An amine is separated from an aqueous solution of amine and volatile organic compounds by distillation in a column. The vapors generated during distillation are condensed. The condensed vapors are then passed into a separating device in which the volatile organic compounds are removed. The liquid remaining in the separating device is then fed to the head of the distillation column. Water is removed from the column in a sidestream and diamine is the residue. This process is particularly effective in recovering aromatic diamines from solutions which accumulate during hydrogenation of dinitro aromatic compounds.