The presence of dyes in water is the most popular problem recently, so the current study was directed towards the synthesis of an effective material consisting of NiO and MWCNTs. The NiO/F-MWCNTs nanocomposite was synthesized using a simple hydrothermal method after functionalization of MWCNTs using sulfuric acid and nitric acid and utilized as an efficient surface to adsorption of malachite green dye from polluted water. The nanocomposite sample was characterized using several techniques are X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Thermogravimetric analysis (TGA), Field emission scanning electron microscopy (FESEM), High- resolution transmission electron microscopy (HRTEM), Brunauer–Emmett–Teller (BET) surface area analysis, Barrett-Joyner-Halenda (BJH) analysis and Energy dispersive X-ray (EDX). The analytical results showed that the prepared nanocomposite is of good crystalline nature with a particle size of 25.43 nm. A significant specific surface area was 412.08 m2/ g which indicates the effective impact of the nanocomposite in the adsorption of malachite green (MG) dye. On the other hand, the effect of adsorbent dose, temperature, acidic function and contact time on the adsorption efficiency of dye was studied. The kinetics of dye adsorption were also investigated employing two kinetic models, pseudo-first-order model and pseudo-second-order model. Finally, the thermodynamic functions were determined to identify the type of the reaction and the spontaneity of the process.