Three surfactants were selected from a series of EOx/POy/EOx triblock copolymers and ethoxylated octylphenol as nonionic templating agents for the synthesis of silica mesoporous materials at room temperature and by hydrothermal treatment. The surfactants were ethylene oxide-propylene oxide-ethylene oxide tri-block copolymers (Pluronic F68) and a polydisperse ethoxylated octylphenol (Triton X-100). The obtained materials were compared with SBA-15 mesoporous silica synthesized with Pluronic P123 surfactant and were used as support to obtain Ni and NiTi-silica catalysts (2.5% NiO, 5% TiO2). The synthesized materials were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), N2 adsorption-desorption, IR and UV-Vis spectroscopy. Catalytic and photocatalytic activity of Ni and NiTi-silica samples were tested, with and without H2O2, for phenol and Brilliant Blue FCF dye oxidative degradation in the liquid phase. The obtained results showed a significant effect of surfactant on silica structure, morphology and texture, and catalytic and photocatalytic properties.