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In this study, TiO2/Carbon fibre (CF) composite photocatalyst was prepared by sol‐gel method, and its characterization was analysed by SEM and XRD. Under the ultraviolet light, the effects of various single factors on the removal of ammonia nitrogen from aquaculture wastewater by TiO2/CF were discussed. Orthogonal experiments were performed to determine the most beneficial conditions for ammonia nitrogen removal. When the dosage of TiO2/CF was 2.0 g/L, the initial concentration of ammonia nitrogen was 30 mg/L, the calcination temperature was 600°C, the concentration of H2O2was 0.8 g/L, the illumination time was 1 hr, TiO2/CF had excellent performance of remove ammonia nitrogen. The results show that compared with the treatment of ammonia nitrogen by CF or TiO2, TiO2/CF was more effective in the removal of ammonia nitrogen. TiO2/CF composite material was applied to the treatment of ammonia nitrogen in marine aquaculture wastewater for the first time, which provides a scientific and effective treatment method for photocatalytic technology in later industrial treatment process.

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