Electrospun nanofiber membranes based on cellulose acetate (CA) have gained increasing attention for wastewater treatment due to their high surface area, tuneable structure, and ease of functionalization. In this study, the performance of CA membranes was enhanced by incorporating aluminum oxide (Al
2
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Electrospun nanofiber membranes based on cellulose acetate (CA) have gained increasing attention for wastewater treatment due to their high surface area, tuneable structure, and ease of functionalization. In this study, the performance of CA membranes was enhanced by incorporating aluminum oxide (Al
2O
3) nanoparticles (NPs) at varying concentrations (0–2 wt.%). The structural, morphological, and thermal properties of the resulting CA/Al
2O
3 nanocomposite membranes were investigated through FTIR, XRD, SEM, water contact angle (WCA), pore size measurements, and DSC analyses. FTIR and XRD confirmed strong interactions and the uniform dispersion of the Al
2O
3 NPs within the CA matrix. The incorporation of Al
2O
3 improved membrane hydrophilicity, reducing the WCA from 107° to 35°, and increased the average pore size from 0.62 µm to 0.86 µm. These modifications led to enhanced filtration performance, with the membrane containing 2 wt.% Al
2O
3 achieving a 99% removal efficiency for Indigo Carmine (IC) dye, a maximum adsorption capacity of 45.59 mg/g, and a high permeate flux of 175.47 L·m
−2 h
−1 bar
−1. Additionally, phytotoxicity tests using
Lactuca sativa seeds showed a significant increase in germination index from 20% (untreated) to 88% (treated), confirming the safety of the permeate for potential reuse in agricultural irrigation. These results highlight the effectiveness of Al
2O
3-modified CA electrospun membranes for sustainable wastewater treatment and water reuse.
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