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The deoxygenation of triglycerides via hydrotreating is a promising route for producing hydrocarbon fuels from renewable biomass. Because triglycerides are bulky esters possessing multiple C=C bonds, mass transfer limitation and coke deposition within the pore space of catalysts are significant problems. In this study, the catalytic effects of porous structure and surface acidity of Pt/Al₂O₃ were rigorously investigated in triglyceride deoxygenation. Pt was supported on a series of Al₂O₃ materials with various crystal structures (γ, θ, and α), pore sizes (3.3–28.6 nm), and Lewis acid amounts (0–337 µmol g⁻¹), which were prepared by sol–gel synthesis. The γ- and θ-Al₂O₃ phases containing appreciable pentacoordinated Al sites effectively stabilized highly dispersed Pt particles (1.3–1.5 nm) via strong metal-support interactions and exhibited high catalytic activities. Conversely, Pt on α-Al₂O₃ without pentacoordinated …