Xylene isomers are notorious chemical hazards, and their efficient removal from water solutions is still challenging. The current study reports a polymer nanocomposite as a potential adsorbent for successfully removing dissolved xylene isomers from contaminated water. Polystyrene-1D multiwall carbon nanotube nanocomposite (PS-MWCNT) adsorbent was prepared using the one-step bulk polymerization method. Mesoporous PS-MWCNT was prepared using the nano-crystallization phase separation method. The sulfonation of the mesoporous PS-MWCNT nanocomposites was carried out by treating the samples with concentrated sulfuric acid at elevated temperatures. The sulfonated PS-MWCNT (HO₃S-PS-MWCNT) was found to be a potential adsorbent for dissolved xylene isomers from water solution. In addition, the HO₃S-PS-MWCNT can be efficiently recycled for up to 10 consecutive cycles with negligible decline in adsorption values. The exhibited equilibrium adsorption, rate of adsorption, and rapid regeneration of the HO₃S-PS-MWCNT are clear indications for the possibility of practical utilization of these adsorbents in large-scale water treatment plants.

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