12wt% MoO3/TiO2-SiO2 solid acid catalyst was prepared and calcined at various temperatures. The calcined catalyst was characterized by XRD, FT-IR, BET, SEM, NH3-TPD and pyridine adsorbed FT-IR methods. The effect of calcination temperature on activity of catalyst was studied by choosing liquid phase nitration of phenol as a model reaction. For the same reaction effect of various solvents, effect of reaction time and reusability of the catalyst was also studied. Catalyst calcined at 500 degrees C temperature showed highest phenol conversion whereas greater o-nitrophenol selectivity is claimed over catalyst calcined at 700 degrees C. It was observed that high phenol conversion co-relates with the presence of greater number of strong Bronsted acid sites over the catalyst surface whereas the selectivity of o-nitrophenol is related to the pore size of the catalysts. No use of sulfuric acid along with the nitric acid used in its diluted form in the reaction makes the process safe and environmentally friendly. (C) 2010 Elsevier B.V. All rights reserved.