Organic-inorganic hybrid mesoporous anion-exchange resins were prepared for the adsorption of anions from aqueous solutions. The prepared samples were characterized using nitrogen adsorption-desorption measurements, Fourier transform infrared (FTIR) spectroscopy, and elemental analyses. Batch and kinetic experiments were performed to examine the anion-exchange performances of the prepared samples. Among the prepared samples, the hybrid mesoporous anion-exchange resins functionalized with tributylammonium groups showed higher adsorption capacities for perrhenate ions than did the resin functionalized with trimethylammonium groups. The surfactant, hexadecylamine, which had hydrophobic alkyl chains, also showed affinity for hydrophobic perrhenate anions.