EXPERIMENT NO:3

ABSORPTION IN PACKED BED

COLUMN

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 Contents
Part-1

Aim …………………………………………………………………………3

Utilities required ……………………………………………………………3

Description ………………………………………………………………….3

Theory……………………………………………………………………….3

Experimental Procedure……………………………………………………..5

Standard Data………………………………………………………………...5

Formulae……………………………………………………………………..6

Observations & Calculation Table…………………………………………..8

Precautions & Maintenance Instructions……………………………………12

Trouble shooting…………………………………………………………….12

Part-2

Sample Calculations…………………………………………………………13

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ABSORPTION WITH CHEMICAL REACTION IN A PACKED
BED

(CO2 absorption NaOH Solution)

AIM

To study absorption of CO2 in aqueous NaOH solution in packed bed column.

To determine the gas phase mass transfer coefficient, KG,a

UTILITIES REQUIRED

Compressed air supply at 2 Bar, 4 CFM

Water supply, drain.

Required Chemicals and Laboratory Glassware.

A CO2 cylinder with Pressure Regulator and Pressure gauges is supplied with the set up.

DESCRIPTION

The set up consists of a glass column packed with Rasching rings. Liquid is fed at the top of
the column through distributor. The gas and air are measured separately, mixed in a mixing
chamber and then passed through the packed column vertically upward and absorbed in liquid.
All the flow rates can be independently varied to simulate different conditions. Samples can be
taken out from the sampling point at the bottom of the column for analysis.

THEORY

In absorption, a gas mixture is contacted with a liquid for preferential dissolution of one or
more components of the gas in liquid. Such operation requires transfer of mass from gas stream
of the liquid. In many industrial applications the absorption process is accompanied by
chemical reaction usually, reaction in the liquid of the absorbed component with a reagent in

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the absorbing liquid takes place. The reagent and the product of reaction may be soluble e.g.
absorption of CO2 into an aqueous solution of ethanol amines or other alkaline solutions.

Reactions of the absorbed solute provides higher absorption rates due to:

I. Destruction of the absorbed solute as it forms a compound reduces the equilibrium

partial pressure of the solute that in turn increases the concentration difference between
the bulk phase and the interface.
II. Increase in liquid phase mass transfer coefficient.
In case of absorption in a packed column of cross-sectional area, s, neglecting the
change in molar feed rate of gas, V, the amount of solute absorbed in section dz is:

-Vʹdy = Kya(y-y*) Sdz…………………………………… (1)

Integration yields:
Ky ∫ Ky
= = ∫ 𝑑𝑦/(𝑦 − 𝑦 ∗).................... (2)
𝑍 = 𝐻 +𝑁 Vʹ-molar flow rate of gas. kgmol/h
y a = kgmol/m2-h

where Noy =∫ 𝑑𝑦/(𝑦 − 𝑦 ∗)…………………………..(3)

/
Hoy = ……………………………...……….(4)

In case of absorption with chemical reaction, (eg CO2 absorption in NaOH solution),
The equilibrium P.P.is zero (y*= 0) (if reaction is irreversible)

Noy =∫ 𝑑𝑦/𝑦 = ln yb/ya ………………………………...……...(5)

Hoy = ZT/ Noy ……………………………………………..……(6)

But
/
Hoy = =

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 /
Kya = = …………………………………………(7)

And KG a= Kya/P
(1) Estimate numbers of transfer unit ,(NTU) , Noy , using eq.5.

(2) Estimate height of transfer unit, (HTU), Hoy , using eq.6.

(3) Plot KG a (kgmoles/m3-h-atm) vs mass velocity of liquid, L (kgmoles/m3-h) on log-
log plot for the given packing ,using eq7.

EXPERIMENATAL PROCEDURES:

1. Make 2N (aq.) NaOH solution by dissolving 1600 gms NaOH pellets in 20 ltrs
water.
2. Titrate the above solution with 1N HCl taking methyl orange indicator.
3. Fill the above solution into the respective tank and connect the CO2 &
compressed air supply to the equipment.
4. Record column diameter, Packed height and Packing type and size.
5. Start filling the column with any NaOH flow rate when it comes from the outlet
start passing (CO2 + compressed air) mixture into the column providing pr.
should be less then 1 Kg/cm2.
6. After twice the residence time or 10 min, which is greater take 20 ml, sample
& titrate 10 ml sample with 1N HCl taking indicator phenolphthalein + BaCl 2
& another 10 ml with methyl orange.
7. Take more than two samples for accuracy.
8. Drain the column and repeat the steps from 4 to 7 for another flow rate.

STANDARD DATA:

Column = Borosilicate Glass Dia 55 mm. Length 750 mm Packing

= Borosilicate Glass Rasching Ring size 8-10 mm.

Feed circulation = By compressed air

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Pressure Regulator = 0-2 kg/cm2

Pressure gauge = Bourdon type, 0-2 kg/cm2

Feed tank = Material Stainless Steel 304 grade, Capacity 20 Ltrs.

Flow measurement = Rotameters (one each for feed, air and CO 2)

Collecting tank = Materials Stainless Steel 304 grade, Capacity 10 Ltrs.

FORMULAE:

I.D. of the column = Dc

𝜋 2
Total effective contact volume = Ve = 𝐷 ℎ
4 𝑐

TITARTIONS:

Volume of sample (NaOH solution in which CO2 is absorbed) = V= 10 ml.

Aq.NaOH feed rate:

L =………...LPH =………………..m3/sec at inlet

Air rate =..............LPM =…………………m 3/sec

CO2 feed rate =…….....LPM =…………………m 3/sec

%CO2 in feed =……%

NaOH Conc. at outlet:

Vol. of sample for each titration = V =10 ml

Vol. of 1N HCl used (Methyl Orange as indicator) = T1, ml

Vol. of fresh sample taken for titration =V, ml

Vol. of 1N HCl used (Phenolphthalein as indicator) + 25 ml of BaCl 2 = T2, ml

Conc of (NaOH)o at outlet = T2/V , gmole/L

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Conc of Na2CO3 = (T1-T2)/(2V) ,gmole/L.

Conc of NaOH at inlet = (NaOH)i , gmole/L.

Amount of CO2 absorbed = (1/2)[(NaOH)i-(NaOH)o],gmole/L.

Amount of CO2 absorbed in k mole/sec = Amount of CO2 absorbed, gmole/L × FL

RCO2 = Amount of CO2 absorbed in, (kmole/m3) × FL (m3/sec)

= ….…, K mole/sec

Molar volume at 27 ° C =………… L/gmole (using the gas equation)

22.4 × (273.15 + 27°C)

V2 = = 24.63 L/gmole
273.15

=24.63 m3/kmole

Vol of CO2 absorbed = RCO2 K mole/sec × Molar volume at room temperature

=…..m3/sec

CO2 flow rate at inlet =….LPM/ (1000×60)

=….m3/sec

CO2 flow rate at outlet = CO2 flow rate at inlet – Vol of CO2 absorbed

Qo =…….m3/sec

pp of CO2 at outlet = 𝑃𝑡

po = ….. atm

(air flow rate = ……LPM = 5×10-0.4 m3/sec)

CO2 feed rate

pp. of CO2 at inlet =
CO2 feed rate + air feed rate

pi =……..atm.

ΔPln =

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 = …….atm.
NA = KG.a.Ve.( ΔPln )
KG.a = KG.a × PT = Gas film coefficient, kmole CO2 transferred /m3/h
NA = moles of CO2 transferred per unit time = kmole/h = RCO2
KʹGaVe = NA/ ΔPln = RCO2/ ΔPln
PT = 1 atm =………kmole/s-atm =…….kmole/h-atm
Effective volume = Ve =…….m3
KGa = po × PT
=KʹG a/ Ve , kmol/h-m3

OBSERVATION AND CALCULATIONS:-

Room Temp = T

Atmospheric pressure = P
Column diameter = Dc
Total packed height = ZT
Type of packing = Rasching Ring
Packing dimensions =
Cross Sectional Area of Colum (S) =π/4 Dc2, (m2)
Surface area of one packing=
Total surface area per unit volume of packing =
Gas flow rate = Q, m3/h
Gas Av.mol wt.= Mg ,kg/kgmol
Gas density = ρg , kg/m3
(at Pr , PT, Temp T)
Gas mass velocity = V
= Q ρg / MS kg mol/h-m2
Liquid flow rate = l, m3/h

Liquid density = ρl

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Liquid molecular weight= Ml
So liquid mass velocity. L = l ρl/MlS kgmol/h-m3
Mole fraction of CO2 in inlet gas = ya
Mole fraction of CO2 in outlet gas = yb.
Using equation (5), calculate, Number of transfer unit , Noy.

Using equation (6), calculate, Height of transfer unit, Hoy.

Using equation (7), calculate, overall mass transfer coefficient, Kya.

Repeat these calculations for at least five different values of L.

Plot Kya vs. L on a log log plot for the given packing.

Repeat the experiment for 5 different gas rates changing the inlet conc. of CO2.

Correlate Kya or KGa with V and L.

KGa = const. Va Lb

Using regressions techniques determine the values of constant and exponents a and b.

Also express the experimental data in the film

Sh = Cl Rea Scb

Or Plot Sh/Sc1/3 vs Re

Or Sh/Sc2/3 vs Re

Compare the observed values of Kya with that obtained from some empirical models.

Make an effort to determine the enhancement factor φ , for CO2 –H2O-NaOH system. It ranges
from 1 to 1000 or more.

The range of Kga for CO2 –H2O-NaOH system may be in the range of 1-4 mole/ft3-atm-h.

For CO2 –H2O system Kga may be in the range of 0.05 to 0.2 mole/ft3-atm-h.

CALCULATION:

Conc. of NaOH solution = 800 g/10 L = 2 gmole/L

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 = 2 kgmole/m3

Liquid flow rate =……………….LPH

Run No.1: CO2 + Air

Liquid flow rate = ……..g/min =…..g/sec

= …..kg/sec

Density of NaOH sol.= ……g/ml

=…….m3 (Measured by using Sp. Gravity bottle)

Liquid flow rate (L) =……m3/sec

Liquid velocity =………m/s

%CO2 in feed:

CO2 =…..LPM

Air =……LPm

TITRATION:

Vol. of sample = V = 10 ml

Vol. of 1N HCl used (Methyl Orange as indicator) = T1, ml=…..ml

(End point Orange colour change into light red colour for methyl orange & pink colour into
colourless solution for Phenolphthalein).

Vol. of 1N HCl used (Phenolphthalein as indicator) + BaCl2 = T2, ml = 10 ml

Conc of (NaOH)o at outlet = T2/V = 10/10=1

Conc of Na2CO3 = (T1-T2)/(2V) =…….

Conc of NaOH at inlet = (NaOH)i =……/10=…….

Amount of CO2 absorbed kmole/m3 of liquid = (1/2)[(NaOH)I - (NaOH)o],kmole/m3

Amount of CO2 absorbed in kmole/sec =RʹCO2 =…..(kmol/m3)×(m3/sec)liquid

= RʹCO2=…..kmol/sec

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Rate of absorption of CO2 per unit vol. of packed tower = −s
.

RʹCO2 =……………………………Kmole/m 3-s.

Vol. of packed tower = (π/4 d2 ×Z) = π/4 (50×10 -3)2 ×82×10-2 =1.61×10-3 m3

Vol. of CO2 absorbed =…………..kmol/s × molar volume (m3 /kmol)

Molar volume at 27°C = 24.63 L/gmole = 24.63 m3/kgmol (using the gas equation)

22.4 × (273.15 + 27°C)

𝑉 = = 24.63 L/gmole
273.15

Vol. of CO2 absorbed =……kmole/sec × 24.63 m3/kgmol

=…….m3/sec

CO2 flow rate at inlet =……LPM =…….m3/sec

CO2 flow rate at outlet= θf =…….m3/sec

p.p. of CO2 at outlet = × PT

ΔPln = =……………

Overall volumetric mass transfer coefficient:

KʹGa = NA/ZACPT(Δy) = NA/ZAC(Δp) [ pi = yi PT]

[y] = pi/PT]

KʹGa = kmole/m3- h - atm

( )𝑃𝑇
ΔPln = =

KʹG.a. PT = KG.a = kmole/m3-h [(Δp)L=(Δy)LPT ]

KG.a = ……….kmole/h-m3

KʹG.a =……….lbml/h-ft3-atm

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Ya =………….

Yb =…………….

Hoy = ZT/Noy

But

Hoy = =…………..m4/kgmol
.

Noy =…………………kgmol/m3

PRECAUTIONS AND MAINTENANCE INSTRUCTIONS:

1. Always use clean or distilled water for making feed solution.

2. Clean the packed column after conducting the experiments just passing the clean water
into that.
3. Drain the column and feed tank of NaOH.
4. Don’t slide the equipment during shifting chances of glass accessories broken are more.
5. Close the CO2 cylinder after use.

TROUBLE 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 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 or Rotameter)

REFERENCES:

1. Unit Operations of Chemical Engg., W.L. Mc Cabe, J.C. Smith and P. Harriott, Mc
Graw Hill.
2. Mass transfer, T.K. Sherwood, R.L. Pigford and C.R. Wilke, Mc Graw Hill.
3. Gas- Liquid Reactions, P.V. Danckwerts, Mc Graw Hill.

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ABSORPTION WITH CHEMICAL REACTION IN A PACKED
BED

(CO2 absorption in NaOH solution)

SAMPLE CALCULATION:

Conc. of NaOH solution = 800g/10 L = 2 gmole/L = 2 kgmole/m3

Liquid flow rate = 10.56 LPH

Run No. 1: CO2 + Air

Liquid flow rate = 190 g/min =3.1667 g/sec = 3.1667×10-3 kg/sec

Density of NaOH sol. = 1.08 g/ml = 1080 kg/m3 (Measured by using Sp. Gravity bottle)

Liquid flow rate (L) = 3.1667×10-3 /1080

= 2.93213×10-6 m3 /sec

Liquid velocity = 2.93213×10-6 m3 /sec/1.9678 ×10-3 m2

= 0.00149 m/s

%CO2 in feed:

CO2 = 5 LPM CO2 = 5/(5+30) = 0.14286

Air = 30 LPM

TITRATION:

Vol. of sample = V = 10 ml

Vol. of 1N HCl used (Methyl Orange as indicator) = T1(ml).= 18.9 ml

(End point Orange colour change into light red colour for methyl orange & pink colour into
colourless solution for Phenolphthalein).

Vol. of 1N HCl used (Phenolphthalein as indicator) + BaCl2 = T2(ml) = 10 ml

Conc of (NaOH)o at outlet = T2/V = 10/10=1

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Conc of Na2CO3 = (T1-T2)/(2V)

= (18.9-10)/(2×10)

= 8.9/2.0 = 0.445

Conc of NaOH at inlet = (NaOH)i = 19.6/10= 1.96

Amount of CO2 absorbed kmole/m3 of liquid = (1/2)[(NaOH)i - (NaOH)o], kmole/m3

= (1/2)[1.96-1]= 0.96/2 = 0.48 kmole/m3

Amount of CO2 absorbed in kmole/sec =RʹCO2 = 0.48 (kmol/m3)×(m3/sec)liquid

= R’CO2= 0.48 × 2.9321×10-6 kmol/sec

= R’CO2 = 1.40741× 10-6 kmol/sec

= R’CO2 =…..kmol/sec

Rate of absorption of CO2 per unit vol. of packed tower = −s

.

. ×
R’CO2 = = 8.741 ×10-4 Kmole/m3-s.
. ×

Vol. of packed tower = (π/4 d2 ×Z) = π/4 (50×10 -3)2 × 82 ×10-2 = 1.61×10-3 m3

Vol. of CO2 absorbed =1.40741×10-6 kmol/s × molar volume (m3 /kmol)

Molar volume at 27°C = 24.63 L/gmole = 24.63 m3/kgmol (using the gas equation)

22.4 × (273.15 + 27°C)

𝑉 = = 24.63 L/gmole
273.15

Vol. of CO2 absorbed =1.40741×10-6 kmole/sec × 24.63 m3/kgmol

= 3.4663×10-5 m3/sec

CO2 flow rate at inlet = 5 LPM =3.4663×10-5 m3/sec

CO2 flow rate at outlet = θf =8.333×10-5 - 3.4663×10-5 m3/sec

= 4.867 ×10-5 m3/sec

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p.p. of CO2 at outlet = × PT

. ×
p.p. of CO2 at outlet = × 1 atm = 0.08874 atm
. × ×

. ×
p.p. of CO2 at inlet = × 1 atm = 0.14285 atm
. × ×

. .
ΔPln = = . = 0.11365 atm
( )
.

Overall volumetric mass transfer coefficient :

KʹGa = NA/ZACPT(Δy) = NA/ZAC(Δp) [ pi = yi.PT]

[y] = pi/PT]

KʹGa = kmole/m3-h-atm

( )
ΔPln = =

KʹG.a. PT = KG.a. = kmole/m3-h [(Δp)L = (Δy)LPT ]

KG.a = ( 8.741×10-4 ×3600) × (1 atm/ 0.11365 atm )

KG.a = 27.69 kmole/h-m3

KʹG.a = 1.725 lbml/h-ft3-atm

Ya = 0.142857

Yb = 0.08874

Hoy = ZT/Noy

But

𝑉 . ×
Hoy =
𝐾𝐺 .a
= = 0.19372 m4/kgmol
.

Noy = 0.82 / 0.19372 = 4.23 kgmol/m3

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