Startup and Operation Procedure for the Technovate Still

Note: sampling procedure and times are described in the Experiments

Background
The Technovate still was purchased in 1981 and has undergone a series of upgrades. The most recent
upgrade, completed in the summer of 2000, included the addition of an OPTO 22 LCSX programmable
logic controller (PLC) and the writing of the necessary control software. A Window computer using
Factory Floor software drives the LCSX.

The distillation column is probably the most expensive and complex single piece of equipment in the
undergraduate lab. Computer control of the distillation column is essential for its operation. Care must be
taken when running the column to ensure both safety and accuracy of results. Students must read and
follow the startup procedure given below. Failure to do so may result in removal from the lab and failure
of the course.

Each instruction contains information about what is to happen after you have successfully completed it. If
the system responds differently, consult the instructor before proceeding.

A. Preliminary Preparations.

1. Turn on the power to the still by throwing the “Main Power” switch located in the center front of
the still. Only the red light above this switch should be illuminated. If any other lights are come
on, turn off the switch below them.

2. Place the reboiler power switch to “Manual” (the upper position). This switch is located to the
right of the pumps under the shelf holding them. Locations of switches and valves on the rear of
the still are shown in Figure 1

Fig. 1 Locations of Important Controls on the rear of the distillation column

3. Turn on the computer by pressing the orange switch located on the power strip. This switch also
turns on the PLC and the I/O boards. Turn on all the toggle switches for the power units for the
PLC, which is located on the wall along side the computer. A pair of red LEDs on the
programmable logic controller (PLC) should glow red. The PLC is the white box in the metal
panel with the clear door.
4. The computer should start. Once Windows has completed its startup, launch OptoDisplay
Runtime. Under “Start”, select
“Programs\Opto 22\FactoryFoor R4.1a\OptoDisplay\OptoDisplay Runtime” from the Start Menu.
OptoDisplay Runtime should open and load the still software. The screen should be similar to
Figure 2 below.

Fig. 2 OptoDisplay with Distillation Software loaded

If the still schematic does not appear, see your instructor. NOTE: Do not open any Opto
applications other than the ones you are instructed to. The applications for creating and modifying
the OPTO software are included on the computer for the convenience of the instructor and others
using the equipment. Students are not permitted to modify or tamper with the OPTO programs or
the computers. Violations of this rule can result in immediate removal from the lab and failing of
the course.

5. Click “Start”. Select “Programs\Opto22\FactoryFloor R4.1a\Opto Utilities\OptoTerm” from the

Start Menu. A dialog box should appear showing a list of controllers. The screen is shown in
Figure 3.

Fig 3 OptoTerm Dialog

Click on “ChE Lab 2”. The background for the text will turn blue and a dialog box will appear as
shown in Figure 4 below:
 Fig. 4 OptoTerm Dialog Box

Click the button marked “Run”. This operation turns on communication between the PLC and the
I/O boards. All six LEDS on the PLC should now be flashing red. The temperatures on the
schematic should now be reading room temperature (about 20C). If they are not, report the
situation to your instructor. If everything is functioning, close OptoTerrm.

6. The computer software is equipped with audio alarms. These alarms will alert you of situations
that will require operator action when the still is in automatic mode. If they are activated during
startup, they can be very annoying. Open the “Alarms” window in OptoDisplay Runtime by
selecting the “Window” menu option. Select “Alarms” from the list of windows. If “Alarms” is
not listed, select “open” and select alarms from the list. The radio button next to “Off” should be
green. If it isn’t and the alarms are sounding, click either the “Off” button or the radio button
along side it. This step may not be necessary if the computer’s speakers are turned off or not
connected.

7. Open the Main Still Controls Window in OptoDisplay if it is not already open. Open the window
by clicking the “Window” menu option. Click “Main Still Controls” from the list of windows.
Click “Manual” under the “Mode of Still Operation” list in the upper right hand corner of the
window. .

8. Open the Manual Control Window. Clicking the “Window” menu option. Click “Manual Still
Controls” from the list of windows. Set all the controls to 0 so that the pumps are turned off.
Factory Floor controls the pump rate of the peristaltic pumps. User settable values in Factory
Floor are shown as yellow text on black background. Move the mouse over a value and a box
appears around it. Click on the value and a window appears that allows you to enter a new value.

9. Turn on the power to the pumps by turning on the power strip located under the shelf.. You
should do this AFTER the PLC is started to prevent the pumps from running with nothing in them.

10. You have now turned all the equipment on.

B. Draining and Filling the reboiler

1. Check the liquid level in the reboiler. If the level is low, or if the column has not been recharged
since it was last used in the production mode, you will have to drain the column. If you do not
have to drain the column, skip to step 5. You may check the level by checking the sight tube on
 the side of the reboiler. The reboiler is the large aluminum covered device directly underneath the
distillation column.

2. Open the manual drain valve behind the reboiler. DO NOT open the drain valve directly under the
reboiler because this can cause material to spill onto the floor.

3. On the controls in the front of the still, put the drain switch to open. The drain switch is directly
under the boiler power switch. You should hear a relay and the light above the switch should
come on.

4. Wait until the tank has drained as indicated by the level in the sight tube. Then close the manual
drain valve and move the drain switch to “Auto”.

5. Connect the feed line to the reboiler. The feed line is the long tube that passes through the still
panel near the top of the column. A quick connect fitting is at the end. Attach the quick connect
to the reboiler connection. Pull back on the outer ring on the quick connect, while holding the
outer ring back, slide the quick connect over the male fitting on the top of the reboiler. Release
the outer ring. You should hear the quick connect lock. Pull on the quick connect to check that it
has properly seated. It should not pull off the male connector.

6. Open the valve labeled “FlowMeter Bypass”. This valve opens the feed from the centrifugal
pump.

7. Turn the feed pump on. The feed pump switch is located on the left of the row of switches on the
front of the still. You should hear the pump and liquid flowing into the still.

8. Fill the reboiler until there is only about 2 inches of air left in the sight tube located on the left of
the reboiler.

9. When the reboiler is filled, turn off the feed pump and disconnect the feed line. Disconnect the
feed line by pulling back on the outer ring and sliding the quick connect off the reboiler
connection.

10. You have now filled the reboiler.

C. Starting the distillation column and running at Total Reflux

1. Turn on the condenser cooling water. The valve is located on the wall behind the still. A hose
runs from the valve to the still. Set the flow so that the condenser rotameter reads between 0.5 and
1. The condenser rotameter is located on the front of the still, to the right of the condenser.

2. Verify that the Feed , Tops Product and Reflux pumps are turned off by checking the “Manual
Controls Window”. Also, verify that the manual drain valve behind the reboiler is shut. Verify
that the feed line is disconnected.

3. Turn the reboiler power on. The reboiler power switch is located below and to the right of the
main still power switch. Red lights above the reboiler switch and the “Boiler Temp.” light should
go on. It will take some time for the reboiler to heat the liquid to boiling. YOU MUST STAY
WITH THE COLUMN AT ALL TIMES WHEN THERE IS POWER TO THE REBOILER.

4. Adjust the boiler power to about 10 amps. The control to adjust reboiler power is located just
below the “Boiler Temp.” light. The ammeter is located to the left of the main power switch and
is labeled “AC amperes”. Adjust the knob until the ammeter reads 10 amps.
5. Drain the accumulator to a level until it has no more than about 1 inch (about 10 on the “Still
Conditions” screen). This minimizes accumulator hold up for batch runs and allows time for
actions when condensation begins. If the accumulator is already at this level, skip to step 10.

6. Open the valve on the tops line to the feed tank located on the rear of the still. The feed tank is the
red tank behind the still on the base of the still in Figure 1. The feed tank valve is directly above
it. Open this valve and shut the valve to the product line. The product line is the line with a
plastic hose.

7. Open the “Manual Valve Control” window. Turn on the Product pump by setting the value for
“Product (%)” to 100. Set the controller by moving the mouse cursor to the YELLOW numbers
on BLACK background next to “Product %”. Yellow on black denotes values you can adjust
from the computer. When a rectangle appears around the number, click the left mouse button. A
dialog box will appear. You should hear the pump running and see the level of liquid in the
accumulator go down.

8. When the level of liquid in the accumulator is 2-3 cm or less, shut off the reflux pump by setting
the Product (%) value to 0.

9. Zero the product integrator in OptoDisplay Runtime by moving the mouse cursor over the yellow
word “Zero” in the still conditions window. The product should read 0

10. Switch the PLC to “Total Reflux”. On the “Still Conditions” screen, press the black button next to
the words “Total Reflux”. Open the “Total Reflux Control” window.

11. The controllers have two modes of operation “Manual”, in which you set the signal to the pump
and “Automatic”, in which the controller sets the pump. The radio button next to the work
“Manual” at the bottom of the controller should be green, indicating that the controller is in the
manual mode. If the radio button is not green, move the mouse cursor over it and click the left
mouse button.

12. Set the Accumulator Level PID controller output to 0. Controller outputs are scaled from 0
(closed) to 100 (fully open). Enter the number 0 in the box and click “OK”. A 0 will appear at the
value you entered. DO NOT ATTEMPT TO ADJUST THE PID SETTINGS UNLESS TOLD TO
BY YOUR INSTRUCTOR.

13. Watch the temperatures as the reboiler and the column heats. Several temperatures are displayed
on the upper graph of the main screen of the Stills program. All the temperatures are displayed on
the schematic of this screen. A more complete graphical display can be found by opening the
“Temperatures” window. Open the “Temperatures” window by selecting the “Window” option
from the OptoDisplay Runtime menu and selecting “Temperatures”.

14. Verify that the total reflux controller is in Manual mode and the output is set to 0. Open the “Total
Reflux Control” window. The yellow numbers to the right of the word “Output” should be 0 and
the radio button by the word “Manual” should be green..

15. When the tops temperature (T5) reaches 50C, turn the reboiler power to 7 – 8 amps by adjusting
the “Boiler Temp;” knob on the panel on the front of the still.

16. Allow the level in the accumulator to rise to about 5 cm (two inches). Set the Accumulator Level
PID output to a setting of 20. Then adjust the setting so that the accumulator level stays
approximately constant. The signal from the accumulator will continue to fluctuate as a result of
noise.

17. When the level has been held constant in the manual mode for about 5 minutes, switch the control
to automatic. FIRST, enter the set value equivalent to the current input. Enter this value as you
 did the output signal to the valve. The new set point will appear in yellow. SECOND, switch the
controller to automatic by moving the mouse cursor to the button labeled “Automatic” and
clicking the left mouse button. The radio button next to the word “Automatic will turn green and
the radio button next to the word “Manual” will turn white. The controller will maintain a
constant level in the accumulator. The output signal and the flow will fluctuate slightly.

18. Wait several minutes to verify that the controller is smoothly adjusting level and the still is at
equilibrium.

19. The controller software is equipped with audio alarms that are triggered by events that may require
direct operator action. Enable these alarms by opening the “Alarms” window and clicking the left
mouse button when the cursor is over the word “On”.

20. If your instructor tells you to, turn on the reflux preheater. The reflux preheater switch is located
next to the “Boiler temp” knob on the still front panel. Set the dial to about 5. Both lights over
the dial should come on. The light on the left indicates that the reflux preheater is activated. The
light on the right indicates that power is actually going to the preheater. There is an automatic
cutoff to the preheater to protect it from overheating. The light on the right may go out briefly but
should, in general remain on. Ad just the knob carefully to bring the reboiler feed to within 4
degrees of the tops temperature.

21. You are now running the still under total reflux. This operation can continue indefinitely with the
computer controlling the still.

D. Batch Distillation at Constant Reflux Flow

1. Begin by starting the column and running it under total reflux under automatic control for about
ten minutes so that the system can achieve equilibrium. Allowing the equipment to reach stable
equilibrium is called “lining out”.

2. Place a large (1 L or greater) beaker on the floor alongside the still, where you can easily see it
from the computer desk. Place the end of the hose in this beaker. Do not let the beaker overflow
while you are distilling product.

3. Verify that the tops line valve to the beaker is open and the valve to the product tank is closed.
These valves are located just above the feed tank, which is the red tank behind the still panel on
the floor of the apparatus (see Figure 1).

4. Open the “Main Still Controls” Window in OptoDisplay and select the mode of operation “Batch,
Constant Flow”

5. Open the “Constant Reflux Flow” window. Reduce reflux flow to about 75% of the total reflux
flow by adjusting the value for “Reflux %” to about ¾ of the average value the controller was
maintaining.

6. Set a value for the “Product PID” “Output” that maintains a constant level in the accumulator.
The still will begin sending tops product to the container. When the accumulator is approximately
constant, set the “Set” value to the current value of “Input” and click the button labeled
“Automatic”. The radio button next to the word “Automatic” will turn green. You may want to
increase the distillation rate by increasing reboiler current to ~8 amps

7. Allow the system to line out. Collect the material produced during this time but keep it separate
from the material collected once the system has stabilized. DO NOT ZERO THE INTEGRATOR
IN OPTODISPLAY WHILE YOU ARE DISTILLING PRODUCT.
8. You are now operating the distillation column in batch mode at constant reflux flow. The
distillation would continue until enough of the more volatile component were removed to move
the conditions to total reflux (or until the still was empty).

E. Batch Distillation Constant Temperature

1. Begin by starting the column and running it under total reflux under automatic control for about
ten minutes so that the system can line out.

2. Open the “Constant Temperature” window by selecting the “Window” option. If the “Constant
Temperature” window is not in the list of opened windows, select “Open” and select “Constant
Temperature” from the list. It may take a few seconds for the window to start displaying values.

3. Verify that the controllers in the “Constant Temperature” window are in the Manual mode. The M
for each controller should be yellow. If they are not, move the mouse cursor over the “M” and
click the left mouse button.

4. Turn the audio alarms “off” by moving the mouse cursor over the word “Off” on the “Alarms”
window.

5. Switch to the “Constant temperature” mode by clicking the radio button next to the words “Batch,
Constant T”. The button should turn red.

6. Reduce the preheater power (if it is turned on) by at least one half unit

7. In the controller labeled “Temperature PID” enter the desired control temperature. Reduce the
pump setting to about one half its current value.

8. Gradually reduce the reflux flow and the reflux preheater until the temperature rises to the desired
operating temperature. You may also have to increase the reboiler power.

9. When the still tops is at the desired temperature and steady, switch the temperature control to
automatic. Manually adjust the product flow until the level is approximately steady, make the set
point of the product control the current level and switch the controller to automatic.

10. If the temperature control is unsteady, switch the controller back to manual, line the column
conditions manually and reattempt to switch to automatic mode. It makes take several attempts to
switch to automatic.

11. You are now performing a distillation while maintaining at constant tops temperature. For a
binary distillation, this should be equivalent to maintaining a constant composition at the tops.

12. Distillation will continue until 1) breakthrough will occur and the tops temperature will start to
rise dramatically, 2) the reboiler level drops to a point where the automatic cutoff turns off the
reboiler power, 3) no more product is collected, or 4) you shut down the still

E. Normal Shutdown from Batch Distillation

1. Turn the audio alarms “off” by moving the mouse cursor over the word “Off” on the “Alarms”
window and clicking the left mouse button.

2. Set the Product PID to manual and set the Product Output to 0. This shuts off the product pump.
Switch the mode of operation to Total Reflux.
3. Set the reflux controller to automatic if it is not there already.

4. Follow the steps for Normal Shutdown From Total Reflux

F. Normal Shutdown from Total Reflux

1. Turn off the reflux preheater and allow it to cool to 65 C. The preheater should be cooled before
the distillation process is stopped.

2. When the reflux preheater temperature is <65 C, turn off power to the reboiler.

3. About one minute after turning off the reboiler, shut off the reflux pump and return the PLC to the
Manual mode by clicking the radio button next to the word “Manual” on the “Still Conditions”
screen.

4. On the “Still Conditions” window, switch the mode to manual by moving the mouse cursor over
the black button next to the word “Manual” on the “Still Conditions” screen and clicking the left
mouse button

5. When no more material is coming from the condenser, turn off the cooling water. The valve is on
the wall behind the still

6. Shut off the main power switch for the still. On the control panel in the front of the unit.

7. Turn off power to the pumps by turning off the power strip under the shelf on the rear of the still.

8. Turn off all the toggle switches to the power supplies for the PLC and I/O boards.

9. Exit OptoDisplay Runtime. The history files of your run will be found in the “C:\Still Data”
folder. Your files will have the names Rd000mmdd.*** where mm = the month, dd= the date and
*** are the extensions (there will be at least two). These files are in ASCII and can be converted
by Excel to a spreadsheet. Excel is on the distillation column’s computer so you can convert them
to Excel format and save them to a flash drive. Leave the files on the still computer as a backup.

10. After you have copied your files, exit Windows and shut down the computer.

11. Turn off the power to the computer and the PLC by turning the power strip at the computer desk
off.

12. You have shut down the still. You may now leave the lab.

Rev. 8/26/8 CRN