Crystallization process design

The ideal solubility equation (Eq. 2) is the simplest form of model that is applicable to solvent based crystallization process design. Even though the equation excludes non-ideal interactions in the liquid phase, it is still a useful tool in certain circumstances. 

Case Study - Solubility Modelling and Crystallization Process Design for Cimetidine... 

Cimetidine Crystallization Process Design with NRTL-SAC. 

NRTL-SAC has been demonstrated through the case study on Cimetidine as a valuable aid to solubility data assessment and targeted solvent selection for crystallization process design. The average model error is typically 0.5 Ln (x) [1] and is sufficient as a solvent screening tool. Methods that can deliver greater accuracy would increase the value and utility of these techniques. It is impressive in the case of Cimetidine that the NRTL-SAC correlation is capable of reasonable accuracy and predictive capability on the basis of just 2 fitted parameters. Further work to extend the solvent database and optimize the descriptive parameters will be beneficial, and are planned by the developers. 

Examples in this chapter include sterile crystallization of a labile compound, yield enhancement by crystallization, yield and selectivity enhancement, removal of low-level impurities via crystallization from the melt, crystal formation in vials in a freeze drier, and non-equilibrium resolution of stereoisomers by crystallization. These examples represent unique crystallization processes designed for specific purposes. One lesson to be learned from examination of these nonmainstream applications is that understanding of principles can lead to inventive solutions to problems. For instance, in Examples 11-2 and 11-3, the solubility difference between starting material and desired product is used to optimize the reaction yield/selectivity by crystallizing the product and protecting it from overreaction. 

The above procedure, while rather tedious, will result in a reasonable estimate of the supersaturated solution diffusivity that is quite useful in crystallization process design and development. 

There are numerous examples of purified materials by the above-mentioned two types of suspension crystallization process designs some of them are acetic acid, caprolactam, methacrylic acid, and phenol. The two discussed suspension crystallization concepts, shown in the Figures 17.9 and 17.10, count to the continuous packed column with mechanical forced transport. 

Xylene Isomerization. After separation of the preferred xylenes, ie, PX or OX, using the adsorption or crystallization processes discussed herein, the remaining raffinate stream, which tends to be rich in MX, is typically fed to a xylenes isomerization unit in order to further produce the preferred xylenes. Isomerization units are fixed-bed catalytic processes that are used to produce a close-to-equiUbrium mixture of the xylenes. To prevent the buildup of EB in the recycle loop, the catalysts are also designed to convert EB to either xylenes, benzene and lights, or benzene and diethylbenzene. 

Nucleation. Crystal nucleation is the formation of an ordered soHd phase from a Hquid or amorphous phase. Nucleation sets the character of the crystallization process, and it is, therefore, the most critical component ia relating crystallizer design and operation to crystal size distributions. 

Several reported chemical systems of gas-liquid precipitation are first reviewed from the viewpoints of both experimental study and industrial application. The characteristic feature of gas-liquid mass transfer in terms of its effects on the crystallization process is then discussed theoretically together with a summary of experimental results. The secondary processes of particle agglomeration and disruption are then modelled and discussed in respect of the effect of reactor fluid dynamics. Finally, different types of gas-liquid contacting reactor and their respective design considerations are overviewed for application to controlled precipitate particle formation. 

Thus, methods are now becoming available such that process systems can be designed to manufacture crystal products of desired chemical and physical properties and characteristics under optimal conditions. In this chapter, the essential features of methods for the analysis of particulate crystal formation and subsequent solid-liquid separation operations discussed in Chapters 3 and 4 will be recapitulated. The interaction between crystallization and downstream processing will be illustrated by practical examples and problems highlighted. Procedures for industrial crystallization process analysis, synthesis and optimization will then be considered and aspects of process simulation, control and sustainable manufacture reviewed. 

A common starting point is that the process engineer is given a brief from which to determine a crystallization plant design viz. some specification of the product and process (e.g. mean particle size, production rate) and characteristics of the feed solution (e.g. composition, temperature etc.). Figure 9.1. 

Figure 9.1 Typical crystallization process systems design procedure...

Rossiter and Douglas (1986) state that the first step in process design is to generate a basic structure for the flowsheet i.e. the choice of unit operations and interconnections which can be analysed, refined and costed, and then compared to alternatives. Thus, the generation of an industrial crystallization flowsheet gives rise to a number of optimization problems for which a systematic hierarchical decision process for particulate systems was proposed ... 

The optimal network increases total residence time by 48 per cent when compared with an equivalent MSMPR of the same volume and throughput. This increase would translate into a similar increase in mean crystal size and a 78 per cent increase in yield. Exactly the same residence time as for the single crystallizer have been reported from simple cascade configurations previously designed for stage-wise crystallization processes for slight improvements in... 

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