Separation of acetic acid from acetic acid and water mixture was carried out by melt crystallization. The effect of the cooling rate, the amount of seeds, the seeding temperature, the sweating rate, and the sweating fraction on the distribution coefficient was investigated. The acetic acid was successfully separated by single-stage melt crystallization. As the sweating fraction is increased, the crystalline layers grown at lower cooling rates are purified more highly. Eventually, the crystallization rate is much more important than the sweating rate. The effective distribution coefficient ranges from 0.01 to 0.25 for the crystal growth rates of 1.2 × 10⁻⁶ m/s to 4 × 10⁻⁶ m/s.