Two kinds of hypercrosslinked resin ZH-01 and ZH-03 were prepared in this study. Experimental investigations were conducted to study the adsorption characteristics of 4-chlorophenol on the hypercrosslinked resins by method of static adsorption. The equilibrium adsorption data was fitted to Freundlich adsorption isotherm model to evaluate the related parameters. The results showed that the changes of enthalpy, free energy, entropy indicate an exothermic, spontaneous and disorder decreasing process happened in the adsorption. It was also shown that, respecting to the adsorption capacity, the adsorbents prepared here are better than the Amberlite XAD-4 for removing the 4-chlorophenol in aqueous solutions.