The materials Al2O3:Ce3+/Ce4+ (cerium content 0.5, 1.0, 3.0, and 5.0 wt.%) were synthesized by the sol-gel method. The materials were characterized by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), N-2 physisorption, UV-Vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy (XPS) and energy-dispersive X-ray spectroscopy (EDX); also, some electrochemical tests were performed for the materials characterization. The materials were evaluated in the phenol photodegradation using UV light. The photocatalyst containing 1.0 wt.% cerium (AC1.0) presented the highest photoactivity than the others synthesized samples. This catalyst was selected to photodegrade others phenolic derivatives such as 4-chlorophenol, p-cresol, and 4-nitrophenol. All the synthesized photocatalysts by the sol-gel method showed a better activity than (TiO2, P25 Degussa). The photodegradation reactions were followed by UV-Vis spectroscopy and total organic carbon TOC. A reaction mechanism is proposed involving the sensitization of the organic molecule on Al2O3:Ce3+/Ce4+ with UV light for its mineralization. (C) 2016 Elsevier Ltd. All rights reserved.