Aluminum oxide/polyaniline nanocomposite is prepared by a new and one-pot method including in situ electrooxidation of aluminum and electropolymerization of aniline. The product has been characterized by elemental analysis, FT-IR spectroscopy, X-ray diffraction (XRD), Field Emission Scanning Electron Micrographs (FESEM), and Transmission Electron Micrographs (TEM) techniques. ICP-OES was used for determination of aluminum in the prepared nanocomposite. A porous structure of the prepared composite has been shown by FESEM images. TEM of the product confirms the presence of exfoliated aluminum oxide nanofibers. The adsorption potentials of the prepared nanocomposite towards Cu 2+ , Pb 2+ , Zn 2+ , Cd 2+ , Ni 2+ and Co 2+ ions were evaluated in batch adsorption experiments. The results show that the adsorption efficiency is controlled by aqueous phase pH. The experimental data was well interpreted by considering the Langmuir model. The kinetics of the adsorption processes can be well interpreted by pseudo-second-order equation.