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Adsorptive nanofiber electrospun membranes (ANEMs) show promise for heavy metal removal, particularly in dilute solutions. Nanofibrous polyacrylonitrile (PAN) membranes incorporating Cloisite 20A (C20) organoclay were fabricated via electrospinning for As(V) removal. The impact of C20 on structural properties and As(V) removal efficiency of the nanofiber membranes was investigated. The results indicated that the PAN‐C20 membranes morphology was uniform, with fiber diameters mostly falling within the 100–300 nm range. Incorporation of C20, especially in an exfoliated structure, led to increased hydrophilicity, mechanical strength, and roughness of the membranes. Batch adsorption results revealed that the adding C20 up to 1.5 wt.% significantly enhanced adsorption capacity due to the higher concentration and proper C20 dispersion. Dynamic filtration showed that the PAN‐C20(1.0) membrane achieved over 90% As(V) removal efficiency for 960 min and demonstrated excellent regeneration ability. Highlights: Cloisite 20A organoclay was incorporated into PAN by electrospinning to prepare adsorptive membrane.Adsorptive membranes were used for As(V) removal from water.Type of Cloisite 20A dispersion in PAN in dynamic filtration was more important than in static adsorptionPAN‐C20‐1.0 with exfoliated structure showed higher removal efficiency than PAN‐C20‐1.0 with intercalated structure.PAN‐C20‐1.0 membrane was usable for multiple adsorption–desorption cycles. [ABSTRACT FROM AUTHOR]