Water pollution has been a prime concern for scientists for decades. Different treatment methods have been suggested by different researchers, with photocatalysis emerging as an efficient method for treating industrial textile wastewater. This study is designed to synthesize a nano-photocatalyst for the degradation of two synthetic dyes. The Al₂O₃.Fe₂O₃ nano-photocatalyst was synthesized by a novel technique: ultrasonic-assisted mechanical stirring and synthesized photocatalyst characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive x-ray (EDX) analysis, dynamic light scattering, and BET surface area analysis. The Al₂O₃.Fe₂O₃ nano-photocatalyst was tested for its potential to degrade methyl orange and methylene blue dyes. Important influencing parameters (pH, catalyst dose, initial dye concentration, and reaction time) have been optimized during the dye degradation process. The highest degradation for methyl orange (39%) and methylene blue (45%) was achieved by using 60 mg/100 mL catalyst dose and 120 minutes of reaction time at room temperature. The study results indicated that Al₂O₃.Fe₂O₃ nano-photocatalyst has good potential for the removal of dyes from industrial effluents.