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Superoleophilic and high‐strength electrospun membranes are promising materials for oil/water separation applications. Here we report the fabrication of a mechanically robust, hydrophobic polyurethane/multi‐walled carbon nanotube (PU/MWCNT) electrospun composite membrane for gravity‐driven oil/water separation. Various electrospun composite membranes with different MWCNT loadings were developed. Spinning parameters such as polymer concentration, solvent ratio, applied voltage, flow rate, and working distance were systematically optimized. The incorporation of MWCNT has increased the thermal stability, hydrophobicity, mechanical properties, and dye adsorption capacity of the PU membrane. The optimized composite fibrous membrane (PU/0.2‐MWCNT) exhibited a percentage elongation of 502%. All the PU/MWCNT composite membranes were found to be superoleophilic in nature. The optimized composite membrane showed the highest oil sorption capacity and lab‐scale oil flux of 14.21–24.07 gg−1 and 425.44 Lm−2 h−1, respectively. In the oil sorption process, all electrospun membranes were fitted to a pseudo second‐order kinetic model. Furthermore, electrospun composite membranes could adsorb toxic dye (Methylene blue) from the oil–water mixture. The PU/MWCNT composite membrane could be a potential candidate for oil/water separation applications.

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