One-step nonhydrolytic sol-gel synthesis of mesoporous TiO2 phosphonate hybrid materials

Beilstein Journal of Nanotechnology
Yanhui WangJohan G Alauzun

Abstract

Mesoporous TiO2-octylphosphonate hybrid materials were prepared in one step by a nonhydrolytic sol-gel method involving the reaction of Ti(OiPr)4, acetophenone (2 equiv) and diethyl octylphosphonate (from 0 to 0.2 equiv) at 200 °C for 12 hours, in toluene. The different samples were characterized by 31P magic angle spinning nuclear magnetic resonance, Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, and nitrogen physisorption. For P/Ti ratios up to 0.1, the hybrid materials can be described as aggregated, roughly spherical, crystalline anatase nanoparticles grafted by octylphosphonate groups via Ti-O-P bonds. The crystallite size decreases with the P/Ti ratio, leading to an increase of the specific surface area and a decrease of the pore size of the hybrid samples. For a P/Ti ratio of 0.2, the volume fraction of organic octyl groups exceeds 50%. The hybrid material becomes nonporous and can be described as amorphous TiO2 clusters modified by octylphosphonate units, where the octyl chains form an organic continuous matrix.

References

Jan 13, 2005·Chemical Communications : Chem Comm·Georg GarnweitnerMarkus Niederberger
May 6, 2006·Angewandte Chemie·Frank HoffmannMichael Fröba
Jun 19, 2008·Angewandte Chemie·Nicola Pinna, Markus Niederberger
Jan 14, 2011·Chemical Society Reviews·Clément SanchezSusumu Kitagawa
Apr 26, 2012·Chemical Reviews·Clémence QueffélecBruno Bujoli
Jul 28, 2013·Dalton Transactions : an International Journal of Inorganic Chemistry·Gilles GuerreroP Hubert Mutin

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Citations

Jan 11, 2020·Beilstein Journal of Nanotechnology·Andreas TaubertVerónica de Zea Bermudez

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Methods Mentioned

BETA
X-ray
nuclear magnetic resonance
NMR

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