A new composite photocatalyst (Fe2O3 and ZrO2/Al2O3) combining the properties of both semiconductor and Fenton like catalyst was prepared by loading the Fe2O3 and ZrO2 on an aluminum oxide support through a sol-gel method. The catalyst was characterized by XRD, nitrogen adsorption-desorption, TEM, SEM, ICP-AES, and XPS. The results show that the Fe2O3 and ZrO2 are well loaded on the support, and the crystallite phase composition of the catalyst is alpha-Fe2O3, monoclinic and tetragonal ZrO2 and eta-Al2O3. The catalyst shows high catalytic activity in phenol photodegradation reaction with the phenol conversion efficiency higher than 93% at experimental conditions (catalyst dose, 1.0 g L-1; H2O2 dose, 50 mM; solution pH, 6.0). After two runs of regeneration, the activity of the catalyst shows only a slight decrease. The XPS analysis of the fresh and regenerated catalyst reveals that both the surface elemental composition and their chemical state keep stable. This study presented a new type of photocatalyst for degradation of refractory organic pollutants. (C) 2011 Elsevier B.V. All rights reserved.