Nitrogen‐functionalized active carbons were prepared by post‐treatment method and used as supports for loading nickel to prepare liquid‐phase hydrogenation catalysts. The post‐treatment conditions were investigated, and these nitrogen‐functionalized active carbons supported nickel catalysts were characterized and used in the nitro naphthalene compounds hydrogenation. The characterization results show that the nitrogen‐functionalized active carbon prepared at 800 oC (N‐AC‐800) shows higher nitrogen content and pyridinic nitrogen species. And its supported nickel catalyst (Ni/N‐AC‐800) shows the most finely and extremely dispersion of nickel nanoparticles, the highest content of Ni0, and the largest metallic surface areas and the best H2 uptake quantity. Moreover, Ni/N‐AC‐800 also shows the best catalytic performance in nitro compounds hydrogenation reaction. The yield of 1,5‐diaminonaphthalene reaches to 94.75%, and the catalyst could be recycled for four times and maintained stable catalytic performance. Ni/N‐AC‐800 also shows good catalytic performance in 1‐nitronaphthalene and 1,8‐dinitronaphthalene hydrogenation.

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