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The design of highly efficient organic/inorganic photocatalysts with visible-light response has attracted great attention for the removal of organic pollutants. In this work, the polyacrylonitrile (PAN) worked as the matrix polymer, while polyaniline (PANI) and Sb₂S₃–ZnO were used as organic/inorganic photocatalysts. The heterojunction PAN/PANI–Sb₂S₃–ZnO photocatalyst was prepared using electrospinning and surface ultrasound. PAN/PANI–Sb₂S₃–ZnO exhibited an excellent visible-light absorption intensity in the wavelength range of 400–700 nm. The maximum removal efficiencies of PAN/PANI–Sb₂S₃–ZnO for four organic dyes were all greater than 99%. The mechanism study showed that a dual Z-scheme could be constructed ingeniously because of the well-matched bandgaps between organic and inorganic components in the photocatalyst, which achieved efficient separation of photogenerated carriers and reserved photogenerated electrons (e⁻) and holes (h⁺) with strong redox ability. The active species •OH and •O₂⁻ played an important role in the photocatalytic process. The composite photocatalyst also had excellent stability and reusability. This work suggested a pathway for designing novel organic/inorganic composite photocatalysts with visible-light response.