In order to prepare functionalized mesoporous materials with sulfonic acid groups used as solid acid catalysts or as separation materials, a simple secondary modification method has been developed. Based on our previous work, SBA-15 materials with a high surface silanol density were prepared by simultaneously removing templates and crystallizing under acidic and hydrothermal conditions. Then the functionalization of SBA-15 mesoporous silica with thiol groups and the oxidation of thiol to sulfonic acid groups were carried out under the same hydrothermal conditions with a dilute aqueous H2O2 solution as the oxidizing agent. Furthermore, the idea of coupling functionalization and oxidation into one step was tested, and the functionalized SBA-15 materials with sulfonic acid groups (SO3H-SBA-15) that were successfully prepared had an acid exchange capacity reaching 1 mequiv of H+/g of SO3H-SBA-15 as determined by a corrective base titration. SO3H-SBA-15 characterized by FT-IR, NMR, XRD, nitrogen adsorption and desorption, TGA, and hydrothermal stability experiments, exhibited a good long-range order, high specific surface area (about 600 m(2)/g), uniform pore sizes (about 6 nm), and high thermal and hydrothermal stabilities. SO3Ag-SBA-15 via ion exchange of S03H-SBA-15 with Ag+ was used to remove dibenzothiophene (DBT) from octane. The adsorption capacity reached as high as 17.0 mg S/g Of SO3Ag-SBA-15. (c) 2005 Elsevier Inc. All rights reserved.