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Crystals
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Crystallisation Advances
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Crystallisation Advances

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Industrial Crystallization".

Deadline for manuscript submissions: 15 July 2025 | Viewed by 2756

Special Issue Editor

Dr. Kannuchamy Vasanth Kumar

E-Mail Website
Guest Editor
School of Chemistry and Chemical Engineering, University of Surrey, Guildford GU2 7XH, UK
Interests: crystallisation fundamentals; crystal growth; nucleation; solid/liquid adsorption; gas storage/separation; molecular modelling; machine learning
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This Special Issue aims to showcase recent advances in crystallisation, with a strong emphasis on fundamental aspects such as nucleation, crystal growth, and industrial crystallisation. We also welcome contributions that explore advanced microscopy techniques to uncover crystallisation mechanisms during both the crystallisation process and prenucleation stages. Additional topics within the scope include studies on nonclassical crystallisation pathways, the application of process analytical technology (PAT), and the use of chemometric to analyse crystallisation data. Research focusing on the effects of impurities on crystallisation and investigations into continuous crystallisation processes, particularly for organic compounds, are also highly encouraged. This Special Issue seeks to bring together innovative experimental, computational, and theoretical studies that enhance our understanding of crystallisation and its industrial applications.

Dr. Kannuchamy Vasanth Kumar
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. Crystals 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 2100 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

  • nucleation
  • crystal growth
  • industrial crystallisation
  • crystallisation processes

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Published Papers (6 papers)

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Research

24 pages, 3834 KiB  
Article
Energy and Resource Efficient Continuous Cooling Crystallization with Modular Lab-Scale Equipment
by Norbert Kockmann, Mira Schmalenberg, Benedikt Strakeljahn and Kerstin Wohlgemuth
Crystals 2025, 15(5), 421; https://doi.org/10.3390/cryst15050421 - 29 Apr 2025
Viewed by 281
Abstract
Small-scale modular apparatuses in continuously operated plants are promising for current and future production processes in fine and specialty chemistry. Different lab-scale crystallizers have been developed and characterized as part of the ENPRO-TeiA project—separation processes with efficient and intelligent apparatuses. Two research groups [...] Read more.
Small-scale modular apparatuses in continuously operated plants are promising for current and future production processes in fine and specialty chemistry. Different lab-scale crystallizers have been developed and characterized as part of the ENPRO-TeiA project—separation processes with efficient and intelligent apparatuses. Two research groups at TU Dortmund University have investigated four miniaturized crystallization apparatuses for cooling crystallization and characterized them for scaling up to pilot scale with industrial partners. The use in an industrial environment was successfully demonstrated for two types of crystallizers: the stirred tank cascade as well as a draft tube baffle crystallizer. The ENPRO-TeiA project was thus able to prototypically demonstrate the manufacturer-independent investigation and scaling of modular systems for the crystallization step, which is an essential cornerstone for the process development acceleration for sustainable production in the pharmaceutical and chemical industries. Full article
(This article belongs to the Special Issue Crystallisation Advances)
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20 pages, 4096 KiB  
Article
Process Design for Continuous Crystallization of l-Tryptophan in Water–Alcohol Solvent Mixtures
by Lukas Hohmann, Robert Antpusat (née Hampel) and Norbert Kockmann
Crystals 2025, 15(4), 355; https://doi.org/10.3390/cryst15040355 - 12 Apr 2025
Viewed by 436
Abstract
The study of solid–liquid equilibria in small molecules such as l-tryptophan (l-Trp), which possesses an α-amino group, an α-carboxylic acid group, and an indole compound, presents significant challenges. This research introduces several findings aimed at enhancing process efficiency and sustainability [...] Read more.
The study of solid–liquid equilibria in small molecules such as l-tryptophan (l-Trp), which possesses an α-amino group, an α-carboxylic acid group, and an indole compound, presents significant challenges. This research introduces several findings aimed at enhancing process efficiency and sustainability in downstream processing of l-Trp from fermentative origin via crystallization. Transitioning from batch to continuous processes allows for improved scalability and resource management. Furthermore, solubility measurements combined with thermodynamic data from the literature will provide deeper insights into molecular interactions and allow for systematic and data-driven process design. Lab-scale crystallization experiments in both batch and continuous operation allow for the assessment of the process feasibility and solvent impacts on the process and product. The focus is on process development that emphasizes material savings through strategic solvent selection and co-solvent choices. Full article
(This article belongs to the Special Issue Crystallisation Advances)
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14 pages, 1327 KiB  
Article
On the Molecular Kinetics of Protein Crystal Nucleation and the Causes of Its Slowness: Peculiarities of the Protein–Protein Association
by Christo N. Nanev
Crystals 2025, 15(4), 332; https://doi.org/10.3390/cryst15040332 - 31 Mar 2025
Viewed by 269
Abstract
The rate of nucleation of crystals is the subject of extensive research, since it—together with the nucleation time—determines the number of crystals growing; in turn, their number is related to their size. Experimental studies show that, for biomolecular crystals, despite the required unusually [...] Read more.
The rate of nucleation of crystals is the subject of extensive research, since it—together with the nucleation time—determines the number of crystals growing; in turn, their number is related to their size. Experimental studies show that, for biomolecular crystals, despite the required unusually high supersaturations, the nucleation process is distinctly slow. This slowness arises from the inherent peculiarity of the nucleation of such crystals. Therefore, a prerequisite for management of the crystallization process towards the desired outcome is the molecular level understanding of the nucleation mechanism. In this paper, analyzing the mechanisms behind the nucleation process of protein crystals, it is argued that the highly inhomogeneous molecule surface is the main reason for the slow crystal nucleation: only a few small patches on their surface are capable of forming crystalline bonds. Therefore, the partner proteins must not only be brought to encounter one another but must also find each other’s binding site. In turn, this requirement imposes a severe steric restriction on the association of protein molecules, which, however, is alleviated by a rotational-diffusional reorientation. This is why particular attention is paid to this aspect of the protein crystal nucleation process. Full article
(This article belongs to the Special Issue Crystallisation Advances)
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14 pages, 8388 KiB  
Article
Selective Benzene Recognition in Competitive Solvent System (Cyclohexene, Cyclohexane, Tri- and Hexafluorobenzenes) Using Perfluorinated Dinuclear Cu(II) Complex
by Kazuki Shiomoto, Nanako Oimatsu, Satoshi Hirano and Akiko Hori
Crystals 2025, 15(4), 322; https://doi.org/10.3390/cryst15040322 - 28 Mar 2025
Viewed by 287
Abstract
The selective adsorption and separation of benzene from structurally similar six-membered hydrocarbons and fluorocarbons remain a significant challenge due to their comparable physical properties. In this study, we investigated the molecular recognition and separation properties of a perfluorinated triketonate Cu(II) complex (1 [...] Read more.
The selective adsorption and separation of benzene from structurally similar six-membered hydrocarbons and fluorocarbons remain a significant challenge due to their comparable physical properties. In this study, we investigated the molecular recognition and separation properties of a perfluorinated triketonate Cu(II) complex (1) as a Nonporous Adaptive Crystal (NAC). In addition to the previously reported benzene (2)-encapsulated crystal of 1•(2)3, we report here the crystal structures of guest-free 1 and cyclohexene (3)-encapsulated 1•(O)2•3, where (O)2 represents two water molecules. Single-crystal analysis demonstrated that 1 selectively encapsulates 2 while excluding other hydrocarbons, including 3, cyclohexane (4), trifluorobenzene (5), and hexafluorobenzene (6). Gas adsorption experiments confirmed this high affinity for 2, as reflected in its preferential adsorption behavior in mixed solvent and vapor environments. The molecular selectivity of 1 was attributed to strong π-hole···π and metal···π interactions, which favor electron-rich aromatic guests. Additionally, crystallization experiments in competitive solvent systems consistently led to the formation of 1•(2)3, reinforcing the high selectivity of 1 for 2. These findings highlight the unique molecular recognition capabilities of NACs, providing valuable insights into the rational design of advanced molecular separation materials for industrial applications involving aromatic hydrocarbons. Hirshfeld surface analysis revealed that the contribution of F···F interactions to crystal packing decreased upon guest recognition (48.8% in 1, 34.2% in 1•(O)2•3, and 22.2% in 1•(2)3), while the contribution of F···H/H···F interactions increased (8.6% in 1, 22.2% in 1•(O)2•3, and 35.4% in 1•(2)3). Regarding Cu interactions, the self-assembled columnar structure of 1 results in close contacts at the coordination sites, including Cu···Cu (0.1%), Cu···O (0.7%), and Cu···C (1.3%). However, in the guest-incorporated structures 1•(O)2•3 and 1•(2)3, the Cu···Cu contribution disappears; instead, 1•(O)2•3 exhibits a significant increase in Cu···O interactions (1.2%), corresponding to water coordination, while 1•(2)3 shows an increase in Cu···C interactions (1.5%), indicative of the metal···π interactions of benzene. Full article
(This article belongs to the Special Issue Crystallisation Advances)
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13 pages, 2111 KiB  
Article
A Concept Crystal Habit Phase Diagram and Data for Curcumin in Isopropanol: Classical Versus Non-Classical Crystallization
by Mahmoud Ranjbar, Mayank Vashishtha, Gavin Walker and K. Vasanth Kumar
Crystals 2025, 15(4), 296; https://doi.org/10.3390/cryst15040296 - 25 Mar 2025
Viewed by 294
Abstract
Cooling crystallization experiments of curcumin in isopropanol confirmed that curcumin can crystallize via classical or nonclassical pathways, depending on the levels of supersaturation and supercooling. Light microscopy analysis revealed that classical crystallization produces needle-shaped single crystals with an equilibrium habit, while nonclassical crystallization [...] Read more.
Cooling crystallization experiments of curcumin in isopropanol confirmed that curcumin can crystallize via classical or nonclassical pathways, depending on the levels of supersaturation and supercooling. Light microscopy analysis revealed that classical crystallization produces needle-shaped single crystals with an equilibrium habit, while nonclassical crystallization results in spherulitic mesocrystals. Through a series of experiments under various conditions, we developed a crystal habit phase diagram for curcumin in pure isopropanol. Presented here for the first time, this diagram illustrates the relationship between supersaturation, supercooling, and crystal habit, offering a valuable guide for controlling curcumin crystallization pathways. Full article
(This article belongs to the Special Issue Crystallisation Advances)
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12 pages, 7472 KiB  
Article
The Effect of the Film Thickness, Cooling Rate, and Solvent Evaporation on the Formation of L-Menthol Ring-Banded Spherulites
by Tamás Kovács, Tamás Kovács, Jr., Márton Detrich, Ferenc Gazdag, Masaki Itatani and István Lagzi
Crystals 2025, 15(1), 17; https://doi.org/10.3390/cryst15010017 - 27 Dec 2024
Viewed by 926
Abstract
Periodic pattern formation is a prominent phenomenon in chemical, physical, and geochemical systems. This phenomenon can arise from various processes, such as the reaction and mass transport of chemical species, solidification, or solvent evaporation. We investigated the formation of ring-banded spherulites of l [...] Read more.
Periodic pattern formation is a prominent phenomenon in chemical, physical, and geochemical systems. This phenomenon can arise from various processes, such as the reaction and mass transport of chemical species, solidification, or solvent evaporation. We investigated the formation of ring-banded spherulites of l-menthol using a thin liquid film in a Petri dish. We found that the film thickness and cooling rate strongly influence the generation of crystallization patterns. We performed two-dimensional numerical simulations using the Cahn–Hilliard model to support the experimentally observed trend on the dependence of the layer thickness on the periodicity of the generated macroscopic patterns. In a specific scenario, we observed the formation of rings consisting of needle-like crystals on the cover of the Petri dish. This phenomenon was due to the evaporation of the menthol and its subsequent crystallization. In addition to these findings, we created crystallization patterns by solvent evaporation (using tert-butyl alcohol, methyl alcohol, and acetone). Full article
(This article belongs to the Special Issue Crystallisation Advances)
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