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Title: Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction

Abstract

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 activitymore » of the Ti active species in silylcyanation reaction was evaluated.« less

Authors:
; ; ; ; ; ; ;
Publication Date:
OSTI Identifier:
22443499
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 221; Other Information: Copyright (c) 2014 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 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

Citation Formats

Xu, Wei, Li, Yani, Yu, Bo, Yang, Jindou, Zhang, Ying, Chen, Xi, Zhang, Guofang, E-mail: gfzhang@snnu.edu.cn, and Gao, Ziwei, E-mail: zwgao@snnu.edu.cn. Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction. United States: N. p., 2015. Web. doi:10.1016/J.JSSC.2014.10.011.
Xu, Wei, Li, Yani, Yu, Bo, Yang, Jindou, Zhang, Ying, Chen, Xi, Zhang, Guofang, E-mail: gfzhang@snnu.edu.cn, & Gao, Ziwei, E-mail: zwgao@snnu.edu.cn. Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction. United States. doi:10.1016/J.JSSC.2014.10.011.
Xu, Wei, Li, Yani, Yu, Bo, Yang, Jindou, Zhang, Ying, Chen, Xi, Zhang, Guofang, E-mail: gfzhang@snnu.edu.cn, and Gao, Ziwei, E-mail: zwgao@snnu.edu.cn. Thu . "Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction". United States. doi:10.1016/J.JSSC.2014.10.011.
@article{osti_22443499,
title = {Ligand-tailored single-site silica supported titanium catalysts: Synthesis, characterization and towards cyanosilylation reaction},
author = {Xu, Wei and Li, Yani and Yu, Bo and Yang, Jindou and Zhang, Ying and Chen, Xi and Zhang, Guofang, E-mail: gfzhang@snnu.edu.cn and Gao, Ziwei, E-mail: zwgao@snnu.edu.cn},
abstractNote = {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.},
doi = {10.1016/J.JSSC.2014.10.011},
journal = {Journal of Solid State Chemistry},
number = ,
volume = 221,
place = {United States},
year = {Thu Jan 15 00:00:00 EST 2015},
month = {Thu Jan 15 00:00:00 EST 2015}
}