We developed an effective approach for increasing phenol uptakes on a hypercrosslinked polystyrene resin and separating phenol from methyl orange or Congo red from the mixed solution. The ethylenediamine-modified hypercrosslinked polystyrene resins were synthesized, the equilibrium and breakthrough performance of the resins were determined on a selected resin named HJ-D33. The phenol uptakes on HJ-D33 were remarkably larger than that on its precursor and the commercial adsorbents like XAD-4, D301. The breakthrough capacity of phenol on HJ-D33 was 50.37 mg/ml wet resin at an initial concentration of 800.8 mg/L and a flow rate of 8.0 BV/h and the used HJ-D33 could be completely regenerated by a mixed solvent containing 0.01 mol/L of sodium hydroxide and 50% of ethanol. Methyl orange (or Congo red) and phenol could be dynamically separated by HJ-D33 resin column as the effluent was in the range of 0-60 BV. (C) 2013 Elsevier B.V. All rights reserved.