Biofuels from lignin and novel biodiesel analysis

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Nagy, Máté
Ragauskas, Arthur J.
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The first part of the thesis presents a study based on the forest biorefinery concept, which involves converting a pulp mill into a multi-purpose biofuels, biomaterials, and biopower production facility in which these products are produced in an environmentally compatible and sustainable manner. A key challenge in this process is the recovery of lignin from process streams such that it can be utilized in a variety of innovative green chemistry processes The first study examines the fundamental chemical structure of LignoBoost derived lignin recovered from Kraft pulping streams using an acid precipitation/washing methodology. Functional group analysis and molecular weight profiles were determined by nuclear magnetic resonance (NMR) and size exclusion chromatography. These findings gave valuable insight into the physical properties and the determining chemical properties of this currently underutilized, renewable bioresource. The second study is based on the future second generation bioethanol production process, where ethanol produced from lignocellulosic materials will bring about the co-production of significant amounts of under-utilized lignin. The study examines the potential of conventional heterogeneous and novel homogeneous catalysts for the selective cleavage of the aryl-O-aryl and aryl-O-aliphatic linkages of ethanol organosolv lignin to convert it from a low grade fuel to potential fuel precursors or other value added chemicals. The experimental data demonstrated that aryl-O-aryl and aryl-O-aliphatic linkages could be cleaved and the hydrogenated lignin had a decrease in oxygen functionality and the formation of products with lower oxygen content. The second part of this thesis reports the development and optimization of a novel qualitative method for the determination of the various types of hydroxyl groups present in biodiesel production streams. In the first study, the use of 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane as a phosphitylation reagent for quantitative ³¹P-NMR analysis of the hydroxyl groups in biodiesel process samples has been developed. Subsequently a characteristic chemical shifts library is developed with model compounds to provide quantitative data on the concentration of biodiesel precursors, intermediates and final product. The last part of this thesis depicts the results of an industrial trial based on the novel biodiesel analytical method developed earlier.
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