Preparation of micron-sized spherical particles of mesoporous silica from a triblock copolymer surfactant, usable as a stationary phase for liquid chromatography

Spherical particles (∅>3 μm, with 5–10 nm pore size) of SBA15-type mesoporous silica, usable as stationary phase for HPLC, were prepared with tetraethoxysilane (TEOS) as silica source, triblock copolymer Pluronic P123 (EO20PO70EO20) as surfactant S0 and cetyltrimethylammonium bromide (CTMABr) as co-surfactant S+. The synthesis mechanism involves a surfactant-silica species self-assembly process in acidic medium under quiescent conditions, where S0H3O+X−I+ and S+X−I+ interactions occur. The syntheses were carried out using two procedures: (a) with one heating step and (b) with two heating steps. Synthesis conditions, such as the dilution, temperature and acidity of the reaction mixture and the temperature and duration of the reaction, influence the porous characteristics as well as the morphology and size of the particles. Spherical particles were obtained with one heating step under conditions that weaken the surfactants-silicate interactions such as high dilution, high temperature and low acidity. The modification of the micelle volume with the temperature and acidity allowed the adjustment of the pore size.