Mesoporous TiO2 Was prepared by simply controlling the hydrolysis of Ti(OBu)(4) with the help of acetic acid. The mesoporous TiO2 had a well-crystallized anatase phase and a high surface area of 290 m(2) g(-1) with a pore size of about 4 nm. The anatase phase and the mesoporous structure were maintained in the VOx/TiO2 catalyst with a monolayer dispersion Of V2O5, however, the Surface area decreased to 126 m(2) g(-1). The catalyst was highly active and selective for methanol oxidation, giving about 55% conversion of methanol and 85% selectivity to dimethoxymethane at 423 K. (C) 2009 Elsevier B.V. All rights reserved.