In this work, a series of nano-carbon based catalysts loaded with metal oxides were prepared via liquid phase deposition, and used for low temperature catalytic hydrolysis of carbon disulfide (CS₂). The influences of preparation conditions for catalytic activity were investigated. These factors included species and content of metal oxides, ratio of F : Fe, solution pH, and calcination temperature. The results showed that catalysts with 0.2 mol L⁻¹ Fe ion after calcining at 500 °C had good catalytic activity for the catalytic hydrolysis of CS₂. Furthermore, the catalytic hydrolysis activity could reach the best performance with the optimum preparation conditions with an F : Fe ratio of 3 : 1, and a solution pH of 5.1. The metal species affected the catalytic hydrolysis of CS₂ and the oxidation of H₂S. The solution pH and fluoride affected the generation of Fe³⁺ (Fe₂O₃). The chemical composition, structure and surface properties were characterized by X-ray diffractometry (XRD), temperature programmed desorption of carbon monoxide (CO-TPD), X-ray photoelectron spectrum (XPS) and Brunauer–Emmett–Teller measurements (BET). The XRD and BET results showed that the calcination temperature controlled the crystalline phase and generation of Fe₂O₃ and affected the properties of specific surface area and pore structure.