This work presents both the design of a novel process to produce microparticles with a shell core structure and a bench scale apparatus purposely realized. The developed process was designed to respond to mandatory needs of process intensification. It involved the coupling of two emergent technologies: atomization assisted by ultrasonic energy and microwave heating. The former was used to atomize polymeric solutions; the latter was applied to stabilize the produced droplets by drying. Both operations were performed in the same vessel with the aim to have a single-pot process chamber and were carried out by a semicontinuous procedure. Basic design criteria and advantages of the ultrasonic microwave coupled operations in the realized apparatus are presented and discussed. Results of testing and of operating runs to produce shell core microparticles are also reported, emphasizing the main features of the produced particles.