ChE 4013

PACKED TOWER EXPERIMENT

Objectives: To generate a Strigle-Leva-Eckert data chart for 5/8 Pall rings and measure gas
absorption characteristics of a packed column.

Chemicals: Air, aqueous sodium hydroxide solution.

Theory: A packed column (or tower) takes liquid in the top of the column while a gas (air in our
case) coming in the bottom flows upward in a countercurrent type arrangement. The liquid flows
down over a packing which disperses the liquid as the gas flows up, and the intent is to amplify
the interfacial area between the gas and liquid. A simplified schematic is given in Figure 1.

Packed columns are used in a number of different processes

where components need to pass from one phase to the other. In
a stripping operation, a volatile component in the liquid moves
to the gas phase, while in an absorption process, a gaseous
component moves from the vapor phase to the liquid. A packed
tower can be used for either type of process.

The packing is a critically important component. An efficient

packing will disperse the liquid effectively and help to facilitate
a large interfacial area between the gas flowing up and the
liquid flowing down. A large interfacial area facilitates a large
capacity for transport of mass from one phase to the other.

We are particularly interested in the hydraulics (pressure drop

and flooding phenomena) of this system. You will also be
studying absorption of CO2 from air using the packed column.

Read Flooding and Loading beginning in the second column

on page 14-41 of Perrys, 7th edition [Ref. 1]. Note that there is a
mistake in equation 14-151. The (G/L) 0.5 should be in the
numerator, not denominator of that equation. The correct
equation is given as the abscissa in Figure 14-48. Also note that Figure 1. Simple Packed Column
the label on the ordinate of Figure 14-48 is wrong. The correct ordinate is equation 14-150, or,
the ordinate should simply read Cs (not CsFp0.50.5). Read up to the section Pressure Drop in
the first column of page 14-42. Make sure you understand the equations, units, and Figure 14-48.

The use of this generalized pressure drop correlation chart has several limitations, detailed in
References 2 and 3. When experimental data are combined with literature values for the packing
factor to create a Strigle-Leva-Eckert data chart, the points do not always fall on the lines of the
chart. Sometimes they systematically fall off the lines. The suggestion of these references is to
combine (interpolate between) the experimental data and the chart lines using a chart specific to
the packing and fluid. No such chart exists for our packing, so we will be creating one.

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We will measure four main variables: 1) liquid flow rate, 2) air flow rate, 3) column pressure
drop, and 4) CO2 inlet and outlet concentrations. We will also record the column temperature
which will be used to look up properties of the two main components, sodium hydroxide solution
and air. The liquid flow rate given in gpm (gallons per minute) will be converted to the
superficial mass rate per square foot of column cross-sectional area, L, in lbm/(sec-ft2) and the air
flow rate given in SCFM (standard cubic feet per minute) will be converted first to actual cubic
feet per minute and then to the superficial mass rate per square foot of column cross-sectional
area, G, in lbm/(sec-ft2). Knowing the densities of air and sodium hydroxide solution, FLG, which
is the abscissa of Figure 14-48, can be calculated. We will also calculate the value of the ordinate
from the column pressure drop and the literature value for the packing factor and plot the point
for each run on the graph. If the point does not fall on the existing lines, we will calculate the
value of the packing factor which makes our experimental points fall on the graph lines.

Packing factors are tabulated in the literature for common packings. In lieu of data for a
particular packing, a common practice is to compute Fp as Ap/3whereAp isthetotalsurfacearea
ofthepackingperunitvolumeofbedandisthevoidspaceinthepacking.

For gas absorption, the efficiency of the process can be expressed in terms of the overall height
of gas-phase transfer units, HOG. The smaller the HOG, the more efficient the absorption process
will be. For dilute systems, HOG is defined as:

G
H OG
K y' a
(1)

K y' a
where is the overall mass transfer coefficient (moles/volume/time).

NOG, the number of transfer units, is a function only of compositions and depends on the
operating conditions, e.g., gas and liquid flow rates, temperature, pressure, etc. It is defined as

y A0 y A1
N OG

y A y *A lm (2)

where y A y A lm is the log mean (average) driving force for absorption. Note that yA0 is the gas
*

phase mole fraction of component A at the entrance (bottom) of the column, yA1 is the mole
*
fraction of A in the exiting gas, and y A is the mole fraction of A in equilibrium with the bulk
liquid. The overall height of gas-phase transfer units is then calculated from NOG:

z
H OG
N OG (3)

where z is the height of packing.

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When sodium hydroxide solution is the liquid phase, a chemical reaction occurs between the CO 2
and the hydroxide, which greatly enhances the absorption of CO2. Chemical reaction in the liquid
phase reduces the equilibrium partial pressure of a solute over the solution, which greatly
increases the driving force for mass transfer. If the reaction is considered to be instantaneous and
irreversible (as is the case here), the equilibrium partial pressure will be reduced to essentially
zero, maximizing the driving force for absorption. In this case, NOG reduces to:

y A0
N OG ln
y A1 (4)

Experimental: A dilute solution of sodium hydroxide (~0.1 M) is circulated via pump and a tank
maintains a liquid inventory. The pump is set up to circulate the liquid continuously through the
tank so that the pump exhaust pressure does not rise too high when the liquid flow rate to the
column is small. As demand for column liquid is increased, the circulation rate through the tank
will subside. Similarly, to keep air pressure from building on the exhaust side of the air pumps,
two control valves are arranged to be complementary. As the valve supplying air to the column
opens, a second valve venting the air (currently going to the Plexiglas tray column) opens, and
vice-versa. Two air pumps in parallel are required to provide enough air. A pressure relief valve
protects the equipment.

A distributor at the top of the column is used to initially break the liquid stream into many
smaller streams that flow down from the top of the column. The distributor uses a cup that has a
number of holes in the bottom that let liquid drain out and four larger holes with stacks that let
air out the top. As liquid flows into the center of the cup, a liquid level builds up inside until the
height of the liquid in the cup provides enough head to force flow out the holes at a rate that
balances the liquid flow rate coming into the cup. Adventurous students may get up on the
stairway/stand and observe the operation of this device.

At the bottom of the column, several things are happening. A riser (gray and about 2" in
diameter) with a cap and side slots allows air in. The cap and side slots divert the air toward the
column walls. Otherwise, air would tend to focus more into a jet that would concentrate in the
center of the column, pushing the liquid coming down the column more toward the outside, thus
attenuating the overall gas/liquid interfacial area. Also at the bottom, liquid draining off the
packing accumulates in the bottom, occupying 6-8" of the column. A capacitance-type level
detector senses this level and reports the value to the Honeywell control system. When facing the
column, the control valve to the left of and below the column is used to control the liquid level in
a typical feedback loop. If a liquid level was not properly maintained in the bottom of the
column, supply air would tend to go out the drain port with the liquid and get into the intake of
the pump. This is an operational difficulty that should be avoided as much as possible. Finally,
the bottom flange also contains a tap that connects into a differential pressure transducer which
measures the column pressure drop. The other side of the pressure gauge runs to the top of the
column. Students should also observe the devices and connections in the bottom of the column
under operating conditions.

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Familiarize yourself with the column. Photographs with critical components marked are attached
in the Appendix. Trace the lines running from the air compressors to the air riser in the bottom of
the column. The air flowrate is measured by an orifice meter in the PVC pipe. Trace the liquid
lines beginning at the lower left tap in the bottom of the column running down through the liquid
level control valve, into the pump, through the silver metal turbine meter, and up to the top.
Some valving around the bottom of the tank can be used to drain and circulate liquid through the
tank. Find the differential pressure transducer and trace the lines into the top and bottom of the
column. Review the column in person carefully.

For CO2 measurement there are two electronic boxes, a CO2 scrubber, and a control on the
column control page to switch the CO 2 system on and off. A valve allows you to direct the inlet
or the outlet gas flow to one of the detectors. You can use this to determine the offset between the
two detectors. Another method that will give you a different value of the offset is to run air
through the column with no liquid and compare the inlet and outlet concentrations, but this is not
the preferred method.

Procedure:
1. Column preparation: Empty the sodium hydroxide solution from the air line by opening the
air line drain valve below the column, draining liquid, and closing the valve. Return solution to
the supply tank. The riser seal leaks, but its repair requires disassembling the column. Empty this
line every two hours during your experiment with the air control valve closed. Measure the zero
offset for the column pressure drop. Check that the manual valves in the liquid return from the
column to the pump are open.

2. Check the pH of the solution in the tank with pH paper to make sure that the sodium
hydroxide concentration is about 0.1 M. A fresh NaOH solution may be made by mixing 400 g of
NaOH pellets with 100 liters, but do this only on instructions from the faculty instructor.

3. Power setup: Check the emergency shutoff switch and the two compressor electrical boxes
on the front panel. The emergency shutoff switch should be pulled out, and the two boxes should
have the "Auto" switches set on. Bring up the "Packed Column" display in one instance of
Experion (see the Honeywell operating instructions if necessary).

4. Unlock and enable the pump: The pump is normally left locked out and tagged out at the end
of each lab. The tag will say who has the key. Unlock the three valves isolating the pump. Open
the inlet valve to the column completely and the other two halfway. Change the pump control
box from Off to Auto. The liquid flowrate controller on the Honeywell system is locked out
with a Red Tag, too. You will not be able to change the OP for the sodium hydroxide control until
the Red Tag is removed. If you try to change the OP, the following error message will appear:

.
To clear the Red Tag so you can run the equipment, you must log in as manager (mngr). Double
click on the NaOH control box. On the Main tab, find the section labeled Safety interlock, Red

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tag, and Operator tag. Uncheck the box next to Red tag. You should now be able to change the
OP for the NaOH controller from the main display page.

5. Control valve preparation:

a. Put the liquid flow loop in MAN and set the controller output to 25% (OP = 25%).
b. Put the level control loop into MAN, and set the controller output to zero (OP = 0%).
c. Put the air flow loop into MAN, and set the controller output to 25% (OP =25%).

6. Power up: Click on the empty buttons for the pump, both compressors, and the CO2
Absorber System to turn them on. They will be filled with a when they have been turned on
(the may take a few moments to appear) and the pumps will crank up.
Watch for liquid coming out of the liquid distributor cup at the top of the column, and in a
minute or two, liquid will start flowing down the column. If no liquid is flowing, consider
increasing OP to 30 or 35%. As the liquid works its way down the packing, it will begin
to drip off the packing and into the bottom of the column.

7. Establish liquid level control: When liquid is dripping from the packing and the liquid level
in the bottom of the column is about 4" or more (there is likely at least that much left from the
last time the column was run), set the level controller output to 25% (OP = 25%), then switch the
level controller to AUTO mode.
The trick here is to give the level controller a reasonable starting point. You would prefer
not to overfill the bottom as the liquid will go back into the air riser, but you also do not
want to drain the bottom dry because as air will get into the intake side of the pump.
Thus, you do not want the level controller to open before there is a liquid supply draining
from the packing. The level controller will generally take over without complications and
bring the level to a stable value.

If you drain the bottom of the column dry and air gets in the intake of the pump, the
liquid supply rate to the column will drop and it might even quit flowing completely. To
fix this, proceed as follows:

1. Put the level control valve into MAN mode and close the valve (OP = 0%). This will
stop air from flowing into the intake side of the pump, and liquid from the supply
tank will replace the air in short order.
2. Put the liquid supply valve into MAN mode and set OP = 25% if that is not already
done.
3. Wait for the pump to expel the air and watch for liquid to appear at the top of the
column.
4. Continue to wait as liquid travels down the column and begins to collect in the
bottom.
5. When about 4" of liquid has collected in the bottom of the column, set OP = 25% on
the level controller then switch the level control valve to AUTO mode.

The controller should bring the level to a stable value in a few minutes.

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If you overflow the bottom and liquid goes into the air supply riser, usually, you do not
need to do anything but wait for a minute and see that the level controller gets control and
brings the level down. If you are operating under high liquid flow rates, cut the liquid
flow rate as quickly as possible, but if you are just starting up the column, you should
probably just be patient. Once the upset has subsided and level control is established,
close the air control valve. Then, go into the lab and open the air line drain valve at the
bottom of the column to drain out the liquid that went into the air riser. Close the air line
drain valve and open the air control valve.

If you experience any problems that you do not understand, and the liquid level is rising
in the column such that it has completely covered the air riser and is still rising, shut off
the pump and both air compressors with the pushbuttons on the control page, or in an
emergency, go into the lab and hit the emergency shutoff switch.

8. Establish liquid and vapor flowrate control: Once the column is started up, liquid is flowing
down the packing, and the liquid level is stable in the bottom of the column, set the liquid flow
rate to 1 gal/min (SP = 1.0) and switch the liquid supply flow controller to AUTO mode. Set the
desired air flow rate (SP = 5) and put the air flow control loop into AUTO mode.

9. Packing Factor Experiments: Note what the pressure drop is at 1 gpm liquid and 5 scfm air,
and adjust both the liquid and gas flowrates until the pressure drop is 0.1 inches of sodium
hydroxide solution per foot of packing. Record the liquid flow rate, air flow rate, column
pressure drop, column temperature, and CO2 inlet and outlet concentrations (this is one
experiment). Repeat the experiment near 10 SCFM and 0.25 inches per foot of packing.
Generate at least 6 data points at 0.50 inches per foot of packing and 15 to 20 SCFM and another
6 data points at 1.0 inches per foot of packing and 25 to 30 SCFM.
Do not change the liquid rate more than 1 gal/min in any single change. After making a
liquid rate change, wait for the level in the bottom of the column to stabilize before
changing it again. Remember to drain the liquid from the air riser every two hours or so
during the lab.

10. Absorption Characteristics Experiments: collect data for at least five different liquid
flowrates at a constant gas flowrate.
Do not change the liquid rate more than 1 gal/min in any single change. After making a
liquid rate change, wait for the level in the bottom of the column to stabilize before
changing it again. Remember to drain the liquid from the air riser every two hours or so
during the lab.

11. Shut down the column.

a. Bring the liquid flow rate to 1 gal/min in steps of no more than 1 gal/min, waiting for the
level in the bottom to stabilize between changes.
b. Put the liquid supply control valve in MAN mode.
c. Set OP = 25% on the liquid flow control valve.
d. Wait for the bottom level to stabilize.
e. Turn off both compressors and the CO2 detectors and immediately change the level
controller to MAN mode. Set OP = 0% on the liquid flow control valve to close it.

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f. When most of the liquid has drained from the packing or if the liquid level falls to 4" or
less, close the level control valve (OP = 0%) and turn off the pump. Close the remaining
control valves and the valves isolating the pump. Lock out and tag out the valves
isolating the pump. Set the electrical control for the pump to Off. Return the key to the
person named on the tag. Red tag the NaOH control on the Honeywell system.

12. Check that the concentration of the supply tank is still about 0.1 M.

Data: The inside diameter of the glass column is 150 mm = 5.91". The packing is 5/8" steel Pall
rings, and the length of the packed bed is approximately 42 (students should measure it).

Prelab Report Calculations:

1. The equipment is capable of producing more than 30 SCFM and higher liquid flowrates. For
what other physical reason might we not want to try for 1.5 pressure drop per foot of
packing?
2. Assuming the height of the packing in the column is 42, calculate the pressure drops
required to reach 1.0, 0.5, and 0.10 inches per foot of packing.
'
3. V L From the given data, calculate H , N , and K y a . Plot the data point (using the
OG OG
experimental FLG and Cs calculated using literature packing factor) on Figure 14-48 from
Perrys. If this point (using the literature packing factor and experimental FLV) does not fall
on the experimental pressure drop line, determine the value of the packing factor that will
make the point fall on the right pressure drop line using the same experimental FLV. Include
an error estimate for each calculated value. Show hand calculations.
VG = 17.5 + 0.1 scfm, = 4.2 + 0.1 gpm, h = 1.75 + 0.03 inches, T = 74.5 + 0.1F,
yA0 = 470 + 1 ppm, and yA1 = 275 + 2 ppm.
When the outlet gas is routed to the inlet detector, yA1(0) = 280+ 1 ppm.
4. Fill a 1 liter (or larger) beaker with 5/8" Pall rings. Do not use a graduated cylinder because
the rings are too large to pack randomly in the narrower device. Count the number of pieces
and weigh the packing material. Measure an individual piece with a ruler or micrometer and
make the calculations of Table 1 on the next page: Compare these numbers you have
calculated with properties in Perrys handbook, 5th Edition (see Appendix) and with data from
the Sulzer website. Did you do your measurements and calculations correctly?

Prelab Quiz
Your prelab quiz will be to individually demonstrate that you can successfully get the sodium
hydroxide solution flowing and the level controller in auto with the flowrate and level both
stable.

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Table 1. Physical measurements of the packing

Your calculations from Perrys 5th

pieces of packing / liter ------

pieces of packing / ft3

weight of packing / liter (g/liter) ------

weight of packing / ft3 (lbm/ft3)

surface area (in and out) of a single piece (in2) ------

surface area (in and out) of a single piece (ft2) ------

surface area in one ft3 of packing (ft2/ft3)

Suggested Calculations and Report Requirements:

1. Make a copy of Figure 14-48 in Perrys and place a point on the graph for each of your
data points, assuming that the literature packing factor is correct. Use a different shape for each
pressure drop. If the experimental data do not fall on the right pressure drop lines, calculate the
value of the packing factor that makes the experimental points best agree with the graph. Are
there any trends in discrepancies with liquid and gas flow rates? If so, explain.
2. Compare your best fit packing factor to the literature values and to that computed from
Fp = Ap/3.
3. Calculate HOG and NOG for each set of conditions. Also calculate the mass transfer
'
coefficient K y a for each condition. Calculate the uncertainties for your values. Are you able to
K y' a
see any trend in values with liquid flow rates?

References:
1. Perrys Chemical Engineers Handbook, 7th Edition, Robert H. Perry and Don W. Green,
Ed., McGraw-Hill, 1997.
2. Henry. Z. Kister and David R. Gill, Chemical Engineering Progress, February 1991, p.
32 42.
3. Henry Z. Kister, Distillation Design, McGraw-Hill, 1992, p. 492 506.
4. Perrys Chemical Engineers Handbook, 5th Edition, Robert H. Perry and Cecil H.
Chilton, Ed., McGraw-Hill, 1973, p. 18-24.

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Appendix: Perrys Data and Equipment Pictures

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From Reference 4, p. 18-24.

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Sodium hydroxide solution
tank

Air flowrate control

valves

Sodium hydroxide solution

pump

Air compressors

Figure 2. Air and sodium hydroxide solution feed equipment

Emergency Compressor
cutoff switch switches Level detector

Air riser
Pump
switches

CO2 detectors

Level control valve Drain valves

Figure 3. Control panel and bottom of column equipment

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Air outlet

Thermocouple

Distributer cup

Differential pressure cell

Liquid flowrate
control valve

Figure 4. Equipment near the middle and top of the column

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