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Process Performance and Operational Challenges in Continuous Crystallization: A Study of the Polymorphs of L-Glutamic Acid
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2023-03-14 , DOI: 10.1021/acs.cgd.2c01424 Ramona Achermann 1 , Andraž Košir 1 , Brigitta Bodák 1 , Luca Bosetti 1 , Marco Mazzotti 1
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2023-03-14 , DOI: 10.1021/acs.cgd.2c01424 Ramona Achermann 1 , Andraž Košir 1 , Brigitta Bodák 1 , Luca Bosetti 1 , Marco Mazzotti 1
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The crystallization of the two polymorphs of l-glutamic acid (LGA) is carried out in a continuous crystallization process, and its performance according to different criteria is evaluated. The study aims at identifying suitable operating conditions for producing either αLGA or βLGA with a high polymorphic purity. To this end, we investigate the process both from a theoretical perspective and through experiments using either a single stirred-tank crystallizer or a cascade of two stirred-tank crystallizers in series. In terms of theory, we extend the MSMPR-based steady-state stability analysis of Farmer et al. (Farmer, T. C.
et al. AIChE J. 2016, 62, 3505–3514) by accounting for the possibility of a nonrepresentative withdrawal of the solid phase from the crystallizer. Additionally, the process is simulated using population balance equations, thereby investigating the effect of operating conditions on polymorphic purity, yield, and productivity. Guided by the model-based conclusions, we identified suitable operating conditions and experimentally tested them. The experimental campaign has demonstrated that βLGA could be successfully and continuously produced in both process configurations according to the theory with performance as expected, whereas that was not possible for αLGA. The difference between the two stems from different operational challenges, whose consequence is that steady-state operation is attained in the case of βLGA but not in that of αLGA. In the former case, the needle-like βLGA crystals, which exhibit no agglomeration, tend to be only slightly oversampled; in the latter case, the prismatic αLGA crystals undergo major agglomeration and hence are very difficult to suspend and effectively withdraw from the crystallizer.
中文翻译：
连续结晶的工艺性能和操作挑战：L-谷氨酸多晶型物的研究
L-谷氨酸 (LGA)的两种多晶型物的结晶是在连续结晶过程中进行的，并根据不同的标准对其性能进行了评价。该研究旨在确定生产具有高多晶型纯度的 αLGA 或 βLGA 的合适操作条件。为此，我们从理论角度和通过使用单个搅拌罐结晶器或串联的两个搅拌罐结晶器的级联的实验来研究该过程。在理论方面，我们扩展了 Farmer 等人基于 MSMPR 的稳态稳定性分析。(Farmer, TC et al. AIChE J. 2016 , 62, 3505–3514) 通过考虑从结晶器中非代表性地取出固相的可能性。此外，该过程使用群体平衡方程进行模拟，从而研究操作条件对多晶型纯度、产量和生产率的影响。在基于模型的结论的指导下，我们确定了合适的操作条件并通过实验对其进行了测试。实验活动表明，βLGA 可以根据理论在两种工艺配置中成功连续生产，性能符合预期，而 αLGA 则不可能。两者之间的差异源于不同的操作挑战，其结果是在 βLGA 的情况下可以实现稳态操作，而在 αLGA 的情况下则不能。在前一种情况下，针状 βLGA 晶体没有团聚，往往只是略微过采样；在后一种情况下，棱柱形 αLGA 晶体会发生较大的团聚，因此很难悬浮并有效地从结晶器中取出。
更新日期：2023-03-14
中文翻译：
连续结晶的工艺性能和操作挑战：L-谷氨酸多晶型物的研究
L-谷氨酸 (LGA)的两种多晶型物的结晶是在连续结晶过程中进行的，并根据不同的标准对其性能进行了评价。该研究旨在确定生产具有高多晶型纯度的 αLGA 或 βLGA 的合适操作条件。为此，我们从理论角度和通过使用单个搅拌罐结晶器或串联的两个搅拌罐结晶器的级联的实验来研究该过程。在理论方面，我们扩展了 Farmer 等人基于 MSMPR 的稳态稳定性分析。(Farmer, TC et al. AIChE J. 2016 , 62, 3505–3514) 通过考虑从结晶器中非代表性地取出固相的可能性。此外，该过程使用群体平衡方程进行模拟，从而研究操作条件对多晶型纯度、产量和生产率的影响。在基于模型的结论的指导下，我们确定了合适的操作条件并通过实验对其进行了测试。实验活动表明，βLGA 可以根据理论在两种工艺配置中成功连续生产，性能符合预期，而 αLGA 则不可能。两者之间的差异源于不同的操作挑战，其结果是在 βLGA 的情况下可以实现稳态操作，而在 αLGA 的情况下则不能。在前一种情况下，针状 βLGA 晶体没有团聚，往往只是略微过采样；在后一种情况下，棱柱形 αLGA 晶体会发生较大的团聚，因此很难悬浮并有效地从结晶器中取出。
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