Tri-cresyl phosphate(TCP) was synthesized by reaction of phosphorus chloride with mixed cresol(mixture of m-cresol, p-cresol,and others) in the presence of AlCl₃. Some of unwanted products and unreactants colored TCP. In order to separate TCP from these, vaccume distillation was carried twice, but colorless TCP could not be producted. Separation of unwanted materials by 2% NaOH solution was introduced before first and second distillation and optimal separation conditions such as NaOH concentration, mixing volume ratio, mixing time, and rpm were investigated for new batch separation and production of colorless TCP. Optimal conditions were 2% NaOH solution, 36% mixing volume ratio of 2% NaOH solution, 1.5 hours of mixing time, and 20 rpm.