摘要： In this article, Bi2O3/Bi2MoO6 composites were synthesized hydrothermally under optimized conditions, by adjusting pH, the concentration of polyvinylpyrrolidone (PVP (K30)) and reaction time. During the synthesis process, flower-root shaped zero-gap Bi2O3/Bi2MoO6 heterojunctions were successfully synthesized. The adopted samples were characterized by X-ray diffraction (XRD), Scanning electron microscope (SEM), Energy spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), Diffuse reflectance spectra (DRS), Photoluminescence (PL), and Fourier transform infrared spectroscopy (FT-IR). The photocatalytic activity was measured under visible-light-irradiation (λ > 420 nm) by degrading tetracycline (TC), ciprofloxacin (CPFX) (antibiotics) and rhodamine B (RhB), methylene blue (MB) (dangerous dyes). The degradation results indicated that photocatalyst sample synthesized at pH 9.0, PVP (K30) 0.05 mol/L and 80 min reaction time (Sup-Bi2O3/Bi2MoO6) demonstrated highly efficient performance. The Sup-Bi2O3/Bi2MoO6 showed the highest apparent rate constant (Kapp) that’s 50% more than the samples prepared at ordinary conditions. Photocatalytic degradation order was i.e. RhB> TC> CPFX> MB, which depends on the polarity of the degrading medium.