INTRODUCTION

Distillation is 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 based on the fact that the vapour of a boiling mixture will be richer in the
components that have lower boiling points. Therefore when this vapour is cooled and
condensed, the condensate will contain more volatile components. At the same time, the
original mixture will contain more of the less volatile material.
Distillation columns are designed to achieve this separation efficiently. Although many
people have a fair idea what distillation means, the important aspects that seem to be missed
from the manufacturing point of view are that:
Distillation is the most common separation technique.
Distillation consumes enormous amounts of energy, both in terms of cooling and heating
requirements.
It can attribute to more than 50% of plant operating costs.
The best way to reduce operating costs of existing units, is to improve their efficiency via
process optimization and control. To achieve this improvement, a thorough understanding
of distillation principles and how distillation systems are designed is essential.
DISTILLATION PRINCIPLES
Separation of components from a liquid mixture via distillation depends on the differences in
boiling points of the individual components. Also, depending on the concentrations of the
components present, the liquid mixture will have different boiling point characteristics.
Therefore, distillation processes depends on the vapour pressure characteristics of liquid
mixtures.
Vapour Pressure and Boiling
The vapour pressure of a liquid at a particular temperature is the equilibrium pressure exerted
by molecules leaving and entering the liquid surface. Here are some important points
regarding vapour pressure:
energy input raises vapour pressure
vapour pressure is related to boiling
a liquid is said to boil when its vapour pressure equals the surrounding pressure
the ease with which a liquid boils depends on its volatility
liquids with high vapour pressures (volatile liquids) will boil at lower temperatures
the vapour pressure and hence the boiling point of a liquid mixture depends on the
relative amounts of the components in the mixture
distillation occurs because of the differences in the volatility of the components in the
liquid mixture
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The Boiling Point Diagram

The boiling point diagram shows how the equilibrium compositions of the
components in a liquid mixture vary with temperature at a fixed pressure. Consider an
example of a liquid mixture containing 2 components (A and B) - a binary mixture. This has
the following boiling point diagram.
The boiling point of A is that at which the B is that at which the mole fraction of A is
0. In this example, A is the more volatile component and therefore has a lower boiling point
than B. The upper curve in the diagram is called the dew-point curve while mole fraction of
A is 1. The boiling point of the lower one is called the bubble-point curve.

The dew-point is the temperature at which the saturated vapour starts to condense.The
bubble-point is the temperature at which the liquid starts to boil. The region above the dewpoint curve shows the equilibrium composition of the superheated vapour while the region
below the bubble-point curve shows the equilibrium composition of the subcooled liquid. For
example, when a subcooled liquid with mole fraction of A=0.4 (point A) is heated, its
concentration remains constant until it reaches the bubble-point (point B), when it starts to
boil. The vapours evolved during the boiling has the equilibrium composition given by point
C, approximately 0.8 mole fraction A. This is approximately 50% richer in A than the
original liquid. This difference between liquid and vapour compositions is the basis for
distillation operations.

Relative Volatility
Relative volatility is a measure of the differences in volatility between 2 components, and
hence their boiling points. It indicates how easy or difficult a particular separation will be.
The relative volatility of component i with respect to component j is defined as

yi = mole fraction of component i in the vapour

xi = mole fraction of component i in the liquid
Thus if the relative volatility between 2 components is very close to one,
it is an indication that they have very similar vapour pressure
characteristics. This means that they have very similar boiling points and
therefore, it will be difficult to separate the two components via distillation.
Having discussed the necessary background information, the following section takes
us to the main purpose this term-paper: distillation column design considerations.

DISTILLATION COLUMN DESIGN CONSIDERATIONS

The following are the basic considerations in modern distillation column designs.
1.
2.
3.
4.
5.

Distillation Design Procedure

Operating Pressure
Reflux ratio and Number of stages
Determination of Number of theoretical stages.
Feed location

Specify Separation:
A material balance around the column is the first step in fractionation calculations. In order to
perform this balance, assumption of the product stream compositions must be made. There
are three ways to specifying desired product from the fractionators:

A percentage recovery of a component in the overhead or bottom stream.

A composition of one component in either product.
A specific physical property, such as vapor pressure, for either product.

In a multicomponent mixture, there are typically two components, which are keys to the
separation.

Light Key (LK) Component: Defined as lightest component in the bottom product in a
significant amount.
Heavy Key (HK) Component: Defined as heaviest component in the overhead product
in a significant amount.

Normally, these two components are adjacent to each other in the volatility list. For hand
calculations, it is normally assumed for material balance purpose that all components lighter
than the light key are produced overhead and all components heavier than the heavy product
are produced with the bottom product
Set Column Pressure:
Before any design calculations can be made on a fractionation problem, a tower operating
pressure must be determined. One of the primary considerations for operating pressure is
cooling medium available for reflux condenser. The cooling media typically used are:

Air: The least expensive cooling method. Design limits the process to an 11C
approach to the ambient summer temperature.
Cooling Water: The satisfactory temperature approach is 5 to 10C.
Mechanical Refrigeration: For process temperature below 35C. This is the most
expensive cooling method from both a capital and operating cost.

Example: If cooling water supply is at 32C and return temperature of 40C using above
guideline the condensing temperature is 45C. For total condenser with a distillate
composition of C1, C2, C3 as 5/5/90%, the vapor pressure of the distillate @ 45C is 23.3
kg/cm2a. Set the pressure of the reflux drum equal to or slightly above the vapor pressure of
the distillate at 45C.
Generally, it is desirable to operate at as low a pressure as possible to maximize the relative
volatility between the key components of the separation. For a quick estimate of a gas
oil/resid operation a pressure of 50 mm Hg at the overhead line and a flash zone temp of

370C may be used. However, if reducing the pressure requires a change to a more expensive
cooling method, this is the usually not a desirable choice.
Whereas, in case of lighter hydrocarbon separation, say C2 from C3, use of a suitable
refrigerant is required when the distillate liquid temperature is lower than the cooling water
temperature. Designing such a column at the higher pressure will make:

The refrigerant system smaller, but

Reboiler duty and the column diameter will be larger.

In deciding the operating pressure of a column, a number of factors have to be considered in

relation to the total system. A table is summarized below to indicate the advantages and
disadvantages of operating a column at higher pressure.
Advantages

It increases the boiling points of the distillate and enables a cheaper cooling medium
to be used. If the cooling medium remains unchanged, it reduces the condenser area
requirements.
It reduces energy costs in vacuum operation.
It increases vapor density and vapor handling capacity. Leads to smaller column
diameter for pressure upto 3.5 to 10.5 Kg/cm2.
It increases boiling points of liquids in the column for distillation of liquefied gases
and allows the use of cheaper construction materials.
It reduces the size of pipes and valves for the vapor line.
Below 1 atm, reduces air leakage into the system.

Disadvantages

It decreases relative volatility and makes separation more difficult. It will therefore
increase reflux and stage requirements, and requires higher reboiler and condenser
duties.
It increases bottom product temperature and increases the risk of chemical
degradation, polymerization and fouling.
Above 7 kg/cm2g, column shell thickness will probably increase, whereas below 7
kg/cm2g, the effect is not as significant.
Increases reboiler temperature, needs a more expensive heating medium or increase in
reboiler area requirement.
It increases hazard potential if process materials are inflammable or toxic.

For mature technologies the operating pressures of the column have been standardized except
for some variation due to site condition, reference can be taken from similar plant/equipment.

Determine minimum reflux and minimum number of stage

Relation between Reflux Ratio and Number of stages:
The design of a fractionation column is a capital cost versus energy cost trade-off problem.
The primary parameters are the number of stages and the reflux ratio. For most calculation,
reflux ratio is defined as the ratio of the molar rate of reflux liquid divided by the molar rate
of net overhead product. The desired separation can be achieved between the limits of
minimum reflux and minimum stages. The relationship between reflux ratio and number of
stages for a given separation is shown on figure 1 below. At minimum reflux an infinite
number of stages are required. At total reflux a minimum number of stages are required

Determination of Minimum Number of Stages

Fenskes equation can be used to calculate the minimum number of stages

If volatility varies widely, the approach of Winn is suggested, in which a modified volatility
is used

Determination of Minimum Reflux Ratio

The Underwood method can be used for calculating minimum reflux ratio. The Underwood
method assumes:

Constant molar overflow, and

Constant relative volatility at the average column temperature.

The first step is to evaluate? (Which must lie between the relative volatilities of the keys) by
trail and error from

Once s is determined, the minimum reflux ratio is

Where,
Lo = Liquid Reflux Rate, kgmole/hr.
D = Distillate Product Rate, kgmole/hr
T

Correlating Parameter

a = Relative Volatility
i = any component
X = Liquid Rate, kgmole/h

Set reflux ratio and calculate number of theoretical stages

It is customary to always add a certain safety margin above the minimum reflux level to
avoid potential errors from VLE estimation or from misdistribution at the desired reflux
ratio. The rule of thumb for R/Rmin which is regarded satisfactory as a general guideline is
listed below

There are several considerations in deciding the reflux ratio; the following comments indicate
the effect of a change in the reflux ratio in relation to the number of stages.

The higher the reflux rate, the higher the cost of condensing and reboiling. These
make up the bulk of the column operating costs.
As reflux ratio increases, the number of stages decreases, but column diameter
increases.
Close to minimum reflux rate, small increases in reflux ratio will reduce the number
of stages considerably and therefore column height, but produce only a small increase
in column diameter.
Further increases in reflux will have a smaller effect in the height reduction but
greater increase in column diameter.

The closest possible approach of design to minimum reflux requires accurate methods such as
vigorous stage wise calculations, developed by multiple cases on computers.
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Determination of Number of theoretical stages:

The number of theoretical stages required for a given separation at a reflux ratio between
minimum and total reflux can be determined from Erbar and Maddox Correlation. This
correlation relates the ratio of minimum stages to theoretical stages to the minimum reflux
ratio and the operating reflux ratio as shown below:
We have calculated
Minimum Reflux Ratio = Rm = (Lo/V) m
Minimum number of stages = Sm
R = (Lo/V) = Reflux Ratio.
Knowing Sm/S from the graph below we can calculate S = Number of stage

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Adjust actual reflux for feed vaporization if necessary

The Erbar and Maddox correlation is based on bubble point feed. For a feed stream between
the bubble point and dew point the following relationship adjusts the vapor rate from the top
tray for non bubble point feed.

V = Vapor rate, kg mol/hr

D = Overhead product rate, kg mol/hr
F = Feed rate, kg mol/hr
HVF = Vaporized feed stream enthalpy, Kcal/Kg mol
HBP = Bubble point feed stream enthalpy, Kcal/Kg mol
QC = Condenser duty Kcal/hr
LO = Liquid condensed in a partial condenser, Kg mol/h
Determination of feed location
Once a base case tower has been simulated, optimization studies on trays vs. reflux, feed tray
location, etc. can be carried out. One criterion often used for optimum location of the feed
tray is to try and match the feed composition as closely as possible to a corresponding tray
composition. The approximate feed location can be determined by the ratio of the total
number of theoretical stages above and below the feed plate from following equation:

Fenskes Equation
Kirkbridges Equation
Akashahetals Correction

Fenskes Equation

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CONCLUSION
Generally, the efficiency of any distillation column is its ability to produce maximum output
with minimum cost as much as possible. Thus the design considerations discussed in the
preceding section tend to achieve this goal; perhaps the is no other consideration that can be
place above this in terms of importance.

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REFERENCE
1. Coulson and Richardsons chemical engineering series volume 2 and 6 by J. M.
COULSON & J. F. RICHARDSON
2. Perrys Chemical Engineers Handbook; 7 th Edition
3. http://www.artisan-distiller.net/phpbb3/viewypic.php?f=2326&start=15
4. http://www.lorien.ncl.ac.uk/ming/distil/distil0.htm
5. http://www.seperatontechnology.com/distillation-design/

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