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BUDAPEST UNIVERSITY OF TECHNOLOGY AND ECONOMICS

DEPARTMENT OF BUILDING SERVICE ENGINEERING AND PROCESS ENGINEERING

ABSORPTION
/measurement description/
AIM OF THE MEASUREMENT

In the course of the laboratory measurement, the students can get acquainted in
practice with one of the most frequently applied mass transfer processes, absorption,
as well as the process equipment (absorber), the operational parameters (and the effect
of their change), and the typical problems during industrial application.

MEASUREMENT TASKS

• measurement of the hydrodynamic parameters of the apparatus,


• investigation of the mass transfer parameters of the process,
• plotting of the specific pressure drop with respect to packing height
 ∆p column 
  as a function of gas velocity (v air ) in the column for different liquid
 H 
loads and without liquid load on a log-log plot,
• determination of the number of transfer units (N OG ) and the height equivalent
to one transfer unit (H OG ) ,
• determination of concentration (Yin , Yout , X out ) ,
• determination of the error of mass balance,
• determination and plotting of the operation line and equilibrium curve (based
on literature data),
• evaluation of the results, comparison with literature data.

THEORETICAL BACKGROUND

Gas absorption or simply absorption is a separation method, where a chosen


component (or components) of a gaseous mixture is absorbed (solved) in a liquid (the
absorbent). This means that it is possible to remove components from a gas with the
aid of a liquid by contacting the gas phase with the liquid phase.

The most typical equipment of absorption processes are the tray and the packed
columns. In the measurement, a packed column is used. From a mechanical
engineering point of view, absorbers usually have a simple construction. Their
structural material depends on the medium, the operating pressure, and on the
temperature. For the sizing or selection of the equipment, the flow rate of the gas, its
inlet and prescribed outlet composition has to be known. Knowing the component to
be separated, the solvent has to be selected, then the dimensions of the equipment
(height, diameter) can be determined.

The more intensive the gas-liquid contact, the better the diffusion, and thus the
absorption of gaseous components. The efficiency of the absorption depends also on
the velocity and flow rate of the gas and the liquid, and on the type, size and material
of the packing applied, as well.

By investigating the hydrodynamic properties of the packing, we can distinguish


several regions (Figure 1) with the changing of the gas-liquid ratio.

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Figure 1. Pressure drop of packed column.

• below point „A”

region of free flow: in the case of low liquid and gas loads, liquid is only dripping,
mass transfer is very poor, the concurrent phases are clearly discernible,
laminar region: on the increase of gas load, the liquid flows round the packing
laminarly, poor heat and mass transfer,

• between points „A” and „B”:

turbulent region: the further increase of gas load results in the formation of turbulent
flow, intensive phase contact, good heat and mass,

• above point „B”:

flooding region: the velocity of gas continues to increase, the liquid builds up , the
pressure drop increases more steeply, heat and mass transfer deteriorate.

The optimal operation condition of the column is between points „A” and „B”.

DESCRIPTION OF THE MEASUREMENT (Figure 2)

a. Hydrodynamic investigations

In the course of the measurement, we investigate the pressure drop of a column


packed with Raschig rings (½”, ceramics) by changing the gas velocity, first without
liquid, then at different liquid flow rates.

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First, we measure the pressure drop of the orifice plate and that of the dry column
by U-tube manometers. We change the velocity of gas by adjusting the throttle valve
mounted on the blower, and we note down the values of pressure drop. The aim of the
measurement is the investigation of the hydrodynamic properties of the packing.

The next measurement is conducted as above, but a constant liquid flow rate is
applied. During the measurement, the increase in the liquid level in the column and
the transition between laminar and turbulent region can be observed as the flow rate
of gas is changed (the velocity is increased). We follow the changes in the pressure
drop of the orifice plate and that of the column during the measurement.

b. Investigation of mass transfer

In the second part of the laboratory practice, we measure the ammonia (NH3)
content of the gas entering and leaving the column at the predefined liquid load (in the
laminar and in the turbulent region, that is, at different gas velocities, if possible). If
the NH3 content of every stream (Yin , Yout , X out ) is determined by measurement
(Figure 3.), the error of mass balance can be calculated.

The concentration of NH 3 is determined by a gas analyser (Figure 2).

During the laboratory practice, if possible, we perform the measurement for two
different liquid loads at constant gas velocity. The ammonia content of the inlet gas is
kept constant. We register the temperature of the inlet and outlet gas during the
measurement.

Figure 2. The flow-sheet of the measurement equipment


in the case of using the gas analyser.

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By using the data measured, the values and plots characterising the equipment and
the actual operating points can be determined.

FORMULAE NECESSARY FOR EVALUATION

The fundamental equation of our calculations is the material balance of ammonia:

G air ⋅ Yin + L water ⋅ X in = G air ⋅ Yout + L water ⋅ X out

The NH 3 content of the liquid entering the column is negligible, so using that
X in ≅ 0 the formula is simplified:
G air ⋅ (Yin − Yout ) = L water ⋅ X out ,

 kmol 
where L water : molar flow rate of water  ,
 s 
 kmol 
G air : molar flow rate of air  ,
 s 
 kmol NH 3 
X : mole ratio of NH3 in the liquid  ,
 kmol H 2 O 
 kmol NH 3 
Y : mole ratio of NH3 in the air  .
 kmol air 

If all the variables are known, the error of the mass balance can be calculated:
G air ⋅ (Yin − Yout ) − L water ⋅ X out
h= ⋅ 100 %
G air ⋅ (Yin − Yout )

DETERMINATION OF THE MOLAR FLOW RATE OF AIR

Determination of the pressure drop measured on the orifice plate:

∆p op = ρ water ⋅ g ⋅ ∆h op ,
 kg 
where ρ water : density of the measuring liquid (water)  3  ,
m 
 m
g : gravitational acceleration  g = 9,81 2  ,
 s 
∆h op : difference in levels [m] .

The flow rate of the inlet gas is the sum of two flow rates (that of the solvent and
that of diffusing component):

G = GS + G D ,
in our case: G = G air + G NH3 .

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As ammonia is only present in low concentration, we can use the following
simplifying assumptions:

ρ gas ≅ ρ air , and M gas ≅ M air , and so: G ≅ G air ,


 kg 
where M: molar mass  .
 kmol 

Determination of the volumetric flow rate of air:

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d op π 2∆p op
& = αε
V ,
4 ρ air

& : volumetric flow rate of air  m  ,


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where V  
 s 
α : discharge coefficient (for the actual case α ≅ 0.62 ),
ε : expansibility factor (ε = 1) ,
d op : diameter of the orifice plate (d op = 0.025m ) ,
∆p op : pressure drop on the orifice [Pa ] ,
 kg 
ρ air : density of air  3  , from table as a function of the temperature
m 
measured, or calculated if atmospheric pressure is known.

 kg 
The mass flow rate   can be determined from the volumetric flow rate:
s 
m& =V&ρ ,
air

 kmol  &
m
from which the molar flow rate  : G= ,
 s  M air

 kg 
where M air is the molar mass of air  M air = 29 .
 kmol 
.
DETERMINATION OF THE MOLAR FLOW RATE OF WATER

water ρ water  kmol 


V&
L water =  s ,
M water  
&  m3 
where V water : volumetric flow rate of water  ,
 s 
 kg 
ρ water : density of water  3  ,
m 
 kg 
M water : molar mass of water  M water = 18 .
 kmol 

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DETERMINATION OF CONCENTRATIONS

The concentrations in the gas (Yin , Yout ) can be determined by the gas analysers
(Figure 2).

By using the gas analysers, the NH3 content of the inlet and outlet gases
(Yin , Yout ) can be read off the instrument. The gas analyser has to be calibrated before
the measurement.

Xout is measured by titration of the outlet liquid. By using a small hose, the outlet
liquid is slowly led from the liquid seal into a beaker containing 0.1 mol/dm3
hydrochloric acid (HCl) solution and a few droplet of phenolphthalein solution. One
mole of ammonia reacts with one mole of acid in the following reaction:

NH 3 + HCl → NH 4 Cl

The product of the reaction is of neutral pH. This means that pH of the solution is
also neutral if the molar amount of NH3 added to the solution equals the molar amount
of HCl it originally contained. Phenolphthalein was added to the solution to indicate
the change in pH value, as it is colourless in acidic but purple in basic solutions. The
outlet liquid has to be added into the beaker just until the appearance of a purple hue.
The measurement has to be repeated three times.

The NH3 content can be determined by measuring both the mass of the HCl
solution (macid, including phenolphthalein) and that of the liquid added (mliquid).

The molar amount of NH3 which equals that of HCl, by using that ρHCl≈ρwater is:
m
n NH 3 = n HCl = 0.1Vacid = 0.1 acid ,
ρ water
where n: molar amount of NH3 and HCl, respectively [mol],
Vacid: volume of HCl solution [dm3].

The molar amount of water ( n water ) in the liquid sample:


m liquid − n NH3 M NH3
n water = ,
M water
 g 
where M NH3 : molar mass of ammonia  M NH 3 = 17.03 .
 mol 

The ammonia content of the outlet liquid is:


n NH3
X out =
n water

CALCULATION OF THE NUMBER OF TRANSFER UNITS AND THE HEIGHT EQUIVALENT TO


ONE TRANSFER UNIT (Figure 4)

The mass transfer on the contacting surface dA :

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(
d(G air Y ) = K y Y − Y * dA )
According to the definition of the effective interfacial mass transfer area per unit
volume:

dA dA
a= = ,
dV A 0 dH

by using the above equation:

( )
G air dY = K y Y − Y * aA 0 dH

H=H Ybe
G air dY

H =0
dH =
K y aA 0 ∫ Y−Y
Yki
*
= H OG ⋅ N OG

Figure 4. Operating line and equilibrium curve

(At low concentrations, we can assume that y ≅ Y .)

The number of transfer unit in a closed from, if both the operating line and the
equilibrium curve can be considered linear:

Yin − Yout
N OG = ,
∆Y1* − ∆Y2*
∆Y1*
ln
∆Y2*

where N OG : number of overall gas-phase mass-transfer units,


∆Y1* : the higher mole ratio difference,

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∆Y2* : the lower mole ratio difference.
The number of transfer unit:

Yin
G dY H
H=
K y aA 0 ∫
Yout Y−Y *
= H OG ⋅ N OG ⇒ H OG =
N OG
,

where H : packing heigth (H = 0.6 m ) ,


Y * : equilibrium mole ratio,
H OG : height of one overall gas-phase mass-transfer unit,
 kmol 
K y : Overall gas-phase mass-transfer coefficient  2  ,
m s
 π (0.13 m ) π 
2
d2
A 0 : cross-section of the column  A 0 = column = ,

 4 4 
 m2 
a : effective interfacial mass transfer area per unit volume  a = 400 3  .
 m 

REPORT ABOUT THE MEASUREMENT

The report of the measurement has to contain the followings:


- Description of the equipment and a sketch about it,
- Data measured in a table (level differences in the manometers, temperatures,
concentrations, data of titration),
- Data calculated:
- molar flow rate of air and water, gas velocity, pressure drop of the
orifice plate and that of the column,
- NH3 content of the outlet liquid (Xout),
- error of the mass balance
- number of transfer unit and the height equivalent of one transfer unit.
- Plots:
- specific pressure drop of the column as a function of gas velocity
(logarithmic scale)
- the operating line and the equilibrium curve
- Observations, conclusions.

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DATA OF THE UNITS OF MEASUREMENT EQUIPMENT

Gas analyser (1)


Type: Hartmann & Braun Advance Optima (with URAS 14 module)
Serial number: 123-008227

Rotameter for adjusting water flow rate (2)


Type: UNIROTA KM03
Serial number: 95-271-1727

Rotameter for adjusting NH3 flow rate (3)


Type: UNIROTA 95-271-100
Serial number: 64-712-800

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Thermometer (4)
Type: Testo 110
Serial number: 037392

Column (5)
Diameter: d oszlop = 0.13 m
Packing height: H = 0.6 m
Packing: ½” Raschig ring (ceramics)
m2
Effective interfacial area: a = 400 3
m

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PHYSICAL PROPERTIES OF AIR AT 1 BAR

T ρ c λ
o
C kg / m 3 kJ / kgK W / mK
0.0 1.252 1.011 0.0237
10.0 1.206 1.010 0.0244
20.0 1.164 1.012 0.0251
30.0 1.127 1.013 0.0258
40.0 1.092 1.014 0.0265
50.0 1.057 1.016 0.0272
60.0 1.025 1.017 0.0279
70.0 0.996 1.018 0.0286
80.0 0.968 1.019 0.0293
90.0 0.942 1.021 0.0300
100.0 0.916 1.022 0.0307

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