A mesoporous MoO 3 /TiO 2 composite was prepared from titanate derivative by consecutive self-supporting and ammonia method. All samples were characterized by X-ray Diffraction, N 2 adsorption-desorption, Raman Spectra and Field-Emission Scanning Electron Microscopy. The results showed that mesoporous MoO 3 / TiO 2 composite had a higher surface area (173 m 2 /g) and a better MoO 3 dispersion than that prepared by traditional impregnation (90 m 2 /g). As for hydrodesulfurization tests, mesoporous MoO 3 /TiO 2 composite in this case presented a better catalytic performance, attributed to its high surface area and good dispersion of MoO 3 . It can be found that self-supporting played a key role in preparing mesoporous MoO 3 /TiO 2 composite with high surface area. Additionally, aqueous ammonia could effectively dissolve excess MoO 3 , which helped to obtain mesoporous MoO 3 /TiO 2 composite with better dispersion of MoO 3 .