In this study, novel magnetic chelating ligands focused on Cu 2þ removal from aqueous solutions were synthesized. The magnetic adsorbents were obtained by amidoximation of nitrile groups on starch-g-polyacrylonitrile/montmorillonite/Fe 3 O 4 . The magnetic Fe 3 O 4 nanoparticles were obtained in situ in the presence of montmorillonite clay. The structure of nanocomposites was characterized by FT-IR, SEM, TEM, XRD, TGA, and VSM techniques. Batch adsorption experiments were done on the subject of nanocomposite composition, pH, adsorption time, initial Cu 2þ ions concentration, and temperature. Moreover, the thermodynamic and kinetic of adsorption process as well as the equilibrium of adsorption process were studied. The efficiency of Cu 2þ removal by nanocomposites was dependent on the content of magnetic montmorillonite, and the magnetic adsorbents showed high adsorption capacity for Cu 2þ .Adsorption capacity of adsorbents was found to increase with increasing the pH of Cu 2þ solution up to 5.5. According to the thermodynamic parameters, the adsorption of Cu 2þ on magnetic adsorbents occurred spontaneously. The equilibrium adsorption data were analyzed with Langmuir and Freundlich models and it was found that the equilibrium process followed the Langmuir model well.