The invention relates to the field of sewage treatment, and discloses a preparation method of a magnetic sewage treatment agent. The preparation method comprises the steps of weighing ferroferric oxide nano magnetic powder, adding pure water for ultrasonic dispersion, and obtaining a dispersion solution; weighing a dispersing agent, dissolving the dispersing agent into anhydrous ethanol, adding the dispersion solution, and conducting ultrasonic treatment to obtain a stable dispersion solution; under ultrasonic conditions, adding an aqueous solution of polyethylene glycol chitosan grafted materials into the stable dispersion solution, and obtaining coated magnetic nanoparticles; adding the coated magnetic nanoparticles into a bismuth nitrate solution, then adding a molybdate solution, and obtaining a solvothermal reaction system; making the system subjected to a solvothermal reaction to obtain a reaction product; obtaining the magnetic sewage treatment agent after the reaction product is washed, centrifuged, dried and calcined at high temperature. The preparation method has the advantages that the process is simple, the cost is low, catalyst load is firm, the thickness of a coatinglayer on the surface of each magnetic nanoparticle is small, the magnetic properties of the particles cannot be influenced, and the preparation method of the magnetic sewage treatment agent is suitable for industrial production.