Photo-Fenton oxidation is one of the most promising processes to remove recalcitrant contaminants from industrial wastewater. In this study, we developed a novel heterogeneous catalyst to enhance photo-Fenton oxidation. Multi-composition (Fe-Cu-Zn) on aluminosilicate zeolite (ZSM-5) was prepared using a chemical process. Subsequently, the synthesized catalyst was characterized by using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray (spectroscopy) (EDX), and Brunauer-Emmett-Teller (BET). Activity of the synthesized catalyst is analysed to degrade an azo dye, methyl orange. Taguchi method is used to optimize color removal and total carbon content (TOC) removal. The dye completely degraded, and 76% of TOC removal was obtained at optimized process conditions. The amount of catalyst required for the desired degradation of dye significantly reduced up to 92% and 30% compared to conventional homogenous and heterogeneous Fenton oxidation processes, respectively.