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In this work, particles of activated carbon supported by Fe-N-TiO2 (Fe-N-TiO2/AC) were synthesized and used as the three-dimensional (3D) particle electrode for folic acid wastewater treatment in the 3D electrolysis and photocatalysis coupling process. The structure, morphology, and physical and electrochemical properties of the Fe-N-TiO2/AC particles were characterized, and the results showed that Fe-N-TiO2 was bound on the surface of AC particles by chemical attachment, and the Fe-N-TiO2/AC particles had better capability of adsorption