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PublicationApplied Catalysis A: General
Year2011
Volume409-410
Pages106–112
International

Monitoring the catalytic synthesis of glycerol carbonate by real-time attenuated total reflection FTIR spectroscopy

Authors:Vanesa Calvino Casilda, José Francisco Fernández , Fernando Rubio-Marcos , Miguel A. Bañares
Groups of research:Spectroscopy and industrial catalysis

n situ Attenuated Total Reflectance FTIR spectroscopy was used to study the carbonylation of glycerol with urea. Cobalt oxide nanoparticles, Co3 O4 , hierarchically dispersed on zinc oxide microparticles, ZnO, were used as catalysts. The present work demonstrates that in situ real-time attenuated total reflection ATR-FTIR spectroscopy is a valuable tool for monitoring reaction progress and analyzing the reaction mechanism of the synthesis of glycerol carbonate. ATR-FTIR spectroscopy during the carbonylation reac- tion of glycerol with urea reveals differences in reactivity of various Co3 O4 /ZnO catalysts, and in particular demonstrates that the first (fast) step in the conversion of glycerol with urea is the formation of glycerol urethane, whereas the consecutive conversion to glycerol carbonate is relatively slow. In addition, pos- sible interactions of the catalytically active sites with in particular the product glycerol carbonate were also evaluated. Interactions of the 2-hydroxyethyl chain of the product with the surface of the catalysts were identified, suggesting product inhibition might be of relevance to the reaction kinetics.

Keywords:Glycerol, Urea, Glycerol carbonate, Biomass, ATR-FTIR, spectroscopy
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