An experimental study was carried out to construct a type 11 phase diagram of the liquid-liquid equilibrium of the mixed solvents of (2,2,2-trifluoroethanol + methanol + cyclohexane) at the temperatures T = (283.15, 293.15, 303.15, and 313.15) K, and under atmospheric pressure of 101.2 kPa. Gas-liquid chromatography was used to obtain the mole fractions of the tie line ends of the two liquid phases at equilibrium. The NRTL and UNIQUAC equations reproduced satisfactorily all the measured data with an average root-mean-square deviation in phase-mole fractions equal to 1.04 %. The binary intermolecular interactions governing the mixture of unlike molecules were estimated by means of the same equations. The temperature effect on the system miscibility is slightly more significant on the cyclohexane-rich phase than on the (trifluoroethanol + methanol)-rich phase.