Primary Nucleation of Benzoic Acid in Aqueous Ethanol Solution

Zhao, Yan; Hou, Guangyang; Kamaraju, Vamsi Krishna; He, Yunliang; Power, G.; Glennon, Brian

doi:10.1021/acs.iecr.9b05640

Cited by 14 publications

(16 citation statements)

References 41 publications

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“…40 As described in previous publication, when the water composition in solvent mixture was increased from 0.60 to 0.75, the interfacial energy also increased from 1.83 to 6.46 mJ/m 2 . 25 Thus, the decrease in water composition contributes to the occurrence of primary nucleation, resulting in a wider MSZW. 4a) showed that no significant change of CLDs was observed.…”

Section: Resultsmentioning

confidence: 99%

“…Both the probes were inserted into the crystallizer, located 19 mm above the impeller. 21,25 Figure 1 presents a set of typical ATR-FTIR spectra of benzoic acid in ethanol−water solution with different concentrations. It is clear that the peak heights at wavenumbers around 1275 and 1455 cm −1 increase with increasing concentration, where the concentration of the black line is the highest and the purple line corresponds to the lowest concentration.…”

Section: Methodsmentioning

confidence: 99%

“…The FBRM probe was employed to monitor the evolution of chord length distribution (CLD) of crystals, and the ATR-FTIR probe was used to monitor the concentration decay of the liquid phase during the crystal growth experiments. Both the probes were inserted into the crystallizer, located 19 mm above the impeller. , …”

Section: Methodsmentioning

confidence: 99%

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Crystal Growth Kinetics of Benzoic Acid in Aqueous Ethanol Solution

Zhao

Cui

Liu

et al. 2021

Ind. Eng. Chem. Res.

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Crystallization is one of the most important operations in the manufacturing of active pharmaceutical ingredients, where crystal growth is of vital importance for the final particle properties. The crystal growth kinetics of benzoic acid in antisolvent crystallization has been investigated by isothermal seeded desupersaturation experiments, applying the process analytical technology (PAT) tools and population balance modeling. The population balance equation (PBE) model selection incorporating different supersaturation expressions, growth rate expressions together with the solvent compositions was explored by fitting to corresponding concentration data sets. The results demonstrated that growth rate parameters depend heavily on solvent compositions. Therefore, a size-independent growth rate model concerning the effect of solvent compositions demonstrated the best fitness with respect to objective function values and confidence intervals. The estimated parameters with the corresponding model were consequently validated experimentally, demonstrating reasonable agreements with experimental concentrations, which illustrates the potential of the developed model in further experimental design and control.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

See 1 more Smart Citation

Crystal Growth Kinetics of Benzoic Acid in Aqueous Ethanol Solution

Zhao

Cui

Liu

et al. 2021

Ind. Eng. Chem. Res.

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“…Wang experimentally determined the MSZW of adipic acid in different polar solvents and confirmed the link between interfacial energy and the nucleation driving force [14]. Antisolvent crystallization is widely used in crystallization processes, and the effect of mixed solvents on solute nucleation has been reported, but most studies are based on the induction period method [15]. There are a few reports on the nucleation kinetics of mixed-solvent systems using the method of determining MSZW.…”

Section: Introductionmentioning

confidence: 90%

Insight into the Nucleation Mechanism of p-Methoxybenzoic Acid in Ethanol-Water System from Metastable Zone Width

et al. 2022

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The metastable zone width (MSZW) of p-methoxybenzoic acid (PMBA) in an ethanol-water system was measured using the polythermal method. The nucleation order m obtained by the Nývlt’s model indicates the nucleation of PMBA following a progressive nucleation mechanism at low saturation temperature (m = 3.18–7.50) and an instantaneous nucleation mechanism at high saturation temperature (m = 1.46–2.55). Then, combined with the metastable zone experiment and the Sangwal model, we found that the MSZW and the interfacial energy reached the maximum when the mass fraction of ethanol was 0.8, which resulted in the smallest crystal product size. Meanwhile, the maximum and obtained based on the modified Sangwal model indicating the PMBA needs to overcome a higher nucleation barrier in the ethanol mass fraction of 0.8. Finally, we proposed a preferential strategy for adjusting MSZW by correlating the interfacial energy with the change in ethanol mass fraction, saturation temperature, and cooling rate, respectively.

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“…In practice, in the presence of foreign particles, the effective interfacial energy (γ het ) can be derived from γ hom for a pure homogeneous process as 31 Furthermore, the radius of critical nuclei ( r het crit ) as well as the number of molecules in them ( n het crit ) are calculated by 33 , 34 The J het can be finally expressed as 29 , 35 Here, m refers to the molecular mass of solute; meanwhile, ρ stands for the number of solute molecules in one volume of nucleating solution.…”

Section: Classical Heterogeneous Nucleation Theory (Chnt)mentioning

confidence: 99%

Direct Crystallization Resolution of Racemates Enhanced by Chiral Nanorods: Experimental, Statistical, and Quantum Mechanics/Molecular Dynamics Simulation Studies

Cao

Lou

et al. 2022

ACS Omega

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Three chiral nanorods of C 14 - l -Thea, C 14 - l -Phe, and C 14 - d -Phe were first synthesized and utilized as heterogeneous nucleants to enhance the resolution of racemic Asp via direct crystallization. Through the statistical analysis from 320 batches of nucleation experiments, we found that the apparent appearance diversity of two enantiomeric crystals of Asp existed in 80 homogeneous experiments without chiral nanorods. However, in 240 heterogeneous experiments with 4.0 wt % chiral nanorods of solute mass added, the appearance of those nuclei with the same chirality as the nanorods was apparently promoted, and that with the opposite chirality was totally inhibited. Under a supersaturation level of 1.08, the maximum ee of the initial nuclei was as high as 23.51%. When the cooling rate was 0.025 K/min, the ee of the product was up to 76.85% with a yield of 14.41%. Furthermore, the simulation results from quantum mechanics (QM) and molecular dynamics (MD) revealed that the higher chiral recognition ability of C 14 - l -Thea compared to C 14 - l -Phe that originated from the interaction difference between C 14 - l -Thea and Asp enantiomers was larger than that between C 14 - l -Phe and Asp enantiomers. Moreover, the constructed nanorods exhibited good stability and recyclability.

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Primary Nucleation of Benzoic Acid in Aqueous Ethanol Solution

Cited by 14 publications

References 41 publications

Crystal Growth Kinetics of Benzoic Acid in Aqueous Ethanol Solution

Crystal Growth Kinetics of Benzoic Acid in Aqueous Ethanol Solution

Insight into the Nucleation Mechanism of p-Methoxybenzoic Acid in Ethanol-Water System from Metastable Zone Width

Direct Crystallization Resolution of Racemates Enhanced by Chiral Nanorods: Experimental, Statistical, and Quantum Mechanics/Molecular Dynamics Simulation Studies

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