The aim of this work was the two-aqueous phase extraction of neutral red and methylene blue from wastewater. This has been achieved on the basis of phase separation properties of non-ionic surfactants above the so-called cloud point curve and the solubilization phenomena of coacervate micelles (surfactant rich phase). Three commercial surfactants were used in this work; the OXo-C15E7 which is an ethoxylate fatty alcohol (Dehydol LT 7), Triton X-114 (iso-C8H17-C6H4(OCH2CH2)(7,5)OH), and Triton X-100 (iso-C8H17-C6H4-(OCH2CH2)(9,5)OH) which are alkyl phenol ethoxylate surfactants. The phase diagrams of binary water/surfactants systems were drawn and the effect of sodium sulphate on water-surfactant systems was therefore studied. OXO-C15E7 and Triton X-114 were used for the cloud point extraction of neutral red and methylene blue from their aqueous solutions at 100mg/L and 7mg/L, respectively. The experimental extraction results were expressed by the following three responses: percentage of the extracted dye (E), residual concentrations of dye in the dilute phase (X-S,X-W), and the volume fraction of coacervate (phi(C)) at the equilibrium. The results obtained for each parameter were also represented on three-dimensional diagrams using an empirical smoothing method. The empirical modelling data were in agreement with the experimental ones. The main advantage was sought between E, which has reached 99% in the case of neutral red, whereas in the case of mehtylene blue 92% was obtained with respect to (phi(C)), which should have a minimum value. At the optimal conditions, neutral red and methylene blue concentrations in the effluent were reduced to about 500 times and 7 times, respectively.