Continuous slug flow crystallization: Impact of design and operating parameters on product quality.

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Title: Continuous slug flow crystallization: Impact of design and operating parameters on product quality.
Authors: Termühlen, Maren (AUTHOR), Etmanski, Matthias Markus (AUTHOR), Kryschewski, Ines (AUTHOR), Kufner, Anne Cathrine (AUTHOR), Schembecker, Gerhard (AUTHOR), Wohlgemuth, Kerstin (AUTHOR) kerstin.wohlgemuth@tu-dortmund.de
Source: Chemical Engineering Research & Design: Transactions of the Institution of Chemical Engineers Part A. Jun2021, Vol. 170, p290-303. 14p.
Subjects: Crystallization, Product quality, Supersaturation, Crystal growth, Particle size distribution, Single crystals, Quality control
Abstract: [Display omitted] • Plug-flow-like RTD for slug flow crystallizer holds for whole operating window. • Innovative cooling concept enables smooth cooling from 50 to 31 ° C. • Reproducible product quality and no fouling by using seed crystals. • Crystal growth of 240 μ m despite residence time of 10 min due to high cooling rate. • Less agglomeration for high volume flow rates. A slug flow crystallizer for cooling crystallization with focus on enhanced product quality control in terms of narrow particle size distribution (PSD) was designed and characterized. Emphasis was put on slug flow stability while maintaining a convex shape of slugs to make use of the advantage of a narrow residence time distribution. Measurements of the latter one showed plug-flow-like behavior for the liquid and solid phase independent of the operating conditions within the range investigated. A tube-in-tube temperature concept led to smooth cooling from 50 to 31 ° C avoiding supersaturation peaks. Seeded cooling crystallization of aqueous l- alanine solution successfully led to reproducible product PSDs avoiding secondary nucleation. Thereby the crystals' median diameter was increased by 240 μ m. Within a residence time of 10.5 min only, a relative process yield of approximately 83% was achieved. To identify optimized operating conditions for narrow PSD and reduced agglomeration, the effect of total volume flow rate, slug length, and cooling rate on the PSD and agglomeration degree was quantified. A high flow rate (40 mL min − 1) and a high cooling rate (3.6 K min − 1) reduced agglomeration to its minimum and shifted the size distribution of single crystals without its broadening by in average 90 μ m. [ABSTRACT FROM AUTHOR]
Copyright of Chemical Engineering Research & Design: Transactions of the Institution of Chemical Engineers Part A is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: Continuous slug flow crystallization: Impact of design and operating parameters on product quality.
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  Data: <searchLink fieldCode="DE" term="%22Crystallization%22">Crystallization</searchLink><br /><searchLink fieldCode="DE" term="%22Product+quality%22">Product quality</searchLink><br /><searchLink fieldCode="DE" term="%22Supersaturation%22">Supersaturation</searchLink><br /><searchLink fieldCode="DE" term="%22Crystal+growth%22">Crystal growth</searchLink><br /><searchLink fieldCode="DE" term="%22Particle+size+distribution%22">Particle size distribution</searchLink><br /><searchLink fieldCode="DE" term="%22Single+crystals%22">Single crystals</searchLink><br /><searchLink fieldCode="DE" term="%22Quality+control%22">Quality control</searchLink>
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  Data: [Display omitted] • Plug-flow-like RTD for slug flow crystallizer holds for whole operating window. • Innovative cooling concept enables smooth cooling from 50 to 31 ° C. • Reproducible product quality and no fouling by using seed crystals. • Crystal growth of 240 μ m despite residence time of 10 min due to high cooling rate. • Less agglomeration for high volume flow rates. A slug flow crystallizer for cooling crystallization with focus on enhanced product quality control in terms of narrow particle size distribution (PSD) was designed and characterized. Emphasis was put on slug flow stability while maintaining a convex shape of slugs to make use of the advantage of a narrow residence time distribution. Measurements of the latter one showed plug-flow-like behavior for the liquid and solid phase independent of the operating conditions within the range investigated. A tube-in-tube temperature concept led to smooth cooling from 50 to 31 ° C avoiding supersaturation peaks. Seeded cooling crystallization of aqueous l- alanine solution successfully led to reproducible product PSDs avoiding secondary nucleation. Thereby the crystals' median diameter was increased by 240 μ m. Within a residence time of 10.5 min only, a relative process yield of approximately 83% was achieved. To identify optimized operating conditions for narrow PSD and reduced agglomeration, the effect of total volume flow rate, slug length, and cooling rate on the PSD and agglomeration degree was quantified. A high flow rate (40 mL min − 1) and a high cooling rate (3.6 K min − 1) reduced agglomeration to its minimum and shifted the size distribution of single crystals without its broadening by in average 90 μ m. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Chemical Engineering Research & Design: Transactions of the Institution of Chemical Engineers Part A is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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RecordInfo BibRecord:
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    Identifiers:
      – Type: doi
        Value: 10.1016/j.cherd.2021.04.006
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      – Code: eng
        Text: English
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      Pagination:
        PageCount: 14
        StartPage: 290
    Subjects:
      – SubjectFull: Crystallization
        Type: general
      – SubjectFull: Product quality
        Type: general
      – SubjectFull: Supersaturation
        Type: general
      – SubjectFull: Crystal growth
        Type: general
      – SubjectFull: Particle size distribution
        Type: general
      – SubjectFull: Single crystals
        Type: general
      – SubjectFull: Quality control
        Type: general
    Titles:
      – TitleFull: Continuous slug flow crystallization: Impact of design and operating parameters on product quality.
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            NameFull: Termühlen, Maren
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            NameFull: Etmanski, Matthias Markus
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            NameFull: Kryschewski, Ines
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            NameFull: Kufner, Anne Cathrine
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            NameFull: Schembecker, Gerhard
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          Dates:
            – D: 01
              M: 06
              Text: Jun2021
              Type: published
              Y: 2021
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              Value: 170
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            – TitleFull: Chemical Engineering Research & Design: Transactions of the Institution of Chemical Engineers Part A
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