LAUSR

Microwave‐induced spray distillation, exploiting the microwave‐induced relative volatility change (MIRVC) effect, offers transformative approaches to intensifying liquid mixture separations. However, industrial adoption is hindered by challenges in electric field uniformity during scale‐up and the lack of pilot‐scale validation. To this, we employed rigorous numerical simulations to guide the innovative design of the microwave heating system, integrating a leaky waveguide with a structurally optimized quasi‐optical resonant cavity, thereby achieving exceptional electric field uniformity and enabling the successful development of a pilot‐scale system with a processing capacity of 500 tons/year. Experimental results aligned closely with theoretical predictions, confirming the pilot system's efficacy and validating the reliability of the MIRVC effect in scaled‐up applications. A comprehensive sensitivity analysis identified key process optimization strategies while demonstrating the system's robustness, underscoring its advantage for energy‐saving and separation intensification. This study provides critical engineering validation and a generalizable framework for the industrial‐scale development of microwave‐enhanced separation technologies.