l脯氨酸抗溶剂对晶体大小和形状的影响.pdf

Available online at Powder Technology 186 (2008) 137 – 144 /locate/powtec Drowning-out crystallization of L-proline: Effect of anti-solvent composition and processing parameters on crystal size and shape Woochan Hyung a , Yehoon Kim a,c , Chan-Hwa Chung b , Seungjoo Haam a,⁎ a Department of Chemical Engineering, Yonsei University, Seoul 120-749, South Korea b Department of Chemical Engineering, Sungkyunkwan University, Suwon 440-746, South Korea c Chemicals Polymers Research and Development, LG Chem Research Park, Daejeon, 305-380, Korea Received 28 March 2006; received in revised form 2 November 2007; accepted 11 November 2007 Available online 17 November 2007 Abstract Crystallization of L-proline was investigated using a drowning-out method. Due to the high water and alcohol solubility of L-proline, the recovery of an L-proline product by precipitation using the drowning-out method required suitable anti-solvents selected from immiscibility and solubility studies. Through past experience, acetone and NMP were carefully chosen for analogy and solubility tests in pure anti-solvent. Although phase separation occurred in acetone, ultrasound was used to mix the two immiscible phases and generate fine emulsion droplets. L-proline crystals were obtained using NMP with a general drowning-out method. A spherical agglomerate of L-proline was also obtained using acetone by emulsion solvent diffusion methods. The ultrasound power controlled the agglomerate sizes, and the agglomerate surface transfo