A new separation technique, called stripping crystallization (SC), is applied in this work for the purification of a 2,6-xylenol/m-cresol mixture. Basically, SC combines distillation and crystallization to produce pure crystals based on the three-phase equilibrium. A thermodynamic model is proposed to simulate the three-phase equilibrium conditions during the SC operation. The experiments show that SC can be applied to purify 2,6-xylenol from a 2,6-xylenol/m-cresol mixture, while it is rather difficult to purify m-cresol. For purification of 2,6-xylenol, the recovery rate increases with increasing operating pressure, while the final purity of the product decreases with increasing operating pressure.