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Processes
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Continuous Crystallization Processes and Product Design
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Continuous Crystallization Processes and Product Design

A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Chemical Processes and Systems".

Deadline for manuscript submissions: closed (31 March 2022) | Viewed by 9892

Special Issue Editor

Dr. Kerstin Wohlgemuth

E-Mail Website
Guest Editor
Laboratory of Plant and Process Design, Department of Biochemical and Chemical Engineering, TU Dortmund University, 44227 Dortmund, Germany
Interests: small scale continuous crystallization; gassing crystallization; product design; agglomeration processes; image analysis using artificial intelligence

Special Issue Information

Dear Colleagues,

Crystal product design is a very complex task in the field of fine chemical and pharmaceutical industry. The complexity is a consequence of several process steps, which are involved, starting from the target compound in solution ending with the final solid product with desired quality, in combination with the nature of the processed material. In all these process steps operating parameters chosen affect the quality attributes, like particle size distribution and depend strongly on the physicochemical properties of the material system used. Therefore, key for reliable product design of crystalline solids is a deeper process understanding covering all these process steps.

Continuous crystallization is in focus in recent years to overcome the bottleneck in the fully continuous production process for high efficient operation. But, there is a lack of reliable equipment and online analysis techniques for small-scale continuous crystallization and subsequent downstream steps like solid-liquid separation and drying, which are needed in the field of pharmaceuticals and fine chemicals.

This special issue on "Continuous Crystallization and Product Design" aims to bring together new advances in the development and application of small-scale continuous crystallization, solid-liquid separation and drying to overcome the long-standing challenges of fully continuous production of pharmaceuticals and fine chemicals. The topics include, but are not limited to:

  • Advances in fundamental knowledge for process understanding
  • new equipment and use of existing equipment on new products
  • continuous nucleation methods
  • online process analysis technologies (PAT)
  • modelling and simulation of continuous processes

Dr. Kerstin Wohlgemuth
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Processes is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • crystallization
  • solid-liquid separation
  • drying
  • process understanding
  • agglomeration
  • modelling
  • PAT
  • nucleation

Published Papers (3 papers)

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Research

14 pages, 4405 KiB  
Article
Continuous Crystallization Using Ultrasound Assisted Nucleation, Cubic Cooling Profiles and Oscillatory Flow
by Arne Vancleef, Ward De Beuckeleer, Tom Van Gerven, Leen C. J. Thomassen and Leen Braeken
Processes 2021, 9(12), 2268; https://0-doi-org.brum.beds.ac.uk/10.3390/pr9122268 - 17 Dec 2021
Cited by 2 | Viewed by 2966
Abstract
Continuous tubular crystallizers have the potential to reduce manufacturing costs and increase product quality. However, designing tubular crystallizers is a complex and challenging task as crystallization is a complex, multiphase process with a propensity for fouling and clogging. While several designs have been [...] Read more.
Continuous tubular crystallizers have the potential to reduce manufacturing costs and increase product quality. However, designing tubular crystallizers is a complex and challenging task as crystallization is a complex, multiphase process with a propensity for fouling and clogging. While several designs have been proposed to overcome these issues, these designs are either unproven or poorly scalable and complex. In this work a continuous crystallizer is designed and evaluated to mitigate these issues. The tubular crystallizer combines a novel method to obtain a cubic cooling profile to control the supersaturation, ultrasound to induce nucleation and oscillatory flow to improve mixing and minimize fouling and sedimentation. The results show that the crystallizer was able to operate for more than 4 h without clogging, with high yields and a narrow particle size distribution. The design proposed here is therefore considered a viable approach for continuous crystallizers. Full article
(This article belongs to the Special Issue Continuous Crystallization Processes and Product Design)
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17 pages, 3393 KiB  
Article
Towards Continuous Primary Manufacturing Processes—Particle Design through Combined Crystallization and Particle Isolation
by Claas Steenweg, Anne Cathrine Kufner, Jonas Habicht and Kerstin Wohlgemuth
Processes 2021, 9(12), 2187; https://0-doi-org.brum.beds.ac.uk/10.3390/pr9122187 - 03 Dec 2021
Cited by 9 | Viewed by 2766
Abstract
Integrated continuous manufacturing processes of active pharmaceutical ingredients (API) provide key benefits concerning product quality control, scale-up capability, and a reduced time-to-market. Thereby, the crystallization step, which is used in approximately 90% of API productions, mainly defines the final API properties. This study [...] Read more.
Integrated continuous manufacturing processes of active pharmaceutical ingredients (API) provide key benefits concerning product quality control, scale-up capability, and a reduced time-to-market. Thereby, the crystallization step, which is used in approximately 90% of API productions, mainly defines the final API properties. This study focuses on the design and operation of an integrated small-scale process combining a continuous slug flow crystallizer (SFC) with continuous particle isolation using the modular continuous vacuum screw filter (CVSF). By selective adjustment of supersaturation and undersaturation, the otherwise usual blocking could be successfully avoided in both apparatuses. It was shown that, during crystallization in an SFC, a significant crystal growth of particles (Δd50,3≈ 220 µm) is achieved, and that, during product isolation in the CVSF, the overall particle size distribution (PSD) is maintained. The residual moistures for the integrated process ranged around 2% during all experiments performed, ensuring free-flowing particles at the CVSF outlet. In summary, the integrated setup offers unique features, such as its enhanced product quality control and fast start-up behavior, providing a promising concept for integrated continuous primary manufacturing processes of APIs. Full article
(This article belongs to the Special Issue Continuous Crystallization Processes and Product Design)
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36 pages, 7962 KiB  
Article
Continuous Cooling Crystallization in a Coiled Flow Inverter Crystallizer Technology—Design, Characterization, and Hurdles
by Mira Schmalenberg, Stephanie Kreis, Lena K. Weick, Christian Haas, Fabian Sallamon and Norbert Kockmann
Processes 2021, 9(9), 1537; https://0-doi-org.brum.beds.ac.uk/10.3390/pr9091537 - 29 Aug 2021
Cited by 10 | Viewed by 3191
Abstract
Continuous small-scale production is currently of utmost interest for fine chemicals and pharmaceuticals. For this purpose, equipment and process concepts in consideration of the hurdles for solids handling are required to transfer conventional batch processing to continuous operation. Based on empirical equations, pressure [...] Read more.
Continuous small-scale production is currently of utmost interest for fine chemicals and pharmaceuticals. For this purpose, equipment and process concepts in consideration of the hurdles for solids handling are required to transfer conventional batch processing to continuous operation. Based on empirical equations, pressure loss constraints, and an expandable modular system, a coiled flow inverter (CFI) crystallizer with an inner diameter of 1.6 mm was designed. It was characterized concerning its residence time behavior, tested for operation with seed crystals or an ultrasonic seed crystal unit, and evaluated for different purging mechanisms for stable operation. The residence time behavior in the CFI corresponds to ideal plug flow behavior. Crystal growth using seed crystals was demonstrated in the CFI for two amino acids. For fewer seed crystals, higher crystal growth rates were determined, while at the same time, secondary nucleation was observed. Feasibility for the interconnection of a sonicated seeding crystal unit could be shown. However, the hurdles are also identified and discussed. Prophylactic flushing combined with a photosensor for distinguishing between solvent and suspension phase can lead to stable and resource-efficient operation. The small-scale CFI technology was investigated in detail, and the limits and opportunities of the technology are presented here. Full article
(This article belongs to the Special Issue Continuous Crystallization Processes and Product Design)
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