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

V. Calvino-Casilda, Guido Mul, J.F. Fernandez, F. Rubio-Marcos, M.A. Banares

Research output: Contribution to journalArticleAcademicpeer-review

28 Citations (Scopus)

Abstract

In situ Attenuated Total Reflectance FTIR spectroscopy was used to study the carbonylation of glycerol with urea. Cobalt oxide nanoparticles, Co3O4, 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 reaction of glycerol with urea reveals differences in reactivity of various Co3O4/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, possible 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.
Original languageEnglish
Pages (from-to)106-112
Number of pages7
JournalApplied catalysis A: general
Volume409-410
DOIs
Publication statusPublished - 2011

Fingerprint

Carbonates
Glycerol
Spectroscopy
Monitoring
Urea
Carbonylation
Catalysts
Zinc Oxide
Urethane
Zinc oxide
Reaction kinetics
Cobalt
Nanoparticles
Oxides

Keywords

  • METIS-280558
  • IR-95294

Cite this

Calvino-Casilda, V. ; Mul, Guido ; Fernandez, J.F. ; Rubio-Marcos, F. ; Banares, M.A. / Monitoring the catalytic synthesis of glycerol carbonate by real-time attenuated total reflection FTIR spectroscopy. In: Applied catalysis A: general. 2011 ; Vol. 409-410. pp. 106-112.
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Monitoring the catalytic synthesis of glycerol carbonate by real-time attenuated total reflection FTIR spectroscopy. / Calvino-Casilda, V.; Mul, Guido; Fernandez, J.F.; Rubio-Marcos, F.; Banares, M.A.

In: Applied catalysis A: general, Vol. 409-410, 2011, p. 106-112.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - Monitoring the catalytic synthesis of glycerol carbonate by real-time attenuated total reflection FTIR spectroscopy

AU - Calvino-Casilda, V.

AU - Mul, Guido

AU - Fernandez, J.F.

AU - Rubio-Marcos, F.

AU - Banares, M.A.

PY - 2011

Y1 - 2011

N2 - In situ Attenuated Total Reflectance FTIR spectroscopy was used to study the carbonylation of glycerol with urea. Cobalt oxide nanoparticles, Co3O4, 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 reaction of glycerol with urea reveals differences in reactivity of various Co3O4/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, possible 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.

AB - In situ Attenuated Total Reflectance FTIR spectroscopy was used to study the carbonylation of glycerol with urea. Cobalt oxide nanoparticles, Co3O4, 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 reaction of glycerol with urea reveals differences in reactivity of various Co3O4/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, possible 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.

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KW - IR-95294

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M3 - Article

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JO - Applied catalysis A: general

JF - Applied catalysis A: general

SN - 0926-860X

ER -