CHAPTER 1

INTRODUCTION
Distillation is a physical process for the separation of liquid mixtures that is based on differences
in the boiling points of the constituent components. Distillation is the most widely separation
process used in many industries. Distillation makes about 95% of all current industrial
separation processes. It has been used in chemical industries, pharmaceutical and food
industries, environmental technologies and in petroleum-refineries. The most common use is
after a chemical reactor where we obtain some products. Distillation is used in order to separate
the desired product from the rest obtaining a high purity product. Examples of the most
important applications in food industries are concentrating essential oils and flavors; the
deodorization of fats and oils or in alcohol distillation. Some pharmaceutical processes based on
concentration of antibiotics are also related with distillation columns.
On the other hand, distillation is the main part in petroleum refineries. The crude oil which
contains a complex mixture of hydrocarbons is pumped into a huge distillation column in order
to be separated them by different temperatures. Environmental legislation is becoming very
strict. Consequently, plants for the recovery and cleaning of solvents are continually gaining in
importance in order to avoid the waste emit into the environment. So separation processes are
very important, and distillation is one of this which is used for example in water treatments,
etc… As we can see, distillation is applied for many different processes because of its reliability,
simplicity and low-capital costs although these systems have relatively high energy
consumption. However, there are many active researches regarding making the process more
energyefficient.
Distillation is the process of heating a liquid until some of its ingredients pass into the vapor
phase, and then cooling the vapor to recover it in liquid form by condensation. The main
purpose of distillation is to separate a mixture by taking advantage of different substances’
readiness to become a vapor. If the difference in boiling points between two substances is great,
complete separation may be easily accomplished by a single-stage distillation. If the boiling
points differ only slightly, many redistillations may be required. In the simplest mixture of two
mutually soluble liquids with similar chemical structures, the readiness to vaporize of each is
undisturbed by the presence of the other. The boiling point of a 50-50 mixture, for example,
would be halfway between the boiling points of the pure substances, and the degree of
separation achieved by a single distillation would depend only on each substance’s readiness to
vaporize at this temperature.
There are a variety of configurations for distillation columns, each designed to perform specific
types of separations. A simplified way of classifying distillation columns is to look at how they
are operated. In this manner, the two major types are batch and continuous columns. In a batch
operation, the feed to the column is introduced batch-wise. That is, the column is charged with a
‘batch’ and then the distillation process is conducted. When the desired separation is achieved, a
next batch of feed is introduced. In contrast, continuous columns process a continuous feed
stream.

1
1.1 HISTORY
Distillation was developed into its modern form with the invention of the alembic by Islamic
alchemistJabir ibnHayyan in around 800 C.E. He is also credited with the invention of numerous
other chemical apparatus and processes that are still in use today.
The design of the alembic has served as an inspiration for some modern micro-scale distillation
apparatus such as the Hickman still head.
As alchemy evolved into the science of chemistry, vessels called retorts became used for
distillation Both alembics and retorts are forms of glassware with long necks pointing to the side
at a downward angle which act as air-cooled condensers to condense the distillate and let it drip
downward for collection.
Later, copper alembics were invented. Riveted joints were often kept tight by using various
mixtures, for instance a dough made of rye flour. These alembics often featured a cooling
system around the beak, using cold water for instance, which made the condensation of alcohol
more efficient. These were called pot stills.

2
CHAPTER 2

THEORY
The process of distillation begins with a feed stream that requires treatment. The feed is
separated into two fractions in a conventional column (Fig1.): the light product and the heavy
product. Throughout the report, the feed molar flow rate F will be reported by (kgmol/h) feed
mole fraction is z and the stage that feed enters is denoted by NF (normally the tray on which
the characteristics of the fluid is closest to that of the feed).

Fig 2.1 Distillation Column

As it shown in Fig.2.1 the liquid leaving the top of the column is the light component, while the
liquid leaving the bottom of the column is the heavy component. Liquid leaving the bottom of
the column is split into a bottoms product and a fraction that is made available for boiling.
The reboiler (heat exchanger) is employed to boil the portion of the bottom liquid that is not
drawn off as product. The vapor produced flows up through the column and comes into intimate
contact with the downflowing liquid. After the vapor reaches and leaves the top of the column,
another heat exchanger (the condenser) is encountered where heat is removed from the vapor to
condensate it. The condensed liquid is split into two streams. One is the overhead product; the
other liquid stream is called reflux and is returned to the top of the column to improve the
separation.
3
 CHAPTER 3

NDA FUNDAMENTALS OF VAPOR – LIQUID PHASE

EQUILIBRIUM
The process of distillation is aimed at the separation of components from a liquid mixture. This
process 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. This means that distillation processes depends on the
vapor pressure characteristics of liquid mixtures.
The vapor pressure of a liquid at a particular temperature is the equilibrium pressure exerted by
molecules leaving and entering the liquid surface. Some general concepts to recognize about
regarding vapor pressure are first, energy input raises the vapor pressure. Also, vapor pressure is
related to boiling. A liquid boils when its vapor pressure equals the surrounding pressure. The
ease with which a liquid boils depends on its volatility. Liquids with high vapor pressures (i.e.,
volatile liquids) will boil at lower temperatures. We should also recognize that the vapor
pressure and hence the boiling point of a liquid mixture depends on the relative amounts of the
components in the mixture. Distillation is accomplished because of the differences in the
volatility of the components in a liquid mixture.
It is the boiling point diagram that provides an understanding of the process. 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. Figure 3.1 shows the boiling point diagram for this binary mixture. The
boiling point of A is that at which the mole fraction of A is unity. The boiling point of B is that
at which the mole fraction of A is zero. 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 the lower one is called the bubble-point curve. The region above the dew-
point curve shows the equilibrium composition of the superheated vapor 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.

Figure 3.1 boiling point curve

4
This difference between liquid and vapor compositions is the basis for any distillation process.
A term of great importance is relative volatility. Relative volatility is a measure of the
differences in volatility between two 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 by the followingrelationship:

∝ij = (yi / xi ) / ( yj / x j )

Where yiis the mole fraction of component “i” in the vapor, and xi is the mole fraction of
component “i” in the liquid. We can conclude that if the relative volatility between two
components is very close to one, it is an indication that they have very similar vapor pressure
characteristics. This means that they have very similar boiling points and therefore, it will be
relatively difficult to separate the two components by means of distillation.
Since the boiling point properties of the components in the mixture being separated are so
critical to the distillation process, the vapor-liquid equilibrium (VLE) relationship is of
importance. Specifically, it is the VLE data for a mixture which establishes the required height
of a column for a desired degree of separation. Constant pressure VLE data is derived from
boiling point diagrams, from which a VLE curve can be constructed. The VLE plot shown
expresses the bubble-point and the dew-point of a binary mixture at constant pressure. The curve
is called the equilibrium line, and it describes the compositions of the liquid and vapor in
equilibrium at a constant pressure condition.

Figure 3.2 VLE diagram

The design of a distillation column is based on information derived from the VLE diagram
describing the mixtures to be separated. The vapor-liquid equilibrium characteristics are
indicated by the characteristic shapes of the equilibrium curves. This is what determines the
number of stages, and hence the number of trays needed for a separation.

5
 CHAPTER 4

TYPES OF DISTILLATION

 Simple or BatchDistillation
 FractionalDistillation
 FlashDistillation
 SteamDistillation
 VacuumDistillation
 AzeotropicDistillation

4.1 BATCHDISTILLATION

In batch operation, the feed is introduced batch-wise to the column. That is, the column is
charged with a 'batch' and then the distillation process is carried out. When the desired task is
achieved, a next batch of feed is introduced. Consider a binary mixture of components A (more
volatile) and B (less volatile). The system consists of a batch of liquid (fixed quantity) inside a
kettle (or still) fitted with heating element and a condenser to condense the vapour produced as
shown in figure 4.1

Figure 4.1 Simple Batch or Differential Distillation Process

6
The condensed vapour is known as the distillate. The distillate is collected in a
condensate4receiver. The liquid remaining in the still is known as the residual. The process is
unsteady state. The concentration changes can be analyzed using the phase diagram, and detailed
mathematical calculations carried out using the Rayleigh Equation. As the process is unsteady
state, the derivation is based on a differential approach to changes in concentration with time.

Let L1 = initial moles of liquid originally in still,

L2 = final moles of liquid remained in still,

x1 = initial liquid composition in still (mole fraction of A),

x2 = final liquid composition in still (mole fraction A).

At any time t, the amount of liquid in the still is L, with mole fraction of A in the liquid being
x. After a small differential time (t + dt), a small amount of vapor dL is produced, and the
composition of A in the vapor is y (mole fraction). The vapor is assumed to be in equilibrium
with the residue liquid. The amount of liquid in the still is thus reduced from L to (L - dL), while
the liquid composition changed from x to (x - dx). Then the material balance on A can be
written as:

Initial amount in still = Amount left in still + Amount vaporized xL = (x - dx)(L - dL) + ydL
or
xL = xL - xdL - Ldx + dxdL + ydL (1.1)
Neglecting the term (dx)(dL), the Equation (1.1) may be written as: Ldx = ydL – xdL

Re-arranging and Integrating from L1 to L2, and from x1 to x2, one can obtain the following
Equation which is called Rayleigh Equation:

The integration can be obtained graphically from the equilibrium curve, by plotting 1/(y-x)
versus x.

7
4.2 FRACTIONAL DISTILLATION

For many cases, the boiling points of the components in the mixture will be sufficiently close
that Raoult's law must be taken into consideration. Therefore, fractional distillation must be
used in order to separate the components by repeated vaporization-condensation cycles within a
packed fractionating column. This separation, by successive distillations, is also referred to
asrectification.
As the solution to be purified is heated, its vapors rise to the fractionating column. As it rises, it
cools, condensing on the condenser walls and the surfaces of the packing material. Here, the
condensate continues to be heated by the rising hot vapors; it vaporizes once more. However,
the composition of the fresh vapors are determined once again by Raoult's law. Each
vaporization-condensation cycle will yield a purer solution of the more volatile
component.Infractionating column; theoretical plate is thus a concept rather than an accurate
description.
More theoretical plates lead to better separations. A spinning band distillation system uses a
spinning band of Teflon or metal to force the rising vapors into close contact with the
descending condensate, increasing the number of theoretical plates.

4.3 STEAM DISTILLATION

Like vacuum distillation, steam distillation is a method for distilling compounds which are
heat-sensitive. The temperature of the steam is easier to control than the surface of a heating
element, and allows a high rate of heat transfer without heating at a very high temperature. This
process involves bubbling steam through a heated mixture of the raw material. By Raoult's law,
some of the target compound will vaporize (in accordance with its partial pressure). The vapor
mixture is cooled and condensed, usually yielding a layer of oil and a layer of water.
Steam distillation of various aromatic herbs and flowers can result in two products; an
essential oil as well as a watery herbal distillate. The essential oils are often used in perfumery
and aromatherapy while the watery distillates have many applications in
aromatherapy,food processing and skincare.

4.4 VACUUM DISTILLATION

Some compounds have very high boiling points. To boil such compounds, it is often better to
lower the pressure at which such compounds are boiled instead of increasing the temperature.
Once the pressure is lowered to the vapor pressure of the compound (at the given temperature),
boiling and the rest of the distillation process can commence. This technique is referred to as
vacuum distillation and it is commonly found in the laboratory in the form of the rotary
evaporator.
This technique is also very useful for compounds which boil beyond their
decompositiontemperatureat atmospheric pressure and which would therefore be decomposed
by any attempt to boil them under atmosphericpressure.
Molecular distillation is vacuum distillation below the pressure of 0.01 torr. 0.01 torr is one
orderofmagnitudeabovehighvacuum,wherefluidsareinthefreemolecularflowregime,
8
 i.e. the mean free path of molecules is comparable to the size of the equipment. The gaseous
phase no longer exerts significant pressure on the substance to be evaporated.

4.5 AZEOPROPIC DISTILLATION

Interactions between the components of the solution create properties unique to the solution, as
most processes entail nonideal mixtures, where Raoult's law does not hold. Such interactions can
result in a constant-boiling azeotropewhich behaves as if it were a pure compound (i.e., boils at
a single temperature instead of a range). At an azeotrope, the solution contains the given
component in the same proportion as the vapor, so that evaporation does not change the purity,
and distillation does not effectseparation. For example, ethylalcohol and water form an
azeotrope of 95.6% at 78.1°C.
If the azeotrope is not considered sufficiently pure for use, there exist some techniques to break
the azeotrope to give a pure distillate. This set of techniques are known as azeotropic
distillation. Some techniques achieve this by "jumping" over the azeotropic composition (by
adding another component to create a new azeotrope, or by varying the pressure). Others work
by chemically or physically removing or sequestering the impurity. For example, to purify
ethanol beyond 95%, a drying agent (or desiccant, such as potassium carbonate) can be added to
convert the soluble water into insoluble water of crystallization. Molecularsieves are often
used for this purpose aswell.
Immiscible liquids, such as water and toluene, easily form azeotropes. Commonly, these
azeotropes are referred to as a low boiling azeotrope because the boiling point of the azeotrope
is lower than the boiling point of either pure component. The temperature and composition of
the azeotrope is easily predicted from the vapor pressure of the pure components, without use of
Raoult's law. The azeotrope is easily broken in a distillation set- up by using a liquid–liquid
separator (a decanter) to separate the two liquid layers that are condensed overhead. Only one of
the two liquid layers is refluxed to the distillation set-up.
High boiling azeotropes, such as a 20 weight percent mixture of hydrochloric acid in water, also
exist. As implied by the name, the boiling point of the azeotrope is greater than the boiling point
of either pure component.

4.6 INDUSTRIAL DISTILLATION

Large scale industrial distillation applications include both batch and continuous fractional,
vacuum, azeotropic, extractive, and steam distillation. The most widely used industrial
applications of continuous, steady-state fractional distillation are in
petroleumrefineries,petrochemical and chemical plants and natural gas processingplants.
To control and optimize such industrial distillation, a standardized laboratory method, ASTM
D86, is established. This test method extends to the atmospheric distillation of petroleum
products using a laboratory batch distillation unit to quantitatively determine the boiling range
characteristics of petroleumproducts.
Industrial distillation is typically performed in large, vertical cylindrical columns known as
distillation towers or distillation columnswith diameters ranging from about 65 centimeters
to 16 meters and heights ranging from about 6 meters to 90 meters ormore.
9
 Figure 4 .2 Typical Industrial Distillation Tower

When the process feed has a diverse composition, as in distilling crude oil, liquid outlets at
intervals up the column allow for the withdrawal of different fractions or products having
different boiling points or boiling ranges. The "lightest" products (those with the lowest boiling
point) exit from the top of the columns and the "heaviest" products (those with the highest
boiling point) exit from the bottom of the column and are often called the bottom.
Such industrial fractionating towers are also used in cryogenic air separation, producing
liquid oxygen,liquid nitrogen, and high purity argon. Distillation of chlorosilanesalso enables
the production of high-purity silicon for use as asemiconductor.
Design and operation of a distillation tower depends on the feed and desired products. Given a
simple, binary component feed, analytical methods such as the McCabe–Thielemethodor the
Fenskeequationcan be used. For a multi-component feed, simulation models are used
both for design and operation. Moreover, the efficiencies of the vapor–liquid contact devices
(referred to as "plates" or "trays") used in distillation towers are typically lower than that of a
theoretical 100% efficient equilibrium stage. Hence, a distillation tower needs more trays than
the number of theoretical vapor–liquid equilibrium stages. A variety of models have been
postulated to estimate trayefficiencies.
In modern industrial uses, a packing material is used in the column instead of trays when low
pressure drops across the column are required. Other factors that favor packing are: vacuum
systems, smaller diameter columns, corrosive systems, systems prone to foaming, systems
requiring low liquid holdup, and batch distillation. Conversely, factors that favor platecolumns
are: presence of solids in feed, high liquid rates, large column diameters, complex columns,
columns with wide feed composition variation, columns with a chemical reaction, absorption
10
 columns, columns limited by foundation weight tolerance, low liquid rate.

This packing material can either be random dumped packing (1–3" wide) such as Raschig
rings or structured sheet metal. Liquids tend to wet the surface of the packing and the vapors
pass across this wetted surface, where masstransfertakes place. Unlike conventional tray
distillation in which every tray represents a separate point of vapor–liquid equilibrium, the
vapor–liquid equilibrium curve in a packed column is continuous. However, when modeling
packed columns, it is useful to compute a number of "theoretical stages" to denote the
separationfficiency of the packed column with respect to more traditional trays. Differently
shaped packings have different surface areas and void space between packings. Both of these
factors affect packing performance.
Another factor in addition to the packing shape and surface area that affects the performance of
random or structured packing is the liquid and vapor distribution entering the packed bed. The
number of theoretical stages required to make a given separation is calculated using a specific
vapor to liquid ratio. If the liquid and vapor are not evenly distributed across the superficial
tower area as it enters the packed bed, the liquid to vapor ratio will not be correct in the packed
bed and the required separation will not be achieved. The packing will appear to not be working
properly. The height equivalent to a theoretical plate (HETP) will be greater than expected. The
problem is not the packing itself but the mal-distribution of the fluids entering the packed bed.
Liquid mal-distribution is more frequently the problem than vapor. The design of the liquid
distributors used to introduce the feed and reflux to a packed bed is critical to making the
packing perform to it maximum efficiency. Methods of evaluating the effectiveness of a liquid
distributor to evenly distribute the liquid entering a packed bed can be found in
references.Considerable work has been done on this topic by Fractionation Research, Inc.
(commonly known asFRI).

4.7 MULTI – EFFECT DISTILLATION

The goal of multi-effect distillation is to increase the energy efficiency of the process, for use in
desalination, or in some cases one stage in the production of ultrapure water. The number of
effects is inversely proportional to the kW·h/m3 of water recovered figure, and refers to the
volume of water recovered per unit of energy compared with single-effect distillation. One
effect is roughly 636kW·h/m3.

 Multi-stage flash distillation can achieve more than 20 effects with thermal energy input, as
mentioned in thearticle.
 Vapor compression evaporation – Commercial large-scale units can achieve around 72 effects
with electrical energy input, according tomanufacturers.
There are many other types of multi-effect distillation processes, including one referred to as
simply multi-effect distillation (MED), in which multiple chambers, with intervening heat
exchangers, are employehcontractors
The typical gas-liquid contacting operations include distillation, absorption, stripping, leaching
and humidification. Distillation and absorption are two most widely used mass transfer
processes in chemical industries. Design of plate column for absorption and distillation involves

11
many common steps of calculation such as determination of number of theoretical plates,
column diameter, plate hydraulic design, etc.In absorption process, a soluble component is
absorbed in a liquid (called solvent) from a gaseous mixture. The gas and liquid streams leaving
the tray are in equilibrium under the ideal condition. The separation in distillation is based on
the relative volatility of the components. Additional vapor phase is generated by the
vaporization of more volatile components (called stripping) and by condensation of relatively
less volatile components(called absorption) adds to the liquidphase.

12
 CHAPTER 5

THEORTICAL FACTORS OF DISTILLATION COLUMN

5.1 SELECTION OF COLUMN TYPE

Plate or Packed: Packed towers (columns) are also used as the contacting devices for gas
absorption, liquid-liquid extraction and distillation. The gaseous mixture is allowed to contact
continuously with the liquid counter-currently in a packed column. The liquid flows downward
over the packing surface, and the gaseous mixture flows upward through the space in the
packing. The performance of the column strongly depends on the arrangement of the packings to
provide good liquid and gas contact throughout the packed bed. The solute gas is absorbed by
the fresh solvent (liquid) entering at the top of the tower where the lean gas leaves system. The
liquid enriched with absorbed solute gas, leaves the column bottom through the exit port. In a
plate tower, the liquid and gas are contacted in stage-wise manner on the trays; while gas-liquid
contact is continuous in a packed column. There are always some uncertainly to maintain good
liquid distribution in a packed tower. For this reason, it is difficult to accurately estimate the
packed tower efficiency. The course content is limited to design of plate column only and some
typical criterions for the selection of column type are discussed below.

The relative merits of plate over packed column are as follows:

1. Handle wide range of liquid flow rates withoutflooding.

2. If a system contains solid contents; it will be handled in plate column, becausesolid

accumulate in the voids, coating the packing materials and making itineffective.

3. Dispersion difficulties are handled in plate column when flow rate of liquid are low
compared togases.

4. For large column heights, weight of the packed column is more than platecolumn.

5. If periodic cleaning is required, man holes will be provided for cleaning. In packed columns
packing must be removed before cleaning.

6. For non-foaming systems the plate column ispreferred.

7. Design information for plate column is more readily available and more reliable thanthat for
packedcolumn.

8. Inter stage cooling can be provided to remove heat of reaction or solution in platecolumn.

13
5.1.1 Platetypes
Gas and liquid flow across the tray can either be by cross-flow or counter-flow manner . The
cross-flow plates are most widely practiced and the three main types of cross flow plates are:
bubble cap, valve and sieve trays with downcomer.

Figure 5.1 Classification of plate types based on flow mode- side view shown: (a) Cross- flow
plate, (b): Counter flow plate.

5.1.2 Bubble cap plates

An enhanced gas-liquid contact can be achieved having bubble caps on the tray at very low
liquid flow rates. A bubble cap consists of a riser (also called chimney) fixed to the tray through
a hole and a cap is mounted over the riser (Figure 7.5). The gas flows up through the riser,
directed downward by the cap through the annular space between riser and cap. Finally, the gas
is dispersed into the liquid. A number of slots in the lower part of the cap help in gas bubble
dispersion. Un-slotted types of cap designs are also common in application. Bubble caps are
especially suitable for higher turndown ratio. Turndown ratio is the ratio of maximum operating
vapor rate to the minimum allowable vapor rate, below which weeping starts.

Figure 5.2 Bubble caps

14
5.1.3 Valve plates

Valve trays are the modified design of sieve trays where relatively large plate perforations are
covered by movable caps/valves . Valves cover may be round or rectangular. The very common
hole diameter is 40 mm but upto 150 mm are also used. The valve lifts up as the vapor flow rate
increases and the valve sits over the perforation at lower flow rate, thus stops the liquid from
weeping. Valve trays provide good vapor-liquid contact at low flow rates (high turndown ratio).

Figure 5.3Valve tray

5.1.3 Sieveplate

The sieve tray (also known as perforated plate) is a flat perforated metal sheet.Thehole diameter
from 1.5 to 25 mm are very commonly used. The sieve tray layout is a typical square or
equilateral triangular pitch holes. The gas/vapor flows upward through the perforation and
disperses into the flowing liquid over the plate. There is no liquid seal in case of trays without
downcomer and the liquid weeps (called weeping) through the holes at low flow rates, reducing
the efficiency of plate. For this reason, sieve tray has the lowest turndown ratio. Sieve tray
construction is simple and relativelycheap.

Figure 5.4 Sieve tray

15
 5.2 SELECTION OF TRAY TYPE

The comparative performances of three common types of trays are summarized in Table 5.1.
The capacity, efficiency, pressure drop and entrainment of sieve and valve trays are almost
same. Bubble cap trays have lower capacity and efficiency and but higher pressure drop and
entrainment compared to valve and sieve trays. The turndown ratio comes in the order of:
bubble cap>valve>sieve. However, valve trays have the best turndown ratio in case of refinery
applications. Sieve trays are the least expensive and suitable for almost all applications.
Cap trays should be used at very low liquid flow rate which is not achievable using sieve trays.

Table 5.1: Comparison of three types of cross-flow trays

5.2 FACTORS AFFECTING

Operation Vapor FlowConditions
1. Foaming
2. Entrainment
3. Weeping/dumping
4. Flooding

Foaming

• Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it provides
high interfacial liquid-vapor contact, excessive foaming often leads to liquid buildup on trays. In
some cases, foaming may be so bad that the foam mixes with liquid on the tray above. Whether
foaming will occur depends primarily on physical properties of the liquid mixtures, but is
sometimes due to tray designs and condition. Whatever the cause, separation efficiency is
alwaysreduced.

Entrainment

• Entrainment refers to the liquid carried by vapor up to the tray above and is again caused by
high vapor flow rates. It is detrimental because tray efficiency is reduced: lower volatile material
is carried to a plate holding liquid of higher volatility. It could also contaminate high purity
16
 distillate. Excessive entrainment can lead toflooding.

Weeping/Dumping

• This phenomenon is caused by low vapor flow. The pressure exerted by the vapor is insufficient
to hold up the liquid on the tray. Therefore, liquid starts to leak through perforations. Excessive
weeping will lead to dumping. That is the liquid on all trays will crash (dump) through to the
base of the column (via a domino effect) andthe column will have to be re-started. Weeping is
indicated by a sharp pressure drop in the column and reduced separationefficiency.

Flooding

• Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the vapor
up the column. The increased pressure from excessive vapor also backs up the liquid in the
down comer, 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
separationefficiency.

Reflux Conditions

• Minimum trays are required under total reflux conditions, i.e. there is no withdrawal of distillate.
On the other hand, as reflux is decreased, more and more trays are required.

Feed Conditions

• The state of the feed mixture and feed composition affects the operating lines and hence the
number of stages required for separation. It also affects the location of feed tray.

State of Trays and Packings

• Remember that the actual number of trays required for a particular separation duty is determined
by the efficiency of the plate. Thus, any factors that cause a decrease in tray efficiency will also
change the performance of the column. Tray efficiencies are affected by fouling, wear and tear
and corrosion, and the rates at which these occur depends on the properatedties of the liquids
being processed. Thus appropriate materials should be specified for trayconstruction.

Column Diameter

• Vapor flow velocity is dependent on column diameter. Weeping determines the minimum vapor
flow required while flooding determines the maximum vapor flow allowed, hence column
capacity. Thus, if the column diameter is not sized properly, the column will not perforated

17
CHAPTER 6

ANALYSIS OF DISTILLATION COLUMN

6.1 MECAB THIELE METHOD

This method uses the equilibrium curve diagram to determine the number of theoretical stages
(trays) required toachieve a desired degree of separation. It is a simplified method of analysis
making use of several assumptions, but nonetheless a very useful tool for the understanding of
distillationoperation.

6.1.1 Analysis using the McCabe-ThieleMethod

The following notations shall be used :

y : mole fraction of more volatile component in vapour phase x : mole fraction of more volatile
component in liquid phase V : molar flowrate of vapour, mole/time
L : molar flowrate of liquid, mole/time
F : molar flowrate of feed (vapour or liquid or mixed), mole/time

Refer to the Figure 2.1 below that shows several plates inside a distillation column. Assume that
the plates are numbered serially from the top down and that the plate under consideration is the
n-th plate from the top. Then the plate immediately above this plate is plate (n-1) and the plate
immediately below this plate is plate (n+1).

Figure 6.1

18
 Table 6.1

Stream TotalMolar Composition(Mole

Flowrate FractionMVC)

Vapour
leaving Vn Yn
plate
Liquid
leaving Ln Xn
plate
Vapour xn-1
entering Vn+1
plate
Liquid xn-1
entering Ln-1
plate

The VLE data must be available at the operating pressure of the column.

Information required are the feed condition (temperature, composition), distillate and bottom
compositions; and the reflux ratio, which, as we seen earlier, is defined as the ratio of reflux
liquid over the distillate product. This is shown in the Figure below.

Figure 6.2

19
For example, a column is to be designed for the separation of a binary mixture. The feed has a
concentration of xF (mole fraction) of the more volatile component, and a distillate having a
concentration of xDof the more volatile component and a bottoms having a concentration of xB
isdesired.

In its essence, the method involves the plotting on the equilibrium diagram 3 straight lines: the
rectifying section operating line (ROL), the feed line (also known as the q-line) and the
stripping section operating line(SOL).

Each of these lines passes through the points representing the mole fractions of the more volatile
component in the distillate, bottoms and feed (xD, xB and xF) respectively. These lines
represent the relationship between the concentrations in the vapour phase (y) and the liquid
phase (x).

The number of theoretical stages required for a given separation is then the number of triangles
that can be drawn between these operating lines and the equilibrium curve. The last triangle on
the diagram represents the reboiler.

To obtain the number of theoretical trays using the McCabe-Thiele Method, we shall used the
"Parts-Whole Relationship": analysis is first carried out by partitioning the column into 3
sections: rectifying, feed and stripping sections as shown in left Figure below. These sections are
then represented on the equilibrium curve for the binary mixture in question and re- combined to
make a complete design, as shown in the right Figure

Figure 6.3

20
 Figure 6.4

In the simplest case, the McCabe-Thiele Method to determine the number of theoretical stages
follows the steps below:

1. Analysis of the Rectifying section, and determine the ROL using xD andR
2. Analysis of the Feed section, and determine the feed condition(q)
3. Determination of the feed line (q-line) using xF andq
4. Locate the intersection point between ROL andq-line
5. Analysis of the Stripping Section, and determine the SOL andxB

On the completed design (equilibrium diagram): The number of triangles drawn = Number of
theoretical trays + 1 Reboiler (last triangle).
As an example, see the Figure above. The number of theoretical trays = 6 + 1 Reboiler

21
For a given separation from a given feed condition using reflux ratio will result in lesser number
of theoretical trays required and vice versa. In other words, there are many possible combination
of reflux ratio R and number of theoretical trays, N.

7.2 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. See the
followinganimation:
Recall the operating line equation for the rectifying section:

At a specified distillate concentration (i.e. constant xD), when R changes, the slope and intercept

of the ROL changes. The ROL therefore rotates around the point (xD, xd )

When the required separation is clearly defined - with a given feed condition (i.e. x F and q
and a specified product compositions (i.e. xDand xB fixed) - increasing R will results in lesser
number of theoretical stagesrequired.
From the ROL equation, we can see that when R increases (with x Dconstant), the slope of ROL
becomes steeper, i.e. (R/R+1) and the intercept (xD/R+1) decreases. This is shown in
theFigurebelow.

Figure 6.5

22
Thus, as R increases, the ROL rotates downwards around (xD, xD). The SOL also moved down
accordingly. The area between the equilibrium curve and ROL is now larger, and we can draw
larger triangles between the operating lines. This means that there are now greater driving force
for separation, which in turns mean that lesser number of theoretical stages are required. The
reverse is true when Rdecreases.
The reflux ratio can assume any number between a minimum value and an infinite value, and
the number of theoretical stages required for separation changes accordingly. In the next
sections, we will first look at two extremes of the reflux ratios, and then an analysis of how the
most suitable reflux ratio is determined. At one end of the limit is the minimum refluxratio (that
results in infinite stages) and at the other end is the total reflux or infinite refluxratio (which
results in minimum stages). The minimum reflux ratio and the infinite reflux ratio place a
constraint on the range of separation operation. Any reflux ratio between Rmin and Total R
will produce the desired separation, with the corresponding number of theoretical stages varying
from infinity at Rmin to the minimum number (Nmin at Total R). The relationship between R and
N is shown in the Figure below. The choice of reflux ratio to use is governed by
costconsiderations.

23
 CHAPTER 7

Column Principal Dimensions (D/H)

• A design guideline that should be used is thatthe
• height of the column should not be higher than 175 ft.
• Height-to-diameter ratio should be less than 20 to 30.
• Packed towers are used when column has small Dia (1.5 ft) or area ( 1.77ft2) rather than
platetowers.
• Either plate or packed towers may be used when the column Dia is between 1.5-4.5 ft (area:
1.77- 15.9 ft2).
• If the tower is higher than 190 ft, then a design with smaller tray spacing should be considered.
• The tower height can be related to the number of trays in the column. The following formula
assumes that a spacing of two feet between trays will be sufficient including additional 5-10 ft at
both ends of the tower. This includes a fifteen percent excess allowance ofspace.

Htower = 2.3 * Nactual

7.1 DESIGNING STEPS OFCOLUMN

Calculation of:
 optimum reflux ratio.
 Minimum refluc ratio.
 theoretical number ofstages.
 actual number ofstages.
 height of the column.
 diameter of thecolumn.

7.2 GRAPHICALMETHOD

Step 1. Determine Process Operation Variables (F, D, W, xF ,xD , xW)

F=D+W

Step 2. Determine the Minimum Reflux Ratio

Y = αx / 1 + x (α-1)

Step 3. Choose Actual Reflux Ratio

Ractual =Rmin *1.2

24
Step 4. Determine the Minimum Number of Trays
Step 5. Determine Actual Number of Trays
Nactual = Nth/
Step 6 . Dimensions of Column (Diameter/Height):
Htower = 2.3  Nactual

Figure7.1

Figure7.2

25
 Flow parameter (Rectifying section):
0.5
FLG =

7.3 : CAPACITY PARAMETERS

• Assumed tray spacing = 18in.

• From Fig, sieve tray flooding capacity, Csb(18) = ……….m/s

• Surface tension,  = ……..dynes/cm

• CorrectedCsb

•
Unf = Csbf( 𝜎/20)0.2 ( (𝜌𝑙 − 𝜌𝑣)/𝜌𝑣)0.5


• Diameter

26
CHAPTER8 .

DESIGN PROBLEM

8.1 PROBLEM 1

100 kmol/h of a bubble point mixture of 75 mol% water and 25 mol% acetic acid is
distilled continuously in a distillation tower at a pressure of 1 atmosphere. Distillate
contains 95 mol % of light component and bottom 95 mol% of heavy component. The
reflux ratio is 2 times of minimum reflux ratio. Determine the number of theoretical plates.
DATA
Table 8.1 :Equilbirium data for Water and Acetic Acid at 1 atm. ( mol fraction )

X Y
0.0055 0.0112
0.053 0.133
0.125 0.240
0.206 0.338
0.297 0.437
0.510 0.630
0.649 0.751
0.803 0.866
0.9594 0.9725
1 1

SOLUTION
Step 1 : Scheme and material balance

Figure 8.1 - Distillation column

F = D+B
Fxf = Dxd + Bxb (xf)W=0.75
(xf)A =0.25

(xd)A =0.95
(xd)A =0.05
(xb)W =0.95
F = 100
100 = D+B
100(0.25) = D(0.95) + B(0.05)
25 = 0.95D + ( 100-D )0.05
25 = 0.95D +5-0.05D
20 = 0.9D D = 20/0.9 D = 22.22

F = D+B
100 = 22.22 + B
B = 77.77

Step 2 : Prepare x-y diagram using equilibrium data

Figure 8.2 : x-y diagram

Step 3 : Select the point Xd, Xf, Xb

Figure 8.3 - point Xd,Xf, Xb on x- y diagram

Step 4 : Draw q- line

q-line
line is graphical interpretation of material balance of the feed stage , q represents the
amount of liquid
uid that accumulates at the feed stage by feeding of 1 kmol of the feed.
q-line equation
y =(qx / q-1 ) - ( xf / q - 1 ) For bubble point liquid, q=1
 Figure 8.4 - q line on x- y diagram

Step 5 : Calculation
ulation of minimum reflux ratio Rmin the operating line in the rectifying
section of the column for at Rmin should be drawn.

y = ( Rmin x / Rmin + 1 ) + ( xD
D / Rmin + 1 )

We have two points of this line one is the intersection of the q-line
q line and equilibrium
equilibri curve
and another in the intersection of 450 line and xDline.
 Figure 8.55 - Intercept on x-y diagram
The minimum reflux ratio can be calculated from the slope of this line
Rmin = ( xD- y, ) / ( y, - x, )
Rmin = ( 0.95 - 0.83 ) / ( 0.83 - 0.7 )
Rmin = 0.92

Step 6 : Reflux ratio , R = 1.2 Rmin R = 1.2 ( 0.92 )

R = 1.104

Step 7 : Intercept of the line is

xD// R + 1 = 0.95 / ( 1.104 + 1 ) = 0.35

Step 8 : Draw the operating line of the stripping section of the column , by connecting
point of intersection of q-line
line and operating line of rectifying section of point ( xxw , xw )

Step 9 : Draw steps between equilibrium line and operating line

 Figure 8.5 : Number of stages on x-y
x diagram

Number of theoretical stages = 14

Number of actual plates = 14 – 1 = 13
8.2 PROBLEM 2

100 kmol/h of a bubble point mixture of benzene and toluene containing 60 mole %
benzene is to be seperated to give a product of 95 mole % benzene and a bottom product
containing 10 mole % benzene. The feed enter a column at its bubble point. It is proposed
to operate the column with reflux ratio of 2.5. it is required to find the number of
theoretical and actual plates needed .
DATA
Table 8.2 : Equilibrium data
X y
0 0
0.1 0.21
0.3 0.5
0.5 0.7
0.6 0.77
0.8 0.9
1 1

SOLUTION
Step 1 :scheme
scheme and material balance

Figure 9.2 - Distillation column

Given data :
( Xf)B =0.60
( Xf)T =0.40

( Xd)B =0.95
( Xd)T =0.05

( Xb)B =0.10
( Xb )T =0.90

Overall material balance

F=D+B
Benzene material balance
FXf= DXd+ BXb
100 (0.60) = D (0.95) + B(0.10)
60 = 0.95D + (100 - D) 0.10
60 = 0.95 D + 10 - 0.10 D
50 = 0.85 D
D = 58.82

B = 100 - D
B = 100 - 58.82
B = 41.18

Step 2 :x - y diagram using equilibrium data

Figure 8.6 : E
Equilibrium curve
Step 3 :select the point xd, xf , xd

Figure 8.7 : point xd, xf , xdon x – y diagram

Step 4 : Draw q- line

q-line
line is graphical interpretation of material balance of the feed stage , q represents the
amount
ount of liquid that accumulates at the feed stage by feeding of 1 kmol of the feed.
q-line equation
y =(qx / q-1 ) - ( xf/ q - 1 )

For bubble point liquid, q=1

Figure 8.8 : q line on x – y diagram

Step 5 : Reflux ratio = 2.5

Step 6 :Intercept of the line is

Xd/ R + 1 = 0.95 / (2.5 + 1) = 0.27

Figure
igure 8.9 : intercept on x – y diagram

Step 7 : Draw the operating line of the stripping section of the column
column , by connecting
point of intersection of q-line
line and operating line of rectifying section of point ( xw , xw)

Step 8 : Draw steps between equilibrium line and operating line

Figure 8.10 :Plates on x – y diagram

Number of theoretical plates = 8

Number of actual plate = 7

41
8.3 PROBLEM 3

Design a continuous distillation column to recover acetone from a 50 – 50 mole % acetone

– water mixture available at 300C. The feed stream flow rate is 25000 kg/h. The top
product should contain at least 95 mole% acetone and the bottom product should contain
less than 1 % acetone by mole. This column is operated at atmospheric pressure. Column
efficiency of 60% and pressure drop per plate of 1.25 kPa may be assumed .you can take
the minimum liquid flow as 70% of the maximum rate both above and feed plate. The
vapour liquid equilibrium data for acetone – water system at atmospheric pressure is
provided in table

Data given :
Latent heat of water = 41360 J/mol
Latent heat of acetone = 28410J/mol
Specific heat of water = 75.3J/mol0C
Specific heat of acetone = 128 J/mol0C

X y
0 0
0.05 0.6381
0.10 0.7301
0.15 0.7716
0.20 0.7916
0.25 0.8034
0.30 0.8124
0.35 0.8201
0.40 0.8376
0.45 0.8376
050 0.8387
0.55 0.8455
0.60 0.8532
0.65 0.8615
0.70 0.8712
0.75 0.8817
080 0.895
0.85 0.9118
0.90 0.9335
0.95 0.9627
1 1

Table 8.3

x = mole fraction of acetone in liquid

y = mole fraction of acetone in vapour
42
SOLUTION :
Step 1 :Mass balance
( Xf) A = 0.50
( Xf) W = 0.50

( Xd) A = 0.95
( Xd )W = 0.05

( Xb) A = 0.01
( Xb ) W = 0.99

Bubble point of feed = 59.950C

Latent heat of the feed = 28410 ( 0.5 ) + 41360 ( 11- 0.5 ) = 34885 J/mol
1 0.5 ) = 101.75 J/mol0C
Specific heat of the feed = 128 ( 0.5 ) + 7503 ( 1-
Average molecular weight of feed = 0.5(58) + 0.5 (18) = 38
Molar feed flow rate ( F ) = 25000/38 = 657.9 kmlo/h
Acetone balance : D 0.95 = 657.9 (0.5 )
D = 346.2 kmol/h
Bottom product : B = F – D = 657.9 – 346.2 = 311.7 kmol/h

Step 2 :x - y diagram using equilibrium data

Figure 8.11 : Equilibrium curve

Step 3 :select the point xd, xf , xd

Figure 8.12 : point xd, xf , xdon x – y diagram

Step 4 : Draw q- line

q-line
line is graphical interpretation of material balance of the feed stage , q represents the
amount of liquid that accumulates at the feed stage .
Heat required to vapourize 1 mole of the given feed = ( 59.95 – 30 ) 101.75 + 34885 =
37933
q = heat required t vaporize 1 mole of the given feed / latent heat of the feed
= 37933 / 34885 = 1.09
Slope of q line = q / q-1
= 1.09 / (1.09 – 1 ) = 12.44

figure 8.13 : q line on x – y diagram

Step 5 :Intercept = Xd / Rmin+ 1
= 0.95 / 0.67 + 1 = 0.57

Figure 8.14 : intercept on x – y diagram

Step 6 :Reflux ratio,

io, R = 2.5 Rmin= 2.5 ( 0.67 ) =1.675
Step 7 : Draw the operating line of the stripping section of the column , by connecting
point of intersection of q-line
line and operating line of rectifying section of point ( xw , xw)

Figure
igure 8.15 intercept on x – y diagram
Step 9 : Draw steps between equilibrium line and operating line

figure 8.16 : plates on x – y diagram

Number of theoretical plates = 7

Number of actual plates = ( 7 – 1 ) / 0.6 = 10

Step 10 :estimation of physical

cal properties
Column top pressure = 101325 Pa2
Column pressure drop =1.25 * 1000 * 14 = 16800 kPa
Pressure drop of 1.25 kPa per tray is specified

FOR TOP SECTION

Column top pressure =101325 Pa
Column top temperature = 56.3 0C
Density of vapour = PM/ RT = 10135 * 56.5 / 329.3 * 8.314 * 1000 = 2.08 kg/m3
Density of liquid ( mixture ) = 744 kg/m3
Water density = 985 kg/m3
Acetone density =735 kg/m3
Average molecular weight of liquid : M = 56
Surface tension = 20 * 10-3 N/m

FOR BOTTOM SECTION

Column bottom pressure
Column bottom temperature boiling point of water at 118825 Pa = 1050C
From the steam table at 118825 Pa and 1050C :
Density of vapour = 0.693 kg/m3
Density of liquid = 955 kg/m3
Average molecular weight of vapour = 40.58
Average molecular weight of liquid = 18.4
Surface tension = 58 * 10-3 N/m

Step 11 :column diameter

Design is performed for 80% flooding at maximum gas flow rate

FOR TOP SECTION

Flow parameter ( FLG) based on mass flow rate ,
0.5
FLG =
= 580 * 56 / 926.2 *56.5 (2.08/744)0.5
= 0.033

Capacity parameter (Csbf) = 0.12 m/s

Gas velocity through the net area at flooding :

Unf =Csbf( 𝜎/20)0.2 ( (𝜌𝑙 − 𝜌𝑣)/𝜌𝑣)0.5
= 0.12 * (20/20)0.2 (( 744 – 2.08 )/2.08)0.5
= 2.26

The linear gas velocity ( Un) based on 80 % flooding :

Un = 0.8 * 2.26 = 1.8 m/smaximum volumetric vapor flow rate ( Qmax):
Qmax = (V*M)/𝜌𝑣
= ( 926.2 * 56.5 ) / 2.08
6.98 m3/s

Net area required :

Qmax/ Un= 6.98 / 1.8 = 3.88 m2
Total tower cross section area :
3.88/0.9 = 4.31

Column diameter = √4.31/0.785 = 2.34 m

FOR BOTTOM SECTION

0.5
FLG =
= (1285.7 * 18.4)/ (974 *40.58 ) (0.693/955)0.5
= 0.016

Csbf= 0.11 m/s

Unf =Csbf( 𝜎/20)0.2 ( (𝜌𝑙 − 𝜌𝑣)/𝜌𝑣)0.5

= 0.11 * ( 58/20)0.2 ((955-0.693)/0.693)05
=5.05 m/s

47
Un = 0.8 *5.05 = 4.04 m/s

Qmax = (V*M)/𝜌𝑣
= 975 *4058/0.693
= 15.84 m/s

Net area required :

Qmax/ Un= 15.84 / 4.04 = 3.92 m2
Total tower cross section area :
3.92/0.9 = 4.36m2

Column diameter = √4.36/0.785 = 2.36 m

Use the higher value of the tower diameter for the uniformity between sections, if the
difference is not greater than 20%. In this case , the bottom diameter is used both in top
and bottom sections.

Step 12 :height of the tower

Htower= 2.3 * Nactual
= 2.3 * 10 = 23

48
 REFERENCES

1. Robert EwaldTreybal, Mass Transfer Operations, Third Edition, McGraw Hill

Education (India) PrivateLimited.
2. Binay K. Dutta, Principles of Mass Transfer and Separation Process, Prentice Hall of
India
3. M.V. Joshi & V.V. Mahagani,Process Equipment Design, Macmillan IndiaLtd.
4. Henry Z. Kister: DistillationDesign.
5. Perry's Chemical Engineers Handbook8thEd.
6. Kiran D. Patil, Mass Transfer Operations -2

49
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