Iron-incorporated mesoporous silica materials (MFS-9) have been successfully prepared in strong acidic media by a two-step synthesis procedure, which has an hexagonal structure with uniform mesopores and exhibits superior hy-drothermal stability and high catalytic activities for the hydroxylation of phenol and also of bulky trimethylphenol. X-ray diffraction data show that mesoporous ferrisilicate (MFS-9) can retain its mesoporous structure in boiling water up to 100 h. Characterization of MFS-9 by a variety of spectroscopic techniques, including electron spin resonance, UV– vis and UV–Raman spectroscopies, suggests that Fe species in the framework of MFS-9 are mainly tetrahedrally co-ordinated even after calcination at 823 K.