Catalytic dehydration of fructose into 5-hydroxymethylfurfural by microwave heating was studied in acetone-water mixtures in the presence of a cation exchange resin catalyst. The use of acetone-water reaction media resulted in yields of 5-HMF as high as 73.4% for 94% conversion at 150 • C. It was confirmed that there was no decrease of catalytic activity and selectivity for five reuses of the resin, which was in accordance with the elemental analysis results that showed that sulfonic acid groups attached on the resin were stable at the experimental conditions. A comparison between conventional sand bath heating and microwave heating revealed that the latter had a remarkable accelerating effect not only on fructose conversion, but also on 5-HMF yield. Under the conditions (5 ml of 2 wt% fructose solution, 0.1 g of resin, 150 • C and 10 min), fructose conversion and HMF yields by microwave heating (91.7% and 70.3%, respectively) were higher than those by sand bath heating (22.1% and 13.9% respectively). Therefore, the process that we developed in this study showed that high 5-HMF yields from fructose could be achieved under mild conditions.

No abstract

No abstract

Biorefinery which utilize lignocellulosic biomass as renewable energy source and sustainable carbon feedstock is a promising solution to alleviate the excessive dependence on depleting fossil resources and to address climate...

An efficient method for converting glucose into 5-hydroxymethylfurfural (5-HMF), in the presence of CrCl3 catalyst, is developed by using the ionic liquid 1-butyl-3-methyl imidazolium chloride as solvent. A 5-HMF yield of 71 % is achieved in 30 s for 96 % glucose conversion with microwave heating at 140 °C. The activation energy of glucose conversion is determined to be 114.6 kJ mol(-1), with a pre-exponential factor of 3.5 x 10(14) min(-1). Fructose, sucrose, cellobiose, and cellulose are studied and 5-HMF yields of 54 % are obtained for cellulose conversion at 150 °C during 10 min of reaction time. Recycling of the ionic liquid and CrCl3 is demonstrated with six cycles of use.

No abstract

Catalytic dehydration of D-fructose to 5-Hydroxymethylfurfural (5-HMF) in acetone/dimethyl sulfoxide solvent mixtures was studied in the presence of a strong acidic cation-exchange resin catalyst (DOWEX 50WX8-100) by microwave heating. The addition of acetone to the dimethyl sulfoxide (DMSO) solvent promoted the formation of 5-HMF from D-fructose. For a D-fructose conversion of 97.9%, the 5-HMF selectivity was 91.7% for a 20-min reaction time in 70:30 (w/w) acetone/DMSO solvent mixtures. Concentrations as high as 10 wt % D-fructose were studied, for which it was found that 5-HMF yields of 82.1% for a reaction time of 10 min could be obtained. The stability of the ion-exchange resin used as the catalyst was confirmed. Compared to pure DMSO solvent, the combination of low-boiling-point acetone with DMSO used as the reaction medium not only gives highly selective 5-HMF formation, but also improves the separation efficiency and reduces environmental risk.

Carbonaceous solid (CS) catalysts with --SO₃H, --COOH, and phenolic --OH groups were prepared by incomplete hydrothermal carbonization of cellulose followed by either sulfonation with H₂SO₄ to give carbonaceous sulfonated solid (CSS) material or by both chemical activation with KOH and sulfonation to give activated carbonaceous sulfonated solid (a-CSS) material. The obtained carbon products (CS, CSS, and a-CSS) were amorphous; the CSS material had a small surface area (<0.5 m² g⁻¹) and a high --SO₃H group concentration (0.953 mmol g⁻¹), whereas the a-CSS material had a large surface area (514 m²  g ⁻¹) and a low --SO₃H group concentration (0.172 mmol g⁻¹). The prepared materials were evaluated as catalysts for the dehydration of fructose to 5-hydroxymethylfurfural (5-HMF) in the ionic liquid 1-butyl-3-methylimidazolium chloride ([BMIM][Cl]). Remarkably high 5-HMF yields (83 %) could be obtained efficiently (80 °C and 10 min reaction time). CSS and a-CSS catalysts had similar catalytic activities and efficiencies for the conversion of fructose to 5-HMF in [BMIM][Cl]; this could be explained by the trade-off between --SO₃H group concentration (high for CSS) and surface area (high for a-CSS). The cellulose-derived catalysts and ionic liquid exhibited constant activity for five successive recycles, and thus, the methods developed provide a renewable strategy for biomass conversion.