Professional Documents
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Lectures
19.11.2013
P 09
26.11.2013
P 10
03.12.2013
P 11
Exercises
19.11.2013
Assignment date
26.11.2013
C 10
03.12.2013
C 11
10.12.2013
C 12
13.12.2013
Due date
In the previous analysis, we have assumed that the vapor leaving each stage was in equilibrium with
the liquid leaving the same stage. However, in practice, the trays are not perfect, i.e. there are deviations from ideal conditions. The assumption of thermal equilibrium is reasonable, but the assumption
of equilibrium with respect to the mass transfer is seldom justified due to:
insufficient time of contact between the liquid and vapor phases
insufficient degree of mixing of the both phases (the presence of stagnant zones on largediameter distillation trays)
the effects of entrainment and weeping.
To determine the actual number of trays required for a given separation, the number of theoretical
stages must be adjusted with a overall column efficiency and a safety coefficient:
Neff
Nth s
2 Nth
EOV
Neff
Nth
EOV
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 3 |
The overall column efficiency EOV depends on the geometry and design of the trays, flow rates and flow
paths of vapor and liquid streams, compositions and properties of both phases. Values of EOV can be
predicted by comparsion with performance data from industrial columns for similar systems, by use of
empirical correlations or semitheoretical tray models or by scale-up from laboratory data. Guideline
values are:
Tray Type
Tunnel Tray
Sieve Tray
Valve Tray
0,5 0,7
0,6 0,8
0,7 0,8
0,7 0,9
EOV
The Murphree tray efficiency Ej that describes the separation achieved on individual tray j is usually
based on the vapor phase:
Ej
y% y%j 1
Separation effect of the actual stage
a
*j
1
Separation effect of the theoretical stage y%j y%j 1 b
y%j 1
x%j 2
y%
Equilibrium
Curve
j+1
z
y%j
x%j 1
j
y%j 1
Operating Line
*
y%
j
y%j
x%j
y%j 1
j1
y%j 2
x%j 1
x%j
x%j 1
x%
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 4 |
Once the overall column efficiency EOV is known, it can be used on the McCabe-Thiele graphical me-thod
in the form of a pseudo-equilibrium curve. In stepping off stages, the overall vapor-side effi-ciency EOV
= a/b, can be used to dictate the percentage of the vertical distance taken from the operating line to
the equilibrium curve. Following the staircase construction between the pseudo-equilibrium curve and
the operating lines the number of actual stages Neff required for the given separation is determined:
1
b
y%
EOV
a
Operating lines
e.g., for
x%
B
x%
x%
D 1
Nth s
4
EOV
The height of trayed portion of column H and the column height Htot, required to meet the product
specifications, are
H Neff z
Nth s
z
EOV
Htot H Hmin H 3 z
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 5 |
Tray columns can only be operated within certain limits of gas and liquid flow. The operating region of a
tray column can be represented in a diagram with x-coordinate
and
y-coordinate . Often
these two
V&
V&
G
L
loads are referred to the active area Aac. The upper borders for the gas and liquid flow (bold lines) are
absolute borders that can never be crossed without causing mechanical damages. The lower bor-ders
(dashed lines) may be exceeded to a certain extent without encountering any flow problems. However the
mass transfer efficiency may gradually decrease. The shape and size of the operating re-gion depends on
the design parameters. The operation point should be chosen so that a sufficient sa-fety margin to the
operation limits remains.
&
VL height
Froth
Entrainment
Operating region
D
Downcomer
capacity
Minimum crest
over weir
Weeping
Aac
As described below the gas and liquid loads has to be kept between a maximum and a minimum value.
Therefore, four limitations can be defined:
at low gas velocities either the gas no longer flows uniformly though
all the tray openings (bypassing part of the tray) or the liquid leaks
though the tray (weeping)
both modes of operation should be avoided due to tray efficiency
losses because of insufficient degree of mixing of the both phases
the main factor that affects weeping is the hole diameter (the
minimum gas load increases with increasing hole diameter)
at high gas velocities the gas blows the liquid off the tray in form of
fine droplets (entrainment, jet flood)
the liquid flows no longer countercurrently to the gas, and proper
column operation ends
the maximum feasible gas load depends on system properties (density of gas and liquid, surface tension) as well as on tray design
entrainment flooding of trays is decisive at very large tray spacings
z, for smaller tray spacings z the froth height on the tray sets a
lower limitation
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 7 |
Minimum Liquid
Load:
V&
L
hl
hwo
V&
G
lw
exceed
should not
Ideally, the column is operated in the range of 60 to 90 % of the flooding vapor velocity.
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 8 |
3
1
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 9 |
2
2
3
3
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 10 |
The tower diameter and, consequently, the cross-sectional area of the column must be sufficiently
large to handle the gas and liquid rates within the operating region. The diameter of a distillation
column is generally controlled by the vapor velocity.
For designing a column the vapor velocity of the inside cross-sectional area of the empty tower is
used. The vapor flows vertically upward usually at velocity from 0,5 to 2,5 m/s, and from 3 to 6 m/s in
bubble-cup or tunnel tray columns. In contrast, the downflow velocity range of the liquid is from 110-3
to 1510-3 m/s.
The required free cross-sectional area of the column is determined using the maximum vapor volumetric flow rate during the operation and the allowable vapor velocity referred to the total column crosssectional area:
AQ
&G max
V&
m
N&
MG
Di 2 G max
G max
4
wG zul
G wG zul
G wG zul
AQ
Di
V&
G max
w
&GG max
m
zul
N&G max
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 11 |
AQ
N&G max MG
G wG zul
Assuming ideal gas behavior for the vapor phase, the average vapor density can be substituted:
&
m
N&
M
p MG
G &G G max& G
R T
VG
VG
Thus, the column internal diameter at a given operating pressure and operating temperature is:
Di
where Di [m],
N&G max R T
N&
T
102, 89 G max
p wG zul
p wG zul
[kmol/s],
T [K], p [Pa], wG zul [m/s]
N&G max
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 12 |
The allowable vapor velocity referred to the total column cross-sectional area wG zul depends mainly on
the tray type and its geometry, on the liquid load, and on the physical properties of the both phases.
The usual design limit is entrainment flooding, which is caused by excessive carry-up of suspended
liquid droplets by rising vapor to the tray above. At low vapor velocity, a droplet settles out; at high
vapor velocity, it is entrained. At flooding velocity wG max, the droplet is suspended such that the vec-tor
sum of the buoyant force FA, drag force FW, and gravitational force FG acting on the droplet will be zero.
From the balance of forces at a liquid doplet and a safety margin (fraction of flooding) results the
allowable vapor velocity wG zul referred to the total column cross-sectional area:
A
wG zul f wG max 0,7 ac kV
AQ
G
L
G
wL
FA
FW
z
Two-phase
Layer
wG max
FG
kV
capacity parameter of
Souders/Brown [m/s]
Aac
AQ
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 13 |
tray spacing
liquid surface tension
pst
pdyn
The first term in the equation above accounts for the liquid head on a tray, the second term refers to
the dry pressure loss of the tray, the third term is small compared with pcol and is usually negligible.
Due to the numerous variables such as tray geometry, physical properties of vapor and liquid, gas and
liquid loads, operating pressure, etc. a general equation to calculate the columns pressure drop has
not yet been developed. In most cases, the pressure drop must be found depending on the tray type
experimentally.
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 14 |
The hydrostatic pressure drop of liquid pst depends on the mass of the clear liquid inside the column,
as given by:
pst
mL g
AQ
mL
AQ
For tray columns the hydrostatic pressure drop is given by the sum of the pressure drops across the
trays:
pst Neff S g h
S
N
eff (1
) L g hS
Neff
hS
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 15 |
The pressure drop due to the friction for vapor flow up the column pdyn can be expressed approximately by:
pdyn
G wG2
2
wG
The orifice coefficient depends on the type and geometry of the column internals, and on the surface
tension of the liquid. In tray columns, the orifice coefficient can be taken from:
Neff B
B
If the column is operated at 85 % of the flooding vapor velocity, the pressure drop per tray is, depending on tray type, approximately from 2 to 8,5 mbar.
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 16 |
With the availibilty of economical and efficient packings, packed towers are finding increasing use in
new distillation processes and for retrofitting existing trayed towers. They are particularly useful in
applications when the separation is relatively easy and the required column diameter is not very large,
where pressure drop must be low, as in low-pressure distillation, and where liquid holdup must be
small, such as when separating heat-sensitive materials whose exposure to high temperatures must be
minimized.
Packed columns are continuous, differential-contacting devices that do not have the physically distinguishable, discrete stages found in trayed towers. Thus, packed columns are better analyzed by masstransfer models than by equilibrium-stage concepts. However, in practice, packed-tower performance
is often presented on the basis of equilibrium stages using a packed height equivalent to a
theoretical plate, called the HETP and defined by the equation
HETP
Packed height
H
Values of the HETP depend mainly on packing type and size, liquid viscosity, surface tension, and
operating conditions. In the absence of detailed information on the HETP, following rough approximations are sufficient: HETP 0,6 m for random packings, HETP 0,3 m for structured packings.
The required height of the packing within the column H and the total height of the column Htot are:
(0,5...1 m) + (1...2 m)
H Nth HETP with HH
min
tot H Hmin
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 17 |
For rough estimates of the HETP the following relations can be used (all values are in ft,
1 ft = 0,3048 m)
1. Random packings of second and third generation with low-viscosity liquids
HETP 1,5 dP dP nominal packing diameter [in] (1 in = 25,4 mm)
2. Structured packings at low-to-modarate pressures with low-viscosity liquids
HETP
100
0,333
a packing surface area per packed volume [ft/ft]
a
100
0,333
a
Type Packing
Material
Nominal
Diameter
dP [in]
Packing
Factor
FP [ft/ft]
Raschig rings
Ceramic
1,0
2,0
3,0
157
58
33
Raschig rings
Metal
1,0
2,0
3,0
165
71
40
Intalox saddles
Ceramic
1,0
2,0
3,0
92
30
15
Intalox saddles
Plastic
1,0
2,0
36
25
Pall rings
Metal
1,0
1,5
2,0
3,5
56
29
27
16
Pall rings
Plastic
1,0
2,0
3,5
53
25
15
Sources: W. D. Seider et al.: Product and Process Design Principles. 3. Aufl., John Wiley, Hoboken 2010;
Vereinigte Fllkrper-Fabriken GmbH & Co. KG., Ransbach-Baumbach
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 19 |
Packing
Material
Size
[mm]
Packing
Factor
FP [ft/ft]
Mass-transfer Surface
Area per Unit Volume
a [m/m]
Void Fraction
[-]
Random Packings
Hiflow rings
Ceramic
Metal
Plastic
50
50
50
29
16
20
89,7
92,3
117,1
0,809
0,977
0,924
Nor-Pac rings
Plastic
Plastic
Plastic
50
35
15
14
21
86,8
141,8
311,4
0,947
0,944
0,918
Tellerettes
Plastic
25
40
190,0
0,930
Top-Pak rings
Aluminium
50
105,5
0,956
VSP rings
Metal
Metal
50
25
104,6
199,6
0,980
0,975
110,0
202,0
0,936
0,977
250,0
100,0
200,0
300,0
200,0
200,0
0,970
0,987
0,979
0,930
0,954
0,900
Structured Packings
Euroform
Gempak
Koch-Sulzer
Koch-Sulzer
Mellapak
Montz
Montz
Montz
Montz
Montz
Plastic
Metal
Metal
Metal
Plastic
Metal
Metal
Metal
Plastic
Plastic
PN-110
A2 T-304
CY
BX
250 Y
B1-100
B1-200
B1-300
C1-200
C2-200
70
21
22
33
Source: E. J. Henley et al.: Separation Process Principles. 3. Aufl., John Wiley, Hoboken 2011
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 20 |
The column diameter is determined so as to safely avoid flooding and to ensure that pressure drop is
below 1,2 kPa/m of packed height. At the flooding point, the pressure drop increases infinitely with
increasing vapor velocity. The internal column diameter Di is based again on a fraction f of flooding
velocity wG max by:
Di
N&G max MG
G wG zul
N&G max MG
The generalized correlation of Leva gives reasonable estimates of the flooding gas velocity wG max [ft/s]:
Y wG2 max
G
FP
and
F F
g L H2O
2
3
a
FP packing
3
factor [ft/ft] (usually
determined experimentally)
g gravitational constant
(g = 32,174 ft/s)
G
FLG
&L
m
G
&G
m
L
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 21 |
The functions F and F are corrections for liquid properties given by:
F 0, 8787 2, 6776
L H2O
L
L H O
L H2O
0, 6313
, valid for 0, 65 2
L
L
1, 4
An estimation of pressure drop in Pa/m can be made by using the generalized pressure drop correlation for packed beds according to Sherwood et al. and Leva:
FLG
&L
m
G
&G
m
L
Y FP wG2 G
L G
0,1
L
&L
m
liquid flow rate [kg/s]
&G
m
gas flow rate [kg/s]
[m/s], wG = f wG max
FLG
The flooding curve in the above figure corresponds to a pressure drop of 1200 Pa/m of packed height
and can be accurately described by the polynomial regression:
2
YFlooding
exp 3,5021 1, 028 ln FLG 0,11093 ln FLG
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 23 |
FS wG zul G
CS wG zul
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 24 |
G
L G
Distillation/Absorption/Stripping
Tray Columns
Random-/Structured-Packed Columns
(sieve, valve, bubble-cup trays)
Concept of equilibrium stages: determination of the number of theoretical stages Nth
stagewise
contact
between
the phases
continuous contact between the phases
McCabe-Thiele
graphical
equilibrium-stage
method
Kremser equation (analytically, assuming straight equilibrium and operation lines absorption/
stripping)
Estimation of the actual number of contacting trays
Neff applying an overall column efficiency EOV:
Neff
Nth
EOV
HETP
Hmin 1,5 K 3 m
G&max MG
G wG zul
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 26 |
(1) Sketch the column, set the given feed and product specifications
(2) Determine the operating temperature and pressure by the available utilitiy temperatures, the boiling tem-perature
of the mixture, the desired purity of the separation, and any contraints on the stability of the mixture
(3) Make a material balance over the column to determine the unknown top and bottom compostions and/or flow rates
(4) Plot the vapor-liquid equilibrium curve from data available at the column operating pressure and the diagonal line
on the equilibrium diagram, mark given compositions of feed, distillate and bottom product on the diagram
(5) Draw the q-line
(6) Determine the minimum reflux ratio rmin from intersection of rectifying section operating line and the equilibrium
curve or by calculation
(7) Determine the optimum reflux ratio, e.g. r = 1,2 rmin
(8) Draw operating lines for rectifying and stripping section
(9) Determine the number of theoretical stages Nth using the equilibrium diagram or by analytical methods
(10)Select the type of contacting device: trays or packings
(11)Determine the actual number of trays Neff or HETP and specify the column height Htot
(12)Determine the allowable vapor velocity wG zul
(13)Design the column: inner diameter, column internals (trays, packing, liquid and vapor distribution systems,
packing supports, etc.)
(14)Estimate the total column pressure drop pcol
(15)Evaluate pressure drop according to pcol palow, if necessary select another column internals and return to step
(11)
(16)Determine the energy requirements
and reboiler) and the utiliy flows
Q&B , Q&C
(17)Estimate the annual total costs Ctot (r) = Cop (r) + Ccap (r)
(18)To minimize the annual total costs modify the reflux ratio, return to step (8) and cycle through steps (8) to (17)
until Ctot (r) min
(19)Carry out the mechanical design of the column considering the operating temperature and pressure and the
corrosion properties of the mixture
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 27 |
Multicomponent mixtures are often separated in more than two products. In this case, there is a choice of order in
which the products are separated. Consider the design of distillation systems comprising only simple columns,
which have a single feed and two products.
If there is a mixture of three components A, B, C (in order of increasing boiling point) to be separated into three
relatively pure products, then the decision is between two distillation sequences:
a) direct sequence (the lightest component
is taken overhead in each column)
b) indirect sequence (takes the heaviest component as bottom product in each column)
In general, to separate an n-component mixture into nearly pure products n1 simple columns are sufficient, and
the number of different distillation sequences is Nseq 2(n 1) !/ n !(n 1)!
.
The following table shows some sequences of splits that can be used to separate multicomponent nonazeotropic
mixtures. These can all be accomplished in simple columns, which have a single feed and two products. The components are A, B, C, D, E in order of increasing boiling point. Each of the splits listed corresponds to one simple
column. Actually, more columns can be used, and this is sometimes more economical.
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 28 |
Column 2
A / BC
B/C
AB / C
A/B
Column 2
Column 3
A / BCD
B / CD
C/D
A / BCD
BC / D
B/C
AB / CD
A/B
C/D
ABC / D
A / BC
B/C
ABC / D
AB / C
A/B
Column 2
Column 3
Column 4
A / BCDE
B / CDE
C / DE
D/E
A / BCDE
B / CDE
CD / E
C/D
A / BCDE
BC / DE
B/ C
D/E
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 29 |
General Heuristics:
1) Remove corrosive, hazardous, chemically reactive, or thermally unstable components as early as
possible.
2) Remove final products one-by-one as distillates (prefer the direct sequence) or as vapor streams
from total reboilers.
3) Prefer to reduce the number of columns in a recycle loop.
4) Lump pairs of components with relative volatilities less than 1,1 and remove these as a single
product to be separated using another separating technology the relative volatility between the
two selected key components for the separation in each column is > 1,05.
Heuristics for Simple Columns:
1) Remove the components of greatest molar percentage in the feed first.
2) Remove the lightest component first.
3) Make splits with the highest recoveries last.
4) Sequence separation points in the order of decreasing relative volatility make the most difficult
separation in the absence of the other components last.
5) Favor splits which give molar flows of distillate and bottom products as near equal as possible.
6) Make the cheapest split next in selecting a sequence of columns.
| Prof. Dr. M. Reppich | Conceptual Design of Distillation, Absorption and Stripping Systems | 30 |