Abstract
In this study, the selective crystallization and characterization of the stoichiometric forms of the p-toluenesulfonamide/triphenylphosphine oxide (p-TSA-TPPO) co-crystal system in acetonitrile (MeCN) is demonstrated using batch and semi-batch crystallizers. In the batch study, both 1:1 and 3:2 p-TSA-TPPO were successfully isolated as pure forms. However, process variability was observed in a few experimental runs. To address the batch process variability issue, a control strategy was implemented using temperature cycling, aided by in situ process analytical technologies (PAT) to convert from 3:2 to 1:1 p-TSA-TPPO. In the semi-batch co-crystallization studies, the two molecular co-formers, p-TSA and TPPO, were dissolved in MeCN and pumped separately to the crystallizer. Changing the flow rates of the respective active ingredients allowed control over the co-crystallization outcome, and presents as a promising opportunity for development of a continuous co-crystallization process.
| Language | English |
|---|---|
| Pages | 95-108 |
| Number of pages | 14 |
| Journal | Chemical Engineering Science |
| Volume | 152 |
| Early online date | 3 Jun 2016 |
| DOIs | |
| Publication status | Published - 2 Oct 2016 |
Fingerprint
Keywords
- co-crystal
- co-crystallization
- process analytical technologies
- stoichiometric
Cite this
}
PAT-based design of agrochemical co-crystallization processes : a case-study for the selective crystallization of 1:1 and 3:2 co-crystals of p-toluenesulfonamide/triphenylphosphine oxide. / Powell, K.A.; Croker, D.M.; Rielly, C.D.; Nagy, Z.K.
In: Chemical Engineering Science, Vol. 152, 02.10.2016, p. 95-108.Research output: Contribution to journal › Article
TY - JOUR
T1 - PAT-based design of agrochemical co-crystallization processes
T2 - Chemical Engineering Science
AU - Powell, K.A.
AU - Croker, D.M.
AU - Rielly, C.D.
AU - Nagy, Z.K.
PY - 2016/10/2
Y1 - 2016/10/2
N2 - In this study, the selective crystallization and characterization of the stoichiometric forms of the p-toluenesulfonamide/triphenylphosphine oxide (p-TSA-TPPO) co-crystal system in acetonitrile (MeCN) is demonstrated using batch and semi-batch crystallizers. In the batch study, both 1:1 and 3:2 p-TSA-TPPO were successfully isolated as pure forms. However, process variability was observed in a few experimental runs. To address the batch process variability issue, a control strategy was implemented using temperature cycling, aided by in situ process analytical technologies (PAT) to convert from 3:2 to 1:1 p-TSA-TPPO. In the semi-batch co-crystallization studies, the two molecular co-formers, p-TSA and TPPO, were dissolved in MeCN and pumped separately to the crystallizer. Changing the flow rates of the respective active ingredients allowed control over the co-crystallization outcome, and presents as a promising opportunity for development of a continuous co-crystallization process.
AB - In this study, the selective crystallization and characterization of the stoichiometric forms of the p-toluenesulfonamide/triphenylphosphine oxide (p-TSA-TPPO) co-crystal system in acetonitrile (MeCN) is demonstrated using batch and semi-batch crystallizers. In the batch study, both 1:1 and 3:2 p-TSA-TPPO were successfully isolated as pure forms. However, process variability was observed in a few experimental runs. To address the batch process variability issue, a control strategy was implemented using temperature cycling, aided by in situ process analytical technologies (PAT) to convert from 3:2 to 1:1 p-TSA-TPPO. In the semi-batch co-crystallization studies, the two molecular co-formers, p-TSA and TPPO, were dissolved in MeCN and pumped separately to the crystallizer. Changing the flow rates of the respective active ingredients allowed control over the co-crystallization outcome, and presents as a promising opportunity for development of a continuous co-crystallization process.
KW - co-crystal
KW - co-crystallization
KW - process analytical technologies
KW - stoichiometric
UR - http://www.scopus.com/inward/record.url?scp=84973321154&partnerID=8YFLogxK
UR - http://www.sciencedirect.com/science/journal/00092509
U2 - 10.1016/j.ces.2016.06.005
DO - 10.1016/j.ces.2016.06.005
M3 - Article
VL - 152
SP - 95
EP - 108
JO - Chemical Engineering Science
JF - Chemical Engineering Science
SN - 0009-2509
ER -