Sulfate-promoted metal oxides of ZrO2 (SZ) and Fe2O3 (SF) and the mixed oxide ZrO2-Fe2O3 (SZF) have been prepared by coprecipitation and wet impregnation techniques. The synergistic effect of the dopant metal oxide in the matrix of the parent sulfated oxide, SQ(4)(2-)/ZrO2 (SZ), has been studied for the alkylation reaction of benzene with benzyl chloride. An attempt has been made to decrease the polyalkylation observed on the highly reactive catalyst, SO42-/Fe2O3(SF), Detailed kinetic study of the reaction has been carried out to evaluate the kinetic parameters.