In this research, nanostructured zinc cobalt oxide was synthesized via a new and facile Approach. To find the optimal conditions for the synthesis of the nanostructured zinc cobalt oxide, the role of some preparation factors was explored. Outcomes of this investigation exhibited that the size and shape of zinc cobalt oxide nanostructures were substantially affected with the examined factors. The as-formed zinc cobalt oxide nanostructures were characterized by FT-IR, FESEM, EDS, and XRD. From the obtained findings, it was found that with the aid of this new approach may be produced sphere-like zinc cobalt oxide nanostructures with appropriate homogeneity. Furthermore, the photocatalyst efficiency of as-formed zinc cobalt oxide nanostructures was evaluated via removal of the toxic pollution under visible light.