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Open AccessArticle

Secondary Nucleation Kinetics of AIBN Crystallisation in Methanol: Online Imaging-Based Measurement and Modelling

by Yang Li 1, Yang Zhang 1 and Xue Zhong Wang 2,1,*
1
School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, China
2
Center for Pharmaceutical and Crystallization Process Systems Engineering, Beijing Key Laboratory of Enze Biomass Fine Chemicals, School of Chemical Engineering, Beijing Institute of Petrochemical Technology, Beijing 102617, China
*
Author to whom correspondence should be addressed.
Crystals 2020, 10(6), 506; https://doi.org/10.3390/cryst10060506
Received: 6 May 2020 / Revised: 10 June 2020 / Accepted: 11 June 2020 / Published: 13 June 2020
(This article belongs to the Section Crystal Engineering)
The secondary nucleation process of 2,2-azobisisobutyronitrile (AIBN) seeded crystallisation in methanol in a stirred tank reactor was studied at varying initial supersaturation levels, temperatures, crystal seed numbers, and stirrer speeds. The average secondary nucleation rate, induction time, and agglomeration ratio were measured using on-line microscopic imaging. The initial supersaturation level, temperature, and stirrer speed were found to be positively correlated with the secondary nucleation rate. A small change in the crystal seed number, i.e., 1-20, did not substantially affect the secondary nucleation rate throughout the secondary nucleation process. An increase in the initial supersaturation level and crystal seed number decreased the induction time, and an increase in the strength of agitation promoted the initiation of secondary nucleation at a stirring rate greater than 250 revolutions per minute (rpm). Temperature exerted a complex effect on the induction time. Regarding the agglomeration ratio, the initial supersaturation level positively correlated with the agglomeration ratio, while the stirrer speed negatively correlated with this parameter. Finally, based on the measured data, the average secondary nucleation rate, induction time, and final crystal suspension density were correlated. This study provides guidance for the control of supersaturation, induction time, stirring, and other factors in the crystal seed addition process in AIBN crystallisation. View Full-Text
Keywords: secondary nucleation kinetics; modelling; seeds adding process; on-line imaging; 2,2-azobisisobutyronitrile (AIBN) secondary nucleation kinetics; modelling; seeds adding process; on-line imaging; 2,2-azobisisobutyronitrile (AIBN)
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Li, Y.; Zhang, Y.; Wang, X.Z. Secondary Nucleation Kinetics of AIBN Crystallisation in Methanol: Online Imaging-Based Measurement and Modelling. Crystals 2020, 10, 506.

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