Isothermal by Design: An Accelerated Approach to the
Prediction of the Crystallizability of Slowly Nucleating Systems
Version 2 2019-09-06, 23:44
Version 1 2019-08-23, 19:34
Posted on 2019-09-06 - 23:44
A route
to the accelerated nucleation of α-para-aminobenzoic
acid in ethanol/water (EtOH/H2O) mixed solvent
solutions, using antisolvent crystallization, is presented. An isothermal by design approach is adopted, whereby the exothermic
enthalpy of mixing associated with antisolvent addition is offset
by the control of the temperature of the antisolvent added. Induction
times (τ) are found to be reduced by 4 orders of magnitude using
this methodology, consistent with the use of this approach as a nucleation
acceleration technique. Calculation of the nucleation kinetic parameters
for a range of solution concentrations, compositions, and supersaturations
(S) reveal that effective interfacial tensions (γeff) vary from 8.4 to 2.3 mJ m–2 from solutions
in H2O solvent and EtOH solvent, respectively, in line
with the trend in solubility. The critical nucleus radius (r*) decreases from 1.98 to 0.40 nm associated with a decrease
in the number of molecules in the critical nucleus (i*) from 196 to 2 molecules. A change in nucleation mechanism from
heterogeneous nucleation to homogeneous nucleation is observed to
take place at S ≈ 1.5. Limitations, particularly
with focus toward larger-scale operation, are highlighted together
with potential solutions to overcome such aspects.
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Kaskiewicz, Peter
L.; Xu, Guangyi; Lai, Xiaojun; Warren, Nicholas J.; Roberts, Kevin J.; Morton, Colin; et al. (2019). Isothermal by Design: An Accelerated Approach to the
Prediction of the Crystallizability of Slowly Nucleating Systems. ACS Publications. Collection. https://doi.org/10.1021/acs.oprd.9b00242
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AUTHORS (8)
PK
Peter
L. Kaskiewicz
GX
Guangyi Xu
XL
Xiaojun Lai
NW
Nicholas J. Warren
KR
Kevin J. Roberts
CM
Colin Morton
PD
Peter Dowding
NG
Neil George