Cu-SBA-16 has been prepared by one-pot synthesis method, and Characterized by XRD, TEM, and N-2 adsorption measurements. An extended study about the nature of copper species in the Cu-SBA-16 has been performed by FT-IR, UV-DRS, H2-TPR and XPS. The copper species is mainly present on the mesoporous SBA-16 in the form of isolated mononuclear Cu2+ ions and highly dispersive CuO nanoclusters. The excellent catalytic activity has been obtained for phenol hydroxylation due to the presence of high amount of highly dispersive Cu species. The conversion to phenol and selectivity to diphenol are 29.4 and 91.5%, respectively.