| Summary: | N,S-TiO<sub>2</sub> deposited on three kinds of pre-treated sugarcane bagasse was synthesized via a sol–gel method. The obtained composites were characterized by various techniques, including scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and photoluminescence spectroscopy (PL). UV-visible induced degradation of ciprofloxacin was investigated. The influence of some experimental parameters such as contact time, pH, dosage, and initial concentration on the efficiency of ciprofloxacin elimination was also evaluated. The highest efficiency was observed for the alkaline pre-treated sugarcane bagasse combined with N,S-TiO<sub>2</sub>, about 86% under optimal conditions (contact time 150-min irradiation, pH 5.5–6, dosage 0.5 g L<sup>−1</sup>, and the initial concentration CIP 30 ppm). There may be a rapid ciprofloxacin transition from the adsorption site to the photocatalytic site, and the alkaline pre-treated sugarcane bagasse/N,S-TiO<sub>2</sub> prevented the recombining of holes and electrons of the photocatalyst. Furthermore, the alkaline pretreatment sugarcane bagasse/N,S-TiO<sub>2</sub> composite material was sustainable, with only a 10% reduction after reusing the material three times. The presence of sugarcane bagasse made the material easy to recover from the liquid phase.
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