SEPARATION EQUIPMENT

1. Selection of suitable separation processes by exploitable property differences

2. Separating homogenous mixtures

Membrane separations
3. Separating non-homogenous mixtures
A. PROCEDURAL STEPS IN THE DESIGN OF DISTILLATION COLUMN

1. Establish the composition and

physical properties of feed and
products, feed and product rates and
any special limitations for
separation

2. Select operating pressure

o Bubble point of overhead gaseous
product is at least 5-10°C above
cooling water temperature for non-
refrigerated systems
o Set reflux ratio – at least 1.2 or
above of the Rmin

3. Establish physical equilibrium data

(x-y equilibrium data or relative
volatility)

4. Shortcut method for stage

calculation
o Fenske-Underwood-Gilliland
method for multicomponent
systems
o Graphical method for binary
systems: Mc Cabe-Thiele and
Ponchon-Savarit methods

5. Column internals:
o Tray – good for high liquid
flowrates and operating pressure
o Tray spacing is standard, not
computed but set for
accessibility
o Random packing is good for
small diameter column, batch
process, with corrosion and
foaming issues
o Structural packing – for low
pressure and vacuum operation,
low pressure drop, low liquid
hold-up

6/7. Calculations generally involve the

use of correlation equations
There are several recommended methods for “fast” calculation for the preliminary
design of distillation column but for our needs, we will only discuss the method
given by Peters and Timmerhaus (latest edition). In addition, only the sieve/tray
column design will be discussed. You may refer to our reference books for
alternative design purposes.

EXAMPLE PROBLEM:
Design a distillation column to separate a multicomponent mixture which is
completely vapor at a temperature of 43.3 °C, a pressure of 1668 KPa and a
composition shown below:

Component Mass flowrate, It is desired to obtain a product with a

kg/s propylene concentration of 99.6 mol%.
Acetylene 1.3x10-6 Tray spacing of 0.762 m is specified.
ethylene 1.3x10-6 Determine the column height and
Ethane 3.3x10-6 diameter.
Propylene 6.41
Propane 4.62
MAPD 5.4x10-4
1,3-butadiene 3.71x10-4
i-butene 1.9x10-4
1-butene 1.2x10-4

Solution:
The given mixture is multicomponent but since most components are too small
compared to propylene and propane, we can neglect them and assume that
essentially it is just a separation of propylene (C3H6 as the light key component LK)
and propane (C3H8 as the heavy key component HK). One also has to arrange the
components according to their volatility to support the selection process of the HK
and LK.

QUESTION: Is there a sort of a useful arrangement of the

chemicals above in their listing? What should this be?
Material balance (in moles):
Overall material Balance:

F = B+D
0.257 = B + D

Material balance for C3H6:

FxF = BxB + Dy D
0.257 (0.5924 ) = BxB + D(0.996 )

Material balance for C3H8:

F (1 − x F ) = B(1 − x B ) + D(1 − y D )
F (1 − 0.5924 ) = B(1 − x B ) + D(1 − 0.996)

Solving simultaneously:
XB
B = 0.1043 kgmol/s
D = 0.1527 kgmol/s
xB = 0.0022

For multicomponent distillation, the minimum number of stages is given by the Fenske
equation:

  
ln  y LK   x HK
 
  y HK  D  x LK  B 
N min =
ln  LK KH

where αLK/HK = geometric mean of relative volatility of the light key component over the
heavy key component throughout the column. The best estimate is obtained by taking α at
dew point temperature of distillate and taking α at the bubble point temperature of the
Pv , LK
bottoms and take the geometric mean. For ideal mixtures,  = where Pv is the vapor
Pv , HK
pressure of the component.

Note: you should be able to calculate iteratively or formulate a worksheet that utilizes
GoalSeek for the calculation of dew or bubble point temperature of a gas mixture
assuming that ideality applies. In both cases, the mole fractions of the components (vapor
phase for the dew point, and liquid phase for the bubble point) are previously set by the
results of our material balance calculations. This is your assignment; review VLE for ideal
mixtures: Raoult’s law if needed. You may also factor in for mixture non-ideality for a
more rigorous approach, if that information is avialable.

The following should be obtained (approximately, assuming ideal mixture behavior):

Pv , LK Pv , propylene
Distillate dew point Tdp = 40.87°C →→  = = = 1.1701
Pv , HK Pv , propane

P Pv
→→  = = , propylene = 1.1654
v , LK
Bottoms bubble point Tbp = 47.98°C
Pv , HK Pv , propane

Geometric mean of αLK/HK :

 LK / HK = ( LK / HK )T ( LK / HK )T = (1.1654 )(1.1701) = 1.1678

dp bp

The minimum number of stages:

ln[( 0.996 / 0.004 )(0.9978 / 0.0022 )]

N min =  75 stages
ln(1.1678 )

To obtain Rmin, we can use the following equations (Underwood):

n
 i xF , i n
 i xD , i
 = 1 − q and Rmin + 1 = 
i =1  i −  i =1  i − 

where:  i = Average geometric relative volatility of component i in the mixture

relative to the heavy key (based on average column temperature)
xF ,i = Mole fraction of component i in the feed
xD,i = Mole fraction of component i in the distillate
q = Moles of saturated liquid on the feed tray per mole of feed
 = A parameter determined numerically and lies between the relative
volatilities of the two key components

Thus:
n
 i xF ,i 1.1678 (0.5924 ) 1(0.4076 )

i =1 − 
=
1 . 1678 − 
+
1 − 
=1− q but q = 0 ( feed is all vapor)
i

 = 1.0684 (can be calculated by trial and error or by using MS Excel Goal Seek with set
limits of 1.0 to 1.1678 since it is expected to be within this range)
 n
 i xD , i 1.1678 (0.996 ) 1(0.004 )
Rmin + 1 =  = + = 11.64
i =1  i −  1.1678 − 1.0684 1 − 1.0684
Rmin = 10.64
Assume R = 1.65 Rmin
R = 1.65(10.64) = 17.56

Note on the ratio of Ractual (R) to Rmin:

The Ractual (R) that one picks should be optimized from economics data (determination of reflux
ratio value that results to minimum total distillation costs). For ballpark estimate, use 1.1-1.2
Rmin for refrigerated system and 1.2-1.35 Rmin for a hot system. In our example above, we can
interpret that optimization results to R = 1.65Rmin.

The actual number of theoretical stages can be estimated according to the following (Gilliland-
Eduljee):

N − N min  R − Rmin 
0.566

= 0.751 − 
N +1  R +1 
hence :
N − 75  (17.56 − 10.64) 
0.566

= 0.751 − 
N +1  17.56 + 1 
N  179 stages

The feed tray location can be also estimated using the following equation:

N  B  x   ( xLK ) B 
2
  0.1043  0.4076   0.0022  2 
log D = 0.206 log   HK     = 0.206 log    
NB  D  xLK  F  ( xHK ) D    0.1527  0.5924   0.004  
ND
= 0.6651
NB
but N = N D + N B
179 = 0.6651 N B + N B
N B = 107 stages →→→ no. of stages below the feed tray
N D = 72 stages →→→ no. of stages above the feed tray

Hence, the feed enters the column 72 theoretical stages above the bottom stage.

The estimation of the column diameter involves the determination of the net vapor velocity at
flood conditions. This is normally obtained at both ends of the column to determine the
maximum column diameter required. For this design, maximum column diameter will occur at
the top of the column. To do this, we need to determine the liquid and vapor densities and the
liquid surface tension.

Considering the top of the column, distillate is essentially pure propylene which exists as gas
(prior to condenser) and liquid after the condenser. The needed properties of pure propylene (at
the indicated T and P) are:

V = 27 kg / m3 (by ideal gas law)

 L = 476 kg / m3
 L = 6 dyne / cm (estimated surface tension of liquid propylene)

The liquid-vapor flow factor (FLV) is calculated according to the following equation:
0.5
 L   
0.5
 17.56  27 
Liquid-vapor flow factor, FLV =   V  =   = 0.225
 V   L   18.56  476 

where L and V are the mass flowrates (kg/s) of the liquid and vapor stream, respectively. The
ratio L/V was derived according to:

Mat’l balance at the V

node:

L D

𝐿
We know that = 𝑅 so 𝐿 = 𝑅𝐷 and that V = L + D
𝐷

Formulating L/V:
𝐿 𝑅𝐷 𝑅𝐷 𝑅
= 𝐿+𝐷 = 𝑅𝐷+𝐷 = 𝑅+1
𝑉

Thus
0.5
 L   
0.5
 17.56  27 
Liquid-vapor flow factor, FLV =   V  =   = 0.225
 V   L   18.56  476 
From the chart for Souder and Brown factor (Csb) at flood conditions (you may obtain the one in
the latest edition of Timmerhaus and Peters since it is in SI units):

Alternatively, the following equation can be used where the plate spacing S is in mm:

CSB = 0.0105 + 8.127 10−4 S 0.755 exp(−1.463FLV

0.842
)

Csb = 0.075 m/s

0.5
    L − v   6   476 − 27 
0.2 0.2 0.5

Hence: Vnf = Csb     = 0.075    = 0.240 m / s

 20    v   20   27 

For design, it is recommended that 80-85% of the flooding velocity should be used:

Vn = 0.8Vnf = 0.8(0.240) = 0.192 m / s

Net column area used in the separation process:

 m V
An =  V is the volumetric flowrate of the vapor
where m
Vn

 (17.56 + 1) kgmol / s vapor  0.1527 kgmol D  42.08 kg  m3 

    
m V  1 kgmol / s D  s  kgmol  27 kg 
An = = = 23.00 m 2
Vn 0.192 m / s

Assume that the downcomer occupies 15% of the column cross-sectional area (that is, net area
An corresponds only to the light-blue shaded area of the trays illustrated in the figure below):

An 23.00 m 2
Ac = = = 27.07 m 2
(1 − 0.15) 0.85
D 2 4(27.07 )
Ac =  D= = 5.87 m
4 

Note: Some references put limit to the column diameter up to 3 or 5 m. If this is decided (3 or 5
m limit), then parallel columns would be designed. The minimum diameter for tray columns is
0.75 m. Otherwise (dia < 0.75 m), packed tower is recommended.

For column height evaluation, the following equations have to be considered:

N
N actual =
Eo
H c = ( N actual − 1) H s + H

where: Eo = overall tray efficiency

Hs = tray spacing (0.15 to 1 m apart; when D > 1 m, Hs is generally set at 0.5 m)

The overall height of the column will depend on the plate spacing. Plate spacing from
0.15 m (6 in.) to 1 m (36 in.) are normally used. The spacing chosen will depend on the
column diameter and operating conditions. Close spacing is used with small-diameter
columns, and where head room is restricted; as it will be when a column is installed in a
building. For columns above 1 m diameter, plate spacing of 0.3 to 0.6 m will normally be
 used, and 0.5 m (18 in.) can be taken as an initial estimate. This would be revised, as
necessary, when the detailed plate design is made.

∆H = additional height for liquid holdup and vapor disengagement (can be roughly
assumed 5-10% of column height Hc)

As a rough guide for preliminary design, 70% is generally assumed for Eo.

Alternatively, O’Connel correlation for Eo can be used:

𝐸𝑜 = 0.492 [𝜇𝐿 (𝛼𝐿𝐾/𝐻𝐾 )𝑎𝑣𝑒 ]−0.245

where  L is the molar averaged liquid feed viscosity taken at average column temperature.

For our design problem:

N 
H c =  − 1 H s + H
 Eo 
 179 
Hc =  − 10.762 + 0.05 H c
 0.70 
H c = 204 m

This column height is inordinately too high. According to Sinnott and Towler (2009), the
practical limit of column height should be less than 60 m as there are only 48 cranes worldwide
that can possibly lift a column up to 60 m. Therefore, multistage separation could be considered
for this problem.

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B. DRYER DESIGN