ENGINEERING LABORATORY

Packed Bed Absorber

Grup A1
Adrián Martínez
Emili Brau
13/11/2023
Introduction

Objective

The purposes of this practice include characterizing a packed column, measuring the transfer
unit height and obtaining the overall matter transfer coefficient in relation to the gas phase
under various operating conditions, as well as identifying the operating range of the column.
This objective will be achieved by applying an analytical approach to calculate the inlet and
outlet conditions of the column, as well as evaluating the repeatability and resolution of the
method used.

Theoretical Basis

The absorption of carbon dioxide (CO2) in a column using a solution of sodium hydroxide
(NaOH) and water (H2O) is an essential process in chemical engineering, with a wide range
of applications both in industry and in the environmental field. This separation technique is
used to remove CO2 from gas streams, especially in situations where it is crucial to reduce
greenhouse gas emissions and purify gasses in chemical processes. The efficiency and
optimization of this process is of great relevance, given its key role in climate change mitigation
and its contribution to environmental sustainability.

Column operation

The absorption system consists of a column with specific dimensions, which includes a
packing material inside to ensure continuous contact between the liquid and gas phases.
Normally, a countercurrent flow is used in this process: the liquid enters from the top of the
column and descends due to gravity, while the gas rises from the bottom of the column to the
top due to pressure differences. The choice of a countercurrent flow provides a more uniform
driving force compared to equicurrent flow.

In the context of carbon dioxide (CO2) absorption using a solution of sodium hydroxide
(NaOH) and water, the process is based on the interaction between the CO2 present in the
gas and the hydroxyl ions (OH-) present in the aqueous NaOH solution. The absorption of
CO2 in this solution leads to a series of chemical reactions that result in the formation of
carbonate ions (CO3^2-) in equilibrium with carbon dioxide.

Figure 1: Absorption Column

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The balance of matter is carried out using the molar flow rates with the following equation:

Eq.1

The operating line is calculated using the following equation:

Eq.2

Types of Column Filling::

The use of filler is intended to increase the contact surface between the two phases, which in turn
improves the efficiency of matter transfer. The most common types of fillers are as follows:

- Structured packing: Structured packing is designed to optimize the contact efficiency between the
gas and liquid phases and can have more complex and specific configurations to suit the needs of the
process.

- Packed-type packing: this type of packing consists of a series of solid materials, such as Raschig
rings or pall rings, which are arranged inside the column. These materials significantly increase the
contact surface area and facilitate mass transfer between the phases.

Absorption efficiency

The efficiency of CO2 absorption in a column is influenced by the equilibrium between gaseous
CO2and dissolved species in solution. The concentration of CO 2 in the gas and in the liquid phase is
crucial for the process. The equilibrium is governed by the equilibrium constant of the chemical
reaction and is influenced by factors such as temperature and pressure.

In this practice, it is essential to create an Eckert diagram for the purpose of identifying the optimum
flow rate range to operate near the column flood, which ensures maximum efficiency in the process.
Eckert diagrams use dimensionless variables, Y Eckert and X Eckert, represented on a logarithmic
scale for various head losses. Through this diagram, a line of operation is established that will guide
the operation of the system. The equations used are shown below.

Eq.3 Eq.4

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Characterization of the column

In order to characterize the column, it is necessary to determine three fundamental data,

namely the overall transfer coefficient for the gas phase and the height of the various
transfer units.

Overall transfer coefficient

The gas phase transfer coefficient in an absorption process is a measure of the efficiency
with which a gas dissolves in an absorbing liquid. It works by determining the rate of mass
transfer from gas to liquid, influenced by the concentration difference and the physical
properties of the system. How to determine it can be seen below.

Eq.5

Number of transfer units

The number of transfer units is essential in an absorption process, as it directly affects the
ability to separate components in a gas stream. An adequate number optimizes the efficiency
of the process by ensuring efficient and economical mass transfer, while an insufficient
number can result in incomplete absorption and low yield. On the other hand, too many
transfer units can lead to unnecessary costs. Therefore, determining the optimal number is a
critical aspect of absorption process engineering.

Eq.6

Height of transfer units

The height of the transfer units is critical in an absorption process, as it influences the mass
transfer efficiency and thus the ability to separate components in a gas stream. Inadequate
heights can negatively affect the performance of the process. How to determine this can be
seen below:

Eq.7

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Experimental Part

Equipment and material:

For this experiment, the packed bed absorber equipment was used, containing a packed
absorption column, three big deposits, a pump and a set of pipes and valves. A conductivity
meter was also used. This can be seen below in figure 2.

Figure 2: Packed bed absorber P&ID

- two 250 mL volumetric flasks

- two 250 mL beakers
- one 50 mL beaker
- one 1L beaker
- two 10 mL pipette
- one pipette bulb
- one 50 mL burette
- one 100 mL graduated cylinder
- twenty 10 mL vials

Reagents and indicator:

- Deionized Water, H2O

- Carbon Dioxide, CO2
- Sodium Carbonate, Na2CO3
- Sodium Hydroxide, NaOH
- Methyl orange, C14H14N3NaO3S

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Experimental procedure:

NaOH, Na2CO3 and HCL solution preparation

First the necessary quantities are calculated to obtain a 250 mL NaOH solution 1% w/w. On
the granataria balance, 2,52 g of NaOH are weighed in a 250 mL beaker, dissolved with 200
mL of deionized water, and transferred to a 250 mL volumetric flask where it is made up to the
mark.

The stoichiometric quantity of Na2CO3 is calculated and therefore 3,28 g of Na2CO3 are
weighed in a 250 mL beaker, dissolved with 200 mL of deionized water, and poured and made
up to the mark in a 250 mL volumetric flask.

Finally in order to be able to make sure the prepared solutions have the proper molarity, a 250
mL 0,25 M HCL solution is prepared. This is done by pipetting 62,5 mL of a 1 M HCl solution
and dissolving it with deionized water up to the mark in a 250 mL volumetric flask.

Acid-Base Titration

The concentrations of the NaOH and Na2CO3 solutions prepared will dictate the results from
the experimentation, which is why it is of utmost importance to verify the molarity of the
solutions.

The burette is filled up with 0,25 M HCl solution and both solutions are titrated using 10 mL of
either NaOH or Na2CO3 and methyl orange as the indicator. The HCl solution is poured until
the color changes from orange to red. The titrations are repeated 3 times for each solution in
order to assure the repeatability of the procedure.

Conductivity - Concentration Curve

In the next step, in order to relate the concentration of the mixture to its conductivity, 11 vials
are prepared with different volumes of each component and their conductivity is measured
with the conductometer in μS. In each vial a volume fraction of one of the components is put
from 0 to 1 with a variation of 0,1. It is very important to clean the conductometer electrode
with deionized water between measurements.

Flooding Curve

In order to know the operating conditions for the absorption to take place, the Eckert diagram
with the flooding curves must be found. To do this, 3/4 of the T-103 is filled with deionized
water and all the valves are put in the correct position. The pump P-101 is turned on, different
water flow rates are set with the rotameter ROT-103 and the air flow rate is varied with the
rotameter ROT-102 until flooding occurs at 5 cm in the column. This procedure is repeated for
7 different water flow rates from 50 L/h to 200 L/h.

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 Characterization of the Packed Bed Absorber Column

The next step is to characterize the absorption column. In order to do so the column must work
very close to flooding conditions in order to maximize absorption without flooding.

In order to do so, a 60 L solution of 1% (w/w) NaOH is prepared in the tank T-102 by weighing
1268 g of a 50% (w/w) NaOH solution. This is done by knowing the radius of the tank and then
calculating the necessary height for the volume to equal 60 L and marking the distance with a
marker. Deionized water is poured inside the tank along with the weighed 50% NaOH solution
until it reaches the mark. The solution is homogenized with a big paddle and the conductivity
of the solution is measured to assure it matches that of the analytic method. If it doesn’t, more
water or NaOH solution is added to the tank to match the desired value.

In order to study the column, 3 flooding factors are set (0,7 - 0,8 - 0,9). For each flooding
factor, 3 volumetric flows of liquid are set and for each one of these, 3 different concentrations
of CO2 mixed with air (2 - 3,5 - 5 % v.v).

The column outlet valve is positioned in order to discharge into the T-101 tank, and the pump
P-101 pumps the solution from the T-102 tank. The CO2 outlet resistance is plugged in, turned
on at 10% and the CO2 canister valve is opened. The air inlet is also opened. The flow rate of
NaOH solution, air and CO2 are set. Conductivity measurements are taken of the outlet of the
column and when the value remains constant the CO2 and air flow rates are changed. Each
time the tank where the NaOH solution is being pumped from is emptied, the valves are
changed and after recirculating the liquid into the new tank in order to homogenize the solution,
the new conductivity of the solution is measured. When the conductivity of the solution in the
tank is low enough or when the experimentation is stopped until the next day, the 3 tanks are
emptied and the same NaOH solution is prepared again.

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Results and Discussion

Acid - Base Titration

The first step is to titrate the solutions, knowing that the following reactions occur:

𝑁𝑎𝑂𝐻 + 𝐻𝐶𝑙 = 𝑁𝑎𝐶𝑙 + 𝐻2 𝑂

𝑁𝑎2 𝐶𝑂3 + 2 𝐻𝐶𝑙 = 2 𝑁𝑎𝐶𝑙 + 𝐻2 𝑂 + 𝐶𝑂2

The results obtained for the titration of both NaOH and Na2CO3 are shown below in Table 1.

Table 1: Experimental values obtained for the Acid-Base Titration

NaOH Titration Na2CO3 Titration

V NaOH / mL V HCl / mL V Na2CO3 / mL V HCl / mL

10 10,6 10 10,4
10 10,6 10 10,3
10 10,5 10 10,4

Average / mL 10,6 Average / mL 10,4

It can be observed that the 3 different volumes of HCl used to titrate the solution of both NaOH
and Na2CO3 have basically the same value, indicating the high repeatability of the procedure.
By obtaining the average of the volumes used of HCl, the real concentrations of the two
solutions are found: NaOH 1,06 % (w/w) and Na2CO3 1,37% (w/w).

Conductivity - Concentration Calibration

The second step is to obtain the conductivity - concentration calibration line for a solution of
NaOH and Na2CO3. The obtained values of conductivity are plotted versus the molar fraction
of Na2CO3 in the graph 1 below.

Graph 1: Conductivity calibration

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A second degree polynomial equation is adjusted to the collected data points and the R2 value
obtained is 0,9972 which means that the equation accurately describes the relationship
between both variables. It can be observed that the values of conductivity obtained for NaOH
are higher than the values for Na2CO3. This is due to the OH- ion which allows for a better
conductivity than the bigger CO3-2 ions.

With the obtained equation, we will be able to use the conductivity from the outflow of the
packed bed absorber to find the concentration of each ion after the reaction occurs in the
column.

A second calibration graph is needed for the calculations which relationates the molar fraction
of NaOH with the conductivity. The respective graph is shown below.

Graph 2: Conductivity calibration

Flooding curve

The different volumetric flows of gas obtained for the flooding of the packed bed absorber
column at different volumetric flows of water are shown below in table 2.

Table 2: Volumetric flows of gas for flooding at 5 cm

Volumetric flow water (L/h) Volumetric flow air (Nm3/h)

50 7
70 6,5
100 6
120 5,5
150 5
170 4,7
200 4,3

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 Eckert diagram

With the information obtained from table 2, the X Eckert and Y Eckert variables are calculated
and shown in table 3.

Table 3: Eckert variables for flooding

Gx Gy X Eckert Y Eckert
1,7649 0,2981 0,2058 0,0064
2,4708 0,2768 0,3102 0,0055
3,5297 0,2555 0,4801 0,0047
4,2356 0,2342 0,6285 0,0039
5,2946 0,2129 0,8642 0,0032
6,0005 0,2001 1,0420 0,0029
7,0594 0,1831 1,3399 0,0024

The values of X Eckert and Y Eckert are plotted against each other in graph 2 below in a
logarithmic way. It can be observed that at larger values of X Eckert, the values of Y Eckert
decrease.

Graph 3: Eckert diagram

With the data obtained in table 3, the X Eckert and Y Eckert values for the flooding factors 0,7,
0,8 and 0,9 are calculated and shown below in table 4.

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 Table 4: Eckert variables for flooding factors of 0,7, 0,8 and 0,9

Flooding factor = 0,7 Flooding factor = 0,8 Flooding factor = 0,9

X Eckert Y Eckert X Eckert Y Eckert X Eckert Y Eckert

0,2058 0,0044 0,2058 0,0051 0,2058 0,0057
0,3102 0,0038 0,3102 0,0044 0,3102 0,0049
0,4801 0,0033 0,4801 0,0037 0,4801 0,0042
0,6285 0,0027 0,6285 0,0031 0,6285 0,0035
0,8642 0,0023 0,8642 0,0026 0,8642 0,0029
1,0420 0,0020 1,0420 0,0023 1,0420 0,0026
1,3399 0,0017 1,3399 0,0019 1,3399 0,0022

These values are plotted in an Eckert diagram with the flooding curve below in graph 4.

Graph 4: Eckert diagram with flooding factors

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Balance de materia: composición de CO2 a la salida

The CO2 matter balance is carried out in order to characterize the absorption column by
means of the number of transfer units in the column, the transfer unit height and the overall
transfer coefficient. In order to carry out the balance, the conductivity was measured at the
beginning and at the outlet, and from the correlations of this conductivity and the mole fractions
of NaOH and Na2CO3, the CO2 gas fraction was determined using Equation 2. The balance
was carried out for a flooding factor of 70%, 80% and 90%. The results are shown in the table
below:
Table 5

In all cases the exit vapor mole fraction is lower than the initial one. It is therefore consistent
because the reaction consumes CO2.

Also the higher the CO2 percentage, the lower the fraction of carbon dioxide at the outlet. The
obtained result is also consistent since it contains a higher amount of CO2 which can react
with the soda. Furthermore, it is also observed that as the volumetric flow rate increases, the
carbon dioxide fraction decreases for the same percentage of CO2. This is due to the fact that
there is a higher amount of soda reacting with the carbon dioxide inside the column, and
consequently its concentration decreases.

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Characterization of the column

Number of transfer units

Graph 5: NOG for flood factor of 70%.

Graph 5 shows the relationship between the NOG variable, which represents the number of
transfer units, and the gas flow rate used. This analysis is carried out considering a flooding
factor of 70%.

An upward trend is observed for each CO2 concentration. There is more difference between
160 L/h and 180 L/h, the trend is more marked than between 180 and 200 L/h, where the
difference in the number of transfer units is less significant.

The upward trend is explained by the fact that when working with higher flow rates, the transfer
from the gas phase to the liquid phase is more effective. This is due to the increase in the
transfer surface area, since there is more liquid content in the column path, and also the
reaction time between the components of the phases is increased.

Graph 6: NOG for flood factor of 80%.

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Graph 6, as in the previous case, shows the relationship between the NOG variable, which
represents the number of transfer units, and the gas flow rate used, evaluated in this case at
a flooding factor of 80%.

An upward trend is observed for all CO2 concentrations, being more pronounced between 180
L/h and 200 L/h where the difference in the number of transfer units is more noticeable.

This upward trend is explained by the fact that when working with higher flow rates, the transfer
from the gas to the liquid phase intensifies. This is due to the increase in the transfer surface
area, as there is more liquid content in the column path, and also the reaction time between
the phase components increases.

This trend can be explained as the experimentation conditions are near to the flooding
conditions, resulting in higher adsorption efficiency. Transfer is favored by the higher flow
rates.

Graph 7: NOG for flood factor of 90%.

Graph 7 shows the relationship between the NOG variable with respect to the gas flow rate
used, in this case it is being evaluated under the 90% flooding factor.

The trend is upward for all concentrations and is due to the fact that when working with higher
flow rates the transfer from the gas phase to the liquid phase is higher, the reason is that the
transfer surface increases because there is more liquid content in the path of the column and
also increases the reaction time between the components of the phases.

There is a greater transfer of matter due to the higher flow rates, but this is also due to the fact
that the flooding factor is 90%, therefore, the number of transfer units of this factor is greater
than for 70% and 80%.

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 Transfer unit height

The head of the transfer unit was determined using Equation 7 for each volumetric flow rate
and flood factor. The results obtained are shown below:

Graph 8: HOG for flood factor of 70%.

There is a clear tendency that, as the volumetric flow rate increases, the height of matter
transfer decreases with it. Taking this into account, it can be said that the result obtained is
coherent given that increasing the flow rate implies increasing the contact surface, achieving
a better transfer of matter between both phases.

Graph 9: HOG for flood factor of 80%.

As in the previous case, there is a clear trend that, as the volumetric flow rate increases, the
matter transfer height decreases. This behavior is expected, since increasing the flow rate
implies increasing the contact surface, thus achieving a better separation.

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 Graph 10: HOG for flood factor of 90%.

Again, there is a clear trend that, as the volumetric flow rate increases, the matter transfer
height decreases. The result is correct, since increasing the flow rate implies increasing the
contact surface, thus achieving a better separation. In addition, it is also observed that, when
working with a higher flooding factor, a lower height of the transfer unit is achieved. In this
case for a 180 L/h flow rate, there is an outrageous point that is discarded so the tendency of
the results it’s more correct.

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 Overall transfer coefficient

With Equation 6, using the obtained values of HOG and the molar flow rates of the gas phase
(G), all the values of KOG ·av are calculated for each flow rate of water and air mixture working
at 70% ,80% ,90%. flooding.

Graph 11: KOG for flood factor of 70%.

Graph 11 shows the relationship between the variable KOG ·av, with respect to the gas flow
rate used, in this case it is being evaluated under the flooding factor of 70%.

For the determination of the KOG ·av variable, equation 5 has been used, which can be found
in the theoretical basis section; the variables taken into account are HOG and the different
molar flow rates of the gas phase.

This trend agrees with the theoretical basis that when working at a higher volumetric flow rate,
the transfer of matter is more effective between the liquid and aqueous phases within the
absorption column.

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 Graph 12: KOG for flood factor of 80%.

In graph 12, as in the previous case, the relationship between the KOG ·av variable and the gas
flow rate used is shown, in this case under a flooding factor of 80%. The KOG ·av variable was
determined as in the previous case.

There is a definite trend among the values represented, it is observed that as the volumetric
flow rate increases, the KOG ·av variable also increases (to a small extent).

This tendency agrees with the theoretical basis that when working at a higher volumetric flow
rate the transfer of matter is more effective between liquid and aqueous phase within the
absorption column.

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 Graph 13: KOG for flood factor of 90%.

Graph 13 shows the relationship between the KOG ·av variable with respect to the gas flow rate
used, in this case it is being evaluated under the 90% flooding factor.

The same method has been used to determine the KOG ·av variable as in the two previous
cases.

There is a definite trend among the values represented; it is observed that as the volumetric
flow rate increases, the KOG ·av variable also increases. The fact that these trends are
consistent with respect to the trends described for the rest of the factors makes logical sense
if we consider that we are working closer to the flooding and the efficiency in this case is higher
than the rest of the factors.

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Conclusions

In this practice, the main objectives related to the characterization of an absorption column by
the number of transfer units, height of the transfer unit and the overall transfer coefficient were
achieved.

Preparations of soda and carbonate solutions were made and titrated with hydrochloric acid.
To ensure repeatability and improve accuracy, two titrations of each solution were carried out,
one by each member of the team.

The working margin was determined by measuring different vials with varying concentrations
of soda solution and carbonate, obtaining the corresponding correlations with the conductivity.
The working margin is visualized through the flooding curve, represented in the Eckert diagram
in logarithmic scale. We always operated below this curve, since working in flooding could
lead to erroneous results and inadequate absorption. The flood factors used were 70%, 80%,
and 90%.

Finally, by means of the balance of matter, it has been possible to satisfactorily determine the
composition of carbon dioxide in working conditions of 70% and 90% flooding, obtaining logical
results at working conditions of 70% 80% and 90% flooding, obtaining logical results since the
mole fraction of CO2 output is considerably lower than that of input.
CO2 output mole fraction is considerably lower than the input one.

The determination of NOG has been satisfactory for all flooding conditions, since the increase
of NOG with respect to the increase of the liquid flow is in accordance with the definition of this
parameter.

Similarly, HOG shows a logical behavior in flooding conditions, decreasing its value as the liquid
flow rate increases. Its value decreases as the liquid flow rate in the column increases.

Finally, in the determination of the overall transfer coefficient referred to the gas phase
(KOG·av),the obtained values which adjust perfectly to its definition values that meet its
definition at 90% flooding conditions, increasing its value as the liquid flow rate increases.

On the other hand, for 70% and 80% flooding, no logical pattern is presented on the results
obtained. This is attributed to possible experimental errors that have led to a deviation in the
results.

In conclusion, it is determined that the objectives of the practical have been fulfilled, since all
the relationships, diagrams and all the relationships, diagrams and parameters that were
proposed have been calculated and determined.

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Nomenclature

Nomenclature of the different variables that appear during the practice.

VARIABLE MEANING UNITS

FP Packing factor h-1

G Volumetric outlet flow m3·h-1

G1 Volumetric inlet flow m3·h-1

GX Mass liquid flow kg2·m-4·s-2

GY Mass gas flow kg2·m-4·s-2

g Gravity constant m·s-2

HOG Height of the transfer unit m

hpacking Filling height m

L Volumetric outlet flow m3·h-1

L0 Volumetric inlet flow m3·h-1

NOG Number of transfer units -

ΔP Pressure drop Pa

x Gas molar outlet fraction -

xo Gas molar inlet fraction -

XEckert Eckert x axis -

y Gas molar outlet fraction -

y1 Gas molar inlet fraction -

yN+1 Gas molar inlet fraction -

YEckert Eckert y axis -

ρG Gas density kg·m-3

ρL Liquid density kg·m-3

μG Center fluid viscosity Pa·s

μW Wall fluid viscosity Pa·s

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Annex

Annex 1: P&ID Diagram for the Packed Bed Absorber

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 T-104
ROT-103
C-101

V-103 PI-4

RE-101

V-101 ROT-101 V-114

PI-1

PI-2
V-115

V-113
V-102 ROT-102
V-116

V-108
CO2 PI-3

V-104 V-105 V-106

T-101
AIRE T-102 T-103

V-109

V-110 V-111

V-112

P-101

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