Abstract: The mixed mesoporous sieves Ti-AlKIT-1 materials were prepared through Ti grafting on AlKIT-1 obtained either directly or by post-synthesis using relatively inexpensive aluminium and titanium precursors,and characterized by FT-IR,XRD,MAS NMR,DRS,EDS and physical adsorption-desorption of nitrogen and used as catalysts toward the oxidation of cyclohexanol in 30% H₂O₂.XRD and N₂ adsorption-desorption showed that the original mesoporous structure of the Ti-AlKIT-1 was retained with a lower BET surface area,pore volume and smaller pore size.Based on the combined FT-IR and DRS studies,it was concluded that the infrared spectroscopy can result a powerful tool to verify the Ti(Ⅳ) incorporation into the framework of AlKIT-1.²⁷Al MAS NMR spectra indicated that the ammoniun-washed samples present only tetracoordinated aluminium.All Ti-AlKIT-1 catalysts showed significant activity in the oxidation of cyclohexanol due to the cooperative action of Ti and Al.Ti-Al(ds)KIT-1 with higher Ti/Al molar ratio and BET surface area and pore volume showed better catalytic activity than Ti-Al(ps)KIT-1.The as-prepared catalyst is stable and reusable.The conversion of cyclohexanol was 51.3% after three runs,only decreased by 4.31% after 48 h catalytic reaction at 80℃.