PLMM Chemical Engineering Distillation Process

Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology

Chemical Engineering Department
DISTILLATION
PROCESS
Presented By:
Barros, Diego
Mingaracal, Michelle Leigh
Villaluna, Edson Valter
Submitted to:
Engr. Clydelle Rondaris
December, 2015
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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
VII. PRESSURE SWING DISTILLATION ............................................................................................................... 28
A.Operations ................................................................................................................................................ 28
B. Applications ............................................................................................................................................. 28
D. Homogeneous Azeotropic Distillation ................................................................................................ 29
E. Heterogeneous Azeotropic Distillation ................................................................................................ 30
VIII. FACTORS AFFECTING DISTILLATION COLUMN OPERATION ............................................................... 32
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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 & ethanolwater solution), which means all components will be present in the vapor phase;
compared to evaporation, where there is a presence of non-volatile 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 watersulfur 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 vapor
liquid 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 and thus are concentrated in
the vapor, but heavier volatile components also have a (smaller) partial pressure
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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
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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 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:
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
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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.
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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, 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 Cap Trays
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
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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.
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 self-creating 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
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rate and feed compositions, a fluctuations in feed rate, and servicing of auxiliary
equipment operating the entire unit at low rate.
Sieve Trays
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.
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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 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.
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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 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
DISADVANTAGES
Most cost efficient distillation
Higher
pressure drops than
column for diameters greater
packed columns which could
than 0.6 m.
cause column flooding.
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The liquid/vapor contact in the

cross-flow of plate columns is
more
effective
than
the
countercurrent-flow in packed
columns.
Cooling coils can easily be added
to the plate column (cryogenic
applications).
Can handle high liquid flow rates
cost-effectively.
Foaming can occur due to

agitation of the liquid by the
vapor flowing up through it.
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 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.
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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 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 down-flowing 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
DISADVANTAGES
Most cost-efficient distillation
Packing can break during
column when the diameter of
installation, or due to thermal
the column is less than 0.6 m.
expansion.
Because packing can be made
Not cost efficient for high liquid
from inert materials, packed
flow rates.
beds are able to handle
Contact efficiencies are
corrosive materials.
decreased when the liquid flow
Lower pressure drop than in plate
rate is too low.
columns preventing column
flooding.
Good for thermally sensitive
liquids.
Suitable for low pressure
operations.
25 | P a g e

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.
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
26 | P a g e

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.

ADVANTAGES
Can be used for mixtures with
close- boiling components that
cannot be distilled using simple
distillation techniques.
27 | P a g e
DISADVANTAGES
Large quantities of solvent are

needed compared to the feed.
High energy costs for reboiling
and condensing with all the
excess solvent.

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 is used in the plant pictured below
to the right to recover hydrogen from a methane or methanol feed.
28 | P a g e


ADVANTAGES
DISADVANTAGES
Can separate azeotropes that
High energy and capital costs.
are impossible to separate under
Large columns are sometimes
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.
29 | P a g e

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 of columns
close-boiling systems that cannot
is very difficult.
be
separated
with
simple
Creates
two azeotropes to
distillation.
separate an azeotrope
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
30 | P a g e

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.
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.
31 | P a g e

Advantages
Disadvantages
Can separate azeotropic and
Simulation and design of columns
close-boiling systems that can't
is difficult.
be
separated
with
simple
Large recycle rates.
distillation.
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
32 | P a g e

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
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
33 | P a g e

to be re-started. Weeping is indicated by a sharp pressure drop in the

column and reduced separation efficiency.
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.
34 | P a g e

Other Factors
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.
35 | P a g e

PLMM Chemical Engineering Distillation Process

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Pamantasan ng Lungsod ng Maynila

College of Engineering and Technology

Engr. Clydelle Rondaris

Pamantasan ng Lungsod ng Maynila

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iii. Distillation vs other Vapor-Liquid Separation Processes

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II. TYPES OF DISTILLATION METHOD

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2. Simple Batch/Differential Distillation

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III. CLASSIFICATION OF DISTILLING COLUMNS

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IV. BASIC DISTILLATION EQUIPMENT AND OPERATION

a vertical shell where the separation of liquid components is carried out

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Pamantasan ng Lungsod ng Maynila

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E. Advantages and Disadvantages

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The liquid/vapor contact in the

Foaming can occur due to

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VI. PACKED BED COLUMN

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C. Advantage and Disadvantages

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VII. EXTRACTIVE DISTILLATION

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

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C. Advantage and Disadvantages

Large quantities of solvent are

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VII. PRESSURE SWING DISTILLATION

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C. Advantage and Disadvantages

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E. Heterogeneous Azeotropic Distillation

Phase Diagram of a heteroazeotrope

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Pamantasan ng Lungsod ng Maynila

VIII. FACTORS AFFECTING DISTILLATION COLUMN OPERATION

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Vapor Flow Conditions

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

Entrainment - Entrainment refers to the liquid carried by vapor up to the tray

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

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to be re-started. Weeping is indicated by a sharp pressure drop in the

Flooding - Flooding is brought about by excessive vapor flow, causing liquid

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