Electrospun MIL‐101(Fe)/Graphene Oxide Nanofibrous Composites for Efficient Removal of Heavy Metals From Wastewater

Timoth Mkilima, Kulzipa Dakieva, Gulmira Adilbekkizi Adilbektegi, Yelena S. Tatina, Mansur Khussainov, Salauat Kassymkhanov, Kanagat Kamzanovna Tolubayeva, Bitmanov Yertas Zhantasuly, Bibigul Daukenova

2025

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DOI 10.1002/wer.70105
Data confidence 70 medium
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Abstract

ABSTRACT Heavy metal contamination in industrial wastewater poses a critical environmental challenge due to the toxicity and persistence of metals such as Pb(II) and Cd(II). This study evaluated the performance of MIL‐101(Fe)/Graphene Oxide (GO) electrospun nanofibrous membranes as advanced adsorbents for the efficient removal of these metal ions. Structural characterization confirmed a high surface area and uniform integration of MIL‐101(Fe) and GO within the fibrous matrix. Batch adsorption experiments revealed maximum removal efficiencies of 93% for Pb(II) and 95% for Cd(II), with optimum performance observed at pH 5.5 and 6.0, respectively. The adsorption process followed pseudo‐second‐order kinetics ( R 2 > 0.98), suggesting chemisorption, and was well described by both Langmuir (q max : 126 mg/g for Pb(II), 100 mg/g for Cd(II); R 2 ≥ 0.98) and Freundlich isotherms (1/ n < 1), indicating favorable monolayer and multilayer adsorption on heterogeneous surfaces. The thermodynamic analysis confirmed that adsorption was spontaneous (ΔG° values as low as −8.6 kJ/mol for Pb(II)) and endothermic (ΔH° values of 21.5 kJ/mol for Pb(II) and 18.9 kJ/mol for Cd(II)). In continuous flow systems, the membranes maintained removal efficiencies above 85% for both metals across 10 cycles at a flow rate of 10 mL/min. The membranes also exhibited excellent fouling resistance, with flux decline remaining below 10% over 5 cycles, and demonstrated high cleaning efficiency, recovering up to 99.2% of flux through simple deionized water rinsing. Reusability studies showed that the membranes retained over 80% of their original adsorption capacity after eight regeneration cycles in batch mode, and over 70% removal efficiency and 83% water flux after 10 regeneration cycles in real industrial wastewater conditions. These findings demonstrated the robustness, reusability, and scalability of MIL‐101(Fe)/GO membranes for the effective treatment of heavy metal‐contaminated industrial effluents. Future studies should explore membrane performance under mixed contaminant conditions and assess techno‐economic feasibility at the pilot scale. Practitioner Points Advanced nanofibrous membranes with MIL‐101(Fe)/Graphene Oxide (GO) tested for heavy metal removal. Outstanding performance compared to conventional adsorbents. 93% Pb(II) and 95% Cd(II) removal at optimum pH conditions (Pb(II): pH 5.5, Cd(II): pH 6.0). Rapid equilibrium kinetics with 60 minutes compared to 120 minutes. High surface area and optimal pore size critical for superior performance.