The removal of dye from textile industry wastewater using a photo-Fenton like catalyst system was investigated wherein the removal efficiency of phenol and chemical oxygen demand (COD) was studied by varying various parameters of pH (3–11), reaction time (1–50 min), activated Carbon/CoFe2O4 (AC/CFO) nanocomposite dosage (0.1–0.9 g/L), and persulfate amount (1–9 mM/L). The highest removal rates of reactive red 198 and COD were found to be 100% and 98%, respectively, for real wastewater under the optimal conditions of pH = 6.5, AC/CFO nanocomposite dosage (0.3 g/L), reaction time, 25 min, and persulfate dose of 5 mM/L up on constant UV light irradiation (30 W) at ambient room temperature. The result showed that this system is a viable and highly efficient remediation protocol relative to other advanced oxidation processes; inexpensive nature, the ease of operation, use of earth-abundant materials, and reusability for removal of organic pollutants being the salient attributes.