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This paper reports on the process of industrial-type wastewater purification carried-out through continuous anodic dissolution of aluminum alloy sacrificial anode for artificially aerated Cu-Al alloy galvanic (macro-corrosion) cells and synthetically prepared wastewater solutions. Electrochemical experiments were performed by means of a laboratory size electrolyzer unit, where the electrocoagulation process along with surface-induced electrooxidation phenomena were examined for wastewater containing Acid Mixture and <i>Disperse Red 167</i> dyes. Final reduction of the dyes concentrations came to 32 and 99% for Acid Mixture and <i>Disperse Red 167</i>, correspondingly. The above was visualized through the employment of electrochemical (cyclic voltammetry and a.c. impedance spectroscopy techniques) and instrumental spectroscopy analyses.