Chapter 2

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There are four basic regeneration methods in common use for

the cyclic batch adsorption system using fixed beds such as


Temperature-swing adsorption (TSA),
Pressure-swing adsorption (PSA),
Inert-purge gas stripping cycle and
Displacement-purge cycle.

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In general, these four basic methods operate with two or sometimes
three fixed beds in parallel, one in adsorption cycle and the other
two in a desorbing cycle to provide continuity of flow.

 After a bed has completed the adsorption cycle, the flow is switched
to second newly regenerated bed for adsorption.
 These methods differ from each other mainly in the means used to
regenerate the adsorbent after the adsorption cycle

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Fixed Bed Adsorption process (Percolation)
The cyclic-batch operating mode using fixed
bed, as shown below, is widely used with
both gas and liquid feeds.

Adsorption only occurs in a particular region of


the bed, known as the mass transfer
zone (MTZ), which moves through the bed.
Applications of fixed bed adsorption, also called
percolation, include the removal of dissolved
organic compounds from water.

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The main advantages of fixed bed system are the
simplicity of equipment needed and
They are relatively inexpensive to fabricate.

Disadvantages of fixed bed system :


As fluid is passed through the fixed bed of solid adsorbents, the
transfer of molecules from the feed fluid to the solid initially
occurs at the bed entrance.

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The MTZ then progressively move through the bed once the adsorbent in a
region becomes saturated with the adsorbate molecules. Thus at any instant in
time, the adsorbent particles upstream or downstream of the MTZ do not
participate in the mass transfer processes.

Upstream of MTZ, the adsorbent is already saturated and in equilibrium with


the feed, and unable to adsorb further solutes.
Downstream of MTZ, the absorbent is not yet in contact with any solutes.
Thus, despite having the capability to adsorb, will be unable to do so.
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Practical methods of desorption and regeneration include one, or
more usually a combination, of the following:
⸎Increase in temperature
⸎Reduction in partial pressure
⸎Reduction in concentration
⸎Purging with an inert fluid
⸎Displacement with a more strongly adsorbing species

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Regeneration of Adsorbent Beds

When one adsorbent bed reaches capacity,


it is taken offline and the process stream is
routed through a second adsorbent bed.
Meanwhile, the saturated bed is taken out
of service and regenerated.

While one bed is in service, the saturated bed is


regenerated to remove adsorbed contaminants.
Each bed has a fixed adsorption capacity, and
once that capacity is reached, the adsorbed
contaminants must be removed. The saturated
bed is then taken out of service and regenerated.
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Regeneration of Adsorbent Beds

The “core” cycle consists of four steps:


pressurization, adsorption, countercurrent
blowdown, and countercurrent purge. In
step 1, feed flows into bed 1, and raises
its pressure, while the fully loaded
second bed is connected to the extract
product

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Regeneration of Adsorbent Beds

Once the desired pressure has been


reached, the system enters step 2, where
the more strongly adsorbed component is
retained in bed 2 and the gas outlet
stream is enriched in the less strongly
adsorbed component.

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Regeneration of Adsorbent Beds

A portion of the raffinate product is


diverted to the second bed, to help fully
regenerate it. Once the first bed has been
loaded, and the second bed regenerated,
a pressure equalization step may take
place. This allows for energy saving by
reducing the quantity of gas that needs to
be compressed.
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The regeneration sequence consists of the following five steps:
Recover the process fluid.
Heat and purge the bed with a regeneration fluid to shift the
equilibrium and remove the contaminants.
Hold at the elevated temperature to ensure the bed is hot and
contaminants are swept from the bed.
Cool the bed to the process temperature with a contaminant-free
stream.
Return the bed to standby service.

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Pressure Swing Adsorption (PSA)
For PSA cyclic batch adsorption the bed is desorbed by reducing
pressure at essentially constant temperature and purging the
adsorbate.
This process for gases uses very short cycle time for regeneration
compared to that for the temperature-swing cycle. However, the
major limitation is that PSA cycles are restricted to components
that are not too strongly adsorbed.

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Pressure Swing Adsorption (PSA)
Regeneration in a PSA process is achieved by reducing the partial
pressure of the adsorbate. There are 2 ways in which this can be achieved:
 A reduction in the system total pressure, and
 Introduction of an inert gas while maintaining the total system
pressure. In the majority of pressure swing separations a combination of
the 2 methods is employed.

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REGENERATION METHOD
Pressure swing adsorption (PSA)

Adsorption occurs at elevated pressure whereas desorption


(regeneration of adsorbent) occurs at near-ambient pressure
Used for bulk separation
The bed can rapidly pressurized & depressurized (sec to min)

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• In a PSA process, compressors are incorporated into the system for
pressurization and depressurization of the adsorbent, thus consuming
electricity.

• Additionally, these processes are slow due to large mass transfer resistances
in large adsorbent particles and sluggish diffusion through porous gaps.

• Nevertheless, PSA processes are preferred due to their ease of operation.

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• If adsorption takes place at near-ambient pressure and desorption
under vacuum, the cycle is referred to as vacuum-swing-adsorption.
PSA and VSA are widely used for the bulk separation of air

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By swinging the pressure from high to low, it is possible to adsorb
large quantities of moisture at the higher pressure, and then release that
moisture at the low pressure. This technique is called pressure swing
adsorption.

• By alternating between two adsorbent filled vessels, one vessel being on


line and removing moisture at high pressure, and the other off line releasing
the trapped moisture at low pressure, it is possible to thoroughly dry a gas.

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Pressure swing adsorption processes rely on the fact that under high
pressure, gases tend to be attracted to solid surfaces, or "adsorbed".

The higher the pressure, the more gas is adsorbed; when the
pressure is reduced, the gas is released, or desorbed.

PSA processes can be used to separate gases in a mixture because


different gases tend to be attracted to different solid surfaces more or
less strongly.

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If a gas mixture such as air, is passed under pressure through a vessel
containing an adsorbent bed of zeolite that attracts nitrogen, ozone, carbon
dioxide more strongly than it does oxygen, part or all of these other gases
will stay in the bed, and the gas coming out of the vessel will be enriched
in oxygen.

When the bed reaches the end of its capacity to adsorb nitrogen, it can be
regenerated by reducing the pressure, thereby releasing the adsorbed
nitrogen. It is then ready for another cycle of producing oxygen-enriched
air.
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Production of oxygen using PSA

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• APPLICATIONS
 To supply medical oxygen, or as a substitute for bulk cryogenic or compressed-
cylinder storage, which is the primary oxygen source for any hospital,

 Primary applications of PSA is in the removal of carbon dioxide (CO2) as the final
step in the large-scale commercial synthesis of hydrogen (H2) for use in oil
refineries and in the production of ammonia (NH3).

 Refineries often use PSA technology in the removal of hydrogen sulfide (H2S)
from hydrogen feed and recycle streams of hydro treating and hydrocracking
units.

The separation of CO2 from biogas to increase the methane (CH4) ratio. Through
PSA the biogas can be upgraded to a quality similar to natural gas.

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To column 2 Purge with H2

1 1 2 2

Inlet flue gas Inlet flue gas CO2 separation


Step1: pressurization CO2 separation Step4:Desorption
Step2: Adsorption
Step3: Depressurization

Figure Operational steps of pressure Swing adsorption system.

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PSA Process Design

Following parameters should be determined in designing a PSA


process:
• Type of adsorbent(s)
• Temperature & pressures
• Number & size of vessels
• Number and type of steps
• Cycle and steps times

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 Generally the most important industrial applications

of PSA processes will be used to address its


technological evolution:
Air separation and
Hydrogen purification

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Fundamentals of Pressure Swing Adsorption

The essential feature of the PSA is that when the adsorbent is


saturated, using a sequential valve arrangement, the feed is
stopped and simultaneously the total pressure of the column is
reduced.

The reduction in pressure results in a partial desorption of all the

species loaded in the column, “regenerating” the adsorbent.

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 In this cycle, in the feed step, air is fed to
the first column (C1) at a pressure higher than
atmospheric.
 The adsorbent initially used (zeolite 5A) is selective to
nitrogen, making the exiting stream (after valve V7)
richer in oxygen.

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When the adsorbent packed in C1 is saturated and
cannot adsorb more nitrogen, the feed is directed to
the second column (C2).
In order to release part of the nitrogen adsorbed in C1,
the flow direction is reversed and the total pressure of
the column is reduced by venting to atmosphere
(opening valve V3).

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 The purge consists of recycled part of the enriched
air from the other column which is flowing by the
pressure differential between the two columns.
 After the adsorbent is ready to load more nitrogen,
the overall pressure of the system should be
restored.

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 That is done in the pressurization step using the feed
stream.
 After all these steps were finished, a complete cycle
was completed. It is important to notice that although
the column operation is discontinuous, the feed stream
is being employed so the process can be viewed as
continuous.
 However, the exit is discontinuous and a tank is
required to be coupled for a continuous discharge.
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Section B Start here

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Adsorption system, the light naphtha from the feeding bottle flowed into an electric
heater pumped by a metering pump, and thereafter passed through a regular valve
(V-1) and a check valve (V-2) into the adsorption bed. Subsequently, the purified
light naphtha flowed through the regular valve (V-3) into the downstream.

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Desorption. In the desorption system, steam was applied as a regenerant to desorb MDEA
from 13X. As shown in Fig., steam at a rated temperature of 443 K passed through a
regular valve (V-4), and then flowed from the top to the bottom of the adsorption bed.
Steam-carried MDEA entered the water cooler and was cooled to approximately 303 K
before it was discharged through a regular valve (V-5) into the environment.
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Look the videos of PSA

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Effects of pressure Further ↑ p form Further ↑ p
As p↑ a multilayer cause complete
adsorption↑, coverage P2>P1 coverage P3>P2
Free sites start form a monolayer
to adsorb gas P1>Po
mols @ low
Po

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Temperature Swing Adsorption (TSA)
 Regeneration of adsorbent in a TSA process is achieved by an increase in
temperature.
 It is an attractive technology for CO2 removal from gas streams. CO2
capture by a TSA process in which the recovered CO2 product is heated
and used as regeneration purge gas.

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Thermal (Temperature) Swing Adsorption (TSA)
⸎ The adsorbent regenerated by desorption at a temperature >used adsorption
⸎ Bed temperature is increased by:
 Indirect heat transfer from jackets surrounding the beds or coils located in
the beds
 Heat transfer from an inert, nonadsorbing, hot purge gas, such as steam
⸎ Because heating and cooling of the bed requires hours due to the low bed
thermal conductivity, a typical cycle time for TSA is long, usually hours to
days
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q Isothermal @ T ads
q*ads

T swing

Isothermal @ Tdes>Tads
q*des

P des P ads P

Fig schematic isotherms in a PSA operation for an adsorption process.


(the effect of partial pressure on equilibrium loading)
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Inert-purge-swing regeneration

Desorption is at the same temperature and pressure as the adsorption step

The gas used for purging is nonadsorbing (inert) or only weakly adsorbing

Used only when the solute is weakly adsorbed, easily desorbed, and of little or no value

The purge gas must be inexpensive so that it does not have to be purified before recycle

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Purging with an innert gas

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Purging with inert gas
Introduction of an inert (non-combustible) purge gas into a closed vessel to
prevent the formation of an ignitable atmosphere
That is reducing the existing gas content with in a vessel to a level below which
combustion cannot be supported if air is subsequently introduced
It is the act of removing the contents of a pipe and replacing it with another gas
or liquid.
It removes contaminants from the piping and vessels, which reduces chances of
corrosion.
It also helps to prevent unwanted reactions from taking place
Prevent an unstable and potentially ignitable atmosphere.

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Temperature Swing Adsorption (TSA)

TSA applications make use of the fact that the sieve will adsorb a greater
amount of contaminants when the sieve bed temperature is lower.
Thus, a gas or liquid stream is fed to the sieve bed at a low temperature
for a period of time to adsorb a contaminant onto the sieve and remove it
from the stream.
The sieve bed is then heated, typically by feeding a hot, clean stream (a
gas that isn’t contaminated) to regenerate the sieve for reuse. Next, the
bed is cooled down so the adsorption process can start all over again.

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Temperature Swing Adsorption (TSA)
 TSA applications allow for the greatest use of the sieve capacity because
the high temperature regeneration is the most effective at removing
adsorbed contaminants.
 These applications are also best for removing contaminants from the
product stream, making TSA with molecular sieves uniquely qualified for
the removal of contaminants in certain applications.
 In most cases TSA is required for the removal of the contaminants CO2
and H2O. TSA is found in cryogenic oxygen plants and natural gas
dehydration units.
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Thermal regeneration
Regeneration is carried out by blowing steam through the
bed so that the bed warms up and the VOC desorbs. This
happens at temperatures between 80 and 200 °C.
Thermal regeneration is most suitable for volatile VOC.

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What is thermal regeneration?

• Regeneration, often referred to as reactivation, is a method of thermally

processing the activated carbon to destroy the adsorbed components contained

on its surface. In regeneration, the adsorbed components are almost completely

removed, yielding a regenerated carbon that can again function as an adsorbent.

• TSA processes have not been commonly used for industrial gas separation due

to the difficulty in heating the low thermal conductivity adsorbent material to

desorb impurities and regenerate the adsorbent.


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Section A start here

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REGENERATION METHOD

THERMAL SWING ADSORPTION (TSA)

Adsorbent is regenerated by desorption at T higher than that used during the


adsorption step

T is increased commonly by heat transfer from inert, purge gas: i.e. steam

The bed is then cooled before the adsorption step is resumed

Disadv: heating & cooling takes time: hours to days

Only PRACTICAL for purification involving small rates of adsorption

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There are advantages to PSA over TSA.
 Keeping the sieve from overheating, which can cause certain
components of the feed stream to break down into other
compounds. That would cause part of the feed to be lost when it is
converted to those other compounds.
 Those broken-down components can stick to the sieve and reduce
its effectiveness in each cycle. PSA regeneration avoids that
problem.

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How does vacuum swing adsorption work?
 They use the process of air separation by adsorption. This works through the
use of specific zeolite adsorbents for the selective adsorption of nitrogen over
oxygen and argon.

 VSA segregates certain gases from a gaseous mixture at near ambient pressure; the
process then swings to a vacuum to regenerate the adsorbent material.
 VSA differs from other PSA techniques because it operates at near-ambient temperatures
and pressures.

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• Vacuum pressure swing adsorption oxygen generation plant (VPSA oxygen plant)
is used to adsorb:

Nitrogen, in the air selectively using special VPSA molecular


Carbon dioxide, sieve, after which oxygen is enriched and released.
Moisture and The molecular sieve is desorbed under a vacuum
Other impurities condition when it's saturated, thus generating
enriched oxygen in cycles.

The gases which are released at the desorption must be treated further.
In the case of steam or vacuum regeneration the solvent can be
recovered easily using a condenser from the desorption gasses.

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1.Adsorption

• After removing the mechanical impurities through the filter, the air enters
the adsorber through the Roots blower. The adsorbent bed selectively
adsorbs N2, H2O, CO2 and hydrocarbons from the pressurized air when it
goes through the adsorbent while O2 is enriched and discharged out of the
adsorber through its outlet.

• Part of the oxygen produced by this step is sent to the buffer tank, and the
other part is reserved for the next step to purge and repressurize the low-
pressure adsorption tower.
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2. Depressurization

• After adsorption at a high pressure, the pressure falls to a lower level and a proportion of
the adsorbed components will be desorbed. Along the outlet of the adsorber A, the
enriched oxygen is fed into adsorber B which is in the repressurization step to boost its
pressure

3.Vacuum Desorption

• In order to desorb the impurities as much as possible, the adsorber needs to be evacuated
and depressurized, that is, a vacuum pump is applied to further evacuate the adsorption
vessel to lower the partial pressure of the impurities for them to be desorbed, and then
discharged out of the vessel through the pump to realize the adsorbent regeneration
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4.Purging

For more thorough desorption of impurities in the adsorption vessel, at


the end of the vacuum desorption step, a small amount of product oxygen
is introduced from another high-pressure adsorber to purge the adsorbent.

At this time, the partial pressure of oxygen rises while impurities’ is
further reduced, resulting in more complete regeneration of the adsorbent
however, which is more conducive to the next cycle of adsorption.

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5.Repressurization

Once the adsorbent is regenerated, the pressure in the vessel is


relatively low. To quickly recover to the adsorption pressure, it is
necessary to introduce enriched oxygen released from another
adsorber in the pressure reducing step to lift the pressure.

At the end of the repressurization step, pressure in the adsorption


vessel reaches the level required by the adsorption and is ready for
the next cycle.

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Look the videos of PSA

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In the VPSA oxygen generating (VPSA-O2) process,
the blower allows the air to enter the adsorber of the
VPSA O2 unit under pressure.
Then adsorption of nitrogen, carbon dioxide, water
vapor and other components in the air takes place in the
adsorber, and oxygen streams through the adsorbent
with a small amount of rare gases, thus realizing the
separation of oxygen and nitrogen.

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The saturated adsorbent is vacuumized to desorbe
the impurities , and regenerate the adsorbent. The
whole oxygen production system is controlled by
PLC (programmable logic controller) and DCS (data
control system), and the program controlling valves
are cyclically switched to ensure constant oxygen
generation.

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To column 2 Purge with N2

1 2
2

CO2 separation CO2 separation


Inlet flue gas Step2: Evacuation Step4: Repressurization
Step1: Adsorption

Fig operational steps of Vacuume swing adsorption

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PSA and VSA Widely used for air separation
If zeolite adsorbent is used, adsorption equilibrium is the controlling
factor, with N2 more strongly adsorbed than O2 and argon
- The adsorbed gas, which is desorbed at low pressure, is quite impure
- For the separation of air, large plants use VSA because it is more
energy-efficient than PSA
- Small plants often use PSA because that cycle is simpler

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Displacement-purge adsorption (DPA); displacement-desorption

It is considered only where TSA, PSA, and VSA cannot be used because
of pressure or temperature limitations

A strongly adsorbed purge gas (displacement fluid) is used in desorption to


displace adsorbed species

Another step is required to recover the purge gas

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Displacement-purge adsorption (DPA);
 Adsorbates can be removed from the adsorbent surface by replacing
them with a more preferentially adsorbed species.
 This displacement fluid, which can be a gas, a vapour or a liquid,
should adsorb about as strongly as the components which are to be
desorbed.
 If the displacement fluid is adsorbed too strongly then there may be
subsequent difficulties in removing it from the adsorbent.

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Displacement-purge adsorption (DPA);
The mechanism for desorption of the original adsorbate involves two aspects:
 Partial pressure (or concentration) of original adsorbate in the gas phase
surrounding the adsorbent is reduced
 There is competitive adsorption for the displacement fluid. The displacement
fluid is present on the adsorbent and thus will contaminate the product.

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Displacement-purge adsorption (DPA);
One advantage of the displacement fluid method of regeneration is that the net
heat generated or consumed in the adsorbent will be close to zero because the
heat of adsorption of the displacement fluid is likely to be close to that of the
original adsorbate. Thus the temperature of the adsorbent should remain more or
less constant throughout the cycle.

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Displacement-purge adsorption (DPA);
With neither pressure nor temperature changes from adsorption to
desorption, regeneration by displacement purge depend solely on the
ability of the displacement fluid to cleanse the bed in readiness for the
next adsorption step. A typical. Displacement Purge Adsorption (DPA)
process is shown in the Figure below.

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Displacement-purge adsorption (DPA);
One application is the separation of medium-molecular-weight
linear paraffin’s (C10-C18) from mixtures of branched-chain and
cyclic hydrocarbons by adsorption on zeolite. Ammonia, which
is easily separated from the paraffin’s by flash vaporization, is
used as the purge

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A is the more strongly adsorbed component in the
binary feed mixture of (A and B) while D is the
displacement purge gas. The feed mixture of (A
and B) is passed through Bed 1 acting as the
adsorber, which is preloaded with D from the
previous cycle (when Bed 1 was the regenerator).

A is adsorbed and the product of a mixture of (B


and D) emerges from the top of the column. (B
and D) are easily separated by distillation so
that B is collected in a relatively pure state

The displacement gas D then enters Bed 2 acting as


regenerator and from which emerges a mixture of
(A and D). (A and D) can be separated
without difficulty in another distillation column.
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SECTION c FINISHED PSA AND TSA

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