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Fixed Bed Adsorption Column Process

Fixed bed adsorption column is used to separate gases like CO2 from a gas stream using a packed bed of adsorbent material. The document describes the equipment used, which includes a column, mass flow meters, valves and a control interface. It then lists the experimental steps to measure CO2 adsorption by flowing a mixture of CO2 and helium through the column, monitoring the CO2 concentration and temperature over time. Data is analyzed by comparing the adsorption isotherm to the Langmuir-Freundlich equation and calculating theoretical and experimental values of q (CO2 uptake) at different flow rates and pressures.

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Mayank Vashishtha
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122 views3 pages

Fixed Bed Adsorption Column Process

Fixed bed adsorption column is used to separate gases like CO2 from a gas stream using a packed bed of adsorbent material. The document describes the equipment used, which includes a column, mass flow meters, valves and a control interface. It then lists the experimental steps to measure CO2 adsorption by flowing a mixture of CO2 and helium through the column, monitoring the CO2 concentration and temperature over time. Data is analyzed by comparing the adsorption isotherm to the Langmuir-Freundlich equation and calculating theoretical and experimental values of q (CO2 uptake) at different flow rates and pressures.

Uploaded by

Mayank Vashishtha
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as DOCX, PDF, TXT or read online on Scribd

Fixed bed adsorption column

M7
Introduction
Fixed bed adsorption column is a technique used in the chemical industry and other fields. This
includes a broad array of applications, including air purification, gas dehydration, solvent or
hydrocarbon vapor recovery, as well as water purification. The main principle of the technique is to
use a packed column containing a solid mass separation material to separate gases from a moving
stream. In this fixed bed adsorption unit, a gas mixture containing both CO 2 and helium enters the
bed in plug flow, and only CO2 is absorbed by the adsorbent, separating it from helium. In this
instance, helium is referred to as an inert gas carrier. Granular activated carbon is present in the
packed bed to absorb CO2 from the stream.

Learning Objectives:

 Comprehending the fundamental experimental principles of gas adsorption


 Calculating the adsorption rate and total yield.
 Practicing using an adsorption apparatus.

Equipment Description

Figure 1. Equipment layout (UOP 15)

As shown in Figure 1, the equipment consists of the following components:

1 - Fixed bed adsorption(FBA) column 8 - Hot water circulation system


2 - Mass flow meter F3 5 - Mass flow meters F1,F2 9 - Gas cylinders
3 - On/Off rig Switch 6 - IR sensor 10 - Pump rotary valve ( V3)
4 - Needle valves(V1,V2) 7 - Control interface
Figure 2. Valves layout of the (UOP 15)

Experimental steps for measuring CO2 adsorption


1- Ensure that the gas cylinders are closed and the On/Off switch on the rig is set to the Off
position. Proceed to the computer and launch the adsorption unit software (UOP15 – Fixed
bed adsorption unit)
2- First, direct the helium flow around the column (through the bypass), by directing valves V3
and V4 (inlet and outlet column valves) towards each other (position 3).
3- Adjust the He flow rate by adjusting the V1 valve to a reading of approximately 3 standard
liter per minute (SLPM). Check the value displayed on the F1 icon on the computer's display.
4- Direct the V3 and V4 to the position 2 in which they start flowing inside the column instead
to the bypass as it is mentioned in an earlier step. Then the He stream will flow through the
column.
5- Using the PID controller on the rig, adjust the set point temperature to 40℃ in the PID.
6- Switch on the pump and heater after adjusting the temperature to the desired value.
7- Ensure that the temperature of the column is stabilized around the desired value.
Usually it takes between 15-20 minutes to raise the temperature by 10℃ so you
should allow around 30-35 minutes to reach the 40℃ temperature (if not possible
to reach the temp after this time, work with highest steady state temp).
8- Start logging data with a sample interval of 10 s by pressing the start button on the
computer screen associated with the UOP15 rig.
9- When the temperatures are steady, direct V3 and V4 to position 3 and gradually open the
CO2 cylinder valve and to regulate the CO 2 flow rate, then the stream will pass through the
by-pass again.
10- Adjust the valve V5 until the gauge pressure, P1, is at 0.2 bars.
11- Adjust the flow F2 on the screen using V2 to reach a value of 0.15 SLPM which is 5% of the
He flow rate to start the adsorption process in the column.
12- Adjust V3 and V4 to position 2 as it is shown in Figure 2 and observe the adsorption curve on
the software.
13- Make sure that V3 and V4 are open simultaneously for the accuracy of the results.
14- Using a stopwatch, record the time that the experiment started.
15- Ensure that the flow rates of both gases remains constant and the concentration is the same
all the time (small adjustments could be necessary depending on the flow rate and
temperature)
16- When the temperature in the column is uniform and the feed and exit CO 2 Concentrations
are equal. The adsorption is complete and the bed is completely saturated with CO 2 reaching
equilibrium.
17- Stop the flow of CO2, using V2 so that only helium is flowing.
18- Record the time that you stopped the flow of the CO 2.
19- Once you have stopped the flow of the CO 2, the desorption process starts.
20- Wait until the % infrared (IR) reading reached 0% - this means that there is no more CO 2
present in the column and all the carbon dioxide has been desorbed and the desorption
process is complete
21- Check the T (temperature) profiles using the software.
22- Stop data loading.
23- Stop the flow of He using V1 and also stop the hot water circulation system by turning the
pump off and the heater.
24- Save the date then, repeat the experiments using different gas flow rates including different
CO2 flow rates and helium rates. Start with He at 2 SLPM and 5 SLPM.
25- Make sure that all the changing of the flow rate of He and CO 2, that the CO2 percentage
should not exceed 5% of the He flow rate.
26- Save the data and move to the calculation section below.

Data analysis
We will need to compare the experimental results obtained from the software. With the theoretical
calculated data and discuss the obtained results. The difference between the theoretical data and
the experimental data.

In terms of theory, the adsorption inside the column can be explained by Langmuir-Freundlich’s
equation (1):
1
n
(bp)
q=Q (1)
1
n
1+(bp)
Q, b and n are constants of the Langmuir-Freundlich’s

p - partial pressure

Calculation steps:
1. Obtain the adsorption isotherm curves which come from the desorption breakthrough and
compare to the curve derived from the Langmuir- Freundlich equation (equation 1) qCO 2 = f
(PCO2).
2. Plot the q against the partial pressure of CO 2.
3. Once that the breakthroughs of the temperature profiles and CO 2 concentration are
obtained from the software. Obtain the q (mol/kg) from the breakthrough experimental
4. Compare the obtained q (mol/kg) from the breakthrough experimental and compare it with
the theoretical.
5. Repeat the same calculations for every different flow rate.

Common questions

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The experimental setup involves a fixed bed adsorption column, mass flow meters, IR sensors, and control interfaces. To prepare, helium is initially directed around the column using valves, and its flow rate is set using V1. The system temperature is set to 40℃ and stabilized using PID controllers. CO2 flow is then gradually introduced for adsorption by adjusting valves to allow the gas mixture into the column .

The Langmuir-Freundlich equation is used to model the adsorption equilibrium within a fixed bed adsorption column. This equation helps in understanding the relationship between the adsorption capacity (q) of the adsorbent material and the partial pressure of CO2 (p) in the gas phase. The constants Q, b, and n are specific to the adsorbent material and influence the adsorption behavior, allowing theoretical calculations to be compared with experimental data .

Comparing theoretical and experimental data is crucial to validate the theoretical model, identify discrepancies, and refine adsorption theories for better predictability. In this scenario, the Langmuir-Freundlich equation is applied, providing a theoretical framework to understand adsorption dynamics based on pressure variations and adsorbent capacities. This enables the evaluation of model accuracy against real-world data .

Inconsistent temperature can lead to erratic adsorption behavior, as it affects the kinetic energy of gas molecules and the adsorbent's absorption properties. This can cause an irregular breakthrough curve, deviation from expected theoretical models, and unreliable adsorption capacity data, compromising the experiment's validity and reproducibility .

Accuracy is ensured by monitoring flow meters and adjusting valves V1 and V2 to maintain consistent helium and CO2 flow rates. These adjustments are crucial as fluctuations can affect the adsorption dynamics and lead to inaccurate data regarding the adsorption capacity and breakthrough times. Moreover, CO2 flow should not exceed 5% of the helium rate to ensure the experiment's accuracy and repeatability .

According to the Langmuir-Freundlich model, the adsorption capacity of CO2 on granular activated carbon increases with rising partial pressure of CO2 until saturation is reached. The model posits a nonlinear relationship, accounting for potential heterogeneity at the adsorbent sites as indicated by constants Q, b, and n. This relationship is critical for predicting how changes in pressure affect adsorption efficiency .

Desorption is monitored using an IR sensor, which detects the presence of CO2 in the column. The process is complete when the IR reading returns to 0%, signifying the column is free of CO2. The helium flow helps purge CO2 from the adsorbent, and adjustments to flow rates and temperatures are critical until desorption equilibrium is reached, ensuring complete removal .

Adsorption completion is determined when the exit concentration of CO2 equals the feed concentration, indicating the bed's saturation. After completion, the CO2 flow is stopped, initiating desorption. The process ends when the IR reading reaches 0%, indicating all CO2 has desorbed. The flow of helium is then stopped, and the equipment is turned off for data saving and analysis .

Temperature affects the adsorption rate by influencing the kinetic energy of the gas molecules and the adsorbent surface interaction. Typically, increasing the temperature can cause desorption and reduce adsorption capacity. In the experiment, temperature is controlled using a PID controller, which adjusts the set point temperature to 40℃ and employs a heating system to stabilize it before beginning data logging .

Careful regulation of the CO2 flow rate ensures it remains a small fraction (5%) of the helium flow rate to prevent rapid saturation and breakthrough, which can confound data interpretation. This low percentage allows accurate tracking of adsorption dynamics and ensures helium effectively carries CO2 through the column without overwhelming the adsorbent's capacity .

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