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m-Cresol and p-cresol, important chemical intermediates, are widely used in medicine and pesticides. The mixture of m-cresol and p-cresol is easily produced in the industrial scale. However, it is very difficult to separate the mixture due to the boiling point. In this work, a new coupling process route combining complex crystallization and melt crystallization was proposed for the mixture separation. The key parameters in terms of crystallization temperature, solvent dosage, complexing agent dosage, initial purity of p-cresol, and crystallization time are investigated. The response surface methodology was employed to optimize the proposed process. The results show that the m-cresol and p-cresol mixture can be effectively separated, where the purity is >99% and the yields of m-cresol and p-cresol are over 63% and 55% respectively. In addition, recovery of solvents and complexing agents is achieved. The coupling route is proven to be a simple, environment-friendly, and sustainable process to separate industrial cresol. This study provided a reference for the isomerization separation process.

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