Abstract: Hypercrosslinked resin BE-CME was synthesised in one pot using simple aromatic molecule benzene and chloromethyl methyl ether (CME), using anhydrous ZnCl₂ and FeCl₃ as catalyst. The chemical structure of resin BE-CME was characterized by IR, elemental analysis and BET methods. The results indicated that the specific surface area of resin BE-CME was 812.43m²/g. The postcrosslinking reaction of BE-CME was carried out use the unreacted chloromethyl group on resin BE-CME. After postcrosslinked the specific surface area of P-BE-CME increased to 974.37m²/g. Batch adsorption runs of aniline in aqueous solution onto adsorbent BE-CME and P-BE-CME were researched. The adsorption capacity of aniline on P-BE-CME was larger than that on BE-CME and XAD-4. The adsorption process for aniline onto the resins was proved to be exothermic