Turkish perlite supported nickel oxide as the heterogeneous acid catalyst for a series of Claisen?Schmidt condensation reactions

Authors: SAKSHI KABRA MALPANI, DEEPTI GOYAL, STUTI KATARA, ASHU RANI

Abstract: Potentially active and eco-friendly solid acid catalysts have been synthesized by loading different weight percentages (10, 15, and 50) of nickel oxide on thermally activated Turkish perlite through the deposition-precipitation method. Structural features of prepared catalysts were analyzed using BET surface area analysis, X-ray diffraction, scanning electron microscope (SEM), SEM-EDX, transmission electron microscopy (TEM), Fourier-transform infrared (FT-IR), pyridine adsorbed FT-IR, UV-Vis diffuse reflectance spectroscopy (DRS), and thermogravimetric analysis (TGA) techniques. Pyridine adsorbed FT-IR analysis confirmed the presence of the optimum amount of Bronsted acidic sites in a catalyst having 15 wt. % loading of nickel oxide, which was tested for catalyzing a series of Claisen-Schmidt condensation of cyclohexanone and aromatic aldehydes to produce good isolated yield (90%-93%) of 2,6-bis(substituted benzylidene)cyclohexanones, significantly used in anti-tumor and cytotoxic activities. The high catalytic efficiency of the chosen catalyst remains almost intact up to six reaction cycles. On higher wt. % loading of nickel oxide, crystallite size increases along with agglomeration of larger nickel oxide particles on catalyst surface resulting in pore blockage and poor catalytic activity. Loading of NiO on the surface of thermally activated Turkish perlite was confirmed by SEM-EDX analysis, and TEM observations show that the particle size of the preferred catalyst was less than 50 nm. Based on results drawn from XRD, FT-IR, pyridine adsorbed FT-IR, UV-Vis DRS studies, model structures were proposed for Turkish perlite and all prepared catalysts. During this work, the catalytic potential of the preferred catalyst was compared with other previously reported catalysts, and it showed appreciable results. The formed products were further confirmed by their melting point and ¹H-NMR analysis.

Keywords: Turkish perlite, nickel oxide, solid acid catalyst, Claisen-Schmidt condensation, 2,6-bis(substituted benzylidene) cyclohexanones

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