It was successful synthesized the ion exchange resin poly([(2-methacryloyloxy) ethyl]) trimethylammonium chloride) PClMETA by radical polymerization to study the removal properties towards vanadium (V) and molybdenum (VI) and compared with the commercial resin AmberliteIRA-402 which contains the same functional group. The resin was characterized by FT-IR and SEM. Parameters including water adsorption capacity, effect of the pH, maximum retention capacity of the metal ions, elution, regeneration, adsorption time, and adsorption isotherms were studied. All the studies were carried out in Batch and Column equilibrium procedures. Thermodynamic parameters such as enthalpy, entropy, and free energy were calculated. The PClMETA resin showed higher capacity to remove V(V) and Mo(VI) from water solution than Amberlite IRA-402 commercial resin. The higher capacity displayed by PClMETA resin was attributed to the higher degree of swelling and different structure that Amberlite IRA-402 resin.