A functionalized NiFe2O4/MnO2 nanocomposites have been synthesized via a facile hydrothermal approach. The NiFe2O4/MnO2 nanocomposites shows the fast Pb(II) adsorption performance and high adsorption capacity. The NiFe2O4/MnO2 nanocomposites is easily separated from the solution by an external magnet within a short period of time. The NiFe2O4/MnO2 nanocomposites exhibits a good regeneration and reusability performance after six-cycle regenerations.