For the first time the mesoporous titanium phosphates with high surface area and highly thermal stability were synthesized using long-chain n-alkylamine as structure-directing agents under an ethanol system containing a small quantity of water. Powder X-ray diffraction (XRD) and transmission electron micrograph (TEM) show that the disorder mesopores exist in the mesostructured materials. The mesoporous titanium phosphates calcinated at 500 degrees C for 10 h still retain the refined pore structure and the high surface area. UV-vis absorption suggests most of titanium is tetrahedrally coordinated in the framework of calcinated mesoporous titanium phosphates. The high catalytic activity in the liquid-phase partial oxidation of cyclohexene with H2O2 oxidant supports the tetrahedral coordination of titanium in these materials. (C) 2006 Elsevier B.V. All rights reserved.