Considering the drawbacks of iron-based Fenton process, this work was aimed at designing of an efficient photo-Fenton like process via coupling of CuO/g-C3N4 photocatalyst with H2O2. The photo-Fenton like catalytic process was used for degradation of 2, 4-dimethyl phenol (DMP). The X% CuO/g-C(3)N(4 )Z-shceme photocatalyst samples were fabricated by thermal calcination method, varing the CuO percentage (X = 2 %, 4 % and 8 %) loaded on g-C3N4. A lab-scale photoreactor was used to assess and select the optimal removal efficiency for DMP degradation. The photocatalyst was characterized by advanced spectral techniques. Coupling of CuO/GCN system with H2O2 significantly improved photocatalytic activity via photo-Fenton process. The kinetics of photo-degradation was found to exhibit pseudo-first order reaction rules. The rate of photodegradation was strongly influenced by pH and different concentrations of H2O2. 4%CuO/g-C3N4/H2O2 system proved to be the most efficient and exhibited much higher photo removal efficiency than CuO/g-C3N4 system and permitted attaining 99 % degradation of DMP in reaction time of 120 min. The successful implementation of this work was effective and of significance for the economical decomposition process of pollutants present in water under visible light irradiation. Overall, utilization of the studied system leads to high catalytic efficiency in a relatively short degradation period, which is of immense potential in water purification. (C) 2020 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.