Abstract: Mesoporous carbon supported Ni-Mo hydrodesulfurization (HDS) catalysts have been successfully prepared with Anderson polyoxometalate (NH₄)₄NiMo₆O₂₄ H₆·5H₂O, thiourea, citric acid, and sodium chloride to evaluate the HDS performance with dibenzothiophene. The catalysts were prepared by one-step vacuum freeze-drying, followed by calcination under nitrogen and washing off the template, and then structurally characterized via many devices, including XRD, Raman, low temperature N₂ adsorption-desorption isotherm, SEM, HRTEM, XPS, and TPR. The results show these catalysts possess weaker metal-support interaction, shorter MoS₂ particles (4.9 nm) and appropriate stacking number (4.8), and higher percent of NiMoS active phase. The dibenzothiophene conversion, overall pseudo-first order rate constant and the turnover frequency can reach 94.1%, 1.7 × 10^–6 mol/(g·s) and 2.8 × 10^–3 s^–1, respectively. By using in-situ formed NaCl and H₂S as hard template and sulfidizing agent respectively, this methodology opens a new avenue for the simple and environmental friendly fabrication of HDS catalysts via the synchronization and riveting of mesoporous carbon support and MoS₂ particles.