1,3,2-Dioxathiolane 2,2-dioxide (DTD) is an essential intermediate in organic synthesis and plays a vital role in improving the performance and service life of lithium-ion batteries. A large amount of heat is released during the synthesis process of DTD, leading to its hydrolysis. Therefore, the low heat exchange efficiency of traditional batch reactors leads to lower product yield and certain safety hazards. Continuous flow microreaction technology is a significant development direction for the synthesis of DTD. Based on the advantages of efficient dispersion and mixing of fluids at the micrometer scale in microreactors, the effects of temperature, catalyst concentration, residence time, ratio of the two-phase flow rates and other factors on the conversion and selectivity to DTD are investigated, and the optimal process conditions are determined. When the temperature is 14.73 °C, the catalyst concentration is 0.5 g L⁻¹, the flow rate ratio between the continuous phase and the dispersed phase is 0.6, the total flow rate is 2 mL min⁻¹, and the residence time is 117.75 s, the continuous reaction yield can reach 92.22%. The synthesis kinetic data of DTD are measured, and the activation energy and preexponential factor of the reaction are obtained. This study lays the foundation for the synthesis and application of DTD in microreactors, as well as the numbering-up of microreactors.