Design of Distillation Columns

Submitted by:
Muhammad Faisal

Department of Chemical Engineering UET

Lahore
3 Design of Distillation Columns
Summary of Distillation Column Design

(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 , calculate the size of the heat exchangers (basic design of condenser
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
3 Design of Distillation Columns
Determination of the Number of Actual Stages
Overall Column Efficiency, Murphree Tray Efficiency

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 Bubble Cup Tray Sieve Tray Valve Tray
EOV 0,5 0,7 0,6 0,8 0,7 0,8 0,7 0,9

The Murphree tray efficiency Ej that describes the separation achieved on individual tray j is usually
based on the vapor phase:
Separation effect of the actual stage y% - y%j -1 a
Ej = = *j = 1
Separation effect of the theoretical stage y%j - y%j -1 b

y%j +1 x%j + 2 y%
Equilibrium
j+1 Curve

z y%j x%j +1 Operating Line

y%
*
j

j y%j b
a y%j - y%j -1 actual composition change
z y%j -1 x%j y%j -1
y%
*
% maximal feasible composition
j - y j -1
j1 change (predicted by equilibri-
um)
y%j - 2 x%j -1 x%j x%j +1 x%
3 Design of Distillation Columns
Determination of the Tray Column Height

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
Pseudo-equilibrium curve for
EOV = a/b = const.
b a
y% Equilibrium curve for EOV = 1
Operating lines
a
EOV =
b
b e.g., for EOV = 0,75; s = 1; Nth = 3:
a
N s
Neff = th =4
EOV
0 x%
B x% x%
D 1

The height of trayed portion of column H and the column height Htot, required to meet the product
specifications, are
N s
H = Neff
z = th z
Htot = H + Hmin H + 3
z
EOV

where z is the tray spacing, typically z = 0,2 0,6 m.

3 Design of Distillation Columns
Operating Region of Tray Columns

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 withV& x-coordinate
L
V&
andG y-coordinate

. Often these two 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
Entrainment Froth

Operating region
D
Downcomer
capacity

Minimum crest Weeping

over weir Aac
3 Design of Distillation Columns
Operating Region of Tray Columns

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
Minimum Gas Load:
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
Maximum Gas Load:
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 (den-
sity 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
3 Design of Distillation Columns
Operating Region of Tray Columns

Minimum Liquid at extremely low liquid loads, liquid flows unevenly V&
L

Load: across the tray (maldistribution), which decreases the

mass transfer efficiency hl
minimum height of the weir overflow hwo 5 mm

this corresponds to a minimum liquid weir load of: hwo

z
V&
L / lw 2 m/(m h)

Maximum Liquid the liquid flow downward through the downcomers is V&
G

Load: enforced by gravity forces which results in a limitation

of the maximum liquid load
the following four empirical rules are often used to
determine the maximum liquid flow rate
lw
the weir load shouldV&
be/ l < 60 m/(m
L w h)
the liquid velocity in the downcomer should not exceed
a value of 0,1 m/s
the volume of the downcomer should permit a liquid
residence time of more than 5 s
the height of the clear liquid in the downcomer should not
exceed half of the tray spacing (hl z/2)

Ideally, the column is operated in the range of 60 to 90 % of the flooding vapor velocity.
3 Design of Distillation Columns
Comparsion of Common Tray Types

3
1 2

Source: RASCHIG GmbH, Ludwigshafen * within optimum operating range

3 Design of Distillation Columns
Summary of the Geometry and Layout of Common Tray Types at Different Operating
Pressures

3
1 2

* DS column diameter in m, hw outlet weir height in m Source: RASCHIG GmbH, Ludwigshafen

3 Design of Distillation Columns
Determination of the Tray Column Diameter

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 volume-
tric flow rate during the operation and the allowable vapor velocity referred to the total column cross-
sectional area:

p V& m&G max N& MG

AQ = Di 2 = G max =
= G max
4 wG zul G
wG zul G wG zul

AQ free (total) cross-sectional area of the column [m]

Di column internal diameter [m]

V&
G max maximum vapor volumetric flow rate [m/s]
wG zul allowable vapor velocity referred to the area AQ [m/s] (0,56 m/s)
&G max
m
maximum vapor mass flow rate [kg/s]
N&G max
maximum vapor molar flow rate [kmol/s]
G avarage density of the vapor phase [kg/m]

MG average molecular weigth of the vapor phase [kg/kmol]

3 Design of Distillation Columns
Determination of the Tray Column Diameter

Column internal diameter Di can be expressed as:

2 2 N&G max
MG
Di = AQ =
p p 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 = p operating pressure [Pa]
VG VG RT
T operating temperature [K]
R universal gas constant
(R = 8314,5 J/(kmolK)

Thus, the column internal diameter at a given operating pressure and operating temperature is:

2 N&G max
R T N&G max
T
Di =
102, 89
p p wG zul p wG zul

where Di [m], [kmol/s], T [K], p [Pa], wG zul [m/s]

N&G max
3 Design of Distillation Columns
Determination of the Tray Column Diameter

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 - G
wG zul = f
wG max = 0,7 ac
kV L
AQ G
wL
FA f fraction of flooding, e.g. f=0,7
kV capacity parameter of
FW
Souders/Brown [m/s]
Two-phase
z Layer Aac active area of a tray [m]

AQ total column cross-sectional

FG area [m] z tray spacing
wG max liquid surface tension
L liquid density [kg/m]

G vapor density [kg/m]

3 Design of Distillation Columns
Pressure Drop in Tray Columns

Generally, the column pressure drop should be as low as possible because

obtaining the number of theoretical trays using the McCabe-Thiele graphical method
assumes that the pressure is constant over the whole column
low pressure drop leads to a reduced energy requirement and to a heat supplied by the
reboiler at the bottom at a lower boiling temperature level.

Pressure loss of the vapor significantly depends on both gas and liquid load. The total column pressure
drop is the sum of the hydrostatic pressure loss caused by the clear liquid holdup on the trays, the
pressure drop due to the friction for vapor flow through the openings in the trays, and a loss due to
the formation of bubbles by the gas:
pcol = pst + pdyn + p

pcol total column pressure drop [Pa]

pst hydrostatic pressure drop of clear liquid [Pa]

pdyn pressure drop due to vapor flow resistance [Pa]

p pressure drop due to surface tension [Pa]

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.
3 Design of Distillation Columns
Pressure Drop in Tray Columns

The hydrostatic pressure drop of liquid pst depends on the mass of the clear liquid inside the column,
as given by:
mL g
pst =
AQ

mL total mass of the liquid in the column [kg]

g gravitational constant g = 9,81 m/s

AQ total cross-sectional area of the column [m]

For tray columns the hydrostatic pressure drop is given by the sum of the pressure drops across the
trays:
pst = Neff
S
ghS = Neff
(1 - )
L
ghS

Neff number of actual trays [-]

S average density of the two-phase layer [kg/m]

L density of clear liquid [kg/m]

relative gas/vapor fraction in the two-phase layer [-]

hS average heigth of the two-phase layer [m]
3 Design of Distillation Columns
Pressure Drop in Tray Columns

The pressure drop due to the friction for vapor flow up the column pdyn can be expressed approxima-
tely by:

G wG2
pdyn =
2

orifice coefficient of column internals [-]

G vapor density [kg/m]

wG vapor velocity referred to the column cross-sectional area [m/s]

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 orifice coefficient of a dry tray [-]

If the column is operated at 85 % of the flooding vapor velocity, the pressure drop per tray is, depen-
ding on tray type, approximately from 2 to 8,5 mbar.
3 Design of Distillation Columns
Rate-Based Method for Packed Columns

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 distin-
guishable, discrete stages found in trayed towers. Thus, packed columns are better analyzed by mass-
transfer 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

Packed height H
HETP = =
Number of equivalent equilibrium stages Nth

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 approxima-
tions 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:

H = Nth
HETP with HHtot =(0,5...1
min H + Hmin m) + (1...2 m)
3 Design of Distillation Columns
HETP Estimation for Random and Structured Packings

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 d nominal packing diameter [in] (1 in = 25,4 mm)
P

2. Structured packings at low-to-modarate pressures with low-viscosity liquids

100
HETP = + 0,333
a packing surface area per packed volume [ft/ft]
a

3. Distillation with viscous liquid

HETP = 5 K 6 ft

4. Vacuum service
HETP = 1,5
dP + 0,5

5. Structured packings at high pressures

100
HETP > + 0,333
a

6. Small-diameter columns with internal diameter Di < 2 ft

HETP = Di , but HETP 1 ft
3 Design of Distillation Columns
Characteristics of Random Packings

Type Packing Material Nominal Packing

Diameter Factor
dP [in] FP [ft/ft]

Raschig rings Ceramic 1,0 157

2,0 58
3,0 33
Raschig rings Metal 1,0 165
2,0 71
3,0 40
Intalox saddles Ceramic 1,0 92
2,0 30
3,0 15
Intalox saddles Plastic 1,0 36
2,0 25
Pall rings Metal 1,0 56
1,5 29
2,0 27
3,5 16
Pall rings Plastic 1,0 53
2,0 25
3,5 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
3 Design of Distillation Columns
Characteristics of Random and Structured Packings

Packing Material Size Packing Mass-transfer Surface Void Fraction

[mm] Factor Area per Unit Volume [-]
FP [ft/ft] a [m/m]

Random Packings
Hiflow rings Ceramic 50 29 89,7 0,809
Metal 50 16 92,3 0,977
Plastic 50 20 117,1 0,924
Nor-Pac rings Plastic 50 14 86,8 0,947
Plastic 35 21 141,8 0,944
Plastic 15 311,4 0,918
Tellerettes Plastic 25 40 190,0 0,930
Top-Pak rings Aluminium 50 105,5 0,956
VSP rings Metal 50 104,6 0,980
Metal 25 199,6 0,975
Structured Packings
Euroform Plastic PN-110 110,0 0,936
Gempak Metal A2 T-304 202,0 0,977
Koch-Sulzer Metal CY 70
Koch-Sulzer Metal BX 21
Mellapak Plastic 250 Y 22 250,0 0,970
Montz Metal B1-100 100,0 0,987
Montz Metal B1-200 200,0 0,979
Montz Metal B1-300 33 300,0 0,930
Montz Plastic C1-200 200,0 0,954
Montz Plastic C2-200 200,0 0,900

Source: E. J. Henley et al.: Separation Process Principles. 3. Aufl., John Wiley, Hoboken 2011
3 Design of Distillation Columns
Determination of the Packed Column Diameter

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:

2 N&G max
MG 2 N&G max
MG
Di = =
f fraction of flooding 0,65 < f < 0,9 (f 0,7)
p G
wG zul p G f wG max

The generalized correlation of Leva gives reasonable estimates of the flooding gas velocity wG max [ft/s]:

F G
Y = wG2 max P and F
F
g L H2O h

&L
m
( ) ( )
2 3
Y = exp
-3,7121 - 1, 0371
ln FLG - 0,1501
with ln F - 0, 007544 ln F
FLG = G
LG LG
&G
m L

a
FP packing
3 factor [ft/ft] (usually a packing surface area per packed

determined experimentally) volume [m/m]
g gravitational constant void fraction [m/m, %, -]
(g = 32,174 ft/s)
G avarage density of the vapor phase [kg/m]
L H2O average density of water [kg/m] ( L H O = 999,5 kg/m at 20 C, 1 bar)
2

The above regression model for the dimensionless flooding velocity factor Y = f (FLG) is valid for
0,01 Y 10.
3 Design of Distillation Columns
Determination of the Packed Column Diameter

The functions F and Fh are corrections for liquid properties given by:
2
L H2O L H O L H2O
F 0,
- 8787
+-= 2, 6776 0, 6313 2 , valid for 0, 65 1, 4
L L
L

L H2O average density of water [kg/m] ( L H O = 999,5 kg/m at 20 C, 1 bar)

2

L average density of liquid [kg/m]

hL0,19 , valid for 0,3 cP hL 20 cP

Fh = 0, 96

hL average dynamic viscosity of liquid [cP]

For a certain value of the flow parameter FLG can firstly be calculated the dimensionless factor Y, and
the superficial gas velocity at flooding wG max = f (Y) is then estimated for a given packing type and size
(FP = f (a, )) and the correction functions F and Fh.

Finally, using the allowable vapor velocity wG zul, the internal diameter of the distillation column Di can
be determined. The tower inside diameter should be at least 10 times the nominal packing diameter
and preferably closer to 30 times,

Di ( 10...30 )
dPdP nominal packing diameter [mm] .

Under these conditions, the negative effect of maldistribution on mass-transfer efficiency is minimised.
Therefore, the column diameter may need to be adjusted accordingly.
3 Design of Distillation Columns
Pressure drop in Packed Columns

An estimation of pressure drop in Pa/m can be made by using the generalized pressure drop correla-
tion for packed beds according to Sherwood et al. and Leva:

&L
m
FLG = G
&G
m L

wG2 G
Y = FP h0,1
L
L - G

Y &L
m
liquid flow rate [kg/s]
gas flow rate [kg/s]&G
m
L liquid density [kg/m]
G gas density [kg/m]
FP packing factor [ft/ft]

J. Bentez: Principles and Modern w G gas

Applications ofvelocity
Mass [m/s], wG = f wG max
Transfer Operations. 2. Aufl., John Wiley, Hoboken 2009
hL liquid viscosity [Pas]
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:
ln FLG - 0,11093 ( ln FLG )
2
YFlooding
= exp
-3,5021 - 1, 028

3 Design of Distillation Columns
Summary of Distillation Column Design

Distillation/Absorption/Stripping

Tray Columns
Random-/Structured-Packed Columns
(sieve, valve, bubble-cup trays)
stagewise contact between the phases continuous contact between the phases
Concept of equilibrium stages: determination of the number of theoretical stages Nth
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 Estimation of HETP depending on packing type
Neff applying an overall column efficiency EOV: and size, liquid viscosity, and surface tension:
Nth 0,3 K 0, 9 m for random packings

Neff = 0,1 EOV 0,9 HETP =
EOV 0,2 K 0,7 m for structured packings

Height of the actual equipment:

Htot = Neff
z + Hmin z = 0, 45 K 0, 6 m; Hmin 3
z Htot = Nth
HETP + Hmin Hmin = 1,5 K 3 m

Internal Column Diameter:

2 G&max
MG
Di = with wG zul = f
wG max ; 0, 65 < f < 0, 9
p G wG zul
Vapor-side pressure drop:
pcol = f (tray type) pcol = f (packing type)

GPDC charts, correlations