화학공학소재연구정보센터
Journal of the Korean Industrial and Engineering Chemistry, Vol.15, No.1, 86-91, February, 2004
냉각에 의한 용액결정화에서 용매선정
Selection of Solvents for Cooling Crystallization in Solution
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초록
Retinol 중간체인 C15 sulfone의 냉각에 의한 용액결정화에서 적합한 용매 선정을 위한 연구가 수행되었다. 결정크기, 형상 및 수율에 미치는 용해도, 용해도 매개변수, 준안정영역의 넓이, 온도의 의존성과 혼합열의 영향이 고려되었다. C15 sulfone에 대한 용해도의 온도 의존성은 methanol > ethanol > heptane > hexane > ethyl acetate > acetone > DMF > toluene > dichloromethane > THF 이었으며 용질의 용해도 매개변수 값과 차이가 큰 용매에서 큼을 알 수 있었다. 용해도와 준안정영역은 C15 sulfone의 용해도 매개변수 값과 유사한 용매에서 최대였다. 입도는 준안정영역의 넓이가 증가함에 따라 감소하였다. 입자 형상은 C15 sulfone의 용해도 매개변수 값과 차이가 큰 용매에서 긴 침상형을 보였다. 냉각결정화에 의한 C15 sulfone을 분리정제하기 위해 알맞은 용매는 hexane이었다.
Selection of solvent for the cooling crystallization of a retinol intermediate like C15 sulfone was explored. Effects of solubility, solubility parameter, metastable zone width, temperature and heat of mixing on yield, and crystal size and crystal shape were investigated for various solvents. The temperature dependence of C15 sulfone on solubilities was in the order of methanol > ethanol > heptane > hexane > ethyl acetate > acetone > DMF > toluene > dichloromethane > THF, which depended on the difference between solvent parameters of solute and solvent. Solubility and metastable zone width were the highest when solubility parameter of solvent was similar to that of C15 sulfone. The wider metastable zone width leaded to the larger crystal size. The higher difference between solubility parameters of C15 sulfone and solvents leaded to the higher aspect ratio of needle-like crystals. Eventually, hexane was an appropriate solvent in cooling crystallization of C15 sulfone.
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