Chapter I: Literature Review

1. Introduction
The separation of chemical mixtures into their constituents has been practiced, as an art, for hundreds
of years ago. In the early civilizations, different techniques have been developed to (1) extract metals
from ores, perfumes from flowers, dyes from plants, and potash from the ashes of burnt plants, (2)
evaporate seawater to obtain salt, (3) refine rock asphalt, and (4) distill liquors. The human body
could not function for long if it had no kidney, a membrane that selectively removes water and waste
products of metabolism from the blood.
The chemical industry manufactures products that differ in chemical content from process feeds,
which can be (1) naturally occurring raw materials, (2) plant or animal matter, (3) chemical
intermediates, (4) chemicals of commerce, or (5) waste products. Especially common are oil
refineries, produce a variety of useful products.
Figure I.1 represents a variety of marketable products that can be produced by the refining of crude
oil in refineries. The relative amounts of these products are produced from, for example, 150,000
bbl./day of crude oil. This amount depends on the constituents of the crude oil and the types of
refinery processes. From the conversion of this amount of crude oil, we can obtain different products
like motor gasoline, fuel oils, lubricants, … that can be used directly.

Figure I.1.: Refinery for converting crude oil into a variety of

marketable products
In chemical industries, and especially in oil refineries, different processes can be applied including:

 distillation to separate crude oil into various boiling point fractions or cuts,
 alkylation to combine small hydrocarbon molecules into larger molecules,
 catalytic reforming to change the structure of medium-size hydrocarbon molecules,
 fluid catalytic cracking to break apart large hydrocarbon molecules,
 hydrocracking to break apart even larger molecules,
 and other processes to convert the crude-oil residue to coke and lighter fractions.[1]

Mixing of chemicals is a spontaneous and natural process that is accompanied by an increase in

entropy. The inverse process, the separation of that mixture into its constituent chemical species, is
not spontaneous; it requires a wide amount of energy.
Figure I.2 represents the general separation process of a feed mixture. A feed mixture to be separated
usually originates as a single and homogeneous phase (solid, liquid, gas). If it exists as two or more
immiscible phases, first we should use a mechanical means based on gravity, centrifugal force,
pressure reduction, or an electric and/or magnetic field to separate the phases; then, appropriate
separation techniques are applied to each phase.[1]

Figure I.2.: General separation process

Distillation can be carried out by:
1. The production of vapor by boiling the liquid mixture to be separated in a single stage and
recovering and condensing the vapors:
 Flash or equilibrium distillation.
 Batch or differential distillation.
For more information about these two types of distillation, [1] may be used as a reference.
2. The returning of a portion of the condensate to the still. The vapors ascend through a
progression of stages or trays, and part of the condensate flows descending, counter currently to
the fumes (vapors). This strategy is called fractional distillation or distillation with reflux or
rectification:

This technique has been developed and produced for specific applications, for
example, petroleum oil refining since basic refining or simple distillation is not proficient for
separating liquids whose boiling points lie close to each other. In this operation the vapors from a
distillation are repeatedly condensed and re-vaporized in an insulated protected vertical column.
Particularly significant in this association are the still heads, fractionating columns, and
condensers that license the arrival of a portion of the condensed vapor toward the still. The goal
is to achieve the closest possible contact between rising vapor and dropping liquid to permit only
the most volatile material to continue in the form of vapor to the receiver while returning the less
volatile material as liquid toward the still. The purification of the more unstable component,
which is the more volatile, by contact between such countercurrent streams of vapor and liquid is
alluded to as rectification, or enrichment.
The separation requires that:

 a second phase be shaped so that both liquid and vapor phases are available and can contact
each other on each stage or phase within a separation column,
 the components have various volatilities so that they will parcel between the two stages to
different extents,
 the two phases can be separated by gravity or other mechanical methods.

2. History
For over 5,000 years, distillation has been utilized as a method for separating binary and
multicomponent liquid mixtures into pure components. Indeed, even today, it has a place to the most
commonly applied separation technologies and is used at such a large scale around the world that it
is liable for up to 50% of both capital and operating costs in modern industrial processes. Also, it
absorbs about 50% of the total process energy utilized by the chemical and oil refining industries
consistently.[1]
According to Forbes [2], the specialty of distillation goes back to at least the primary century A.D.
By the eleventh century, distillation was being used in Italy to create mixed refreshments known as
alcoholic beverages. At that time, distillation was likely a batch process dependent on the use of only
a single stage, the evaporator, or the boiler. The feed to be separated, a liquid, was put in a vessel to
which heat was applied, making some portion of the liquid to evaporate. The vapor dropped out of
the heating vessel and was cooled in another chamber by heat transfer through the wall of the
chamber to water, creating condensate that dripped into, product receiver. The word distillation is
derived from the Latin word “destillare”, which means dripping or streaming down. By at least the
sixteenth century, it was realized that the degree of separation could be improved by giving various
vapor-liquid contacts (stages) in a so-called Rectificatorium. Current distillation derives its capacity
to produce almost pure products from the utilization of multistage contacting. All through the
twentieth century, multistage refining was by far the most broadly used industrial method for
separating liquid mixtures of chemical components. Tragically, distillation is a very energy-intensive
method: roughly 66% of the distillation energy was consumed by petroleum oil refining, where
distillation is generally used to separate crude oil into petroleum fractions or divisions, light, and
aromatic chemicals. The separation of the organic chemicals, frequently in the presence of water, is
most extensively practiced in the chemical industry.

3. Distillation column and its principle of work

Distillation is the most developed and broadly utilized separation operation, with design procedures
and operation practices well established. Distillation is most normally directed in trayed towers
equipped with a sieve or valve trays, or in columns packed with random or structured packings.
Many older towers are furnished with bubble-cap trays. Most distillation towers are equipped with a
condenser, cooled with cooling water, to give reflux, and a reboiler, warmed with steam, to give boil-
up.
Distillation includes various contacts between counter currently flowing liquid and vapor phases.
Each contact consists of blending the two phases to advance the rapid partitioning of species by mass
transfer, followed by phase separation. The contacts are often made on horizontal trays (referred to
as stages) arranged in a vertical column. Vapor, while streaming up the column, is progressively
improved concerning the more volatile species. Correspondingly, liquid flowing down the column is
progressively advanced for the less-volatile species. Feed to the distillation column enters on a plate
somewhere close to the top and bottom trays, and regularly close to the center of the column. The
portion of the column over the feed passage is called the enriching or rectification section, and that
underneath is the stripping section. Feed vapor starts up the column; feed liquid beginnings down.
Liquid is required for making contacts with vapor above the feed plate, and vapor is required for
making contacts with liquid beneath the feed tray. Frequently, vapor from the top of the column is
condensed in a condenser by cooling water or a refrigerant to give contacting liquid, called reflux.
Additionally, liquid at the bottom of the column goes through a reboiler, where it is warmed by
gathering (condensing) steam or some other heating medium to provide contacting vapor, called boil-
up.[1]
At the point when two or more components differ in boiling point by approximately 50°C or less and
form a non-ideal liquid solution, the relative volatility might be beneath 1.10. At that point,
separation by ordinary distillation might be uneconomical and if an azeotrope forms even impossible.
In that occasion, the accompanying separation techniques, referred to as enhanced distillation by
Stichlmair, Fair, and Bravo, should be explored:[3]
1. Extractive Distillation:
A technique that utilizes a large amount of a relatively high-boiling solvent to modify the liquid-
stage activity coefficients of the mixture, so that the relative volatility of the key components turns
out to be increasingly great. The solvent enters the column above the feed entry-stage and a couple of
trays underneath the top and exits from the bottom of the column without causing an azeotrope to be
formed. In the vent that the feed to the column is an azeotrope, the solvent breaks it. Additionally,
the solvent may switch volatilities.

2. Salt Distillation:
A variety of extractive distillation in which the relative volatility of the key components is modified
by dissolving a solvent, ionic salt in the top reflux. Since the salt is nonvolatile, it remains in the
liquid phase as it goes down the column.

3. Pressure-Swing Distillation:
A technique for separating a pressure-sensitive azeotrope that uses two columns worked in
arrangement at two different pressures.

4. Homogeneous Azeotropic Distillation:

A technique of separating a mixture by including an “entrainer” that forms a homogeneous
minimum- or maximum-boiling azeotrope with at least one feed component. The “entrainer” is
added close to the top of the column, to the feed, or close to the bottom of the column, depending
upon whether the azeotrope is expelled from the top or bottom.

5. Heterogeneous Azeotropic Distillation:

A progressively valuable azeotropic-distillation technique in which a minimum-boiling
heterogeneous azeotrope is formed by the “entrainer”. The azeotrope parts into two liquid phases in
the overhead condensing system. One liquid phase is sent back to the column as reflux, while the
other liquid phase is sent to another separation step or is a product.

6. Reactive Distillation:
A technique that adds a separating agent to respond selectively and reversibly with at least one of the
constituents of the feed. The reaction product is in this manner distilled from the nonreactive
components. The reaction is then turned around to recuperate the separating agent and the other
reacting components. Reactive distillation additionally refers to the situation where a chemical
reaction and multistage distillation are conducted simultaneously in a similar mechanical assembly to
deliver other chemicals. This combined operation, sometimes referred to as catalytic distillation if a
catalyst is used, is particularly fit to chemical reactions restricted by equilibrium constraints, since
one (or more) of the products of the reaction is (are) continuously separated from the reactants.

4. Classification of Distillation Processes

Distillation columns are of two types depends on the mode of operation, specifically, batch
distillation and continuous distillation.

4.1. Batch Distillation Processes

In batch distillation, the feed is introduced batch-wise to the column. This column is first charged
with a “batch” and afterward the distillation process is done. At the point when the desired task has
been accomplished, the following batch of feed is fed into the reactor. Vasudha Pharma Chem
Limited utilizations Batch Distillation Process to produce its final products. Even though the
columns are capable of being operated under both batch and continuous conditions, the organization
uses all its columns in a batch mode.
In batch distillation processes, various types may be recognized: (1) simple batch distillation, (2)
constant-level batch distillation, (3) multi-stage batch distillation, and (4) inverted batch distillation.
For further information about each type, [1] may be used as a reference.

4.2. Continuous Distillation Processes

In continuous distillation columns, a continuous feed stream is employed to enter the products. No
volunteered interruptions are made during the operation of a continuous distillation column.
Continuous columns are capable of handling high throughputs. Aside from this, parallel variations
can come helpful in a continuous distillation column, for example as multiple feed points and
multiple output points. Continuous distillation columns are used in the majority of petroleum and
chemical industries.
 5. Types of Distillation Columns
There are different types of distillation columns each varying concerning efficiency and
utility. The most generally used types of distillation columns used in the industry are: (1)
Tray Columns and (2) Packed Columns. Figure I.3 shows the two types of distillation
columns: trays and packed columns with the equipment of each column.

Tray Column Packed Column

Tray Figure I.3.: Types of Distillation Column in Chemical industries

Columns
take advantage of differences in pressure and temperature to separate the components. In a tray
column, the weir keeps up and holds a level of liquid. The entry of the liquid is from the down-comer
of the plate which is directly above it. The vapor comes from the bottom with sufficient pressure that
it overcomes the pressure applied due to the height of the liquid in the tray. Therefore, in this way,
mass and energy transfer takes place between the two components.[4]

In Packed Columns, solid packing is utilized to facilitate contact between the two phases. Packed
columns are the most productive distillation columns since they can perform well at low pressure and
low liquid and vapor packing. At high flow rates, their efficiency is heavily compromised due to
heavy fouling and corrosive conditions. Packed Columns are capable of giving a contact zone of
more than double that of tray columns.[4]

6. Distillation column components

A distillation column can be divided into four main components that can be studied:
1- R section or Rectifying Section.
2- S section or Stripping Section.
3- Feed Stream.
4- Condenser/Reboiler.

6.1. Rectifying section

The rectification section is the part of the distillation column which lies above the feed point. The
procedure occurring in Rectifying Section is
called “Rectification”.
This procedure is shown in Figure I.4(a).
During this process, the vapor phase is
continuously enriched in the lighter
component which makes the final product. A
condenser is utilized at the top of the
rectifying section to condense these vapors to
liquid. To accomplish further purification, this
liquid is sent again into the rectifying column
in the form of reflux. A mass balance, further
showed in chapter II should be elaborated to
deduce the relation of the equation for this (a)
section.[1] (b)
Figure I.4.: (a) Rectifying section, and (b) Stripping section in a
distillation column
6.2. Stripping Section

Stripping Section is the part of the distillation column which lies below the feed point. The process
occurring in the Stripping Section is called “Stripping”. Figure I.4(b) represents the striping section
in a distillation column.
During this procedure, the heavier component is stripped off and concentrated liquid phase forms the
bottom product. A reboiler is used at the bottom of the stripping section to vaporize the liquid. At
each separation stage, the vapor enters from the stage below at a high temperature while this liquid
stream enters from the stage above at a lower temperature. Heat and mass transfer occur such that the
exiting streams (bubble point liquid and dew point vapor at the same temperature and pressure) are in
equilibrium with each other. Also, for the stripping section, and later on in chapter II, mass and
energy balances are done and the relation of the equation for the stripping section is given. [1]
 6.3. Feed Stream
There are different manners by which feed streams can be given to a distillation column. Feed stream
considerations are important in determining the operating lines for rectifying and stripping sections.
Knowledge of operating lines is important because it provides us with information regarding the
theoretical number of stages.
Feed streams are extensively of 5 types:
6.3.1. Sub-Cooled Liquid
Sub-Cooled feed contains liquid feed cooled to a very less temperature, but more than its freezing
point. Accordingly, as soon as feed is fed into the column, the vapors going up from the stripping
section get cooled and changed over into liquid.
6.3.2. Bubble-Point Liquid
Bubble point liquid contains feed which is warmed up to its bubble point. There are no traces of
vapor in the feed and the rising vapors inside the column also remain unaltered in the composition.
6.3.3. Partially vaporized
The partially vaporized feed contains both liquid and vapors given as input to the distillation column.
Liquid feed settles to the bottom in the stripping section, while vapor feed goes to the top in the
rectifying section.
6.3.4. Dew-Point Vapor
Dew-Point vapor contains purely vaporized feed. The whole feed goes into the rectifying section
along with vapors already inside the column.
6.3.5. Superheated Vapor
Superheated Vapor feed contains vapor heated to an extremely high temperature. Because of this, a
portion of the liquid slipping from the rectifying section gets vaporized and joins with the rising
vapors.

6.4. Condenser/Reboiler

6.4.1. Condenser

A condenser is a two-phase flow heat exchanger in which heat is created from the change or the
conversion of vapor into liquid (condensation) and the heat generated is expelled from the system by
a coolant. Condensers might be classified into two principal types: those in which the coolant and
condensate stream is separated by a solid strong surface, generally a tube wall, and those in which
the coolant and condensing vapor are brought into direct contact.[4]
The direct contact type of condenser may consist of a vapor which is risen into the liquid, a liquid
which is sprayed into a vapor, or a packed-column where the liquid flows descending as a film over a
packing material against the upward flow of vapor. Condensers in which the streams are separated
might be partitioned into three main types: air-cooled, shell-and-tube, and plate.
  In the air-cooled type, condensation happens inside tubes with cooling provided by air blown
or sucked over the tubes.
 In shell-and-tube condensers, the condensation may happen inside or outside the tubes. The
direction of the unit might be vertical or horizontal.
 In the refrigeration and air-conditioning industry, different types of two-phase flow heat
exchangers are used. They are characterized by whether they are coils or shell-and-tube heat
exchangers. Evaporator and condenser coils are utilized when the subsequent fluid is air as a
result of the low heat transfer coefficient on the airside.

In a mechanical side, the condenser that is used in distillation columns is shell-and-tube condenser E-
type. It has two outlet nozzles: one for the vent and the other for the condensate outlet. Non-
condensable has the impact of depressing the condensation temperature and, in this manner,
decreasing the temperature difference between the streams. In this way, plainly that there is no
chance of non-condensable accumulation during condenser operation. Hence, the vent is provided.[4]
There are mainly three types of condensers which are used in a distillation column, two are the most
used:

 Total condenser,
 Partial condenser,
 Mixed condenser (total and partial). It is rarely used in distillation columns.

These 2 types of condensers are illustrated in Figure I.5.

(a) (b)
Figure I.5.: Condensers used in distillation columns, (a) Total condenser, and (b) Partial
condenser

 Total Condenser

The schema of this type of condenser is shown in Figure I.5(a). As the name suggests a total
condenser will condense the vapor that is coming inside the condenser from the top of the highest
point of the distillation column into the liquid form or condensate form. So essentially, all vapor is
being condensed and only the liquid condensate is coming out from the condenser.
Now whatever liquid is coming out from this condenser, a part of it is sent back to the distillation
column as reflux, and the rest is taken out as the distillate (top product). Both the distillate and the
reflux will be in the liquid form when the total condenser is utilized. But if the distillate or the top
product is needed in vapor form then the partial condenser comes into the situation.

 Partial Condenser

It is shown in Figure I.5(b). Partial Condenser will only condense a part of the incoming vapor from
the top of the distillation column and the condensed liquid would flow into the column as reflux
whereas the uncondensed vapor will be collected as distillate or the top product.

In most cases, the condensed liquid is refluxed into the column and the overhead product drawn is in
the vapor form. On the other hand, there are some cases where only part of the condensed liquid is
refluxed. In these cases, there will be two overhead products, one a liquid with the same composition
as the reflux stream while the other is a vapor product that is in equilibrium with the liquid reflux.

The selection of a condenser majorly depends on: [5]

1- Vapor leaving from the top of the column.

2- Desired form of product from the distillate.

When vapor leaving from the top contains non-condensable components and when the required final
form of distillate is gaseous then partial condenser can be used. When vapor leaving from the top
has no non-condensable components and when the required form of the product is liquid then total
condenser is used. So, the main purpose of using the total condenser is to condense all the vapors
from the top of the column.

6.4.2. Reboiler

A reboiler is a heat exchanger that is used to produce the vapor provided to the bottom tray of
a distillation column. The liquid from the bottom of the column is partially vaporized in the
exchanger, which is usually of the shell-and-tube type. The heating medium is regularly condensing
steam, but commercial fluid sand different procedure streams are also used. Boiling happens either in
the tubes or in the shell, depending on the type of reboiler. Exchangers that supply vapor for other
unit operations are referred to as vaporizers, but are similar in most respects to reboilers.[4]

Various types of reboilers are utilized to provide boil-up vapor to the stripping section of a
distillation column. For small laboratory, the reboiler consists of a reservoir of liquid located just
below the bottom plate to which heat is supplied from (1) a jacket or mantle that is heated by an
electrical current or by condensing steam, or (2) tubes that pass through the liquid reservoir carrying
condensing steam. Both of these types of reboilers have limited heat-transfer surfaces and are not
suitable for industrial applications.[1]
For plant-size distillation columns, the reboiler is typically an external heat exchanger of either the
kettle or vertical/horizontal thermosyphon type.

 Kettle type Reboiler

Figure I.6 shows the schema of this type of reboiler.

Figure I.6.: Kettle-type reboiler

In this reboiler, the liquid leaving the sump (reservoir) at the bottom of the column enters the kettle,
where it is partially vaporized by the transfer of heat from tubes carrying condensing steam or some
other heating medium. The bottoms product liquid leaving the reboiler is assumed to be in
equilibrium with the vapor returning to the bottom tray of the column. Thus, the kettle reboiler is a
partial reboiler equivalent to one equilibrium stage. The kettle reboiler is sometimes located at the
bottom of the column to avoid piping.
For the following condition we can use kettle type reboiler:

 Pressure drop in kettle type reboiler is lower so it is suitable for the Vacuum services.
 In kettle type reboiler liquid converted into vapor so when you need a higher vaporization
rate then it is suitable.
 When hot fluid and cold fluid have more temperature difference then you have to use an
expansion joint for the compensation of expansion and contractions of shell and tube but in
kettle type U-bend tube arrangement used so, this problem can eliminate.[1]

 Vertical Thermosyphon Reboiler

The vertical thermosyphon reboiler may be of the type shown in Figure I.7(a) or I.7(b). In the
former, both the bottoms product and the reboiler feed are withdrawn from the column bottom sump.
Circulation through the tubes of the reboiler occurs because of the difference in static heads of the
supply liquid and the column of partially vaporized fluid flowing through the reboiler tubes. The
partial vaporization provides enrichment of the exiting vapor in the more volatile component.
However, the exiting liquid is then mixed with liquid leaving the bottom tray, which contains a
higher percentage of the more volatile component. The result is that this type of reboiler arrangement
provides only a fraction of an equilibrium stage and it is best to take no credit for it.[1]
 (a) (b)
Figure I.7.: Vertical Thermosyphon Reboiler, (a) down-comer far from the
inlet of the reboiler, (b) down-comer next to the inlet of the reboiler

A more complex and less common vertical thermosyphon reboiler is that of figure 1.7(b), where the
reboiler liquid is withdrawn from the down-comer of the bottom tray. Partially vaporized liquid is
returned to the column, where the bottoms product from the bottom sump is withdrawn. This type of
reboiler does function as an equilibrium stage.
Horizontal thermosyphon reboilers are sometimes used in place of the vertical types when only small
static heads are needed for circulation, surface-area requirement is very large, and/or when frequent
cleaning of the tubes is anticipated. A pump may be added for either thermosyphon type to improve
circulation. Liquid residence time in the column bottom sump should be at least 1 minute and
perhaps as much as 5 minutes or more.[1]

 Horizontal Thermosyphon Reboiler

Horizontal Thermosyphon reboiler again classified into two categories:

 Natural circulation.
 Forced circulation.

o Natural circulation:
Natural circulation-type Thermosyphon reboiler is used for sensitive materials with lower viscosity
because here circulation is done because of the temperature difference. The operating cost is lower
because we are not using a pump at the bottom of the distillation column. When the vaporization
requirement is lower, then it is suitable. It is used for fouling service because process fluid is on the
tube side so we can easily clean the tube.[1]

o Forced circulation:
In forced circulation we provide a pump between distillation column bottom and reboiler. It is used
for the high viscosity fluid when vaporization required is less and for fouling services.
7. Trays in distillation columns

Any physical device that provides good contact between the vapor and liquid phases present in
industrial-scale distillation columns or laboratory-scale glassware distillation columns constitutes a
"plate" or "tray".[6]
In the distillation column, trays are used to provide liquid holdup to achieve the proper vapor-liquid
mass transfer that the distillation process requires for separation. Also, they facilitate contact
between the vapor phase and the liquid phase so that mass transfer between the two phases can take
place.[7]

Figure I.8.: Vapor and liquid flows through a tray of a distillation column

The passage of vapor and liquid flow is shown in Figure I.8.[6]. Each tray can be considered as being
made up of three sections: weir, bubbling area, and down-comer.

 The weir maintains a desired liquid level on the tray.

 Down-comers guide liquid flows from an upper tray to a lower tray.
 The bubbling area is the place where vapor-liquid contact takes place. Vapor flows through
the openings on the tray from below, and into the liquid flowing across the tray, forming a
foaming, turbulent mixture.[6]

For most trays, liquid flows across an “active area” of the tray and then into a “down-comer” to the
next tray below, and so on. Inlet and/or outlet weirs control the liquid distribution across the tray.
Vapor flows up the tower and passes through the tray active area, bubbling up through (and thus
contacting) the liquid flowing across the tray. At excessively high vapor rates, liquid is carried
upward from one tray to the next (essentially back mixing the liquid phase in the tower). [8]

Trays are supported in a vessel through support rings or beams. On the operating principles, there are
four major types of tray column: bubble cap tray, sieve tray, dual flow tray, valve tray.
 7.1. Bubble Cap Tray

The oldest widely used equilibrium-stage plate is the bubble cap tray. A bubble cap tray is perforated
flat which has a riser (chimney) fitted 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
bubbles where the mass transfer takes place. Each tray is provided with one or more down-comers
which the liquid flowing.[9] The passage of liquid and vapors through the bubble cap tray is shown
in Figure I.9.

Figure I.9.: Liquid and Vapor flowing through the bubble cap tray

 Advantages:
 They are used primarily where large turndown ratios are required. Turndown ratio is
the range of highest to the lowest flow rates.
 Their construction allows very low liquid rates to be handled with little or no
leakage.
 Due to their ability to operate at low vapor and liquid rates, bubble cap trays are used
in a significant portion of fractionation tray installations.

 Disadvantages:
 Bubble cap tray requires high tray spacing and has a significant liquid gradient.
 There is a problem of coking and fouling in case of dirt mixture.
 The design is also expensive to adopt and has resultant poor turndown performance.
[10]

7.2. Sieve Tray

Sieve trays are simply perforated metal plates punched into the plate with holes in them. Vapor
comes out from the holes to give a multi-orifice effect. Vapor flow through the tray deck to contact
the liquid is controlled by the number and the size of the perforations. The liquid flow is transported
down the tower by down-comers, a dam, and an overflow device on the side of the plate. The vapor
flows upward through the perforation and disperses into the flowing liquid over the plate. There is no
liquid seal in case of trays without down-comer and the liquid weeps (called weeping) through the
holes at low flow rates, reducing the efficiency of the plate. This weeping is due to the vapor
velocity: when it is low, weeping happens [9]. The general form of the flow on a sieve tray is typical
of a cross-flow system with perforations in the tray taking the place of the more complex bubble
caps.[11] Figure I.10. shows liquid and vapor flows through sieve trays.

Figure I.10.: Liquid and Vapor flowing through the sieve tray

 Advantages:
 Sieve trays can be used in almost all services.
 They are simple and easy to fabricate and therefore relatively inexpensive.

 Disadvantages:
 They have minimum capacity (approximately 70%).
 Not flexible.
 Turndown is poor (efficiency falls below the design condition).

7.3. Dual Flow Tray

A dual flow tray is a sieve tray without a down-comer. Vapors move up to the tray above through
the hole, while the liquid travels down in the same hole that can result in small-distribution and
low efficiency.[11]
  Advantages:
 Suitable handling slurries, corrosive services, and highly fouling services because they have
enough open area on the tray deck.
 Greater capacity due to the biggest bubbling area.
 Easy to maintain and to install and less expensive.

 Disadvantages:
 Poor turndown ratio resulting from the rapid fall-off in efficiency as the vapor loading
decreases.
 Mal-distribution problems in the case of improper feed, reflux, or vapor distribution.
 Not robust: if something goes wrong, the column may not work at all instead of operating at a
lower efficiency.

7.4. Valve Tray

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. This valve tray is a steel sheet on
which liftable valves are mounted. They are much more efficient than sieve trays. Valves can be
round or rectangular.[9] Each hole is fitted with a valve consisting of a cap that overlaps the hole,
with legs or a cage to limit vertical rise while maintaining the valve cap in a horizontal orientation.
Without vapor flow, each valve covers a hole. As the vapor rate increases, the valve rises, providing
a larger opening for vapor to flow. At high vapor velocities, the valve fully open leading to a
maximum slot for gas flow. When gas velocity drops, valve drops resulting in constant gas velocity
through the slot, so constant efficiency and weeping (entrainment) prevention. At intermediate
velocities, some of the valves on the tray will be open and some closed. Usually, the valves alternate
between open and closed positions. [12]. The principle of liquid and vapor flows is shown in Figure
I.11.

Figure I.11.: Liquid and vapor flowing through valve trays.

 Advantages:
 Better turndown properties than sieve trays, so more flexible when feed rate varies.
  High separation efficiency and large flexibility because they can operate over a wide range of
flow rates.
 Efficient cost (not expensive).

 Disadvantages:
 In dirty or fouling services, the valves may get stuck due to the build-up of sludge or
corrosion products around the valve. This results in reducing the tray open area and it can
lead to premature flooding.
 Weeping may result if excessive valve opening occurs prematurely. This will reduce the tray
turndown.

When comparing the performance of bubble-cap, sieve, and valve trays are, different factors
should be taken into consideration:
 Cost:
Bubble-caps are more expensive than sieve or valve trays. The relative cost of the trays
depends on the material of construction used. Sieve trays are normally the cheapest because
of its simple design.

 Operating Range:
It refers to the range of vapor and liquid rates over which the tray will operate satisfactorily:
Bubble-cap trays have a positive liquid seal and can operate at very low vapor rates with high
efficiency.
Sieve trays cannot operate at very low vapor rates because they rely on the flow of vapors
through the holes to hold the liquid on the tray
Valve trays give greater flexibility than sieve trays and with a low cost than bubble-caps.
Thus, first, bubble-cap trays have the widest operating range, followed by a valve tray, and
then sieve tray.
 Pressure Drop:
The pressure drop is very important in vacuum operations. The tray pressure drop will
depend on the detailed design of the tray, but in general, arranging from the lowest to the
highest pressure drop, sieve trays give the lowest pressure drop, followed by valves, and
finally bubble-caps.

 Maintenance:
Sieve trays can be easily cleaned. Bubble-caps aren’t suitable because they plug in dirty
services.

In summary, sieve trays are the cheapest and are useful for most applications. Valve trays should be
considered if the specified turndown ratio cannot be met with sieve trays. Bubble-caps should be
used only when very low vapor rates have to be handled and a positive liquid seal is essential at all
flow rates.
 Table I.1.: Comparison between various tray types [1]

Table I.1 shows a comparison of different types of trays based on cost, pressure drop, mass-transfer
efficiency, vapor capacity, and flexibility in terms of turndown ratio (ratio maximum to minimum
vapor capacity).
At the limiting vapor capacity, flooding of the column occurs because of excessive entrainment of
liquid droplets in the vapor causing the liquid flow rate to exceed the capacity of the down-comer,
so, it goes back up the column. At low vapor rates, the weeping of the liquid becomes more
excessive through the tray openings. Because of their low relative cost, sieve trays are preferred
unless flexibility is required, in which case valve trays are best. Bubble-cap trays, which exist
already, are rarely specified for new installations but they can be used when the amount of liquid
holdup on a tray must be controlled to provide adequate residence time for a chemical reaction.

On trays, different flow regimes can be observed, depending on the gas flow rate: (1) Bubble
regime, (2) Foam regime, (3) Froth regime, and (4) Spray regime.[12]

(a) (c)
(b)
Figure I.12.: Different flow regimes observed on the surface of a tray: (a) Bubble regime, (b) Froth regime,
and (c) Spray regime.
 1. Bubble regime:
This regime is represented in Figure I.12(a). It occurs at low gas flow rates. The liquid is similar to a
stagnant pool with distinct bubbles rising through it. Since the mixing is poor, the liquid and vapor
are poorly contacted, which leads to low stage efficiency. This type of regime is undesirable in
commercial applications.

2. Foam regime:
It occurs at higher gas flow rates. The liquid phase is continuous and has distinct bubbles rapidly
rising through it. Because of the large surface area in a foam, the area for vapor-liquid mass transfer
is large, and stage efficiency is high. If the foam is too stable, it can fill the entire region between
stages → Entrainment becomes excessive → stage efficiency drops → column may flood so it fills
up with liquid and becomes inoperative. So, the use of a chemical antifoam agent is required. This
type of regime is usually at vapor flow rates that are too low for most industrial applications.

3. Froth regime:
Figure I.12(b) shows this type of regime. This is almost the flow regime used in commercial
operation. It occurs even when the vapor flow rates are high. The liquid is continuous and has large
voids of vapor to pass rapidly through it. The surface of the liquid is boiling violently, and there is
splashing. The liquid phase is mixed, but the vapor phase is not. This type of regime is efficient in
most distillation systems where the liquid-phase mass transfer controls.

4. Spray regime:
The considered regime is shown in Figure I.12(c). The vapor is continuous while the liquid occurs as
a discontinuous spray of droplets. The vapor is very well mixed, but the liquid droplets usually are
not, this results in low mass transfer rate and stage efficiencies. If the velocity of the vapor increases
slightly, it can cause the column to go from the froth to the spray regime and cause a significant
decrease in stage efficiency.[12]

8. Methods for calculation in distillation columns

Depending on the type of distillation process that is used (Binary Distillation Column,
Multicomponent Distillation Column, Batch Distillation Column …), different methods for the
calculation can be applied:

 Batch Distillation Column is used in biochemical, biomedical, and pharmaceutical industries,

where production amounts are small and very high purity and ultra-clean product is needed.
In this type of distillation, usually, we use the Rayleigh Method. This method is based on an
equation that relates the quantity to the concentration of the more volatile component in
 batch distillation. The equation is formulated from an unsteady-state material balance in
which vapor leaving the still is in equilibrium with the liquid. [1,13]
 Multicomponent Distillation Column is usually used when the feed is mainly composed of
more than two components like the mixture of alkanes (propane, butane, pentane, hexane,
heptane). Here, different methods can be applied for a specific purpose:
 Fenske Method or Fenske Equation in case of a total reflux.
 Underwood Method or Underwood Equation in case of a minimum reflux.
 Gilliland Correlation to determine the number of stages at the finite reflux ratio.
We can notice that these three methods can work concerning each other, depending on the
application needed, and can be combined by the FUG method (Fenske, Underwood, and
Gilliland method). [1]
 For Binary Distillation Column, we have:
 W.K. Lewis Method called “Constant Molar Overflow CMO”. It’s a stage-by-stage
solution method where, in each stage of the column, the amounts of vapor and liquid
are calculated.
 McCabe THIELE Method is a graphical technique, based on a simple principle of
calculation, used in different purposes or applications:
 The number of equilibrium stages and Feed stages location.
 Open Steam heating.
 Effect of Reflux Ratio (total reflux ratio or minimum reflux ratio).
 Multiple feeds and side streams.
So, because of its wide variety of applications, McCabe THIELE Method will be used later for
calculation of any component or characteristic in Chapter 3 dedicated to the distillation column
design procedure.

9. Simple Binary Mixtures

Binary mixtures are the combination of two components having relatively different volatilities, or
tendency to reside in a vapor phase. When the components in a mixture are more than two, then the
mixture is not called “binary mixture”, thus it is called “multi-component mixture”.
In distillation, we can separate binary and multi-component mixtures. In this project, we will focus
only on binary mixtures since our goal is to separate a specific binary mixture with a small difference
between the volatilities of the two components.
In binary mixtures, the more volatile component, or the one with the lower boiling point temperature,
is known as the Light Key (LK); and the other is referred to as the Heavy Key (HK). When heat is
applied to the mixture, the molecules become excited from the added kinetic energy and some of the
mixture will gain enough energy to escape into the vapor phase. Once the mixture reaches vapor-
liquid equilibrium (VLE), the vapor phase will consist of a higher concentration of the light key than
the original mixture and less of the heavy key.[1]
Table I.2, taken partially from the study of Mix et al. [2], lists just some of the more common
commercial binary distillation operations in decreasing order of difficulty of separation. Included are
representative nominal values of relative volatility, number of trays, column operating pressure, and
reflux-to-minimum-reflux ratio. Although the data in Table I.2 refer to trayed towers, distillation can
also be carried out packed columns. More and more frequently, additional distillation capacity is
being achieved with existing trayed towers by replacing all or some of the trays with sections of
random or structured packing.

Table I.2.: Representative Commercial Binary Distillation Operation [2]

10. Conclusion
In this chapter, an overview of the separation process is done with a small history of the distillation
columns. Then different details have been explained point by point including the classification of
distillation column (batch/continuous), its type (packed or trayed column), its principal components
like condenser and reboiler. Also, different types of trays are detailed (bubble-cap, sieve, or valve).
Besides, in this chapter all methods for calculation that can be used are discussed briefly, similar to
binary mixtures which are discussed in the end.
Later on, in chapter II, we will discuss the McCabe THIELE method that is used in binary distillation
columns for separating a specific binary mixture with all its assumptions, equations, and
specifications.

List of References:
1. J. D. Seader, Ernest J. Henley, Separation Process Principles, 2nd ed., Wiley,2005.
2. FORBES, R.J., Short History of the Art of Distillation, E.J. Brill, Leiden (1948).
3. STICHLMAIR, J., J.R. FAIR, and J.L. BRAVO, Chem. Eng. Progress, 85(1), 6369 (1989).
4. Kakaç, Sadik_ Liu, Hong tan_ Pramuanjaroenkij, Anchasa - Heat Exchangers _ Selection,
Rating, and Thermal Design, Third Edition-CRC Press (2012)
5. http://Kolmetz.com/pdf/EDG/ENGINEERING%20DESIGN%GUIDELINES
%2%20distillation%20column%20-%20Rev%2004%20web.pdf
6. Perry, Robert H. & Green, Don W. (1984). Perry's Chemical Engineers' Handbook  (6th ed.).
McGraw-Hill.  ISBN  0-07-049479-7.
7. Distillation Tray Fundamentals. Cambridge University Press, 2009.
8. R. Perry, D. Green and R. Perry, Perry’s Chemical Engineers’ Handbook, New York:
McGraw-Hill,2008
9. https://www.slideshare.net/mobile/MohamedSalah69/types-and-design-of-the-towers-trays
10. https://issuu.com/mtpi2/docs/untitleddocument__7_
11. J.F. RICHARDSON, ... J.R. BACKHURST, in Chemical Engineering (Fifth Edition),
Volume 2, 2002
12. Fractional Distillation course 3rd year of chemical/petrochemical engineering.
13. https://www.oxfordreference.com/view/10.1093/acref/9780199651450.001.0001/acref97801
99651450-e-2411
14. IX, T.W., J.S. DWECK, M. WEINBERG, and R.C. ARMSTRONG, Chem. Eng. Prog., 74
(4), 49-55 (1978).