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
- Turn on the cooling water. If the reboiler liquid level is too low, add feed to it; if too high, use the bottoms pump to return liquid to the feed tank.
- Turn on the main reboiler heater from the interface and the strip heaters using the switch on the unit at top right. Put the reboiler temperature controller in manual (MAN), give it an output (OP) of at least 60%, then wait for the overhead vapor to condense and the reflux drum to start filling, as seen on the interface. The reflux preheater power will start up with the reboiler heater.
- When the reflux drum level reaches 50%, put the reflux flow controller in AUTO, give it a setpoint (SP) of 20%, and turn on the reflux pump.
- As soon as you measure a reflux flow on the controller, gradually decrease the setpoint in steps of a percent every few seconds until the reflux flow rate is 12 - 13% of span (span = the total range of the transmitter).
- Put the reflux preheat controller in AUTO, and give it a setpoint of ~65 °C, or some other suitable value near the temperature of the top tray.
- Wait for the reflux drum level to reach at least 50% before manually adjusting the reflux rate by changing the setpoint on the reflux flow controller as necessary to provide a constant reflux drum level of 25 - 75%.
- When all flows, levels, temperatures and compositions are close to their setpoints and aren't changing significantly over 2 min, steady state has been achieved.
2. Transitioning to Finite Reflux Mode
- Put the feed flow controller to AUTO, and give it a setpoint corresponding to ~120 cm3/min.
- Turn on the feed pump and feed preheater. Put the feed preheat controller in AUTO and give it a setpoint of ~65 °C or other temperature near that of the feed tray temperature.
- Put the reflux flow rate controller in AUTO and give it a setpoint of ~80 % of the total reflux case as a starting point.
- Start withdrawing distillate product (adjust flow controller to >0 flow) to maintain a level of 25 - 75% in the reflux drum. Put the distillate flow controller in AUTO and adjust its setpoint unless other instructions specifically call for MANUAL control. Try 3 different reflux ratios around 1 (e.g., 0.8, 1.2, 1.6), but hold the boilup rate constant by keeping the heat duty constant at a value that gives distillate flow.
- Start withdrawing bottoms product (adjust flow controller to >0 flow) to maintain a constant level of 60-80 % in the reboiler. Put the bottoms flow controller in AUTO, turn on the bottoms pump, and adjust its setpoint, unless other instructions specifically call for MANUAL control. Both products should flow back to the feed reservoir.
- When all flows, levels, temperatures and compositions are close to their setpoints, steady state has been achieved. The flow controllers may need to be adjusted; recall, F = B + D (feed = bottoms + distillate on a molar basis, and the distillate will be mostly methanol).
- Collect a few mL volume samples of the feed, bottoms and distillate at the same time (see Figure 3, Appendix A). To collect the feed, insert a pipette through the top port of the feed tank. Only one set of samples per steady state is needed. It is also possible to sample liquid from each tray through its septum port using curved needle syringes Do this as only one of the steady states.
3. Setting Up the Gas Chromatograph
The gas ghromatograph (GC) is operated through the vendor's software. The column is Porapak Q, 1/8" in diameter and 2 ft long.
- Select the Method and Run Control window. On the icon-filled menu bar, select Method and pick the START.M method.
- On the front panel of the GC, press the Front Inlet button. The pressure should be set to 4.5 psi.
- Inject a 0.1 microliter sample (same volume each time) and press the Start button on the GC front panel. The software will show 'Run' in Progress / Data Acquisition, with the elapsed time counting up.
- Results will appear in a report on the software screen after approximately 3 min in the form of a chart containing GC peaks. Scroll down the report to see the Area% results.
4. Shutting down the Distillation column
- Turn off all three heaters, the bottoms pump and the feed pump.
- Put all controllers except the reflux flow rate in MAN and set their outputs (OP) to 0%.
- Put the reflux flow rate controller in MAN and set its OP to 20%.
- Turn on the reflux pump override and leave the reflux pump on until the reflux drum is empty.
- As soon as the reflux drum is empty, take off the reflux pump override, turn off the reflux pump, put the reflux flow rate controller in MAN, and set its OP to 0%.
- Leave the cooling water on until all six tray temperatures are below 60 °C, and then turn it off.
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 RD = 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
- Turn on the cooling water. If the reboiler liquid level is too low, add feed to it; if too high, use the bottoms pump to return liquid to the feed tank.
- Turn on the main reboiler heater from the interface and the strip heaters using the switch on the unit at top right. Put the reboiler temperature controller in manual (MAN), give it an output (OP) of at least 60%, then wait for the overhead vapor to condense and the reflux drum to start filling, as seen on the interface. The reflux preheater power will start up with the reboiler heater.
- When the reflux drum level reaches 50%, put the reflux flow controller in AUTO, give it a setpoint (SP) of 20%, and turn on the reflux pump.
- As soon as you measure a reflux flow on the controller, gradually decrease the setpoint in steps of a percent every few seconds until the reflux flow rate is 12 - 13% of span (span = the total range of the transmitter).
- Put the reflux preheat controller in AUTO, and give it a setpoint of ~65 °C, or some other suitable value near the temperature of the top tray.
- Wait for the reflux drum level to reach at least 50% before manually adjusting the reflux rate by changing the setpoint on the reflux flow controller as necessary to provide a constant reflux drum level of 25 - 75%.
- When all flows, levels, temperatures and compositions are close to their setpoints and aren't changing significantly over 2 min, steady state has been achieved.
2. Transitioning to Finite Reflux Mode
- Put the feed flow controller to AUTO, and give it a setpoint corresponding to ~120 cm3/min.
- Turn on the feed pump and feed preheater. Put the feed preheat controller in AUTO and give it a setpoint of ~65 °C or other temperature near that of the feed tray temperature.
- Put the reflux flow rate controller in AUTO and give it a setpoint of ~80 % of the total reflux case as a starting point.
- Start withdrawing distillate product (adjust flow controller to >0 flow) to maintain a level of 25 - 75% in the reflux drum. Put the distillate flow controller in AUTO and adjust its setpoint unless other instructions specifically call for MANUAL control. Try 3 different reflux ratios around 1 (e.g., 0.8, 1.2, 1.6), but hold the boilup rate constant by keeping the heat duty constant at a value that gives distillate flow.
- Start withdrawing bottoms product (adjust flow controller to >0 flow) to maintain a constant level of 60-80 % in the reboiler. Put the bottoms flow controller in AUTO, turn on the bottoms pump, and adjust its setpoint, unless other instructions specifically call for MANUAL control. Both products should flow back to the feed reservoir.
- When all flows, levels, temperatures and compositions are close to their setpoints, steady state has been achieved. The flow controllers may need to be adjusted; recall, F = B + D (feed = bottoms + distillate on a molar basis, and the distillate will be mostly methanol).
- Collect a few mL volume samples of the feed, bottoms and distillate at the same time (see Figure 3, Appendix A). To collect the feed, insert a pipette through the top port of the feed tank. Only one set of samples per steady state is needed. It is also possible to sample liquid from each tray through its septum port using curved needle syringes Do this as only one of the steady states.
3. Setting Up the Gas Chromatograph
The gas ghromatograph (GC) is operated through the vendor's software. The column is Porapak Q, 1/8" in diameter and 2 ft long.
- Select the Method and Run Control window. On the icon-filled menu bar, select Method and pick the START.M method.
- On the front panel of the GC, press the Front Inlet button. The pressure should be set to 4.5 psi.
- Inject a 0.1 microliter sample (same volume each time) and press the Start button on the GC front panel. The software will show 'Run' in Progress / Data Acquisition, with the elapsed time counting up.
- Results will appear in a report on the software screen after approximately 3 min in the form of a chart containing GC peaks. Scroll down the report to see the Area% results.
4. Shutting down the Distillation column
- Turn off all three heaters, the bottoms pump and the feed pump.
- Put all controllers except the reflux flow rate in MAN and set their outputs (OP) to 0%.
- Put the reflux flow rate controller in MAN and set its OP to 20%.
- Turn on the reflux pump override and leave the reflux pump on until the reflux drum is empty.
- As soon as the reflux drum is empty, take off the reflux pump override, turn off the reflux pump, put the reflux flow rate controller in MAN, and set its OP to 0%.
- Leave the cooling water on until all six tray temperatures are below 60 °C, and then turn it off.
Tray distillation is a crucial chemical engineering technique used to separate compound mixtures in various industrial settings. Such as chemical plants, oil refineries, and natural gas processing. Distillation is performed in a column with many different levels called trays. A liquid feed stream travels through the column and after exposure to heat is either condensed or vaporized, enabling the mixture to be separated based on the difference in volatilities. In order to design a cost-productive distillation apparatus the separation efficiencies of the trays in the system are studied. Here we will investigate the separation efficiency of a Sieve tray column used to separate a mixture of methanol, isopropanol, and water.
In a distillation column, the liquid feed is introduced and it flows downward while simultaneously contacting a rising vapor stream. When the liquid reaches the bottom it enters a re-boiler and is either vaporized and re-enters the column or remains liquid and exits the system. This exiting stream, called the bottoms, contains the heavier components. The boil up ratio VB, is the ratio of liquid recycled into the column to the amount of liquid leaving in the bottoms. The vapor stream flows upward through the column and is condensed before entering a reflux drum. It is then split into two streams. The distillate containing the more volatile components which exit the system, and the reflux stream which is cycled to the column. The reflux ratio, which is the ratio of reflux rate to distillate rate can influence separation efficiency. In total reflux mode, 100% of the streams are recycled back into the column. However, practical distillations are operated in partial reflux mode to achieve economic separation. Now let's take a look at the McCabe-Thiele analysis to determine the number of stages needed for a separation using VLE data for the two components. Starting from the distillate composition, draw an operating line with slope equal to RD over RD plus one. Starting from the bottoms composition draw an operating line with slope equal to VB plus one over VB. Step down the plot between the BLE curve and operating lines until the bottom is reached. The number of steps minutes one for the reboiler is equal to the number of trays needed. To evaluate efficiency, the Murphree Method is used. The Murphree efficiency for a single tray, EML, describes the change of the liquid composition over the tray divided by the change off the exiting liquid composition, assuming it was in equilibrium with the exiting vapor. Low efficiencies on a tray are often associated with low interfacial area or low superficial velocities, enabling engineers to pinpoint problems in a column and improve design. Now that we've discussed how a distillation column works and how the reflux ratio can affect the separation, let's test and demonstrate the effects in a laboratory experiment.
Before you start, familiarize yourself with the tray distillation unit. The unit consists of a column containing six sieve trays. The feed reservoir contains the mixture of methanol 50 weight percent, isopropanol 30 weight percent, and water 20 weight percent. Which is directed via a pump to the feed preheater and then to the column. The distillate from the column is collected in the total condenser equipped with a valve to collect the samples. A reflux drum, reflux pump, and preheater are used to provide a continuous reflux of which the ratio is adjusted for a better efficiency. Lastly, the reboiler and bottoms pump provide heating of the mixture and the bottoms valve is used to obtain the samples for analysis. The majority of the trade distillation unit is operated using a graphical interface. To start the experiment for the total reflux mode, turn on the cooling water and check the level of the reboiler liquid. Adjust the level by either adding feed liquid or removing some liquid using the bottom pump. Turn on the main reboiler heater and the strip heater. Then, via the controls, set the reboiler temperature controller to manual and adjust the output to at least 60%. And wait for the overhead vapor to condense, filling the reflux drum. Once the reflux drum has reached a level of 50%, set the reflux flow controller I auto with a set point of 20% and turn on the reflux pump. As soon as you measure the reflux flow on the controller, gradually decrease the set point in 2% increments every 20 to 30 seconds until the reflux flow rate is 12 to 13% of span. When the reboiler heater was activated, the system also started the reflux preheater. Now set the controller in auto and give the reflux preheater a set point of approximately 65 degrees Celsius. Make sure that the reflux drum level is around 50%, and if necessary manually adjust the rate by changing the set point on the reflux flow controller to provide a constant reflux drum level of 25 to 75%. When all flows, levels, temperature, and compositions are close to their set points and aren't changing significantly for approximately two minutes, one can say that steady state of the total reflux mode has been achieved.
Now that the system has reached a steady state, let's transition to the finite reflux mode. Set the feed flow controller to auto with a set point of approximately 120 cubic centimeters per minute. Next turn on the feed pump and the feed preheater, set the controller in auto, and give it a set point of approximately 65 degrees Celsius. Once the feed settings are set, put the reflux flow rate controller in auto and set the starting point of the reflux flow to a set point of approximately 80%. Start withdrawing the distillate product to maintain the reflux drum level between 25 and 75%. Put the distillate flow controller in auto and adjust it's set point above zero flow. Start withdrawing the bottoms product to maintain a constant level of 60 to 80% in the reboiler. Put the bottoms flow controller in auto, turn on the bottom pump, and adjust the set point to a flow rate above zero. Repeat the finite reflux operation at approximately three different reflux ratios while keeping the boil up rate constant. This is carried out to adjust to different steady states in the finite reflux mode. When all flows, levels, temperature, and composition are close to their set points and are not changing significantly, then stead state is reached. Once a stead state is reached, open the sample valves and use sample bottles to collect one set of three to four milliliter samples of the bottoms and distillate products at their respective sample points. Using a pipette, insert it through the top of the feed tank to collect a feed sample. Next, using a curved needle syringe, insert it through the septum port of each tray to acquire tray samples. Secure the samples and analyze them using a gas chromatograph after the experiment is finished.
Now that you have finished the experiment, let's focus on analyzing the results. The McCabe-Thiele analysis for this system shows that 4.5 stages are needed for the separation. Though the system utilizes six stages plus the reboiler. Next, obtain the mass fraction of the samples using the GC data. Apply the Murphree tray efficiency equation and calculate the efficiency of each tray. Tray two was significantly more efficient than its counterparts and visual observation showed it to be very frothy. So high in interfacial area. Tray one was even more frothy, but some entrainment could be observed. This behavior is a consequence of a low surface tension for an alcoholic mixture. In the top two trays, almost all of the water had been removed, leaving behind mostly methanol with some isopropanol. Tray three had poor methanol efficiency, which is observed when a different compound, water in this case, undergoes a profound concentration change on the tray. Now repeat the calculations for each reflux ratio to determine the effect on the composition of the distillate and bottoms. In general, the lower reflux rate reduces the methanol purity of the distillate. A higher reflux rate improves the separation at high operating costs.
Lastly, let's take a look at a couple applications of trade distillation and measuring tray efficiencies in the chemical industry. Oil refineries separate crude oils into multiple products. The feed stream is heated crude oil at atmospheric pressure. Fuels, such as fuel oil for ships, diesel, kerosene, naphtha, and gasoline are separated based on their boiling points and thus chain length. Chemical engineers use tray efficiencies to optimize the separation processes of the desired products. To generate distilled spirits such as vodka or whiskey, a mixture of grain fermentation products known as wash, which is 10 to 12% alcohol by volume is boiled in a still and the resulted vapor is separated by simple or trade distillation. This allows the ethanol to be separated from other alcohols like propanol and water, which have higher boiling points.
You've just watched Jove's introduction to distillation. You should now understand the distillation process, how to operate a tray distillation unit, and how to evaluate its efficiency. You have also seen several applications of distillation in industrial settings. Thanks for watching.
The appropriate response factor (RFi) 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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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/...
Chapters in this video
0:07
Overview
0:58
Principles of Distillation
3:35
Distillation Column Operation: Adjusting the Reflux
6:20
Transitioning to Finite Reflux Mode
8:25
Results
9:52
Applications
10:54
Summary
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