A method of incorporating iron onto the mesoporous silica network using potassium ferricyanide (K3Fe (CN)6) as the iron source was established. The Fe (CN)63 + ions interact with the template and attached onto the silica network after the as-synthesized sample calcined at 823 K. FT-IR spectroscopy provided a clear evidence for the interaction between cyanide ligands and template. XANES spectroscopic displayed that the Fe3 + changed from octahedral to tetrahedral coordinated during thermal treatment. XRD and HRTEM results indicated that the iron ions incorporated onto the silica network without destroying the lattice structure of the parent MCM-41. The synthesized material exhibited a good activity for phenol hydroxylation.