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Introduction: After cellulose, lignin represents the most abundant biopolymer on earth that accounts for up to 18-35 % by weight of lignocellulose biomass. Today, it is a by-product of the paper and pulping industry. Although lignin is available in huge amounts, mainly in form of so called black liquor produced via Kraft-pulping, processes for the valorization of lignin are still limited [1]. Due to its hyperbranched polyphenol-like structure, lignin gained increasing interest as biobased building block for polymer synthesis [2]. The present work is focused on extraction and purification of lignin from industrial black liquor and synthesis of lignin-based polyurethanes.
Ultra-fast photopolymerization of experimental composites: DEA and FT-NIRS measurement comparison
(2015)
In this doctoral thesis the curing process of visible light-curing (VLC) dental composites and 3D printing rapid prototyping (RP) materials are investigated with the focus on dielectric analysis (DEA). This method is able to monitor the curing of resins in an alternating electric fringe field with adjustable frequencies and is often used for cure control of composites manufacturing in the aviation and automotive industry but hardly established in dental science or RP method development. It is capable of investigating very fast initiation and primary curing processes using high frequencies in the kHz-range. The aim of the Thesis is a better understanding of the curing processes with respect to curing parameters such as resin composition, viscosity, temperature, and for light-curing composites also light intensity and irradiation depth. Due to the nature of both dental and RP systems an application of specific experimental set-up had to be designed allowing for the generation of reproducible and valid results. Subsequently, different evaluation methods were developed to characterize the curing behavior of both material types. A special focus was paid to the determination of kinetic parameters from DEA measurements. Reaction rates of the curing of the corresponding thermosets were calculated and applied to the ion viscosity curves measured by DEA to evaluate reaction kinetic parameters. For the dental composites it could be clearly shown that the initial curing rate is directly proportional to light intensity and not to its square root as proposed by many others authors. A good description of the curing behaviour of 3DP RP materials was also achieved assuming a reaction order smaller than one. This data provides the base for the kinetic modeling of polymerization and curing processes proposed within the Thesis.