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This invention belongs to the field of materials technology and discloses a polystyrene microsphere / chitosan composite film loaded with hydrophobic substances and its electrodeposition preparation method. First, a polystyrene microsphere emulsion loaded with hydrophobic substances is prepared by combining a compound emulsifier, styrene, water, hydrophobic substances, and azobisisobutyronitrile (AIBN). Then, chitosan is dissolved in an aqueous acetic acid solution to prepare a chitosan solution. The two solutions are then mixed, and sodium chloride solution and hydrogen peroxide are added to prepare an electrodeposition solution. Finally, using Pt as the anode and ITO as the cathode, the polystyrene microsphere / chitosan composite film loaded with hydrophobic substances is obtained by electrodeposition. This invention utilizes polystyrene microspheres as a carrier for hydrophobic substances, co-depositing them with chitosan to form a composite film. The hydrophobic substances in this composite film can remain stable for a long time and retain their original color development and catalytic properties, thus showing good application prospects in coatings, catalysis, and other fields.