1. Study the performance of a binary distillation column operated in batch mode.

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1 Goals for batch distillation using the East distillation column: 1. Study the performance of a binary distillation column operated in batch mode. 2. Determine the overall and local efficiency of the column of the column. 3. Study the effect of reflux ratio on the concentrations of the top and bottom product. Week 1 experiment: To run the column at the total reflux condition and determine the overall and local efficiencies. Overall efficiency can be calculated by comparing the actual number of plates in the column with the number obtained from McCabe-Thiele diagram when the column operates at total reflux. Local or point efficiencies can be calculated by measuring the compositions of the liquid streams corresponding to two successive plates. The local efficiency is typically close to the overall efficiency Week 2 and 3 experiment: To run the distillation column at six different reflux ratios. The reflux ratio is changed by changing the liquid being refluxed to the column which in turn can be changed by steam flow rate. The amount of the distillate needs to be held at a constant value. The concentration of the top and bottom product as a function of reflux ratio or steam flow usage can be studied.

2 General Operation Procedures Preparation for Start-up: Key purposes: Get familiar with the system; locations of the valves and sample taps Check the liquid level in the reboiler Check the composition in the reboiler and feed tank Turn the Siemens system on Check if the valves are in the correct position 1. Using the sight-glass on the reboiler to assess its level of the liquid (in the range of around 70%). (see Figure 1). East Column Reboiler Reboiler Sight glass Green Valve Sample tap Red gauge valve on Bottoms line Figure 1: East Column Reboiler 2. Prepare to mix the contents of the reboiler. a. Close the red gauge valve on the bottoms line (see Figure 2). Open the green valve on the same line just after it exits the reboiler (see Figures 1 and 2) b. Follow the line down to the bottom of the reboiler. Open the orange ball valve and make sure that the blue ball valve on the sample port is closed (see Figure 2). 3. Ask the TA/Lab Assistant to turn on the computer system hooked to the East column.

3 Red gauge valve on Bottoms line Blue manual bypass valve on Bottoms line Blue ball valve on line exiting reboiler Orange valve at bottom of reboiler open while mixing Figure 2: East Column Reboiler Pumping Line 4. Using the computer control system, turn on the reboiler-mixing pump on the 1 st floor, as shown in Figure 2 to mix the contents of the reboiler. Let mix for at least twenty minutes. 5. While you are waiting, check that the manual by-pass valves are closed. a. Reflux red valve parallel to the Reflux control valve (see Figure 3) b. Distillate red valve parallel to the Distillate control valve (see Figure 3) c. Bottoms blue valve parallel to the Bottoms control valve (see Figure 2) d. Water blue valve parallel to the Water control valve (see Figure 3)

4 Figure 3. East column second floor control valves 6. Check that the following control valves are closed. a. Feed on 2 nd floor (see Figure 3) (What is the function of this valve? For a batch system, feed is infact the starting material in the reboiler, isn t it?) b. Distillate (DISTILLATE/PID) on 2 nd floor (see Figure 3) c. Bottoms (BOTTOM PrODUCT/PID) on 1 st floor (see Figure 4) d. Steam (STEAM/PID) on 1 st floor (see Figure 4)

5 Red Steam Valve (in back) Steam Pressure gauge Blue Water Valve Steam purge valve Figure 4: East Column Reboiler Mixing Pump, First Floor Steam and Water Lines 7. Open and close appropriate manual and control valves so that the system will start under total reflux operation: a. Open the red ball valve on the reflux/distillate line (see Figure 5) b. Open the blue ball valves on the reflux pump line (see Figure 5)

6 Distillate valve This valve open This valve open This valve open Figure 5: East Column Second Floor set-up for Total Reflux Operation c. Use the computer system to open the Reflux control valve (REFLUX/PID). Put the valve in Manual mode. To open the valve: click on the box to the right of MAN ; a small window will pop up; enter 100 and click OK. 8. If reboiler mix-time has exceeded twenty minutes, drain reboiler (Figure 1) sample tap. Drain the dead volume from each. 9. Take a sample of the batch in the reboiler from the reboiler sample tap for running total reflux condition. If you are going to run the column with a feed to reach a continuous steady-state condition, you need to take a sample from the feed tank. And make sure to the difference of the compositions between the feed tank and reboiler is less than 3-5%. (Do we have feed?) 10. Determine reboiler composition by GC. Start-up to run total reflux condition 1. Ensure that the reboiler has enough material and then turn on the air for the 1 st floor by manually opening the air valve fully. The exact position of the valve is shown in Figure 6. Air is needed to operate pneumatic control valves.

7 Figure 6. Air valves for East Column on First floor 2. Turn the water on for the 1 st floor by opening the large water ball valve slightly. (see Figure 4). Water is needed for cooling purposes. 3. Ask the Lab Assistant or the TA to turn on the steam on for the 1 st floor. This can be done in two ways: 1) by manually opening the steam valve. The lab assistant or the TA should use gloves because the valve is not insulated. This valve is a red valve located on the equipment (see Figure 4).(However, this is the main steam valve which is usually on. The steam is infact made on by turning on the steam valve behind the assembly shown in Figure 4). 2) by setting the STEAM/PID on the computer hooked to the East Column in the control room to something like 50%. The steam pressure gauge should read about 20 psi. Steam is needed for heating purposes. Kindly note the sequence of turning on the utilities, it is air first (no cost) followed by water (somewhat expensive) followed by steam (highly expensive). The sequence will be exactly reversed while turning them off. The rationale is to cut-off the steam and save the operating cost as much as possible. 4. Ask the lab assistant or the TA to purge the steam line. a. Make sure the area where the steam will be released is clear of people. b. Open the steam purge valve fully. WEAR GLOVES! This is a blue valve located near the large pressure gauge (see Figure 4). c. Let the steam flow through the valve until the sound of steam exiting the pipe reaches a constant roar (typically 5-10 seconds). d. Close the purge valve. 5. Turn the air on for the 2 nd floor. The air valves are located on the wall to the right of the double doors (see Figure 7).

8 Figure 7. Second floor air valves. 8. Turn the water on for the 2 nd floor by manually opening the water valve completely. This valve is for distillate condenser and is located on the equipment (see Figure 8).. Figure 8. Valves for water on second floor.

9 9. Then go the control room. The computer hooked to the East Column will indicate the values of different parameters like temperature, pressure and flow rates as well as the positioning of different valves. Note that the values of some of the parameters might not be correctly shown on the screen due to some or the other reason and typically such values will be grayed out.you should see the temperature of the material in the reboiler rising slowly. Allow a stable level to be attained in the sight glass. Now, set the Reflux/PID to 100%. It essentially means that you are operating at total reflux. When the sight glass starts getting overfilled, the reflux motor automatically gets turned on and you will see the level of the material in the sight glass. After the level of the material in the stand pipe is at a fairly stable for some time, check if the system has attained steady state or not. This can be done by measuring the composition of one of the streams (reflux is the easiest because it is located on the first floor) as a function of time. When the composition changes by less than 5% with time, the system can be considered to be at steady state. The reflux sample port is located on the second floor. (should we include a figure?). Notes: 1. All composition measurements are done with a Perkin Elmer Gas Chromatography instrument in the Lab. Get help from the lab assistant on using it. (Should we include a operating procedure for GC also?) 2. The general start up procedure followed is the same during all the three weeks. 3. Do not leave the column unattended Drawing off Distillate Product 1. Monitor distillate tank level visually using the sight-glass. If the level in the distillate tank on the 1 st floor. If the tank is full, seek the Lab Assistant for assistance. (see Figures 9). Figure 9. Tanks on the first floor.

10 2. Control the flow of the distillate manually by using the bypass valve shown in Figure? The flow rates of the distillate and the reflux can be obtained by using the rotameters shown in Figure? The flow rate of the distillate and the reflux can then be used to obtain the reflux ratio at which the column is being operated. 3. Measure the composition of the distillate and the bottoms by using the appropriate sample ports. 4. At the end of the run, pump the material from the top product tank back into the reboiler. This makes the comparison more meaningful because the starting material would be the same. Note: If the distillate tank becomes full during operation, seek assistance. Shutting Down 1. As mentioned before, the utilities will be turned off exactly in the reverse order meaning steam first, then water and lastly air. Use the computer system to close the Steam control valve To close the steam valve, click on the display box labeled STEAM/PID located above the valve symbol on the reflux line. Click on the box to the right of MAN. A small window will pop up. Change the opening of the valve to 0 and click OK. Turn off the Steam valve on the 1 st floor. Check the pressure reading on the large pressure gauge (see Figure 4). If it is not zero, open the steam purge valve to release the pressure, then close it. Wait five minutes and check the pressure again. If pressure has built up, then the main red steam valve needs to be closed more tightly. 2. Turn off the reboiler mixing pump (EBTP/PUMP): a. To turn off the reboiler-mixing pump: click on Bottoms/PUMP or the pump icon; if not yet in manual mode, click on Manual ; click Stop and close the window. 3. With the reflux control valve (Reflux/PID) fully open, use the reflux pump (Reflux/PUMP) to drain the standpipe. Turn pump off. a. To open the reflux valve: Click on the display box labeled Reflux/PID located above the valve symbol on the reflux line. Click on the box to the right of MAN. A small window will pop up. Change the opening of the valve to 100 and click OK. 4. Open the red reflux valve (also serves as a manual bypass valve) (see Figure 7). 5. Close manual valves associated with the distillate tank (Figure 9). 6. Turn off the water and air valves by manually turning them fully in the clockwise direction on both floors.

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