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The precipitation method was employed to synthesize hollow column-like CuS with copper nitrate and sodium thiosulfate as materials. The related morphology and crystalline phase of the sample were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and the fourier transform infrared (FT-IR). Meanwhile, the degradation performance of hollow column-like CuS was investigated with methyl orange (MO) as a contamination. The results show that the as-prepared hollow column-like CuS is assembled from CuS nanosheets. The diameters and the length of hollow column-like CuS are 400 nm and 2.0 μm, respectively. The Fenton-like catalyst consisting of hollow column-like CuS and H₂O₂ shows excellent degradation ability for dye. After 110 min, the degradation rate of methyl orange reaches 86.6%, which is superior to the degradation ability of CuS with a solid structure.