Application of on-line Raman spectroscopy on monitoring semi-batch anti-solvent crystallization

作者：Han, Bing; Sha, Zuoliang; Qu, Haiyan; Louhi-Kultanen, Marjatta^*; Wang, Xuekui

来源：CrystEngComm, 2009, 11(5): 827-831.

DOI：10.1039/b817299d

• SYNDIOTACTIC POLYSTYRENE GLASS
• POTASSIUM DIHYDROGEN PHOSPHATE
• PHASE-TRANSFORMATION
• MOLECULAR MECHANISM
• ANHYDRATE/HYDRATE
• POLYMORPHS
• SYSTEMS
• SUPERSATURATION
• SOLUBILITY
• TRANSITION

Anti-solvent crystallization of potassium dihydrogen phosphate (KDP) from aqueous solution was studied by using on-line Raman spectroscopy. The used anti-solvent was acetone and semi-batch crystallization experiments were conducted by adding acetone into an initially pure aqueous KDP solution saturated at 25 degrees C. The solubility of KDP in acetone-water mixtures was determined at 25 degrees C. A calibration model of Raman spectra was created using a series of KDP-water-acetone ternary or binary solutions, and the calibration model was used to attain the on-line KDP concentration profile during the crystallization. The evolution of supersaturation during the whole process was then obtained. The reliability of the calibration model was validated by the off-line measured KDP concentrations. The effects of the feeding rate and feeding position of the anti-solvent on precipitation were discussed based on the obtained supersaturation profile.

• 出版日期2009
• 单位天津科技大学