EXPERIMENT NO : 2

LIQUID –LIQUID EXTRACTION

IN A PACKED BED
 LIQUID –LIQUID EXTRACTION IN A PACKED BED
(EXTRACTION OF BENZOIC ACID FROM TOLUENE BY WATER)

AIM:

To determine the following:

To determine overall mass transfer coefficient based on continuous phase (water), Kwa.

To determine overall mass transfer coefficient based on dispersed phase (toluene), Kta.

To determine overall ‘Height of Transfer Unit’ based on continuous phase (water), HTU ow.

To determine individual ‘Height of transfer unit’ based on continuous phase (water), HTUw
and dispersed phase (toluene), HTUt.

To study the extraction of benzoic acid from toluene (dispersed phase) by water (continuous
phase) in a packed bed.

THEORY:

Towers filled with some random packing (say rasching rings) are widely used for extraction of
valuable chemicals from dilute solutions by liquid –liquid extraction. The packing provides a
larger extract area for mass transfer and also reduces the axial mixing to some extent. The
extraction rate in such columns depend on:

- Choice of either continuous or dispersed phase.

- Packing and column variables.
- Velocity of the liquid phases in the tower.
- Variation in packed height.

The tower performance is generally based on extraction rate data and evaluated in terms of
overall height of transfer unit, based on continuous phase. HTUow and the extraction factor

expressed in terms of flow rate ratios of the liquid phases, . These two variables are plotted

against each other on Cartesian coordinates. As suggested by Colburn, the slope and intercept
of such a plot would represent the resistance of the individual films as:
OVERALL HEIGHT OF TRANSFER UNIT:

HTUow = HTUw + HTUt [m Vw/Vt]………………………………………………….(1)

HTUot = HTUt + HTUw [Vt/mVw]…………………………………………………….(2)

Where, m is the slope of equilibrium curve, m = dCw/dCt

Under certain conditions (e.g. low concentrations) m is a constant.

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 the continuous phase is defined as:

( ∗ ) ( ∗ )
= 𝐾 𝑎 𝑉[ ( ∗ ) ]
( ∗ )

( )
= 𝐾 𝑎 𝑉[ ( ]

The capacity coefficient based on continuous phase (water), Kwa, is thus defined as:

𝐾 𝑎= ………………………………….(3)
( )

( )
Where, (𝛥𝐶 ) = (

Similarly, the capacity coefficient based on dispersed phase (toluene). Kta, is defined as:

𝐾𝑎= …………………………………….(4)
( )

As per Chilton and Colburn, the overall height of transfer unit based on continuous phase
(water), HTUow is defined as:

HTUow = …………………………………………………………….(5)

And the overall height of transfer unit based on dispersed phase (toluene), HTUot is defined as:
HTUot = …………………………………………………………….(6)

Where:

N/θ is the kgmole of benzoic acid transferred from toluene to water per hour.

V is the effective volume of packed section, m3.

Vw is water flow rate, l/h-sq.m cross section of empty column.

Vt is toluene flow rate, l/h-sq.m cross section of empty column.

Cw1 is concentration of benzoic acid in water at its outlet, kgmol/l.

Cw2 is concentration of benzoic acid in water at its inlet, kgmol/l.

Ct1 is concentration of benzoic acid in toluene at its inlet, kgmol/l.

Ct2 is concentration of benzoic acid in toluene at its outlet, kgmol/l.

C*w is equilibrium solute (benzoic acid) concentration in water phase.

C*t is equilibrium solute (benzoic acid) concentration in toluene phase.

Equilibrium distribution coefficient, H = C*w / C*t .

Water in, Cw2 Dc Toluene out, Ct2 + Benzoic acid

Qw , L/H

Benzoic Acid +Toluene in, Water out, C w1+

Ct1, Qt, L/H Benzoic acid.

DESCRIPTION:

In this system the two different liquids are used in which the one is heavier which is used as
solvent and the other in the solute is present. The heavier liquid is inserted from the top and the
lighter from the bottom; both the feeds are compressed by air. The interfaced maintained in the
column 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 in this case) into the column. The samples are taken from the top
and bottom and analysis that as per the procedure.

UTILITIES REQUIRED:

1. Compressed air supply at 2 bar, 0.5 CFM.

2. Drain.
3. Required chemicals & Laboratory Glassware.

CHEMICAL REQUIRED:

1. Toluene,
2. Benzoic acid
3. Distilled water
4. N/2 or N/5 NaOH in Alcohol.
5. N/10 or N/20 NaOH in water.
6. Phenolphthalein as indicator.

BENZOIC ACID: C7H6O2: M.W = 122; EQ.WT =122

TOLUENE; C7H8: M.W = 92

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.

Starting Procedure:

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 kmole/m 3 means 24.4 gm/lt or
488 gm in 20 ltrs.
1. Fill the column with the continuous phase (water).
2. Allow the dispersed phase (toluene + benzoic acid) to enter from the bottom of the
column at some minimum rate.
3. Adjust the rotameter readings for both the phases to some prefixed values.
(1 to 5 LPH for dispersed phase and 3 to 10 LPH for continuous phase)
Note: The rotameter should be calibrated for these liquids. In case the rotameters are
not provided use measuring cylinders.
4. 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 id to be maintained at about 1 inch
above the point of introduction of the heavier liquid (water in this case) into the column.
5. In case lighter liquid is the continuous phase, the same valve should be used to keep the
interface at about 1 inch below the introduction of lighter liquid at the bottom.
6. Take the first observation after the steady state has been established i.e. after ≈ 10 to 20
minutes.
Steady state record the following:
a) Flow rate of water phase, Qw, l/h
b) Flow rate of toluene phase, Qt , l/h
c) Ambient temperature , T, °C

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/2 or N/5) for titration
against toluene solution and NaOH solution (N/10 or N/20) in water for titration against water
solution)
Repeat the above steps for 5 to 6 different flow rates of continuous phase/dispersed phase.

STANDARD DATA:

Extraction column = Material Borosilicate Glass

Dia.45 mm, Height 750 mm (approx.).

Packing Material = Borosilicate Glass Rasching Rings size 8-10 mm (approx.).

Feed Tanks = Material Stainless Steel 304 grade, Capacity 20 Ltrs. 2 nos.

Extract & Raffinate Tanks = Material Stainless Steel 304 grade, Capacity 10 Ltrs.2 nos.

Piping = SS 304 and PVC, Size 1/4”

Feed circulation = By compressed air.

Pressure Regulator = 0-2 kg/cm2

Pressure Gauge = Bourdon type, 0-2 kg/cm2.

Flow Measurement = Rotameters (one each for solvent & solute)

Special arrangement for changing interface zone at any level in extraction column.

The whole set-up is well designed and arranged in a good quality painted structure.

FORMULAE:

A. Concentration of benzoic acid in toluene:

1) At bottom: (feed Concentration)

V1 = 10 ml (Toluene) Volume of N/5 NaOH (In Alcohol) used = 10.9 ml = V2

N1 = ?

‫ ؞‬V N =V N
1 1 2 2

‫؞‬N= 1

Concentration of Benzoic Acid in the Toluene at bottom = CT1 = (N1×122.gm/L)

C T1 = …….gmole/L.
Molecular weight of Benzoic Acid = 122. g mole/gram.

V1 = 10 ml (Toluene) Volume of N/5 NaOH (In Alcohol) used for

Titration=10.2 ml (V2) Phenolphthalein as indicator.

N1 = ?

‫؞‬N =
1

Conc. of benzoic acid in toluene at top = Ct2 =…….gmole/L.

Volumetric flow rate of Toluene Phase:

QTol = …………………………..L/H.

‫؞‬ Amount of benzoic acid extracted by water, NA1 = (C1-C2) × QTol

= ………gmole/h.

B. Concentration of benzoic acid in water:

1) Top:

Pure Water Cw2 =0

2) Bottom:

Volume of water sample used for titration V1 = 10 ml.

Normality of acid in water = N1

Normality of acid in water = V1N1 =V2N2

N1 =

Conc. of acid in water at bottom = N1 =…….gmole/L. Cw1 = N1 gmole/L

Volumetric flow rate of water Qw = …..L/H.

‫؞‬ Amount of benzoic acid recovered by water, NA2 = (C1-C2) × Qw

= ………gmole/h
Average amount of Benzoic Acid recovered N/θ = gmole/h.

Column cross sectional area = 𝐴 = Dc2 = 12.5664 cm2 = 0.00125664 m2

Effective volume = V = Dc2 z = 942.478 cm3 = 0.9425 L

OVERALL MASS TRANSFER COEFFICIENT BASED ON DISPERED PHASE:

Kta

CT1 = gmole/l

CW1 = gmole/l

From equilibrium data = H1

ΔCt1 = CT1- (Cw1/H1)

At top:

CT2 = gmole/l

CW2 = 0

= H2 at Ct = Ct2 (using equilibrium data)

ΔCt2 = CT2- (Cw2/H2)

( )
(𝛥𝐶 ) =

(𝛥𝐶 ) = gmole/L.

Since.

= 𝐾 𝑎𝑉(𝛥𝐶 )
𝐾𝑎= = 𝐾 𝑎 = gmole/h-L-gmol/L
( )

OVERALL MASS TRANSFER COEFFICIENT BASED ON CONTINUOUS PHASE:

Kwa

𝐾 𝑎=
( )

ΔCw1 = H1Ct1 – Cw1

ΔCw2 = H2Ct2 – Cw2

( )
(𝛥𝐶 ) = gmol/L.

𝐾 𝑎= , gmol/L-h-ΔC
( )

OVERALL HEIGHT OF TRANSFER UNIT BASED ON CONTINUOUS PHASE:

Superficial velocity of water phase Vw = Qw / empty cross section of the column.

Vw = m/h

HTUow = = m

= cm.

OVERALL HEIGHT OF TRANSFER UNIT BASED ON DISPERED PHASE:

Superficial velocity of toluene phase Vt = Qw / empty cross section of the column.

Vw = m/h

HTUot = = m
OBSERVATIONS & CALCULATION:

Column diameter: Dc, m

Packed height: z, m
Packing: Rasching Rings
Diameter of rasching ring:
Length of rasching ring:
Ambient temperature: T, °C
System: toluene- benzoic acid- water.
Solute: benzoic acid.
Initial conc. of benzoic acid in toluene = Ct1 = gmol/L
Initial conc. of benzoic acid in water = Cw1 = 0.0 gmol/L (using pure water)

OBSERVATIONS:
VOL OF N/2 NaOH (IN VOL OF N/10 NaOH (IN
RUN NO. Qw, L/H Qt, L/H
ALCOHOL) USED FOR WATER) USED FOR 10
10 ML OF TOLUENE ML OF WATER
SOLUTION SOLUTION

ESTIMATE THE FOLLOWING:

RUN NO. Qw, L/H Qt, L/H Cw1 Cw2 Ct1 Ct2 RATE OF
gmol/L gmol/L gmol/L gmol/L M.T
N/θ,gmol/h
RUN NO. (HTU)ow (HTU)ot 𝑉 𝑉 (HTU)w (HTU)t
𝑚
m m 𝑉 𝑚𝑉 m m

EQUILIBRIUM DATA FOR:

BENZOIC ACID- TOLUENE-WATER

Aqueous phase, Cw gmole/L, Benzoic Organic phase, Ct gmole/L, Benzoic
Acid acid
0.0000 0.0000
0.0016 0.0080
0.0032 0.0240
0.0064 0.0336
0.0080 0.0673
0.00961 0.08811
0.011211 0.12015
0.012816 0.14097
0.01442 0.17301

0.025

0.02
0.02

0.015
0.015
CW

0.01
0.01

0.005
0.005

0
0.05 0.1 0.15 0.2
CT
The equilibrium data can be represented by:

= H = 0.2015 - 1.4273Ct + 4.3672 C2t

And

Cw = 0.0745Ct + 0.0019

Or slope of the equilibrium line can be assumed to be constant at

m = dCw/dCt = 0.0745

SAMPLE CALCULATIONS AND OBSERVATIONS:

(Extraction in a packed bed)

Water in 3.525, Cw2 Dc Toluene out, Ct2 + Benzoic acid

Qw , L/H = 0 gmole/L

Benzoic Acid + Toluene in, Water out, C w1+

Ct1, Qt, L/H = 3.9 L/H Benzoic acid. (gmole/L)

 A. Concentration of benzoic acid in toluene:

1) At bottom: (feed Concentration)

V1 = 10 ml (Toluene) Volume of N/5 NaOH (In Alcohol) used = 10.9 ml = V 2

N1 = ? N2 = 1/5

‫ ؞‬V N =V N
1 1 2 2

‫؞‬N= 1

Concentration of Benzoic Acid in the Toluene at bottom = CT1 = (N1×122.gm/L)

C T1 = …….gmole/L.

Molecular weight of Benzoic Acid = 122. gmole/gram.

2) At top:

V1 = 10 ml (Toluene) Volume of N/5 NaOH (In Alcohol) used for

Titration = 10.2 ml (V2) Phenolphthalein as indicator.

N1 = ?

‫؞‬N = 1

Conc. of benzoic acid in toluene at top = Ct2 =…….gmole/L.

Volumetric flow rate of Toluene Phase:

QTol = …………………………..L/H.

‫؞‬ Amount of benzoic acid extracted by water, NA1 = (C1-C2) × QTol

= ………gmole/h.

B. Concentration of benzoic acid in water:

1) Top:

Pure Water Cw2 = 0

2) Bottom:

Volume of water sample used for titration V1 = 10 ml.

Normality of acid in water = N1

Normality of acid in water = V1N1 = V2N2

N1 =

Conc. of acid in water at bottom = N1 =…….gmole/L.

Cw1 = N1 gmole/L

Volumetric flow rate of water Qw = …..L/H.

‫؞‬ Amount of benzoic acid recovered by water, NA2 = (C1-C2) × Qw

= ………gmole/h

Average amount of Benzoic Acid recovered N/θ = gmole/h.

Packing height, Z = 75 cm.

Packing: Rasching rings

Diameter of rasching ring: I.D = 6 mm

O.D = 9 mm

Length of rasching ring: L = 9 mm

Column diameter = Dc = 40 mm = 4.0 cm

Column cross sectional area = 𝐴 = Dc2 = 12.5664 cm2 = 0.00125664 m2

Effective volume = V = Dc2 z = 942.478 cm3 = 0.9425 L

OVERALL MASS TRANSFER COEFFICIENT BASED ON DISPERED PHASE:

Kt a
At bottom:

CT1 = gmole/l

CW1 = gmole/l

From equilibrium data = H1

ΔCt1 = CT1- (Cw1/H1)

At top:

CT2 = gmole/l

CW2 = 0

= H2 at Ct = Ct2 (using equilibrium data)

ΔCt2 = CT2 - (Cw2/H2)

( )
(𝛥𝐶 ) =

(𝛥𝐶 ) = gmole/L.

Since.

𝐾𝑎=
( )

𝐾 𝑎 = gmole/h-L-gmol/L

OVERALL MASS TRANSFER COEFFICIENT BASED ON CONTINUOUS PHASE:

Kwa

𝐾 𝑎=
( )
 ΔCw1 = H1Ct1 – Cw1 =…………….
ΔCw2 = H2Ct2 – Cw2 =…………….

( )
(𝛥𝐶 ) = gmol/L.

𝐾 𝑎= =…………… gmol/L-h-ΔC
( )

OVERALL HEIGHT OF TRANSFER UNIT BASED ON CONTINUOUS PHASE IS:

Superficial velocity of water phase Vw = Qw / empty cross section of the column.

Vw =………… m/h

HTUow = =…………. m

=…………cm.

OVERALL HEIGHT OF TRANSFER UNIT BASED ON DISPERED PHASE IS:

Superficial velocity of toluene phase Vt = Qw / empty cross section of the column.

Vw = ………………..m/h

HTUot = =………… m

Repeat the above calculations for five different flow rate ratios of continuous and dispersed
phases ( Vw/Vt) and use equations (1&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 (HTU)ow vs Vw/Vt on a simple graph & determine the slope and the
intercept.

Intercept = (HTU)w

Slope = (HTU)t
 (HTU)ow
Slop

m. Vw/Vt

PRECAUTIONS & MAINTENANCE INSTRUCTION:

1. Prepare the feed solution in exactly as per our manuals.

2. Make the interface always ‘1’ inch above the water inlet sparger.
3. Interface should not be disturbed.
4. Water outlet should be toluene free.
5. Feed tank should be clean.
6. Always use clean water.
7. Don’t exceed the flow rate at 15 LPH.

TROBLUE SHOOTING:

1. If any type of suspended particles are 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 afte 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.)
 LIQUID LIQUID EXTARCTION IN PACKED BED COLUMN

SAMPLE CALCULATIONS AND OBSERVATIONS:

(Extraction in a packed bed)

Water 3.525 L/H, Dc Toluene out, Ct2 + Benzoic acid

Cw2 =0 gmole/L

Benzoic Acid +Toluene in, Water out, C w1+

Ct1, Qt, L/H = 3.9 L/H Benzoic acid. (gmole/L)

A. Concentration of benzoic acid in toluene:

1) At bottom: (feed Concentration)

V1 = 10 ml (Toluene) Volume of N/5 NaOH (In Alcohol) used = 10.9 ml = V 2

N1 =? N2 =1/5

‫ ؞‬V N =V N
1 1 2 2

‫؞‬N= 1 =
. ×

×
= 0.218 g eq/L

Concentration of Benzoic Acid in the Toluene at bottom = CT1 = (0.218 ×122.gm/L)

C T1 = 0.218gmole/L.
Molecular weight of Benzoic Acid = 122. gmole/gram.

2) At top:

V1 = 10 ml (Toluene) Volume of N/5 NaOH (In Alcohol) used for

Titration = 10.2 ml (V2) Phenolphthalein as indicator.

N1 =?

‫؞‬N =
1 =
. ×

×
= 0.204 g eq./L

Conc. of benzoic acid in toluene at top = Ct2 = 0.204 gmole/L.

Volumetric flow rate of Toluene Phase:

QTol = 3.9 L/H.

‫؞‬ Amount of benzoic acid extracted by water, NA1 = (0.218 - 0.204) × 3.9

= 0.0546gmole/h.

B. Concentration of benzoic acid in water:

1) Top:

Pure Water Cw2 = 0

2) Bottom:

Volume of water sample used for titration V1 = 10 ml.

Normality of acid in water = N1

Normality of acid in water = V1N1 = V2N2

×
N1 = = = 0.01 g eq./L
×

Conc. of acid in water at bottom = N1 = 0.01gmole/L.

Cw1 = 0.01 gmole/L

Volumetric flow rate of water Qw = 3.525 .L/H.

 ‫؞‬ Amount of benzoic acid recovered by water, NA2 = (0.01-0) × 3.525

= 0.03525 gmole/h

. .
Average amount of Benzoic Acid recovered N/θ = = 0.044925 gmole/h.

Packing height , Z = 75 cm.

Packing : Rasching rings

Diameter of rasching ring: I.D = 6 mm

O.D = 9 mm

Length of rasching ring: L = 9 mm

Column diameter = Dc = 40 mm = 4.0 cm

Column cross sectional area = 𝐴 = Dc2 = 12.5664 cm2 = 0.00125664 m2

Effective volume = V = Dc2 z = 942.478 cm3 = 0.9425 L

OVERALL MASS TRANSFER COEFFICIENT BASED ON DISPERED PHASE:

Kt a

At bottom:

CT1 = 0.218 gmole/l

CW1 = 0.01 gmole/l

From equilibrium data = H1 = 0.08485, [H1 = 0.018497/0.218 = 0.08485]

ΔCt1 = CT1- (Cw1/H1)

ΔCt1 = 0.218- (0.01/0.08485) = 0.1001 gmole/L

At top:

CT2 = 0.204 gmole/l

CW2 = 0

= H2 at Ct = Ct2 (using equilibrium data) = 0.0855745

ΔCt2 = CT2- (Cw2/H2) = 0.204 gmole/L

( ) . .
(𝛥𝐶 ) = = .
.

(𝛥𝐶 ) = 0.1459 gmole/L.

Since.

𝐾𝑎=
( )

.
𝐾𝑎= = 0.3267 gmole/h-L-gmol/L
. × .

OVERALL MASS TRANSFER COEFFICIENT BASED ON CONTINUOUS PHASE:

Kwa

𝐾 𝑎=
( )

ΔCw1 = H1Ct1 – Cw1 = 0.08497 × 0.218-0.01 = 0.0084973

ΔCw2 = H2Ct2 – Cw2 = 0.0855745 × 0.204 - 0 = 0.0174572
( )
(𝛥𝐶 ) = = 0.012444 gmol/L.

𝐾 𝑎= = 0.044925/(0.9425 × 0.012444) = 3.8305 gmol/L-h-ΔC

( )
OVERALL HEIGHT OF TRANSFER UNIT BASED ON CONTINUOUS PHASE:

Superficial velocity of water phase Vw = Qw / empty cross section of the column.

Vw = 3.525 × 10-3 /12.564 × 10-4 = 2.8055 m/h

HTUow = = 2.8055/3.8305 = 0.7324 m

=73.24 cm.

OVERALL HEIGHT OF TRANSFER UNIT BASED ON DISPERED PHASE:

Superficial velocity of toluene phase Vt = Qt / empty cross section of the column.

Vt = 3.9 × 10-3/12.564 × 10-4 = 3.104 m/h

HTUot = = 3.104/0.3267= 9.5 m

m = 0.067155

= 14.89096

Repeat the above calculations for five different flow rate ratios of continuous and dispersed
phases ( Vw/Vt) and use equations (1&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 (HTU)ow vs Vw/Vt on a simple graph & determine the slope and the
intercept.

Intercept = (HTU)w

Slope = (HTU)t

(HTU)ow SloS

m. Vw/Vt