Professional Documents
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Experiment No: 01
LIQUID-LIQUID EXTRACTION IN
A PACKED BED COLUMN
OBJECTIVE:
To study the extraction of benzoic acid from mixture of toluene and benzoic acid (dispersed phase) by
water (continuous phase) in a packed bed.
AIM:
1. To determine overall mass transfer coefficient based on continuous phase (water), Kwa
2. To determine overall mass transfer coefficient based on dispersed phase (toluene), Kta
3. To determine overall ‘Height of Transfer Unit’ based on continuous phase (water), HTUow
4. To determine Individual ‘Height of Transfer Unit’ based on continuous phase (water), HTU w and
dispersed phase (toluene), HTUt
INTRODUCTION:
Liquid extraction sometimes called solvent extraction is the separation of the constituents of a liquid
solution by contacting with another insoluble liquid. If the substances constituting the original solution
distribute themselves differently between the two liquid phases, a certain degree of separation will result
& this can be enhanced by the use of multiple contacts or their equivalent in the manner of gas
absorption and distillation.
THEORY:
Towers filled with some random packing (say raschig rings) are widely used for extraction of valuable
chemicals from dilute solutions by liquid-liquid extraction. The packing provides a larger extraction area
for mass transfer and also reduces the axial mixing to some extent. The extraction rate in such columns
depends on:
(a) Choice of either continuous or dispersed phase.
(b) Packing and column variables.
(c) Velocity of liquid phases in the tower.
The tower performance is generally based on extraction rate data and evaluated in terms of overall height
of transfer unit, based on continuous phase, HTU ow and the extraction factor expressed in terms of flow
mVw
rate ratios of the liquid phase, . These two variables are plotted against each other on Cartesian
Vt
co-ordinates. As suggested by Colburn, the slope and intercept of such a plot would represent the
resistance of the individual films as:
V is the superficial velocity of the liquid phase based on empty cross section of the column, subscript ‘w’
for continuous phase (water) and ‘t’ for dispersed phase (toluene). Rate of mass transfer from dispersed
phase to continuous phase is defined as:
N C w1 C w1 C w 2 C w2
K w aV (1)
ln C w1 C w1 / C w2 C w 2
N C1 C 2
or K w aV (2)
ln C1 / C 2
the capacity coefficient based on continuous phase (water), Kwa, is thus defined as:
N
Kwa (3)
V C w ln
C w C w2
C w ln
where, C w1
ln
C w 2
Similarly, the capacity coefficient based on dispersed phase (toluene), Kta, is defined as:
N
Kt a (4)
V C t ln
As per Chilton and Colburn, the overall height of transfer unit based on continuous phase (water),
HTUow is defined as:
Vw
HTU ow (5)
K wa
and the overall height of transfer unit based on dispersed phase (toluene), HTUot is defined as:
V
HTU ot t
Kt a
(6)
DESCRIPTION:
In this system two different liquids are used in which the one is heavier (water) which is used as solvent
and other is lighter in which the solute is present (toluene). The heavier liquid is inserted from top and
lighter from the bottom. The interface maintained in the column between the lighter phase and the
heavier phase at the top of the column can be adjusted up or down as necessary by regulating the
arrangement provided at the water stream leaving the column. The position of the interface to
be maintained at about 1 inch above the point of introduction of the heavier liquid (water in this case)
into the column. The samples are taken from the top for lighter liquid and bottom for heavier liquid and
are analyzed.
UTILITIES REQUIRED:
1. Compressed Air Supply at 2 Bar, 0.5 CFM
2. Drain
3. Laboratory Glassware
4. Water Supply
5. Weighing Balance (least count ±1gm)
CHEMICALS REQUIRED:
1. Toluene = 20 Ltrs
2. Benzoic Acid = 500gms
3. Distilled Water = 20 Ltrs
4. N/5 NaOH in alcohol = 500ml
5. N/20 NaOH in water = 500ml
6. Phenolphthalein as indicator = 10ml
EXPERIMENTAL PROCEDURE:
For the case where continuous phase (water) flow is downwards while the dispersed phase (Toluene +
Benzoic Acid) flow is upwards, the extract will be collected through the bottom while the raffinate will
be collected from the top.
1. Prepare a mixture of toluene and benzoic acid as a feed mixture, with the concentration of benzoic
acid in the range of 0.1- 0.2 kmol/m3 means 24.4gm/lit or 488gm in 20litres (i.e N/5)
2. Fill the column with the continuous phase (water).
3. Allow the dispersed phase (toluene+ benzoic acid) to enter from the bottom of the column at some
minimum rate.
4. Adjust the rotameter readings for both the phases (1 to 5 LPH for dispersed phase and 3 to 10 LPH
for continuous phase).
5. The interface between the lighter phase and the heavier phase at the top of the column must be
worked up or down as necessary by regulating the valve in the water stream leaving the column. The
position of the interface is to be maintained at about 1 inch above the point of introduction of the
heavier liquid.(water) into the column.
6. In case lighter liquid is the continuous phase, the same arrangement should be used to maintain the
interface.
7. Take the first observation after the steady state has been established i.e after 10 to 20 minutes.
8. Collect the samples of extract and raffinate and measure the concentration of benzoic acid in each by
titrating a known volume of sample with standard NaOH solution using phenolphthalein as indicator.
Use standard NaOH solution in alcohol (N/5) for titration against toluene and NaOH solution ( N/20)
in water for titration against water.
9. Repeat the above steps for 5 to 6 different flow rates of continuous/dispersed phase.
SPECIFICATION:
Extraction Column : Material Borosilicate Glass
Dia. 45mm, Height 750mm (approx)
Packing Material : Borosilicate Glass Raschig Rings Size 8-10mm (approx.)
Feed Tanks : Material SS, Capacity 20 Ltrs, 2 No.s
Extract and Raffinate Tanks : Material SS, Capacity 10 Ltrs, 2 No.s
Piping : SS and PVC, Size ¼”
Feed Circulation : By compressed air
Pressure Regulator : 0-2 kg/cm2
Pressure Gauge : Bourdan type, 0-2 kg/cm2
Flow Measurement : Rotamaters (One each for Continuous phase and dispersed phase)
Special arrangement for changing interface zone at any level in extraction column.
OBSERVATION TABLE:
S.No. Flow rate of Flow rate of water Volume of N/5 Volume of N/20
toluene phase, phase, Qw in L/h NaOH(in alcohol) NaOH(in water)
Qt in L/h used for titration for used for titration for
10ml of toluene 10ml of water
solution solution
CALCULATION:
At Top:
CT2 = g mole/L
Cw2 = 0
Cw
H2 = at CT = CT2
CT
ΔCT2 = CT2- (CW2/H2) g mole/L
C T 2 C T 1
CT ln
ln CT 2 / CT 1
(ΔCT)ln = g mole/L
N
Kt a = (g mol/ h-L-gmol/L)
V CT ln
C w1 H 1CT 1 C w1
C w 2 H 2 CT 2 C w 2
C w 2 C w1
C w ln
C w 2 g mol/L
ln
C w1
N /
Kwa g mol/L-h-ΔC
V C w ln
Vt
HTUOT = m
Kt a
Repeat the above calculations for five different flow rate ratios of continuous and dispersed phase
(Vw/Vt) and use equations (1 and 2) to determine the individual ‘ Height of Transfer unit’ based on
continuous phase (HTU)w and ‘Height of Transfer Unit’ based on dispersed phase (HTU) t, by plotting
Vw
(HTU)ow vs on a simple graph. Determine the slope and
Vt
intercept.
Intercept = (HTU)w
Slope = (HTU)t Slope
Intercept
CALCULATION TABLE:
Run Cw1 gmol/L Cw2 gmol/L CT1 gmol/L CT2 gmol/L Rate of M.T,
No. N/θ gmole/h
Aqueous Phase, Cw g mole/L, Benzoic Acid Organic Phase, CT g mole/L, Benzoic Acid
0.0000 0.0000
0.0016 0.0080
0.0064 0.0336
0.0080 0.0673
0.00961 0.08811
0.011211 0.12015
0.012816 0.14097
0.01442 0.17301
and
C w 0.0745CT 0.0019
NOMENCLATURE:
6. Always drain the column once before running the experiment on desired second flow
rates.
==== X ====
Experiment No: 02
OBJECTIVE:
Study of Adsorption in a packed bed for a Solid Liquid System.
AIM:
Plotting the break through curve of adsorption for a given system and calculation of length of unused
bed for the system.
INTRODUCTION:
A substantial number of unit operations of chemical engineering are concerned with the problem of
changing the compositions of solutions & mixtures through methods not necessarily involving chemical
reactions. One of the well known operations for solid liquid contacting is adsorption. The colored
material which contaminates impure cane sugar solution can be removed by contacting the liquid
solutions with activated carbon, whereupon the colored substances are retained on the surface of the
solid carbon.
In adsorption the molecules distribute themselves between two phases, one of which is a solid whilst the
other can be the liquid or gas. Adsorption suffers one drawback, that the capacity of the adsorbent for the
adsorbate in question is limited. At intervals, the adsorbent has to be removed from the process and
regenerated, that is restored to its original condition. For this reason, in its early applications in industry,
the adsorption unit was considered to be more difficult to integrate with a continuous process.
THEORY:
Adsorption is the selective transfer of a solute from Feed (a) (b) (c) (d)
a fluid phase to a batch of rigid particles. The usual Solution
selectivity of a sorbent between solute and carrier Concen- Co Co Co Co
tration.
fluid or between different solutes makes it possible Adsorpti
to separate certain solutes from the carrier or from on
one another. Zone
Ads
It occurs when molecules diffusing in the fluid Zone
phase are held for a period of time by forces
emanating from an adjacent surface. The surface Effluent
represents a gross discontinuity in the structure of Concen- Ca Cb Cc Cd
the solid and atoms at the surface have a residue of tration
molecular forces which are not satisfied by
surrounding atoms like those in the body of the
Break
structure. These residual or Vander Waals forces through
are common to all surface and the only reason that Curve
certain solids are designated “adsorbents” is that
they can be manufactured in a highly porous form,
giving rise to a large internal surface. 0 Ca Cb Cc o Break Point
Volume of Effluent
The uppermost layer of the bed is practically saturated, and the bulk of the adsorption takes place over a
relatively narrow adsorption zone in which the concentration changes rapidly, as shown. As solution
continues to flow, the adsorption zone moves downward as a wave, at a rate ordinarily very much slower
than the linear velocity of the fluid through the bed. At a later time, as at b in the figure, roughly half the
bed is saturated with solute, but the effluent concentration C B is still substantially zero. At c in the figure
the lower portion of the adsorption zone has just reached the bottom of the bed, and the concentration of
solute in the effluent has suddenly risen to an appreciable value C C for the first time. The system is said
to have reached the Breakpoint. The solute concentration in the effluent now rises rapidly as the
adsorption zone passes through the bottom of the bed and at ‘d’ has substantially reached the initial value
co. The portion of the effluent concentration curve between positions ‘c’ and‘d’ is termed the
Breakthrough curve. If solution continues to flow, little additional adsorption takes place since the bed is
for all practical purposes entirely in equilibrium with the feed solution.
DESCRIPTION:
The apparatus is provided for the process of Adsorption in Packed column with Solid phase being static
& fluid phase is following. For flow of fluid a pump & rotameter is provided. Three borosilicate
columns are provided having different diameters & lengths. At the inlet of column, valves are provided
to feed only one column at a time. Valves are provided at the bottom of columns & liquid tanks to drain
out after running the apparatus. Filters are provided before the column drain valves to prevent the
charcoal from drain.
UTILITIES REQUIRED:
Drain
Electricity Supply : 1 Phase, 220Volt AC and 1 KW
Floor Area : 1.2 m x 1m
Colorimeter or Spectrophotometer.
CHEMICALS REQUIRED:
Activated Charcoal : 1 Kg
KMnO4 : 15 gms.
EXPERIMENTAL PROCEDURE:
SPECIFICATION:
FORMULAE:
A calibration curve between Optical Density & Concentration is plotted, as shown below.
1E -06
8E -07 y = 2E – 06 x
6E -07
4E -07
2E -07
0E +00
O.D.
1.2E -05
8.0E -06
6.0E -06
4.0E -06
2.0E -06
0.0E +00
Data :
Initial Optical density = I0
Initial Concentration = C0 (Using calibration chart)
Height of Charcoal in 1st column = Z1
Height of Charcoal in 2nd column = Z2
Height of Charcoal in 3rd column = Z3
OBSERVATION TABLE :
CALCULATIONS:
A curve between θ & Cθ is plotted, which is called Breakthrough Curve. A curve between Wθ & Cθ may
also be plotted. ZS is calculated using flow rate V and saturation time θB. Then length of unused bed is Z-
ZS Also velocity of advancement of adsorption plane can be calculated as Z/θS.
CONCLUSIONS:
NOMENCLATURE:
1. Before starting the pump ensure that bypass valve is not fully closed & rotameter is properly
closed.
2. Before starting apparatus check properly that the drain valves of all the columns are properly
closed.
3. It should be ensure that there is no leakage from the bottom of the column.
4. Check properly that only one feed valve is open at a time.
5. The apparatus should be drained off as soon as possible as the color of liquid would clot over the
inner surfaces of the apparatus, making the apparatus yield incorrect results.
6. Pump should not be switched on at low voltage.
7. Carefully note the bed height & initial solution concentration.
TROUBLESHOOTING:
In case of any problem regarding operation of the apparatus; the apparatus should be quickly switched
off and electric supply should be cut off.
Electrical :
Electric shock : It means that either earth wire inside the panel is loose or there is no earth provide in
the socket to which the equipment is plugged. So make it sure that the equipment is earthed properly.
General :
Leakage : The point of leakage should be detected & the concerned part is tightened properly. If the
problem still persists then the part is removed & Teflon tape is wrapped on the threads properly & the
part is then refitted carefully.
==== X ====
Experiment No: 03
PERFORMANCE OF
WATER COOLING TOWER
OBJECTIVE:
Study of the heat and mass transfer in Water Cooling Tower for different flow & thermodynamic
conditions.
AIM:
To measure Tower Characteristic parameter( KaV/L) for various liquid and air flow rates(L/G) in a
counter-current Forced draft Cooling Tower. To determine the effect of L/G on [KaV/L] and estimate the
values of mass transfer coefficient Ka for various values of L/G
INTRODUCTION:
Water from condensers and heat exchangers is usually cooled by an air stream in spray ponds or in
Cooling Towers using natural draft or forced flow of air. Mechanical draft towers are of the forced draft
type, where the air is blown into the tower by a fan at the bottom. The forced draft materially reduces the
effectiveness of cooling.
THEORY:
Water may be cooled by the air as long as its temperature is above the wet bulb temperature of the
entering air. Markel’s theory is used which is based on enthalpy potential difference as the driving force.
Packing
Cooling Tower
Each particle of water is assumed to be surrounded by a film of air and the enthalpy difference between
the film and the surrounding air provides the driving force for the cooling process. In the integrated form
Markel’s equation can be written as:
T
KaV 5
dT
L T6
h h
T
KaV 5 dT T T 1 1 1 1
5 6
L h ha
T6 w
4 h1 h2 h3 h4
The carrying of liquid with gas stream is termed as Liquid Entrainment. This may be due to a high rate
of air flow. This should be avoided to get better performance. This can be avoided by following the
Operational limits of the equipment.
DESCRIPTION:
The apparatus is provided for the process of Forced draft countercurrent cooling of hot water using air.
The water to be cooled is heated in a heating tank using a heater. It is then circulated; through a
rotameter; to the top of the cooling tower mounted over the heating tank. Cooled water is then re-
circulated to the heating tank. A blower is provided for the cooling air. A valve is provided in air line to
regulate the flow rate of air. There is an Orificemeter mounted with its taps connected to a manometer to
find the flow rate of air. A set of two temperature sensors are provided both at inlet and outlet of air
stream. These sensors give Dry bulb and Wet bulb air temperatures. The cooling tower is packed with
Aluminium expanded wire mesh.
UTILITIES REQUIRED:
Water Supply
Drain
Electricity Supply:1 Phase, 220V AC, and 3kW.
Floor area of 1.2m ×1m
EXPERIMENTAL PROEDURE:
(1) Fill the heating tank with water, set the temperature with the help of D.T.C and switch on heater.
(2) Switch on pump & blower after desired temperature achieved.
(3) Set the flow rate of water and air.
(4) Record the flow rate of water and manometer reading after steady state achieved.
(5) Record the temperatures.
(6) Steps 3 to 5 may be repeated for different water and air flow rates within operational range.
SPECIFICATION:
Tower : Material Stainless Steel, Size- Cross-section 6”×6”, Height 30”
Packing : Expanded wire mesh made of Aluminium.
Air Flow Measurement : Orificemeter with U-tube manometer.
Water Flow Measurement : Rotameter
Hot Water Tank : Material Stainless Steel, Double wall, insulated with ceramic wool
Hot Water Circulation : Magnetic Pump made of Polypropylene to circulate Hot Water.
Maximum
working temperature is 85°.
Heater : 1.5 kW
Temperature Sensors : 7 No.s
Dry & Wet bulb Temp.-
- Measurement : RTD PT-100 type Sensos
Control Panel comprising of-
Digital Temp. Controller : Range:0-200°C. (for hot water tank)
Digital Temperature Indicator: Range:0-200°C, with multi-channel switch.
With Standard make On/Off switch, Mains Indicator and fuse etc.
A good quality painted rigid MS Structure is provided to support all the parts.
FORMULAE:
R water
Head in terms of air, H 1
100 air
a1 a 2
Flow rate of air, Q0 C d 2 gH
a 22 a12
Mass flow rate of air, m air Q0
Mass flow rate of dry air, G= [m/(1+Y1)]/cross-sectional area of column
Rate of humidification= mass flow rate of dry air ×(Y2-Y1) kg moisture/sec
DATA:
Orifice dia., d1 = 34mm
Cross section area of Orifice, a1 = 9.1×10-4m2
d2 = 68mm
Orifice constant, Co = 0.6
ρwater = …… kg/m3
ρair = …… kg/m3
Acceleration due to gravity ‘g’ = 9.81 m/s2
Cross section area of Chamber, A = 0.0232m2
Height of Packing = 0.75m
From the Psychometric Chart for air-water vapor at 1 atm. pressure, determine the following
corresponding to dry bulb and wet bulb temperature of the entering and leaving air:
Y1, (corresponding to T1 and T2)
h1 (corresponding to T5)
Y2, (corresponding to T3 and T4)
h2 (corresponding to T6)
OBSERVATION TABLE:
CALCULATIONS:
T
KaV 5 dT T T 1 1 1 1
5 6
L h ha
T6 w
4 h1 h2 h3 h4
CONCLUSIONS:
NOMENCLATURE:
==== X ====
Experiment No: 04
To study the rates and phenomena of diffusion into gases flowing through the pipe and also to compare
the results obtained with literature values (Sherwood& Gilliland).
THEORY:
A thin film of liquid falling down the inside of a vertical pipe through which the gas flows, constitutes a
wetted wall column. Wetted wall column have been used successfully as absorbers for Hydrochloric acid
gas, Ammonia, Acetone, Benzene and other volatile liquids. They have also been used for theoretical
studies for mass transfer because the interfacial surface between the phases is kept under control and is
measurable.
The height of a wetted wall column required for many mass transfer operations is excessive and
consequently this is not widely used. Where large quantities of liquid or gas have to be handled it would
be necessary to arrange many vertical pipes in parallel and this leads to difficulties in the distribution of
the liquid into the inner surface of the tubes. The gas pressure drop from this type of equipment is very
low, however since it is almost entirely confined to skin friction effects, with few or no expansion or
contraction losses.
Mass transfer rates for fluids flowing through pipes have been studied more completely than other cases.
The rates of diffusion into gases flowing through pipes have been studied with the help of wetted wall
columns, shown schematically in Figure. A volatile liquid is permitted to flow down the inside surface of
a circular tube, while a gas is blown upward or downward through the center of the pipe.
Measurement of the rate of evaporation of liquid into the gas stream over the known surface permits the
calculation of the mass transfer coefficient for the diffusion of the vapor into the gas stream. Since the
liquids may be pure liquids, the concentration gradient for the diffusion exists entirely within the gas
stream and coefficient KG may be obtained directly from the data. Sherwood and Gilliland conducted a
series of experiments of this sort, using a variety of volatile liquids with air in turbulent flow. For
graphical representation refer to Coulson & Richardson volume 2. Here the mass transfer coefficients in
the form of a dimensionless group are plotted against the Reynold number of the gas for the system Air-
Water (SC=60).Similar data obtained for volatile liquids is shown in the upper line. For gases, values of
Re from 2000 to 35000 were covered and Sc from 0.6 to 2.5 with gas pressure varying from 0.1 to 3.0
atm.
The average slope of the line in graph is 0.83 so that the groups (KG*d/D)* (PB,M/P) and (KL*d/D) vary as
Re0.83. In another graph the intercepts of these lines at Re = 1000 are plotted against the corresponding
values of Sc on logarithmic coordinates. The principal line of this graph has a slope of 0.333. The
equation, which describes all the data, for both the liquid and gas flow, is therefore,
This empirical relation is quite remarkable in the manner in which it generally confirms the relationship
between heat, mass and momentum transfer developed theoretically. It should be noted that the
evaporation of the volatile liquids in a wetted wall column results in cooling of the liquids
and consequent simultaneous heat transfer between liquid and gas.
The heat transfer rates are somewhat higher than those given by the equation,
Owing to ripples and waves on the liquid surface, it should also be noted that data for gases only in
graphs (Sc = 0.6 to 2.5) are correlated empirically better by the relation,
DESCRIPTION OF EQUIPMENT:
Air is supplied to the column at the bottom by means of blower. Bypass valve V 1 and control valve V2
are used for varying the airflow rate. The condition of air at inlet and outlet from the column are
measured by the wet bulb and dry bulb thermometer, respectively. Water inlet and outlet temperatures
are measured by the thermometers T1 and T2. A wire mesh screen is placed over the surface of the tube.
Manometer M1 and M2 measure the pressure drop across column and air flow rates. Water flow rate is
measured by rotameter readings.
PROCEDURE:
Water is fed to the column at a rate at which complete wetting with a minimum of ripple
formation is visible.
The blower is started and a minimum flow of air is maintained.
After about 5 minutes when steady state conditions could have reached, the humidity of air inlet
and outlet are determined by the readings of the wet and dry bulb thermometers and by the use of
a psychrometric chart.
Water flow rate and inlet and outlet temperatures are recorded.
From steam tables vapor pressure at the water temperature is noted.
OBSERVATION TABLE:
***Sample observations
CALCULATIONS:
∆PW1 = Pw1-pw1
Where,
Pw1 = pure component vapor pressure of water at outlet water temperature T1
∆Pw2 = Pw2-pw2
Where,
Pw2 = pure component vapor pressure of water at inlet water temperature T2.
NOTE: The partial pressure can be calculated from the humidity values obtained from psychrometric
chart by using recorded wet and dry bulb temperature of air at top and bottom.
SAMPLE CALCULATIONS:
(for sample observations)
= 0.95 /1.2267
=0.7743
Amount of water absorbed by air (evaporated)
Nw = QA ((pw2-pw1)/P) K-mole/sec
= 0.0095*2.5/760
NW = 0.00003125
Where,
d = ID of the column
In terms of mass transfer coefficient Kg the rate of mass transfer is given by,
Nw /A = KG*(∆PB, M)
KG = NW / (A*∆PB,M) k-mole/m2.s.mm Hg
= 0.00003125/3.14*0.0254*0.7743)
= 0.0005060 k-mole/m2.s.mmHg
CONCLUSIONS:
NOTES:
lnP = A-B/(T+C)
where,
A = 18.3036; B = 3816.44; C = -46.13 (for water)
H = [pw/(P-pw)]*(Mwater/Mair)
Where,
H = absolute humidity
P = atm. pressure
Mwater = 18 kg/Kg-mole
Mair = 29 Kg/Kg-mole
==== X ====
Experiment No: 05
AIM:
To determine diffusion coefficient or diffusivity, of given liquid (acetone) in air by using ARNOLD’s
cell.
APPARATUS:
Arnold’s cell, Thermometer and Scale for measuring drop in height of solvent.
CHEMICALS: Acetone
THEORY:
This is the case of pseudo-steady state diffusion in which one of the boundaries shift with time the effect
that the length of the diffusion path changes, though only by a small amount over a long period of
exposure.
When this condition exists:
NA,Z = (DAB/Z)×(P/RT)×(1/PB,lm)×(PA1-PA2)
Where,
Z = Z1 - Z2 = the length of the diffusion path in time t.
NA,Z = (ρA,L/M)×(dz/dt)
(ρA,L/M)×(dz/dt) = (DAB/Z)×(P/RT)×(1/PB,lm)×(PA1-PA2)
DAB(P/RT)×(1/PB,lm)∫dt = (ρA,L/M)∫Zdz
(DAB)×(P/RT)×(1/PB,lm)×(PA1-PA2)t=(ρA,L/M)×(1/2)×(z12-z22)
PROCEDURE:
Acetone is filled in capillary tube and air bubble, if present, is removed from the tube carefully.
Note down the initial height (H0) of the acetone level in the tube.
The tube is placed in a water bath to maintain the constant temperature. Note down the
temperature of the water by thermometer.
Switch on blower, which blown air across the opening of capillary tube continuously to remove the
vapors evaporated that rises from the surface of the liquid.
At regular interval of time note down the drop in the level of acetone.
Do necessary calculations and find out the diffusivity (D) from the equation.
Also calculate the diffusivity from the GILLILAND’s equation (as given below) at the same
temperature using standard data and compare the result with the experimental one.
Repeat the same procedure for two-three different temperatures by increasing and maintaining
constant temperature of the water bath and calculate the diffusivity by both the methods. State your
conclusion precisely at the end.
D = (4.3×10-4)×(T)1.5(1/MA+1/MB)0.5/(P×(VA1/3+VB1/3))
OBSERVATION TABLE:
SR.NO. TEMP (°C) INITIAL HEIGHT FINAL HEIGHT OF TIME (Sec.)
OF LIQUID (mm) LIQUID (mm)
CALCULATIONS:
PA1 = ___________________ mm Hg
2. PB1 = P-PA1
4. PB2 = P-PA2
PB,lm = (PB2-PB1)/ln(PB2/PB1)
5. ρA = ______________________kgmol/m2sec
6. Z1 = __________cm , Z2 = __________cm
DATA:
2. R = 8314 N. m/kmol K
4. Density of acetone
D = (4.3×10-4)×(T)1.5(1/MA+1/MB)0.5/(P×(VA1/3+VB1/3))
= ________________m3/kmol
=_________________m3/kmol
=_________________kg/kgmol
= _________________kg/kgmol
T = Absolute temp.
=__________K
RESULTS:
CONCLUSIONS:
==== X ====
Experiment No : 06
GAS ABSORPTION IN
MECHANICAL AGITATOR
THEORY:
The process of absorption of the gas in the liquid is really entirely a physical one. However in number of
cases in which the gas on absorption reacts chemically with a components of the liquid phase. Thus in
absorption of CO2 by NaOH the CO2 reacts directly with the NaOH and the process of absorbed in
Ethanolamine solutions there is direct chemical reaction between the Amine and the gas. In such cases
there is a liquid film followed by a reaction zone.
The effective interfacial area a in the gas liquid contractor is an important mass transfer characteristic in
the design of the contractor.
The system used in this experiment is a gaseous solvent ‘A’ dissolving in a liquid acid simultaneously
reacting with the reactant ‘B’ present in the liquid phase.
A + bB AB Products
The new products AB formed diffuse towards the main body of the liquid. The concentration of B at the
interface falls; this results in diffusion of B from the bulk of the liquid phase to the interface. Since the
chemical reaction is rapid, B is removed very quickly so that it is necessary for the gas A to diffuse
through the part of the liquid film before meeting B. There is thus a zone of reaction between A and B
which moved away from the gas liquid interface taking up some position towards the bulk of the liquid.
The final position of the reaction zone will be such that the rate of diffusion of A from the gas liquid
interface is equal to the rate of diffusion of B from the main body of the liquid. When this condition has
been reached the concentration of A, B and AB can be indicated as shown in the figure.
According to the film model if the reaction is fast enough the solute A will be consumed by the reaction
in the liquid film itself and its concentration will be zero at the end of the liquid film. The condition for a
fast second order reaction is,
D A * K A * BO / K L 2 >3 (1)
Where,
DA - Diffusivity of A, m2 / sec
KA - Second order reaction constant, m3 /kmol. Sec
[Bo] - Concentration of B in bulk liquid, kmol / m3
KL - Liquid side mass transfer coefficient, m /sec
In such a case the reaction occurs simultaneously with the diffusion process in the liquid film and
therefore enhances the rate of absorption significantly. If the reactant B is present in far excess of the
stoichiometric requirements for the reaction in the film, then the depletion of the reactant concentration
in the film is negligible. The condition for such a case is given by,
Under such conditions the reaction can be considered to be pseudo first order with respect to the solute
A, and the volumetric rate of absorption of A is given by,
*
R A a a * Ao * D A * K 2 * Bo (3)
From the equation (1) it is clear that the rate of absorption is a unique function of the physico-chemical
properties and completely independent of the hydrodynamics of the system.
The absorption of carbon dioxide by caustic soda or potash is accompanied by an irreversible chemical
reaction and the partial pressure of CO 2 in equilibrium with the solution is zero. The reaction with
sodium carbonate to form sodium bicarbonate is reversible; the equilibrium partial pressure depends on
the normality of the solution (as ½ Na2CO3 + NaHCO3), on the fraction of carbonate converted to
bicarbonate and on the temperature. This relation may be expressed graphically (Sherwood and pigfor,
1952) or by the equation,
p 137 f 2 N 1.29 / 1 f 365 t
Where,
P is the equilibrium partial pressure, mm. of mercury,
N is the normality,
f the fractional conversion to bicarbonate,
t the temperature, 0F
and S is the solubility of pure CO2 in water at a pressure of 1 atm, in gmole/litre.
The equation may be used also to determine the partial pressure in equilibrium with potassium carbonate
– bicarbonate solutions. If the constant 137 and 365 are replaced by 45 and 302 respectively.
The absorption of carbon dioxide is followed by a hydrolysis reaction in solution which can
be represented by the equations:
CO2 OH HCO3 I
CO2 H 2 O H HCO3 II
The reaction rate constants determined by Himmelblau and Babb (1958) at 200C are
The first reaction is operative in the absorption of carbon dioxide by caustic solutions. Since this is a fast
reaction the factors controlling the absorption are the rates of diffusion of the reactants in the liquid
phase. The second reaction is slow and controls the rate of absorption in carbonate solutions. Nijsing et
al. (1958, 1959) have investigated the kinetics of absorptions by caustic and carbonated solutions in
Wetted-wall columns and Danckwerts and Kenddedy (1959) discuss the results obtained from
experiments of absorption in a liquid film on a rotating drum. The experimental results on the absorption
of carbon dioxide by alkaline solutions are usually expressed as the overall gas film coefficient because
the concentration gradient in the liquid is unknown. Justification of this procedure is afforded by the
work of Pozin (1947) who showed that the rate of absorption in a batch absorber was proportional to the
partial pressure of carbon dioxide in the gas phase.
The results of spector and Dodge show that the coefficient K Ga is inversely proportional to the square
root of the absolute gas pressure and tends to decrease as the packed height is increased. The data
showed good agreement with results from a commercial installation. The coefficients for caustic potash
solution were 20 to 30 % higher than those for caustic soda of the same normality.
The dependence of the coefficient on the gas flow rate is an indication that at very low concentrations
the absorption of carbon dioxide is partially controlled by the gas phase coefficient. Tepe and dodge
(1943) showed that at higher concentrations (2% CO 2) the absorption is wholly controlled by the liquid
film. The coefficient was independent of the gas rate and proportional to the 0.28 power of the liquid
rate.
Effect of temperature and the effect of the sodium hydroxide concentration and the degree of conversion
to sodium carbonate. The coefficient value when the total sodium concentration is 1.8 normal.
The effect of varying the carbon dioxide concentration in the gas phase over a rang e form 3 to 28% has
been investigated by Blum, Stutzmanb and Dodds (1952). The overall gas film coefficient, K Ga was
found to be independent of the gas flow rate but dependent on the liquid flow rate, the concentration
(normality) of the alkali, and on the partial pressure of carbon dioxide in the gas. The experiments of
absorption in sodium hydroxide solution showed that KGa increased with the normality of the sodium
hydroxide up to 1.5N, but was not affected by a further increase in concentration.
The effect of the partial pressure of the carbon dioxide was a function of the normality of the liquid. At
high normality (above 1.5 N) K Ga decreased as the average partial pressure had no effect on the
coefficient. At lower normality (0.99 N) the coefficient decreased as the partial pressure increased
throughout the range of the experimental data. The coefficient decreased progressively as the sodium
hydroxide was converted to carbonate. The volumetric coefficient, K Ga appeared to be independent of
the packing size. The coefficients of absorption of carbon dioxide in potassium hydroxide were
appreciably higher than those for sodium hydroxide under equivalent conditions. It was
assumed that the following chemical reactions occur in solution:
OH CO 2 HCO3
OH HCO3 H 2 O CO3
CO3 CO2 H 2 O 2HCO3
The second reaction was throught to be rapid and the third reaction irreversible in the presence of OH -
ions. The rate of absorption Na (lb.mole/hr.) in a tower of unit cross section (1ft2) and height h (ft.)
Na K ' h OH CO3
/ ' m
Where K’ is a function of the liquid rate and μ’ is the lonic strength of the solution. A satisfactory
correlation of the results was obtained when
m = 1.09
K’ = 0.0176L0.84
The absorption of carbon dioxide by sodium and potassium carbonate solutions has been studied by
Payne and Dodge (1932), Comstock and Dodge (1937) and Furnas and Bellinger (1941). The rate of
absorption is controlled by a slow chemical reaction in the liquid phase. It is independent of the gas rate
and decreases with increasing normality of the solution and with conversion of the carbonate to
bicarbonate. Payne and Dodge noted that the coefficient is approximately proportional to the liquid hold-
up in the tower.
One of the most important industrial applications of carbon dioxide absorption lies in the production of
synthesis gas for synthetic ammonia or the manufacture of hydrocarbon products by the Fischer-Tropsch
process. The synthesis gas, which may be produced by the partial combustion of natural gas or by the
gasification of coke in producer gas or water gas plants, contains a high proportion of carbon dioxide
which must be removed by absorption in a suitable solvent. To overcome the relatively low solubility of
carbon dioxide, the absorption is usually carried out at a pressure of 10 to 50 atm. At high pressure it is
possible to remove the carbon dioxide by solution in water, but this has the disadvantage that the
pumping costs are high owing to the large quantities of water which must be circulated through the
absorption towers. The liquid flow rates can be reduced by absorbing the carbon dioxide in a solution of
sodium or potassium carbonate or mono-or diethanolamine. The solution is regenerated by heating at a
lower pressure to drive off the carbon dioxide.
Benson, Field and Jimeson (1954) Benson, Field and Haynes (1956) have discussed the relative merits
of carbonate and amine solutions for the removal of carbon dioxide from synthesis gas at 300 lb / in 2
pressure. Potassium carbonate is preferred to sodium carbonate owing to its greater solubility in water
and the reduced risk of deposition of solid bicarbonate in the absorber. A comparison of potassium
carbonate and mono-ethanolamine showed that the farmer had two important advantages; less heat is
liberated in the absorber owing to the smaller heat of solution of carbon dioxide in potassium
carbonate solution, and the regeneration can be carried out at a lower temperature. This made it possible
to carry out the absorption and regeneration of potassium carbonate solution over the same temperature
range (225 to 2400F) and considerable savings in heat could be effected. The absorption was carried out
at a gas pressure of 300 lb / in2 and the solution regenerated by reducing the pressure to 5 lb / in 2 gauge
and stripping the solution with steam.
PROCEDURE:
Initially start the air compressor and collect sufficient air in the pressure tank so as the pressure is
about 3-4 kg/cm2. Prepare the dilute NaOH solution in the tank. Open the valve of the pressure
tank and allow the air to pass through the column. Set the air flow at the desired value and then
open the valve on the CO2 cylinder and adjust the flow rate to predetermined value. After
sometime take the sample at various points (liquid as well as gas) and analyze them.
Initially start the liquid flow at sufficiently high rate to ensure that the agitation in the vessel
should be well.
The flow rates of gas and liquid are adjusted at predetermined values. The CO 2 flow rate should
be such that the % CO2 in the mixed gas is about 8-10%. The gas velocity has no effect on the
interfacial area in a vessel.
Hence a value of VG between 0.1-0.2 m/s may be chosen for all the experiments and keeping it
constant. The linear superficial liquid velocity V is the most important variable. The range for V
should be fixed between 0.001-0.007 m/s.
The system is allowed to reach steady state after fixing the liquid level in the bottom section at a
marked height. Inlet and outlet liquid samples are withdrawn for analysis. This procedure is to be
repeated for 6-7 different values of VL chosen in such a way that the range indicated is fully
covered.
OBSERVATIONS:
Chemical Reaction:
CO2 + NaOH NaHCO3
NaHCO3 + NaOH Na2CO3 + H2O
Final Reaction:
2NaOH + CO2 Na2CO3 + H2O
OBSERVATION TABLE:
Sr. No. Flow rate of Air Flow rate of Burette Time Sec.
LPM CO2 LPM Reading ml
CALCULATION:
The concentration of NaOH used should be between 2 – 2.5 g mol/lt. The inlet CO 2 percentage is
kept around 10%. Under these conditions the equations (1) and 92) are satisfied and the
absorption of CO2 is accompanied by a fast pseudo first order reaction.
5 ml of sample (or 10 ml) is titrated against standard HCl of molarity (approx. 1 gmol/litre) using
phenolphthalein as an indicator. Titrate Value (V1) = …………. ml.
Initially feed of NaOH in gmol/min.
Feed normality of NaOH solution is = …………… gmol/min.
After steady state titrate the product with 0.1 N HCl solution use phenolphthalein as an indicator.
gmmoles of CO2 in feed = [(Flow rate*10-3*density) / Molecular weight] * 1000
= [(………...*10-3*1.5) / 44] * 1000
= ……………………. mmmoles / min.
gmmoles of NaOH in feed
= Normality of feed
=
=
RESULT:
CONCLUSION:
==== X ====
Experiment No : 07
BATCH CRYSTALLIZATION
BATCH CRYSTALLIZATION
OBJECTIVE:
Study of crystallization
AIM:
To study the crystallization of MgSO4.7H2O in a batch crystallizer.
To verify the material balance around the crystallizer.
To determine the yield of MgSO4.7H2O crystals.
INTRODUCTION:
Crystallization is the formation of solid particles within a homogeneous phase. Its wide use has a two-
fold basis, a crystal formed from an impure solution is itself pure and crystallization affords a practical
method of obtaining pure chemical substances in a satisfactory condition for packing and storing. This
operation involves both heat and mass transfer.
THEORY:
Crystallization is the process whereby a solid separates from a solution because conditions have been
imposed on the solution to allow the solid phase to form and particles of crystalline character to grow to
a size sufficiently large to allow separation by physical methods.
A saturated solution containing the solute is altered by either cooling, evaporation of solvent, or addition
of another substance so that the ability of the solvent to dissolve the solute is lessened, and a fraction of
the solute forms a solid phase, which may be removed from the mixture.
From the solubility or phase diagram the effect of changes in the temperature and solute and solvent
concentrations can be seen.
Based on the material balance, the yield of crystals resulting from cooling and or loss of solvent due to
evaporation can be estimated from:
WR C1 C 2 1 V
Y
1 C 2 R 1
The physical properties of saturated solutions and slurries may be obtained from:
p F
s
F X 1 X p
Viscosity:
4.11
0.64
s f e
SATURATED SOLUTION:
A saturated solution is a solution which is in equilibrium with a solid phase of the dissolved material. A
saturated solution has in it the maximum quantity of the solute at that temperature.
The super saturation of a given solution cannot become infinitely large. There is a limit. This limit is
encountered when there occurs a spontaneous formation of solid crystals known as nuclei.
If these nuclei are allowed to grow, crystals are formed and the system reverts to the equilibrium state.
The process of crystallization is show in figure:
Temp.
Coolin
g
Equilibrium Solubility
BATCH CRYSTALLIZATION: Batch crystallization is characterized by the fact that the system is
always in the unsteady state. The initial super saturation at which crystallization starts will drop quickly
from relatively high value to the saturation value. If crystal growth is to continue, the
solution must be maintained in the meta-stable region. As a consequence, cooling must continue and the
batch temperature must continue to drop during the growth period. In batch crystallization it is
comparatively easy to penetrate the labile zone producing a fine mass of fine crystals. By using
controlled seeding the solution will not become labile thereby aiding crystal growth.
T vs Concentration
50
Concentration (gm solid / gm solution)
45
40
35
30
25
20
15 C = 0.494 T + 25.85
10
05
0
0 5 10 15 20 25 30 35 40 45
T (0C)
DESCRIPTION:
Cooling type agitated batch crystallizer set up consists of an open jacketed stirred vessel provided with
water heating and cooling arrangement. The feed is prepared in the crystallizer itself with hot water and
stirrer. The hot super saturation solution in the crystallizer is then cooled by circulation of cooled water
and crystals are formed.
UTILITIES REQUIRED:
Water Supply
Drain
Electricity Supply: 1 Phase, 220V A.C, 1.5kW
Required Chemicals: MgSO4.7H2O
EXPERIMENTAL PROCEDURE:
1. Prepare a saturated solution of MgSO4.7H2O in water at 80°C by dissolving 66.2gm MgSO 4.7H2O in
100gms of solution (1.9856gm MgSO4.7H2O per gm of free water). The crystallizer should be filled
to 3/4th the capacity. Prepare about 1.5L of solution of MgSO4.7H2O and water. During mixing, the
agitator should be used for effective mixing.
2. After uniform mixing has been achieved, stop the electric supply to the electric heater.
3. Allow the flow of cold water (20°C) to pass through the jacket at a pre-fixed flow rate with the help
of water by-pass valve & a Rotameter. Record the flow rate (flow rate may be fixed such that the rise
in cooling water temperature is maximum around 5-7°C maintain by using ice.)
4. Record the temperature of inlet water and solution temperature with the help of respective sensors.
5. Put 10gm MgSO4.7H2O in the crystallizer when the temperature rises to 50°C for
seeding.
6. Carry out the crystallization process for about 2 hours.
7. After 2 hours, stop the cooling water supply, open the valve fixed at the cone of the crystallizer and
collect the slurry in the bottom receiving tank that is fixed with a mesh at the top. The crystals shall
be collected on the mesh and liquid in the tank.
8. Collect all the crystals from the mesh on a filter paper and weigh. Let the weight of the product
crystals be P (kg). For collecting all the crystals you may flush the crystallizer tank with 100-200ml
of saturated MgSO4 solution.
9. Steps 1-8 may be repeated with the addition of known weight of seed crystals at step 6.
10. Steps 1-8 may also be repeated for different values of cooling water flow rates.
SPECIFICATION:
Crystallizer = Material SS, Capacity: 2Ltrs with (jacketed) conical bottom.
Stirrer = FHP
Heater = Nichrome Wire Heater
Cooling Water Tank = Material SS, Capacity 30 Ltrs, fitted with
pump
Flow measurement = Rotameter for cooling water
Pump = FHP
Receiving Tank = Material SS, Capacity 2Ltrs, with SS sieve
Piping = SS and PVC ¼”
Temp. Sensors = RTD PT-100 type
Control Panel consists of:
Digital Temp. Indicator = 0-199.9°C, RTD PT-100 Type with multi-channel switch
With Standard make on/off switch, Mains Indicator etc. the whole set up is well designed and arranged
in a good quality painted structure.
FORMULAE:
Amount of wet crystals of MgSO4.7H2O collected after 2 hrs = P kg
Crystal yield = Feed – Mother Liquor
This must be equal to P the observed yield.
P
% Re cov ery
CrystalYie ld
CALCULATIONS:
0.662 gmMgSo4 .7 H 2 O
= 1.9586 gm MgSO4.7H2O /gm of water
(1 0.662) gmOfWater
MATERIAL BALANCE:
Feed
Mother liquor
Material balance as expressed in the table can be compared with the actual quantities recorded during the
experiment. Discrepancy if any should be accounted for.
P
% Recovery = 100
3.305
CONCLUSIONS:
NOMENCLATURE:
TROUBLESHOOTING:
1. If any type of suspended particles comes in the rotameter, then remove the rotameter, clean the
tube and then fit it at its place.
2. If there is any leakage, tight that part or remove that and re-fix that again after wrapping Teflon
tape.
3. If D.T.I display ‘I’ on display board it means sensors connection are not O.K tight that.
4. If switch ON the heater but temperature can’t rise but panel LED is ON it means bath heater had
burned replace that.
==== X ====
Experiment No: 08
DIFFERENTIAL DISTILLATION
DIFFERENTIAL DISTILLATION
AIM:
To verify Rayleigh’s Equation by carrying out differential distillation of Binary Mixture.
THEORY:
Differential distillation is a batch operation. The operation is used to separate a liquid mixture whose
components have fairly large difference in their boiling points. This type of distillation is frequently
employed in laboratory to concentrate one component in the distillate or residue and where some loss of
the material is tolerated.
Differential distillation is a process of infinite number of successive steps, where, in each step an
infinitesimal portion of a liquid is vaporized and the resulting vapor, which is in equilibrium with the
liquid, is removed. Distillation is continued until the desired composition of the distillate is obtained.
Rayleigh developed a mathematical equation to give the composition of the distillate and the bottoms.
Let y* be the mole fraction of more volatile component in vapor. Y* is in equilibrium with x.
If dL differential amount of liquid vaporized, then by applying the material balance with respect to the
more volatile component we get:
Lx =(L-dL)(x-dx)+y*dL
=L x-x dL -L dx + dL dx + y*dL
dL(y*-x)= Ldx
(dL/L) = ( dx/y*-x)
ln(F/B)= ∫(dx/y*-x)
Using the vapor-liquid equlibrium data for the binary system, the plot is made of 1/(y*-x) vs. x. Area
under the curve between the ordinates at xB and xF gives the value of the integral on the R.H.S. of the
above equation.
From this we can obtain the value of B, the amount of bottoms to be left to attain the given composition
xB of the liquid. Alternatively if we want to calculate the composition of bottoms, when B is known, then
L.H.S. of the above equation can be found out and value of xB adjusted to obtain the area under the curve
equal to ln (F/B).
For an ideal system, relative volatility is constant. Therefore for an ideal system we can use:
y* = (α x /1 + (α -1)x)
ln(FxF/BxB) = α ln(F(1-xF)/B(1-xB))
EXPERIMENTAL SETUP:
The experimental set up to study the differential distillation consist of a 2000 ml single neck round
bottom flask with suitable heating mantle (with sun wig regulator to control the temperature, ON/OFF
switch and indicator lamp), a still head with thermo-pocket (to measure the temperature) is provided
over the flask to route the vapors emerging from the flask to the Lei big type water condenser 400 mm
long). Condensed vapors are collected in collecting beaker and the entire assembly is supported with the
help of a stand.
EXPERIMENTAL PROCEDURE:
1. The distillation assembly is charged with 700-750 gm of binary mixture after noting the
refractive index with the help of Abbe’s Refractometer.
2. The heating mantle is turned ON with the regulator set near to 40% and the condenser water is
then started.
3. The distillation is continued for sufficient time so that 70% of the distillate is collected.
4. The weight of the bottoms and refractive index is noted after cooling down to room
temperature. Similarly the weight and refractive index of the distillate is noted.
5. Using Abbe’s Refractometer prepare a graph of the more volatile component vs. refractive
index. For this initially take 10 ml of comp. A and 90 ml of component B. Measure the
refractive index and convert the composition of the mixture in mole fraction. Repeat the same
for (20+80, 30+70, 40+60, 50+50, 60+40, 70+30, 80+20, 90+10). You will find this plot to be a
linear one and this can now be used to determine the composition in terms of mole
fraction once the refractive index is known.
Use the equation with relative volatility (α) assuming it to be as constant and calculate the x B and
compare it with experimentally obtained value.
SAMPLE CALCULATIONS:
N1 V1= N2 V2
= 31.05
3) Weight of water in feed solution
= (200/18)/11.628 = 0.955
To find mole fraction of water (molar volatile component) in distillate in residue after distillation.
1) Normality of residue
N1 V1 = N2 V2
N1 = 1×15.2/5 = 3.04 N
= 3.04× 60.05×0.058
= 10.58 gms.
= (10.58/60.05) + (47.41/18)
= 2.8099
= (47.41/18)/2.8099
= 0.9373
Ln(F/W) = ln(2.633/2.8099)
= 0.9329
CONCLUSIONS:
==== X ====
Experiment No: 09
ABSORPTION IN
PACKED BED COLUMN
THEORY:
The process of absorption of the gas in the liquid is entirely a physical one. However in number of cases
in which the gas on absorption reacts chemically with a component of the liquid phase. Thus in
absorption of CO2 by NaOH the CO2 reacts directly with the NaOH and the process of mass transfer is
made much more complicated. Similarly when CO2 is absorbed in Ethanolamine solutions there is direct
chemical reaction between the Amine and the gas. In such cases there is a liquid film followed by a
reaction zone.
The effective interfacial area a in the gas liquid contactor is an important mass transfer characteristic in
the design of contactor. In the case of packed column a is determined by the velocity of the liquid
(dispersed phase) and properties like wetting characteristic of packing etc. this experiment is designed to
verify the theory of absorption accompanied by a fast chemical reaction. Due to fast chemical reaction
the concentration of CO2 is bulk of the liquid is always zero and hence the liquid phase residence time
need not be determined.
In packed column a increases very rapidly with V L initially (at low values of VL in the range of 0.001-
0.004 m/s). The increase in a become less significantly at higher values of V L and eventually the lot of a
Vs. VL flattens. The value of VL beyond which there is no significant increase a is called the minimum
wetting velocity (MWV).
The system used in this experiment is a gaseous solvent ‘A’ dissolving in a liquid acid simultaneously
reacting with the reactant ‘B’ present in the liquid phase.
A + bB AB Product
The new product AB formed diffuses towards the main body of the liquid. The concentration of B at the
interface falls, this results in diffusion of B from the bulk of the liquid phase to the interface. Since the
chemical reaction is rapid, B is removed very quickly so that it is necessary for the gas A to diffuse
through the part of the liquid film before meeting B. there is thus a zone of reaction between A and B
which moved away from the gas liquid interface taking up some position towards the bulk of the liquid.
The final position of the reaction zone will be such that the rate of diffusion of A from the gas liquid.
Interface is equal to the rate of diffusion of B from the main body of the liquid. When this condition has
been reached the concentration of A, B and AB can be indicated as shown in the figure.
According to the film model if the reaction is fast enough the solute A will be consumed by the reaction
in the liquid film itself and its concentration will be zero at the end of the liquid film. The condition for a
fast second order reaction is,
D A * K A * BO / K L 2 3 -- (1)
Where,
DA Diffusivity of A, m2/sec
KA Second order reaction constant, m3 /kmol.sec
[BO ] Concentration of B in bulk liquid, kmol/m3
KL Liquid side mass transfer coefficient, m/sec
In such a case the reaction occurs simultaneously with the diffusion process in the liquid film and
therefore enhances the rate of absorption significantly. If the reactant B is present in far excess of the
stoichiometric requirements for the reaction in the film, then the depletion of the reactant concentration
in the film is negligible. The condition for such a case is given by,
Under such conditions the reaction can be considered to be pseudo first order with respect to the solute
A, and the volumetric rate of absorption of A is given by,
from the equation (1) it is clear that the rate of absorption is a unique function of the physico-chemical
properties and completely independent of the hydrodynamics of the system.
The absorption of Carbon dioxide by caustic soda is accompanied by an irreversible chemical reaction
and the partial pressure of CO2 in equilibrium with the solution is zero. The absorption of CO 2 is
followed by a hydrolysis reaction in solution which can be represented by the equations:
CO2 + OH- = HCO3-
CO2 + H2O = H+ + HCO3-
The reaction rate constants determined at 25°C are;
Reaction I: k = 2.77×10-5 sec-1
Reaction II: k = 0.0149 sec-1
The first reaction is operative in the absorption of CO 2 by caustic solutions. Since this is a fast reaction
the factors controlling the absorption are the rates of diffusion of the reactants in the liquid phase. The
second reaction is slow and controls the rate of absorption in carbonate solution. The experimental
results on the absorption of CO2 by alkaline solutions are usually expressed as the overall gas film
coefficient because the concentration gradient in the liquid is unknown. The results show that the
coefficient KG a is inversely proportional to the square root of the absolute gas pressure and tends to
decrease as the packed height is increased The dependence of the coefficient on the gas flow rate is an
indication that at very low concentration the absorption of CO2 is partially controlled by the
gas phase coefficient. At higher concentration (2% CO2) the absorption is wholly controlled by the liquid
film.
The effect of temp, NaOH concentration and degree of conversion to sodium carbonate:
The effect of varying the carbon dioxide concentration in gas phase over a range from 3 to 28%, the
overall gas film coefficient, KG a, was found to be independent of the gas flow rate, the concentration of
alkali, and the partial pressure of CO2 in the gas .The experiments of absorption in NaOH solution
showed that KG a increased with the normality of the NaOH up to 1.5 N, but was not affected by a further
increase in concentration. The effect of the partial pressure of CO 2 was a function of the normality of the
liquid. At high normality (above 1.5 N), KG a decreased as the average partial pressure increased up to a
value of 0.06 atm , but further increase in partial pressure had no effect on the
coefficient The coefficient decreased progressively as the sodium hydroxide was converted to carbonate.
The volumetric coefficient, KG a appeared to be independent of the packing size
EXPERIMENTAL SETUP:
The equipment consists of one column arranged on the top of the other. Liquid re-distributor and
sampling point (pressure tapping) is provided at the top, bottom of the assembly. Rota meters to measure
the flow rate of Carbon Dioxide, Air and dilute solution of Sodium Hydroxide individually are also
included. The CO2 is supplied from the cylinder provided and air from the air compressor. Online
mixture is provided for the gases and then they enter the column assembly from the bottom with the help
of gas distributor. The column is filled with Rasching rings of 12 mm size. Aq. NaOH solution is sprayed
with the help of a SS tank, pump, bypass line and pre calibrated Rotameter in counter current manner to
the gas flow. Liquid level adjuster is also provided to ensure liquid seal at the bottom. One manometer is
provided to measure the pressure drop across the columns. The vent of the top column shall always be
kept open. Sample collection bottle is also provided along with it.
PROCEDURE:
Initially start the air compressor and collect sufficient air in the pressure tank so as the pressure is about
3-4 kg/cm2. Prepare the dilute NaOH solution in the tank. Open the valve of the pressure tank and allow
the air to pass through the column. Set the air flow at the desired value and then open the valve on the
CO2 cylinder and adjust the flow rate to predetermined value. Now start the pump for the NaOH solution
and using the bypass valve and feed valve set the desired value of flow rate. After sometime take the
sample at various points (liquid as well as gas) and analyze them.
Initially start the liquid flow at sufficiently high rate (V L = 0.03 m/s) to ensure that all the packing are
wetted. The flow rates of gas and liquid are adjusted at predetermined values. The CO 2 flow rate should
be such that the %CO2 in the mixed gas is about 8-10%. The gas velocity has no effect on the interfacial
area in a packed column. Hence a value of V G between 0.1-0.2 m/s may be chosen for all the
experiments and keeping it constant. The linear superficial liquid velocity V is the most important
variable. The range for V should be fixed between 0.001-0.007 m/s.
The system is allowed to reach steady state after fixing the liquid level in the bottom section at a marked
height. Inlet and outlet samples are withdrawn for analysis. This procedure is to be repeated for 6-7
different values of VL chosen in such a way that the range indicated is fully covered.
OBSERVATIONS:
CHEMICAL REACTION:
Final Reaction:
2NaOH + CO2 Na2CO3 + H2O
SAMPLE CALCULATIONS:
The concentration of NaOH used should be between 2-2.5 g mol/lit. The inlet CO 2 percentage is kept
around 10%. Under these conditions the equations (1) and (2) are satisfied and the absorption of CO 2 is
accompanied by a fast pseudo first order.
5 ml of sample (or10 ml) is titrated against standard HCl of molarity (approx.1 g mol/liter) using
phenolphthalein as an indicator.
After steady state, titrate the product with 0.1 N HCl solution use phenolphthalein as an indicator.
Burette reading = 16 ml
= (0.04/0.0538)×100
= 74.5%
RESULT:
CONCLUSION:
By increasing the gas velocity, the rate of absorption and overall efficiency of tower decreases. And vise
versa decreasing gas velocity or increasing liquid flow rate, absorption tower capacity increases. Gas
velocity and liquid flow rate should be in proper range otherwise flooding, channeling can occur.
PRECAUTIONS:
==== X ====
Experiment No : 10
BATCH RECTIFICATION IN
A PACKED DISTILLATION COLUMN
OBJECTIVE:
To study the operation of a packed bed batch rectification column under constant or total reflux
condition.
AIM:
To operate the column under total reflux condition and estimate the minimum number of
theoretical stages required using both Fenske’s equation & McCabe -Thiele’s graphical method.
To estimate the theoretical number of stages at the operating conditions using McCabe Thiele’s
graphical method.
INTRODUCTION:
Batch distillation is often preferable to continuous distillation in cases where relatively small quantities
of material are to be handled at irregularly scheduled periods. The simplest case of batch distillation is
one in which the material to be separated is charged to a heated kettle, fitted with a total condenser and
product receiver. The material is distilled without reflux until a definite change in composition of still
contents has been effected.
In all types of batch distillation, a quantity of feed is charged to a still pot, or kettle, and heat is applied to
it. The vapor, which is usually passed through a fractioning column, is then condensed, giving the
overhead product while a less volatile residue remains in the kettle at the end of distillation. Continuous
distillation is a steady state process because once equilibrium has been attained, conditions at any given
point remains constant, whereas batch distillation is an unsteady state process, the concentration of the
more volatile component decreasing continually so that the temperature and composition of the mixture
at a point in the system alter as the distillation proceeds.
THEORY:
Batch distillation with only a single still does not give a good separation unless the relative volatility is
very high. To obtain product with a narrow composition range, a rectifying batch still is used that consist
of a re-boiler, a rectifying column, a condenser, some means of splitting of a portion of condensed vapor
or distillate as reflux and the receiver. The operation of a batch still and column can be analyzed using
the same operating line equation as for the rectifying section of the continuous distillation:
R x
y n 1 xn D (1)
R 1 R 1
y2 = 1-y1 ; x2 = 1- x1
Since the slope of the operating line is R / (R+1), the slope increases as the reflux increases, until when
reflux is infinite. Under total reflux slope is 1. The operating line then coincides with the diagonal. The
numbers of plates are minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of x B and xD
based on the relative volatility of the components, which is defined in terms of equilibrium
concentrations:
Y1e / X 1e
(2)
Y2 e / X 2 e
log x D 1 x B / x B 1 x D
N min 1 (3)
log
An ideal mixture follows Raoult’s law, and the relative volatility is the ratio of vapor pressure. Thus,
p1 = P*1 x1
p2 = P*2 x2
p1
y1 (4)
P
p2
y2 (5)
P
y1 / x1 P '1
(6)
y 2 / x 2 P' 2
y1 = p1/P (4)
y2 = p2/P (5)
The final ratio does not change much over the range of temperature encountered in a typical column, so
the relative volatility is taken as constant.
DESCRIPTION OF EXPERIMENT:
The packed column is packed with glass Rasching rings. An electrically heated re-boiler is installed at
the bottom of the column. The bottom product is collected in the tank. The vapors from the top of the
column are condensed in the shell and tube type condenser by circulating cooling water.
A tank with pump and Rotameter is provided for condenser cooling water. The condensate is collected in
reflux drum and feedback to column as reflux and part of it is collected as distillate in product receiving
tank. The complete column is insulated for minimizing the heat loss. Instrumentation is done for pressure
& temperature measurement wherever is necessary.
Condenser
Automatic
Reflux Rotameter
Devider
Reflux
Distillate
By-pass-valve
X
T3 = Vapor temp.
T4 = Condensate temp.
UTILITIES REQUIRED:
REQUIRED CHEMICALS:
EXPERIMENTAL PROCEDURE:
1. Fill the re-boiler with a composition of Methanol-water solution (say 50-50%). The total amount
of solution should not be less than 15 liters. The composition of solution should be in the range
of 20 to 70% of methanol by volume.
2. Set a process temperature for the process using the digital temperature controller (DTC). The
temperature range should be in the range 85 to 100°C.
4. Adjust the cooling water flow rate to a moderate value (say 60 LPH). Never fully close the
bypass valve.
6. Wait for 25-30 min. for the system to achieve steady state.
7. Now take out the samples from the bottom & distillate stream (by closing the timer
for short while).
8. Cool down the samples to room temperature & measure the refractive indices.
10.Now adjust the cyclic timer to a desired reflux ratio & wait for 10-15 min.
11.Now take out the samples from both distillate & bottom product.
13.The experiment can be repeated with different set points temperatures & reflux ratios.
x 1 x B
In D
x B 1 x D
N min
In
Also calculate the minimum number of trays using the McCabe- Thiele’s method.
Intercept = xD/R+1
Plot the equilibrium curve, and the operating line. Draw the stages as described in McCabe- Thiele’s
method.
TROUBLE SHOOTING:
In case of any problem regarding operation of the apparatus; the apparatus should be quickly switched
off and electric supply should be cut off.
Electrical:
1. Electric Shock: It means that either earth wire inside the panel is loose or there is no earth
provided in the socket to which the equipment is plugged. So, make it sure that the equipment is
earthed properly.
2. Display of ‘1’ on D.T.C./D.T.I. : it means sensors connections are loose. Locate the
point of loose connection and solder it properly.
==== X ====
Experiment No: 11
BATCH RECTIFICATION IN
A SIEVE PLATE COLUMN
OBJECTIVE:
To analyze the performance of a Laboratory Scale Seive Plate Column. To obtain a desired separation of
an alcohol waste feed product.
AIM:
To operate the column under total reflux condition and estimate the minimum number of
theoretical stages required using both Fenske’s equation & McCabe-Thiele’s graphical method.
To obtain T-x data under total reflux at steady state and compare it with theoretical value.
To estimate the theoretical number of stages at the operating conditions using McCabe-Thiele’s
graphical method.
INTRODUCTION:
Distillation is the method of separating the components of a solution, which depends upon the
distribution of the substances between a gas and liquid phase, applied to cases where all components are
present in both phases. Instead of introducing a new substance into the mixture in order to provide the
second phase, as is done in gas absorption or desorption, the new phase is created from the original
solution by vaporization or condensation.
The direct separation which is ordinarily possible by distillation, into pure products requiring no further
processing has made this perhaps the most important of all the mass transfer operations.
THEORY:
Batch distillation with only a single still does not give a good separation unless the relative volatility is
very high. To obtain product with a narrow composition range, a rectifying batch still is used that consist
of a re-boiler, a rectifying column, a condenser, some means of splitting of a portion of condensed vapor
or distillate as reflux and the receiver. The operation of a batch still and column can be analyzed using
the same operating line equation as for the rectifying section of the continuous distillation:
R x
y n 1 xn D (1)
R 1 R 1
y2 = 1-y1 x2 = 1- x1
Since the slope of the operating line is R / (R+1), the slope increases as the reflux increases, until when
reflux is infinite. Under total reflux slope is 1. The operating line then coincides with the diagonal. The
numbers of plates are minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of x B and xD
based on the relative volatility of the components, which is defined in terms of equilibrium
concentrations:
y1e / x1e
(2)
y 2e / x 2e
log x D 1 x B / x B 1 x D
N min 1 (3)
log
An ideal mixture follows Raoult’s law, and the relative volatility is the ratio of vapor pressure. Thus,
p1 = P’1 x1
p2 = P’2 x2
p1
y1 (4)
P
p2
y2 (5)
P
y1 / x1 P '1
(6)
y 2 / x 2 P' 2
The final ratio does not change much over the range of temperature encountered in a typical column, so
the relative volatility is taken as constant.
DESCRIPTION OF EXPERIMENT:
The column is made of Stainless Steel material with seven plates. An electrically heated re-boiler is
installed at the bottom of the column. The bottom product is collected in the tank. The vapors from the
top of the column are condensed in the shell and tube type condenser by circulating cooling water. A
tank with pump and Rota-meter is provided for condenser cooling water. The condensate is collected in
reflux drum and feedback to column as reflux and part of it is collected as distillate in
product receiving tank. The complete column is insulated for minimizing the heat loss. Instrumentation
is done for pressure & temperature measurement wherever is necessary.
Condenser
Automatic
Reflux Rotameter
Devider
Reflux
Distillate
By-pass-valve
X
UTILITIES REQUIRED:
REQUIRED CHEMICALS:
EXPERIMENTAL PROCEDURE:
2. Fill the re-boiler with a composition of Methanol-water solution (say 50-50%). The total amount
of solution should not be less than 15 liters. The composition of solution should be in the range
of 20 to 70% of methanol by volume.
3. Set a process temperature for the process using the digital temperature controller (DTC). The
temperature range should be in the range 85 to 100°C.
5. Adjust the cooling water flow rate to a moderate value (say 60 LPH). Never fully close the
bypass valve.
7. Wait for 25-30 min. for the system to achieve steady state.
8. Now take out the samples from the bottom & distillate stream (by closing the timer for short
while).
9. Cool down the samples to room temperature & measure the refractive indices.
10. Now adjust the cyclic timer to a desired reflux ratio & wait for 10-15 min.
11. Now take out the samples from both distillate & bottom product.
12. Cool down the samples & measure their refractive indices.
13. The experiment can be repeated with different set points temperatures & reflux ratios.
SPECIFICATIONS:
Distillation Column : Material Stainless Steel, Dia 110 mm, Seven trays.
Re-boiler : Made of Stainless Steel, (25 Liters) provided with Pressure Gauge, Level
indicator & Safety valve.
Water supply tank : Made of Stainless Steel, capacity 100 Liters for condenser.
The whole set-up is well designed and arranged in a good quality painted structure.
FORMULAE:
y1 = αx1/(1+(α–1)x1) ; V = D(R+1)
log x D 1 x B / x B 1 x D
N min 1
log
T °C X y
100 0 0
96.4 0.02 0.134
93.5 0.04 0.23
91.2 0.06 0.304
89.3 0.08 0.365
87.7 0.1 0.418
84.4 0.15 0.517
81.7 0.2 0.579
78.0 0.3 0.665
75.3 0.4 0.729
73.1 0.5 0.779
71.2 0.6 0.825
69.3 0.7 0.87
67.5 0.8 0.915
66.0 0.9 0.958
65.0 0.95 0.979
64.5 1 1
DATA:
Number of plates = 7
Tray No. 1 2 3 4 5 6 7
R.I.
Temp.(°C)
Values of compositions are found for the respective trays using the calibration curve. These values are
plotted against the respective temp.
xF = 0.5
xD = 0.72
xB = 0.40
Feed Temperature = 21 °C
x 1 x B
In D
x B 1 x D
N min
In
Also calculate the minimum number of trays using the McCabe- Thiele’s graphical method.
Intercept = xD /R+1
Plot the equilibrium curve, the operating line. Draw the stages as described in McCabe-Thiele’s method.
= (NT/7)×100
NOMENCLATURE:
SUBSCRIPTS:
1 = First component of binary mixture
2 = Second component of binary mixture
B = Bottom product (residue)
D = Distillate
e = Equilibrium
f = Final state
i = Initial state
n = Number of plates
CONCLUSIONS:
==== X ====
Experiment No: 12
TO DETERMINE DIFFUSIVITY
COEFFICIENT BY PITOT TUBE
PITOT TUBE
AIM:
OBJECTIVES
THEORY:
A pitot tube is used to find the velocity of an open stream at any point. The tube bent at its end and
drawn out into a nozzle may be used to find the velocity at point nozzle axis is aligned toward the
direction of flow. The water of stream will rise in the tube at a height equal to stagnation pressure head
which will project out of the free surface by the amount of velocity head. Thus the velocity at tip of
nozzle can be calculated.
V = CP 2( p 2 p 1 ) /
= Cp 2p /
P = (P2-P1) = ( m- )*g
m 13.6 kg/cm3
ρ = 1 kg/cm3
APPARATUS:
PROCEDURE
OBSERVATIONS:
Data:
Area of measuring tank a =50*40 =2000cm3
Plot pressure average velocity vs. pressure drop in a log-log graph paper and determine the value of pitot
co-efficient.
RESULTS:
CONCLUSIONS:
Experiment No: 13
STEAM DISTILLATION
STEAM DISTILLATION
AIM:
(a) To carry out steam distillation of Acetic Acid from water system.
INTRODUCTION:
Steam distillation is a unit operation of considerable practical importance. Steam distillation is a term
applied to a distillation process with open steam, i.e., wherein the steam is in direct contact with the
distilling system in either a batch or a continuous operation. Steam distillation has special value where it
is desired to separate substances at a temperature lower than their normal boiling point because of heat
sensitivity or other reasons.
In steam distillation, feeding open steam to a distillation still distills the liquid. The steam carries with it
vapors of volatile liquid and is condensed to separate the liquid from water. Steam distillation is
generally carried out in a cylindrical still with injection of the steam through coils placed in the bottom
of the still with numerous perforations to obtain uniform distribution. The relation between the number
and size of these distributors and pressure drop and rate of flow through them may be determined by
considering the perforations as orifices.
For a binary system, the steam requirement can be calculated from the following equation:
WB/WA = (101.3-ηV.PA) / (ηV.PA)×(MB/MA)
EXPERIMENTAL SETUP:
The experimental setup consists of 1000 ml three neck round bottom flask with suitable heating mantle
(with regulator to control the temperature, ON/OFF switch and indicator lamp).
Steam necessary for the distillation is generated using a 3000 ml steam generator(inner body SS 304,
outer body Mild steel, and 500 W heater) and is fed to the round bottom flask using a dip pipe. The
vapors generated in the flask are transferred to the condenser using a bend. The condensed vapors are
collected with the help of beaker. The temperature of the flask is measured by using a thermometer. The
entire assembly is supported with the help of a stand.
PROCEDURE:
The distillation still is charged with the predetermined volume of A (about 2000 ml).
The steam generator is filled upto75% of its height and the heater is turned on.
Wait till the pressure into the steam generator build up-to nearly 1.5 kg/cm2.
Now open only the jacket valve and allow the steam to enter into the jacket to heat the distillation
kettle mixture.
When the temperature in the still reaches 2°C below the boiling point determined in first step,
stop the supply of steam in the jacket and the flow of live steam is started through the dip pipe
into the distillation kettle.
The distillation is continued for a sufficient length of time so that about 60-70% of A charged is
distilled.
The distillate collected in the accumulator separates into the organic layer and an aqueous layer.
The two phases are then separately weighted. Similarly the components in the bottoms are
weighted after cooling to room temperature.
Vaporization Efficiency,
ηV = PA°/P
W B 101.3 V p A M B
* ….. {Ref: B.K Dutta, Principle of Mass
WA V PA MA
transfer
and separation process, pp 351}
OBSERVATION TABLE:
DISTILLATE:
RESIDUE:
NO. Of Of Of Of Of (molesofwater)/ 1/
Acetic Acid A.A. A.A. Water Water (molesof A.A. (y-x)
+Water)
DISTILLATE:
Normality of distillate,
N 1 * V1
N2
V2
=
Moles of A.A. in distillate,
= Mass of A.A.
m.wt.of A.A.
= Mass of water
m.wt. of water
y* =. moles of water
moles of(water+A.A.)
RESIDUE:
Normality of residue,
N 1 * V1
N2
V2
=
= …………. gm
= Mass of A. A.
mol.wt.of A.A.
= …………. gm
= mass of water
mol.wt.of water
= …………. moles
XW =. moles of water
moles of( water+A.A.)
GRAPH:
The area under the curve obtained beginning at xF, when the area equals the
calculated ln F/W, integration is stopped at that point which gives the practical value of xW.
From yD,avg.find the xW using equation: F.xF=D.yD,avg.+W.xW
Which will give theoretical value of xW.
RESULTS:
CONCLUSIONS:
==== X ====
Experiment No: 14
ROTARY DRYER
ROTARY DRYER
OBJECTIVE:
To study the rate of drying for rotary dryer for different air flow rates and different air inlet temperatures.
INTRODUCTION:
In many cases, the drying of materials is the final operation in the manufacturing process, carried out
immediately prior to packaging or dispatch. Drying refers to final removal of water, and the operation
then follows evaporation, filtration or crystallization. Drying is carried out for more or more of the
following reasons:
To reduce the transportation cost
To make a material more suitable for handling, for example soap powders, dyestuffs, fertilizers.
To provide definite properties, such as maintaining free flowing nature of salts.
To remove moisture; which may otherwise lead to corrosion, for example, the drying of coal gas
or benzene prior to chlorination.
Almost all drying processes involve the removal of water by vaporization, & thus require the addition of
heat.
THEORY:
Consider a rotary continuous counter-current dryer fed with a nonporous material having all moisture as
unbound moisture. As this material enters the dryer, it is first heated to the drying temperature. It will
then pass through the length of dryer at nearly the wet bulb temperature and theoretically at the end of
the dryer, the material shall be discharged as dry material nearly at the wet bulb temperature.
Assumptions:
No heat losses from the dryer
Heat is applied to the material only from the air, not by conduction from the dryer shell.
All the moisture present is free moisture.
There is no evaporation of moisture in the preliminary heating period.
Drying proceeds at a constant wet bulb temperature until desired amount of water has been removed.
The entering air is assumed at be 100% saturated, so its temperature needs to be raised so as to decrease
the relative saturation. This would enable the air to absorb moisture from the wet solid feed. In turn the
exit air is more saturated than the entering air.
DESCRIPTION:
A rotary dryer consists of a cylindrical shell, set with its axis at a right angle to the horizontal and
mounted on rollers so that it can be rotated. The material to be dried is fed to the high end of the dryer
and by rotation of the dryer, usually assisted by internal shelves of flight, is gradually advanced to the
lower end where it is discharged. The source of heat for a rotary dryer is usually the hot air that
circulates through the dryer. Air flow rate can be measured by the Orificemeter and manometer provided.
Inlet/ Outlet air temperatures (D.B, W.B)are measured by a hygrometer.
UTILITIES REQUIRED:
Electricity Supply: 1 Phase, 220V AC, 4kW
Wet Solid
Floor Space of 1.5m ×2m
EXPERIMENTAL PROCEDURE:
1. Set the preheating temperature of air.
2. Run the blower and note down the wet bulb and dry bulb temperatures of the entering air at the
prevailing temperature.
3. Switch ON the heaters & wait till the set point temperature is arrived.
4. Fill the feed hopper with wet solid.
5. Start the dryer in rotary motion.
6. Allow the wet solid to flow through the dryer by starting the screw conveyor.
7. At steady state record the following:
Air Flow rate( Orifice meter, manometer reading and convert it to volumetric flow rate
and mass flow rate) =GG
Wet bulb air temperature at outlet = tw2
Dry bulb temperature at outlet = tD2
SPECIFICATION:
Drying Shell: Material: SS, Length 1.5m, Dia: 110mm
Feed Hopper: Material: SS, Compatible Capacity
Product Receiver: Material: SS, Compatible Capacity
Rotating Action: Using FHP Crompton/GE make motor coupled with a Reduction Gear Box
Hot Air Circulation: FD Blower fitted with Crompton/GE make motor
Heating Chamber: Fitted with Nichrome wire heater
Air Flow Measurement: Orifice meter and manometer
Control Panel comprises of:
Digital Temperature Controller: 0-200°C, RTD PT-100 ype
(For Hot Air)
OBSERVATIONS:
= h10010001 1 9.99h(meter)
Diameter of Orifice = 26mm
Diameter of the pipe through which air flows= 52mm
Area of pipe, a1 = 5.31×10-4 m2
Area of Orifice, a2 = 2.12× 10-3 m2
a1 a 2
Flow rate of air, Q0 C 2 gH
a22 a12 d
= 5.484×10-4×0.61×4.43×√ΔH
= 1.482×10-3×√ΔH m3/sec
Mass flow rate of air = ρQ0
= 1×1.482×10-3×√ΔH kg/sec
= 4.684×10-3×√h kg/sec
CONCLUSIONS:
==== X ====
Experiment No : 15
OBJECTIVE:
Drying of solids in a tray dryer under forced draft tray condition.
AIM:
To determine the drying rate of a solid under forced draft condition and determine the critical moisture
content.
INTRODUCTION:
In many cases, drying of materials is the final operation in the manufacturing process, carried out
immediately prior to packaging or dispatch. Drying refers to the final removal of water, and the
operation often follows evaporation, filtration or crystallization. Drying is carried out for one or more of
the following reason:
To reduce the cost of transport.
To make a material more suitable for handling.
To provide definite properties.
To remove moisture this may otherwise lead to corrosion.
THEORY:
Drying of solids is considered to occur in two stages, a constant rate period followed by a falling rate
period. In the constant rate period, the rate of drying corresponds to the removal of water from the
surface of the solid. The falling rate period corresponds to the removal of water from the interior of the
solid. The rate in either case is dependent on:
The rate of drying can be determined for a sample of substance by suspending it over an electronic
balance in the duct, in a stream of air, from a balance. The weight of the drying sample can then be
measured as a function of time. Certain precautions must be observed if the data are to be of maximum
utility. The sample should not be too small. Further, the following conditions should resemble as closely
as possible those expected to prevail in the contemplated large-scale operation:
If possible, several tests should be made on samples of different thicknesses. The dry weight of the
sample should also be obtained. The drying rate is calculated from:
dx 1
N S
d A
kg / m 2 s .
DESCRIPTION:
AIR IN AIR
OUT
TRAY
The air flow is controlled by a valve in the blower outlet and its flow rate is measured by a pre-calibrated
orifice meter. Thermometers are placed at the inlet and outlet of the drying chamber.
UTILITIES REQUIRED:
EXPERIMENTAL PROCEDURE:
1. Load the pre-weighed tray with solid and record the weight of sand & tray.
2. Start the blower and heater. Fix the air flow rate and let the system to achieve steady state as the
air flow rate would make the temperature steady.
3. When the desired conditions of temperature and air velocity are reached( in about 10-15min),
remove the sample tray and put known amount of water in it to give desired initial moisture
content.
4. Place the tray gently in the drying chamber and start the stopwatch.
5. Record the balance reading with time at about 3-5min time interval.
6. Drying is assumed to be complete when at least 3 consecutive readings are unchanged.
7. The temperatures at the inlet and outlet of the drying chamber and the air flow rate( manometer
reading fixed across the orifice) are recorded at least three times during the course of run to give
average operating conditions.
8. The same steps are repeated for other runs at different operating conditions.
Initial Moisture Content = 20-50% (Prepare the sample in this range of moisture content)
SPECIFICATION:
FORMULAE:
Moisture content present in solid, X(kg water/kg dry solid)
X = (W-S)/S
The drying rate is thus calculated from:
dx 1 kg
N S 2
d A m s
S X
N
A
Plot X Vs θ and draw a straight line through all points. Fit a second degree polynomial to the X Vs θ
data and obtain the slope dX/dθ corresponding to various values of θ
Plot drying rate N (kg/m2-s)Vs moisture content X (kg of water/kg of dry solid). From this plot
critical moisture content (Xc) can be obtained.
The experiment can be repeated at constant air flow rate and constant air temperature.
CONCLUSIONS:
NOMENCLATURE:
==== X ====
Experiment No : 16
HUMIDIFICATION-DEHUMIDIFICATION
COLUMN
(Evaluation of Mass Transfer Co-efficient)
HUMIDIFICATION-DEHUMIDIFICATION COLUMN
(Evaluation of Mass Transfer Co-efficient)
AIM:
To calculate the mass transfer coefficient in the Humidification and Dehumidification column.
THEORY:
In the processing of materials it is often necessary either to increase the amount of vapor present in a gas
stream, an operation known as humidification; or to reduce the vapor present, a process referred to as
dehumidification. In humidification, the vapor content may be increased by passing the gas over a liquid
which then evaporates into the gas stream. This transfer into the main stream take place by diffusion, and
the interface simultaneous heat and mass transfer take place according to the system. The reverse
operation is called dehumidification. The most widespread application of humidification and
dehumidification involves the air-water system. Drying of wet solids is an example of humidification.
The mass transfer coefficient, Ka, can be measured in a humidification and dehumidification column in
which area of contact between two phases is known and boundary layer separation does not take place. A
humidification and dehumidification column also provides useful information on mass transfer to and
from fluids in turbulent flow.
For turbulent flow mass transfer to pipe involving evaporation of liquids in wetted wall
towers, Gilland and Sherwood proposed the correlation:
0.81 0.44
N Sh 0.023 N Re N Sc (1)
for N Re 2000 3500
N Sc 0.6 2.5
P 0.1 3atm
The known flow rate of air at a measured humidity is brought into contact with a film of water at a
certain temperature and vapor pressure. Moisture is absorbed be the air from water film and the resultant
humidity of the exit air and the temperature and vapor pressure of the entry water measured. The rate of
diffusion through the gas film, NA, is given by:
Ka = gas film coefficient, kgmole of water transferred.m2/h per atmospheric partial pressure difference.
A = Wetted surface of column = πdL
(ΔP)m = Log mean partial pressure driving force across the ends of the column.
The value of Ka obtained experimentally can be compared with that predicted from Sherwood –
Gilleland correlation:
0.8 0.44
D.d d .V .
K a (3)
R.T .d
d= Column diameter.
DESCRIPTION:
The setup consists of two glass columns with packings of raschig ring and silica gel. Air flow rates can
be set and measured by Rotameter and temperature by RTD. The setup studies are in volumetric mass
transfer coefficient.
FEAUTRES:
In this system the air is firstly free from moisture by passing in the heated chamber and then inserted in
the column from the bottom and water is from the top and comes down with the packing wall. The
moisture is absorbed from the glass column and goes up in the cooling chamber for dehumidification and
then passed into the silica gel filled glass column for complete dehumidification and then passed into the
atmosphere. Water is recycled in the sump tank through the pump. The temperature of the air dry bulb
and wet bulb are measured by RTD 100 provided.
UTILITIES REQUIRED:
Water Supply
Drain
Electricity Supply : 1 Phase, 220V AC, 0.5kW
EXPERIMENTAL PROCEDURE:
1. Fill the sump tank with water and also connect the air supply to the point provided.
2. Connect the plug to mains and start heating the chamber and also start the air and maintain air
flow rate.
3. Fill the wet bulb thermometer bottle with water and wait for 30 minutes and control the air
temperature by regulating the voltage variac provided.
4. Commence the operation with minimum airflow and after 15-20 minutes, the humidity of inlet
air and the outlet air at this flow rate of air is noted and read corresponding vapor partial
pressure, from the psychometric chart. Simultaneously the temperature of the water in and out is
noted and flow rates are measured. From Steam tables obtain vapor pressure of water
corresponding to these temperatures.
5. Repeat step 3 for 3-4 air flow rates.
6. Calculate experimental value of Ka using equation (2)
7. Calculate the predicted value of Ka using equation (3)
8. Compare the experimental and predicted value of Ka
N Sh
9. Plot 0.44 VsN Re on log-log scale and check the slope approximates to 0.8.
N Sc
SPECIFICATION:
FORMULAE:
18 p H 2O
Humidity =
29 pT p H 2O
From steam tables, corresponding to water inlet and outlet temperature calculate the vapor pressure.
Calculate (ΔP)m as:
p B1 p B
ln p B1
(ΔP)m =
pB
where pB1 = (pT – pa1)
and pB = (pT – pa)
Column diameter = d
Effective Column Height = L
Room Temperature
Atmospheric Pressure (Total Pressure) = pT
Surface Area = πdL
OBSERVATION TABLE:
18 p H 2O
Humidity =
29 pT p H 2O
From steam tables, corresponding to water inlet and outlet temperature calculate the vapor pressure.
Calculate (ΔP)m as:
p B1 p B
Pm
ln p B1
pB
and pB = (pT-pa)
N sh
Plot 0.44
vsN Re
N Sc
CONCLUSIONS:
TROUBLESHOOTING:
1. If any type of suspended particle come in the Rotameter, remove the rotameter, clean it and then
fit it.
2. If there is any leakage, tight that part or remove that and refix that again after wrapping Teflon
tape.
3. If Rotameters fluctuating more than average tight control knob of that.
( Procedure: Two nuts are there loose first nut and tight the second slightly, and then first also.
Both nuts are on Rotameters)
4. If D.T.I display ‘I’ on display board it means sensors connection are not O.K tight that.
5. If switch ON the heater but temperature can’t rise but panel LED is ON it means bath heater had
burned replace that.
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Experiment No : 17
LIQUID-LIQUID EXTRACTION IN
A SPRAY COLUMN
OBJECTIVE:
AIM:
To study the effect of dispersed phase flow rate on:-
1) Over all volumetric mass transfer coefficient, KLa
2) Dispersed phase hold up.
INTRODUCTION:
Liquid Extraction sometimes called solvent extraction is the separation of the constituents of a liquid
solution by contact with another insoluble liquid. If the substances constituting the original solution
disturb themselves differently between the two liquid phases, a certain degree of separation will result &
this can be enhanced by use of multiple contacts. Spray column involves the dispersion of one of the
liquids involved in liquid- liquid extraction. Usually the liquid with largest volume rate is dispersed
giving largest interfacial surface for a given drop size. Also, the dispersed phase should not wet the
material of the nozzle.
THEORY:
A Spray column may be operated as continuous counter current extraction equipment wherein one of the
liquids forms the dispersed phase, or in semibatch operation, where the continuous phase has zero
velocity. However, in such columns, the back-mixing in continuous phase decreases the driving force for
mass transfer. As a result, the spray columns have low extraction efficiency. The height of a transfer unit
is more as compared to other extraction equipments. Usually the spray columns are used for systems
where number of transfer units is less than five.
At flow rates below those causing flooding, the ratio of slip velocity (Vs) to the terminal velocity of a
single particle in a quiescent fluid, is a unique function of dispersed phase hold-up for all vertically
moving fluid particle systems. Slip velocity is the net linear velocity between the dispersed phase liquid
and the continuous phase liquid.
where Vc and Vd are the superficial velocities of the continuous and dispersed phase liquids respectively.
m3
Vd = FD s (2)
D 2 2
4 c m
Dc = Column I.D (m)
FD = Volumetric flow rate of dispersed phase, m3/s
At the flooding condition, the hold-up is best established by a characteristic velocity of the droplet V k,
given by
V Vc
Vs d = Vk (1- Φd) (4)
d 1 d
Thus a plot of Vd Vs Φd(1- Φd) should yield a straight line through (0,0) with slope Vk
Consider a quiescent continuous liquid phase (Toluene) with Benzoic acid dissolved in it, having an
initial conc. of CTi, kmol/m3; using pure water as dispersed phase.
Let Ci be the initial conc. of Benzoic acid in inlet water (kmol/m3)
C0 be the conc. of Benzoic acid in outlet water (kmol/m3)
C* be the equilibrium conc. of Benzoic acid.
Defining log mean conc. difference (driving force) as
C * Ci C * C0
C ln (6)
ln C * C i C * C 0
Ci = 0 for pure water.
Dispersed
Phase Ci
Continuous Phase
Interface
C 0 Fd
RAa
Ve
(7)
N
or Rate of mass transfer C a C i Fd , gmol / h
DESCRIPTION:
The present set up is shown for semi-batch operation, though same set up can be used for continuous
operation as well as by allowing the continuous phase liquid to flow at a low flow rate.
The dispersed phase liquid (water) is metered through a pre-calibrated Rotameter. In case of continuous
operation, the continuous phase liquid (Toluene) can also be metered through another pre-calibrated
Rotameter provided with the setup. The liquid-liquid interface is maintained at a suitable height from the
bottom by adjusting the extract flow rate at the bottom. This is done by adjusting the height of the
flexible pipe provided at the bottom outlet of the dispersed phase liquid.
UTILITIES REQUIRED:
EXPERIMENTAL PROCEDURE:
1. Prepare a solution of Toluene+Benzoic Acid by dissolving Benzoic Acid in Toluene such that the
conc. of Benzoic Acid in Toluene is = 0.2gmole/L or 0.2kgmole/m3
2. Fill the spray extraction column with Toluene containing Benzoic Acid to such a height that the
dispersed phase nozzle just dips in the pool of Toluene.
3. Adjust the Rotameter reading for water (dispersed phase) to a prefixed value (4LPH to 15LPH)
4. Adjust the outflow from the column such that the liquid-liquid interface is maintained at a
suitable height from the bottom. Maintain the interface at the same height for all observations.
Record the volumetric flow rate of water (Fd)
5. Collect 40ml of water sample at the outlet stream of the column after 10 to 15 minutes of
operation (S.S condition). Since the continuous phase is already saturated w.r.t the dispersed
phase, the direction of mass transfer, therefore is only from continuous phase to the dispersed
phase. Titrate the sample with N/10 or N/20 NaOH using Phenolphthalein as indicator and
determine the conc. of Benzoic Acid in water at the outlet (C0)
6. Close the inlet and outlet to the column simultaneously and allow the dispersed phase
droplets to coalesce and settle.
7. Collect the hold up until the interface drops to the initial height from the bottom. Measure the
volume of the hold up.
8. Repeat the above steps for at least four different values if dispersed flow rates.
SPECIFICATION:
FORMUILAE:
FD
Dispersed phase superficial velocity = Vd = ( m / h)
Ac
Vw 10 3 L
Fractional Hold up = Φd =
Ve L
Conc. of Benzoic Acid in water at the outlet :
40×N1 = V2 × 1/10
V2
N1 gmeq / L gmole / L
400
= kmole/m3
= Ci
C*w/CT = 0.167267-0.837941CT+2.27418CT2
Cw/CT = 0.090646 = m
Cw1 = 0
C * Ci C * C0
C ln
ln C * C i C * C 0
Vd
Vk m/h
d 1 d
Temperature =
Run Water Flow rate (Fd), LPH Hold up collected Vw, Vol. of N/10 NaOH used for
No. ml titration (V2), ml
CALCULATIONS:
V2
N1 gmeq / L gmole / L
400
= Ci kmole/m3
C*w/CT = 0.167267-0.837941CT+2.27418CT2
Cw/CT = 0.090646m
Considering CT1 = CT2 = CT = 0.2 gmol/L
Cw1 = 0
C ln
C1 C 2
ln C1
C 2
N
M.T Coefficient = KLa =
Ve C ln
Vd
Vk m/h
d 1 d
OBSERVATION TABLE:
Plot Vd Vs Φd(1- Φd), draw a straight line through (0,0) and obtain the slope Vk.
Plot KLa Vs Vd on a log-log scale
Discuss your results.
CONCLUSIONS:
NOMENCLATURE:
TROUBLESHOOTING:
1. If any type of suspended particles come in the Rotameter, remove the rotameter clean the tube
and fit it at its place.
2. If there is any leakage, tight that part or remove that and refix again after wrapping Teflon tape.
3. If Rotameter fluctuates more than the average tight control knob of that.
(Procedure: Two nuts are there lose first nut and tight the second slightly, and then first also. Both
nuts are on rotameter.)
==== X ====
Experiment No : 18
OBJECTIVE:
Study of Solid Liquid Extraction in a Column with Solid in Batch & Liquid in Continuous Recirculation.
AIM:
To study the effect of various system parameters like: solvent temperature, solvent rate and particle size
on the % recovery of oil from oil seeds.
INTRODUCTION:
Leaching is a method of extracting a desired chemical that is dispersed or dissolved in a solid. The solid
is ground up into small pieces and “washed” with a solvent in which the desired chemical is soluble.
Sometimes the solid and solvent from slurry that can be conveyed. In any event the desired chemical is
transferred from the solid to the liquid phase. The resultant liquid, which is rich in the desired chemical,
is filtered to remove fine suspended grains of the solid. The liquid can then be distilled or otherwise
purified.
THEORY:
Leaching is a common industrial process, but it also occurs in natural systems, such as in the motion of
water through soil. In this case, the solid phase is soil particles, and the leaching solvent is water,
presumably rain water that percolates through the soil. Some chemicals attached to the soil particles are
water-soluble. These chemicals are transferred to the water as it flows through the soil. Such a process
sometimes called in-situ leaching, because it occurs with the solid phase fixed in place.
The laboratory experiment uses simple equipment to explore a leaching operation that is familiar to all of
us—the extraction of oil from oil seeds using hexane as the leaching solvent.
DISCUSSION:
Oil seeds contain edible oil in it. When oil seeds are mixed with hexane oil, oil is transferred from the
solid oil seeds. The rate of mass transfer and, therefore, the concentration of the oil in the hexane phase,
are strongly affected by several variables. We will examine quantitatively a few of the variables that
affect the leaching process.
Oil seed is placed inside a glass column in the form of a packed bed. Hot or cold hexane flows up the
packed bed, extracting the oil that is present in the seeds. The concentration of the oil probably depends
upon many variables, like: the amount of oil seed in the bed, the volume of hexane used, temperature of
hexane and the coarseness of the solid oil seeds.
UTILITIES REQUIRED:
Electricity Supply : 1 Phase, 220V AC, 3kW
Hexane : 50 Ltrs
Oil seeds : 30kg
PROCEDURE:
1. Fill the glass column with the known weight of air-dried oil seeds (W 0), gms, the initial amount of
oil present in the dried oil seeds must be known (x0), gm of oil/gm of seed..
2 Fill the solvent feed tank with hexane. Select a suitable operating temperature (25 to 45°C) and heat
the hexane to this temperature.
3. Allow the hot hexane to enter the packed bed slowly and return the solvent to the feed tank i.e the
operating process shall be in a closed cycle.
4. Note the flow rate of hexane and run the experiment for 3 hours. After 3 hours, stop the solvent
supply and remove the wet seeds from the column in an open tray. Dry the material first in open air
then in an oven till constant weight.
6. Weigh the dry seeds. Let the weight of dry seeds=W, gm
7. Oil extracted = Oe =( W0- W), gm
8. Max. oil present in seeds = Omax = W0 x0 , gm
9. % recovery= (Oe/ Omax)100
SPECIFICATIONS:
A good quality painted rigid MS structure is provided to support all the parts.
DATA:
Column diameter:
Packed Height:
Bed Porosity:
Oil seed size:
Solvent:
Solvent rate:
Solvent temperature:
Compare the % recovery for different parameters under which the leaching was carried and discuss your
results.
CONCLUSIONS:
NOMENCLATURE:
1. Always use fresh oil seed or expeller waste that should be some oil.
2. Hexane should be oil free or not used.
3. Don’t switch on the heater before filling the water in the bath.
4. Proper cleaning should be necessary for the set-up.
==== X ====
Experiment No : 19
THEORY:
Granular solids fluidized by a drying medium such as hot air, can be dried and cooled in a fluidized bed.
The principal characteristics of such beds include cross flow of solid and drying gas, a solid residence
time controllable from seconds to hours and suitably for any gas temperature. It is necessary that solids
be free flowing and of a size range 1mm to 2mm. Since the mass flow rate of gas for thermal
requirements is substantially less than that required for fluidization, the bed is most economically
operated at the minimum velocity for fluidization.
During fluidization the particles are circulated within the fluidized bed. This circulation has a direct
bearing on the heat transfer properties of gas solid fluidized bed systems. Fluidized beds have been used
for heat exchange in both physical operations and chemical processes because of rapid transport. Also
because of mixing, uniform temperatures throughout the bed can be maintained.
If a sample of wet material containing Z0 kg of dry material, is dried at a constant flow rate of air, L0 kg
of dry air per hour, whose initial humidity is x’, the time dependence of moisture content of the sample,
can be determined from the changes in humidity of the drying medium, Δx = x”x’, where x” is the final
moisture content of the drying medium.
(2)
c0 = Initial moisture content of the material
c = Moisture content of the material at any time t, (gm of water / gm of dry solid) ×100
The value of the integral can be determined graphically.
From the course of Δx, time dependence of the fraction of water evaporated and χ can be calculated
from:
xdt
0
xdt
0
(3)
c0 c
= fraction of water removed from the material.
c0 c
gm of moisture
c0= Initial moisture content of the material, gm of dry solid 100 = % moisture based on dry wt.
DESCRIPTION:
FIGURE - 1
UTILITIES REQUIRED:
1. Overall Space = 2m L × 2m W × 2m Ht
2. Fluidizing material = Silica sand of size < 2mm. Qty approx 200
3. Electricity = 1 Phase, 230V AC, 3kW
4. Compressed Air Supply = 4CFM max.
EXPERIMENTAL PROCEDURE:
SPECIFICATION:
1. Process Column
Material = Borosilicate Glass
Conical Portion:
Internal Diameter = 77mm
Height = 97mm
Straight Portion:
Internal Diameter = 74mm
Height = 500mm
2. Fluidizing Material = Silica Sand
Size = < 1mm
3. Heating Capacity = 2.0 kW (2 No., 1kW each)
4. Temp. Measurement = with temperature Indicator
5. Control Panel comprises of = Digital temp. controller : 0 – 199.9°C
6. Standard make on/off Switch, Mains Indictor etc.
FORMULAE:
wt. of water
% Moisture present is sample c, = 100
wt. of dry solid
c0 c
Fraction of water removed, χ =
c 0 c
OBSERVATION & CALCULATION:
Initial dry wt. of solid = Z0 gm
Initial moisture content = W0 gm
W0
c0 gm of moisture/ gm of dry solid
Z0
W0
or c0 100(%)
Z0
OBSERVATION TABLE:
∞ c∞ 1
∞ : Large time or till c remains constant.
Plot c vs t
Determine c at t & ∞
Estimate χ
Plot χ vs t and get the drying curve.
TROUBLESHOOTING:
1. If D.T.I display ‘I’ on display board it means sensors connection are not O.K tight that.
2. If switch ON the heater but temperature can’t rise but panel LED is ON it means heater had
burned replace that.
CONCLUSIONS:
==== X ====