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Received November 12, 2015
Accepted January 25, 2016
articles This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/bync/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.
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HMF synthesis in aqueous and organic media under ultrasonication, microwave irradiation and conventional heating

Biomass Conversion Science and Technology (BCST) Division, Iran Polymer and Petrochemical Institute, P. O. Box 14965-115, Tehran, Iran 1Department of Chemistry, Karaj Branch, Islamic Azad University, Karaj, Iran
Korean Journal of Chemical Engineering, June 2016, 33(6), 1964-1970(7), 10.1007/s11814-016-0031-8
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Abstract

5-Hydroxymethyl furfural (HMF) is known as a noteworthy platform in a biorefinery concept. HMF was prepared via fructose dehydration in aqueous and organic media, using three methods, i.e., conventional heating, ultrasonication and microwave irradiation. Water, methyl isobutyl ketone (MIBK), methyl ethyl ketone and ethyl acetate were used as media for HCl-catalyzed synthesis of HMF. FTIR and 1H-NMR spectroscopies were used for analysis. The synthesis yield and selectivity were investigated to optimize variables such as fructose concentration, catalyst dosage, temperature, irradiation power, solvent, and the reaction atmosphere. It was found that the yield in the organic media was superior to that of the aqueous ones. In addition, nitrogen atmosphere favored higher yield than air, due to lack of HMF oxidation. As conclusion, the highest yields of the conventional, ultrasonicated and microwave-assisted reactions were 87, 53, and 38%, respectively. In the reactions ultrasonically promoted, the reaction time scale was highly reduced from hours to minutes. The yield was varied with treatment times, so that ultrasonication was recognized to be the best approach in terms of yield, while the microwave method was the fastest one. Selectivity varied from 60 to 90% depending the reaction media and promotion method.

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