Surfactant‐assisted synthesis of photocatalysts for water treatment has received extensive attention from researchers. In this paper, a novel and efficient BiOBr/graphene oxide (BiOBr/GO) photocatalyst assisted by sodium dodecyl sulfate (SDS) was synthesized by a simple solvothermal method. Compared with use of other surfactants, like polyvinylpyrrolidone (PVP) and cetyltrimethylammonium bromide (CTAB), BiOBr/GO (SDS) shows outstanding photocatalytic degradation activity under optimal conditions: The degradation rate constants of BiOBr/GO (SDS) for oxytetracycline (OTC), tetracycline hydrochloride (TCH), brilliant blue (BB), and Rhodamine B (RhB) are 0.073, 0.057, 0.166, and 0.626 min−1, which are 2.8, 1.8, 9, and 1.5 times larger than pure BiOBr, respectively. In addition, after five cycles, BiOBr/GO (SDS) exhibits superior cycling stability. The enhanced photocatalytic performance can benefit from the introduction of SDS and GO. With the assistance of SDS in the preparation process, BiOBr/GO (SDS) nanosheets have good adsorption performance and dispersion effect, which is favorable for raising their specific surface area. Meanwhile, the electron capture effect of GO improves the transfer and separation efficiency of photogenerated carriers. Moreover, the possible degradation pathway for TCH is identified through liquid chromatography–mass spectrometry (LC–MS). This research can become a valuable reference for synthesizing photocatalysts with visible light response to degrading organic pollutants such as antibiotics and dyes.
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