γ-Al2O3/ NiO/ TiO2 as a novel photocatalyst that is active in visible light was synthesized by a simple sol-gel method. The prepared samples were characterized by XRD, DRS-UV/Vis, and TEM analysis. The photocatalytic effect of synthesized samples was examined on methyl tert-butyl ether (as a model hazardous contaminant) degradation. Experimental condition including pH, irradiation time, and photocatalyst mass were optimized. Overall, the UV/Vis spectrophotometry results indicated that the synthesized nanoparticles have an extraordinary photocatalytic activity for the degradation of methyl tert-butyl ether under visible light.