Hydrothermal Synthesis of Carbon Microspheres from Lignocellulosic Bio-Oil

Biomass valorization into carbon-rich materials has attracted increasing attention as a sustainable alternative to fossil-based resources. This work is devoted to the study of hydrothermal carbonization (HTC) of spruce lignocellulose liquid pyrolysis products (the target product of the pyrolysis is levoglucosan)—bio-oil (B). In addition, the fractionated B compounds, including the phenol-enriched fraction remaining after anhydrosugar removal, were evaluated as potential precursors for hydrochar production. Hydrochars were produced at 200, 250, and 300 °C and characterized using SEM, revealing that spherical morphology agglomerates can also be obtained from the phenol-enriched fraction. The chemical composition and structural evolution of the hydrochars were investigated by Py-GC/MS, elemental analysis, and FTIR, demonstrating the significant influence of both precursor composition and carbonization temperature on hydrochar chemistry. In addition, the organic compounds in the process water were analyzed using UHPLC and complementary chemical analysis. The results show that the chemical composition of the precursor strongly influences the yield, morphology, and chemical composition of the obtained hydrochar.