A new class of supermicroporous mixed oxides, with pore sizes in the 10-20 Å range has been prepared utilizing basic metal acetates. The reactions are carried out in non-aqueous solvent media to which an excess of amine is added. Hydrolysis of the reagents is effected by addition of a water-propanol mixture and refluxing. The amine and solvent are removed by thorough washing and/or calcining at temperatures as low as 200° C. Mixtures of transition metal oxides with either ZrO2, TiO2, La2O3, SiO2, Al2O3 or mixtures thereof were prepared. The surface area curves of the pure oxides are Type I with surface areas of 400-600 m2/g and up to 1100 m2/g for the mixed oxides.