Occurrence of fluoride in groundwater is a serious concern due to its fatal effects. Functionalized hexagonal boron nitride sheets have been combined with nickel hydroxide nanoparticles by a one step process and a hybrid adsorbent Ni(OH)2@hBN has been developed with an exceptionally high fluoride adsorption capacity of 365 mg g−1, higher than those of Ni(OH)2 and hBN. This maximum adsorption capacity is higher than those of most common adsorbents used for defluoridation including activated alumina, reported nickel oxide and carbon-based 2D material-supported alumina adsorbents. The presence of functionalized boron nitride significantly increased the surface area to 680 m2 g−1 with a pore volume of 0.33687 cm3 g−1 and provided rich hydroxyl group-containing surface sites for the removal of fluoride present in contaminated water. In addition, the adsorption of fluoride onto boron nitride-modi fied nickel hydroxide followed pseudo-second-order kinetics and the equilibrium data fitted well with the Langmuir adsorption isotherm, suggesting a monolayer adsorption mechanism. Furthermore, the material developed is tested with the water sample collected from a real affected area, from the Dhar district of India, and the material showed promising results in terms of fluoride removal efficacy.