In the present work, a TiO2/activated carbon (AC) photocatalyst with high activity and easy separation was prepared using a hydrothermal method. Phenol, methyl orange (MO) and Cr(VI) were used as target pollutants to test the activity and decantability. SEM, XRD, FTIR, diffuse reflectance spectra (UV/DRS) and N2 adsorption isotherms were used to characterize the crystalline and electronic structure. Results show that the AC composite has a significant effect on the TiO2 activity. With suitable AC content, the TiO2/xAC catalysts prepared were much more active. The TiO2/5AC catalyst exhibited easy separation and less deactivation after several runs, and was less sensitive to pH changes. UV/DRS revealed that no electronic bandgap changes in TiO2 occurred on addition of the AC. SEM and XRD results suggest that better TiO2 distribution can be achieved when an optimal AC content is used. A Ti-O-C bond was formed and a slight conjugation effect appeared between the AC bulk and TiO2. The advantages of the obtained TiO2/5AC catalyst revealed its great practical potential in wastewater treatment.