Photocatalysis is one of the techniques used for the eradication of organic pollutants from wastewater. In this study, Co−ZnO was tested as a photocatalyst for the degradation of methyl orange under irradiation of visible light. Co−ZnO loaded with 5%, 10%, and 15% Co was prepared by the precipitation method. The advanced techniques including X-ray diffraction, X-ray photoelectron spectroscopy, diffuse reflectance UV−visible spectroscopy, photoelectrochemical measurements, temperatureprogrammed desorption, photoluminescence, and fluorescence spectroscopy related to OH • measurements were used for characterization of prepared Co−ZnO. Experiments showed that 10% Co−ZnO was a highly efficient catalyst for the photodegradation of methyl orange as compared to ZnO. The enhanced photocatalytic activity of Co−ZnO is attributed to the implantation of Co which inhibits the electron−hole recombination. A 100 mg/L solution of methyl orange dye was completely degraded within 130 min. The reaction kinetics has been described in terms of the Eley−Rideal mechanism.