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[Display omitted] • Ni 2 P/Al 2 O 3 with small nanoparticles and pure phase was controllably synthesized. • Ni 2 P/Al 2 O 3 shows excellent hydrogenation and desulfurization activities. • Nanoflower-like structure improves dispersion and accessibility of active sites. • The outstanding performance can be attributed to the rich Niδ+ active sites. The hydrogenation of unsaturated bonds and elimination of sulfur impurities in C 9 petroleum resin (C 9 PR) are crucial for improving its quality and performance. In this study, we prepared a nanoflower-like Ni 2 P/Al 2 O 3 catalyst using an in-situ synthesis combined with liquid-phase phosphidation strategy and applied for the production of value-added hydrogenated C 9 PR. In-situ synthesis of Ni-Al hydrotalcite anchors and disperses Ni nanoparticles, while liquid-phase phosphidation introduces high-content Niδ+ and Pδ− active sites and prevents the formation of inactive AlPO 4 , synergistically enhancing both hydrogenation and desulfurization activities. The synthesized Ni 2 P/Al 2 O 3 catalyst achieves a 99.6 % hydrogenation degree and reduces sulfur content from 137 ppm to 0 ppm, much better than the catalysts prepared by conventional impregnation and metal phosphate reduction methods. These results give valuable insights for designing efficient catalysts and advancing single-step hydrorefining processes to generate high-quality, value-added hydrogenated petroleum resins. [ABSTRACT FROM AUTHOR]

[Display omitted] • The flower-like nickel phosphide catalysts were prepared by a hydrotalcite strategy. • Ni 2 P/Al 2 O 3 catalyst showed excellent catalytic activity and desulfurization ability. • The outstanding performance ascribed to the rich active Niδ+ species. • The enhanced stability was due to strong interaction between active sites and support. The catalytic hydrogenation of petroleum resin (PR) to high value-added hydrogenated PR (HPR) represents a forward-looking technology for upgrading the pyrolysis petroleum by-product. Herein, flower-like and pure-phase supported nickel phosphide catalysts were controllably fabricated through a hydrotalcite strategy with red phosphorous as the P source. The PR hydrogenation activity of the catalysts followed the order of Ni 2 P/Al 2 O 3 > NiP 2 /Al 2 O 3 > Ni/Al 2 O 3 > imp-Ni 2 P/Al 2 O 3 catalysts (prepared by the impregnation method). Such enhanced performance of Ni 2 P/Al 2 O 3 could be ascribed to small nickel phosphide particle size and rich active Niδ+ species. Notably, the sulfur contents of PR were effectively reduced from 55.4 (C 5 PR) and 72.3 ppm (C 9 PR) to 3.8 and 7.9 ppm after hydrogenation by Ni 2 P/Al 2 O 3. Meanwhile, Ni 2 P/Al 2 O 3 also exhibited good stability with the hydrogenation degree of HC 5 PR maintaining at 94.39 % after 100 h. Our work provides a promising nickel phosphide catalyst with outstanding hydrogenation activity, hydrodesulfurization ability, and stability toward PR hydrogenation. [ABSTRACT FROM AUTHOR]