Post-crosslinked poly(meta-divinylbenzene) (PMDVBpc) resin was synthesized from the precursor resin poly(meta-divinylbenzene) (PMDVB) by Friedel-Crafts reaction, and the adsorption behavior of PMDVBpc was evaluated using phenol as the adsorbate from aqueous solutions. The BrunauerEmmett-Teller (BET) surface area and pore volume of PMDVBpc increased significantly in comparison with PMDVB, inducing an enhanced adsorption to phenol. The equilibrium data could be well fitted by both of the Langmuir and Freundlich models, and the isosteric adsorption enthalpy decreased with increasing of the fraction loading. At an initial concentration of 580.5 mg/L and a flow rate of 8.0 BV/h (1 BV = 10 mL), the breakthrough point of phenol on 10 mL of wet PMDVBpc be 26.13 BV, and 7 BV of industrial alcohol could regenerate the resin column completely.