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Surfactant with amphiphilic substance has a vital impact on the synthesis of photocatalysts, which can affect surface property and morphology of materials. Herein, we proposed a Triton X-100 (TX-100)–assisted method for the synthesis of layered BiOBr nanosheet–assembled flower-like nanostructures. It was found that the TX-100 played a key role on the morphology and photocatalytic performance of the product. The prepared multilayered BiOBr nanosheet–assembled flower-like nanostructures exhibited larger specific surface area, broadened light absorption, and enhanced separation rate of photo-generated electrons and holes. The adsorption and photocatalytic degradation properties of ciprofloxacin (CIP) by our prepared BiOBr were investigated, and the results indicated that BiOBr assisted with 7 mL TX-100 exhibited higher adsorption ability and enhanced photocatalytic activity with 94.0% of ciprofloxacin degradation rate within 180 min. Superoxide radicals (·O2−) and holes (h+) were confirmed to be the two main reactive species for the degradation of ciprofloxacin. This work provides a novel surfactant-assisted method for the synthesis of layered nanosheet-assembled flower-like nanostructures, which would have potential applications in the photocatalytic field. The illustration of the photocatalytic degradation mechanism for ciprofloxacin under visible light. [ABSTRACT FROM AUTHOR]