Abstract Hydrodeoxygenation (HDO) of lignocellulosic derivatives to bio‐aviation fuel remains challenging due to the demand for precise control over metal–acid bifunctionality. Herein, we report a hierarchical Ni/HZSM‐5 catalyst (Ni/HZ5‐0.4‐EG) engineered via ethylene glycol‐assisted impregnation, which achieves spatial confinement of highly dispersed Ni nanoparticles within mesopores. This unique architecture establishes proximity between metallic Ni and acid sites, enabling efficient cascade conversion of biomass derivatives into C 8 C 16 alkanes. The catalyst delivers 73.2% alkane yield with an iso/ n ratio of 3.6, and the product exhibits low freezing point (≤60°C) and favorable density (0.79 g mL −1 ), meeting key specifications for bio‐aviation fuel. Characterizations reveal that the mesoporous confinement and metal‐support interactions synergistically stabilize Ni nanoparticles against sintering and coke formation, endowing the catalyst with robust durability over five consecutive cycles. This work demonstrates a strategy for designing metal–acid catalysts with tailored nanoscale architectures and provides mechanistic insights into active site modulation for complex HDO reactions.
Lu et al. (Fri,) studied this question.