This study investigated the treatment of an azo dye, as a biorecalcitrant model, from industrial wastewater by using Cu/Mg/Al-chitosan in a fluidized catalyst-bed reactor. A number of variables were used to study the impact they had on the oxidation process involving azo dye. The maximum degradation of the azo dye was achieved at 7 g Cu/Mg/Al-chitosan. The chloride and sulfate ions had a synergistic effect on azo dye removal. The oxidation of the azo dye under the selected conditions was of pseudo-first-order. Textile wastewater could effectively be treated using a low concentration of about 7 g of Cu/Mg/Al-chitosan in a short hydraulic retention time of 10 min. The use of Cu/Mg/Al-chitosan demonstrated a promising method to eliminate the azo dye from the wastewater.