The invention relates to a process wherein a stream comprising dichlorohydrin, water, and HCI is separated into a stream which is rich in dichlorohydrin and low in HCI and an aqueous HCI stream which is low in dichlorohydrin. The process involves the distillation of the mixture comprising dichlorohydrin, water, and HCI with an amount of water being added before and/or during the distillation such that the water concentration during the distillation is on the line D-E, or to the right thereof, in the phase diagram of FIG. 1.