AbstractA series at mixed oxides of titanium and phosphorus were prepared by co‐precipitation method accompanying refluxing treatment. The effect of the pH values of the solutions on the structures, compositions, and surface acidities of the resultants compounds was determined. The samples were characterized by BET surface area measurement, X‐ray powder diffraction (XRD) for structural analysis and amine‐titration for surface acidities. After calcinating the oxides at 773 K, the surface acidities were attributed mainly to Ti(OH)PO4structure. Elemental analysis revealed that the P/Ti ratios in the samples decreased with increasing the pH value of the preparative solution. When the mixed oxides were used as catalysts for 2‐propanol decomposition reaction, the highest activities were obtained over the samples prepared in the solutions with the pH values being 2 or 3. That result was in agreement with the variation in surface area and acid amount of the ca