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Novel iron-copper-carbon (FeCuC) aerogel was fabricated through a one-step process from metal-resin precursors and then activated with CO2 and N2 in environmentally friendly way. The activated FeCuC aerogel was applied in a heterogeneous electro-Fenton (EF) process and exhibited higher mineralization efficiency than homogeneous EF technology. High total organic carbon (TOC) removal of organic pollutants with activated FeCuC aerogel was achieved at a wide range of pH values (3-9). The chemical oxygen demand (COD) of real dyeing wastewater was below China's discharge standard after 30 min of treatment, and the specific energy consumption was low (9.2 kW·h·kg(-1)COD(-1)), corresponding to a power consumption of only ∼0.34 kW·h per ton of wastewater. The enhanced mineralization efficiency of FeCuC aerogel was mostly attributable to ultradispersed metallic Fe-Cu nanoparticles embedded in 3D carbon matrix and the CO2-N2 treatment. The CO2 activation enhanced the accessibility of the aerogel's pores, and the secondary N2 activation enlarged the porosity and regenerated the ultradispersed zerovalent iron (Fe(0)) with reductive carbon. Cu(0) acted as a reduction promoter for interfacial electron transfer. Moreover, activated FeCuC aerogel presented low iron leaching (<0.1 ppm) in acidic solution and can be molded into different sizes with high flexibility. Thus, this material could be used as a low-cost cathode and efficient heterogeneous EF technology for actual wastewater treatment.

Metal–organic frameworks (MOFs) are a new class of porous crystallized materials, which have attracted great interest for sustainable energy and environmental remediation. The functionalization of MOF‐based catalysts has been investigated to improve their photocatalytic ability. Here, we present a way of enhancing a magnetic MOF‐based photocatalyst composed of MIL‐100(Fe) and Fe3O4. The photocatalytic performance of the MOFs was significantly enhanced by the simultaneous introduction of a Fe3O4 core and H2O2, as the photoinduced holes and electrons of the MOF were relayed to the core F3O4 and reacted with H2O2, respectively. The optimal thickness of the MOF shell is ≈50 nm for core–shell Fe3O4@MIL‐100 microspheres to achieve the highest photocatalytic ability. Moreover, core–shell Fe3O4@MIL‐100(Fe) can be easily recycled without significant loss of photocatalytic ability after being used several times.

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