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.