Aluminum production industry tailings are considered as hazardous solid wastes accompanied by a variety of serious disposal, environmental, and public health issues. This study is devoted to presenting a promising solution for dealing with such problems. Within the scope of the present study, synthesis of nanostructured γ-alumina from aluminum foundry tailing using a novel process was presented. The proposed process will provide a multilateral advantage to both environment and industries. Firstly, the amount of tailing and accordingly, disposal cost could be partly lessened; secondly, the environmental pollution can be reduced, and finally, if possible, green production of advanced materials from this kind of waste at a rational expense can bring about the conservation of natural sources and also gain economic benefits. Characterization of the as-synthesized products was performed using X-ray diffractometry (XRD), X-ray fluorescence (XRF), Fourier-transform infrared (FTIR) spectroscopy, field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDAX), and dynamic light scattering (DLS) for crystalline phase analysis, chemical composition, chemical bond recognition, morphology, elemental analysis, and particle size distribution, respectively. The chemical composition analyzed by XRF indicated that the as-synthesized alumina exhibits a purity of more than 97 wt%. The XRD pattern majorly possessed characteristic peaks related to the gamma phase of alumina. Microstructural analyses by FESEM and TEM confirmed the nano-sized morphology of the as-synthesized γ-alumina.