The removal of congo red (CR) is a critical issue in contemporary textile industry wastewater treatment. The current study introduces a combined electrochemical process of electrocoagulation (EC) and electro-oxidation (EO) to address the elimination of this dye. Moreover, it discusses the formation of a triple composite of Co, Mn, and Ni oxides by depositing fixed salt ratios (1:1:1) of these oxides in an electrolysis cell at a constant current density of 25 mA/cm2. The deposition ended within 3 hours at room temperature. X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and energy dispersive X-ray (EDX) characterized the structural and surface morphology of the multi-oxide sediment. Marvelously, the deposition has simultaneously occurred on both anodic and cathodic graphite electrodes. These electrodes besides aluminum (Al) are employed as anodes in the EC-EO system, and the results were optimized by response surface methodology (RSM). The optimum operating conditions were a current density of 6 mA/cm2, pH = 7, and NaCl of 0.26 g/L. The results showed that the combined system eliminated more than 99.91% of the congo red dye with a removal of chemical oxygen demand (COD) of around 97% with 1.64 kWh/kg of dye of the consumed energy. At low current density, the current delivered for the composite anode was more than for the Al anode with the same surface area. On top of this superiority, the EC-EO scenario is a practical hybrid process to remove CR in an environmentally friendly pathway.
