Polymorph Selection and Process Intensification in a Continuous Crystallization–Milling Process: A Case Study on l-Glutamic Acid Crystallized from Water,Organic Process Research & Development

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Polymorph Selection and Process Intensification in a Continuous Crystallization–Milling Process: A Case Study on l-Glutamic Acid Crystallized from Water
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2019-01-31 00:00:00 , DOI: 10.1021/acs.oprd.8b00420
Till Köllges ₁ , Thomas Vetter ₁

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The continuous crystallization of l-glutamic acid from water in a single-stage mixed-suspension mixed-product-removal crystallizer coupled to a milling loop is studied. We show that the stable β polymorph can be obtained in the presence of milling under operating conditions that would lead to the metastable α polymorph without milling. The effect is first shown through a series of experiments carried out at different residence times and feed concentrations in the absence or presence of milling. The experimental observations are rationalized through the use of a population balance equation model. We conclude that the observed effects result from fines generation and the corresponding increase in crystal surface area. Using the model, we obtain a map of polymorphic outcomes and process productivity in dependence on the operating conditions. It is shown that the combined crystallization–milling process exhibits higher productivity and an enlarged region of operating conditions where the stable polymorph of l-glutamic acid can be reliably obtained in comparison with a conventional crystallization process.

中文翻译：

连续结晶-铣削过程中多晶型物的选择和过程强化：以水结晶出的l-谷氨酸为例

l的连续结晶研究了在与研磨回路耦合的单级混合悬浮混合产物去除结晶器中从水中提取谷氨酸。我们表明，稳定的β多晶型物可以在存在研磨条件下的操作条件下获得，这将导致亚稳态的α多晶型物无需研磨。首先通过在不存在或存在研磨的情况下，在不同的停留时间和进料浓度下进行的一系列实验来显示效果。通过使用人口平衡方程模型可以合理化实验观察结果。我们得出结论，观察到的效果是由细粉的产生和晶体表面积的相应增加引起的。使用该模型，我们根据操作条件获得了多态结果和过程生产率的地图。与常规的结晶方法相比，可以可靠地获得1-谷氨酸。

更新日期：2019-01-31

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