Using a long alkyl-polyamine triethylene-tetramine as structure-directing agent, FeZSM-35 zeolites were synthesized and characterized by XRD, SEM, FTIR and TG-DTA techniques. EDS and ICP-AES indicate that the transition metal iron ions were framework elements and the mass fraction was 0.48%. The catalytic activity of as-synthesized crystals was examined for the aqueous hydroxylation of phenol with hydrogen peroxide. The phenol conversion was 18.8% and the selectivity on catechol and hydroquinone was ca. 69.1% and 30.9%, respectively. The as-synthesized FeZSM-35 zeolites show relative high selectivity towards catechol and could be a promising catalyst.