Phosphorus Modulation Effect on the Solvent-free Oxidation of Cyclohexylamine to Cyclohexanone Oxime Catalyzed by TiO2/MCM-41
TiPO/MCM-41 was synthesized by liquid phase hydrolysis method.The structure and properties of these catalysts were characterized by BET,FT-IR,XPS,XRD,SEM and TEM characterization techniques.The catalytic performance of TiPO/MCM-41 in the solvent-free oxidation of cyclohexylamine to cyclohexanone oxime was further studied.The probable liquid phase oxidation pathway of cyclohexylamine was also suggested.The results indicated that the titanium hydroxyl groups on the surface of TiPO/MCM-41 were the active centers for catalytic oxidation of cyclohexylamine.It was verified that TiPO/MCM-41 demonstrated goodish catalytic activity and repeatability.The optimal reaction conditions were obtained that temperature was 90℃,pressure was 1.0 MPa,time was 5 h and catalyst amount was 0.3 g,and 59.0%of cyclohexylamine conversion with 87.9%of selectivity to cyclohexanone oxime was achieved.The method developed in this study provides a green route for the highly efficient synthesis of cyclohexanone oxime,and has certain industrial application potential.
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