ZnAl2O4 spinel was synthesized by co-precipitation using ammonia as precipitating agent, followed by thermal treatment at 750 ºC. The structural properties of particles were investigated by X-ray diffraction (XRD), atomic force microscopy (AFM), differential thermal analysis (DTA), and N2 adsorption/desorption isotherms (BET) techniques. The photocatalytic activity was evaluated in the degradation of organic pollutant in aqueous solution under sunlight. The results showed that the ZnAl2O4 particles exhibited a mesoporous structure, and a promising photocatalytic activity for the degradation of pollutant molecules.