Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts

The catalytic dehydration of fructose to 5-hydroxymethylfurfural (HMF) in water was performed in the presence of pristine Nb<sub>2</sub>O<sub>5</sub> and composites containing Nb and Ti, Ce or Zr oxides. In all experiments, fructose was converted to HMF using water as the sol...

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Main Authors: Elisa I. García-López, Francesca Rita Pomilla, Bartolomeo Megna, Maria Luisa Testa, Leonarda Francesca Liotta, Giuseppe Marcì
Format: Article
Language:English
Published: MDPI AG 2021-07-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/11/7/1821
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author Elisa I. García-López
Francesca Rita Pomilla
Bartolomeo Megna
Maria Luisa Testa
Leonarda Francesca Liotta
Giuseppe Marcì
author_facet Elisa I. García-López
Francesca Rita Pomilla
Bartolomeo Megna
Maria Luisa Testa
Leonarda Francesca Liotta
Giuseppe Marcì
author_sort Elisa I. García-López
collection DOAJ
description The catalytic dehydration of fructose to 5-hydroxymethylfurfural (HMF) in water was performed in the presence of pristine Nb<sub>2</sub>O<sub>5</sub> and composites containing Nb and Ti, Ce or Zr oxides. In all experiments, fructose was converted to HMF using water as the solvent. The catalysts were characterized by powder X-ray diffraction, scanning electron microscopy, N<sub>2</sub> physical adsorption, infrared and Raman spectroscopy and temperature-programmed desorption of NH<sub>3</sub>. Experimental parameters such as fructose initial concentration, volume of the reacting suspension, operation temperature, reaction time and amount of catalyst were tuned in order to optimize the catalytic reaction process. The highest selectivity to HMF was ca. 80% in the presence of 0.5 g·L<sup>−1</sup> of bare Nb<sub>2</sub>O<sub>5</sub>, Nb<sub>2</sub>O<sub>5</sub>-TiO<sub>2</sub> or Nb<sub>2</sub>O<sub>5</sub>-CeO<sub>2</sub> with a maximum fructose conversion of ca. 70%. However, the best compromise between high conversion and high selectivity was reached by using 1 g·L<sup>−1</sup> of pristine Nb<sub>2</sub>O<sub>5</sub>. Indeed, the best result was obtained in the presence of Nb<sub>2</sub>O<sub>5</sub>, with a fructose conversion of 76% and a selectivity to HMF of 75%, corresponding to the highest HMF yield (57%). This result was obtained at a temperature of 165° in an autoclave after three hours of reaction by using 6 mL of 1 M fructose suspension with a catalyst amount equal to 1 g·L<sup>−1</sup>.
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spelling doaj.art-4ec262726ff048b28d46fba6d64565192023-11-22T04:34:24ZengMDPI AGNanomaterials2079-49912021-07-01117182110.3390/nano11071821Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based CatalystsElisa I. García-López0Francesca Rita Pomilla1Bartolomeo Megna2Maria Luisa Testa3Leonarda Francesca Liotta4Giuseppe Marcì5Department of Biological, Chemical and Pharmaceutical Sciences and Technologies (STEBICEF), University of Palermo, Viale delle Scienze, 90128 Palermo, Italy“Schiavello-Grillone” Photocatalysis Group, Department of Engineering, University of Palermo, Viale delle Scienze, 90128 Palermo, Italy“Schiavello-Grillone” Photocatalysis Group, Department of Engineering, University of Palermo, Viale delle Scienze, 90128 Palermo, ItalyInstitute of Nanostructured Materials (ISMN)-CNR, Via Ugo La Malfa, 153, 90146 Palermo, ItalyInstitute of Nanostructured Materials (ISMN)-CNR, Via Ugo La Malfa, 153, 90146 Palermo, Italy“Schiavello-Grillone” Photocatalysis Group, Department of Engineering, University of Palermo, Viale delle Scienze, 90128 Palermo, ItalyThe catalytic dehydration of fructose to 5-hydroxymethylfurfural (HMF) in water was performed in the presence of pristine Nb<sub>2</sub>O<sub>5</sub> and composites containing Nb and Ti, Ce or Zr oxides. In all experiments, fructose was converted to HMF using water as the solvent. The catalysts were characterized by powder X-ray diffraction, scanning electron microscopy, N<sub>2</sub> physical adsorption, infrared and Raman spectroscopy and temperature-programmed desorption of NH<sub>3</sub>. Experimental parameters such as fructose initial concentration, volume of the reacting suspension, operation temperature, reaction time and amount of catalyst were tuned in order to optimize the catalytic reaction process. The highest selectivity to HMF was ca. 80% in the presence of 0.5 g·L<sup>−1</sup> of bare Nb<sub>2</sub>O<sub>5</sub>, Nb<sub>2</sub>O<sub>5</sub>-TiO<sub>2</sub> or Nb<sub>2</sub>O<sub>5</sub>-CeO<sub>2</sub> with a maximum fructose conversion of ca. 70%. However, the best compromise between high conversion and high selectivity was reached by using 1 g·L<sup>−1</sup> of pristine Nb<sub>2</sub>O<sub>5</sub>. Indeed, the best result was obtained in the presence of Nb<sub>2</sub>O<sub>5</sub>, with a fructose conversion of 76% and a selectivity to HMF of 75%, corresponding to the highest HMF yield (57%). This result was obtained at a temperature of 165° in an autoclave after three hours of reaction by using 6 mL of 1 M fructose suspension with a catalyst amount equal to 1 g·L<sup>−1</sup>.https://www.mdpi.com/2079-4991/11/7/1821biomass valorization5-HMFheterogeneous acid catalysisniobium oxidetitanium oxidegreen chemistry
spellingShingle Elisa I. García-López
Francesca Rita Pomilla
Bartolomeo Megna
Maria Luisa Testa
Leonarda Francesca Liotta
Giuseppe Marcì
Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts
Nanomaterials
biomass valorization
5-HMF
heterogeneous acid catalysis
niobium oxide
titanium oxide
green chemistry
title Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts
title_full Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts
title_fullStr Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts
title_full_unstemmed Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts
title_short Catalytic Dehydration of Fructose to 5-Hydroxymethylfurfural in Aqueous Medium over Nb<sub>2</sub>O<sub>5</sub>-Based Catalysts
title_sort catalytic dehydration of fructose to 5 hydroxymethylfurfural in aqueous medium over nb sub 2 sub o sub 5 sub based catalysts
topic biomass valorization
5-HMF
heterogeneous acid catalysis
niobium oxide
titanium oxide
green chemistry
url https://www.mdpi.com/2079-4991/11/7/1821
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