Hydroxypropionitrile is an intermediate for many organic synthesis reactions such as medicines, pesticides, and polymers, and is also used as a hydrogenation raw material for the synthesis of 3-aminopropanol. The adsorption of hydroxypropionitrile by macroporous adsorption resin is an ideal process. The macroporous adsorption resin directly separates and concentrates the hydroxypropionitrile from the acrylonitrile hydration reaction liquid, thereby not only eliminating the evaporation and concentration, the solvent extraction two-step process, the equipment investment is small, the operation is convenient, and the heat loss of the hydroxypropionitrile is effectively avoided.