Aerosol-assisted synthesis of mesoporous organosilica microspheres with controlled organic contents.

Periodic mesoporous organosilica (PMO) spherical particles with different organic contents were synthesized in one pot by reacting 1,2-bis(triethoxysilyl)ethane (BTSE) with tetraethylorthosilicate (TEOS) using a spray-drying technique. The scanning electron microscopy observation of spray-dried products clearly showed the formation of spherical particles. The 29Si magic angle spinning nuclear magnetic resonance data revealed that the organic contents due to ethane fragments embedded in the frameworks were controllable and consistent with the BTSE/TEOS molar ratios of precursor solutions. Transmission electron microscopy, small-angle x-ray scattering, and N2 adsorption data of PMO with controlled organic contents indicated that the ethane fragments were embedded in the frameworks with the formation of ordered mesostructures. PMO with a high organic content (BTSE/TEOS=0.50) only showed a hydrophobic property. According to the same procedure, benzene groups were also integrated to a similar degree in the frameworks by using 1,4-bis(triethoxysilyl)benzene.