Three titanium-containing aluminum phosphate catalysts with a general formula Al 0.77 Ti 0.23 PO 4 were prepared by the sol-gel method at room temperature(APTS), and a nonuniform precipitation procedure at room temperature(APTR) and under reflux(APTF), respectively. The structural features and the surface properties of the three catalysts were determined by means of the physical adsorption of nitrogen at liquid N 2 temperature, XRD, UV-Vis, NH 3-TPD and IR of adsorbed pyridine. The vapor phase O-alkylation of catechol with ethanol over the prepared catalysts was studied. It was found that the activity and the selectivity of these catalysts are greatly dependent on the preparation method, and catalyst APTF shows the highest activity and selectivity. The characterization evidence indicates that the weak Brnsted acid sites were more effective for the reaction. Three titanium-containing aluminum phosphate catalysts with general formula Al 0.77 Ti 0.23 PO 4 were prepared by the sol-gel method at room temperature (APTS), and a nonuniform precipitation procedure at room temperature (APTR) and under reflux (APTF) respectively. The structural features and the surface properties of the three catalysts were determined by the method of the physical adsorption of nitrogen at liquid N2 temperature, XRD, UV-Vis, NH3-TPD and IR of adsorbed pyridine. The vapor phase O- alkylation of catechol with ethanol over the prepared catalysts was studied. It was found that the activity and the selectivity of these catalysts are significantly dependent on the preparation method, and catalyst APTF shows the highest activity and selectivity. The characterization evidence indicates that the weak Brnsted acid sites were more effective for the reaction.