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(219a) Spatially-Oriented Control in Batch Crystallization Processes Using Population Balance Modeling

de Moraes, M. G. F. - Presenter, Federal University of Rio de Janeiro
Crystallization is an important separation and purification process with relevant applications in the food, pharmaceutical, fine chemical and fertilizing industries. In these processes, modeling and process control for crystallization are focused on crystal size distribution (CSD) and shape of the crystals in order to make it possible to achieve the desired quality and purity of the product of interest. The control of crystal size and shape is of considerable importance for industrial crystallization processes, as crystal morphology has great influence on downstream steps and also from the point of view of product specification criteria. The consideration of crystal shape in modeling of crystallization processes is also important due to its impact on product effectiveness, such as the bioavailability and tablet stability in pharmaceuticals. Control of the crystallization process is can be facilitated with online measurements, which provide information to be used in the modeling of the process. However, if online measurements are not available, the strongly nonlinear dynamics of these processes makes difficult to establish relations between some inputs (e.g. temperature) and the final desirable characteristics of the crystal product. In this context, image analysis has been shown to be a suitable technique to monitoring the process [1].

In our present work, a population balance model-based scheme for controlling the size and shape of crystals is presented. The modeling was performed using a two-dimensional population balance (2D-PBM) in terms of the two characteristic dimensions of the crystals, describing the evolution of crystal size and shape distributions along the batch time. To identify the nucleation, growth and dissolution kinetics parameters using the 2D-PBM approach along the length and width directions, QICPIC-LIXELL’s high speed dynamic image analysis equipment was used for the online measurement of the CSD, shape parameters and aspect ratio distribution of crystals during the experiments. In this way, the developed model allowed for the prediction of the crystal size and shape distributions during growth-dissolution cycles.

The developed framework was employed to obtain optimal temperature policies for controlling the crystal size and shape distributions that meet target criteria for size, morphology and productivity using the dynamic image analysis along the runs. Based on the concept of using measurements along batch crystallization processes as a trajectory in a phase space [2], a trajectory-endpoint control problem is presented with an oriented control scheme that is applied to the shape of the crystals. The scheme was used to control the batch cooling crystallization of potassium dihydrogen phosphate. The results demonstrate the application of the control policies for temperature to produce crystals of the desired average shape and size in different batch times. Thus, using the first principle modeling coupled to the developed trajectory tracking control, the proposed framework has the potential to be applied to industrial crystallization processes for shape control and to be extended to polymorph control investigations.


[1] Eisenschmidt, H.; Bajcinca, N.; Sundmacher, K. (2016) Optimal Control of Crystal Shapes in Batch Crystallization Experiments by Growth-Dissolution Cycles. Crystal Growth & Design, v. 16, p. 3297-2803.

[2] Griffin, D. J., Grover, M. A., Kawajiri, Y., Rousseau, R. W. (2015) Mass-count plots for crystal size control. Chemical Engineering Science, v. 137, p. 338-351.


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