| Summary: | Herein, novel ternary kaolin/CeO<sub>2</sub>/g-C<sub>3</sub>N<sub>4</sub> composite was prepared by sol-gel method followed by hydrothermal treatment. The self-assembled 3D “sandwich” structure consisting of kaolin, CeO<sub>2</sub> and g-C<sub>3</sub>N<sub>4</sub> nanosheets, was systematically characterized by appropriate techniques to assess its physicochemical properties. In the prerequisite of visible-light irradiation, the removal efficiency of ciprofloxacin (CIP) over the kaolin/CeO<sub>2</sub>/g-C<sub>3</sub>N<sub>4</sub> composite was about 90% within 150 min, 2-folds higher than those of pristine CeO<sub>2</sub> and g-C<sub>3</sub>N<sub>4</sub>. The enhanced photocatalytic activity was attributed to the improved photo-induced charge separation efficiency and the large specific surface area, which was determined by electrochemical measurements and N<sub>2</sub> physisorption methods, respectively. The synergistic effect between the kaolin and CeO<sub>2</sub>/g-C<sub>3</sub>N<sub>4</sub> heterostructure improved the photocatalytic performance of the final solid. The trapping and electron paramagnetic resonance (EPR) experiments demonstrated that the hole (h<sup>+</sup>) and superoxide radicals (•O<sub>2</sub><sup>−</sup>) played an important role in the photocatalytic process. The photocatalytic mechanism for CIP degradation was also proposed based on experimental results. The obtained results revealed that the kaolin/CeO<sub>2</sub>/g-C<sub>3</sub>N<sub>4</sub> composite is a promising solid catalyst for environmental remediation.
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