Aluminated mesoporous silica was prepared by multiple post-grafting of alumina onto uniform mesoporous SiO_2 ,which was assembled from monodisperse SiO_2 microspheres.Hydrodesulfurization(HDS)catalyst was prepared by loading Ni and Mo active components onto the aluminated uniform mesoporous SiO_2 ,and its HDS catalytic performance was evaluated using hydrodesulfurization of dibenzothiophene as the probe reaction at 300°C and 6.0 MPa in a tubular reactor.The samples were characterized by N_2 physisorption,scanning electronic microscopy,Fourier transform infrared spectrum,X-ray diffraction(XRD),temperature-programmed desorption of ammonia(NH_3-TPD),~(27)Al nuclear magnetic resonance(~(27)Al-NMR)and high-resolution transmission electron microscopy(HRTEM).The results showed that the Si–OH group content of SiO_2 was mainly dependent on the pretreatment conditions and had significant influence on the activity of the Ni Mo catalyst.The surface properties of the aluminated SiO_2 varied with the Al_2O_3-grafting cycles.Generally after four cycles of grafting,the aluminated SiO_2 behaved like amorphous alumina.In addition,plotting of activity of Ni Mo catalysts supported on aluminated meso–macroporous silica materials against the Al_2O_3-grafting cycle yields a volcano curve. Aluminated mesoporous silica was prepared by multiple post-grafting of alumina onto uniform mesoporous SiO 2, which was assembled from monodisperse SiO 2 microspheres. Hydrogen desulfurization (HDS) catalyst was prepared by loading Ni and Mo active components onto the aluminated uniform mesoporous SiO 2, and its HDS catalytic performance was evaluated using hydrodesulfurization of dibenzothiophene as the probe reaction at 300 ° C and 6.0 MPa in a tubular reactor. These samples were characterized by N2 physisorption, scanning electronic microscopy, Fourier transform infrared spectrum, X-ray diffraction (XRD), temperature- (27) Al nuclear magnetic resonance (~ (27) Al-NMR) and high-resolution transmission electron microscopy (HRTEM). The results showed that the Si-OH group content of SiO_2 was mainly dependent on the pretreatment conditions and had significant influence on the activity of the Ni Mo catalyst. The surface properties of the aluminized SiO 2 varied with the Al 2 O 3 -grafting cycles. Generally after four cycles of grafting, the aluminized SiO 2 behaved like amorphous alumina. In addition, plotting of activity of Ni Mo catalysts supported on aluminated meso-macroporous silica materials against the Al 2 O 3 -grafting cycle yields a volcano curve.