Mesoporous Ta2O5 materials functionalized with both alkyl group and a Keggin-type heteropoly acid. Ta2O5/SiO2-[H3PW12O40/R] (R = Me or Ph), was prepared by a single step sol-gel co-condensation method followed by a hydrothermal treatment in the presence of a triblock copolymer surfactant. The catalytic performance of the resulting multifunctionalized organic-inorganic hybrid materials was evaluated by a direct use of soybean oil for biodiesel production in the presence of 20 wt% myristic acid under atmosphere refluxing, and the influences of the catalyst preparation approaches, functional component loadings, and molar ratios of oil to methanol on the catalytic activity of the Ta2O5/SiO2[H3PW12O40/R] were studied. In addition, the recyclability of the hybrid materials was evaluated via four catalytic runs. Finally, the network structures of the hybrid materials and the functions of the incorporated alkyl groups on the catalytic activity of the materials were put forward. (C) 2009 Elsevier B.V. All rights reserved.