Macroporous resin (D201)-supported quarternary ammonium bisulfate (D201-HSO4) was prepared and effectively used in catalyzing the hydrolysis of epoxides or aziridines under mild and non-metal conditions to give the corresponding 1,2-diols and b- amino alcohols in high yields. The catalyst was facilely prepared and recyclable. Macroporous resin (D201) -supported quarternary ammonium bisulfate (D201-HSO4) was prepared and effectively used in catalyzing the hydrolysis of epoxides or aziridines under mild and non-metal conditions to give the corresponding 1,2-diols and b-amino alcohols in high yields. The catalyst was facilely prepared and recyclable.