1

STUDY AND DESIGN OF PACKED TOWER FOR

ABSORBING GASES WITH LOW SOLUBILITIES

Heat and Mass Transfer Laboratory project by

Vishal Surana
Vivek Nagar
Vivek Nigam

under the guidance of

Dr. A. Kannan and Dr. R. Ramnarayan

Department of Chemical Engineering

Indian Institute of Technology Madras
Chennai - 600 036
 2

Contents

Topic Pages
1 Acknowledgements 1
2 Introduction 2
2 Brief outline of issues tackled in this project 4
3 Theory of gas absorption 5
4 Determination of HTU and NTU for various packing 7
 Experimental Procedure
 Precautions to be followed
 Experimental Observations
 Sample Calculations
 Error Analysis
5 Design of packed tower using different packing 16
 Introduction
 Theoretical Predictions of model
 Experimental Observations
6 Design of optimum packed 18
 Introduction
 Matlab Code for finding out the optimal packing
 Experimental Observations
7 Results and discussion 24
8 Suggestions for improvement 24
9 References 25
 3

Acknowledgements

First of all, we would like to thank Dr. A. Kannan and Dr. R. Ramnarayan for giving us
an opportunity to design our own experiment. And at the end of it, we have to accept the
fact that it was a very challenging experience and but for their constant guidance and
support the project couldn’t have been completed. To have come up with not only an
experiment but to also have put forth a general strategy to design packed towers has
indeed been a very thrilling and satisfying experience. We would also like to that Dr.
Krishnamurthy and Mr. Meghanathan of the Chemical Engineering Workshop
Laboratory who were very patient and helpful throughout the course of this project.
 4

Introduction

Gas absorption is one of the major mass transfer unit operations used in the separation or
purification of gas mixtures. The operation is carried out by contacting the gas with a
liquid solvent, usually in a packed or plate column. The dissolved solute is frequently
recovered by thermal "desorption" or "stripping", and the regenerated solvent is recycled
to the absorption column.

Among major industrial uses are the absorption of SO3 in oleum in the production of
H2SO4, and of HCl and NO2 in water in hydrochloric and nitric acid manufacturing.
Another major application is the purification of various process streams to prevent
pollution, corrosion, catalyst poisoning or condensation in subsequent low temperature
treatment. Examples of these applications are the large scale removal of CO2 from air or
natural gas prior to liquefaction, absorption of sulphur compounds from natural gas and
CO2 removal from ammonia synthesis gas.

A packed bed is a hollow tube or pipe that is filled with a packing material. The packing
can be randomly filled small objects like Raschig rings or else it can be a specifically
designed structured packing.

The purpose of a packed bed is typically to improve contact between two phases in a
chemical or similar process. Packed beds can be used in a chemical reactor, distillation
process, or a scrubber, but packed beds have also been used to store heat in chemical
plants. In this case, hot gases are allowed to escape through a vessel that is packed with a
refractory material until the packing is hot. Air or other cool gas is then fed back to the
plant through the hot bed, thereby pre-heating the gas feed.

Distillation columns with packing are often called packed columns. Columns used in
certain types of chromatography consisting of a tube filled with packing material can also
be called packed columns and their structure has similarities to packed beds.
 5

A packed column is usually favorable, when

1. Only a small pressure drop is allowed in the column (for example in vacuum
columns).
2. The components are corrosive.
3. The diameter of the column is small (below 1 m).
4. The hold-up must be small (for example due to thermal decomposition).
5. The liquid foams.
 6

Brief outline of issues tackled in this project

1. Study the mass transfer from gas to liquid phase in a tower filled with random
packing.
2. Explore how changing the water flow rate affects absorption. Carbon dioxide gas
flow rate is fixed.
3. What are the HTU and NTU for this condition?
4. Compare the changes in gas absorption arising due to using different kind of
packing.
5. Study the performance of a tower having different packing of various heights.
6. Optimize the tower packing so as to reduce the cost of packing used.
 7

Theory of Gas Absorption

The simpler theoretical equations for gas absorbers serve three main purposes:
They are used to "design" the column, i.e., to find the height of a column necessary to
achieve a given separation.
They are used in adapting an existing column to a new process or to new operating
conditions. The problem might then be: what flow rates should be used to achieve a given
separation, knowing the mass transfer and equilibrium characteristics of the system?
Finally, they can be used to evaluate the mass transfer characteristics themselves from
measured concentrations and flow rates. The experiment described here falls in this
category.

In all the three cases, what is needed is an equation relating all the system variables, i.e.:
Concentration=f(height of column, flow rates, mass transfer rate, feed concentration)

Since CO is sparingly soluble in water, operation of the scrubbing column requires large
2

water to air flow rate (L/V) ratio. If the L/V ratio is too small, the flow rate of CO in the
2

effluent gas stream will be almost the same as in the incoming gas stream and the
operating line will appear to be almost horizontal. To achieve a large L/V ratio, operate at
low gas flow rates and CO concentrations. Under these conditions, the concentration of
2

CO in the effluent gas stream will be significantly smaller than in the incoming gas
2

stream.

Let
a is the interfacial area per unit volume (m2/m3)
c* is the solubility of CO2 in water at 250C (mol/l)
c is the bulk concentration in the differential element (mol/ l)
dZ is the differential length of the column taken for consideration (in m)
S is the cross sectional area (m2)
Co is the concentration of CO2 in the output liquid stream (mol/ l)
 8

L is the liquid flow rate (m3/hr)

Ka is the liquid phase mass transfer coefficient (in m/hr)

L dC = S a dZ Ka (c - c*)

co
L dc
Z 
S  K a  a 0 c * c

Z = HTU X NTU

co
dc L
NTU =  c * c
0
and HTU =
S * Ka * a

HTU values generally vary with gas and liquid flow rates, going through a minimum and
rising again as flooding conditions are approached. In order to reduce the tower cost, it is
advantageous to operate near this minimum, and one of the objectives of the present
experiment is to study the variation of HTU with L to establish the region of optimum
operation. In addition, the experiment provides an opportunity to test various mass
transfer concepts and design procedures taught in mass transfer courses.
 9

DETERMINATION OF HTU AND NTU FOR VARIOUS PACKINGS

Experimental Procedure

Start up

1. Switch on the CO2 heater and heat it for about an hour or so so as to prevent cold

carbon dioxide from damaging the pipes.

2. Prepare 0.05N NaOH solution in distilled water. For preparing a 0.05N solution,
weigh out NaOH (1g for 500 ml) in a beaker and add distilled water (500 ml) in it
and stir the beaker to get a uniform solution.

Building the Column

1. Disconnect all the pipes connecting the tower to the water and the gas supplies.
2. Unscrew the nuts and bolts using a spanner.
3. Empty the earlier packing, and then fix the tower back to its original place.
4. Fill the tower with the desired packing. Use a wire gauze to make the flow of
fluids more uniform.
5. Screw back the nuts and bolts using a spanner.
6. Connect the supply lines, and test the tower for any leakages. If there are no
leakages then we can go ahead with the next stage of the experiment.
7. Before starting the experiment, the water flow is turned on full to allow air
bubbles to escape, and to clean the column.

Mass transfer process

1. Open the appropriate valves to start CO2 gas flow to the system. Control the CO2

flow rate using the valve.

2. Similarly adjust the liquid flow meter.
 10

3. Meanwhile when the system reaches steady state take a sample of the output
liquid stream.
4. Titrate known volume of the sample against 0.05N NaOH solution using
phenolphthalein as indicator.
5. Repeat the procedure for different liquid flow rates.

Shut down

1. Turn off water flow to the system by closing the water valve
2. Close the CO2 gas cylinder. Check that the pressure gauges on the cylinder read

zero.
3. Close all valves on the CO2 inlet line, starting from the gas cylinder and working

up to the flow meter.

4. Unplug the CO2 gas heater.

Precautions to be followed

1. All the apparatus should be rinsed with distilled water and dried before every
titration.
2. System should be allowed to reach steady state for every reading.
3. Liquid flow rates tend to fluctuate quite a lot, and so care must be taken to ensure
that it is reasonably constant.
4. During titration, the indicator must be added in minimal quantities.
5. Do not leave pressure in lines after shut down.
 11

Experimental Observations

Gas Rate=2.5m3/hr
Height Z=0.9m
C*=0.0329

Data for rashcig rings

Water Flow Initial Final Volume of base Concentration
Rate(LPH) Volume(ml) Volume(ml) required(ml) of CO2 (M) NTU HTU(m)
30 0 3.2 3.2
0.0020 0.0566 15.8958
50 8 13 5
0.0031 0.0937 9.6045
70 13 16.2 3.2
0.0020 0.0566 15.8958

Variation of NTU with liquid flow rate

0.1000
0.0800
NTU(m)

0.0600
0.0400
0.0200
0.0000
0 20 40 60 80
Liquid flow rate(l/hr)
 12

Data for spherical packing (7 mm dia)

Water Flow Initial Final Volume of base Concentration
Rate(LPH) Volume(ml) Volume(ml) required(ml) of CO2 (M) NTU HTU(m)
30 16.3 19.3 3
0.0019 0.0526 17.1162
50 19.3 24.8 5.5
0.0034 0.1043 8.6325
70 24.8 29.3 4.5
0.0028 0.0833 10.8088

Variation of NTU with liquid flow rate

0.1500
NTU(m)

0.1000

0.0500

0.0000
0 20 40 60 80
Liquid flow rate(l/hr)

Data for spherical packing (4 mm dia)

Water Flow Initial Final Volume of base Concentration
Rate(LPH) Volume(ml) Volume(ml) required(ml) of CO2 (M) NTU HTU(m)
30 29.3 33.5 4.2
0.0026 0.0771 11.6803
50 33.5 39.8 6.3
0.0039 0.1214 7.4151
70 39.8 44.6 4.8
0.0030 0.0895 10.0540

Variation of NTU with liquid flow rate

0.1500
NTU(m)

0.1000

0.0500

0.0000
0 20 40 60 80
Liquid flow rate(l/hr)
 13

Data for plastic pall ring

Water Flow Initial Final Volume of base Concentration
Rate(LPH) Volume(ml) Volume(ml) required(ml) of CO2 (M) NTU HTU(m)
30 1 2.9 1.9
0.0024 0.0688 13.0759
50 3.4 4.2 0.8
0.0010 0.0248 36.3356
70 4.8 5.8 1
0.0013 0.0326 27.5761

Variation of NTU with liquid flow rate

0.0800
0.0600
NTU(m)

0.0400
0.0200
0.0000
0 20 40 60 80
Liquid flow rate(l/hr)
 14

Sample Calculations

Solubility of CO2 in water at 250C (c*) = 0.0329 mol/l

The conc. of CO2 in inlet water flow rate = 0.0002 mol/l

The following chemical reaction is assumed to take place without any side reactions:
CO2 + 2 NaOH Na2CO3 + H2O

VB  N B
Mole/litre of CO2 =  Co
2  sample(ml )
VB = 1.9 ml
NB = 0.05 N
Sample volume = 20 ml
Concentration of CO2 = 0.0022

C
dc
NTU =  c * c
Co
 c * co 
= ln 
 c * c 
 = 0.0631
 15

SAMPLE ERROR ANALYSIS

N1V1  N 2V2
dN1 dW1 dV10
 
N1 W1 V10
dC dN1 dV1 dV2
Thus,   
C N1 V1 V2
Where C is Concentration of CO2
dC  0.0001 10 0.1 1 
 100 =      100 =9.135
C  1 1000 3.2 20 

 C 
NTU  ln   
 C C 
dNTU dC 1
  
NTU 
C C   C 
ln   
 C C 
dNTU 0.004  9.135 1
100 =  =9.7535
NTU  0.0329  0.004  
ln 
0.0329 

 0.0329  0.004 
 16

DESIGN OF A PACKED TOWER WITH MIXED PACKINGS

The above set of experiments gives us an idea of the absorption characteristics of a

packed tower when the tower is filled with one kind of packing only. In the next stage,
we study the effect of packing the tower with different kinds of packing and observing
whether the process of gas absorption follows the same relationship as earlier or whether
it is different. Differences could arise due to change in flow characteristics, etc.
Discounting any such effects, the theory behind such an experiment would follow
analogously.

1
HTU 
k

z C *  C1/
 ln( * )
HTU C  C 2/
C *  C1/
kz  ln( * )
C  C 2/
C*
k1 z1  ln( * )
C  C1
C *  C1
k 2 z 2  ln( * )
C  C2
C *  C n 1
k n z n  ln( * )
C  Cn

So if different packing materials were to be stacked upon each other in the tower, then the
net effect of the entire tower will be described as

C* Co C* C1 C* Cn1

k1z1  k2z2.....  knzn  ln( * )  ln( * )......  ln( * )
C C1 C C2 C Cn

C *  C o C *  C1 C *  C n 1 C *  Co
 ln( * . ....... * )  ln( * )
C  C1 C *  C 2 C  Cn C  Cn
 17

Additionally, we have a constraint on the height of packing:

z1  z2  z3 .....  zn  Z

Summarily,

i 1
zi  Z
n
C *
 Co
i 1
k i z i  ln (
C *
 Cn
)

0  zi  Z

Thus, if we choose zi such that they add up to the height of tower, then the final outlet
concentration can be obtained from the second relation. The values of HTU for each of
the packing were obtained in the first part of the project and with the assumptions that we
have made, their values can be used here too. In effect, packing a tower with different
materials is equivalent to passing it through towers of height zi. In order to verify our
model, we performed an experiment with different packing materials and the results of
that experiment are described in the next section.
 18

Experimental Observations

Gas Rate=2.5m3/hr
Height Z=0.9m
C*=0.0329 M
Individual heights of each packing = 0.225m
Predicted final concentration is given by the relation:

C* Co C* C1 C* Cn1 C *  Co

k1z1  k2z2.....  knzn  ln( * )  ln( * )......  ln( * )  ln( * )
C C1 C C2 C Cn C  Cn

Thus, Cn=0.0021

Actual experimental data:

Water Flow Initial Final Volume of base Concentration of

Rate(LPH) Volume(ml) Volume(ml) required(ml) CO2 (M) NTU HTU(m)
70
16.5 18.6 2.1 0.0026 0.0771 11.6803

The difference between experiment and actual values of outlet concentrations of carbon
dioxide turn out be 12%. This may seem too large an error, but one has to take into
account the fact that an error of 10% is possible due to limit on the accuracy of the
apparatus itself. It is very much possible that with better apparatus, the theoretical and
experimental results would match very well. From the experiment, it can be seen that
packing a tower with various materials is equivalent to, with reasonable accuracy, a group
of tower filled with a single kind of packing material. This finding can be used to design
towers with different kinds of packing materials so as to minimize the total cost of
packing. This is exactly what is done in the section that follows.
 19

DESIGN OF AN OPTIMUM PACKED TOWER

Before we discuss the details of the experiment, it is necessary to understand the

interpretation of optimum for there are several ways in which a packed tower could be
optimized. In our case, we shall propose a strategy that can be used to absorb some
desired amount of gas while minimizing the total cost of the packing used. This is
because different packing materials have different costs and contacting properties and so
we can neither go in for the material which provides the best contacting, since the cost o f
the material may be prohibitive, nor the cheapest, since that may require a very long
tower, but settle for a compromise between the two. The basic theory comes from the
theory behind the design of packed tower using different packing materials. Let Ci denote
the cost per unit height of packing. By unit height we mean unit height of the same tower
that we worked on. This can be found out by filling the tower and measuring the mass of
packing taken and the height of the packing. Using this value of Ci, we will have an
additional equation. So now the problem is described as follows:
1
HTU 
k
n

i 1
zi  Z
n
C *  Co
i 1
k i z i  ln ( *
C  Cn
)

0  zi  Z

The total cost of packing materials, C is given by:

C1 z1  C2 z2  C3 z3 .....  Cn zn  C
 20

We have to find out that combination of heights of packing so that C, the total cost of
packing is minimized. As it can be seen, we have several equations and inequations, all of
which are linear. That is to say that the above set of equations form a linear program and
so we can use tools like Simplex to solve for the optimum cost.

We solved the above linear program using Matlab 7 and found out the optimum tower
heights. Then the tower was setup based on the output of this program and the absorption
experiment was carried out using in order to verify the model put forth by us.
 21

MATLAB CODE FOR FINDING OUT THE OPTIMAL PACKING

Z=0.9; %Total height of tower

cstar=0.0329 %Solubility
cf=0.0024 %Desired final concentration
ntu=log(cstar/(cstar-cf))

%Inverse of htu for a particular experiment

ihturaschig=0.1296
ihtuysphere=0.1875
ihtuwsphere=0.2013
ihtuclock=0.0387

%kg per metre of individual packing

draschig=1.55
dysphere=1.98
dwsphere=2.39
dclock=0.67

%There is no inequations
A=[]
b=[]

%Constraints due to effect of packing and total height of packing

Aeq = [ihturaschig ihtuysphere ihtuwsphere ihtuclock
1 1 1 1]
Beq = [ ntu
Z]

lb=zeros(4,1); %Lower bound on the individual heights of packing

ub=[Z; Z; Z; Z] %Upper bound on the individual heights of packing
 22

%cost per kg of individual packing

for craschig=1:100
for cysphere=1:100
for cwsphere=1:100
for cclock=1:100

%Objective function
f =[craschig*draschig cysphere*dysphere cwsphere*dwsphere cclock*dclock]

%The linear program

[x, fval, exitflag, output, lambda]=linprog(f, A, b, Aeq, beq, lb, ub)

end
end
end
end
 23

Experimental Observations

The final concentration was set to 0.0024 and the program was executed. It turns out that
the cost is minimized when 7mm dia spheres of height 0.76m and plastic pall ring of
height 0.14m.

Gas Rate=2.5m3/hr
Height Z=0.9m
C*=0.0329 M

Water Flow Initial Final Volume of base Concentration

Rate(LPH) Volume(ml) Volume(ml) required(ml) of CO2 (M) NTU HTU(m)
70
37.5 39.6 2.1 0.0026 0.0771 11.6803

The difference between experiment and actual values of outlet concentrations of

carbon dioxide turn out be 12%. This may seem too large an error, but one has to take
into account the fact that an error of 10% is possible due to limit on the accuracy of the
apparatus itself. It is very much possible that with better apparatus, the theoretical and
experimental results would match very well. From the experiment, it can be seen that
packing a tower with various materials is equivalent to, with reasonable accuracy, a group
of tower filled with a single kind of packing material. This finding can be used to design
towers with different kinds of packing materials so as to minimize the total cost of
packing. This is exactly what is done in the section that follows.
 24

Results and Discussions

1. The gas absorption process in a packed tower was studied for various packing
materials at constant gas flow rate but varying liquid flow rates were studied.
2. The NTU vs. liquid flow rate curve goes through a minimum and then rises for all
but one packing for which the trend is the opposite.
3. The tower was filled with packing of different kinds and the process of gas
absorption studied. It turn out that filling a tower with different packing is
equivalent to carrying the gas absorption in different towers but consisting of
single packing only.
4. Based on the results obtained, we proposed a method to fill the tower so as to
minimize the total cost of materials used. This is a simple linear program for
which numerous techniques exist and can readily be solved using tools such as
Matlab.
5. One must remember that these results were observed for carbon dioxide gas,
which is sparingly soluble in water. Had a more soluble gas been taken, then we
may not have obtained results that match with predictions so well.

Suggestions for Improvement

1. Keep all the flow rates constant. Explore how water temperature affects
absorption.
2. Using gases other than carbon dioxide, perhaps even a mixture of gases.
3. The effect of increasing Z on HTU, NTU, and outlet solute concentrations
4. Relationship between the height of the packed column and the rate of absorption
5. The characteristics of flooding point can be studied using this setup.
 25

References

1. Treybal R.E. (1981). Mass Transfer Operations (3rd Edition). McGraw-Hill, New
York.