Drowning-out crystallization of l-proline

Effect of anti-solvent composition and processing parameters on crystal size and shape

Woochan Hyung, Yehoon Kim, Chan Hwa Chung, Seungjoo Haam

Research output: Contribution to journalArticle

10 Citations (Scopus)

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 transformed from amorphous to crystalline as the residence time increased. Alternatively, when NMP was used as an anti-solvent, l-proline monocrystals with needle type morphology were produced.

Original languageEnglish
Pages (from-to)137-144
Number of pages8
JournalPowder Technology
Volume186
Issue number2
DOIs
Publication statusPublished - 2008 Aug 11

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Crystallization
Proline
Solubility
Acetone
Crystals
Processing
Chemical analysis
Emulsions
Ultrasonics
Phase separation
Needles
Alcohols
Crystalline materials
Recovery
Water

All Science Journal Classification (ASJC) codes

  • Chemical Engineering(all)

Cite this

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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 transformed from amorphous to crystalline as the residence time increased. Alternatively, when NMP was used as an anti-solvent, l-proline monocrystals with needle type morphology were produced.",
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Drowning-out crystallization of l-proline : Effect of anti-solvent composition and processing parameters on crystal size and shape. / Hyung, Woochan; Kim, Yehoon; Chung, Chan Hwa; Haam, Seungjoo.

In: Powder Technology, Vol. 186, No. 2, 11.08.2008, p. 137-144.

Research output: Contribution to journalArticle

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