AbstractThis study presents a novel approach to decontaminate ferrocyanide‐contaminated wastewater. The work effectively demonstrates the use of bimetallic Mo/Zr‐UiO‐66 as a super‐adsorbent for rapid sequestration of Prussian blue, a frequently found iron complex in cyanide‐contaminated soils/groundwater. The exceptional performance of Mo/Zr‐UiO‐66 is attributed to the insertion of secondary metallic sites, which deliver synergistic effects, benefiting the inherent qualities of the framework. Moreover, to extend the industrial applications of metal‐organic frameworks (MOFs) in real‐world scenarios, an approach is delivered to structure the nanocrystalline powders into MOF‐based macrostructures. The work demonstrates an interfacial process to develop continuous MOF nanostructures on ordinary laboratory‐grade filter papers. The novelty of the work lies in the development of robust free‐standing filtration materials to purify PB dye‐contaminated water. Additionally, the work embraces a circular economy concept to address problems related to resource scarcity, excessive waste production, and maintenance of economic benefits. Consequently, the PB dye‐loaded adsorbent waste is re‐employed for the adsorption of heavy metals (Pb2+ and Cd2+). Simultaneously, the study aims to address the problems related to the real‐time handling of powdered adsorbents, and the generation of ecologically harmful secondary waste, thereby, progressing toward a more sustainable system.

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