Disulfides are important organic intermediates commonly used in drug synthesis, materials science, and organic biochemistry. However, the synthesis of disulfides is still facing great challenges, such as organic contamination, low yield, etc. We report a recyclable approach in aqueous system for thiol coupling based on iodine oxidation, achieving a 98% oxidation yield for mercaptoethanols. The method utilizes potassium iodide to solubilize iodine monomers in an aqueous phase, and employs hydrogen peroxide to regenerate iodine from by-product iodide ions, conceiving a recyclable and green process without catalyst and organic solvents.