Abstract: ⁹⁰Y is a significant medical radionuclide that can be labeled with monoclonal antibodies, microspheres and peptides for tumor therapy. In this study, inorganic adsorbent polyantimonic acid with excellent adsorption performance was prepared by vacuum freeze-drying method as the separation material, and the ⁹⁰Sr-⁹⁰Y generator was developed by the separation strategy of double column method and hold-back carrier method. The effect of reaction conditions, drying method and other factor on the preparation of polyantimonic acid were systematically investigated, and the optimized preparation process was obtained. The static adsorption capacity of polyantimonic acid for strontium is 121 mg/g, the adsorption equilibrium time is 4 h, and the dynamic adsorption capacity reached 73 mg/g. The adsorption performance of polyantimonic acid was significantly improved compared with previous reports. The separation of Sr and Y was carried out by the double column method with ⁸⁹Sr as tracer, and the separation factor of Sr and Y could be increased to more than 10⁷ after adding Sr hold-back carrier into the primary column eluent. This study puts forward new ideas and methods for the key technical problems in the preparation of ⁹⁰Sr-⁹⁰Y generator, and carries out experimental verification, which is of great significance to the preparation of ⁹⁰Sr-⁹⁰Y generator.