The contamination of aquatic systems by tetracycline hydrochloride (TC) has emerged as an urgent environmental concern necessitating immediate intervention. Herein, a mechanochemical approach was utilized to synthesize a FeOOH@AC nanocomposite through the co-grinding of goethite (FeOOH), hydroxylamine hydrochloride (NH2OH⋅HCl), and activated carbon (AC). The FeOOH@AC nanocomposite acted as a catalyst for the activation of sodium persulfate (PS), producing strong oxidizing radicals for the removal of TC from water. The results demonstrated that the physicochemical properties and crystal structure of FeOOH were altered via ball-milling treatment. The activation of PS-generated sulfate radicals (SO[Formula: see text] and hydroxyl radicals ([Formula: see text]OH) synergistically degraded TC. Additionally, the degradation rate of TC in a 50[Formula: see text]mg/L solution reached 91.26% after the addition of FeOOH@AC and PS. This work offers a theoretical and technical foundation for the mechanochemical ball milling preparation of FeOOH@AC, facilitating PS activation for the degradation of TC in water.