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PMo or PW heteropoly acids supported on MCM-41 silica nanoparticles: Characterisation and FT-IR study of the adsorption of 2-butanol

AutorCarriazo, Daniel ; Domingo, Concepción ; Martín, Cristina; Rives, Vicente
Palabras claveHetero-polyoxometalates
Decomposition of 2-butanol
FT-IR spectroscopy
Fecha de publicación10-may-2008
CitaciónJournal of Solid State Chemistry 181(8): 2046-2057 (2008)
ResumenMesoporous silica, prepared in basic conditions, has been loaded (20% weight) with 12-molybdophosphoric (PMo) or 12-tungstophosphoric (PW) acid and calcined at different temperatures ranging between 250 and 550°C. The samples have been characterised by N2 adsorption–desorption at −196°C, transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), UV–visible diffuse reflectance, Raman spectroscopy and temperature programmed reduction (TPR). The acidity and catalytic activity have been, respectively, examined by monitoring the adsorption of pyridine and 2-butanol by FT-IR spectroscopy. The results indicate that PW and PMo acids are highly dispersed on mesoporous silica MCM-41 spherical nanoparticles. While PMo retains its Keggin structure up to 550°C, PW decomposes at this temperature into crystalline WO3 and phosphorous oxides. In both cases, the morphology, hexagonal symmetry and long-range order observed for the support are preserved with calcination up to 450°C. The Brönsted-type acid sites found in all samples, whose surface concentration decreases as the calcination temperature increases, are responsible for the selective formation of cis-butene detected upon adsorption of 2-butanol. The sample containing PW calcined at 450°C also shows selectivity to methyl ethyl ketone.
Descripción12 pages, 13 figures.-- Printed version published on Aug 2008.
Versión del editorhttp://dx.doi.org/10.1016/j.jssc.2008.05.004
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