In order to develop the high photocatalytic activity of TiO2 under visible light as that under ultraviolet light and make it easy to be separated from treated liquor, a visible light response and spherical activated carbon （SAC） supported photocatalyst doped with upconversion luminescence agent Er3＋：YAlO3 was prepared by immobilizing Er3＋：YAlO3/TiO2, which was obtained by combination of Er3＋：YAlO3 and TiO2 using sol-gel method, on the surface of SAC. The crystal phase composition, surface structure and element distribution, and light absorption of the new photocatalysts were examined by X-ray diffraction （XRD）, energy dispersive X-ray spectra （EDS） analysis, scanning electron microscopy （SEM） and fluorescence spectra analysis （FSA）. The photocatalytic oxidation activity of the photocatalysts was also evaluated by the photodegradation of methyl orange （MO） in aqueous solution under visible light irradiation from a LED lamp （λ400 nm）. The results showed that Er3＋：YAlO3 could perform as the upconversion luminescence agent which converts the visible light up to ultraviolet light. The Er3＋：YAlO3/TiO2 calcinated at 700 °C revealed the highest photocatalytic activity. The apparent reaction rate constant could reach 0.0197 min-1 under visible light irradiation.
