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This project has received funding from the European Union’s Horizon 2020
research and innovation programme under grant agreement No 869993.
Introduction to
crystallization
Crystallization
• In the crystallization process,
atoms, ions or molecules
are arranged into rigid
crystals from gas, melt, or
most commonly, from
solution.
• Crystallization is a widely
used separation and
purification technique in
industry.
• Crystallization occurs also in
nature, e.g. in formation of
ice crystals or salt. Crystallized salt along the Dead sea coast. (Pixabay)
Various crystals
Steps of the crystallization process
• Crystallization requires a
supersaturated solution. There are
different methods to achieve the
supersaturation.
• In the supersaturated solution, the
nucleation may take place. Some
seed crystals are usually needed to
initiate the nucleation process. Nuclei
are like little baby crystals.
• When stable nuclei are formed, they
begin to grow into crystals.
Supersaturation
• Most solids are more suluble at
higher temperatures. When you have
a saturated solution and then cool it
down, you will get a supersaturated
solution.
• If the solubility does not vary with
temperature, the concentration can
be increased by evaporation.
• Other methods for supersaturation
are anti-solvent addition and
precipitation.
The solubility of sucrose increases strongly
with temperature.
Nucleation
• The process in which nuclei start to form in
supersaturated solution, is called nucleation.
• If the solution is supersaturated enough,
nucleation might start spontaneously.
(Primary, homogeneous nucleation)
• Sometimes nuclei are generated by crystals
existing in the supersaturated solution.
(Secondary nucleation)
• Nuclei may also occur on the surface of the
vessel or on some impurities in the system.
(Primary, heterogeneous nucleation)
Crystal growth
• When stable nuclei have formed, they begin
to grow into crystals.
• At the same time, the concentration of the
solution reduces, because the particles of
the substance are attached onto the
crystals.
• The crystal growth may go on until the
saturation point of the solution is reached.
Then the solution is not supersaturated any
more. In practice, the crystal growth ends
before the saturation point is reached.
Filtration, washing and drying
• At the end of the crystal growth, crystals must
be separated from the mother liquid.
• After filtration, crystals are usually washed.
• Crystals should be insoluble in the wash
liquid and the wash liquid should be miscible
in the original solvent and also reasonably
volatile for rapid drying.
• The main objective of these final steps is to
minimize crystal changes.
• Sometimes the mother liquid is the desired
product of the crystallization process.
Objectives
• The crystallization process can be
modified with various techiques.
• Typical objectives are:
• high yield
• narrow crystal size distribution
• maximum crystal purity
• specific crystal morphology
• economic and trouble-free process
• The choices between different
alternatives are usually compromises.
This project has received funding from the European Union’s Horizon 2020
research and innovation programme under grant agreement No 869993.
References
Beckmann, W (ed.) 2013. Crystallization: Basic Concepts and Industrial Applications. Weinheim:
Wiley‐VCH Verlag GmbH & Co. KGaA. pp. 1-5.
Hipple, J. 2017. Chemical Engineering for Non‐Chemical Engineers. Hoboken, New Jersey: John
Wiley & Sons, Inc. pp. 209-216.
Mullin, J. W. 2001. Crystallization. Oxford: Elsevier Science & Technology. pp. 181, 216, 244.
Videos:
• What is crystallization? https://youtu.be/xzCF_IHWRXg
• Grow crystals from sugar: https://youtu.be/Vp7cWycX35w
• Beauty of crystallization: https://youtu.be/lo0cp2uhxb0

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Introduction to crystallization

  • 1. This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No 869993. Introduction to crystallization
  • 2. Crystallization • In the crystallization process, atoms, ions or molecules are arranged into rigid crystals from gas, melt, or most commonly, from solution. • Crystallization is a widely used separation and purification technique in industry. • Crystallization occurs also in nature, e.g. in formation of ice crystals or salt. Crystallized salt along the Dead sea coast. (Pixabay)
  • 4. Steps of the crystallization process • Crystallization requires a supersaturated solution. There are different methods to achieve the supersaturation. • In the supersaturated solution, the nucleation may take place. Some seed crystals are usually needed to initiate the nucleation process. Nuclei are like little baby crystals. • When stable nuclei are formed, they begin to grow into crystals.
  • 5. Supersaturation • Most solids are more suluble at higher temperatures. When you have a saturated solution and then cool it down, you will get a supersaturated solution. • If the solubility does not vary with temperature, the concentration can be increased by evaporation. • Other methods for supersaturation are anti-solvent addition and precipitation. The solubility of sucrose increases strongly with temperature.
  • 6. Nucleation • The process in which nuclei start to form in supersaturated solution, is called nucleation. • If the solution is supersaturated enough, nucleation might start spontaneously. (Primary, homogeneous nucleation) • Sometimes nuclei are generated by crystals existing in the supersaturated solution. (Secondary nucleation) • Nuclei may also occur on the surface of the vessel or on some impurities in the system. (Primary, heterogeneous nucleation)
  • 7. Crystal growth • When stable nuclei have formed, they begin to grow into crystals. • At the same time, the concentration of the solution reduces, because the particles of the substance are attached onto the crystals. • The crystal growth may go on until the saturation point of the solution is reached. Then the solution is not supersaturated any more. In practice, the crystal growth ends before the saturation point is reached.
  • 8. Filtration, washing and drying • At the end of the crystal growth, crystals must be separated from the mother liquid. • After filtration, crystals are usually washed. • Crystals should be insoluble in the wash liquid and the wash liquid should be miscible in the original solvent and also reasonably volatile for rapid drying. • The main objective of these final steps is to minimize crystal changes. • Sometimes the mother liquid is the desired product of the crystallization process.
  • 9. Objectives • The crystallization process can be modified with various techiques. • Typical objectives are: • high yield • narrow crystal size distribution • maximum crystal purity • specific crystal morphology • economic and trouble-free process • The choices between different alternatives are usually compromises.
  • 10. This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No 869993. References Beckmann, W (ed.) 2013. Crystallization: Basic Concepts and Industrial Applications. Weinheim: Wiley‐VCH Verlag GmbH & Co. KGaA. pp. 1-5. Hipple, J. 2017. Chemical Engineering for Non‐Chemical Engineers. Hoboken, New Jersey: John Wiley & Sons, Inc. pp. 209-216. Mullin, J. W. 2001. Crystallization. Oxford: Elsevier Science & Technology. pp. 181, 216, 244. Videos: • What is crystallization? https://youtu.be/xzCF_IHWRXg • Grow crystals from sugar: https://youtu.be/Vp7cWycX35w • Beauty of crystallization: https://youtu.be/lo0cp2uhxb0