Distillation Columns: 1 March 2012

DISTILLATION COLUMNS
 Distillation is one of the most common liquid-liquid separation

processes, and can be carried out in a continuous or batch
system.
 Distillation columns are one of the most often used types of
separation equipment in industry.
 There are many types of distillation columns, each designed to
perform specific types of separations, and each design differs in
terms of complexity.
 Distillation can be used to separate binary or multi-component
mixtures. Many variables, such as column pressure, temperature,
size, and diameter are determined by the properties of the feed
and the desired products.
Copyright of Shell International RESTRICTED March 2012 1
DISTILLATION COLUMNS
 Some specialized columns perform other functions, such as
reactive distillation columns, which combine reaction and
separation of products into a single unit.
 Distillation works by the application and removal of heat to
exploit differences in relative volatility. The heat causes
components with lower boiling points and higher volatility to be
vaporized, leaving less volatile components as liquids.
 Mixtures with high relative volatilities are easier to separate. This
makes separations of close-boiling and azeotropic feeds difficult,
so special distillation techniques have to be used to separate
these mixtures.

TYPES OF DISTILLATION
 BATCH COLUMNS
In batch operation, the feed to the column is introduced batch-wise.
That is, the column is charged with a 'batch' and then the distillation
process is carried out. When the desired task is achieved, a next
batch of feed is introduced.
 CONTINUOUS COLUMNS
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 most common of the two types.
We shall concentrate only on this class of columns.

PRACTICAL POINTS TO BE DISCUSSED
 H2S Stripper / CO2 Absorber & Stripper in NH3 plant in

Coromandel Fertilizers Ammonia Plant. (To Discuss HSE incident also)
 Maleic Anhydride De hydration column (Azeotropic Distillation
column) & Pure Maelic Anhydride column issues in Malaysia Plant
 Water Distillation column issues in Shell GTL – Running column
without Reflux for certain period of time & Running column when
steam to re boiler fails.
 LES Column issues Shell GTL. (Corrosion issues CS + SS column)
 Reaction column issues in BDO plant.
 Trays fallen in Butanol Recovery column in Petronas plant.
 Start up & Shutdown sequence steps in Distillation Column.

TYPES OF CONTINUOUS COLUMNS
Continuous columns can be further classified according to:
 THE NATURE OF THE FEED THAT THEY ARE PROCESSING
Binary column - feed contains only two components

Multi-component column - feed contains more than two components
 THE NUMBER OF PRODUCT STREAMS THEY HAVE
Multi-product column - column has more than two product streams

 WHERE THE EXTRA FEED EXITS WHEN IT IS USED TO HELP WITH THE
SEPARATION
 Extractive distillation - where the extra feed appears in the bottom product
stream
 Azeotropic distillation - where the extra feed appears at the top product
stream

BASIC OPERATION AND TERMINOLOGY
 The liquid mixture that is to be processed is known as the feed and

this is introduced usually somewhere near the middle of the column to
a tray known as the feed tray.
 The feed tray divides the column into a top (enriching or rectification)
section and a bottom (stripping) section. The feed flows down the
column where it is collected at the bottom in the reboiler.
 Heat is supplied to the reboiler to generate vapour. 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 vapour 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.


PROBLEMS IN DISTILLATION & ITS TROUBLE SHOOTING
Foaming, Entrainment, Weeping, Flooding , Channeling & Dumping:

 Foaming in a distillation column is the expansion of liquid that provides
high interfacial liquid-vapor contact. Although one of the least common
causes of distillation column malfunctions, foaming can increase until the
fluid in one tray mixes with the liquid on the above tray in a process called
entrainment.
Causes of foaming:
 Foaming causes may be because of the gas velocity is to too high or the
rate of evaporation is too fast.
 The design, condition and placement of the trays used in the column can
add to a foaming problem.
Example: When the overhead disengaging space is not high enough. This
means the trays are not separated far enough above each other to keep the
liquid in the bottom trays from foaming up into the top trays.
 You can improve the purity of the fraction by increasing the surface area of
the fractionation column. Replacing some of the trays on the top section of
the column with steel structured packed bed.
 Shifting the top product ( Pure Maleic Anhydride ) Draw off point to high
level to improve the purity of the top product.
Note: Discuss Maleic Anhydride Distillation column changes (like above 2
points) done to improve the quality of Maleic Anhydride in one of the plant in
Malaysia where I worked.
 Entrainment refers to the liquid carried by vapour up to the tray above and
is again caused by high vapour 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.
Note: Discuss some of the practical problems faced related to above.
H2S STRIPPER & CO2 REMOVAL STRIPPER problems in AMMONIA PLANT
 Loading & Flooding - is brought about by excessive vapour flow, causing
liquid to be entrained in the vapour up the column. The increased pressure
from excessive vapour also backs up the liquid in the down comer, causing
an increase in liquid holdup on the plate above.
 Loading point of a column is when the gas velocity is high enough to restrict
the flow of liquid. After this point, the pressure drops at a much faster rate till
another point, known as the flooding point, when all the liquid is carried
away by the gas.
 Dumping & Weeping - This phenomenon is caused by low vapour flow. The
pressure exerted by the vapour is insufficient to hold up the liquid on the
tray. Therefore, liquid starts to leak through perforations. Weeping is
indicated by a sharp pressure drop in the column and reduced separation
efficiency.

 Channeling - In packed column, mal distribution is detrimental to

packing efficiency and turndown. Mal distribution occurs at low
liquid and/or vapour flows, or if the liquid feed is not distributed
evenly over the packings. Down in the bed, the liquid tends to flow
toward the wall. This condition is also known as channeling.
NOTE:
1. To Discuss some of the practical problems in Reaction column in
BDO plant in SIPCHEM.
2. To Discuss some of the safety related incidents happened in
Distillation column ( Fire at the bottom of the distillation column
during shut down ) + Confined space entry issue incident in CO2
stripper etc.,

OTHER PRACTICAL PROBLEMS IN DISTILLATION COLUMNS
 Change in feed composition –Discuss Dehydration column
(Azeotropic column) feed issues in Maleic Anhydride plant in Malaysia.
 Faulty Level / Flow / DP indications. Discuss Maleic Anhydride Column
issues (where solidification point of the liquid is 53 deg c) in one of the
Malaysia & Saudi palnt.
 Tray collapse inside
 Column flooded with liquid and steam to re boiler introduced at full rate
 Some of the valve suction valve leaks ( need to be attended ) without any
upstream isolation keeping column under running – Discuss WDU column
issue in SHELL GTL.
 Residence time for liquid and gas contact.
 Condenser / Re boiler choke.

REFLUX AND REFLUX RATIO IN DISTILLATION COLUMNS
 Reflux is a technique involving the condensation of vapors and the

return of this condensate to the system from which it originated.
 Reflux involves heating the chemical reaction for a specific amount of
time, while continually cooling the vapour produced back into liquid
form, using a condenser.
 Many organic reactions are unreasonably slow and can take an
extended period of time to achieve any noticeable effect so heating is
often used to increase the rate of reaction. To address this, heating
under reflux is used.
 Reflux ratio is the ratio between the boil up rate and the take-off rate.
Or in other words, it is the ratio between the amount of reflux that
goes back down the distillation column and the amount of reflux that
is collected in the receiver (distillate).
 Minimum Reflux Ratio (R min) is the lowest value of reflux at which

separation can be achieved even with an infinite number of plates. It
is possible to achieve a separation at any reflux ratio above
the minimum reflux ratio.
 At total reflux, the number of theoretical plates required is a
minimum. As the reflux ratio is reduced (by taking off product), the
number of plates required increases.
 Optimum Reflux Ratio (R0) is that at which the total cost of
the distillation is a minimum, taking into account the capital cost of
the column (which depends on the number of theoretical plates) and
running cost, which depends on the reflux ratio.

 Refulx ratio = L/D = Condesate back to column /distillate discarded

from column.
 As we increase Refulx ratio, more and more, almost Condesate we
have to route to column back. So number of plate for separation
decreases but reboiler and condenser load will be maximum in case
of Total reflux ratio. And as vapor load will be increased,
diameter5of column will be increased.
 As we decrease reflux ratio, it will give purity maximum untill certain
limit called minimum reflux ratio. At this time purity will be high ,
both reboiler and condenser duty will be minimum. But infinite
number of plates required for desired separation.

STRIPPING & DISTILLATION COLUMNS
 Stripping is essentially a distillation process where the heavy product is
water/liquid and the lighter product is generally mixture of organic volatile
materials. Generally steam is used for heating purpose in the column.
Ex: Wastewater stream (i.e. contains some organic volatile materials) is put into
stripping tower at the top. Steam or hot air is introduced at the bottom and it
makes contact with liquid in counter current fashion either in a packed or tray
tower. As the liquid proceeds down the tower it becomes leaner in organic
material and vapor which rises up becomes richer in organic material. In this
way clean water is collected at the bottom of the tower.
Typical examples are
 Benzene separation from wastewater
 Removal of organics from quench waters.

STRIPPING & DISTILLATION COLUMNS
 Distillation is general known process where multi components are

separated into pure components based on their difference in boiling
points. This column typically consists of enriching section where
concentrated vapors are sent to condenser and a stripping section
where liquid/heavies are present.
 A column is divided into a series of stages. These correspond to a
cascade of equilibrium stages. Liquid flows down the column from
stage to stage and is contacted by vapor flowing upward.
 Typical example
1. Distillation of petroleum product.

AZEOTROPIC DISTILLATION COLUMN
 Azeotropic distillation is a process of distillation wherein you can add

certain components into the mixture to have a better separation process.
 Usually, the certain component added into the mixture is water or
benzene, because these can help in increasing the volatility of a
substance – Discuss here the Dehydration column in MAN Process.
(Volatility is the capacity of the substance to vaporize).
 In this process, the distillation process could form an azeotrope which
can greatly help in the exact process of the separation because it won’t
alter the components like a simple distillation would.
 Azeotropic distillation produces a heterogeneous mixture. In this
method, an entrainer is used to trap particles in the current to separate
the azeotrope.

EXTRACTIVE DISTILLATION
 Extractive distillation is a distillation technique wherein the capability
of mixing or miscibility, the component of being non-volatile, and even
a high boiling point, could be the measurement of separating a
mixture without even forming an azeotrope.
 This kind of method is usually used for mixtures with almost the same
volatility.
 In this method, a separation solvent will be used to interact with the
mixture, thus helping the separation of the components.
 The good thing about this method is that by using the separation
solvent, you can already easily separate the mixture without forming
an azeotrope, which is common in other separation methods.

DIFFERENCE BETWEEN AZEOTROPIC & EXTRCTIVE DISTILLATION
 Azeotropic and extractive distillations are both methods of separating mixtures.
Both of them also use a certain separating solvent to help in the process. The
main difference between the two is in the process of separating the mixture.
 Azeotropic distillation forms an azeotrope right after combining the separation
solvent. This azeotrope can be a complicated way of separating the mixture
because it cannot be easily changed by just a simple distillation.
 In extractive distillation, a specific separation solvent is used in every mixture that
should not form an azeotrope.
 In this way, extractive distillation is a better and easier method than the
azeotropic distillation.
 But you need to bear in mind that if you have a mixture with very different
volatilities, then the most effective separation method would be the azeotropic
distillation.

COMPONENTS OF DISTILLATION COLUMNS
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.

THE TYPE OF COLUMN INTERNALS
 Tray column - where trays of various designs are used to hold up the
liquid to provide better contact between vapour and liquid, hence
better separation
 Packed column - where instead of trays, 'packings' are used to
enhance contact between vapour and liquid

PACKED BED COLUMN OPERATION
 Although packed bed columns are used most often for absorption, they are
also used for the distillation of vapor-liquid mixtures.
 The packing provides a large surface area for vapor-liquid contact, which
increases the column's effectiveness.
 The feed mixture contains components of different volatilities, and enters the
column approximately at the middle. The liquid flows downward through the
packing, and the vapor flows upward through the column.
 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. The exiting vapor contains the most volatile components, while the
liquid product stream contains the least volatile components.

PACKED BED COLUMN OPERATION
 Types of packing include dumped or random packing and stacked

packing.
 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.

PACKING TYPES

PACKINGS IN DISTILLATION COLUMN – TYPES
 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 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.

ADVANTAGES & DISADVANTAGES OF PACKING COLUMNS
 Packed bed columns are often used to recover solvents.
 Most cost-efficient distillation column when the diameter of the

column is less than 0.6 m.
 Because packing can be made from inert materials, packed beds are
able to handle corrosive materials.
 Lower pressure drop than in plate columns preventing column
flooding.
 Good for thermally sensitive liquids.
 Suitable for low pressure operations.
 Packing can break during installation, or due to thermal expansion.
 Not cost efficient for high liquid flow rates.

PLATE OR TRAYCOLUMNS
 The plate, or tray column is the most widely used type of distillation
column.
 The number of trays, or stages in the column is dependent on the
desired purity and difficulty of separation.
 The number of stages also determines the height of the column.

 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


ADVANTAGES & DISADVANTAGES
 Most cost efficient distillation column for diameters greater than

0.6 m.
 The liquid/vapor contact in the cross-flow of plate columns is
more effective than the countercurrent-flow in packed columns.
 Can handle high liquid flow rates cost-effectively.
 Higher pressure drops than packed columns which could cause
column flooding.
 Foaming can occur due to agitation of the liquid by the vapor
flowing up through it.

VACUUM DISTILLATION
 To vaporize a liquid, its temperature can be raised or its pressure
can be decreased. During vacuum distillation, the pressure inside the
distillation column is maintained at a vacuum to lower the
temperature need to vaporize the liquid.
 This method of distillation is applied in situations with heat sensitive
products, liquids with low viscosities, and liquids that tend to foul or
foam.
 In vacuum distillation, vacuum pumps are added to the distillation
system to decrease the column pressure below atmospheric pressure.
In addition, steam ejectors also can be used to create vacuum.
 Vacuum regulators are used to ensure that the pressure within the
column is maintained at a vacuum.

VACUUM DISTILLATION
 Oil refineries often make use of vacuum distillation.

 Normal distillation techniques separate lighter
hydrocarbons and impurities from the heavier
hydrocarbons.
 This bottoms product is further distilled under vacuum
distillation. This allows high boiling point hydrocarbons,
such as lubricants and waxes, to be separated at
economical temperatures.
 Vacuum distillation is also used in the separation of
sensitive organic chemicals and recovery of organic
solvents.
 Columns can be operated at lower temperatures.

 More economical to separate high boiling point components under
vacuum distillation.
 Avoid degradation of properties of some species at high
temperatures.
 High energy costs of vacuum pumps.
 Pressure and energy losses due to any leaks or cracks.
 Large column diameters needed for the process to be efficient.

CRYOGENIC DISTILLATION
 In cryogenic distillation, common distillation techniques are applied

to gases that have been cryogenically cooled into liquids. The system
must operate at temperatures below -150°C.
 During cryogenic distillation, heat exchangers and cooling coils
lower the temperature inside the distillation column. The resulting
system is called a cold box .
 Cryogenic gases are fed into a cold box and distilled at very low
temperatures.
 The cryogenic distillation column can be either a packed bed or a
plate design; the plate design is usually preferred since packing
material is less efficient at lower temperatures.

DESIGN & USAGE EXAMPLES
 In a typical cold box, a nitrogen rejector cryogenically distills out nitrogen
from a feed gas using two tray or packed distillation columns.
 The nitrogen can be bled off to the atmosphere or stored in cryogenic storage
tanks.
 Heat exchangers keep the gases at low enough temperatures to be separated.
 The system's pipes often need specially designed cryogenic valves and
cryogenic fittings.
 Air separation is one of the main uses of cryogenic distillation . Facilities will
contain a cold box as well as storage tanks for the distilled products. Outside
air is pumped in and is liquefied cryogenically. This liquid air is then sent to
the cold box, where it is separated into its components.

 Most cost-efficient process for production of large

volumes of high-purity oxygen.
 Can produce both gaseous and liquid products.
 Liquid forms of cryogenic gases are easier and cheaper
to transport.
 Packing is not as effective at low temperatures.
 High energy costs to cryogenically cool gases.
 Special cryogenic equipment, such as valves and pumps,
required.

REACTION COLUMN
 Reactive distillation, or catalytic distillation, combines reaction and
distillation into a single column.
 A reactive distillation column can replace a separate reactor and distillation
column system.
 Reactive distillation columns have a reactive zone lined with catalyst, contain
beads of catalyst resin to provide as much surface area as possible for the
reactants.
 The two feed streams react in this zone. The liquid then leaves the bottom of
the reactive zone as the vapor leaves the top. Depending on the reaction, the
desired product may end up in the vapor stream or in the bottoms.
Unreacted feed can be recycled back to the reactive zone within the
distillation column.
 EXAMPLE: Formation of DMM from METHANOL & MMM – Discuss the
Reaction column problems here in BDO
 Suppression of side reactions or by-product formation.

 Higher product selectivity.
 If reaction is exothermic, heat expelled can be used for
reboiler.
 Packings/catalysts for reaction can be expensive.
 Temperature needed for highest reaction rate isn't usually
temperature needed for distillation.
 Possible high pressure drop across reactive zone.
 Complex design due to integration of reaction and
distillation.
PACKED VS PLATE COLUMNS
Conditions favouring packed columns:

 Small-diameter columns (less than 0.6 M).
 More choices in materials of construction for packings
especially in corrosive service (e.g. plastic, ceramic, metal
alloys)
 Lower pressure drop (important in vacuum distillation).
 Less liquid entrainment, low liquid hold-up, especially
suitable for thermally sensitive material.
 Foaming liquids can be handled more readily (less
agitation of liquid by the vapour)
Conditions favouring plate columns:

 Variable liquid and / or vapour loads.
 Low liquid rates & large number of stages and / or
diameter .
 High liquid residence time.
 Dirty service (plate columns are easier to clean).
 Presence of thermal or mechanical stress due to large
temperature changes which might lead to cracked
packings.
 Exotherms requiring cooling coils inside column.
 As a rule of thumb, plates are always used in columns of large diameters and
towers that have more than 20 to 30 stages.
 Packed columns offers narrower operating range than cross-current columns.
For too low liquid flow rate

 The wetting of the packing material may not be adequate.
For too high liquid flow rate

 The treatment in plate columns is often more economical.
 Moreover, If solid particles are present in the liquid the cleaning of a packing
section is much too complicated and expensive compared with the
plate discharge.
 Working under stressed conditions of temperature variations and pressure*
the packing elements are easily breakable.

However packed column are the best options when

 Less expensive than plate column for small column diameter (0.6 m).
 Corrosive chemicals handling cheap ceramic packing material, or

other chemicals resistant packing element can be easily used.
 For foaming liquid handling of foaming liquid in packed column is
more appropriate because of the relatively low degree of agitation by
the gas.

OTHER POINTS
VORTEX BREAKER:
 Vortex formation limits outflow from a tank,
 A vortex breaker is a device used in engineering to stop the formation of

a vortex when a fluid (liquid or gas) is drained from a vessel such as a tank
or vapor-liquid separator.
 The vortex is caused by the Coriolis effect.
BAFFLE PLATE:
 A plate or mechanical device designed to restrain or regulate the flow of
a fluid.
 APHA color, also referred to as the Hazen scale, and more appropriately as
the Platinum Cobalt(Pt/Co) scale, is a color standard named for the
American Public Health Association.
 Maleic acid is more soluble in water than fumaric acid is due to the
hydrogen bonding in maleic acid that is not present in fumaric
Copyright of Shell International RESTRICTED
acid.
March 2012 46
HO₂CCH=CHCO₂H – Fumaric Acid. M.P 287 Deg C.
Maleic Anhydride – C4H203
Diphenyl Pthalate -

Distillation Columns: 1 March 2012

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DISTILLATION COLUMNS

 Distillation is one of the most common liquid-liquid separation

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In contrast, continuous columns process a continuous feed stream.

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 H2S Stripper / CO2 Absorber & Stripper in NH3 plant in

 Reaction column issues in BDO plant.

 Trays fallen in Butanol Recovery column in Petronas plant.

 Start up & Shutdown sequence steps in Distillation Column.

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Binary column - feed contains only two components

Multi-product column - column has more than two product streams

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 The liquid mixture that is to be processed is known as the feed and

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Foaming, Entrainment, Weeping, Flooding , Channeling & Dumping:

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 Channeling - In packed column, mal distribution is detrimental to

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 Condenser / Re boiler choke.

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 Reflux is a technique involving the condensation of vapors and the

 Minimum Reflux Ratio (R min) is the lowest value of reflux at which

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 Refulx ratio = L/D = Condesate back to column /distillate discarded

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 Removal of organics from quench waters.

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 Distillation is general known process where multi components are

1. Distillation of petroleum product.

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 Azeotropic distillation is a process of distillation wherein you can add

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 Column internals such as trays/plates and/or packings which are used to

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 Types of packing include dumped or random packing and stacked

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 Most cost-efficient distillation column when the diameter of the

 Suitable for low pressure operations.

 Packing can break during installation, or due to thermal expansion.

 Not cost efficient for high liquid flow rates.

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 Most cost efficient distillation column for diameters greater than

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 Oil refineries often make use of vacuum distillation.

 Columns can be operated at lower temperatures.

 Pressure and energy losses due to any leaks or cracks.

 Large column diameters needed for the process to be efficient.

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 In cryogenic distillation, common distillation techniques are applied

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