This contribution elaborates the design considerations of a simplified version of a four-product multiple dividing wall column in pilot plant scale that will be built at Ulm University. This will be the first realization of a multiple dividing wall column worldwide. A detailed simulation approach, starting from the initialization by V_min-method, is presented to obtain a feasible design of the column, taking into account the constraints of the operation within a university environment. The operating point was found by simulation studies, using the integrated optimization tool of AspenPlus^© V10. It is shown that an NQ-curve can be applied on simplified multiple dividing wall columns. Based on the determined operating point, the thermodynamic and the fluid dynamic design of the pilot plant are discussed in detail. It is shown that the designed column can be operated to obtain all products with a purity of at least 98 mol%.

Dividing Wall Columns (DWCs) allow the separation of a ternary mixture in one column shell by applying a vertical partition wall, yielding a reduction of operational and capital costs of up to 30%. Multiple DWC (mDWC), the consequent advancement of standard DWC, makes use of more than one partitioning wall, allowing the separation of quaternary or even higher mixtures in one column shell accompanied by a further reduction of energy consumption. Since no dedicated models for these columns are available in commercial process simulators, thermodynamic consistent flowsheets have to be designed and implemented. The thermally fully coupled Petlyuk arrangement is one important example. However, the initial convergence of these substituting flowsheets is demanding, since a large number of meaningful initial guesses have to be provided. A promising method for generating these first estimates are minimum vapor (V_min) diagrams. All internal flows can be extracted from these diagrams and used for robust initialization of the simulation. The goal of this work is to present the V_min method in a comprehensive way in order to initialize mDWC simulations to predict the separation of four component mixtures. Additionally, the adaptation of the diagram to configurations different than Petlyuk arrangements for mDWC is evaluated and a systematic procedure to obtain them is presented. In the end, an example of a converging simulation is given, which was obtained with the values from the V_min diagram.

This work presents two novel methods to investigate in situ the carbon dioxide (CO₂)-induced gelation of biopolymer-based solutions. The CO₂-induced gelation is performed in a viewing cell at room temperature under CO₂ pressure (20 to 60 bar), whereby calcium precursors are used as cross-linkers. The novel methods allow the in situ optical observation and evaluation of the gelation process via the change in turbidity due to dissolution of dispersed calcium carbonate (CaCO₃) particles and in situ pH measurements. The combination of both methods enables the determination of the gelation direction, gelation rate, and the pH value in spatial and temporal resolution. The optical gelation front and pH front both propagate equally from top to bottom through the sample solutions, indicating a direct link between a decrease in the pH value and the dissolution of the CaCO₃ particles. Close-to-vertical movement of both gelation front and pH front suggests almost one dimensional diffusion of CO₂ from the contact surface (gel–CO₂) to the bottom of the sample. The gelation rate increases with the increase in CO₂ pressure. However, the increase in solution viscosity and the formation of a gel layer result in a strong decrease in the gelation rate due to a hindrance of CO₂ diffusion. Released carbonate ions from CaCO₃ dissolution directly influence the reaction equilibrium between CO₂ and water and therefore the change in pH value of the solution. Increasing the CaCO₃ concentrations up to the solubility results in lower gelation rates.