Fe(III)-salim anchored MCM-41: synthesis,characterization and catalytic activity towards liquid phase cyclohexane oxidation |
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Authors: | Sudarshan Singha K M Parida Anadi C Dash |
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Affiliation: | (1) Colloids and Materials Chemistry Department, Institute of Minerals & Materials Technology, Bhubaneswar, Orissa, 751013, India;(2) Department of Chemistry, National Institute of Science Education and Research, Institute of Physics Campus, Bhubaneswar, Orissa, 751005, India; |
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Abstract: | Abstract A novel organic–inorganic hybrid catalyst MCM-41-FeIII(salim)] was synthesized by covalently anchoring FeIII(salim) complex into the pore channels of MCM-41. The material was synthesized by the co-condensation of tetraethyl orthosilicate
(TEOS) and the precursor of salicylaldehyde modified with 3-aminopropyl triethoxysilane in the presence of cetyltrimethyl
ammonium bromide (CTAB). The Fe(III)-salicylideneimine MCM-41 mesoporous silica was generated (in situ) by taking MCM-41-salimH
(I) and FeCl3 in ethanol solution. The immobilization of the complex on the functionalized silica was confirmed by small angle X-ray diffraction
(XRD), N2 adsorption–desorption, electron paramagnetic resonance (EPR), Fourier transform infrared spectroscopy (FT-IR) and diffuse
reflectance UV–vis spectroscopy. Solid state CP-MAS NMR spectroscopy of 29Si (29Si CP-MAS NMR) showed a highly condensed siloxane network. Catalytic activity of the supported catalyst was examined by the
oxidation of cyclohexane. Cyclohexane was successfully oxidized in good conversion (68%) to cyclohexanone, as a major product
with 72% selectivity using tert. butylhydroperoxide as oxidant and acetonitrile as solvent. The catalysts can be reused up
to three cycles without losing much of its activity. |
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