ABSTRACT One of the most important tasks in the chemical industry is the separation of multicomponent liquid mixtures into one or more high-purity products. Several technologies are feasible for this task, either alone or in combination, such as distillation, extraction, crystallization, ect. Among these, distillation is by far the most widely spread and has a long history in chemical technology. However, until recently, there has been no systematic approach for understanding the separation of complex mixtures where azeotropes and multiple liquid phases may occur. There has been a growing interest in the use of residue curve and column profiles for the preliminary design of distillation columns. Residue curves and column profile are not only used to predict the composition changes in the distillation column but also to determine the feasibility of the proposed separation. Recently, theory underlying column profile maps has been developed by Tapp, Holland and co-workers. However there has been no direct experimental validation of the predictions of the column profile map theory. The main aim of this thesis is to experimentally verify some of the predictions of column profile map theory. A simple experimental batch apparatus has been developed to measure residue curve maps (RCMs) by Tapp and co-workers, the apparatus was modified so that it could be used to measure column profile maps (CPMs) in this thesis. CPM theory has shown that CPMs are linear transforms of the residues curve maps (RCMs). A stable node which was the apex of a mass balance triangle (MBT) was introduced inside the MBT, this was done by transforming the RCMs to CPMs using the appropriate distillate composition xd and reflux ratio R. It was also shown that the saddle point which was on the boundary of the triangle of the RCM can be shifted inside the MBT by transforming the RCM to CPM. This is again in accordance with theoretical predictions of CPM theory. iv Residue curves (RCs) and pinch point curves (PPCs) are used to determine the operation leaves and hence the feasible region for distillation columns operating at a specific distillate and bottoms composition for all fixed reflux ratio. The operating leaves were expanded beyond the pinch point curve by varying the reflux ratio from a higher reflux to a lower reflux ratio. This showed that one can effectively cross the pinch point curve hence expanding the operating leave. Finally the importance of experimentally measuring CPMs is demonstrated. Two thermodynamic models were used to predict the profiles of a complex system. The binary vapor-liquid equilibrium (VLE) diagrams and the residue curves produced from using these two thermodynamic models did not predict the same topology. The composition of the profiles were not the same because there were multiple liquid phases involved in this system, which made it difficult for the researchers to measure the correct profiles. Column profile maps were simulated using the different thermodynamic models, they also showed that there is some discrepancy between the predictions of the two models.

Student Number : 9903549T - MSc dissertation - School of Process and Materials Engineering - Faculty of Engineering and the Built Environment / Preliminary evaluations during flowsheet synthesis require simple effective tools for comparison and elimination of process alternatives. This work investigates three areas of interest in distillation. Column profile map theory has simplified complex column investigations. The predictions of the difference point equation at finite reflux were experimentally verified for the acetone, methanol and ethanol system in a continuous column apparatus. Residue curve analysis is usually limited to systems with four components for distillation system analysis. An alternative representation, based on combinatorial topology and temperature sequencing, is introduced for use in high level synthesis decisions for higher component order systems. Attainable region (AR) theory is applied to an ideal binary distillation system for a geometrically based method of cost analysis. A constrained attainable region is constructed from a series of equilibrium step compositions with varying reflux and corresponding cost associations. The AR is shown to be useful for costing and optimization.