Highly ordered Fe-MCM-48 was synthesized by a mixed templation method under low molar ratio (0.17:1)of mixed surfactants to silica and characterized by XRD, Si-29-MAS NMR, ESR, and UV-Visible. Its catalytic activity and selectivity was studied for phenol hydroxylation using H2O2 (30%) The substituting element (Fe3+) is partially incorporated into the framework position forming a new type of active site which raises the phenol conversion to 43.6% and the diphenol (the mixture of catechol (CAT) and hydroquinone (HQ)) selectivity to 97.7%.