Nickel oxide-carboxymethyl cellulose (NiO-CMC) nanocomposite was synthesized by the co-precipitation method to remove the methylene blue (MB) dye from wastewater. The synthesized nanocomposite was characterized by Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Energy dispersive X-ray analysis (EDX), Transmission electron microscope (TEM) as well as X-ray diffraction (XRD). Different factors such as the effect of the initial dye concentration, contact time, temperature, nanocomposite concentration, and pH parameters were investigated, and the obtained data showed that the optimum conditions to remove the MB were 3 mg/L, 4 hrs, 65 ∘C, 8 mg and pH 6, respectively. Furthermore, the adsorption kinetics, equilibrium isotherms, and thermodynamic were investigated, and data were agreed with the pseudo-secondorder equation and Langmuir model, respectively. Moreover, ΔS o , ΔH o , and ΔG o were calculated, and the results were indicated that the adsorption of MB via prepared Ni/CMC nanocomposite was an endothermic and spontaneous process (Graphical abstract NiO CMC).