In situ UV–VIS spectrophotometry within the second time scale as a research tool for solid-state catalyst and liquid-phase reactions at high temperatures: Its application to the formation of HMF from glucose and cellulose

Abstract

We successfully developed an in situ UV–VIS absorption spectroscopic flow reactor system for investigation of solid-liquid two-phase reactions within the second time scale at high temperatures (solid-state-catalyst-mediated hydrothermal flow reactor system, SSCM-HF). The SSCM-HF consisted of a water reservoir, high-pressure pump, sample injector, high-temperature reactor involving solid-state catalysts, a cooling bath, a pressure regulator, and a temperature controller. The high-temperature reactor contains a reactor column having micrometer sized solid particles, and is connected to an optical window using transparent fused-silica capillary tubing. Liquid samples are exposed for the second time scale, which can be adjusted by changing the flow rate. In situ monitoring of reactions using SSCM-HF was performed at 200–1114nm within 7.36–117.79s at temperatures up to 300°C and pressures up to 30MPa. We demonstrated the usefulness of SSCM-HF by inspecting 5′-hydroxymethylfurfural (HMF) formation from glucose and cellulose. The influence of metal oxides, such as WO3 and Nb2O5, was investigated using both a conventional batch reactor and the SSCM-HF. The simple metal oxides showed catalytic activities for the dehydration of glucose to HMF. The SSCM-HF demonstrated in situ detection of a small amount of HMF in the presence of WO3 deposited solid particles within 29.4s at 200°C. This study demonstrates the application of the SSCM-HF as a new research tool for screening and investigating solid-state catalysts in detail in liquid-phase reactions at high temperatures.