The treatment of industrial polycrystalline diamond (PCD) blanks in aqua regia at atmospheric pressure between 333 K and 353 K was performed via the ultrasound-assisted leaching process to investigate whether the influence of ultrasound is beneficial. Cobalt content in the solution and in the blanks was monitored as well as the effects of leaching temperature, solid-to-liquid ratio, and PCD blank size. The use of intermittent and permanent ultrasound helped reduce the leaching time and thus energy consumption by up to 50%. In all trials with ultrasound, higher temperature only has a slight effect. Solid-to-liquid ratio does not have a positive or negative impact. A new process design was tested using an innovative experimental setup for ultrasound-assisted leaching aiming at maximum cobalt and diamond recovery from PCD and final reuse of fine PCD for cutting and polishing other hard materials in different important industrial applications.