Naproxen Degradation Using NiO Synthesized via Ultrasonic Spray Pyrolysis on Ni–Fe Foam by Ozone

Naproxen (NPX), a nonsteroidal anti-inflammatory drug, is considered an emerging contaminant due to its persistence and potential environmental risks. In this study, NPX degradation was investigated through ozonation using nickel–iron foam (NiFeF) and NiO-modified NiFeF (NiO/NiFeF). The effect of the foam size was investigated using three configurations: S1 (1 cm × 2.5 cm), S2 (2 cm × 2.5 cm), and S3 (2 cm × 5 cm). Complete NPX removal was achieved in all systems, with degradation times of 4 min for ozonation alone, 2 min for NiFeF-S1, and 1 min for NiO/NiFeF-S2 and NiO/NiFeF-S3. The NiO/NiFeF catalyst was synthesized via ultrasonic spray pyrolysis, resulting in a porous structure with abundant active sites. Compared with conventional ozonation, NiO/NiFeF-S1 improved the total organic carbon (TOC) removal rate by 6.2-fold and maintained 87.5% of its activity after five reuse cycles, demonstrating excellent stability. High-resolution mass spectrometry revealed that catalytic ozonation generated fewer by-products (22 vs. 27 for ozonation alone) and promoted more selective pathways, including demethylation, ring-opening oxidation, and partial mineralization to CO2 and H2O. This enhanced performance is attributed to the synergy between NiO and NiFeF, which facilitates reactive oxygen species generation and electron transfer. These results demonstrate the potential of NiO/NiFeF as an efficient and stable catalyst for pharmaceutical removal from water.