A nanofiber mat of styrene−co−vinylbenzyl chloride−co−acrylonitrile copolymer as an anion exchange membrane (AEM) was synthesized via the electrospinning of organic reaction mixtures. The synthesized membranes were characterized using FT-IR spectroscopy for structural analysis. The AEM demonstrated a high ionic conductivity mainly due to the phase segregation in the membrane structure, as analyzed by transmission electron microscopy (TEM). The membrane properties such as water uptake, swelling ratio, and ion exchange capacity, as well as ionic conductivity, varied with the chemical composition. With the molar ratio of styrene, vinylbenzyl chloride, and acrylonitrile at 3:5:2, the highest ionic conductivity of 0.214 S cm⁻¹ at 80 °C was observed. Additionally, the AEM retained 94% of original conductivity after 72 h of soaking in 1 M KOH solution.