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HYDROTHERMAL PRETREATMENT OF BIOMASS SAMPLES FOR PRODUCING ENERGY EFFICIENT HYDROGEN ELECTROCHEMICALLY In this thesis, electrochemical production of hydrogen (H2) gas using two biomass materials, namely microcrystalline cellulose and wood sawdust, has been investigated. Since as obtained samples did not show meaningful activity in hydrogen production, these samples were subjected to hydrothermal pretreatment (HTP) in an autoclave using water as solvent at 200 o C and up to 500 psi pressure. The HTP samples produced activity as high as that of high surface area activated carbon (BP2000) for producing H2 at energy efficient voltages. To understand the changes produced by HTP, structural properties of the parent as well as the HTP samples were determined using x-ray diffraction (XRD), scanning electron microscopy (SEM), and Thermo-gravimetric analysis (TGA). From the x-ray diffraction patterns of the parent and the HTP crystalline cellulose and wood sawdust, the parent samples show the crystalline peaks of cellulose whereas all these Bragg peaks were missing in the HTP samples. Instead only a broad peak is observed suggesting loss of crystallinity in the HTP samples. Results from SEM micrograph of the micro-crystalline cellulose show that the particle size of the parent cellulose are about 12 x 6 μm but after HTP, the particle size is reduced by a factor of 50 to yield particles about 210nm. This reduction in size accompanied by complete less of cellulose crystallinity is the likely reason for the observed high activity of the HTP cellulose to produce H2 electrochemically.

Hydrothermal pretreatment of biomass samples for producing energy efficient hydrogen electrochemically