Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction
A successive anchoring of Ti(NMe{sub 2}){sub 4}, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on silica was conducted by SOMC strategy in moderate conditions. The silica, monitored by in-situ Fourier transform infrared spectroscopy (in-situ FT-IR), was pretreated at different temperatures (200, 500 and 800 °C). The ligand tailored silica-supported titanium complexes were characterized by in-situ FT-IR, {sup 13}C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near edge structure (XANES) and elemental analysis in detail, verifying that the surface titanium species are single sited. The catalytic activity of the ligand tailored single-site silica supported titanium complexes was evaluated by a cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the dehydroxylation temperatures of silica and the configuration of the ligands. - Graphical abstract: The ligand-tailored silica supported “single site” titanium complexes were synthesized by SOMC strategy and fully characterized. Their catalytic activity were evaluated by benzaldehyde silylcyanation. - Highlights: • Single-site silica supported Ti active species was prepared by SOMC technique. • O-donor ligand tailored Ti surface species was synthesized. • The surface species was characterized by XPS, {sup 13}C CP-MAS NMR, XANES etc. • Catalytic activity of the Ti active species in silylcyanation reaction was evaluated.
- OSTI ID:
- 22443499
- Journal Information:
- Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Vol. 221; ISSN 0022-4596; ISSN JSSCBI
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ABSORPTION
ABSORPTION SPECTROSCOPY
BENZALDEHYDE
CATALYSTS
CYCLOPENTADIENE
FASTENING
FOURIER TRANSFORM SPECTROMETERS
FOURIER TRANSFORMATION
INFRARED SPECTRA
LIGANDS
NUCLEAR MAGNETIC RESONANCE
SILICA
SURFACES
SYNTHESIS
TITANIUM
TITANIUM COMPLEXES
X RADIATION
X-RAY PHOTOELECTRON SPECTROSCOPY
X-RAY SPECTROSCOPY