The self-supported ZnS microsphere composed of interwoven nanosheets was synthesized by hydrothermal method. The as-prepared ZnS powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic activity of the fabricated ZnS powders was evaluated by the degradation of 2,4-dichlorophenol (DCP) under UV light. Effects of DCP initial concentration, ZnS dosage, solution pH, light source, and dissolved oxygen on DCP photocatalytic degradation efficiency were investigated and optimized systematically. Results demonstrated that 53% of DCP could be effectively degraded under the optimal experimental conditions. Finally, high-performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC-MS) were used to analyze the degradation products. Based on the experimental results obtained, a prob- able degradation pathway was proposed.