Designing 3D‐MoS 2 Sponge as Excellent Cocatalysts in Advanced Oxidation Processes for Pollutant Control

3D‐MoS 2 can adsorb organic molecules and provide multidimensional electron transport pathways, implying a potential application for environment remediation. Here, we study the degradation of aromatic organics in advanced oxidation processes (AOPs) by a 3D‐MoS 2 sponge loaded with MoS 2 nanospheres and graphene oxide (GO). Exposed Mo 4+ active sites on 3D‐MoS 2 can significantly improve the concentration and stability of Fe 2+ in AOPs and keep the Fe 3+ /Fe 2+ in a stable dynamic cycle, thus effectively promoting the activation of H 2 O 2 /peroxymonosulfate (PMS). The degradation rate of organic pollutants in the 3D‐MoS 2 system is about 50 times higher than without cocatalyst. After a 140 L pilot‐scale experiment, it still maintains high efficiency and stable AOPs activity. After 16 days of continuous reaction, the 3D‐MoS 2 achieves a degradation rate of 120 mg L −1 antibiotic wastewater up to 97.87 %. The operating cost of treating a ton of wastewater is only US$ 0.33, suggesting huge industrial applications.