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Zinc nitrate (ZnO_N) and zinc acetate (ZnO_A) were used as precursors for the synthesis of zinc oxide (ZnO) nanoparticles by the sol–gel method. The ZnO powder was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy, X-ray diffraction (UV–Vis DRS), Fourier transform infrared spectroscopy (FTIR), physisorption of nitrogen, and X-ray photoelectron spectroscopy (XPS). On the other hand, the photocatalytic activity of the samples was tested in the degradation of 2,4-Dichlorophenoxyacetic acid (2,4-D) and 2,4-Dichlorophenol (2,4-DCP) under UV-light irradiation. The ZnO_N and ZnO_A showed polycrystalline irregular structures and rod-like morphology with mean sizes of 40 and 99 nm, respectively. The precursor type influenced the bandgap, crystallite size, surface area, total pore volume, and pore diameter. The XPS results showed high contents of C and N in the ZnO samples, and as a consequence, the solids present remarkable differences in the C/N, O/C, and O/Zn atomic ratios, which significantly influenced the physicochemical characteristics. The ZnO_N and ZnO_A exhibit photocatalytic properties against 2,4-D (74.7 and 90.9%, respectively) and 2,4-DCP (78.4 and 86.7%, respectively) and better performance of ZnO_A. These results are promising and indicate the potential to use this material as a photocatalyst to degrade organic pesticides.