Effect of synthesis conditions on the mesoscopical order of mesoporous silica SBA-15 functionalized by amino groups

Mesoporous amine-functionalized SBA-15 silica has been synthesized directly by the co-condensation of tetraethyl orthosilicate (TEOS) and aminopropyl-trimethoxysilane (APTMS) under acidic conditions with an APTMS/(APTMS + TEOS) molar ratio of 10%. The effect of synthesis conditions, including TEOS pre-hydrolysis, as well as the heating temperature and time, on the mesoscopical order and pore structure of the functionalized SBA-15 have been studied in detail by means of powder X-ray diffraction, nitrogen sorption, transmission electron microscopy, infrared spectra and solid state ²⁹Si nuclear magnetic resonance. A functionalized SBA-15 silica with a highly ordered two-dimensional P6 mm hexagonal symmetry and a narrow pore size distribution centered at 6 nm can be obtained if TEOS is allowed to pre-hydrolyze for 2 h. For the sample with TEOS pre-hydrolysis time of 4 h, aging at 50°C or 150°C leads to a more ordered pore arrangement compared to 100°C and also a narrower pore size distribution with larger pore volume. Increasing aging time is in favor of the formation of mesoscopically ordered structure, but fails to obtain a superior pore structure.