| Summary: | Microcystin-LR (MC-LR), a potent hepatotoxin produced by the cyanobacteria, is of increasing concern worldwide because of severe and persistent impacts on humans and animals by inhalation and consumption of contaminated waters and food. In this work, MC-LR was removed completely from aqueous solution using visible-light-active C/N-co-modified mesoporous anatase/brookite TiO<sub>2</sub> photocatalyst. The co-modified TiO<sub>2</sub> nanoparticles were synthesized by a one-pot hydrothermal process, and then calcined at different temperatures (300, 400, and 500 °C). All the obtained TiO<sub>2</sub> powders were analyzed by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscope (TEM), specific surface area (SSA) measurements, ultraviolet-visible diffuse reflectance spectra (UV-vis DRS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, and photoluminescence (PL) analysis. It was found that all samples contained mixed-phase TiO<sub>2</sub> (anatase and brookite), and the content of brookite decreased with an increase in calcination temperature, as well as the specific surface area and the content of non-metal elements. The effects of initial pH value, the TiO<sub>2</sub> content, and MC-LR concentration on the photocatalytic activity were also studied. It was found that the photocatalytic activity of the obtained TiO<sub>2</sub> photocatalysts declined with increasing temperature. The complete degradation (100%) of MC-LR (10 mg L<sup>−1</sup>) was observed within 3 h, using as-synthesized co-modified TiO<sub>2</sub> (0.4 g L<sup>−1</sup>) at pH 4 under visible light. Based on the obtained results, the mechanism of MC-LR degradation has been proposed.
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