The Mo-promoted the nanosolid acid SO42-/Fe2O3 are characterized by the method of IR, TEM, and B.E.T. The result shows that SO42-/Fe2O3-MoO3 is superfine solid (< 30nm) belonging to nanocrystal and has high specific surface area. SO42- is combined with metal ions of catalysis in a bidentate state. The various metal oxide-promoted nanosolid acid SO42-/Fe2O3 was investigated in the synthesis of 1,1,3-tributoxy-butane. The reactions were carried out in the liquid phase under atmospheric pressure. The dependencies of conversion, selectivity and the product distribution on the ratio of two metals, the calcining temperature, the immersing concentration of ammonium sulfate solution and the reactant/catalyst ratio were investigated. In this reaction, the selectivity to 1, 1,3-tributoxy-butane up to 79.8% at conversions up to 76% have been observed when the SO42-/Fe2O3-MoO3 was uesd. (c) 2005 Elsevier B.V. All rights reserved.