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1.
Objective:
To operate the column under total reflux condition and calculate the minimum number of
theoretical stages using fenskes equation. To operate the column under any desired
reflux condition and calculate theoretical number of stages using Mc-Cabe Thieles
method
1
2.
Description:
The set-up consists of packed column, which is packed with glass rasching rings. An
electrically heated reboiler is installed at the bottom of the column. A tank is provided to
collect the bottom product. Shell and tube type condenser is provided to condensate the
vapour. A tank with pump and rotameter is provided for circulation of cooling water.
Reflux drum is provided to collect the condensate. Receiving tank is for collecting the
distillate. Drain valves are provided for drainage purpose.
3.
Theory
4.1
Part 1
Packed column are often used for distillation when the separation is relatively easy and
the required column diameter is not very large. The column height is generally based on
the number of theoretical plates and the height equivalent to theoretical plate (HETP).
For the calculation of height equivalent to theoretical plate (HETP):
Where Z and Nt are packed height and number of theoretical plates respectively. For
simple batch distillation process, initially the still is filled with F moles of feed with xF
as the mole fraction of the more volatile component. Let at any moment the number of
moles of liquid in the still be B having a mole fraction x of the more volatile component
(i.e A) and let the moles of accumulated condensate be D. Concentration of the
equilibrium vapour is y*. Over a small time, the change in the amount of liquid in the
still is dB and the amount of vapour withdrawn is dD. The following differential mass
balance equations may be written:
The above equation is more convenient form of rayleigh equation. 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 reboiler, 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:
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 number of plate is minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of
xB and xD based on the relative volatility of the components , which is defined in terms
of equilibrium concentrations:
Minimum number of theoretical plates required:
The above equation is known as fenskes eqn. 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.
4.2
Part 2
g) Draw vertical line from the point at equilibrium curve (where horizontal line is end) to
the operating line.
h) The above step made triangular construction.
i) Again draw horizontal line from the point at operating line (where vertical line is end)
to the equilibrium curve.
j) Repeat the above three steps between equilibrium curve and operating line, till cover
the point xB on diagonal.
k) Count the number of triangles made.
l) Number of triangles is equal to number of theoretical stages including reboiler.
m) Subtract one from the number of triangle, and then it is theoretical number of stages
required at desired reflux conditions.
For the overall efficiency of the column can be use following formulae:
4.
Procedure:
4.1 Starting Procedure:
4.1.4
4.1.5
4.1.6
4.1.7
4.1.8
Fill the reboiler with methanol-water solution by open the valve V1 and
air vent valve V2
4.1.9
4.1.10
4.1.11
4.1.12
4.1.13
4.1.14
4.1.15
4.1.16
Now take out the samples from the bottom & distillate stream (by closing
the timer for short while)
4.1.17
Cool down the samples to room temperature and measure the refractive
indices
4.1.18
4.1.19
4.1.20
Now adjust the cyclic timer to a desired reflux ration and for 3-5 min
4.1.21
Now takes out the samples from both distillate and bottom product
4.1.22
Cool down the samples to room temperature and measure the refractive
indices
4.1.23
4.1.24
4.1.25
Repeat the experiment for different set point temperatures and reflux
ratios
4.2
Closing Procedure:
4.2.1
4.2.2
4.2.3
3.32
32 g/mole
18 g/mole
0 kJ/kmole
0.90 m
(b)Observations
Total reflux condition
5.2
Calculations
Time
T (OC)
xthe
T(OC)
Time
y
Time
x
1 (
1)x
T(OC)
6. Nomenclature:
7. Block diagram
1. Objective
To operate the column under total reflux condition and calculate the minimum number of
theoretical stages using fenskes equation. To operate the column under any desired
reflux condition and calculate theoretical number of stages using Mc-Cabe Thieles
method
2. Description
The set-up consists of column with seven sieve trays. A vessel is provided with funnel, at
the bottom of the column. A sight glass is provided with it and two other sight glasses is
given at middle of the column. Safety valve and pressure gauge are given at vessel. A
tank is provided to collect the bottom product. Shell and tube type condenser is provided
to condensate the vapour. Reflux drum is provided to collect the condensate. Receiving
tank is for collecting the distillate. Seven valves are provided at each plate for collecting
the samples. Drain valves are provided for drainage purpose. Temperature sensors are
fitted at the appropriate place to measure the temperatures.
3. Theory
4.1
Part 1
In sieve plate distillation column sieve plate are provided instead of packing material.
For simple batch distillation process, initially the still is filled with F moles of feed with
xF as the mole fraction of the more volatile component. Let at any moment the number
of moles of liquid in the still be B having a mole fraction x of the more volatile
component (A) and let the moles of accumulated condensate be D. Concentration of the
equilibrium vapour is y*. Over a small time, the change in the amount of liquid in the
still is dB and the amount of vapour withdrawn is dD. The following differential mass
balance equations may be written:
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 number of plate is minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of
xB and xD based on the relative volatility of the components , which is defined in terms
of equilibrium concentrations:
Minimum number of theoretical plates required:
4. Experimental Procedure
5.1 Starting Procedure
5.1.1 Measure the refractive index of feed solution.
5.1.2 Note down the volume of methanol.
5.1.3 Close all the valves V1-V13.
5.1.4 Ensure that ON/OFF switches given on the panel are at OFF position.
5.1.5 Fill vessel with methanol-water solution by open the funnel valve V 1 and
5.1.6
5.1.7
5.1.10
V13 respectively.
5.1.19 Cool down the samples to room temperature & measure their refractive
indices.
5.1.20 Now adjust the cyclic timer to a desired reflux ratio & wait for steady
state.
5.1.21 Note down the temperatures of each tray.
5.1.22 Now take out the samples from each tray by open the valve V3-V9
5.1.23 Also collect the distillate and bottom product by open the valve V11 and
V13 respectively
5.1.24 Cool down the samples to room temperature & measure their refractive
indices.
5.1.25 Repeat the experiment for different set point temperatures & reflux ratios
5.2
Closing Procedure
5.2.1 When experiment is over switch OFF the heater.
5.2.2 Switch OFF the main power supply.
5.2.3
3.32
32 g/mole
18 g/mole
0 kJ/kmole
0.90 m
(b)Observations
Total reflux condition
6.2
Calculations
Time
T (OC)
xthe
T(OC)
Time
y
Time
x
1 (
1)x
T(OC)
Nomenclature:
7. Block diagram
1. Objective
To calculate the percentage recovery of turpentine oil.
2. Description
The set-up consists of jacketed pressure vessel. Steam generator is provided to
generate the steam. Condenser is given to condensate the vapour. Rotameter is provided
to measure the flow rate of cooling water supply. Steam trap is for releasing the pressure.
Digital temperature indicator & digital temperature controller are provided to indicate
and control the temperature.
3. Procedure
4.1 Starting Procedure
4.1.1 Take known amount of turpentine oil and note down the volume of it.
4.1.2 Take known amount of water, note down the volume of it & mix it with
turpentine oil.
4.1.3
4.1.4
Ensure that ON/OFF switches given on the panel are at OFF position.
4.1.5
Fill water in the steam generator by open the valve V1 and air vent valve
V2 and close them.
4.1.6
Charge the distillation still with turpentine oil & water mixture by open
4.1.7
4.1.8
4.1.9
4.1.10
4.1.11
4.1.12
115C).
Switch ON the heater.
Wait for the steam formation.
As steam formed, open the steam supply valve V3.
Start the supply of steam in jacket by open the valve V 4 and air vent valve
V9.
4.1.13 When the temperature in the still reaches 2C below the distillation
4.1.14
4.1.15
4.1.16
4.1.17
temperature, stop the supply of steam in jacket by close the valve V4.
Start the flow of live steam by open the valve V5.
Connect cold water supply to condenser.
Note down the live steam pressure.
Collect the condensed vapors in glass separating chamber.
4.1.18
4.1.19
4.1.20
4.1.21
= __________ kg/cm2
T = __________oC
VA
= __________ Lit.
VB
= __________ Lit.
VAD
= __________ Lit.
5.2 Calculations
To calculate the property of turpentine oil ( A ) and water ( B ) at temperature T
(oC) from data book.
A = ________ (kg/m3)
= ________ (kg/m3)
= 13.84799
= 3377.754
C
= 62.817
6. Nomenclature
7. Block Diagram
4.1.5
4.1.6
4.1.7
4.1.8
Wait till the bath attains the set temperature. Note the steady temperature
of the bath.
4.1.9
4.2.2
4.2.3
4.2.4
5.2 Observation
T = _________ C
X= _________ cm
No.
5.3 Calculations
t(min)
X(cm)
No.
6. Nomenclature
t1(sec)
x(cm)
7. Block Diagram
1. Objective
To study the dissolution of benzoic acid in water and in aqueous solution of sodium
hydroxide.
2. Aim
2.1 To calculate the mass transfer coefficient (kr) with chemical reaction.
2.2 To calculate the mass transfer coefficient (k) without chemical reaction.
2.3 To calculate the experimental enhancement factor (exp ) for the given system.
2.4 To calculate the theoretical enhancement factor (THE ) for the given system by
film and boundary layer model.
3. Description
The set up consists of a reactor with stirrer, connected with a variable speed mixer.
Baffles are provided in the mixer. RPM sensor is given to sense the speed of stirrer. A
peltilizer is provided to make the solid cylinder of benzoic acid. Constant temperature
water bath arrangement is provided with heater to conduct the experiment at various
temperatures. Valves are provided for drainage purpose.
4. Procedure
4.1 Starting procedure (for mass transfer with chemical reaction)
4.1.1 Prepare the benzoic acid cylinder first by using the peltilizer.
4.1.2 Record the dimensions of the benzoic acid cylinder.
4.1.3 Fill the burette with N/50 HCl solution.
4.1.4 Ensure that switches given on the panel are at OFF position.
4.1.5 Close all the valves V1-V2.
4.1.6 Fill the water bath with water.
4.1.7 Set the desired temperature of water bath (ambient to 50 oC).
4.1.8 Fill the reactor with aqueous sodium hydroxide solution of known
concentration up to 2/3rd of its volume.
4.1.9
the
sample
solution
against
N/50
HCl
solution
using
4.3.2
4.3.3
4.3.4
4.3.5
= ____________ oC
Di
= ____________ m
Df
= ____________ m
Li
= ____________ m
Lf
= ____________ m
N = ____________ RPM
N1w
V2
= ____________ g eq/L
= ____________ ml
V = ____________ Lit
= 0.0276 kmole/m3
= 0.00321 kmole/m3
= 0.006 m
= 1.04 x 10-9 m2/sec
= 4.1 x 10-9 m2/sec
= 0.5
=1
No.
t (sec)
V1W (ml)
= ____________ oC
Di
= ____________ m
Df
= ____________ m
Li
= ____________ m
Lf
= ____________ m
N = ____________ RPM
N1
= ____________ g eq/L
V2
= ____________ ml
V = ____________ Lit
Sr. No.
5.2
t (sec)
V1 (ml)
Sr. No.
t (sec)
CW (kmole/m3)
1-
CW
C
ln 1
CW
C
6. Nomenclature
7. Block diagram
3.1
Starting procedure
3.1.1
3.1.2
3.1.3
3.1.4
3.1.5
3.1.6
Start the blower and adjust the air flow rate by open the valve V1.
3.1.7
3.1.8
3.1.9
Open the lid of column fill the conical portion of the dryer with
the wet material and close the lid.
3.1.10 Allow the hot air at prefixed flow rate and temperature to pass
through the dryer.
3.1.11 The flow rate should be sufficient to fluidize the material.
3.1.12 At regular intervals of time take out measurable amount of wet
material and weigh it.
3.1.13 Dry it completely and weigh it again.
3.2
Closing procedure
3.2.1
3.2.2
= 0.026 m
= 0.052 m
= 0.6
= 9.81 m/sec2
= 1000 kg/m3
=1.21 kg/m3
= 18 g/mole
= 29 g/mole
Z = ________ gm
No.
4.2
t (sec)
WD (gm)
h1 (cm)
Calculations
Experimental Calculation:
Z
C W
(kg water/kg dry solid) (at t =0)
O
W
C Z WD
WD
TW1 (C)
W W D
C=
(kg water /kg dry solid )
WD
x=
Co C
( kg water /kg dry solid )
Co C
Calculation Table: 1
Sr. No.
X (kg water/kg dry solid)
t(sec)
S=
dx
dt
To calculate the humidity (y1 & y2) of air at temperature (Tw1 & Td1) and (Tw2 & Td2)
respectively by psychometric chart.
Calculation Table: 2
Sr. No.
5. Nomenclature
t (sec)
6. Block Diagram
20 liter of water.
Close all the valves V1-V10.
Ensure that switches given on the panel are at OFF position.
Fill colored liquid in the feed tank.
Keep activated charcoal in all the columns.
Connect electric supply to the set-up.
Open the valve V3 of the column-1.
Partially open the by pass valve V2.
Switch ON the pump.
Open and adjust the flow control valve V1 and by pass valve V2.
Simultaneously start the stop watch.
Collect samples from out let of column-1 after a time intervals.
Note down the time.
4.1.14
4.1.15
Run the experiment till the change in color of outlet liquid becomes almost
stable.
4.1.16
4.1.17
4.1.18
4.1.19
4.1.20
4.1.21
4.1.22
Run the experiment till the change in color of outlet liquid becomes almost
stable.
4.1.23
4.1.24
4.1.25
4.1.26
4.1.27
4.1.28
4.1.29
Run the experiment till the change in color of outlet liquid becomes almost
stable.
4.1.30
7.2.6
7.2.7
Remove the charcoal by open the filter cups of the columns properly.
=1m
= 0.5 m
= 0.3 m
(b) Observations
F = ________ LPH
O.D.F = ________
Sr. No.
(min)
O.D
5.2 Calculations
CF =________[From O.D. vs C graph value of C corresponding to O.D. F]
C = ________ [From O.D. vs C graph value of C corresponding to O.D.]
Sr. No.
(min)
O.D
C/CF
S = ________ (min)[From the graph, time at which areas of the shaded portions are equal]
B = ________ (min)[From the graph, time at which initial minimum concentration shows]
Nomenclature