Pamantasan ng Lungsod ng Maynila

College of Engineering and Technology

Chemical Engineering Department

Presented By:

Barros, Diego
Mingaracal, Michelle Leigh
Villaluna, Edson Valter
Submitted to:

Engr. Clydelle Rondaris

December, 2015

DISTILLAT
ION
PROCESS
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Pamantasan ng Lungsod ng Maynila

College of Engineering and Technology
Chemical Engineering Department

Table of Contents
I. INTRODUCTION TO DISTILLATION..................................................................................3
A. Definition and Purpose............................................................................................... 3
B. Understanding Distillation Process...........................................................................3
C. Idealized Distillation Model........................................................................................ 5
II. TYPES OF DISTILLATION METHOD.................................................................................7
A. Simple Distillation Method......................................................................................... 7
B. Distillation with Reflux................................................................................................ 9
III. CLASSIFICATION OF DISTILLING COLUMNS..............................................................11
A. Based on Mode of Operation....................................................................................11
B. Based on the Nature of Feed that they are processing.......................................11
C. Based on the Type of Column Internals..................................................................11
B. Basic Operation and Terminologies.........................................................................13
V. TRAY COLUMN................................................................................................................ 14
A. Operations.................................................................................................................. 14
B. Column Internals........................................................................................................ 15
C. Liquid and Vapor Flows In A Tray Column..............................................................18
D. Packings versus Trays............................................................................................... 19
E. Advantages and Disadvantages..............................................................................19
F. Application................................................................................................................... 20
VI. PACKED BED COLUMN.................................................................................................. 21
A. Types of Packings...................................................................................................... 21
B. Operation.................................................................................................................... 24
C. Advantage and Disadvantages................................................................................25
VII. EXTRACTIVE DISTILLATION........................................................................................ 26
A. Operation.................................................................................................................... 26
B. Applications................................................................................................................ 27
C. Advantage and Disadvantages................................................................................27
VII. PRESSURE SWING DISTILLATION..............................................................................28
A.Operations................................................................................................................... 28
B. Applications................................................................................................................ 28
C. Advantage and Disadvantages................................................................................29
D. Homogeneous Azeotropic Distillation....................................................................29
E. Heterogeneous Azeotropic Distillation...................................................................30
VIII. FACTORS AFFECTING DISTILLATION COLUMN OPERATION..................................32
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Pamantasan ng Lungsod ng Maynila

College of Engineering and Technology
Chemical Engineering Department

I. INTRODUCTION TO DISTILLATION
A. Definition and Purpose
Distillation is a commonly used method for separating the various
components of a liquid solution by means of the difference in their volatility.
Distillation may result in essentially complete separation (nearly pure
components), or it may be a partial separation that increases the
concentration of selected components of the mixture.
The application of distillation can roughly be divided in four groups:
laboratory scale, industrial distillation, distillation of herbs for perfumery and
medicinal (herbal distillate), and food processing. The latter two are
distinctively different from the former two in that in the processing of
beverages and herbs, the distillation is not used as a true purification
method but more to transfer all volatiles from the source materials to the
distillate. The main difference between laboratory scale distillation and
industrial distillation is that laboratory scale distillation is often performed
batch-wise, whereas industrial distillation often occurs continuously (source:
www.wikipedia.com)
B. Understanding Distillation Process
i. Vapor Pressure and Boiling Point
At any temperature, some molecules of a liquid possess enough kinetic
energy to escape into the vapor phase (evaporation) and some of the
molecules in the vapor phase return to the liquid (condensation). When the
temperature is maintained, an equilibrium is attained between the number of
molecules going back and forth between liquid and vapor. Whenever there is
a change in temperature it upsets the equilibrium; but eventually when the
temperature is maintained at this new point for a short time, a new
equilibrium is soon established.

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The pressure exerted by the vapor of a liquid in a confined space is called its
vapor pressure. It differs for different substances and each substance has a
specific vapor pressure for each given temperature. The higher the
temperature, the higher the vapor pressure, which results in a greater
number of molecules being present in the vapor phase.
The boiling point of a liquid is the temperature at which the vapor pressure of
the liquid equals the pressure around the liquid, enabling bubbles to form
without being crushed. A special case is the normal boiling point, where the
vapor pressure of the liquid equals the ambient atmospheric pressure.

ii. Distillation
Distillation involves the separation of the vapor from the liquid. The vapor
phase is created from the liquid phase by application of heat and thus
vaporization of the mixture at boiling point. All components are present in
both phases. The separation of various components of a liquid solution
depends upon the distribution of these components between a vapor phase
and a liquid phase. The basic requirement is that the composition of the
vapor be different from the composition of the liquid with which it is in
equilibrium at the boiling point of the liquid. (Geankoplis, 700)
In much simple words, the basic principle of distillation is to heat the solution
until its boiling point. The heat causes components with higher volatility to
be first vaporized, leaving less volatile components as liquids. The hot vapor
are then collected, and condensed to separate the component substance
(source: www.buzzle.com).

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iii. Distillation vs other Vapor-Liquid Separation Processes

The distinction of distillation from evaporation is that it is concerned with
solutions where all components are appreciably volatile (e.g. ammonia-water
& ethanol-water solution), which means all components will be present in the
vapor phase; compared to evaporation, where there is a presence of nonvolatile component.
The process of absorption differs from distillation in that one of the
components in absorption is essentially insoluble in liquid phase.
(Geankoplis, 700). An example is the absorption of sulfur-dioxide from air by
water, where air is insoluble in water-sulfur dioxide solution.
C. Idealized Distillation Model
It is a common misconception that in a liquid mixture at a given pressure,
each component boils at the boiling point corresponding to the given
pressure and the vapors of each component will collect separately and
purely. This, however, does not occur even in an idealized system. Idealized
models of distillation are essentially governed by Raoult's law and Dalton's
law, and assume that vaporliquid equilibria are attained.
Raoult's law states that the vapor pressure of a solution is dependent on 1)
the vapor pressure of each component and 2) mole fraction of this
component in the liquid solution. This law applies to ideal solutions, or
solutions that have different components but whose molecular interactions
are the same as or very similar to pure solutions. Dalton's law states that the
total pressure is the sum of the partial pressures of each individual
component in the mixture.
When a multi-component liquid is heated, the vapor pressure of each
component will rise, thus causing the total vapor pressure to rise. When the
total vapor pressure reaches the pressure surrounding the liquid, boiling
occurs and liquid turns to gas throughout the bulk of the liquid. Note that a
mixture with a given composition has one boiling point at a given
pressure, when the components are mutually soluble. A mixture of constant
composition does not have multiple boiling points.
An implication of one boiling point is that lighter components never
cleanly "boil first". At boiling point, all volatile components boil, but for
a component, its percentage in the vapor is the same as its percentage of
the total vapor pressure. Lighter components have a higher partial pressure
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Chemical Engineering Department

and thus are concentrated in the vapor, but heavier volatile components also
have a (smaller) partial pressure and necessarily evaporate also, albeit being
less concentrated in the vapor. Indeed, batch distillation and fractionation
succeed by varying the composition of the mixture. In batch distillation, the
batch evaporates, which changes its composition; in fractionation, liquid
higher in the fractionation column contains more lights and boils at lower
temperatures. Therefore, starting from a given mixture, it appears to have a
boiling range instead of a boiling point, although this is because its
composition changes: each intermediate mixture has its own, singular boiling
point.

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II. TYPES OF DISTILLATION METHOD

A. Simple Distillation Method
Simple distillation involves the production of vapor by boiling the mixture to
be separated in a single-stage and then recovering and condensing the
vapors. No condensed liquid is allowed to return to the single-stage still to
contact the rising vapor.
Simple distillation is effective only when separating a volatile liquid from a
nonvolatile substance or when separating two liquids that differ in boiling
point by 50 degrees or more. If the liquids comprising the mixture that is
being distilled have boiling points that are closer than 50 degrees to one
another, the distillate collected will be richer in the more volatile compound
but not to the degree necessary for complete separation of the individual
compounds
1. Equilibrium or Flash Distillation
Flash distillation (sometimes called
"equilibrium distillation") is a single
stage separation technique. A liquid
mixture feed is pumped through a
heater to raise the temperature and
enthalpy of the mixture. It then flows
through a valve and the pressure is
reduced, causing the liquid to partially
vaporize. Once the mixture enters a
big enough volume (the "flash drum"),
the liquid and vapor separate.
Because the vapor and liquid are in
such close contact up until the "flash"
occurs, the product liquid and vapor
phases approach equilibrium

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2. Simple Batch/Differential Distillation

The liquid is first charge into a
heated vessel. The liquid charged
is heated slowly and the vapors
are withdrawn as rapidly as they
form into a condenser where the
condensed vapor is collected. The
first
portion
of
the
vapor
condensed will be richest in the
more volatile component A. As
vaporization
proceeds,
the
vaporized
product
becomes
leaner in A.
3. Simple Steam Distillation
Steam distillation is used for the
purification of mixtures in which the
components are temperature or heat
sensitive;
for
example,
organic
compounds. Often, these high-boiling
substances are essentially insoluble in
water.
Since there are two liquid phases, the
mixture will boil at the same
temperature, which is lower than the
boiling point of the pure organic
compound alone.
By steam distillation, as long as liquid
water is present, the high-boiling point
component vaporizes at temperature
well below its normal boiling point
without using a vacuum. This way, the temperature sensitive compounds are
separated before decomposition.
The vapors are collected and condensed in the same way as other distillation
types resulting in two immiscible liquid phases separated. This method has
the disadvantage that large amounts of heat must be used to evaporate the
water simultaneously with the high-boiling compound.

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Steam distillation is sometimes used in the food industry for the removal of
volatile taints and flavors from edible fats and oils. In many case, vacuum
distillation is used instead of steam distillation to purify high-boiling
materials. The total pressure is quite low so that the vapor pressure of the
system reaches the total pressure at relatively low temperatures
(Geankoplis)
B. Distillation with Reflux
Distillation with reflux is also called as Rectification, or Fractionation. It
involves the returning of the portion of the condensed to the still
(Geankoplis,702).
Fractionating column is used to separate constituents whose volatility is
nearly similar or differs by 77F (25C, at 1 atmosphere pressure) and which
cannot be separated by simple distillation.
A series of flash-vaporization stages are arranged in series in a manner that
the vapor and the liquid products from each stage flow counter-current to
each other. The liquid in a stage in conducted or flows to the stage below
and the vapor from a stage flows upward to the stage above.
The basic idea behind fractional distillation is the same as simple distillation
only the process is repeated many times. If simple distillation was performed
on a mixture of liquids with similar volatilities, the resulting distillate would
be more concentrated in the more volatile compound than the original
mixture but it would still contain a significant amount of the higher boiling
compound. If the distillate of this simple distillation was distilled again, the
resulting distillate would again be even more concentrated in the lower
boiling compound, but still a portion of the distillate would be the higher
boiling compound. If this process is repeated several times, a fairly pure
distillate will eventually result. This, however, would take a very long time. In
fractional distillation, the vapors formed from the boiling mixture rise into the
fractionating column where they condense on the column's packing. This
condensation is tantamount to a single run of simple distillation; the
condensate is more concentrated in the lower boiling compound than the
mixture in the distillation flask. As vapors continue to rise through the
column, the liquid that has condensed will revaporize. Each time this occurs
the resulting vapors are more and more concentrated in the more volatile
substances. The length of the fractionating column and the material it is
packed with impact the number of times the vapors will recondense before
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passing into the condenser; the

number of times the column
will support this is referred to
as the number of theoretical
plates of the column
In the fractionating column,
the plates are arranged, and
the compounds with the least
boiling point are collected at
the top, while those with
higher boiling point are present
at the bottom.

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III. CLASSIFICATION OF DISTILLING COLUMNS

A. Based on Mode of Operation
In batch column 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 carried out. When the desired task is achieved, a next batch of feed is
introduced.
In contrast, continuous columns process a continuous feed stream. No
interruptions occur unless there is a problem with the column or surrounding
process units. They are capable of handling high throughputs and are the
more common of the two types.
B. Based on the Nature of Feed that they are processing
When the feed contains only two components, it is called binary
distillation; when the feed contains more than two components, it is called
multi-component distillation. Multi-component distillation typically
requires more than one distillation column.
C. Based on the Type of Column Internals
Tray columns uses trays of various designs to hold up the liquid and to
provide better contact between the liquid and the vapor. On the other hand,
packed bed column uses packings of different types to provide contact
between the liquid and the vapor. These packings are arranged and stacked
together along the vertical column.
D. Based on the Technique Used to aid in Separation
Extractive distillation and Azeotropic distillation are similar in a way
that they are both used to separate components with almost the same
volatility by adding a new component (called entrainer) to the distillation
column aside from the feed solution. However, in extractive distillation,
unlike in azetropic distillation, the entrained doesnt form an azeotrope with
one of the component and thus it can be easily separated from that
component by extraction.
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IV. BASIC DISTILLATION EQUIPMENT AND OPERATION

A. Basic Components and Accessories of Distilling Column
Distillation columns are made up of several components, each of which is
used either to transfer heat energy or enhance materil transfer. A typical
distillation contains several major components:

a vertical shell where the separation of liquid components is carried

out
column internals such as trays/plates and/or packings which are
used to enhance component separations
a reboiler to provide the necessary vaporization for the distillation
process
a condenser to cool and condense the vapour leaving the top of the
column
a reflux drum to hold the condensed vapour from the top of the
column so that liquid (reflux) can be recycled back to the column

The vertical shell houses the column internals and together with the
condenser and reboiler, constitute a distillation column. A schematic of a
typical distillation unit with a single feed and two product streams is shown
below:

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The liquid mixture that is to be processed is known as the feed and this is
introduced usually somewhere near the middle of the column to a tray
known as the feed tray. The feed tray divides the column into a top
(enriching or rectification) section and a bottom (stripping) section. The feed
flows down the column where it is collected at the bottom in the reboiler.
B. Basic Operation and Terminologies
Heat is supplied to the reboiler to
generate vapor. The source of heat
input can be any suitable fluid,
although in most chemical plants
this is normally steam. In refineries,
the heating source may be the
output streams of other columns.
The vapor raised in the reboiler is
re-introduced into the unit at the
bottom of the column. The liquid
removed from the reboiler is known
as the bottoms product or simply,
bottoms.
The vapour moves up the column,
and as it exits the top of the unit, it
is cooled by a condenser. The
condensed liquid is stored in a
holding vessel known as the reflux
drum. Some of this liquid is recycled back to the top of the column and this
is called the reflux. The condensed liquid that is removed from the system is
known as the distillate or top product.
Thus, there are internal flows of vapour and liquid within the column as well
as external flows of feeds and product streams, into and out of the column.

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V. TRAY COLUMN
A. Operations
Trays are the most commonly selected type of distillation column. Trayed
Columns utilize a pressure and temperature differential to separate the
products. For most tray columns, the weir holds a liquid level of each tray.
The vapor must overcome this liquid head to move up the column. On the
tray the vapor and liquid are contacted and then above the tray they are
separated. Trayed column perform well in high liquid and vapor loading. At
low flow parameters the capacity and efficiency of trays can be reduced. Tray
have higher pressure drop than packing, and it may also have higher
resistance tocorrosion. Some other items are to consider when to use trays in
a tower.
1 Usually trays have downcomer capacity problems in heavy foaming
service.
2 Trays have higher pressure drop than structured packing column
3 Trays have a high resistance to corrosion
4 Entrainment is an issue with trays. Trays usually have more
entrainment than packing. Excessive entrainment can lead to
efficiency loss.
5 Excessive vapor and liquid maldistribution can lead to a loss of
efficiency in a tray tower.
In order for good separation (or fractionation) to occur in distillation column,
the vapors must have good contact with the liquid on each tray. When the
large bubble is broken into several smaller bubbles, the smaller bubbles
expose more surface area for vapor liquid contact.
The feed enters a plate column towards the middle of the column.
Concentration differences cause the less volatile components to transfer
from the vapor stream to the liquid stream. The vapor exiting the condenser
contains the most volatile components, while the least volatile components
exit through the reboiler in the liquid stream.
Mechanism
After the feed mixture enters the column, liquid flows down the column and
across the trays in either crossflow or countercurrent flow. A reboiler at the
bottom separates the stream into a vapor stream that returns to the column
and a liquid product stream. The vapor stream flows upward through the
trays, and contacts the down-flowing liquid stream, allowing the separation
to take place. At the top of the column, the vapor is condensed in a
condenser. The condensed stream is split into an overhead product stream,
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known as the distillate, and a reflux stream

that returns to the top of the column.

B. Column Internals
The terms "trays" and "plates" are used
interchangeably. There are many types of
tray designs, but the most common ones
are:
Bubble
Trays

Cap

A bubble cap
tray 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
vapor. Vapor 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.

The oldest widely used equilibrium-stage plate is the bubble cap tray. A
bubble cap tray is perforated flat plate which has a riser (chimney) over the
holes covered with a cap. They are usually equipped with slots to allow the
passage of vapor to be mixed with the liquid flowing across the tray forming
bubble where the mass transfer takes place. Each tray is provided with one
or more downcomers which the liquid flowing across the tray is conducted to
the tray below. A liquid head is maintained on the tray by a dam placed on
outlet side of the tray near the downcomer, it called the outlet weir. Bubble
cap tray is able to operate at low vapor and liquid rates (less than 2 gpm per
foot of average of flow width) because liquid and foam is trapped on the tray
to a depth at least equal to the weir height.
Bubble cap trays work well in high turndown applications because the
orifices in the bubble caps are in the form of risers whose top opening is
elevated significantly above the tray deck.
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The size of the cap tends to create hydraulic gradient across the deck and a
high vapor side pressure drop. The cost of bubble cap tray is by far the
highest.
Valve Trays
In valve trays, perforations are covered by
liftable caps. Vapor flows lifts the caps, thus selfcreating a flow area for the passage of vapor.
The lifting cap directs the vapor to flow
horizontally into the liquid, thus providing better
mixing than is possible in sieve trays
Valve Tray uses valve (moveable disc) which
almost closes off completely at low vapor rate,
thus minimize tray open area. When lifted, as vapor rate increases, the open
area increases for vapor flow between the valve disc and the tray deck.
Valves can be round or rectangular, with or without caging structured. Most
types of valves, the opening may be varied by the vapor flow, so that the
trays can operate over a wide range of flow rates with high separation
efficiency and large flexibility.
Because of their flexibility and price (slightly more expensive than sieve
tray), valve trays are tending to replace bubble-cap trays.
Valve tray has minimum capacity of approximately 60%. The dry pressure
drop of valve tray is lower than bubble cap, because the valve does not need
a chimney for the vapor and it depends on weight of valve.
The valve tray can used in condition where vapor rate change
unpredictability over a given section of tower, a tower utilized in blocked
operation at varying rate and feed compositions, a fluctuations in feed rate,
and servicing of auxiliary equipment operating the entire unit at low rate.
Sieve Trays

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Sieve trays are simply metal plates

with holes in them. Vapor 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 the
once highly thought of bubble cap
trays in many applications.
Sieve tray is perforated plate with holes punched into the plate and usually
has holes 3/16 in to 1 in diameter. The standard size is 0.5 inch with the
perforation punched downward. Vapor comes out from the holes to give a
multi orifice effect. The vapor velocity keeps the liquid from flowing do
through the holes (weeping). Vapor flow through the tray deck to contact the
liquid is controlled by the number and size of the perforations.
The punching direction affects the dry pressure drop, a smaller hole diameter
result in lower pressure drop for the same open area. This due to the ratio of
hole diameter to the tray thickness. The number and hole size are based on
vapor flow up the tower. The liquid flow is transported down the tower by
down-corners, a dam and overflow device on the side on the plate.
A sieve tray has higher entrainment than valve tray at the same vapour
velocity. This is due to the spray of liquid directed upwards to the next tray.
For efficient operation, the hole velocity must be sufficient to balance the
head of liquid on the tray deck and thus prevent liquid from passing through
the perforations to the tray Sieve trays can be used in almost all services.
Sieve deck tray has a minimum capacity approximately 70%. Their capacity
and efficiency are at least as high as that of other standard trays used
commercially. Sieve trays may be used in moderately fouling services,
provided that large holes (3/4 to 1 in. [19 to 25 mm)) are used. Sieve trays
are simple and easy to fabricate and therefore relatively inexpensive.
The geometry of the trays within the column affects the extent and
type of contact between the vapor and liquid streams. Tray types include
sieve, valve, and bubble cap. Sieve trays, which contain holes for vapor to
flow through, are used for high capacity situations providing high efficiency
at a low cost. Although less expensive, valve trays, containing holes with
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opening and closing valves, have the tendency to experience fouling due to
accumulation of material. Bubble cap trays contain caps which allow vapor to
flow into and out through tiny openings through the liquid. Bubble cap trays
are the most advanced and expensive of the three trays, and are highly
effective in some low liquid flow rate situations.
C. Liquid and Vapor Flows In a Tray Column

Each tray has 2 conduits, one on each side, called downcomers. Liquid falls
through the downcomers by gravity from one tray to the one below it. The
flow across each plate is shown in the above diagram on the right.
A weir on the tray ensures that there is always some liquid (holdup) on the
tray and is designed such that the the holdup is at a suitable height, e.g.
such that the bubble caps are covered by liquid.
Being lighter, vapor flows up the column and is forced to pass through the
liquid, via the openings on each tray. The area allowed for the passage of
vapour on each tray is called the active tray area.
As the hotter vapor passes through the liquid on the tray above, it transfers
heat to the liquid. In doing so, some of the vapor condenses adding to the
liquid on the tray. The condensate, however, is richer in the less volatile
components than is in the vapor. Additionally, because of the heat input from
the vapor, the liquid on the tray boils, generating more vapor. This vapor,
which moves up to the next tray in the column, is richer in the more volatile
components. This continuous contacting between vapor and liquid occurs on
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each tray in the column and brings about the separation between low boiling
point components and those with higher boiling points.
D. Packings versus Trays

E. Advantages and Disadvantages

ADVANTAGES
Most cost efficient distillation column for diameters greater than 0.6 m.
The liquid/vapor contact in the cross-flow of plate columns is more effective than the
Cooling coils can easily be added to the plate column (cryogenic applications).
Can handle high liquid flow rates cost-effectively.
F. Application

Plate columns are often used to recover solvents from process wastes. In the
system to the left, water is used to recover methanol from a drying
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operation. Water comes out as the liquid product and the volatile organic
waste goes into the vapor phase. Shown on the right is a 40 tray column
used for mineral oils. Plate columns can also be used to purify solvents of
hazardous material, such as the stripping of hydrogen sulfide from "sour
water." Many different inlet temperatures and feed moisture contents can be
used.

VI. PACKED BED COLUMN

As its name implies, the packed tower is a vertical, steel column which
instead of using trays, it contains 'Beds' of packing material which are used
to bring the rising vapours into intimate contact with falling liquid within the
tower.
If a distillation tower uses packing instead of trays, the number of necessary
theoretical equilibrium stages is first determined and then the packing height
equivalent to a theoretical equilibrium stage, known as the height equivalent
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to a theoretical plate (HETP), is also determined. The total packing height

required is the number theoretical stages multiplied by the HETP.
A. Types of Packings
The types of packing used plays an important role in the efficiency of the
separation process. There are two types of packing: it may be dumped at
random or stacked in regular geometric patterns. They all aim to maximise
the surface area per unit volume to maintain good vapour-liquid contact and
to minimise pressure drop.
Random Packings
Dumped packings have either random or geometrically structured shapes
and are composed of bulk inert material, such as clay, porcelain, plastic,
ceramic, metal, or graphite. Individual packings are typically 3 to 75 mm in
size, and have several void spaces that provide a large surface area for
liquid-vapor contact. The advantages of dumped packing include high liquid
flow rate capacity, high pressure capacity, and low cost. Several examples of
metal, plastic, and ceramic type packings are shown in the picture below.

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Metal packings have a high strength and good wettability. Ceramic packings
have a higher wettability than metal packings, but they are not as strong.
Plastic packings have sufficient strength but experience poor wettability at
low liquid flowrates. Because they are corrosion resistant, ceramic packings
are used only at elevated temperatures where plastic packing would fail.
Stacked Packings
Stacked Packing is a structured meshwork of the same diameter as the
column. It provides long uninterrupted channels for liquid and vapor flow.
Although they are more expensive than dumped packings, stacked packings
result in a lower pressure drop. Stacked packing is preferred for low liquid
flow rates and in low pressure situations. They are typically made of wood,
sheet metal, or woven gauze.

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B. Operation
The feed mixture contains components of different volatilities, and enters the
column approximately at the middle.
After the feed mixture enters the column, the liquid flows down the column
through the packing countercurrently and contacts the rising vapor stream.
The liquid at the bottom enters a reboiler. Two streams exit the reboiler; a
vapor stream, which returns to the column, and a liquid product stream. The
vapor stream flows upward through the packing and contacts the downflowing vapor. Differences in concentration cause the less-volatile
components to transfer from the vapor phase to the liquid phase. The
packing increases the time of contact, which increases the separation
efficiency.
When it reach the top, the vapor exits the column, and enters a condenser.
After the vapor condenses, the stream enters a reflux drum, where it is split
into an overhead product stream, known as the distillate, and a reflux stream
that is recycled back to the column
The exiting vapor contains the most volatile components, while the liquid
product stream contains the least volatile components.
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C. Advantage and Disadvantages

ADVANTAGES
Most cost-efficient distillation column when the diameter of the column is less than
Because packing can be made from inert materials, packed beds are able to handle
Lower pressure drop than in plate columns preventing column flooding.
Good for thermally sensitive liquids.
Suitable for low pressure operations.
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VII. EXTRACTIVE DISTILLATION

Extractive distillation is defined as distillation in the presence of a miscible,
high boiling, relatively non-volatile component, solvent that forms no
azeotrope with the other components in the mixture. The method is used for
mixtures having a low value of relative volatility, nearing unity. Such
mixtures cannot be separated by simple distillation, because the volatility of
the two components in the mixture is nearly the same, causing them to
evaporate at nearly the same temperature at a similar rate, making normal
distillation impractical.
A. Operation

The method of extractive distillation uses a separation solvent, which is

generally non-volatile, has a high boiling point and is miscible with the
mixture, but doesn't form an azeotropic mixture. The solvent interacts
differently with the components of the mixture thereby causing their relative
volatilities to change. This enables the new three-part mixture to be
separated by normal distillation. The original component with the greatest
volatility separates out as the top product. The bottom product consists of a
mixture of the solvent and the other component, which can again be
separated easily because the solvent does not form an azeotrope with it. The
bottom product can be separated by any of the methods available.
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It is important to select a suitable separation solvent for this type of

distillation. The solvent must alter the relative volatility by a wide enough
margin for a successful result. The quantity, cost and availability of the
solvent should be considered. The solvent should be easily separable from
the bottom product, and should not react chemically with the components or
the mixture, or cause corrosion in the equipment. A classic example to be
cited
here
is
the
separation
of
an
azeotropic
mixture
of
benzene and cyclohexane, where aniline is one suitable solvent.
B. Applications
Extractive distillation is used mostly for the
separation of mixtures of close-boiling species or
those that form azeotropes. Extractive distillation
is not as widely used in industry as conventional
distillation because column simulation and
design is difficult. For example, extractive
distillation units are used in pulp-making
processes. In the extractive unit an organic
solvent separates cellulose from lignin. The
solvent is then separated, purified and recycled
in the second column. The extractive distillation
unit being installed in the picture below can be
used for solvent recovery, extraction of aromatic
compounds, and purification of organic acids.

C. Advantage and Disadvantages

ADVANTAGES
Can be used for mixtures with close- boiling components that cannot be distilled usi

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VII. PRESSURE SWING DISTILLATION

Pressure-swing distillation is a method for separating a pressure-sensitive
azeotrope that utiltizes two columns operated in sequence at two different
pressures. Its target is to overcome the azeotropic composition by changing
the system pressure. The key factors involved in pressure swing distillation
are the azeotrope sensitive to pressure changes, and recycle ratio which
increases costs
A.Operations

The feed stream and a recycle stream from the second column are fed into
the first column. The first column operates at a specific pressure that
separates the first component as a distillate from an azeotropic mixture
bottoms stream. The azeotropic bottoms stream is fed into a second column
that operates at a differ ent pressure. At this pressure the original azeotrope
is "broken" and a separation can take place, resulting in the second
component as a distillate and an azeotropic bottoms stream of different
composition. This bottoms product is recycled back to the first column.
B. Applications
Pressure swing distillation can be used to break an ethanol-water mixture
that forms an azeotrope. The columns pictured below to the left are used to
distill 190 proof ethanol to 199 proof, so it can be used as a fuel grade
additive, enhancing octane levels in gasoline. The process consists of three
or more columns operating at different pressures. Pressure swing distillation
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is used in the plant pictured below to the right to recover hydrogen from a
methane or methanol feed.

C. Advantage and Disadvantages

ADVANTAGES
DISADVANTAGES
Can separate azeotropes that
High energy and capital costs.
are impossible to separate
Large columns are sometimes
under simple distillation.
necessary.
Some azeotropes disappear at
Large recycle flow rates.
different
pressures,
making
them easier to separate.
D. Homogeneous Azeotropic Distillation
A homogeneous azeotropic distillation system is used to separate an
azeotropic feed. An entrainer is added to the recycle stream. The entrainer is
completely miscible with the original components. Entrainer may (or not)
form additional azeotropes with the original components. The distillation is
carried out in a sequence of columns
Mechanism
An entrainer in the recycle stream, is added to the binary feed azeotrope,
shown entering the first column. The entrainer forms another azeotrope with
one of the feed components and moves into the second column exiting the
top of the first column demonstrates. The other feed component separates
from the azeotrope in the first column and exits through the bottom of the
column.
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In the second column, the pressure is set to break the entrainer-feed

azeotrope, which results in the second component and a third azeotrope
containing the entrainer. Homogeneous azeotropic distillation is not
commonly used because it is so complex.
Advantages
Disadvantages
Can separate azeotropic and
Simulation
and
design
close-boiling
systems
that
columns is very difficult.
cannot be separated with simple
Creates two azeotropes
distillation.
separate an azeotrope

of
to

E. Heterogeneous Azeotropic Distillation

Heterogeneous azeotropic distillation incorporates liquid-liquid separation
into the separation of an azeotropic feed. Entrainer is immiscible and forms
azeotrope with at least one of the original azeotropic components. The
distillation is carried out in a combined column decanter column. The
entrainer is recovered and recycled to the first column.

Phase Diagram of a heteroazeotrope

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Mechanism

An azeotropic feed stream enters the first column, and is split into two
streams: The bottoms contain the first component, and a second azeotrope
exits through the top of the column as the distillate. The distillate is
condensed and sent to a decanter, where it is separated into two liquids: One
is rich in component one and is returned to the first column, as the recycle
stream exemplifies. The second liquid, which is rich in component two, is
sent to a second column. The second column operates at a different pressure
than the first column and is used to separate the stream into pure
component two, and a third azeotrope distillate. This distillate is also
condensed and sent to the decanter. In addition, an entrainer is often added
to improve the separation.
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Applications
Heterogeneous azeotropic distillation is used in chemical processing
industries to separate close-boiling or azeotropic systems. This type of
distillation can be used as an alternative to extractive distillation, pressure
swing distillation, or homogeneous azeotropic distillation. These columns can
be used to separate water-ethanol mixtures.

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Advantages
Can separate azeotropic and close-boiling systems that can't be separated with sim
Self-entraining systems possible.

VIII. FACTORS AFFECTING DISTILLATION COLUMN OPERATION

The performance of a distillation column is determined by many factors, for
example:

Feed conditions
a. State of feed
b. Composition of feed
c. trace elements that can severely affect the VLE of liquid mixtures
Internal liquid and fluid flow conditions
State of trays (packings)
Weather conditions

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. During operation, if the deviations from
design specifications are excessive, then the column may no longer be able
handle the separation task. To overcome the problems associated with the
feed, some column are designed to have multiple feed points when the feed
is expected to containing varying amounts of components.
Reflux Conditions
As the reflux ratio is increased, the gradient of operating line for the
rectification section moves towards a maximum value of 1. Physically, what
this means is that more and more liquid that is rich in the more volatile
components are being recycled back into the column. Separation then
becomes better and thus less trays are needed to achieve the same degree
of separation. Minimum trays are required under total reflux conditions, i.e.
there is no withdrawal of distillate.

On the other hand, as reflux is decreased, the operating line for the
rectification section moves towards the equilibrium line. The pinch

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between operating and equilibrium lines becomes more pronounced

and more and more trays are required.This is easy to verify using the
McCabeThiele method.
The limiting condition occurs at minimum reflux ration, when an infinite
number of trays will be required to effect separation. Most columns are
designed to operate between 1.2 to 1.5 times the minimum reflux ratio
because this is approximately the region of minimum operating costs
(more reflux means higher reboiler duty).

Vapor Flow Conditions

Adverse vapor flow conditions can cause:

Foaming - Foaming refers to the expansion of liquid due to passage of

vapour or gas. Although it provides high interfacial liquid-vapour
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
always reduced.

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 distillate. Excessive entrainment can lead to
flooding.

Weeping/Dumping - This phenomenon is caused by low vapor flow.

The pressure exerted by the vapour 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) and the column will have to be re-started. Weeping is indicated
by a sharp pressure drop in the column and reduced separation
efficiency.

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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
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.

Column Diameter
Most of the above factors that affect column operation is due to vapor flow
conditions: either excessive or too low. 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 perform well. Not only will operational problems occur, the desired
separation duties may not be achieved.
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, and the
packings if packings are used. 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 properties of the liquids being
processed. Thus appropriate materials should be specified for tray
construction.
Weather Conditions
Most distillation columns are open to the atmosphere. Although many of the
columns are insulated, changing weather conditions can still affect column
operation. Thus the reboiler must be appropriately sized to ensure that
enough vapor can be generated during cold and windy spells and that it can
be turned down sufficiently during hot seasons. The same applies to
condensers.
Other Factors
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These are some of the more important factors that can cause poor distillation
column performance. Other factors include changing operating conditions
and throughputs, brought about by changes in upstream conditions and
changes in the demand for the products. All these factors, including the
associated control system, should be considered at the design stages
because once a column is built and installed, nothing much can be done to
rectify the situation without incurring significant costs. The control of
distillation columns is a field in its own right, but that's another story.

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