2018
DOI: 10.1039/c8ra02419g
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SOMC grafting of vanadium oxytriisopropoxide (VO(OiPr)3) on dehydroxylated silica; analysis of surface complexes and thermal restructuring mechanism

Abstract: VO(OiPr)3 was grafted on highly dehydroxylated silica by a surface organometallic chemistry approach and its thermal evolution was analyzed with support of DFT calculations.

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Cited by 11 publications
(12 citation statements)
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“…The isotropic shift position, linewidth, and C Q values for peak 2 in the V+ i PrOH/SiO 2(700) and V+ i PrOH/TMS‐SiO 2(700) spectra are all consistent with a monopodal 51 V site with a weak fifth coordination to a nearby Si−O− i Pr group (Figure , inset), as we have suggested previously . Other groups using different synthesis procedures have proposed a bipodal vanadium site with two surface bonds, however C Q values were not reported for these species …”
Section: Resultssupporting
confidence: 70%
“…The isotropic shift position, linewidth, and C Q values for peak 2 in the V+ i PrOH/SiO 2(700) and V+ i PrOH/TMS‐SiO 2(700) spectra are all consistent with a monopodal 51 V site with a weak fifth coordination to a nearby Si−O− i Pr group (Figure , inset), as we have suggested previously . Other groups using different synthesis procedures have proposed a bipodal vanadium site with two surface bonds, however C Q values were not reported for these species …”
Section: Resultssupporting
confidence: 70%
“…A 1 H NMR spectrum acquired on a 700 MHz spectrometer using a 1.3 mm rotor and a spinning rate of 50 kHz (Figure A) shows detailed features that were not observed in previous studies , due to the poorer resolution resulting from the use of typical, albeit low, rotor spinning rates (ca. 10 kHz) .…”
mentioning
confidence: 68%
“…Here we present the use of multidimensional 1 H-detected solid-state NMR (ssNMR) experiments at high spinning rates in conjunction with computational studies to identify surface sites using supported vanadium compounds prepared via surface organometallic chemistry as a prototypical example because they are an important precursor to model supported vanadium oxide catalysts used in a broad range of applications and because their structure is still debated in the literature. , In this work, we demonstrate how proton-detected ssNMR spectroscopy enables acquiring high-quality NMR spectra for low-abundant (<1%) surface species without the need for labeling. As a showcase example, we will focus on elucidating the local environment of grafted vanadium species. , …”
mentioning
confidence: 99%
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“…Different methods for preparation are known in the literature, yielding catalysts with varying properties and distribution of VO x species. The most prominent ones are wet and incipient wetness impregnation [8,9] and ion exchange [10,11] of vanadium salts, grafting of molecular precursors [12][13][14] and direct preparation via in situ methods during silica synthesis. The latter was applied for different kinds of V-SiO 2 materials as the successful synthesis of V-SBA-15 [5,6,[15][16][17], V-SBA-3 [18], V-MCM-41 [5,19,20], V-MCM-48 [21] or V-MCF [22] catalysts for different catalytic applications demonstrates.…”
Section: Introductionmentioning
confidence: 99%