The potential of a novel magnetic Fenton-like catalyst Fe3O4/MIL-53(Cu)/CNT for the degradation of acid orange 7 has been evaluated. The supported iron-copper bimetallic catalysts, combining the advantages of immobilization and iron-copper synergy, have been developed and demonstrated to significantly increase the efficiency of Fenton-like processes [1]. Furthermore, introducing functionalized nanocarbons to heterogeneous Fenton catalysts with the electron donor property of the carboxyl groups on the surface of nanocarbons promotes the efficiency of catalyst over a wider pH range [2] . The satisfactory treatment of acid orange 7, as azo dyes involving aromatic rings, azoic linkages and amino groups [3], with high degradation efficiency of 84.6% has been obtained. The heterogeneous Fenton-like catalytic process in aqueous solutions was modeled and optimized employing Response Surface Methodology (RSM) based on Central Composite Design (CCD) regarding the influence of effective parameters of pH, nanocomposite dose and hydrogen peroxide concentration on the degradation efficiency as response. The predictability of proposed model has been confirmed with the close to unity regression coefficient (R2=0.9985). The results of reduced quadratic model demonstrated that the highest degradation efficiency has been attained at optimum conditions of pH =5.78, nanocomposite dose (0.3 g/L) and hydrogen peroxide concentration of 1.5 mol/L. Moreover, the kinetics investigation revealed that the degradation reaction followed the first order with desired rate constant. Therefore, the efficient and fast degradation of acid orange 7 proposed utilizing the heterogeneous Fentonlike catalyst has confirmed its extensive applicability for the removal of various organic contaminant pH range.