Oil spills and subsequent cleanup by oil–water separation remain a global concern. For the first time, corn silk-derived cellulose acetate (CSCA) and polyacrylonitrile (PAN) composite nanofiber are reported to create a superhydrophobic oil/water sequestration membrane. CA : PAN solutions with various PAN concentrations were evaluated for viscosity and conductivity. A CSCA nanofiber membrane was fabricated through electrospinning, which was superhydrophobic and oleophilic in water. Scanning electron microscope, energy-dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and thermogravimetric analysis/differential scanning calorimetry were used to analyze the membrane's morphological features. CSCA nanofibers formed a highly spherical bead with a maximum contact angle of 156° (>120°) in pure water solutions, demonstrating their superhydrophobicity. Different oil/water mixtures and emulsions were investigated and both can benefit from the oil-removal properties of the membranes, as gravity is the only force necessary to propel the system. Mineral oil had the highest oil sorption capability (908%), while toluene had the lowest (664%). For mineral oil–water mixtures, the CSCA membrane has the greatest separation flux at a maximum of 442 L/m2/h and the best separation efficiency at up to 99. 67%. These findings provide strong support for using an as-prepared CSCA nanofiber membrane as a viable reusable oil sorbent in oil spill cleaning.

  • Organic eco-friendly corn silk-derived cellulose acetate (CSCA) nanofiber was fabricated.

  • CSCA nanofiber featured exceptional oil/water separation capabilities.

  • The CSCA nanofiber exhibited superior durability and recyclable qualities.

  • With a separation efficiency of 99.67%, membranes are both superhydrophobic and oleophilic.

corn silk cellulose acetate, nanofiber, oil–water sequestration, superhydrophobic membrane
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