Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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Titanium Containing Solid Core Mesoporous Silica Shell: A Novel Efficient Catalyst for Ammoxidation Reactions

  • Venkatathri, N. (Department of Chemistry, National Institute of Technology Warangal) ;
  • Nookaraju, M. (Department of Chemistry, National Institute of Technology Warangal) ;
  • Rajini, A. (Department of Chemistry, National Institute of Technology Warangal) ;
  • Reddy, I.A.K. (Department of Chemistry, National Institute of Technology Warangal)
  • Received : 2012.07.23
  • Accepted : 2012.10.22
  • Published : 2013.01.20
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Abstract

Novel titanium containing solid core mesoporous shell silica has been synthesized by using octadecyltrichloro silane and triethylamine. The synthesized material was characterized by various physicochemical techniques. The mesoporous character of the material has been revealed from PXRD studies. The presence of octadecyltrichloro silane and triethylamine in the sample has been confirmed from EDAX studies. TG/DTA analysis reveals the thermal characteristics of the synthesized material. The presence of titanium in the frame work and its coordination state has been studies by UV-vis DR studies and XPS analysis. Chemical environment of Si in the framework of the material has been studied by $^{29}SiMASNMR$ studies. The surface area of the material is found to be around $550\;m^2g^{-1}$ and pore radius is of nano range from BET analysis. The spherical morphology and particle size of the core as well as shell has been found to be 300 nm and 50 nm respectively from TEM analysis. The catalytic application of this material towards the synthesis of caprolactam from cyclohexanone in presence of hydrogen peroxide through ammoxidation reaction has been investigated. The optimum conditions for the reaction have been established. The plausible mechanism for the formation of core silica and conversion of cyclohexanone has been proposed.

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