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Catalytic dehydration of fructose to 5-hydroxymethylfurfural over Nb2O5 catalyst in organic solvent.

Carbohydrate research (2013-01-26)
Fenfen Wang, Hai-Zhen Wu, Chun-Ling Liu, Rong-Zhen Yang, Wen-Sheng Dong
ABSTRACT

The catalytic dehydration of fructose to 5-hydroxymethylfurfural (HMF) in DMSO was performed over Nb2O5 derived from calcination of niobic acid at various temperatures (300-700 °C). The catalysts were characterized by powder X-ray diffraction, N2 physical adsorption, temperature-programed desorption of NH3, n-butylamine titration using Hammett indicators, infrared spectroscopy of adsorbed pyridine, and X-ray photoelectron spectroscopy. It was found that both catalytic activity and surface acid sites decrease with increasing calcination temperatures. The Nb2O5 derived from calcination of niobic acid at 400 °C reveals the maximum yield of HMF among all the catalysts, although the amount of acid sites on the catalyst is lower than that on the sample calcined at 300 °C. The results suggest that the presence of larger amounts of strong acid sites on the surface of the Nb2O5 calcined at 300 °C may promote side reactions. The Nb2O5 prepared at 400 °C shows 100% fructose conversion with 86.2% HMF yield in DMSO at 120 °C after 2 h. The activity of the catalyst decreases gradually during recycle because of coke deposition; however, it can be fully recovered by calcination at 400 °C for 2 h, suggesting that this catalyst is of significance for practical applications.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Furfural, 99%
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5-(Hydroxymethyl)furfural, ≥99%, FG
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5-Hydroxymethyl-2-furaldehyde, 99%
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Niobium(V) oxide, 99.99% trace metals basis
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Furfural, ≥98%, FCC, FG
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Niobium(V) oxide, −325 mesh, 99.9% trace metals basis
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Furfural, natural, ≥98%, FCC, FG
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Furfural, ACS reagent, 99%
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Niobium, powder, <45 μm, 99.8% trace metals basis
Sigma-Aldrich
Niobium, foil, thickness 0.25 mm, 99.8% trace metals basis
Niobium, IRMM®, certified reference material, 0.02 mm foil
Niobium, IRMM®, certified reference material, 0.5 mm wire
Niobium, IRMM®, certified reference material, 0.02 mm foil
Niobium, IRMM®, certified reference material, 0.5 mm wire
Niobium, IRMM®, certified reference material, 0.1 mm foil