Batch-to-batch Optimization of Batch Crystallization Processes

It is the fact that several process parameters are either unknown or uncertain. Therefore, an optimal control, profile calculated with developed process models with respect to such process parameters may not give an optimal performance when implemented to real processes. This study proposes a batch-to-batch optimization strategy for the estimation of uncertain kinetic.par.ameters in a batch crystallization process of potassium sulfate production. The knowledge of a crystal size distribution of the product at the end of batch operation is used in the proposed methodology. The updated kinetic parameters are applied for determining an optimal operating temperature policy for the next batch run.

A Pioneering Experimental Study on the Batch Crystallization of the Citric Acid Monohydrate

Citric acid is an important organic substance whose marketing concerns various fields. Nevertheless, until 1997 the scientific literature reported little information about the process of crystallization by cooling through which the commercial product is obtained. In particular, the available studies were aimed to investigate only the kinetics of nucleation and crystal growth neglecting some effective aspects of the industrial crystallization in mechanically stirred apparatus. In order to fill that sci-tech gap, the Department of Chemical Engineering at the University ＂La Sapienza＂ of Rome decided to lead a long and meticulous experimental research on the crystallization in discontinuous （batch） of CAM （citric acid monohydrate） in the allotropic form that is stable at room temperature. Due to the number of people involved in that pioneering work, carried out in the historic laboratories of＂La Sapienza＂ （Faculty of Engineering）, and motivated by the publication of related M.Sc. dissertations and research papers, such collective effort was called ＂School of Industrial Crystallization＂. Among the graduate students in Chemical Engineering that 17 years ago participated in that fruitful experience there was also the author who, under the supervision of Prof. Barbara Mazzarotta, had the specific task of assessing the effects on CAM of changing the crystallization operating conditions until their optimization; the achievements are briefly illustrated in this paper.

The Geometry Effect in a Pioneering Experimental Study on the Batch Crystallization of the CAM

Far from being equivalent to host the process, the vessels play an active role in the crystallization thanks to their differently shaped bottoms. It was clearly pointed out through a meticulous experimental research on the batch crystallization of CAM （citric acid monohydrate） carried out in the years 1997-1998 by the author at the historic laboratories of＂La Sapienza＂ University of Rome. Such pioneering M.Sc. thesis, supervised by Prof. Barbara Mazzarotta （Department of Chemical Engineering）, was already summarized in an informative essay but, since the crystallization operating conditions to optimize were illustrated ＂collectively＂, it seemed necessary a further paper expounding uniquely the geometry effect. Our aim is to use all the data, collected and simulated, in order to show why the round-bottomed crystallizer performed better than the conical-bottomed one with the CAM from aqueous solutions, and why we should discard the flat-bottomed crystallizers.

Crystallization Kinetics of Batch Spontaneous Nucleation of Potassium Nitrate

The batch cooling crystallization initiated from spontaneous nucleation for aqueous solution of potassium nitrate was studied. The concentration and transmittance data were acquired on line throughout the operation.Based on solute mass transfer in both liquid and solid phases, a kinetic model was deduced by assuming that the late period of primary nucleation resembles the initial period of the secondary nucleation. Nucleation and crystal growth stages were identified. Kinetic parameters were estimated piecewise from online experimental data and compared with those in literature. The estimated kinetic parameters for stages without apparent primary nucleation agreed well with those in literature. Further, a simulated concentration curve was also drawn from the estimated kinetic parameters and it matched well with that in experiment.

Process Modeling for Batch Cooling Crystallization

The general mathematical model for batch cooling crystallization was established based on the population balance equation considering the change of slurry volume, and simulated with crystallization thermodynamics,kinetics and mass balance employing bed voidage. In the system of vitamin C-water-ethanol, reliability of this model was verified by comparison between simulation results and experimental data. The effects of operation parameters on product quality can be systematically investigated by modeling simulation.

Production of Sucrose Crystals of Uni-Modal Size Distribution by Seeded Batch Cooling Crystallization

From sucrose aqueous solution of high viscosity, sucrose was crystallized by seeded cooling in a batch crystallizer. At low seed loadings, the product crystal size distribution (CSD) was wide-spread because of enormous secondary and primary nucleation. However, at high seed loadings, it became uni-modal, where the crystallization was dominated by seed growth with practically no secondary nucleation. Enough seeding was thus effective in suppressing nucleation even during batch crystallization with high viscosity solution. The volume mean size of the product crystals obtained at high seed loadings agreed with that calculated by a simple mass balance assuming growth-dominated crystallization with no change in the number of crystals.