This study explored the efficient, stable, and continuous treatment of antibiotic-containing wastewater through rapid electron transfer between layered fluorine-free Ti3C2Tx and CoFe2O4 nanomicrospheres. These materials were synthesized into hydrogel beads crosslinked with sodium alginate, resulting high reactivity and stability. Ff-Ti3C2Tx-CoFe2O4 catalyst facilitated peroxymonosufate (PMS) activation through rapid electron transfer and the formation of Ff-Ti3C2Tx-CoFe2O4-PMS* species, as confirmed by experiments and DFT calculations. The cleavage of the S-O bond on Ff-Ti3C2Tx-CoFe2O4 catalyst identified as the primary mechanism for the generation of singlet oxygen (1O2). In a continuous flow system, the degradation efficiency of antibiotics, such as sulfamethoxazole (SMX), remained above 96.9 % with ultra-low metal leaching (<1.3 μg·L−1, 72 h). This research provides significant insights into the practical application of PMS activation for antibiotic degradation, offering a sustainable solution for wastewater treatment.