The heteropolyacid salt Fe2H2P2Mo16V2O62•41H2O catalyst was prepared, and characterized by inductive coupling plasma emission spectrum, Fourier transform infrared spectroscopy, X-ray powder diffraction, and thermal analysis. In this work, the catalytic activity was studied for alkylation of benzene with benzyl chloride to diphenylmethane. The influences of different parameters such as the amount of reactants, the reaction temperature, and the reaction time on alkylation of benzene were also investigated. Experimental results show that Fe2H2P2Mo16V2O62 was found to be a suitable catalyst for the alkylation of benzene with benzyl chloride to diphenylmethane. A maximum of conversion of benzyl chloride was obtained to be 99.5% with selectivity to 98.7% for diphenylmethane under the optimized reaction conditions over Fe2H2P2Mo16V2O62•41H2O.