Titanium-containing mesoporous silica has been prepared by silylation of mixed oxides obtained via sol-gel method. These samples displayed enhanced activity in the epoxidation of styrene with (BuOOH)-O-t in comparison to normal xerogels or other titanium-containing catalytic systems. The influence of the extension of the silylation reaction, as well as the use of different silylating agents, have been investigated. Samples were characterised by FTIR, XRF, Si-29-MAS NMR, diffuse reflectance UV-Vis and N-2 adsorption-desorption isotherms, X-ray photoelectron spectroscopy (XPS) and FTIR of adsorbed deuteroacetonitrile. The improvement in the catalytic activity achieved has been related to the removal of OH groups by means of calcination or silylation treatments. (C) 2000 Elsevier Science B.V. All rights reserved.