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Part II
EKC 313 Separation Processes
Course Strategies:
Course Activities:
Lectures in class;Tutorials; Discussions
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Equilibrium Adsorption
Adsorption can be carries out as
An equilibrium process where the fluid with solute is made to contact until
equilibrium is reached, or
As a plug flow process in a packed bed where particles are saturated with
solute as adsorption
p
front is pprogressed
g
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Equilibrium Adsorption
Equilibrium stage process
((a))
Graphically
p
y or
(b)
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Equilibrium Adsorption
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EXAMPLE
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Solution
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Solution
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EXAMPLE
In an industrial process,
process 10m3/h or glucose solution of concentration 0.2
02
g/litre is to be treated in a two stage adsorbers n series in order to obtain
a final product of concentration 0.05 g/litre. Each adsorber is using equal
amounts of adsorbent.
adsorbent Estimate the adsorbent weight per hour required in
each case.
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Solution
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After a few minutes, the solid near the inlet is nearly saturated and most of
the mass transfer take place farther (t2). The concentration gradient
becomes S-shaped.
Mass transfer zone is referred to the region where most of the
concentration
t ti changes
h
occur with
ith lilimit
it off c/c
/ 0 values
l
off 0.95
0 95 tto 00.05.
05
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At t=to, the outlet stream just begins to show the presence of adsorbate at
the exit. This point is theoretically the breakthrough point.
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Time t indicates the time when outlet concentration is 0.05 times the inlet
concentration.
The figure
g
shows a typical
yp
plot
p of the ratio of outlet solute concentration
to inlet solute concentration in the fluid as a function of time from the
start of flow. The S-shaped curve is called the breakthrough curve.
The steepness
p
of the breakthrough
g curve determines the capacity
p y of an
adsorbent bed, relating to determine the length of the adsorption bed.
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Breakthrough
g curves for (a)
( ) a narrow and ((b)) a wide mass-transfer zone
tb = break-point time
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Breakup Curve
For a unit area of bed cross section, the solute feed rate is the product of
the superficial velocity and concentration.
For an ideal breakthrough curve, all the solute fed in time t* is adsorbed
and the concentration on the solid has increased from initial adsorbate
loading W0 to Wsat. L and b are the length and the bulk density of the bed
respectively. W0 = 0 for fresh or completely regenerated adsorbent.
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The width of mass transfer zone depends on mass transfer rate, flow rate
and the shape of equilibrium curve.
When scaling up an adsorber, the key design parameter is the length of the
bed. The total length
g is split
p into the "required
q
length"
g of an "ideal" fixed
bed process and a segment of "unused bed" that is the length leftover at
breakthrough. By adding these together, a bed can be obtained to achieve
separation without wasting solute.
L design= L required usable capacity +L unused bed
The diameter of the bed is calculated from the fluid flow rate and the
desired cycle
y time. Usually,
y, superficial
p
velocities on the order of 0.15 to
0.45 m/s are targeted.
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Capacity calculations are made based on plots of the composition vs. time
(usually near the exit of the bed). Curves are integrated (analytically,
numerically,
i ll or graphically)
hi ll ) to obtain
b i capacities
i i ((measured
d iin time
i
units,
i or
how long a bed can run).
To calculate the length of unused bed from the breakthrough curve, the
totall solute
l
adsorbed
d b d up to the
h break
b k point is determined
d
d by
b integration.
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In operation, you want to stop the process before solute breaks through,
so integration
g
to the breakpoint
p
time gives
g
the "usable" capacity:
p y Most of
the time the breakthrough time is very close to the time elapsed at usable
capacity.
The unused height can also be readily measured by experiment. The total
design height of a bed is determined by adding the required usable capacity
t the
to
th unused
d height
h i ht
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Example
The adsorption of n-butanol from air was studied in a small fixed bed
(10.61cm diameter) with 300 and 600g carbon, corresponding to bed
l
length
h off 8 and
d 16
16cm. ((a)) FFrom the
h ffollowing
ll i d
data ffor effluent
ffl
concentration, estimate the saturation capacity of carbon and the fraction
of the bed used at c/c0 = 0.05. (b) Predict the breakpoint time for a bed
length of 32 cm
cm. Data for nn-butanol
butanol on Columbia JXC 4/6 carbon are as
follows:
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Solution 1
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Solution 1
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Solution 1
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Solution 1
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Solution 1
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Solution 2
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Solution 2
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Solution 2
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The cyclic-batch operating mode using fixed bed widely used for gas and
liquid feed. Separation in a fixed bed is unsteady state rate-controlled
process, properties in bed varies with position and time.
Adsorption
p
onlyy occurs in mass transfer zone which moves through
g the
bed. Applications of fixed bed adsorption include the removal of dissolved
organic compounds from water.
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Adsorbent have finite capacity for fluid phase molecules. After reaching
thermodynamic equilibrium, it is necessary either to regenerate the
adsorbent
d b
or to dispose
di
off it.
i
a.
Increase in temperature
b.
c
c.
Reduction in concentration
d.
e.
f.
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The next Section discusses typical 2-bed TSA system, and a example of a 3bed TSA system.
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(1) partial pressure (or concentration) of original adsorbate in the gas phase
surrounding the adsorbent is reduced
(2) there is competitive adsorption for the displacement fluid. The
displacement
p
fluid is present
p
on the adsorbent and thus will contaminate the
product.
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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).
g
) A is adsorbed and the pproduct 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
p
ggas D then enters Bed 2 actingg as regenerator
g
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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The equipment is more complex and hence more expensive than fixed
beds. In addition, the equipment will need to be provided to cope with
attrition of the adsorbent which will inevitably occur.
1.
2
2.
3.
4.
5.
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It involves a bed of adsorbent moving downward in a plug flow and the feed
mixture flowing upward in a plug flow through the bed void space.
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Rotary valve may not be used in some designs. The SMB process uses
multiple beds connected by pipes with control valves so that the positions
off various
i
iinlet
l and
d outlet
l flows
fl
can be
b programmed
d as a ffunction
i off time.
i
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From the adsorption section, the solids pass to the desorption section. The
solids first flow down through preheating tubes and then through
d
desorption
i tubes.
b SSteam is
i used
d for
f indirect
i di
hheating
i in
i both
b h sets off tubes
b
and for stripping in the desorption tubes.
Moving beds are used in the desorption section because the stripping
steam flow
fl
rate is insufficient
ff
ffor flfluidizing
d
the
h solids.
ld A
At the
h bottom
b
off the
h
unit, the regenerated solids are picked up by a carrier gas, which flows
upward through a gas-lift line in the centre of the vessel to the top. At the
top the solids settle out onto the top tray to repeat the adsorption part of
top,
the cycle.
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As shown schematically in the figure in next slide, the carbon adsorbent bed
moves downward opposite to the flow of liquid which flows upwards.
Spent carbon is removed from the bottom of the column and an equal amount
of fresh or regenerated
g
carbon is added to the topp of the column.
The column can be connected to a series of fixed beds stacked on top of each
other with the bottom one being removed and a new one being added at the
top.
p The column is normallyy full with adsorbent so that no expansion
p
can occur
which would cause mixing, lengthening of the MTZ and hence reduced
efficiency.
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The wheels offer a simple process by using only one vessel to house the
whole process. Besides that, the cycle times is considerably shorter
compared to fixed bed TSA processes. Thus, wheel-based processes
requiring considerably less adsorbent per unit of gas processed per unit of
time.
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Wheels had been made with diameters in excess of 4-m and are available
with silicalite, alumina, silica gel, and other adsorbents.
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An example:
p
where R represents the solid phase.
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a.
b.
c.
d
d.
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The feed mixture to be separated forms the mobile phase after injection into
the carrier fluid. This may be a liquid (liquid chromatography) or a gas (gas
chromatography).
Oft th
Often,
the mixture
i t
is
i initially
i iti ll a liliquid,
id bbutt iis vapourised
i d without
ith t d
decomposition
iti
by the carrier gas, giving a gas mixture for the mobile phase. Gas carriers are
inert and do not interact with the sorbent or components of the feed. Liquid
carriers (solvents) can interact and must be selected carefully.
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Referencs
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Tasks
Tutorial 1
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