According to the increasing development of the mankind, social and technology activities in the earth, various industry is in a state of uncontrolled growth. In the present study, magnetite/nickel oxide mixed metal oxide nanoparticles (FNMMO NPs) were prepared by a simple method assisted by ultrasonic waves and applied as a novel adsorbent to dispose of dye wastewater. The morphology and chemical structures of the Fe3O4, NiO and FNMMO NPs were characterization by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), energy-dispersive X-ray spectroscopy (EDX), scanning electronic microscope (SEM) and transmission electron microscope (TEM). The adsorption of methylene blue (MB) onto FNMMO NPs was studied in relation to initial concentration of MB, contact time, adsorbent dose and pH value of solution. The equilibrium adsorption isotherm was fitted by Langmuir isotherm. The capacity of adsorption was evaluated 40.1 mg.g-1 and the time required to reach the adsorption equilibrium was 180 min.