Iron and titanium modified MCM-41 materials, prepared by direct synthesis were investigated using X-ray diffraction (XRD), nitrogen physisorption, UV-Vis diffuse reflectance, Mossbauer, FT-IR and EPR spectroscopies. Materials with high surface area and well-ordered pore structure were obtained. All modified mesoporous silicas possess high activity in cyclohexanol conversion. FeTiMCM-41 (Si/Ti = 10, Si + Ti/Fe = 15) catalyst presented the highest activity and selectivity to cyclohexanone.