Abstract: Tellurium-130 dioxide (¹³⁰TeO₂) is a stable isotope product that can serve as a precursor to the commonly used iodine-131 medical isotope and a key isotope material for neutrinoless double beta decay experiment. This study investigated the preparation technology of tellurium-130 dioxide using tellurium-130 hexafluoride (¹³⁰TeF₆) as the raw material, and determined a feasible route for preparation process. The process parameters of hydrolysis, reduction, neutralization, and calcination process were studied and determined through systematic experiments. The research results indicated that the yield of ¹³⁰TeO₂ preparation process could reach over 87%, and the purity of the product could reach over 99.99%. The preparation route determined in this study was suitable for mass production of the product with the high chemical purity. The related technologies provided the basis and reference for isotope preparation techniques with valence state changes, which was conducive to improving the independent supply capacity of related isotope products.