Aim of this work is to synthesizing a new highly efficient adsorbent as of magnesium oxide (MgO 2 ) entrapped Polypyrrole (Ppy) nanocomposite preparation for toxic pollutant of fluoride removal form drinking water. The synthesized MgO 2 /Ppy hybrid nanocomposite shows an extraordinary defluoridation capacity of 4328 mg F − Kg −1 in the room temperature through batch adsorption technique. It was performed to know the effect of various parameters such as contact time, initial concentration, pH, competitor ions and temperature. The structural and morphological changes on the fluoride adsorbent in before and after were analyzed by using XRD, FTIR & SEM techniques. The adsorption isotherm of Freundlich, Langmuir, & Dubnin -Radushkevich isotherms were studied and the fluoride adsorption is well fixed with Langmuir isotherm model. The kinetic model studies were carried out by both diffusion and reaction based models. The mechanism of fluoride on the MgO 2 /Ppy nanocomposite is mainly influence the interaction of electrostatic adsorption and ion-exchange. The reusability and regeneration studies were performed for the reusability of the nanocomposite.