The role of residence time distribution in the continuous steady-state mixed suspension mixed product removal crystallization of glycine

Iyke I. Onyemelukwe; Anna R. Parsons; Helen P. Wheatcroft; Amy Robertson; Zoltan K. Nagy; Chris D. Rielly

doi:10.1021/acs.cgd.8b00853

The role of residence time distribution in the continuous steady-state mixed suspension mixed product removal crystallization of glycine

Iyke I. Onyemelukwe^*, Anna R. Parsons, Helen P. Wheatcroft, Amy Robertson, Zoltan K. Nagy, Chris D. Rielly

^*Corresponding author for this work

Strathclyde Institute Of Pharmacy And Biomedical Sciences

Research output: Contribution to journal › Article › peer-review

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Abstract

In this work, a vacuum-driven intermittent transfer technique has been implemented to solve transfer line blockage issues and facilitate steady-state cooling crystallization studies of α-glycine in a single- and two-stage mixed suspension mixed product removal (MSMPR) crystallizer. Experimental residence time distribution (RTD) analysis of the stirred tank MSMPR cascade is performed using an imperfect pulse method of the axial dispersion model to benchmark the mixing performance against that of tubular crystallizers and determine the influence of RTD on steady-state size distribution of α-glycine product. Process analytical technology (PAT) is used to monitor and understand crystallization process dynamics, and the effect of MSMPR operating temperature, mean residence time, and number of MSMPR stages on mean particle size, crystal size distribution, and yield is studied. Results show the significance of nucleation and growth mechanisms alongside RTD in determining steady-state size distribution, and the need for optimum control of supersaturation to benefit from improved RTDs provided by multistage MSMPR crystallizers.

Original language	English
Pages (from-to)	60-80
Number of pages	21
Journal	Crystal Growth and Design
Volume	19
Issue number	1
Early online date	15 Nov 2018
DOIs	https://doi.org/10.1021/acs.cgd.8b00853
Publication status	Published - 2 Jan 2019

Funding

*E-mail: [email protected]. Phone: +44 (0) 7453 322180. *E-mail: [email protected]. Phone: +44 (0) 1509 222504. ORCID Iyke I. Onyemelukwe: 0000-0003-0220-0877 Zoltan K. Nagy: 0000-0003-4787-6678 Funding This work was supported by the EPSRC (EP/I033459/1) Centre for Innovative Manufacturing in Continuous Manufacturing and Crystallization (CMAC) and the Doctoral Training Centre in Continuous Manufacturing and Crystallization (EP/K503289/1). All data created during this research are openly available from the Loughborough University data repository at https://doi.org/10.17028/rd.lboro.6429194. Notes The authors declare no competing financial interest.

Keywords

msmpr
continuous oscillatory baffled crystallizer
process analytical technology

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Onyemelukwe-etal-CGD-2019-The-role-of-residence-time-distribution-in-the-continuousAccepted author manuscript, 2.35 MB

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abstract = "In this work, a vacuum-driven intermittent transfer technique has been implemented to solve transfer line blockage issues and facilitate steady-state cooling crystallization studies of α-glycine in a single- and two-stage mixed suspension mixed product removal (MSMPR) crystallizer. Experimental residence time distribution (RTD) analysis of the stirred tank MSMPR cascade is performed using an imperfect pulse method of the axial dispersion model to benchmark the mixing performance against that of tubular crystallizers and determine the influence of RTD on steady-state size distribution of α-glycine product. Process analytical technology (PAT) is used to monitor and understand crystallization process dynamics, and the effect of MSMPR operating temperature, mean residence time, and number of MSMPR stages on mean particle size, crystal size distribution, and yield is studied. Results show the significance of nucleation and growth mechanisms alongside RTD in determining steady-state size distribution, and the need for optimum control of supersaturation to benefit from improved RTDs provided by multistage MSMPR crystallizers.",

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AU - Parsons, Anna R.

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AU - Robertson, Amy

AU - Nagy, Zoltan K.

AU - Rielly, Chris D.

PY - 2019/1/2

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N2 - In this work, a vacuum-driven intermittent transfer technique has been implemented to solve transfer line blockage issues and facilitate steady-state cooling crystallization studies of α-glycine in a single- and two-stage mixed suspension mixed product removal (MSMPR) crystallizer. Experimental residence time distribution (RTD) analysis of the stirred tank MSMPR cascade is performed using an imperfect pulse method of the axial dispersion model to benchmark the mixing performance against that of tubular crystallizers and determine the influence of RTD on steady-state size distribution of α-glycine product. Process analytical technology (PAT) is used to monitor and understand crystallization process dynamics, and the effect of MSMPR operating temperature, mean residence time, and number of MSMPR stages on mean particle size, crystal size distribution, and yield is studied. Results show the significance of nucleation and growth mechanisms alongside RTD in determining steady-state size distribution, and the need for optimum control of supersaturation to benefit from improved RTDs provided by multistage MSMPR crystallizers.

AB - In this work, a vacuum-driven intermittent transfer technique has been implemented to solve transfer line blockage issues and facilitate steady-state cooling crystallization studies of α-glycine in a single- and two-stage mixed suspension mixed product removal (MSMPR) crystallizer. Experimental residence time distribution (RTD) analysis of the stirred tank MSMPR cascade is performed using an imperfect pulse method of the axial dispersion model to benchmark the mixing performance against that of tubular crystallizers and determine the influence of RTD on steady-state size distribution of α-glycine product. Process analytical technology (PAT) is used to monitor and understand crystallization process dynamics, and the effect of MSMPR operating temperature, mean residence time, and number of MSMPR stages on mean particle size, crystal size distribution, and yield is studied. Results show the significance of nucleation and growth mechanisms alongside RTD in determining steady-state size distribution, and the need for optimum control of supersaturation to benefit from improved RTDs provided by multistage MSMPR crystallizers.

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The role of residence time distribution in the continuous steady-state mixed suspension mixed product removal crystallization of glycine

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