Hydrothermal liquefaction is a promising technology for the conversion of a wide range of bio-feedstock into a biocrude; a mixture of chemical compounds that holds the potential for a renewable production of chemicals and fuels. Most research in hydrothermal liquefaction is performed in batch type reactors, although a continuous and energy-efficient operation is paramount for such process to be feasible. In this work an experimental campaign in a continuous bench scale unit is presented. The campaign is based on glycerol-assisted hydrothermal liquefaction of aspen wood carried out with the presence of a homogeneous catalyst at supercritical water conditions, 400 • C and 300 bar. Furthermore, in the experimental campaign a water phase recirculation step is incorporated to evaluate the technical feasibility of such procedure. In total, four batches of approximately 100 kg of feed each were processed successfully at steady state conditions without any observation of system malfunctioning. The biocrude obtained was characterized using several analytical methods to evaluate the feasibility of the process and the quality of the product. Results showed that a high quality biocrude was obtained having a higher heating value of 34.3 MJ/kg. The volatile fraction of the biocrude consisted mostly of compounds having number of carbon atoms in the C 6 -C 12 range similar to gasoline. In terms of process feasibility, it was revealed that total organic carbon (TOC) and ash significantly accumulated in the water phase when such is recirculated for the proceeding batch. After four batches the TOC and the ash mass fraction of the water phase were 136.2 [g/L] and 12.6 [%], respectively. Water phase recirculation showed a slight increase in the biocrude quality in terms on an effective hydrogen-to-carbon ratio, but it showed no effects on the product gas composition or the pH of the water phase. The successful operation demonstrated the technical feasibility of a continuous production of high quality biocrude.
Nanocrystalline ZrO(2) samples with narrow size distributions and mean particle sizes below 10 nm have been synthesized in a continuous flow reactor in near and supercritical water as well as supercritical isopropyl alcohol using a wide range of temperatures, pressures, concentrations and precursors. The samples were comprehensively characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), and small-angle X-ray scattering (SAXS), and the influence of the synthesis parameters on the particle size, particle size distribution, shape, aggregation and crystallinity was studied. On the basis of the choice of synthesis parameters either monoclinic or tetragonal zirconia phases can be obtained. The results suggest a critical particle size of 5-6 nm for nanocrystalline monoclinic ZrO(2) under the present conditions, which is smaller than estimates reported in the literature. Thus, very small monoclinic ZrO(2) particles can be obtained using a continuous flow reactor. This is an important result with respect to improvement of the catalytic properties of nanocrystalline ZrO(2).
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