Magnetic NiFe2O4 nanoparticles have been synthesized and used as adsorbents for copper removal from aqueous solution. The NiFe2O4 nanoparticles were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction, and Fourier transform infrared spectroscopy. The batch removal of Cu2+ ions from aqueous solutions using NiFe2O4 magnetic nanoparticles under different experimental conditions was investigated. The effects of initial concentration, adsorbent dose, contact time, and pH were investigated. The adsorption process was pH dependent, and the maximum adsorption was observed at a pH of 6.0. Equilibrium was achieved for copper ion after 25 min. Experimental results showed that NiFe2O4 magnetic nanoparticles are effective for the removal of copper ions from aqueous solutions. The pseudo-second-order kinetic model gave a better fit of the experimental data as compared to the pseudo-first-order kinetic model. Experimental data showed a good fit with the Langmuir isotherm model.