Resin regeneration is crucial in the feasibility of polyol purification by ion exchange. In order to get an economically viable commercial process, a new regeneration process, including initial and final methanol flushing steps and treating with a 4.5 M aqueous mineral acid solution, has been investigated. An important reduction in regeneration costs was reached by minimizing the amount of acid used and recycling one part of the regenerant solution to the process. The composition of regeneration effluents has been studied in order to recover their valuable components. This simple resin regeneration technique lends itself to a technically and economically viable commercial process for the treatment of polyol products.