Nano Co3O4/ZnO have been successfully synthesized by a simple and green gel combustion method followed by calcination at 600 o C. Sugar was used as fuel for combustion in this work. The nano Co3O4-ZnO were characterized by X-ray diffraction (XRD), Energy Dispersive X-Ray analysis (EDAX) and Scanning electron microscopy (SEM). Co3O4-ZnO was applied as an adsorbent to remove lead from aqueous solution. EDAX strongly proved the adsorption of lead on the surface of Co3O4-ZnO adsorbent. By increasing the amount of ZnO on the structure of the Co3O4-ZnO samples, the adsorption of Pb 2+ on the surface increased too. The SEM images also help the confirmation of lead adsorption on the surface of as synthesized samples. The concentrations of remained Pb 2+ ions were also measured by atomic absorption spectroscopy (AAS) and reported in the terms of removal efficiency.