EXPERIMENT NO :6

PACKED BED DISTILLATION

COLUMN
 CONTENTS
Aim……………………………………………………………………………… 1
Theory…………………………………………………………………………… 1
Description………………………………………………………………………. 3
Utilities Required………………………………………………………………... 3
Experimental Procedure…………………………………………………………. 3
Standard Data……………………………………………………………………. 4
Formulae………………………………………………………………………… 4
Observations……………….……………………………………………………. 5
Precautions & Maintenance Instructions………………………………………... 8
Trouble Shootings………………………….……………………………………. 8
 BATCH RECTIFICATION IN A PACKED
DISTILLATION COLUMN
AIM:
To study the operation of a batch rectification column under constant or total reflux condition.
To operate the column under total reflux condition and estimate the HETP.
To study the effect of reflux rate on the average composition of distillate.

THEORY:
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 quantity of one of the components of the mixture has been recovered or until a
definite change in composition of the still contents has been effected.

In a batch rectification set up, vapours generated in the kettle pass up the column counter-
currently to liquid that is passing down the column. The column packing provides a good
contact between the liquid and vapour. As liquid passes up the column, it comes in contact with
thin film of liquid formed around the packing surface. This results in a transfer of mass and
heat. Most of the heat transferred between the two phases and effective for vaporization, is that
due to the latent heat of components. If the molal latent heats of vaporization of components
are very nearly the same, as is often the case, then the moles of vapour condensed are
approximately equal to the moles of liquid vaporized. As a result, the molal vapour up-flow
throughout the column remains constant. Also the liquid down-flow from top to bottom
remains constant.

In the column, the mass is transferred in such a way that the more volatile component passes
from the liquid to the vapour and the less volatile components pass from the vapour into the
liquid. Thus there is an increase in the concentration of the more volatile component in the
vapour as they pass up the column. There is also an increase in the concentration of the less
volatile component in the liquid as it passes down the column.
In all type of batch distillation, a quantity of feed is charged to a still pot, or kettle and heat is
applied to it. The vapour, which is usually passed through a fractionating 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
must alter as the distillation proceeds.

The method of operation of a batch fractionation still is similar to that of a continuous still,
reflux being returned to the top of the column to enable fractionation to take place. At the start
of distillation, the column is either run at total reflux until equilibrium has been attained; or the
reflux ratio is fixed at the required value from the beginning, in which case the distillate is
recycled to the still until conditions are stable. The operation of the batch still can be either of
two methods:

1. Constant reflux ratio variable product composition.

By this method it is possible to split a given feed into a number of fraction in the one
operation by running the column under constant reflux and taking several cuts for the
distillate.
2. Variable reflux ratio constant product composition.
When it is desired to produce a distillate of specific constant composition, the reflux
ratio must be continuously increased and the rate of output consequently decreases.

DESCRIPTION:

In packed distillation column the process is batch rectification. The feed solution is filled in the
steam generator the heater are provided for heating the feed solution. The vapours are goes
through the packed S.S column and condensed in water condenser. Some of the part are
recycled by setting the reflux ratio as per desired. Distillate is collected in the glass collector
and the samples are analyzed by the refractometer.

UTILITIES REQUIRED:

Water supply 4 LPM (approx.) and Drain.

Electricity supply: 1 Phase, 220V AC, 6.5kW.

Required chemicals.

Refractometer for analysis.

Schematic Diagram for Packed Distillation Column

EXPERIMENTAL PROCEDURE:

1. Charge the still 2/3 full with MeOH-water feed mixture.

2. Record the exact feed composition (xf) from the calibration curve either by using
refractometer or using specific gravity bottle.
3. Start the supply to the condenser and switch on the heat supply to the still.
4. Operate the column under total reflux condition and adjust the heat input to the still till
the temperature in the still is ready.
5. Read the temperature at the top and the bottom until they indicate that the system has
reached equilibrium.
 6. Then record the following data:
1. Record the temperature of the still and the vapour.
2. Record the temperature of the reflux and the distillate.
3. Record the flow rate of cooling water, its inlet temperature and outlet temperature.
4. At steady state, record the composition of distillate and still liquid (XD and XB).
T1= Vapours coming out from still temperature
T2= Vapours coming out from packed bed
T3= Still temperature vapour inlet temperature to the condenser
T4= Distillate temperature
T5= Water inlet temperature
T6= Water outlet temperature
7. Take the equilibrium data from Perry hand book and plot it. Plot XD and XB on McCabe-
Thiele diagram and step off the number of theoretical plates under total reflux condition.
8. Measure the height of the packed section (Z) and divide it by number of theoretical
plates to give H.E.T.P.

mL of water VB mL of CH3OH VA Mole fraction CH3OH x R.I At 420C

100 0 0 1.33
90 10 0.059 1.3315
80 20 0.1233 1.3325
70 30 0.194 1.3345
60 40 0.273 1.336
50 50 0.36 1.337
40 60 0.458 1.3375
30 70 0.568 1.337
20 80 0.69 1.3345
10 90 0.837 1.3305
0 100 1 1.3235
 R.I. of Methanol/Water solutions at 420C
1.338

1.337

1.336

1.335
R.I. at 420C

1.334

1.333

1.332

1.331

1.33

1.329
0 20 40 60 80 100 120
Mole % Methanol

Plot R.I. vs x using excel or plot x vs R.I. and fit two polynomials one for CH 3OH rich
section (to be used for finding the distillate composition) and the other for water rich section
(to be used for finding the feed and bottoms composition).

At 150C

e.g. for CH3OH rich section: x= 48.409-35.794 R.I. …. (1)

and for water rich section: x= 3483.5-5273.4 R.I.+1995.7 R.I.2 …. (2)

STANDARD DATA:

Column : Material = SS 304

ID = 80 mm

Length = 0.9 m

Packing : Material = Rasching Ring

Length = 11 mm

O.D = 10 mm

I.D = 6 mm

Packed Height = 720 mm

Heater 2 No. : Capacity = 2 kW each

Reboiler : Material = SS 304

Capacity = 25 ltr

Condenser : Material = SS 304

I.D = 109 mm

Length = 500 mm

Tubes : Material = SS 304

O.D = 12.7 mm

I.D = 9.5 mm

Length = 500 mm

No. of tubes = 12

FORMULAE:
L
R=D

xD
Intercept= R+1

(NT −1)
Overall efficiency of the Packed Distillation Column= × 100
N

H.E.T.P.= Z⁄N

OBSERVATION & CALCULATIONS:

Density of Feed = …... gm/cm3 at ambient temp.

Density of Distillate = …... gm/cm3 at ambient temp.

R.I of Feed = …….

R.I of Distillate = …….

From the calibration curve, corresponding mole fractions of CH3OH are:

xf = ……
xD = …….

L/D = …….

Packed Height = …………… cm

Cooling Water Rate = ……………. LPH

Cooling water inlet temp. = …………….. 0C

Cooling Water outlet temp. = …………….. 0C

Feed temp. = 320C

Steady state temperature of the column:

Sensor No. Temperature, 0C

1
2
3
4
5

Where equilibrium value yf corresponding to xf can be obtained from:

Average value of α for CH3OH-H2O system is

α = 3.32

for xf =

for yf =

L
R = D = ……

xD
Intercept= = ……
R+1

Using the x-y data for CH3OH-H2O, available in Perry, construct the McCabe Thiele
diagram for the given observed conditions, step off the number of ideal stages required.
From McCabe Thiele diagram we obtain eight ideal stages including Reboiler.

Total number of ideal stages (including Reboiler) = NT = ………...

No. of ideal stages required = NT -1 =…….

No. of actual stages required = N =……

(NT −1)
Overall efficiency of the Packed Distillation Column= × 100
N

7
η% = × 100 = 100
7

H.E.T.P.= Z⁄N

H.E.T.P. = …...

T, 0C x y
100 0.000 0.000
96.4 0.020 0.134
93.5 0.040 0.230
91.2 0.060 0.304
89.3 0.080 0.365
87.7 0.100 0.418
84.4 0.150 0.517
81.7 0.200 0.579
78.0 0.300 0.665
75.3 0.400 0.729
73.1 0.500 0.779
71.2 0.600 0.825
69.3 0.700 0.870
67.5 0.800 0.870
66.0 0.900 0.958
65.0 0.950 0.979
64.5 1.000 1.000

Equilibrium data Perry’s hand book.

PRECAUTIONS & MAINTENNANCE INSTRUCTIONS:

1. Always make the calibration chart at room temperature before starting the experiment.
2. Column should be air free.
3. Total reflux time more than 45 mins.
4. For better results use Refractometer.
5. Don’t switch on the heater before filling the feed into it.
6. For condenser the cold water supply should be constant.
7. Don’t switch on the pump at low voltage.

TROUBLE SHOOTING:

1. If any type of suspended particles is come in the rotameter, remove the rotameter
clean the tube and fit that at its place.
2. If there is any leakage tight that part or remove that and refix that again after
wrapping Teflon tape.
3. If Rotameter fluctuating more than 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.)
4. If D.T.C. display ‘1’ on display board it means sensors connection are not OK 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.
 BATCH RECTIFICATION IN A PACKED DISTILLATION
COLUMN

STANDARD DATA:

Column : Material = SS 304

ID = 80 mm

Length = 0.9 m

Packing : Material = Rasching Ring

Length = 11 mm

O.D = 10 mm

I.D = 6 mm

Packed Height = 720 mm

Heater 2 No. : Capacity = 2 kW each

Reboiler : Material = SS 304

Capacity = 25 ltr

Condenser : Material = SS 304

I.D = 109 mm

Length = 500 mm

Tubes : Material = SS 304

O.D = 12.7 mm

I.D = 9.5 mm

Length = 500 mm

No. of tubes = 12
 R.I. of Methanol/Water solutions at 420C
1.338

1.337

1.336

1.335
R.I. at 420C

1.334

1.333

1.332

1.331

1.33

1.329
0 20 40 60 80 100 120
Mole % Methanol
 DESCRIPTION:

The column is made of Stainless Steel 304 grade material with seven plates for mounting
the bubble caps. Each plate is provided with one bubble cap. An electrically heated Reboiler
is installed at the bottom of the column. The bottom product is collected in the tank. The
vapours from the top of 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 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.

mL of water VB mL of CH3OH VA Mole fraction CH3OH x R.I At 420C

100 0 0 1.33
90 10 0.059 1.3315
80 20 0.1233 1.3325
70 30 0.194 1.3345
60 40 0.273 1.336
50 50 0.36 1.337
40 60 0.458 1.3375
30 70 0.568 1.337
20 80 0.69 1.3345
10 90 0.837 1.3305
0 100 1 1.3235

Plot R.I. vs x using excel or plot x vs R.I. and fit two polynomials one for CH 3OH rich
section (to be used for finding the distillate composition) and the other for water rich section
(to be used for finding the feed and bottoms composition).

At 150C

e.g. for CH3OH rich section: x= 1543.2-2295.8 R.I.+854.17 R.I.2 …. (1)

and for water rich section: x= 1436.8-2191.8 R.I.+835.71 R.I.2 …. (2)

OBSERVATION & CALCULATIONS:

Density of Feed = 1.022 gm/cm3 at ambient temp.

Density of Distillate = 0.809 gm/cm3 at ambient temp.

Density of Bottoms = 1.009 gm/cm3 at ambient temp.

R.I of Feed =1.3340C

R.I of Distillate = 1.3230C

R.I of Bottoms = 1.33150C

From the calibration curve, corresponding mole fractions of CH3OH are:

xf = 0.13

xD = 0.90

xB = 0.55

L/D =

Packed Height = 90 cm

Cooling Water Rate = 70 LPH

Cooling water inlet temp. = 37 0C (T10)

Cooling Water outlet temp. = 60 0C (T11)

Feed temp. = 380C

Steady state temperature of the column:

Sensor No. Temperature, 0C

1 89
2 72
3 69
4 33.3
5 32
6 44.6
 Plot observed T-x diagram and compare it with the literature T-x diagram. Discuss you
results.

Where equilibrium value yf corresponding to xf can be obtained from:

ρ 0.803×1000
Molar density of MeOH= (M MeOH
)
= = 25.09 kmol⁄m3 = ρA
W MeOH 32

ρ 1×1000
Molar density of water= (M water
)
= = 55.56 kmol⁄m3 = ρB
W water 18

Average molecular weight of:

1. Feed= Mf = xf ρA + (1 − xf )ρB
Mf = 0.13 × 25.09 + (1 − 0.13) × 55.56
Mf = 51.60 kmol⁄m3
2. Distillate= MD = xD ρA + (1 − xD )ρB
MD = 0.90 × 25.09 + (1 − 0.90) × 55.56
MD = 28.137 kmol⁄m3
3. Bottoms= MB = xB ρA + (1 − xB )ρB
MB = 0.05 × 25.09 + (1 − 0.05) × 55.56
MB = 54.00 kmol⁄m3
4. Determination of q line:
Feed is fed at Tf = 37 0C
H −H
Q = H G−H f …. (3)
G L

With reference to feed temperature i.e. taking feed temperature as the reference temp., Hf =0

Cpf
HL = (1000) Mf (BP − Tf ) in kJ⁄kmol …. (4)

Where HL = Enthalpy of feed at its Bubble point, BP

Enthalpy of saturated vapour, HG at its Dew point (DP) = HG

CpA CpB
HG = xf [1000 × MA (DP − Tf ) + λA × MA ] + (1 − xf ) [1000 × MB (DP − Tf ) + λB × MB ] ..(5)

Where MA= Mol. Wt. of MeOH = 32

MB= Mol. Wt. of Water = 18

CPA= Sp. Heat of MeOH = 2721 J/kg K

 CPB= Sp. Heat of Water = 4187 J/kg K

λA = Latent heat of vaporization of MeOH = 104607 k/kg

λB = Latent heat of vaporization of water = 2284 kJ/kg

Based on the composition of the feed, average Sp. Heat of feed = Cpf

Cpf = xf CpA + (1 − xf )CpB

= 0.13 × 2721 + (1 − 0.13) × 4187

= 3996.42 J/kg-K

From the T-x-y data given in Perry one can obtain the bubble point and the dew point.

Or the given data of T-x-y for MeOH-Water can be fitted to a polynomial given below to
yield Bubble point, BP and Dew point, DP.

BP = 99.0412 − 139.12 xf + 318.721 xf 2 − 359.156 xf 3 + 45.319 xf 4 …. (6)

= 85.58

DP = 100.192 − 26.758 yf − 9.64492 yf 2 …. (7)

= 90.31

Where equilibrium value yf corresponding to xf can be obtained from:

αxf
yf =
1 + (α − 1)xf

= 0.33

Average value of α for MeOH-H2O system is:

α = 3.32

for xf = 0.13

for yf = 0.33

BP = 85.58 0C

DP = 90.31 0C

Using these values in equations 4 & 5 and 3

HL = 10794.52

HG = 475031.4476

Q = 1.023

q 1.023
Slope of the q-line= q−1 = 1.023−1 = 44.00

Average value of α for MeOH-H2O system is:

α = 3.32

for xf = 0.13

for yf = 0.33

L
R= =3
D
x
D
Intercept= R+1 = 0.225

Using the x-y data for CH3OH-H2O, available in Perry, Construct the McCabe Thiele diagram
for the given observed conditions, step off the number of ideal stages required or you can use
tray-by-tray calculations also. From McCabe Thiele diagram we obtain eight ideal stages
including Reboiler.

Total number of ideal stages (including Reboiler) = NT = 6

No. of ideal stages required = NT -1 = 5

No. of actual stages required = N = 7

(NT −1)
Overall efficiency of the Packed Distillation Column= × 100
N

5
η% = × 100 = 71
7

H.E.T.P.= Z⁄N = 0.9⁄7 = 0.129

 T, 0C x y
100 0.000 0.000
96.4 0.020 0.134
93.5 0.040 0.230
91.2 0.060 0.304
89.3 0.080 0.365
87.7 0.100 0.418
84.4 0.150 0.517
81.7 0.200 0.579
78.0 0.300 0.665
75.3 0.400 0.729
73.1 0.500 0.779
71.2 0.600 0.825
69.3 0.700 0.870
67.5 0.800 0.870
66.0 0.900 0.958
65.0 0.950 0.979
64.5 1.000 1.000

Equilibrium data Perry’s hand book.