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Spent carbon cathode (SCC) as a hazardous solid waste produced in aluminum electrolysis industry, contains plenty valuable components but generate a seriously threat to the environment. This paper focus on a closed-circuit cycle process for direct treatment of SCC based on the hydrothermal acid-leaching method. Thermodynamic calculation, single factor experiment, orthogonal experiment and kinetic study are utilized to obtain the leaching properties of impurities, optimize the leaching conditions, study the influence of conditions on leaching, and capture the restriction factors of leaching. The results indicate that the carbon content of the treated SCC can reach 97.3% when the leaching condition attach the optimal (liquid-solid ratio of 25 mL/g, temperature of 413 K, time of 270 min and acid concentration of 4 mol/L), and liquid-solid ratio is regarded as the crucial factor influencing on that. In addition, the activation energy of impurities reaches 6.25 kJ/mol and the whole leaching process is controlled by the diffusion extent. Finally, the filtrate after the hydrothermal acid leaching is treated, and calcium fluoride, cryolite and sodium chloride are successfully separated. The proposed process eliminates the harm of SCC to the environment, and completes a closed-circuit cycle for the treatment of SCC and recovery of valuable components. It enriches the hydrometallurgical processes of SCC, and provides an attractive scheme for the treatment of SCC. [Display omitted] • The environmental hazards of SCC are eliminated. • A closed-circuit cycle process for treating SCC was proposed. • The purity of SCC-HCl reaches 97.3% by hydrothermal acid leaching. • The leaching process follows Avrami model. [ABSTRACT FROM AUTHOR]