Source: Kerry M. Dooley and Michael G. Benton, Department of Chemical Engineering, Louisiana State University, Baton Rouge, LA

Tray and packed columns are both commonly used for distillation, absorption, and stripping separation operations.^1,2 The goal of this experiment is to distill a mixture of alcohols (methanol, isopropanol) and water in a sieve tray column and examine how closely simple theories of distillation based on equilibrium assumptions are followed. Sieve trays provide maximum interfacial area between the liquid and vapor. A P&ID schematic of the sieve tray (each tray contains holes in a support plate) distillation system can be found in Appendix A.

In this demonstration, the Tray Distillation Unit (TDU) is started in total reflux mode. After a steady reflux drum level is attained, a switch to finite reflux mode is made by adjusting the bottoms, distillate and reflux flow rate controllers as necessary to maintain steady levels in the reflux drum and the reboiler, and to maintain a target reflux ratio R_D = L/D. Once steady state is achieved (takes at least 90 min), liquid samples will be taken from the reflux drum, reboiler and on each tray and analyzed in a gas chromatograph. A typical protocol is to investigate the effects of reflux ratio over a wide range. From the sample analyses, the tray efficiencies can be determined for all three components on all six trays assuming constant molar overflow (McCabe-Thiele method). The results can also be simulated using an equilibrium process simulator, if available. These two methods can also be used to determine the overall tray efficiency. Additionally, data reconciliation of the mass balances can be performed to determine if gross measurement errors exist. Any Separations or Unit Operations textbook covers the fundamentals of distillation including basic concepts such as reflux ratio, Murphree efficiencies and the McCabe-Thiele method and diagram.²

The TDU is operated from a computer interface of a distributed control system. The interface is entirely graphical. The column contains 6 trays, a total condenser, and a partial reboiler (Appendix A). The mixture is contained in the feed reservoir, and the feed nominally consists of methanol (~50 wt.%), isopropanol (~30 wt.%), and water (~20 wt.%).

1. Starting Total Reflux Mode

1. Turn on the cooling water. If the reboiler liquid level is too low, add feed to it; if too high, use the

The appropriate response factor (RF_i) for each component, which is the ratio of the signal intensity to the quantity of analyte injected and is provided in the software, is used to determine the wt% of each sample.

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Reflux ratio (R_D = L/D) has a tremendous effect on both column

Tray distillation columns are often of the sieve type, with small holes for the vapor flow and larger downcomers to route the liquid from tray to tray by gravity. More volatile components mostly exit in the distillate, although some of the top vapor is condensed and returned to the column as liquid reflux. It was shown that determining the Murphree tray efficiencies can be important in pinpointing problems on specific trays in distillation columns, such as low mass transfer rates, weeping or flooding. While higher vapor/