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Crystallization is a phase transformation process in which crystals are precipitated from a supersaturated solution or formed from other sources. During crystallization, atoms or molecules arrange themselves into a well-defined, rigid crystal lattice to minimize energy.
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Key Parameters Impacting the Crystal Formation in Antisolvent Membrane-Assisted Crystallization.

Sara Chergaoui1,2, Damien P Debecker3, Tom Leyssens3

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|February 25, 2023
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Membrane antisolvent crystallization offers consistent crystal size distribution for heat-sensitive compounds. This method controls mass transfer, improving crystal properties compared to traditional techniques.

Keywords:
antisolvent compositionantisolvent crystallizationgravityhydrophobic membranetemperaturevelocity

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Area of Science:

  • Chemical Engineering
  • Crystallization Science
  • Materials Science

Background:

  • Antisolvent crystallization is vital for heat-sensitive compounds like active pharmaceutical ingredients.
  • Membranes enhance control over antisolvent mass transfer, preventing local supersaturation and improving crystal quality.
  • Optimization of operating conditions is crucial for membrane-assisted antisolvent crystallization.

Purpose of the Study:

  • To investigate the impact of solution velocity, antisolvent composition, temperature, and gravity on membrane antisolvent crystallization.
  • To evaluate the effectiveness of polypropylene flat sheet membranes in controlling crystal properties.
  • To establish correlations between operating conditions, transmembrane flux, and crystal characteristics using glycine as a model system.

Main Methods:

  • Utilized glycine-water-ethanol as a model system for antisolvent crystallization.
  • Employed polypropylene flat sheet membranes to control antisolvent addition.
  • Varied operating parameters including solution velocity, antisolvent composition, temperature, and gravity.
  • Analyzed crystal size distribution (CSD), crystal shape, and polymorphic form.

Main Results:

  • Membrane crystallization consistently yielded a narrow CSD (CV 0.5-0.6) compared to batch methods (CV 0.7).
  • Glycine crystal shape was generally maintained, with minor edge smoothing at 35 °C.
  • Mean crystal size (23-40 µm) increased with higher temperature or gravity resistance, correlating with antisolvent transmembrane flux (0.0002-0.001 kg/m²·s).
  • The monoclinic form of α-glycine was preserved under all tested conditions.

Conclusions:

  • Membrane antisolvent crystallization provides a robust method for achieving consistent crystal properties.
  • Optimal operating conditions are key to maximizing the benefits of this technique.
  • The control over mass transfer offered by membranes leads to superior crystal characteristics compared to conventional methods.