Nibras N. Mahmood, Zainab F. AL- Bawi
The growing demand for sustainable energy and effective wastewater management necessitate the development of integrated treatment and energy systems. Herein, a multilayer rutile TiO 2 /α‐Fe 2 O 3 /GO photoanode is engineered for the simultaneous treatment of real refinery effluent and hydrogen production in a photoelectrochemical (PEC) system. Laser‐assisted stimulation is introduced to improve interfacial charge transfer kinetics and mitigate electrons‐hole recombination, thereby enhancing the PEC performance under combined UV and visible‐light irradiation (AM 1.5 G, 100 mWcm −2 ). Under optimized conditions (pH 3, 40°C, 50 min, catalyst loading of 0.4 mg cm −2 ), removal efficiencies of 98.7%, 96.0%, and 97.3% for COD, phenol, and TOC, respectively, were achieved through the continuous treatment of actual refinery wastewater. The hydrogen production rate was quantified at 8340.33 μmol L −1 with a current density of 65.23 mA cm −2 . These results demonstrate the effectiveness of multilayer oxide/GO architecture in promoting charge separation and interfacial enabling robust and efficient PEC platform. This study provides a practical pathway for integrating wastewater remediation with renewable hydrogen production, with potential for scalable implementation in energy–environment applications.