The electrocoagulation/flotation process is a novel approach in mining industry that is implemented to return Cu metal to the production cycle, which improves copper recovery and reduces waste water. In this research work, the response surface methodology was applied to optimize the factors effective in Cu metal recovery and sludge volume produced from thickener overflow. To this end, the D-optimal experimental design was utilized. The influences of four independent parameters including the electrolysis time, initial pH, current density, and electrodes type were studied to investigate the initial Cu grade percentage (28%) and sludge volume produced from thickener overflow. All these parameters were found to have important effects on the Cu metal recovery and the sludge volume produced. The linear and quadratic models were utilized for the Cu grade and sludge volume, respectively. The importance of the independent variables and the interaction between them was assessed by ANOVA. The optimum operating conditions with 27.22% Cu grade were taken to be: electrolysis time: 6.5 min, initial pH: 6.7, current density: 50.2 A/m2, and electrode type: Fe-Al. Similarly, for the produced sludge volume of 861 cm3, the following conditions were found: electrolysis time: 15 min, initial pH: 4.1, current density: 48.7, and electrode type: Fe-Al. The outcomes underscored a practical viewpoint of electrocoagulation, known as an acceptable method for Cu recovery from mine industrials, especially in mineral processing plants.