Nano γ-alumina was produced using Nepheline syenite ore by leaching and precipitation process at a certain pH in the presence of sodium dodecyl sulfate (SDS) as a surfactant. The produced nanostructure was characterized by XRD, SEM, EDX, DLS, BET and FT-IR. The XRD pattern confirmed the tetragonal structure of alumina The nano structure of alumina was approved by SEM and the particle size distribution were between 41 to 486 nm, confirmed by DLS. BET analysis showed that the specific surface area of nanopowder was about 39.1 m2/g. The synthesis conditions were modeled and optimized by RSM. The optimum conditions resulted in leaching time, the mass ratio of Nepheline/HCl, and the reflux temperature of 2 h, 20, and 70 °C, respectively. Under optimum conditions, the extraction efficiency was 82%. The prepared nano γ-alumina has higher removal efficiency than commercial types in the removal of p-nitrophenol by adsorption process.