Persulfate Electrosynthesis and Environmental Applications: Mechanistic Insights, Material Engineering, and Activation Methods

Abstract Persulfates play a vital role in the chemical industry and environmental science, serving as key raw materials in chemical production and demonstrating significant potential in environmental remediation through persulfate‐based advanced oxidation processes (PS‐AOPs). However, the persulfate electrosynthesis is hampered by competing oxygen evolution reactions and the electrosynthesis mechanisms remain debated. This review synthesizes recent experimental and theoretical progress to clarify the key intermediates and formation pathways on active (platinum (Pt)) and non‐active (boron‐doped diamond (BDD)) anodes. We highlight the structure‐activity relationships and the regulation strategies for BDD anodes, focusing on boron‐doping level, sp 3 /sp 2 carbon ratio, and substrate. Furthermore, the key electrosynthesis process parameters (such as operation temperature, pH, electrolyte additives, and current density) affecting the persulfate electrosynthesis and the persulfate activation methods are introduced in detail. In parallel, we examine persulfate activation strategies for PS‐AOPs and clarify their relative strengths and limitations. This work will bridge fundamental research and industrial applications, offering actionable guidelines for designing high‐performance anodes and advancing PS‐AOPs toward environmental applications.