Ion exchange resin poly(4-vinylbenzyl) trimethylammonium chloride(P(ClVBTA)) was synthesized and its removal properties toward vanadium(V) and molybdenum(VI) were evaluated and compared with those of the Amberlite IRA-402 commercial resin. The resin was characterized by FT-IR spectroscopy, TGA, and SEM. The water absorption capacity, pH effect, Langmuir and Freundlich adsorption isotherms, and kinetic model parameters were determined. All studies were conducted through a batch equilibrium procedure. Thermodynamic parameters, including enthalpy, entropy, and free energy, were determined. The P(ClVBTA) resin showed faster and higher capacity for the removal of V(V) and Mo(VI) from a water solution than the Amberlite IRA-402 commercial resin with the same ammonium salt functional group. The higher capacity of the P(ClVBTA) resin was attributed to the higher degree of swelling, the exfoliation in the monolayer, and the small particle size.