Abstract: Macroporous crosslinked poly(N-p-vinylbenzyldimethylamine) resin was synthesized from chloromethylated poly(styrene-co-divinylbenzene) with dimethylamine. The residual chlorine in the title resin was 0.24 mmol/g, and its weak basic exchange capacity was 4.0 mmol/g, indicating that the reaction was performed successfully. Adsorption isotherm of phenol onto the title resin from aqueous solution was measured and described with Freundlich isotherm equation with the correlation coefficients greater than 0.99. Isosteric adsorption enthalpies were determined to be -20.81~-30.74 kJ/mol when the adsorption capacities were 15, 20, and 25 mg/g, implying that hydrogen bonding was one of the driving forces for the adsorption. Gibbs adsorption energies and adsorption entropies were both less than 0, which revealed that the adsorption was a spontaneous process leading to higher order. In addition, adsorption of phenol, p-nitrophenol, and p-nitroto-luene onto the resin from aqueous solution as well as that of phenol onto the resin from aqueous, cyclohexane, ethanol, and ethyl acetate solutions were discussed, and the adsorption mechanism via the cooperation between hydrophobic interaction and hydrogen bonding was confirmed.