid mesoporous materials (PMOs) in order to integrate bridging organic groups directly into the framework of the pore walls instead of grafting these organic species onto the pore wall surface. The organic modification of the silica framework provides variation of the optical, electrical and mechanical properties [7]. These materials seem to be of great interest due to their potential application in catalysis, adsorption and luminescence applications and as support for electronic devices. Structures and pore sizes of these PMOs have been varied by using lyotropic triblock copolymer P123 as structure directing agent [8]. Many results on PMOs containing 1,2-bis(trimethoxysilyl)ethane (BTME) have been published up to now [1-6], but only little research has been done on PMO syntheses with 1,4-bis(triethoxysilyl)benzene (BTEB) as silica source [4,9,10]. In order to explore this field of research further we tried to obtain PMOs with large pores from BTEB and triblock copolymer Pluronic P123 reaction mixtures. We also aimed to synthesize PMOs with a new kind of bridging ligand carrying a funtionality which to our knowledge has not been applied for PMO syntheses yet. Therefore bis[3-trimethoxysilyl)propyl]amine was utilized in combination with BTME as precursor at different ratios for co-condensation reactions.
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EXPERIMENTAL The synthesis and extraction procedure for the benzene bridged PMO is analogues to the synthesis of PMOs with BTME already described elsewhe
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