The invention provides a method for removing iron ions from an acrylic fiber solvent by adsorptive separation. Active carbon is used as an adsorbent; the method comprises two parts, namely adsorptive iron removal and periodic regeneration of the active carbon; an adsorption device adopts an adsorptive separation process of a multi-bed fixed bed. The method removes impurities such as iron ions and the like from the cyclic solvent in a two-step acrylic fiber producing process; and after the adsorptive separation, the removal rate of the iron ions in a solvent product is over 70 percent, and the yield of sodium thiocyanate in the solution reaches over 99 percent. The method has the advantages of simple process, consumption of little amount of steam and acid-base, low three-waste discharge and low environmental pollution.