Mesoporous aluminosilicate (MAS) was synthesized by hydrothermal method with zeolite NaY as precursor and CTMAB (cetyltrimethylammonium bromide) as structure directing agent. Desulfurization adsorbents were characterized with XRD, BET, FTIR and NH3-TPD. FTIR results showed that Lewis acid sites act as adsorption centers for dibenzothiophene (DBT) molecules. The adsorption desulfurization ability of MAS was studied in model and hydrotreated diesel. For model oil containing 10mmol/L DBT, the adsorption capacity of adsorbents is NaY > MAS > MCM-41. For hydrotreated diesel, MAS shows the largest adsorption capacity, MCM-41 the second, and NaY shows the least adsorption capacity. The improvement of desulfurization ability of improvement of MAS by Cu(I) is more significant than that of MCM-41. The physicochemical properties of fuels, such as viscosity and aromatics concentration had great influence on the desulfurization property of adsorbents. (c) 2007 American Institute of Chemical Engineers AIChE J, 53: 3263-3268, 2007.