Abstract
In this study, we report on experiments designed to deconvolute the particle breakage kinetics and mechanism from the parallel phenomena (growth-dissolution, agglomeration) in attrition-enhanced deracemization processes. Through such experiments, we derived the specific breakage rates and cumulative breakage distribution functions for three grinding methods typically used in deracemization experiments: (a) bead grinding, (b) ultrasound grinding, and (c) the combination of bead and ultrasound grinding. Subsequently, we tested these methods on their ability to induce deracemization. We show that in the conventional bead grinding process, breakage occurs mostly by fracture. This results in slow deracemization rates due to the delayed formation of submicron particles that are essential to the process. Conversely, ultrasound grinding very efficiently breaks particles by abrasion. This leads to fast generation of an abundance of submicron fragments resulting in fast deracemization. However, using ultrasound, large crystals fracture rates are an order of magnitude lower than those using bead grinding, which results in an insufficient size decrease of the large counter enantiomer crystals and eventually to incomplete deracemization. Remarkably, the simultaneous application of bead and ultrasound grinding leads, due to synergistic effects of both fracture and abrasion, to 2-fold higher total deracemization rates compared to bead grinding alone. The present work offers new insights into the key role of particle breakage in attrition-enhanced deracemization, together with a basis for decoupling the individual phenomena involved in the process.
| Language | English |
|---|---|
| Pages | 3051-3061 |
| Number of pages | 11 |
| Journal | Crystal Growth and Design |
| Volume | 18 |
| Issue number | 5 |
| Early online date | 28 Mar 2018 |
| DOIs | |
| Publication status | Published - 2 May 2018 |
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Keywords
- deracemization
- Viedma ripening
- particle breakage
- bead grinding
- ultrasound grinding
- abrasion
- fracture
- sodium chlorate
Cite this
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Particle breakage kinetics and mechanisms in attrition-enhanced deracemization. / Xiouras, Christos; Fytopoulos, Antonios A.; Ter Horst, Joop H.; Boudouvis, Andreas G.; Van Gerven, Tom; Stefanidis, Georgios D.
In: Crystal Growth and Design, Vol. 18, No. 5, 02.05.2018, p. 3051-3061.Research output: Contribution to journal › Article
TY - JOUR
T1 - Particle breakage kinetics and mechanisms in attrition-enhanced deracemization
AU - Xiouras, Christos
AU - Fytopoulos, Antonios A.
AU - Ter Horst, Joop H.
AU - Boudouvis, Andreas G.
AU - Van Gerven, Tom
AU - Stefanidis, Georgios D.
N1 - This document is the Accepted Manuscript version of a Published Work that appeared in final form in Crustal Growth and Design, copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see hrrps://doi.org/10.1021/acs.cgd.8b00201.
PY - 2018/5/2
Y1 - 2018/5/2
N2 - In this study, we report on experiments designed to deconvolute the particle breakage kinetics and mechanism from the parallel phenomena (growth-dissolution, agglomeration) in attrition-enhanced deracemization processes. Through such experiments, we derived the specific breakage rates and cumulative breakage distribution functions for three grinding methods typically used in deracemization experiments: (a) bead grinding, (b) ultrasound grinding, and (c) the combination of bead and ultrasound grinding. Subsequently, we tested these methods on their ability to induce deracemization. We show that in the conventional bead grinding process, breakage occurs mostly by fracture. This results in slow deracemization rates due to the delayed formation of submicron particles that are essential to the process. Conversely, ultrasound grinding very efficiently breaks particles by abrasion. This leads to fast generation of an abundance of submicron fragments resulting in fast deracemization. However, using ultrasound, large crystals fracture rates are an order of magnitude lower than those using bead grinding, which results in an insufficient size decrease of the large counter enantiomer crystals and eventually to incomplete deracemization. Remarkably, the simultaneous application of bead and ultrasound grinding leads, due to synergistic effects of both fracture and abrasion, to 2-fold higher total deracemization rates compared to bead grinding alone. The present work offers new insights into the key role of particle breakage in attrition-enhanced deracemization, together with a basis for decoupling the individual phenomena involved in the process.
AB - In this study, we report on experiments designed to deconvolute the particle breakage kinetics and mechanism from the parallel phenomena (growth-dissolution, agglomeration) in attrition-enhanced deracemization processes. Through such experiments, we derived the specific breakage rates and cumulative breakage distribution functions for three grinding methods typically used in deracemization experiments: (a) bead grinding, (b) ultrasound grinding, and (c) the combination of bead and ultrasound grinding. Subsequently, we tested these methods on their ability to induce deracemization. We show that in the conventional bead grinding process, breakage occurs mostly by fracture. This results in slow deracemization rates due to the delayed formation of submicron particles that are essential to the process. Conversely, ultrasound grinding very efficiently breaks particles by abrasion. This leads to fast generation of an abundance of submicron fragments resulting in fast deracemization. However, using ultrasound, large crystals fracture rates are an order of magnitude lower than those using bead grinding, which results in an insufficient size decrease of the large counter enantiomer crystals and eventually to incomplete deracemization. Remarkably, the simultaneous application of bead and ultrasound grinding leads, due to synergistic effects of both fracture and abrasion, to 2-fold higher total deracemization rates compared to bead grinding alone. The present work offers new insights into the key role of particle breakage in attrition-enhanced deracemization, together with a basis for decoupling the individual phenomena involved in the process.
KW - deracemization
KW - Viedma ripening
KW - particle breakage
KW - bead grinding
KW - ultrasound grinding
KW - abrasion
KW - fracture
KW - sodium chlorate
UR - http://www.scopus.com/inward/record.url?scp=85046354261&partnerID=8YFLogxK
UR - https://pubs.acs.org/journal/cgdefu
U2 - 10.1021/acs.cgd.8b00201
DO - 10.1021/acs.cgd.8b00201
M3 - Article
VL - 18
SP - 3051
EP - 3061
JO - Crystal Growth and Design
T2 - Crystal Growth and Design
JF - Crystal Growth and Design
SN - 1528-7483
IS - 5
ER -