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The aim of this paper is to present a new concept for separation of a reaction mixture (RM) that is result of degradation of cumenehydroperoxide in industrial plants. Except the main components - phenol and acetone, this mixture contains water and a great number of different compounds, which form a lot of azeotropic mixtures. The separation of RM is difficult, power consuming and is impossible to occur without chemisorption. The proposed method has been implemented in the Phenol plant - “LUKoil Neftochim” in Bourgas, Bulgaria. The difference between the new and the existing technologies is that the main quantity of phenol, presenting in so-called acetone stream, is removed from the bottom of the first column for acetone purification and then it goes back for dilution of the reaction mixture. The application of this method reduces at least by half the quantity of phenol containing waste water and the expenses for the water regeneration: NaOH, H2SO4, steam, cooling water, electric power, etc. It lowers the consumption of steam and cooling water as a result of usage of partial condensers at first two columns. The quality of the finished acetone is improved too.