Chemical Engineering Department

Separation Processes B

LABORATORY REPORT #5

Name: Elvin Garashli

Experiment title: Gas Absorption

Date of experiment: 9 April 2021

Date of submission: 25 April 2021

Supervisor: Elsever Mikayilov, Hajar Nabiyeva

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Contents
Synopsis.............................................................................................................. 2
Introduction........................................................................................................ 2
Theory ................................................................................................................ 4
Experimental technique ...................................................................................... 8
Equipment and Apparatus ........................................................................................................................ 8
Procedure.................................................................................................................................................. 0
Safety ........................................................................................................................................................ 1

Results ................................................................................................................ 2
Discussion ......................................................................................................... 10
Conclusion ........................................................................................................ 13
References ...............................................................Error! Bookmark not defined.

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Synopsis
The report below delineates key concepts and experimental details to have a deeper
understanding about the process of absorption and the working principles of absorbers and
desorbers. Absorption is the process of retention of gases inside the liquid by decreasing the
concentration of that gas in gas mixture. The process of absorption was investigated under two
different temperature conditions whose results are comprehensively compared later by means
of the before and after absorption concentrations of CO2, as well as the CO2 loads. Furthermore,
load diagram is plotted with circuit lines, fresh water line of balance, and equilibrium line. Since
water is desorbed in desorption column, the CO2 load of the absorber inlet water line is zero. The
calculated experimental results are 9.44*10^-5 for XA, 0.42 for YE, and 0.29 for YA at the
temperature of 15 °C. For the case when temperature is 30 °C, the values are changed to
1.35*10^-5 for XA, 0.24 for YE, and 0.22 for YA.

The introduction part consists of the overall significance of the absorbers, along with the
essential information about conducted experimentation by delivering fundamental facts, such as
industry application and significance of absorbers and so on. The following section provides
detailed information about process of absorption and working principle of the utilized device as
well as all necessary equations which are sufficient to profoundly grasp the concept and evaluate
the required data. In experimental technique section, equipment and experimental procedure
along with several safety precautions are mentioned. Following this, the results are evaluated
and required parameters are determined. As soon as all unknown variables are derived, the
possible causes of the deviations and remarkable suggestions are provided while discussing the
results. In the end all the work is summarized and concluded by indicating the final derivations.

Introduction
Nowadays, CO2 emissions are rising at an alarming rate which threatens the environment
and future of the world. To tackle the problem, there are many ongoing researches which
promises great results. One of them is the gas absorption via liquid solvent. In almost every
chemical industry, separation of mixture into components is one of the most crucial parts of the
process. The separation can be achieved by several methods, such as distillation, liquid-liquid
extraction (LLE), absorption and so on. All these techniques of separation have specific
parameters which they depend on. The theory behind the separation is mass transfer which is
basically diffusive or convective transition of materials from high to low concentration. For
instance, the theory of distillation is based on difference in volatility of mixed components, that
of liquid-liquid extraction and absorption is based on solubility of solute in solvent liquid.

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However, the difference is that in LLE the carrier and solute is liquid and for absorption both are
in gas phase. There are two types of absorption process, physical and chemical absorption. The
physical absorption is a nonreactive process which is based on intermolecular forces between
solute gas and solvent molecules. This type of absorption depends on the characteristics of solute
and solvent, as well as the temperature and pressure conditions of absorber. Chemical
absorption on the contrary is based on the reaction between the atoms and molecules of gas and
liquid. Chemical absorption depends on mainly reactant concentrations and reaction
stoichiometry. The removal of hydrogen sulfide in biogas streams, where it is converted into solid
sulfur can be taken as a great example. In our experiment physical absorption is achieved by
absorbing CO2 inside the solvent. The career gas in absorption is insoluble, i.e., inert gas which is
used just for carrying the solute. Solute on the other hand should be fully or partially soluble in
solvent liquid. In industry, the absorbers are utilized in many different scenarios, such as
capturing acid gases, fumes which producing by platting tanks, water purification, extraction of
oxygen from boiler fuel waters, odorous emissions in food industry, pulp mills, mines, steel mills,
waste-to-energy plants and so on. It is worthwhile to mention that in real world application of
carbon dioxide capturing with absorption, ethanolamine compounds (especially
monoethanolamine, diethanolamine, and triethanolamine solutions) are utilized mainly which
provides much higher efficiency than simple water. In almost every application the absorber
column is followed by desorber column where the solute dissolved liquid is regenerated by
emitting solute gas from mixture. To have the optimum absorption and desorption ability, the
operating conditions of absorbers should be low temperature high pressure and that of
desorbers should be high temperature and low pressure. In general, the desorbers are operated
under vacuum conditions which is also true for our case. Typically, packings or sieved trays are
utilized inside the absorption and desorption column in order to have higher amount gas capture
in single pass. In our investigation packed columns are utilized both for absorption and
desorption and the flow is in counter current mode where the liquid enters the column from the
top, and vapor from the bottom.

To emphasize the significance of the absorbers and the process of absorption, a small-
scale laboratory experiment was conducted to expand our scope of knowledge with regards to
the process of absorption. During experiment, air is used as carrier gas while CO2 being solute
which is then transferred from air medium to water medium thanks to solubility of carbon dioxide
inside water. The objectives of the experimentation are detecting CO2 concentration before and
after absorption column in circuit mode, determination of the loads in the gas and water flow
and plotting these values into a graph along with equilibrium line and fresh water line of balance.
To achieve a satisfactory resolution and have comparable results, the experiment is conducted
with the help of CE 400 unit. As in all experiments, whenever a measurement is carried out, some
inaccuracies came into the display which is basically inevitable.

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Theory
All systems tend to reach a state where the Gibbs Free Energy is minimum for the system.
This includes absorption process as well where the system tends to reach equilibrium to have
minimum Gibbs Free Energy. Therefore, when two different streams, namely air + CO 2 mixture
stream and water stream comes into contact, redistribution of phases occurs due to
concentration difference of CO2 in each streams and solubility of CO2 in water. The theory behind
solution of CO2 and H2O can be explained by polarity. Despite carbon dioxide is a non-polar
molecule, it has two polar bonds which are in linear configuration and cancel out each other for
the total molecule. Thus, CO2 has a slightly (-) charge for the oxygen and a slightly (+) charge for
the carbon. These polar areas in carbon dioxide attracts the water molecules. Even though the
bond between carbon and oxygen is not as polar as it is between oxygen and hydrogen, it is polar
enough to dissolve CO2 in water. It is also noteworthy to mention that these bonds between
carbon and oxygen are not as strong as the bonds which hold salt or sugar molecules inside the
water, hence, the reverse desorption process can be carried out easily to release the solved CO2.
Desorption is the process where one substance is released from the other, either through or from
surface. Since in absorption equilibrium is reached between discharge streams, when we change
their conditions, the system will try to reach new equilibrium. Therefore, inside desorber the
temperature is high, and the pressure is low to maintain sufficient level of releasing of CO 2 and
regeneration of carrier liquid – water.

To start with the calculations, we need to know the flow rates of each stream. The
equation below shows the conversion of experimental volumetric flowrate of air to the flowrate
in standard conditions:

𝑃𝐸𝑥𝑝 ∗ 𝑇𝑆𝑡.𝐶𝑜𝑛𝑑
𝑉𝑎𝑖𝑟,𝑆𝑡.𝐶𝑜𝑛𝑑. = 𝑉𝑎𝑖𝑟,𝐸𝑥𝑝 ∗ ( ) (1.1)
𝑇𝐸𝑥𝑝 ∗ 𝑝𝑆𝑡.𝐶𝑜𝑛𝑑.
𝑙
𝑉𝑎𝑖𝑟,𝑆𝑡.𝐶𝑜𝑛𝑑. − 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑖𝑛 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑐𝑜𝑛𝑑𝑖𝑡𝑖𝑜𝑛𝑠 (𝑚𝑖𝑛)

𝑇𝑆𝑡.𝐶𝑜𝑛𝑑 − 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 𝑖𝑛 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑐𝑜𝑛𝑑𝑖𝑡𝑖𝑜𝑛𝑠 (𝐾)

𝑝𝑆𝑡.𝐶𝑜𝑛𝑑. − 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝑖𝑛 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑐𝑜𝑛𝑑𝑖𝑡𝑖𝑜𝑛𝑠 (𝑏𝑎𝑟)

𝑙
𝑉𝑎𝑖𝑟,𝐸𝑥𝑝 − 𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 (𝑚𝑖𝑛)

𝑇𝐸𝑥𝑝 − 𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 (𝐾)

𝑝𝐸𝑥𝑝 − 𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 (𝑏𝑎𝑟)

After that, air molar flow rate is found:

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 𝑉𝐴𝑖𝑟,𝑆𝑡.𝐶𝑜𝑛𝑑.
𝑁𝑎𝑖𝑟 = (1.2)
𝑉𝑚
𝑚𝑜𝑙
𝑁𝑎𝑖𝑟 − 𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑎𝑖𝑟 ( 𝑚𝑖𝑛)

𝑙𝑡
𝑉𝑚 − 𝑀𝑜𝑙𝑎𝑟 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 (22.4 )
𝑚𝑜𝑙

To find the molar flowrate of water, we merge the density and molar mass equations into:
𝜌𝑎𝑞
𝑁𝑎𝑞 = 𝑉𝑎𝑞 ∗ (1.3)
𝑀𝑎𝑞

𝑁𝑎𝑞 − 𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟

𝑉𝑎𝑞 − 𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟

𝜌𝑎𝑞 − 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑎𝑡 𝑖𝑛𝑙𝑒𝑡 𝑐𝑜𝑛𝑑𝑖𝑡𝑖𝑜𝑛𝑠

𝑀𝑎𝑞 − 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟

Next step, it is required to find molar flowrates of carbon dioxide in inlet and outlet from
the volume concentration in % values:
𝜑

𝑁̇𝐶𝑂2 = 100 %
𝜑 ∙ 𝑁̇𝑎𝑖𝑟 (1.4)
1−
100 %

As soon as molar flows of the carrier gas, solute and solvent are found, it is possible to
evaluate the loads in each phase using equation below:
𝑁̇𝐶𝑂2
𝑌= (1.5)
𝑁̇𝑎𝑖𝑟

𝑁̇𝐶𝑂2
𝑋 = 𝑁̇ (1.6)
𝑠𝑜𝑙𝑣𝑒𝑛𝑡

The equations above indicate the loads, i.e., molar ratios. With the equations below, it is
easy to convert those values into mole fractions and vice versa:
𝑋 𝑌
𝑥𝑖 = 1+𝑋𝑖 (1.7) 𝑦𝑖 = 1+𝑌𝑖 (1.8)
𝑖 𝑖

𝑥 𝑦
𝑋𝑖 = 1−𝑥𝑖 (1.9) 𝑌𝑖 = 1−𝑦𝑖 (1.10)
𝑖 𝑖

To measure the efficiency of the absorption we can introduce the recovery of CO2 with
the equation below:

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 ∆𝑌
𝛼= (1.11)
𝑌𝑒

𝛼 − 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑦 𝑜𝑓 𝐶𝑂2 𝑖𝑛 𝑙𝑖𝑞𝑢𝑖𝑑 𝑝ℎ𝑎𝑠𝑒

∆𝑌 − 𝑑𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 𝑏𝑒𝑡𝑤𝑒𝑒𝑛 𝑎𝑏𝑎𝑛𝑑𝑜𝑛𝑖𝑛𝑔 𝑎𝑛𝑑 𝑒𝑛𝑡𝑒𝑟𝑖𝑛𝑔 𝑔𝑎𝑠 𝑙𝑜𝑎𝑑𝑠

𝑌𝑒 − 𝑒𝑛𝑡𝑒𝑟𝑖𝑛𝑔 𝑔𝑎𝑠 𝑙𝑜𝑎𝑑

As it was mentioned earlier the phenomenon behind the absorption process is the mass
transfer. In order the transfer of mass to occur, there should be difference in chemical potential
and when this difference becomes zero, the system reaches the equilibrium. Since both carbon
dioxide and water are pure, mixing these will give an ideal solution. For an ideal solution to form,
the intermolecular forces between like and unlike species should be the same. Assumption of
ideal solution allows us to apply Raoult’s law to our system which links the liquid fraction of the
component to its partial pressure in gas phase:

𝑃𝑖 = 𝑥𝑖 𝑃 𝑠𝑎𝑡 (1.12)

𝑃𝑖 − 𝑝𝑎𝑟𝑡𝑖𝑎𝑙 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖

𝑥𝑖 − 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖 𝑖𝑛 𝑙𝑖𝑞𝑢𝑖𝑑 𝑝ℎ𝑎𝑠𝑒

𝑃 𝑠𝑎𝑡 − 𝑠𝑎𝑡𝑢𝑟𝑎𝑡𝑖𝑜𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒

In application, it is required to conduct the absorption in a temperature that is higher than

the critical temperature. It means our solute gas will not be condensed and solved inside liquid
as a gas phase which makes it hard to utilize saturation pressure term. In addition to that, the
amount of carbon dioxide solved in water is not very high, hence, it is more suitable to utilize the
Henry’s law which determines the partial pressure not with saturation pressure, but with Henry’s
constant and works magnificent with the low concentrated dilute solutions:

𝑃𝑖 = 𝑥𝑖 𝐻𝑖 (1.13)

𝐻𝑖 − 𝐻𝑒𝑛𝑟𝑦 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡

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 The Henry constant depends on the nature of solute and solvent and the temperature. In
𝑔𝑎𝑠 𝑚𝑜𝑙
the manual it is given that the Henry constant for CO2 solved in water at 25 °C is 0.034 𝑙𝑡∗𝑎𝑡𝑚 . In
order to find the Henry constant at a temperature different than 25 °C, it is required to utilize the equation
below:
1 1
𝐶∗( − )
𝐻𝑖,𝑐𝑝 = 𝐻𝑖,𝑐𝑝,25 ∗ 𝑒 𝑇 𝑇25 (1.14)

𝐻𝑖,𝑐𝑝 − 𝐻𝑒𝑛𝑟𝑦 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 𝑤𝑖𝑡ℎ 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑎𝑡 𝑎𝑛𝑦 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒

𝐶 − 2400 𝐾 (𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 𝑓𝑜𝑟 𝐶𝑂2 )

𝑇25 − 298 𝐾 (𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒)

To further develop our calculations, it is

required to utilize 𝐻𝑖,𝑝𝑥 instead of 𝐻𝑖,𝑐𝑝 since the
latter one depends on the concentration. Therefore,
equation below is utilized to obtain 𝐻𝑖,𝑝𝑥 value:
𝜌𝑎𝑞
𝐻𝑖,𝑝𝑥 = 𝑀 (1.15)
𝑎𝑞 ∗𝐻𝑖,𝑐𝑝

𝐻𝑖,𝑝𝑥 − 𝐻𝑒𝑛𝑟𝑦 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 𝑤𝑖𝑡ℎ 𝑤𝑎𝑡𝑒𝑟 𝑚𝑖𝑥𝑖𝑛𝑔 𝑟𝑎𝑡𝑖𝑜

Combining Henry’s law with Dalton’s law, we

can get:

𝑦𝑖 ∙ 𝑃 = 𝐻𝑖,𝑝𝑥 ∙ 𝑥𝑖 (1.16)
𝐻𝑖,𝑝𝑥 ∙𝑥𝑖
𝑦𝑖 = (1.17)
𝑃

𝑃 − 𝑡𝑜𝑡𝑎𝑙 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 Figure 1: Composition Diagram

7
 To get the relationship with loads instead of
mole fraction, we can simply merge the equation __
with the __ and get:
𝑝
𝑌𝑖 ∗
𝐻𝑖,𝑝𝑥
𝑋𝑖 = (1.18)
𝑝
1+(1− )𝑌𝑖
𝐻𝑖,𝑝𝑥

𝐻𝑖,𝑝𝑥
∗𝑋𝑖
𝑝
𝑌𝑖 = 𝐻𝑖,𝑝𝑥 (1.19)
1+(1− )∗𝑋𝑖
𝑝

At this point, it is required to construct the

lines of balances for the system. The total mass Figure 2: Load Diagram
balance equation can be written as:

𝐿𝑎 + 𝑉𝑏 = 𝐿𝑏 + 𝑉𝑎 (1.20)

For the specific components, the equation becomes:

𝐿𝑎 ∗ 𝑋𝑎 + 𝑉𝑒 ∗ 𝑌𝑒 = 𝐿𝑒 ∗ 𝑋𝑒 + 𝑉𝑎 ∗ 𝑌𝑎 (1.21)
𝐿 𝑉 𝐿
𝑌𝑒 = 𝑉𝑒 ∗ 𝑋𝑒 + 𝑉𝑎 ∗ 𝑌𝑎 − 𝑉𝑎 ∗ 𝑋𝑎 (1.22)
𝑎 𝑒 𝑒

Since 𝑉𝑎 = 𝑉𝑒 and 𝐿𝑎 = 𝐿𝑒 :
𝐿𝑎 𝐿
𝑌𝑒 = ∗ (𝑋𝑒 − 𝑋𝑎 ) + 𝑌𝑎 → ∆𝑌 = 𝑉 ∗ ∆𝑋 (1.23)
𝑉𝑎

∆𝑌 𝐿
𝑠𝑙𝑜𝑝𝑒 = ∆𝑋 = 𝑉 (1.24)

Experimental technique
Equipment and Apparatus
The whole model of absorption process can be investigated thoroughly using the CE 400
module manufactured by GUNT. This unit helps us to run the experiment and record necessary
data to evaluate and derive key parameters of the process. The unit consists of mainly two

8
columns: absorber and desorber. Absorber is the column where the CO2 is absorbed by water
and the desorber serves as regenerator for the solvent liquid. The unit has pumps and
compressors to maintain the flow of liquids and gases and provide sufficient operating conditions
for the columns. It is worthwhile to mention the water jet pump which creates vacuum for the
desorber. Moreover, CE 400 has three heat exchangers, one for the first heat exchange between
the bottom products of the columns, one heater and one cooler. All setpoints can be adjusted in
the switch cabinet. The flows of all streams are measured via flow meters. The unit also has a
cooling tank whose working principle is based on that of refrigerators, i.e., it has expansion valve,
condenser, compressor, and evaporator. There are two U-tube manometers to measure the
pressure of top and bottom parts of the column.

Figure 3: CE 400 Unit

1 - Absorption column 8 - Pump (cooling)

2 - Switch cabinet 9 - Cooling tank
3 - CO2 flow meter 10 - Pumps (absorption/desorption)
4 - Air flow meter 11 - Refrigeration system
5 - Solvent flow meter 12 - Heat exchanger
6 - Compressor 13 - Heater
7 - Process schematic 14 - U-tube manometer
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15 - Water jet pump (to create vacuum) 16 - Desorption column

The overall flow diagram of the system is shown below. The mixed gas stream enters the
absorber from the bottom part and rises through the column in a counter current way with the
nearly pure water pouring from top. The column is provided with packings to have higher
efficiency of absorption. After giving some of its CO2 load to the liquid stream, the remaining gas
leaves the absorber from the top. On the contrary, the liquid at the bottom of the column is
pumped to the regenerator (desorber) column through recuperator and heater. Inside the
recuperator the temperature of rich CO2 stream increased to the certain value and the design
temperature of desorber is achieved by further heating the stream with a heater. Heated CO 2
loaded stream entered the partially vacuum operating regenerator from the top and is poured
to bottom of the column where the solved CO2 is again released from water thanks to the high
temperature and low pressure and leaves the desorber from the top. The bottom product of the
regenerator, i.e., nearly pure water is then pumped back to the absorber column through the
same recuperator where it gives its energy to cold liquid stream from bottom of absorber and
then further cooled via cooler to meet the demand of our absorber specifications.

1
Figure 4: Diagram of Gas Absorption Process

1 - Residual gas (treated gas) 6 - Desorption column

2 - Absorption column 7 - CO2/air mixture
3 - CO2 gas mixture 8 - Heater
4 - Recuperator 9 - Cooler
5 - Air

Procedure
• Power cable is plugged in
• Water supply is connected to the system
• CO2 gas supply is connected. For the outlet pressure on cylindrical pressure reducer, the setpoint
need to be approximately 0.8 bar
• By using master switch the trainer is turned on
• Ready to use cooler is switched on. It is needed to switch on cooler first to get low temperature
for cooling water to cool down
• Water is added to the system as absorbent medium by closing valve V23 and connecting
freshwater connection to the water supply

0
• P1 and P2 pumps are switched on and the water is poured to the absorption column. By using
valve V12, the flow rate of water is set to approximately 200 l/h
• Fresh water can be topped up if it is necessary
• P2 and P2 pumps are switched back off
• All flexible hoses should be purged to the differential pressure transducer of air bubbles
• P1 and P2 pumps are switched back online
• The level of the liquid should be adjusted to 5-10 cm above the base level in column
• Valve V10 is opened
• The compressor should be switched on and the flow rate of air should be set at round 5 l/min
• K2 regeneration column should be set to the partial vacuum condition. V19 should be closed and
V20 control valve should be opened. The degree of vacuum is set to 0.5 bar relative vacuum. If
the pressure becomes less than the operation pressure It is needed to open valve V21 slightly to
let the stripping air into the regeneration column which increases pressure
• The back pressure for the solenoid control valve V16 should be increased in order to decrease the
noise level. V17 valve should be closed until the cone of spray in desorber is reduced to minimum
to enable the previous step
• Heater should be switched on. The value of the temperature is shown on the temperature
controller in switch cabinet where the setpoints are adjusted using buttons
• At the end, CO2 flow is added to the system by setting CO2 flow rate to 5 l/min by valve V1, which
means with the secondary pressure on the cylinder pressure reducer already set
• Operating point is set up
• Cooling unit is turned on. To have a quicker cooling, the cooler should be turned on 30 mins before
the experiment
• Turn off the heater
• Flow rates are set up. 300 l/h for water, 5 l/min for air, 0.5 bar rel. for desorber, 1.2 l/min for CO2
flow rate
• After completing the experiment CO2 volumetric flow is shut down
• Heater is switched off
• Cooler is switched off
• Simultaneously disconnect the water jet pump and open valve V19 to balance the pressure
• Compressor is switched off
• P1 pump is turned off
• P2 pump is turned off
• If the system will not be used in near future all drain valves should be opened
• Water and carbon dioxide supply lines are disconnected
• Power supply is plugged off

Safety
• The control cabinet should be protected against moisture
• Any work involving opening of control cabinet should be performed by qualified electricians and
main supply should be disconnected

1
 • Risk of suffocation when CO2 is inhaled at higher concentration (more than MWC – Maximum
Workplace Capacity). The experiment should be done in a space as large as possible. Adequate
ventilation and extraction should be ensured to not to exceed MWC
• Since CO2 is heavier than air, oxygen level must be monitored in low-lying spaces and hollows
• Surfaces of compressors and other tubes should not be touched since they become very hot
during operation which impose the threat of burning
• It is suitable to wear hearing protection during experiment since the unit produces noise
• Maximum column pressure of 1 bar may not be exceeded to minimize the risk of destruction of
the column due to high pressure
• It is suitable to fill the cooling circuit with water glycol mixture in a ratio 3:1 to prevent the freezing
of water in case when the circulation pump is turned off and the water temperature is below 4 °C
• The flow at water inlet or outlet of tank W2 / W3 should be checked and if necessary, the pump
should be bled to be ensured that the pump is actually conveying water or not. If there is no water
flow the heat exchanger after the expansion valve may be freezing
• If the unit will not be used for a long period of time, drain the water by drain valves
• Column should not be filled completely with water since there is a risk of overflow and fluid escape

Results
In this part of the report, all required variables are evaluated and comparisons are made
with the help of plotted graphs. Firstly, the given data for 15 °C case is tabulated into below
tables:
Table 1: Experiment 1 Conditions

Volumetric flow
Components T (C) P (bar)
rate (l/min)
Air 5 20.3 1.013
CO2 1.2 20.3 1.013
Water 5 25 1.013

Table 2: Data of First Experiment

Time (min) CO2 S1 CO2 S2 CO2 S3

5 30.2 27.6 23.7
10 30.1 27.5 23.1
15 30 26.4 22.7
20 29.6 27 23.2
25 29.6 25.6 21.9
30 29.4 26.4 22.5
35 28.2 25.8 22
Avg 29.59 26.61 22.73

2
 Volume concentration values are plotted as a function of a time according to Table 2:

CO2 Concentration Profile

35
CO2 Concentration in Vol%
30
25
20
15
10
5
0
5 10 15 20 25 30 35
Time (min)

CO2 S1 CO2 S2 CO2 S3

Graph 1: Experiment 1 CO2 Concentration Profile

In this step it is required to find molar flow rates of streams. Firstly, we convert
experimental air flow rate to air flow rate at standard conditions:
𝑃𝑒𝑥𝑝 ∗ 𝑇𝑠𝑡𝑑 1.013 ∗ 273
𝑉𝑎𝑖𝑟.𝑠𝑡𝑑 = 𝑉𝑎𝑖𝑟.𝑒𝑥𝑝 ∗ =5∗ = 4.65 𝑙/𝑚𝑖𝑛
𝑃𝑠𝑡𝑑∗𝑇𝑒𝑥𝑝 1.013 ∗ 293.3

After evaluating air flow rate at standard conditions, we divide it by molar volume to get
molar flow rate of air:
𝑉𝑎𝑖𝑟.𝑠𝑡𝑑 4.65
𝑁𝑎𝑖𝑟 = = = 0.21𝑚𝑜𝑙/ min
𝑉𝑚 22.4

Since, we evaluated the air flow rate, now it is time to calculate that of water:
𝜌𝑤 999.869
𝑁𝑙𝑖𝑞𝑢𝑖𝑑 = 𝑉𝑤̇ ∗ =5∗ = 277.43𝑙/𝑚𝑖𝑛
𝑀𝑤 18.02

Following this, we determine the flow rate of carbon dioxide at inlet and outlet gas
streams:
29.58
𝑥𝐸 100
𝑁̇𝐶𝑂2,𝑖𝑛𝑙𝑒𝑡 = ∗ 𝑛𝑎𝑖𝑟 = ∗ 0.21 = 0.087𝑚𝑜𝑙𝑒/𝑚𝑖𝑛
1 − 𝑥𝐸 29.58
1 − 100

3
 22.73
𝑥𝐴 100
𝑁̇𝐶𝑂2,𝑜𝑢𝑡𝑙𝑒𝑡 = ∗ 𝑛𝑎𝑖𝑟 = ∗ 0.21 = 0.061𝑚𝑜𝑙𝑒/𝑚𝑖𝑛
1 − 𝑥𝐴 22.73
1 − 100

Since all the flow rates are known, the loads of each stream are figured out:

𝑁̇𝐶𝑂2,𝑖𝑛𝑙𝑒𝑡 0.087
𝑌𝐸 = = 0.24 = = 0.42
𝑛𝑎𝑖𝑟
̇ 0.21

𝑁̇𝐶𝑂2,𝑜𝑢𝑡𝑙𝑒𝑡 0.061
𝑌𝐴 = = = 0.29
𝑛𝑎𝑖𝑟
̇ 0.21

After finding these values, the recovery of CO2 in liquid phase is found as:

∆𝑌 0.42 − 0.29
𝛼= = = 0.30
𝑌𝑒 0.42

Since the incoming water is assumed to be at zero loading of CO2, only XA is found with
the help of ΔY and slope:
𝑌𝐸 − 𝑌𝐴 0.42 − 0.29
𝑋𝐴 = 𝑛 = = 9.43 ∗ 10−5
𝑙𝑖𝑞𝑢𝑖𝑑 277.43
𝑛𝑎𝑖𝑟 0.21

Now it is time to find the equilibrium data with the help of Henry constant:
1 1 1 1 𝑚𝑜𝑙𝑒
𝐶∗( − )
𝐻𝑖.𝑐𝑝 = 𝐻𝑖.𝑐𝑝.𝑇𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑡 ∗ 𝑒 𝑇 𝑇𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑡 = 0.034 ∗ 𝑒 2400∗(288−298) = 0.045
𝑙𝑎𝑡𝑚
𝜌𝑎𝑞 999.5
𝐻𝑖.𝑝𝑥 = = ∗ 1.013 = 1249.43 𝑏𝑎𝑟
𝑀𝑎𝑞 ∗ 𝐻𝑖.𝑐𝑝 18.02 ∗ 0.045

With the help of the above Henry constant and the equation 1.18, we can easily tabulate
the equilibrium data as:
Table 3: Experiment 1 - Equilibrium line data

Equilibrium data
Xi Yi
0.00000 0.00
0.00004 0.05
0.00007 0.10
0.00011 0.15
0.00014 0.20
0.00016 0.25

4
 0.00019 0.30
0.00021 0.35
0.00023 0.40
0.00025 0.45
0.00027 0.50
0.00029 0.55
0.00030 0.60
0.00032 0.65
0.00033 0.70
0.00035 0.75
0.00036 0.80
0.00037 0.85
0.00038 0.90
0.00040 0.95
0.00041 1.00

Table 4: Points of Circuit of Lines of Balance

Since we know the XA, XE, YA, and YE, it is possible to find Points X Y
other 2 points and plot the load diagram. Here Point 1 is (XE, YA) 1 0.00 0.29
and Point 2 is (XA, YE). The other points each lie on 2 different 2 9.44E-05 0.42
location on load diagram with the same gas load – Y values with 3 2.40E-04 0.42
4 1.46E-04 0.29
Point 1 and Point 2. We assume Point 3 to have same Y with P2
1 0.00 0.29
and the X value for point 3 is found from equilibrium line
equation as it touches the equilibrium point. To finalize the cycle, we need to find Point 4 which
has same Y with Point 1 and the X value can be easily from simple geometry:

𝑋4 = 𝑋1 + (𝑋3 − 𝑋2 )

The values are tabulated into Table 4 and plotted into graph as below:

5
 Load Diagram
1.00

0.90

0.80

0.70
Y Gas Loading

0.60

0.50

0.40

0.30

0.20

0.10

0.00
0.00000 0.00005 0.00010 0.00015 0.00020 0.00025 0.00030 0.00035 0.00040 0.00045
X Liquid Loading

Equilibrium Line Circuit Line, 15°C

Graph 2: Experiment 1 - Load Diagram

All the steps are repeated for the case when the absorber temperature is 30 °C and the
results are indicated below:
Table 5: Experiment 2 Conditions

Volumetric
Components T (C) P (bar)
flow rate (l/hr)
Air 5 20.3 1
CO2 1.2 20.3 1
Water 5 25 1

Table 6: Experiment 2 - Data

CO2 CO2
Time (min) CO2 S1
S2 S3
5 29.1 28.4 27.5
10 22.1 21.6 20.9
15 18.4 17.5 16.9
20 14.9 14.4 13.9
25 12.5 12.1 11.8
Avg 19.4 18.8 18.2

6
 CO2 Concentration Profile
35
CO2 Concentration in Vol%

30

25

20

15

10

0
5 10 15 20 25
Time (min)

CO2 S1 CO2 S2 CO2 S3

Graph 3: Experiment 2 - CO2 Concentration Profile

Table 7: Experiment 2 - Equilibrium Data

Equilibrium data
Xi Yi
0.00000 0.00
0.00003 0.05
0.00005 0.10
0.00007 0.15
0.00009 0.20
0.00011 0.25
0.00012 0.30
0.00014 0.35
0.00015 0.40
0.00017 0.45
0.00018 0.50
0.00019 0.55
0.00020 0.60
0.00021 0.65
0.00022 0.70
0.00023 0.75
0.00024 0.80

7
 0.00024 0.85
0.00025 0.90
0.00026 0.95
0.00027 1.00

Load Diagram
1.00
0.90
0.80
0.70
Y Gas Loading

0.60
0.50
0.40
0.30
0.20
0.10
0.00
0.00000 0.00005 0.00010 0.00015 0.00020 0.00025 0.00030
X Liquid Loading

Equilibrium Line Circuit Line, 30 °C

Graph 4: Experiment 2 - Load Diagram

After that, volumetric flow rate of CO2 and water are altered separately, and the model is
simulated again to obtain the required parameters. All the equations above are repeated and
final values are tabulated into the table below:
Table 8: Calculation Summary of 4 Experiments

Exp No 1 2 3 4
Mode Circuit Circuit Circuit Circuit
Changed Parameter - V CO2 V aq T absorber
T absorber (°C) 15 15 15 30
V CO2 (l/min) 1.2 0.4 1.2 1.2
V air (l/min) 5 5 5 5
V aq (l/min) 5 5 3.3333333 5
Φ E (vol%) 29.6 15.5 29.4 19.4
Φ A (vol%) 22.7 10.8 21.8 18.2
YE 0.42 0.183432 0.4164306 0.2406948
YA 0.293 0.1210762 0.2787724 0.2224939

8
 Recovery 0.2999454 0.3399392 0.330567 0.0756182
XA 9.521E-05 4.67E-05 0.0001546 1.346E-05
XE 0 0 0 0
Slope 1335.32 1335.32 890.21 1352.68

Following this, with the help of liquid and gas loads in table above, four points for each
alteration on load diagram is evaluated and tabulated:
Table 9: Load values of 4 Experiments

Exp No: Experiment 1 Experiment 2 Experiment 3 Experiment 4

Points X Y X Y X Y X Y
1 0.00 0.29 0.00 0.12 0.00 0.28 0.00 0.22
2 9.44E-05 0.42 4.67E-05 0.18 0.000155 0.42 1.35E-05 0.24
3 0.00024 0.42 0.000126 0.18 0.000238 0.42 0.000103 0.24
4 0.000146 0.29 7.9E-05 0.12 8.38E-05 0.28 8.97E-05 0.22
1 0.00 0.29 0.00 0.12 0.00 0.28 0.00 0.22

Using these data, the Circuit mode Load Diagram is plotted with the balance areas of all
four cases:

Load Diagram
1.00
0.90
0.80
0.70
Y Gas Loading

0.60
0.50
0.40
0.30
0.20
0.10
0.00
0.00000 0.00005 0.00010 0.00015 0.00020 0.00025 0.00030 0.00035 0.00040 0.00045
X Liquid Loading
Equilibrium Line at 15 °C
Equilibrium Line at 30 °C
15 °C, CO2: 1.2 l/min, Air: 5 l/min, Water: 5 l/min
15 °C, CO2: 0.4 l/min, Air: 5 l/min, Water: 5 l/min
15 °C, CO2: 1.2 l/min, Air: 5 l/min, Water: 3.33 l/min
30 °C, CO2: 1.2 l/min, Air: 5 l/min, Water: 5 l/min

Graph 5: Circuits lines of Balance of 4 Experiments

9
 In the end the fresh water mode line of balance is found at 15 °C with YA0 value of 0.135
and plotted as below:

Load Diagram
1.00
0.90
0.80
0.70
Y Gas Loading

0.60
0.50
0.40
0.30
0.20
0.10
0.00
0.00000 0.00005 0.00010 0.00015 0.00020 0.00025 0.00030 0.00035 0.00040 0.00045
X Liquid Loading

Equilibrium Line at 15 °C Fresh Water Line of Balance

Circuit Line of Balance at 15°C

Graph 6: Fresh Water Mode

Discussion
To start with, we can review the significance of absorption and the experiment. The
absorption is one of the most important processes in industry. To enhance our knowledge about
the process a lab experiment was carried out with the aims of deeply analyzing the process of
absorption, finding the loads in different streams and conditions and plot their area of balance,
measure the influence of different parameter to the process, and finding the fresh water line of
balance. The CE 400 unit was utilized during the procedure. The overall process is briefly the
mixing and separation of CO2 with air. Initially, we mix the air and CO2. Then the mixture and
water are supplied to the absorber which works at relatively high pressure and low temperature
from top and bottom, respectively. Inside the absorber, the liquid and gas flow in a counter
current way and some amount of the CO2 is transferred to the liquid water and the rest leaves
the column from the top. The liquid mixture is then pumped to desorber through recuperator

10
and heater. Inside the desorber water is separated from CO2 thanks to high temperature and low
pressure – partial vacuum which is created by jet pump.

When we analyze graph 1, we can see that the CO2 concentration is lower for column s3
sensor which is located at the top of the column which is basically the exit for the gas stream. As
gas mixture enters the column from bottom, the concentration of CO 2 decreases gradually
towards top which is also shown from the same graph. The s2 point is located in the middle and
the s1 is the bottom sensor which stands for the highest CO2 concentration.

The equilibrium data is simple mole ratios where the liquid and vapor phases are in
equilibrium. In equilibrium means there is no net mass transfer between the phases. Thus, being
close to the equilibrium line is considered as inefficiency. Xe values for the one circuit is
considered as 0 since at the beginning the water is not loaded with the solute. However, if we
reuse the water that comes from the desorber many times it will loaded with little amount of
CO2 which decreases the efficiency. Graph 2 shoes the circuit area of balance for the 15 °C case.

Graph 3 shows the CO2 profile with time for the experiment carried out at 30 °C absorber
temperature. Here we can observe the dramatic drop of CO2 concentration which is not desired
because one of our aim is to compare different changes of parameters in one graph. However,
here also we can see that the bottom sensor measures the highest and the top sensor measures
the lowest concentration of CO2 which satisfies the theory.

Graph 4 illustrates the equilibrium data and the area of circuit at 30 °C absorber
temperature. Here it is possible to observe lower X and Y load values from the first case which
will be discussed soon.

Table 8 contains data which is used to measure the influence of different parameter
alterations. From this data Table 9 is tabulated which is simply coordinates of the circuit area
parallelograms. Graph 5 is plotted according to these coordinates. When we compare the
equilibrium lines in both graphs, we can see that the line for 30 °C is much steeper than that for
15 °C. This completely underlines the theory, because as we mentioned earlier we need low
temperature for the better absorption. There are few reasons for that. First of all, in low
temperature the energy of gases becomes lower and it is easier to entrain the gas molecules
11
inside the liquid. However, it becomes harder as the gas molecules gains the energy – increases
its temperature. It can also be interpreted in a way that the steep equilibrium line gives less space
on the graph for operating line to lie. And as we mentioned, we need to be less close to the
equilibrium line. Therefore, 15 °C case is much more preferable for the absorption process. When
we analyze the orange and grey graphs, we observe low delta X and delta Y values. Keeping the
same flowrates of air, water and the solute should give us relatively close CO2 concentrations at
the beginning, however in our data it is not the case. This can be due to many reasons, such as
human errors, machine errors, maintenance requirements, and so on. To make a fair comparison
we introduce the alpha which is the recovery of co2 in liquid phase. When we compare the alpha
values for these 2 cases, we can observe dramatic drops which means the 15 C case is much more
efficient. When we compare all 4 points’ alpha values, we can see that for the case 2 and 3 when
the CO2 and water flowrates decreased respectively, the recovery value is increased. This doesn’t
satisfy our theory since higher CO2 concentration should provide better absorption efficiency
and the lower amount of water flow means the amount that water can carry should decrease
correspondingly. When we look these cases on the graph, we can see that lower flowrate of CO2
lies in the region where X and Y values are very low which corresponds to our theory. The blue
circuit here is almost the same as the orange one but it has much less steep slope in comparison.
This is because the slope is defined as L/G and decreasing L – liquid flowrate will substantially
decrease the performance. Having less steep operating line also result in fast degradation of
carrier liquid, i.e., the water. As it can be seen from the graph, the less steep operating line gives
less area which lowers the “lifespan” of the water. Overall, it would be much more efficient to
utilize other absorber liquids, such as ehtanolamines and so on. From all these points we can
select the first point – the base case at 15 C as the most efficient operating condition among
others.

Graph 6 indicates the case when the water is not recycled from the desorber, but instead
new fresh water is used again and again. Here the YA0 value was provided beforehand.
Therefore, the position of the line is fixed. However, we can observe that there is no circuit here
which is completely right because if there is no cycle, there shouldn’t be any circuits as well.

12
Conclusion
Absorption is a vital process in industry with its numerous applications, which makes it
important for a process engineer to have a deep grasp of notion. To expand our scope of
knowledge about condensation process and the mechanism in condensers, a small-scale
laboratory experiment was conducted. The main objective of the experiment was investigating
the before and after concentrations of solute gas in gas mixture, determination of loads in
different conditions and plotting circuit loads in load diagram together with fresh water line of
balance, as well as comparing the effect of adjustment of different parameters. During
experimentation process CE 400 Gas Absorption unit by GUNT was utilized to provide all required
devices and fluids. The unit has a column which equipped with absorption and desorption
columns, heat exchanger which exchanges heat between outlet flows of absorber and desorber,
heater, cooler, and pumps (including water jet pump). The water jet pump is utilized to create
vacuum conditions inside the desorber column. The unit also has multiple sensors, valves, and
adjusters to create optimal conditions for the absorption process.

The calculated experimental results are 9.44*10^-5 for XA, 0.42 for YE, and 0.29 for YA at
the temperature of 15 °C. For the case when temperature is 30 °C, the values are changed to
1.35*10^-5 for XA, 0.24 for YE, and 0.22 for YA. Overall, dependency of absorption capacity, i.e.,
difference between entering and abandoning stream loads from different parameters was
investigated thoroughly. The required parameters for the CO2 loads were obtained and the
results satisfy the theory mentioned before.

References
1. McGraw-Hill. ((1984).). Perry's Chemical engineers' handbook. . New York .

2. CE 400 Laboratory Guidelines by G.U.N.T.

3. J H Harker, J R Backhurst, J.F. Richardson, “Chemical Engineering, Volume 2”, Elsevier, 2013,
pages 656-666
4. [2] J. D. Seader, Ernest J. Henley, D. Keith Roper, “Separation Process Principles Chemical and
Biochemical Operations”, 3rd edition, John Wiley & Sons 2011, pages 206-217
5. Products. (n.d.) Retrieved April 24, 2021, from https://www.gunt.de/en/products/process-
engineering/thermal-process-engineering/absorption-and-adsorption/gas-
absorption/083.40000/ce400/glct-1:pa-148:ca-241:pr-45

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