Lys-Zn, Lys-Co, Lys-Cu and Lys-Ni complexes prepared by reaction of metal acetates with lysine (Lys). Complexes were characterized by elemental analysis (C, H, N and M), (UV/Vis) electronic spectra, FT-IR, 1H-13C NMR, (ESR) spectroscopy, Thermal analyses (TGA) and magnetic moments measurements. Physical studies were applied on the synthesis complexes such as solubility, density, molar volume, refractive index and excess refractive index and electronic (UV/Vis) spectra measurements. Nickel oxide nanoparticles synthesized from calcinations of complex at 800 o C. Nanoparticles were characterized by (XRD) and (TEM). Molecular size is at range 43-52 nm. Nanoparticles were used to remove dyes from aqueous solution such as methylene blue (MB) and the percent of removal is 96 %. The best model which represents the adsorption of MB is Langmuir isotherm. The best model for adsorption kinetic of MB ispseudo-second-order model with determination coefficient (R 2 ) close to the unity.