To ensure a sustainable future, it is imperative to efficiently utilize abundant biomass to produce such as platform chemicals, transport fuels, and other raw materials; hydrochar is one of the promising candidates derived by hydrothermal carbonization of biomass in pressurized hot water. The synthesis of "hydrocharwrapped Ti3AlC2N-derived nanofibers" was successfully achieved by a facile one-pot hydrothermal reaction using glucose as the hydrochar precursor. Meanwhile, cellulose and pinewood sawdust as raw materials were also investigated. Products were characterized by XRD, N-2 adsorption-desorption isotherms, SEM, TEM and FT-IR to investigate their crystal structures, textural properties, morphologies, and surface species. In the adsorption test to remove Cd(II) and Cu(II) in aqueous solution, hydrochar-wrapped nanofibers outperformed pure nanofibers derived from Ti3AlC2, hydrothermal carbon derived from glucose and commercial activated carbon. Finally, the regeneration, sorption kinetics, and possible adsorption mechanism were also explored.