Abstract: The immobilization of TiO2 on ACF (TiO2/ACF) was performed using epoxy resin as binder between TiO2 and ACF, followed by calcination at different temperatures from 400 to 580℃ in a N2 atmosphere. The properties of the resulting materials were characterized by BET, SEM, XRD and UV-Vis spectra. The photodegradation behavior of TiO2/ACF prepared was investigated in aqueous solution using phenol as a target pollutant. It was found that the sample calcined at 460℃ exhibited the highest phenol removal efficiency. When used repeatedly, TiO2/ACF still presented high photocatalytic efficiency, and the phenol removal in the third cycle was almost the same as Degussa P25, mainly anatase. Moreover, TiO2 is tightly bound to ACF, and can be easily handled and recovered from water.