This study investigates the treatment of the distilleries vinasse using a hybrid process integrating ozone oxidation and granular activated carbons (GAC) in both batch and continuous operation mode. The batch-process studies have been carried out to optimize initial influent pH, GAC doses, the effect of the ozone (O3) and hydrogen peroxide (H2O2) concentrations on chemical oxygen demand (COD) and color removal of the distilleries vinasse. The continuous process was carried out on GAC and ozone treatment alone as well as the hybrid process comb both methods to investigate the synergism effectiveness of the two methods for distilleries vinasse COD reduction and color removal. In a continuous process, the Yan model described the experimental data better than the Thomas model. The efficiency of ozonation of the distilleries vinasse was more effective for color removal (74.4%) than COD removal (25%). O3/H2O2 process was not considerably more effective on COD and color removal. Moreover, O3/GAC process affected negatively on the removal efficiency by reducing COD and color from distilleries vinasse. The negative effect decreased by increasing pH value of the influent.