Preparation and Characterization of Ni/Zr-Saponite as Catalyst in Catalytic Hydrogen Transfer Reaction of Isopulegol

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Abstract:

World demand on menthol is so high and it is also a chalenge for organic synthetic chemist to develop new method of synthesis and conversion from another sources. Tandem cyclization-hydrogenation reaction towards citronellal is one important mechanism recently. Within the mechanism, hydrogenation of isopulegol is rate determining step. Considering green chemistry principles, this research deals with the use of heterogeneous catalyst in hydrogenation, Nickel (Ni) and also the use of microwave assisted organic synthesis method. An effort to improve activity and reusability of nickel in the reaction was conducted by dispersion in pillared clay materials, Ni-saponite.Nickel immobilized zirconia pillared saponite (Ni/Zr-Saponite) was prepared using pillarization-impregnation method. The composite, Zr-Saponite and Saponite were characterised by Scanning Electron Microscopy-energy dispersive x-ray (SEM-EDX), x-ray diffraction (XRD), surface acidity and surface area parameter based on nitrogen adsorption-desorption method. Catalytic hydrogen transfer of isopulegol hydrogenation was used as reaction model to show the comparison of catalytic activity.The XRD and SEM-EDX results of the composite indicate that zirconia was successfully distributed as pillar and nickel was dispersed within the pillared material. Both modifications increased the specific surface area, pore volume and surface acidity as a result of pillar formation and homogeneous distribution of the particles. Compared to raw saponite and Zr-Saponite, the composite exhibits significant improvement on total conversion of isopulegol. The presence of nickel affect the hydrogenation mechanism as showed by the product of menthol by catalytic hydrogen transfer.

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311-316

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August 2015

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