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Aim :
To obtain a breakthrough curve, degree of saturation, number of transfer units, and the
volumetric mass transfer co-efficient of a given ion exchange resin.
Glass column packed with resin, stopwatch, measuring cylinder, rotameter, flasks, burette, Ion
exchange resin (Zeo Karb-225, cationic), NaOH solution, HCl solution, Oxalic acid,
phenolphthalein, deionised water.
Theory:
Ion exchange can be considered as a special case of adsorption. Adsorption uses the ability of
certain solids to preferentially concentrate specific substances from fluids in contact onto their
surfaces. A large number of industrially important examples utilizing adsorption can be cited
where fluid involved is a liquid or a gaseous mixture.
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The adsoorption wav
ve:
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reached the
t breakpoiint. The soluute concentraation now risses rapidly as the adsorpttion zone paasses
through the
t bottom of
o the bed annd e has subsstantially reaached the inittial value C0.
0
Factors affecting
a th
he breakpoin
nt and the breakthroug
b gh curve:
Factors contributing
c to the shapee of the curvee produced for
f any systeem are:
1) The actual
a rate an
nd mechanissm of the adssorption proccess
2) Naturre of adsorpttion equilibrrium
3) Fluidd velocity
4) Conccentration off solute in thee feed
5) Lenggth of the adssorbed bed
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Generally, the breakpoint time decreases with:
1) Decreased bed height
2) Increased particle size of the exchanger/adsorbent
3) Increased rate of flow through the bed height below which the solute concentration in the
effluent will rise rapidly from the first appearance of the effluent.
Adsorption equilibria:
Just as in heterogeneous system the equilibrium considerations are of great importance. The
equilibrium is affected by the temperature of the system and concentration of the solute for a
given solute-adsorbent system. In general, the equilibrium data are reported as plots of the fluid
phase (Y) and solid phase (X) concentration of the solute with temperature as a parameter. A
constant temperatire X-Y plot is the adsorption isotherm.
Various relationships for correlating adsorption equilibrium have been proposed. Amongst these,
the Freundlich equation is the most widely used relation in the laboratory and the industry. The
Freundlich equation is particularly suited for waste treatment applications involving dilute
solutions and is mathematically simple. The usual relationship for liquid phase applications is
given by the following equation
Y*=m(X*)1/n
Y* and X* are normally expressed as weight fractions on solute free basis in the liquid and solid
respectively.
An ideal adsorbent in terms of equilibrium is that which can be loaded to high concentration
(high X) at relatively low concentration of solute in the fluid (low Y). Considering the above that
both X and Y are less than unity. Thus a high index value (n<1) indicates high equilibrium
capacity of the adsorbent.
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Adsorption operations:
Both stage wise and differential contact equipments can be used for adsorption operations
1) Stage-wise Operation:
In this case, the adsorbent is brought in intimate contact with the liquid for a sufficient time to
allow close approach to equilibrium. The treated solution is filtered to remove the adsorbent and
the liquid is treated with fresh adsorbent in the next stage. The adsorbent used is generally in the
powdered form than in granular form.
In this type the fluid and solid are in continuous contact throughout the entire apparatus without
periodic separation of phases. The operation can be carried out in strictly continuous, steady state
manner. The fluid and solid continuously flow in and out of the apparatus. In addition, the semi-
batch mode can be advantageously used here since the rigid adsorbent particles can be fixed
adsorbent particles. The operation proceeds under unsteady state conditions.
In the case of solids the granular shape is more amenable to flow. Similarly, for fixed bed
applications the granular type yields much more porous bed (lower pressure drop) than the
powdered type. Therefore, for differential contact, granular adsorbent is preferred over powdered
adsorbent. Fixed bed unsteady state mode is more frequently used because of the equipment
simplicity.
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Principles of ion exchange:
An ion exchange reaction may be defined as the reversible exchange of ions between a solid
phase (the ion exchanger) and a solution phase, the ion exchanger being insoluble in the medium
in which the exchange is carried out.
If an ion exchanger M-A+, carrying cations A+ as the exchanger ions, is placed in an aqueous
solution phase containing B+ cations, the ion exchange reaction taking place is represented by
the following equation:-
M-A+ + B+ M-B+ + A+
The equilibrium represented above is an example of cation exchange, where M- is the insoluble
anionic fixed complement of the ion exchanger M-A+, often called simply the fixed anion. The
cations A+ and B+ are referred to as counter ions, whilst ions in the solution which bear the same
charge as the fixed anion of the exchanger are called co-ions. Similarly, anions can be exchanged
provided that an anion receptive medium is employed.
Most ion exchangers in large-scale use are based on synthetic resins—either preformed and then
chemically reacted, as for polystyrene, or formed from active monomers (olefinic acids, amines,
or phenols). Natural zeolites were the first ion exchangers, and both natural and synthetic zeolites
are in use today.
When NaCl solution is passed through the packed bed containing the above resin, Na+ ions are
replaced by H+ ions and outlet stream contains only HCl. As the process continues, the
adsorption zone travels downward till appoint where the entire bed is saturated by Na+ ions and
outlet stream sharply shows an increase in NaCl content. When the bed is completely exhausted,
outlet NaCl concentration becomes same as inlet NaCl concentration.
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Design of Unsteady state adsorbers based on Mass Transfer Zone or Adsorption concept:
Height of the adsorption zone is Za and θa is the time required for the formation of this zone. If
θa is the time required for travel of this zone from one end to the other end of the column and θb
is the time required for the zone to move its own height. Then,
θa = Wa/Ga where Wa=We-Wb, and Gs is the mass velocity of the effluent, kmol/m2s
θe = We/Gs
f = (Y0-Y)dW
Y0Wa
Where numeratorrepresents quantity of solute removed from the liquid upto the breakpoint
θf = (1-f) θa
Za = Zθa
θe-(1-f) θa
S = Z-Zaf
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Procedure:
Observations:
Observation Table :
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Calculations:
1. Calculation of Y
Amount (in moles) of HCl coming out of the column (a) = Titre reading x molarity of NaOH
Vol of sample titrated
3. Mass Flow Rate of NaCl (M) = Volumetric Flow rate(Q) x Density of the Solution (ρ)
5. W = Gs x t
Now, using the operating line find the values of X corresponding to values of Y obtained
from the experiment.
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Find the equilibrium concentration (Y*) corresponding to X obtained above.
Now plot 1/(Y-Y*) vs Y and find the area under the curve from YB to YE. This area equals
the NTU.
tE = WE/GS tB = WB/GS tA = tE - tB
tF = (1-f)* tA
Results:
1. S =
2. NTU =
3. HTU =
4. Ky-pa =
Conclusion:
Comments:
Refrences:
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