Spent sulfuric acid manufacturingManufacturing (SAM) catalysts, which are rich in heavy metals, present both environmental risks and potential resources. Ensuring safe disposal and efficient metalRecovery recoveryMetal recovery is essential for sustainabilitySustainability and waste valorization. This study focuses on developing and optimizing a hydrometallurgical process to recover vanadiumVanadium (V(V)) from spent SAM catalystsSpent SAM catalysts using alkali leachingLeaching and precipitationPrecipitation techniques. The leach liquor was produced by leaching the spent catalysts powder with 1 M NaOH at room temperature, maintaining a S/L of 250 g/L for 300 min. The resulting solution, rich in V(V) and Al(III), was then treated with NH4Cl at a pH of 7.8, leading to the precipitation of vanadium salt (NH4VO3NHVO). This salt was subsequently calcined at 410 °C for 120 min to convert it into high-purity V2O5. This green and sustainable approach transforms industrial vanadiumVanadium waste into valuable V2O5 materials, contributing to the advancement of the circular economyCircular economy.