Electrodialysis for the preparation of perrhenic acid has advantages such as simple process, low rhenium loss, low equipment investment, low reagent cost, and high product quality, making it the most promising method for preparing perrhenic acid. In a three-chamber electrodialysis cell using KReO4 as the raw material, platinum as the anode, and stainless steel as the cathode, the rhenium utilization rate reached as high as 99.3% under optimal conditions, indicating very low rhenium loss. However, this three-chamber electrodialysis cell has a very small volume, only 750 mL, and the concentration of perrhenic acid only exceeds 300 g/L after 25–26 hours of continuous operation.