Transition metal oxides are extensively investigated as alternative anode materials for lithium ion batteries owing to their high theoretical capacity. In this work, mesoporous nickel oxide nanostructure is synthesized by a simple solution method without high calcination temperature. The sample is characterized using X-ray diffraction, Fourier Transform Infra Red (FT-IR), Scanning Electron Microscopy, Transmission Electron Microscopy, Nitrogen adsorption–desorption isotherm and surface pyridine adsorption. Large surface area, nanosphere particles, mesoporous structure and surface lewis acidic and Brönsted sites are confirmed. The electrochemical properties of mesoporous nanonickel oxide is investigated including the cycling performance as anode material for lithium ion batteries. The results show that nanonickel oxide has a high discharge capacity at 1 C, especially the first 5 cycles, compared to previous studies at low rates (0.035 and 0.14 C) with the same material. Also, nanonickel oxide shows good efficiency through charge–discharge cycles. All results and data are correlated and discussed.