Microwave-assisted liquefaction of carbohydrates for 5-hydroxymethylfurfural using tungstophosphoric acid encapsulated dendritic fibrous mesoporous silica as a catalyst.

Abstract Tungstophosphoric acid (TPA) encapsulated dendritic fibrous silica KCC-1 was prepared via a microemulsion system with the simple reflux method using cetyltrimethylammonium bromide as a structure-directing agent. The TPA impregnated on KCC-1 (ITPA-KCC-1) was also prepared for comparative. Various physicochemical techniques were used to characterize the synthesized materials and their activity evaluated in the 5-hydroxymethylfurfural (HMF) formation from carbohydrates derivatives of fructose, glucose and cellulose. The effect of various factors such as catalyst to substrate ratio, different solvents and temperature were investigated on the formation of HMF. The resultant encapsulated catalyst was very active in fructose dehydration with the yield of 92% HMF and full conversion of fructose at 120 °C for 30 min under the microwave heating condition without any salt additive in the THF solvent system as well as 95% in MIBK solvent. The HMF yield was achieved by 58% and 16.2% from glucose and cellulose in the DMSO solvent, respectively. The TPA-KCC-1 can be separated easily after reaction from the reaction mixture and reused atleast five times without substantial loss in catalytic activity. This study provides an easy encapsulation method for TPA in dendritic fibrous silica KCC-1 as a heterogeneous catalyst, and it should have great application potential in other biomass valorization processes.