Bimetallic Fe-Ti-TUD-1 three-dimensional amorphous mesoporous materials were successfully synthesized via sol-gel method, using tetraethylammonium hydroxide (TEAOH) as a structural directing agent; silatrane, FeCl3, and Ti(OCH(CH3)(2))(4) as silica, iron, and titanium sources, respectively. The obtained Fe-Ti-TUD-1 has a foam-like mesoporous structure with surface area ranging from 625 to 725 m(2)/g, an average pore size of 6 nm, and a pore volume of 0.97 cm(2)/g. The phenol hydroxylation of the samples was evacuated using H2O2 as the oxidant and water as the medium. The effects of influence parameters, such as temperature, reaction time, catalyst amount, amount of oxidant, and metal loading, were investigated; the optimum condition was found to be a ratio of 1:3 phenol:H2O2, using 30 mg of catalyst at 363 K for 1 h. For comparison, photocatalysisfor phenol hydroxylation was studied at room temperature. The result revealed that the activity of 0.01Ti-TUD-1 was improved under UV radiation, but the overall activity resulted in lower performance than the reaction under heat. Phenol hydroxylation using 0.01Fe-0.01Ti-TUD-1 gave 93.1% conversion at 363 K with 53.4% hydroquinone (HQ) and 46.6% catechol (CAT) selectivity. As Fe incorporated into the structure, it improved the catalytic ability of Ti-TUD-1. Unfortunately, the activity of Fe dropped under the UV light since iron species were less active in this condition.