Efficient Catalytic Production of 1,3,2-Dioxathiolane 2,2-Dioxide (DTD) Using In Situ-Generated H ₂ O ₂

1,3,2-Dioxathiolane 2,2-dioxide (DTD) is a critical electrolyte additive used in the lithium-ion battery materials field. The conventional synthesis routes, however, often suffer from the use of hazardous oxidants and generate substantial waste. We developed an anthraquinone-mesitylene-based catalytic system that generates H2O2 in situ under visible light irradiation. We then used this system directly in the catalytic oxidation of TS-1 for the synthesis of DTD, achieving a DTD yield of 88% under batch reaction conditions. A continuous flow reactor was constructed to load the spherical TS-1 catalyst, improving the gas–liquid mass transfer efficiency and preventing TS-1 separation during the oxidation reaction. Owing to these advantages of the continuous flow strategy, the reaction time was shortened from 6 h to 9.5 min, achieving a 92% isolated yield of DTD. This work establishes an efficient, safe, and environmentally benign process for DTD synthesis, highlighting the power of coupling photocatalytic H2O2 production with continuous-flow oxidation as a promising approach for sustainable chemical manufacturing.