Distillation Column Design

Distillation –An Introduction

⚫a process in which a liquid or vapour mixture of two
or more substances is separated into its component
fractions of desired purity, by the application and
removal of heat.

⚫distillation is the most common separation technique

⚫Distillation is based on the fact that the vapour of a

boiling mixture will be richer in the components that
have lower boiling points.
 BASIC DISTILLATION EQUIPMENT AND OPERATION
Main Components of Distillation Columns

⚫ A vertical shell - separation of liquid components is carried out

⚫ Column internals- trays/plates and/or packings
⚫ Reboiler - provide the necessary vaporisation for the distillation
process
⚫ Condenser - cool and condense the vapour leaving the top of
the column
⚫ Reflux drum - hold the condensed vapour from the top of the
column so that liquid (reflux) can be recycled
back to the column
Distillation Column - Schematic
 COLUMN INTERNALS
Bubble cap trays:

⚫ has riser or chimney fitted over each hole,

and a cap that covers the riser.

⚫ The cap is mounted so that there is a

space between riser and cap to allow
the passage of vapour.

⚫ Vapour rises through the chimney

and is directed downward by the cap,
finally discharging through slots in the
cap, and finally bubbling through the
liquid on the tray.
 Valve Trays
• Perforations are covered by liftable
caps.

• Vapour flows lifts the caps, thus self

creating a flow area for the passage of
vapour.

• The lifting cap directs the vapour to

flow horizontally into the liquid, thus
providing better mixing than is possible
in sieve trays.
 Sieve trays
• Sieve trays are simply metal plates with
holes in them.

• Vapour passes straight upward through

the liquid on the plate.

• The arrangement, number and size of the

holes are design parameters.

• Because of their efficiency, wide operating

range, ease of maintenance and cost
factors, sieve and valve trays have replaced
bubble cap trays in many applications.
Liquid and Vapour Flows in a Tray Column
 Packings
⚫increase the interfacial area for vapour-liquid contact
⚫impart good vapour-liquid contact
⚫packings provide extra inter-facial
area for liquid-vapour contact
⚫efficiency of separation is
increased for the same column height
⚫packed columns are shorter than trayed columns
⚫Packed columns are called continuous-contact
columns while trayed columns are called staged-
contact columns because of the manner in which
vapour and liquid are contacted.
 COLUMN REBOILERS
⚫heat-exchangers to bring the liquid at the bottom of
the column to boiling point
COLUMN REBOILERS
McCabe-Thiele Method- Steps involved
1. Analysis of the Rectifying section, and determine the ROL using xD
and R
2. Analysis of the Feed section, and determine the feed condition (q)
3. Determination of the feed line (q-line) using xF and q
4. Locate the intersection point between ROL and q-line
5. Analysis of the Stripping Section, and determine the SOL using (4)
and xB

⚫ When R is unknown (but instead specified as a multiple of the

minimum rate), we will first determine the q-line.

⚫ Usually the SOL is the last line to draw, after both ROL and q-line are
drawn. Fixing the ROL and the q-line automatically fixes the SOL.
Effects of adverse Vapour Flow Conditions
Foaming :
⚫ expansion of liquid due to passage of vapour or gas
⚫leads to liquid buildup on trays
⚫In some cases foam may mix with liquid on the tray above
⚫separation efficiency is always reduced

Entrainment :
⚫liquid carried by vapour up to the tray above
⚫caused by high vapour flow rates
⚫efficiency is reduced
⚫lower volatile material is carried to a plate holding liquid of
higher volatility
⚫contaminate high purity distillate
 Effects of adverse Vapour Flow Conditions
Weeping/Dumping:
⚫This phenomenon is caused by low vapour flow
⚫ pressure exerted by the vapour is insufficient to hold up
the liquid on the tray
⚫liquid starts to leak through perforations
⚫Excessive weeping will lead to dumping
⚫liquid on all trays will crash (dump) through to the base of
the column and the column will have to be re-started
⚫Weeping is indicated by a sharp pressure drop in the
column and reduced separation efficiency
 Effects of adverse Vapour Flow Conditions
Flooding:
⚫Flooding is brought about by excessive vapour flow,
causing liquid to be entrained in the vapour up the
column.
⚫The increased pressure from excessive vapour also backs
up the liquid in the downcomer, causing an increase in
liquid holdup on the plate above.
⚫Depending on the degree of flooding, the maximum
capacity of the column may be severely reduced.
⚫Flooding is detected by sharp increases in column
differential pressure and significant decrease in separation
efficiency
Choice b/w Tray and Packed column
⚫Plate column are designed to handle wide range of
liquid flow rates without flooding
⚫For large column heights, weight of the packed
column is more than plate column.
⚫Man holes will be provided for cleaning in tray
columns. In packed columns packing must be
removed before cleaning
⚫When large temperature changes are involved as in
the distillation operations tray column are often
preferred
⚫Random-Packed Column generally not designed with
the diameter larger than 1.5 m and diameters of
commercial tray column is seldom less than 0.67m
Reflux Ratio Analysis
Reflux Ratio Analysis
 Analysis of Reflux Ratio Changes
⚫There is an inverse relationship between the reflux ratio
and the number of theoretical stages

⚫For a new design, of course the reflux ratio and number of

theoretical stages can both be varied to achieve an
optimum balance.

⚫For an existing column, the number of trays used is fixed,

hence higher distillate concentration (mole fraction xD)
can only be obtained by increasing the reflux ratio.
Analysis of Reflux Ratio Changes
 Minimum Reflux Ratio
⚫Rmin is that point beyond which R cannot be reduced
further
⚫Condition for Rmin occurs when the ROL (from xD) joins
a point on the equilibrium curve
⚫This point also corresponds to the minimum reboiler heat
duty and condenser cooling capacity required for the
separation.
⚫Feed Pinch Point :
⚫ intersection of the ROL and q-line and the equilibrium
curve
⚫ corresponds to infinite number of stages in the column
Minimum Reflux Ratio

q-Line
Total Reflux Ratio
⚫ As R approaches infinity), the slope
approaches 1.0 and the intercept
apraoches Zero. The ROL (thus the
SOL as well) coincides with the 45o
diagonal line
⚫ The entire area between the
equilibrium curve and diagonal line
is used for separation, with the
largest possible driving force
⚫ In practice, the total reflux can be
achieved by reducing the feed to
zero, returning all the overhead
product back to the column as
reflux and reboiling all the bottoms
product
⚫ infinite reboiler heat duty and
condenser cooling capacity for a
given feed rate
Optimum Reflux Ratio
 Optimum Reflux Ratio
⚫ At minimum reflux ratio, the fixed cost is infinite (due to infinite
number of stages required), but the operating cost is at a
minimum, because minimum amount of liquid is to be handled
(e.g. consuming lesser pump horsepower, lesser cooling capacity,
etc).

⚫ As reflux ratio increases, less stages are required but larger

equipment are now needed to handle the increased reflux liquid
and reboiled vapour load. Thus the fixed cost initially decreased
but eventually increase again when the reflux ratio approaches
total reflux. The fixed cost this falls through a minimum and then
rise again to infinity. As for the operating cost, it will continue to
increase with increasing reflux ratio.

⚫ The total cost, which is the sum of fixed cost and operating cost,
must therefore passes through a minimum. The reflux ratio at this
minimum total cost is the optimum (or economical) reflux ratio.
Typically the optimum reflux ratio is approximately 1.2 to 1.5 times
Rmin
Tray Efficiency
⚫Deviation from equilibrium due to :
⚫ Insufficient time of contact

⚫ Insufficient degree of mixing

⚫Two types of tray efficiency:

⚫ Overall Efficiency and

⚫ Murphree Efficiency
 Overall Efficiency
⚫Eo = No. of Theoretical Trays / No. of Actual Trays

⚫Applied throughout the whole column, i.e. every tray is

assumed to have the same efficiency
⚫The O'Connell correlation is given as:
 Overall Efficiency
⚫The Drickamer-Bradford empirical correlation is given as:

⚫The use of the equation is restricted to the range of data

below, and is intended mainly for hydrocarbon mixtures.
⚫Average temperature 157 - 420 oF
Pressure 14.7 - 366 psia
Liquid viscosity 0.066 - 0.355 cP
Overall Efficiency 41 - 88 %
APPROXIMATE COLUMN SIZING
⚫ Plate spacing:
⚫ Plate spacings from 0.15 m (6 in.) to 1 m (36 in.) are normally
used
⚫ For columns above 1 m diameter, plate spacings of 0.3 to 0.6
m will normally
⚫ 0.5 m (18 in.) can be taken as an initial estimate
⚫ larger spacing will be needed between certain plates to
accommodate feed and sidestreams arrangements, and for
manways
⚫ The hole sizes used vary from 2.5 to 12 mm; 5 mm is the
preferred size
⚫ Typical plate thicknesses used are: 5 mm (3/16 in.) for
carbon steel,and 3 mm (12 gauge) for stainless steel.
Continuous Distillation Problem
⚫ A distillation column operating at 1 atm is to be designed
for separating an ethanol-water mixture. The feed is 20
mole% ethanol and the feed flow rate is 1000 kg-mole/hr
of saturated liquid. A distillate composition of 80 mole%
ethanol and a bottoms composition of not more than 2
mole% ethanol are desired. The reflux ratio is 5/3.
⚫ Determine:
(a) the total number of equilibrium stages required
(b) the optimum feed plate location
(c) the distillate and bottoms flow rates in kg-mole/hr
⚫ Top column temperature=371K
⚫ Bottom column temperature=398K
⚫ Vapor velocity to the column=0.5 m/s
Solution
⚫Given:
F = 1000 kg-mole/hr, xF = 0.20 (ethanol is MVC)
Feed is saturated liquid, thus q = 1.0
xD = 0.80,
xB = 0.02;
R = 5/3

⚫Intercept of ROL
0.80 / (5/3+1) = 0.30.
 Solution CONTD…..
⚫From the graph plotted,
⚫ number of triangles = 15.
⚫ number of equilibrium stages required = 14 + 1 reboiler.
⚫ Optimum feed plate location = stage #13.
⚫Material Balance:
F=D+B;
B = 1000 – D
⚫MVC Balance:
F xF = D xD + B xB
Substituting for B gives:
( 1000 ) ( 0.20 ) = ( D ) ( 0.80 ) + ( 1000 - D ) ( 0.02 )
Solving D = 230.77 kg-mole/hr
B = 769.23 kg-mole/hr
SOLN Contd……
 Solution Analysis
⚫Rectifying Section has more trays (12) than the
Stripping Section (3). This is because the relative
volatility of ethanol decreases sharply with increase in
ethanol concentration.
⚫The relative volatility is very high initially, resulting in
fewer trays being required for separation in the
Stripping Section. As concentration of ethanol (mole
fraction) increases, the relative volatility drops
SOLN CONTD……
Calculation of Actual Number of Plates :
N = Nth / Tray Efficiency
Assuming Tray efficiency = 0.8
Nact in Rectification Section = 12/0.8 =15
Nact in Stripping Section = 3/0.8 = 3.75 ==4 stages
Total No. of trays required = 19
= 18 + 1 reboiler
New Feed Location = 16th Tray
SOLN CONTD……
Calculation of column diameter:
At the top:
Number of moles of vapor :
V= L + D = D(R + 1)
V = 230.77 (5/3 + 1) = 615.38 kmol/hr
Ideal gas behavior is assumed for the vapor.
Volumetric flow rate= (615.38)*0.082*371=18721.09
m3/h.
Vapor velocity=0.5m/s
Cross sectional area=18721.09/(3600*0.5)=10.40m2
Column diameter=(10.40*4/3.14) 0.5 = 3.64m
SOLN CONTD……
At the bottom:
Number of moles of vapor = 615.38 kmol/hr
Ideal gas behavior is assumed for the vapor.
Volumetric flow rate= (615.38)*0.082*398=20083.5m3/h.
Vapor velocity=0.5m/s
Cross sectional area=20083.5/(3600*0.5)=11.15m2
Column diameter=(11.15*4/3.14)0.5 = 3.77m
Column is designed for higher diameter, i.e, 3.77m
SOLN CONTD……
Column Height :
For column diameter > 1 m tray spacing b/w 0.3 to o.6 m
Choosing Tray Spacing = 0.5m
Column Height = (18 + 2) * 0.5
= 10 m
Pressure Drop Calculations:

Assume 500 mm water, pressure drop per plate.

Column Pressure drop = 9.81 *500*1000*18/1000 = 88290Pa
= 0.871355 atm
Distillation design – problem 2
Acetone is to be recovered from an aqueous
waste stream by continuous distillation. The feed
will contain 10 per cent w/w acetone. Acetone of
at least 98 per cent purity is wanted, and the
aqueous effluent must not contain more than 50
ppm acetone. The feed will be at 20 o C. Take the
minimum feed rate as 13,000 kg/h. Use sieve
plates.
 Solution
⚫Molecular weights
⚫ Acetone 58,
⚫ Water 18
⚫Mole fractions
 Solution
⚫From McCabe Thiele Diagram :
⚫ total stages Rectification = 7
⚫ total stages Stripping = 9
⚫ Feed Location = 8th Tray
⚫Summary
⚫ Number of stages = 16
⚫ Slope of the bottom operating line = 5.0
⚫ Slope of top operating line = 0.57
⚫ Top composition = 94 per cent mol.
= 98 per cent w/w.
⚫ Bottom composition essentially water.
⚫ Reflux ratio = 1.35
SOLN Contd……
Solution
Assume 60% tray efficiency,
Actual No. of trays = (16 – 1)/0.6 = 25 stages

Initial Estimate of column pressure:

Physical properties

⚫Top, 98% w/w acetone, top temperature 57 o C

 Estimation of column diameter
Flow Parameter:
 K1 values
Take tray spacing = 0.5 m
From the graph,

Correction for surface tensions :

Flooding velocity
Maximum volumetric flow rate
Calculation of column c/s area
Column diameter
Provisional plate design

Active area Aa = Ac - 2 Ad = 0.50 - 0.12 = 0.38 m2

Hole area Ah take 10 per cent Aa = 0.038 m2
Ad/ Ac = 0.12 , From figure,
Lw/dc = 0.76
Weir length = 0.76 x 0.79 = 0.60 m
Take weir height = 50 mm
Hole diameter = 5 mm
Plate thickness = 5 mm
Check weeping
 Plate pressure drop
Dry plate drop:
Check Entrainment
THANK YOU