PETROLEUM PROCESSING-II

Distillation

Dr. P. A Joshi
Dept. of Chemical Engg.,
FOT,D.D.University.
Nadiad-387001.
 Distillation
 Distillation separates chemicals by the difference
in how easily they vaporize.
 Two major types of classical distillation include
continuous distillation and batch distillation.
 Continuous distillation, as the name says, continuously
takes a feed and separates it into two or more
products.
 Batch distillation takes on lot (or batch) at a time of
feed and splits it into products by selectively removing
the more volatile fractions over time.
 Many industries use distillation for critical
separations in making useful products.
 These industries include petroleum refining,
beverages, chemical processing,
petrochemicals, and natural gas processing.
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 Other ways to categorize distillation
are by the
 equipment type (trays, packing),
 process configuration (distillation,
absorption, stripping, azeotropic,
extractive, complex),
 process type (refining, petrochemical,
chemical, gas treating).

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Distillation Categories
 System Composition
 System refers to the chemical components
present in the mixture being distilled.
 The two main groups are binary distillation
and multicomponent distillation.
 Binary distillation is a separation of only two
chemicals. A good example is separating
ethyl alcohol (ethanol) from water.
 Multicomponent distillation is the separation
of a mixture of chemicals. A good example is
petroleum refining. Crude oil is a very
complex mixture
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of hydrocarbons with4
Dr P A Joshi, DDU, Nadiad
literally thousands of different molecules.
Processing Mode

 Processing mode refers to the way in which feed

and product are introduced and withdrawn from
the process.
 Distillation occurs in two modes, continuous
distillation and batch distillation.
 Continuous distillation is feed is sent to the still all
the time and product is drawn out at the same
time. The idea in continuous distillation is that the
amount going into the still and the amount leaving
the still should always equal each other at any
given point in time.
 Batch distillation is when the amount going into
the still and the amount going out of the still is not
supposed to be the same all the time.
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Processing Sequence

 Fractionation systems have different

objectives.
 The major processing objectives set the
system type and the equipment
configuration needed.
 The common objectives include removing a
light component from a heavy product,
removing a heavy component from a light
product, making two products, or making
more than two products.
 We will call these major categories are
called stripping, rectification, fractionation.

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 Stripping systems remove light
material from a heavy product.
 Rectification systems remove heavy
material from a light product.
 Fractionation systems remove a light
material from a heavy product and a
heavy material from a light product at
the same time.

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 Complex fractionation makes multiple
products from either a single tower or a
complex of towers combined with recycle
streams between them.
 A good example of a multiple product
tower is a refinery crude distillation tower
making rough cuts of naphtha (gasoline),
kerosene (jet fuel), and diesel from the
same tower.

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System Type
 The behavior of the chemicals in the
system also determines the system
configuration for the objectives.
 The three major problems that limit
distillation processes are close-boilers,
distributed keys, and azeotropes.

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 Close boiler systems include chemicals that boil
at temperatures very close to each other. So
many stages of distillation or so much reflux
may be required that the chemicals cannot be
separated economically.
 A good example is separation of nitro-chloro-
benzenes. Up to 600 theoretical separation
stages with high reflux may be required to
separate different isomers.
 Distributed keys are systems where some
chemicals that we do not want in either the
heavy or the light product boil at a temperature
between the heavy and the light product.
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 Azeotropic systems are those where
the vapor and the liquid reach the
same composition at some point in the
distillation.
 No further separation can occur.
 Ethanol-water is a perfect example.
Once ethanol composition reaches
95% (at atmospheric pressure), no
further ethanol purification is possible.
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 Reaction
 Reactive distillation uses a reaction in
the distillation equipment to help the
separation.
 The reaction may or may not use a
catalyst. DMT manufacture uses
reactive distillation without a catalyst.
 One process to make methy-tert-butyl-
ether uses a catalyst inside the
distillation tower. The reaction changes
the composition, allowing the
distillation to work better
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Equipment Type
 Distillation equipment includes two
major categories, trays and packing.
 Trays force a rising vapor to bubble
through a pool of descending liquid.
 Packing creates a surface for liquid
to spread on. The thin liquid film has
a high surface area for mass-transfer
between the liquid and vapor.

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 Main Components of Distillation
Columns

 A vertical shell/Column or
tower to house internals
 Column internals
e.g.trays/plates and/or
packings which are used to
provide mass transfer area.
 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 beDr P A Joshi, DDU, Nadiad
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recycled back to the column.
Importance of stripping and
Rectifying section
 Stripping section
 more volatile component are stripped
from the descending liquid
 Rectifying section
 concentration of the less volatile
component in the vapor is reduced

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Distillation of Petroleum
 Separation technique used for
separation of soluble liquid mixtures into
individual components.
 Petroleum being a mixture of
hydrocarbons has a boiling range of -
1600C(methane) to +10000C or
more(pitch), to say a mixture of gas,
liquid and solid which requires an
effective and economic distillation to
process into a number of cuts of small
boiling range.

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 Distillation of
Petroleum(Cont…)
 Distillation of crude mainly takes place in two stages.
 Atmospheric Distillation Unit(ADU)
 Distillation is carried out at atmospheric pressure or
slightly above 1 atm
 Vacuum Distillation Unit(VDU)
 Undistilled portion of crude is further distilled under
reduced pressure
 These two columns differ from conventional distillation by not
providing any reboiler.
 The feed is heated to maximum permissible temperature of
below 400 C only once and allowing it to flash in towers.
 Higher temperature are not permitted due to degradation of
crude by thermal cracking.
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 ADU
 The feed to the atmospheric distillation column consisting of
heated crude oil (part liquid, part gas) is fed to the bottom
sections of the column(around third tray from the bottom).
 The top vapors from the column are condensed.
 A part of the condensate is refluxed to the column and part
of it is drawn out as naphtha which is the top product.
 Liquids are drawn out from different intermediate plates and
stripped in side stripping columns and the bottom products
of the strippers consisting of heavy naphtha, light distillate,
kerosene and diesel are sent to tankages where they are
further treated or blended.
 The bottom product of the atmospheric distillation column
becomes the feed to the vacuum distillation column.

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Atmospheric Distillation
Unit(ADU)

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A typical ADU

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 VDU
 In refineries, the VDU follows the ADU.
 The bottom of the ADU is called reduced
crude.
 The operation of vacuum column is
similar to that described for
atmospheric column with refluxes, side
strippers, pump around, steam injection
etc. except that the operation is under
vacuum conditions.
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 VDU
 Vacuum distillation is performed at a pressure
lower than atmospheric pressure to lower the
boiling point of liquids.
 This permits the distillation of liquids that are
temperature sensitive and avoids any degradation
of such liquids.
 The objective of a vacuum distillation is to
produce either feedstock for FCCU or HCU. This
type of vacuum distillation units are termed as
Fuel Type Vacuum Unit.
 The other kind of vacuum distillation unit is a
Lube Type Vacuum Unit and deployed for
production of fractions for Lube Oil Base stocks.
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 ADU Design
 Column Diameter – 5 to 8 m
 No. of plates -25 to 40
 Press. Drop per plate 0.015 kg/sq.cm.
 Pressure at top of the tower 1.2-1.4
 Temp. at the top of the tower 100-110C
 Steam per barrel of crude 4-5 kg
 Reflux ratio for light fraction 2-3
 Feed plate location from bottom -3
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Vacuum Distillation Unit(VDU)

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Typical VDU-lube type

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 VDU Design
 Column Diameter – Larger then ADU
 No. of plates -20 to 25
 Press. Drop for tower 60 mmHg
 Pressure at top of the tower 15-60 mmHg
 Temp. at the top of the tower 70- 80C
 Steam per barrel of crude 4-5 kg
 Reflux ratio (Reflux:Feed) 0.2-1.0
 Feed plate location from bottom -6
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Conceptual diagram of CDU
along with HENs

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 CDU along with HENs
 It consists of the following important sub-
processes:
 Crude desalter
 Furnace
 Pre-flash column
 Crude distillation column supplemented with side
columns to produce the desired products
 Pump around heat exchanger units
 Heat exchanger network that facilitates energy
recovery from hot product and reflux streams to
heat the crude oil.
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Pre-flash or topping column
 When crude contains good amount of soluble
gases, to avoid load on ADU, a preflashing or
topping column employed.
 Preflashing is also useful when crude has to
be transported to long distance.
 Light ends free crude gives no problem in
transportation
 A crude contains less than 6% light ends, such
that the vapor pressure of crude is about 0.5
kg/cm2,can be considered suitable for
transportation.
 Preflashing is conducted at 1000C under a
pressure of 3-5 atm to remove these light
ends.
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 Crude Oil Distillation

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Arrangements of ADU tower
 The reflux arrangements in ADU towers
are classified into three distinguishable
types( How heat is removed).
 Top Tray Reflux.
 Pump back reflux.
 Pump around Reflux.

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Improvement of distillation
efficiency

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Top Tray Reflux : Reflux is only at
top tray only

 Reflux is cooled and sent into the Tower.

 Heat input: Through Tower bottom.
 Removal: at the top.
 Thus requires large tower diameter.
 Improper reflux and poor quality of
fraction.
 Economic utilization of heat is not
possible.

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 Pump back Reflux

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 Pump back Reflux

 Reflux is provided at regular intervals.

 This helps every plate to act as a true
fractionator.
( because there is always good amount of
liquid).
 Tower is uniformly loaded, hence uniform and
lesser diameter tower will do.
 Heat from external reflux can be utilised as it is
at progressively higher temperatures.
 However design of such tower is costly, but
provides excellent service.
 Most common in refineries.

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Pump around Reflux
 In this arrangement reflux from a lower
plate is taken, cooled and fed into the
column at a higher section by 2 to 3 plates.
 This creates local problem of mixing uneven
composition of reflux and liquids present on
the tray.
 Designers treat all the plate in this zone as
one single plate, the result gives large
number of plates and high tower height.
 Usually, this pump around is not placed at
more than two sections in a column.
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Pump back Reflux & Pump
around Reflux

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 The number of side draws in an
atmospheric column may go up to
seven or eight.
 Side stream strippers are provided to
all crude fractionation units, to ensure
quality and close control of products
to specification limits.

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Advantages
 Better heat recovery (at higher
temperature) and better energy
efficiency
 Better fractionation between product
cuts
 Better tower design (more
proportionate diameter and smaller
height)
 Better vapor-liquid traffic along the
tower
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Pumping of waxy crude
 Important factor for pumping wax is its pour
point.
 Pour point is directly related to the wax content
of oil.
 Indian crudes are waxy and high pour points.
 Crudes from Assam are characteristically famous
for high pour points(wax content 16% and pour
point about 300C).
 Pumping such crudes, is extremely difficult.
 Such crudes can be transported only after
conditioning

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 Waxy crude
 Waxes which can be composed of saturates,
aromatic, polar and asphaltene, vary in
molecular weight and composition with their
temperature of precipitation in waxy crude.
 Waxes that precipitate out of the crude oil
solution at temperature above the pour point are
of higher molecular weight and have a high
asphaltene content.
 The waxes that precipitate at lower temperature
have lower molecular weights and contain
mostly saturates.

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Chemical additives
 These additives act by changing the structure
of wax and retard the crystal growth.
 Pour point of an oil can be lowered by
lowering the viscosity of the oil or by
dewaxing or by the addition of a suitable
pour point depressant.
 The depressant gets adsorbed on the
surface of the wax crystals and reduce their
size and also change the crystal structure,
thus increase the rate of flow at lower
temperature.

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Chemical additives
 Modification of wax structure reduces
viscosity.
 Even small quantities of
additives(300-800ppm) can markedly
depress the pour point by 10 to 160C.
 The additives being hydrocarbons in
nature.(tetradodecyl
polymethacrylate)

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Conditioning of waxy crude
 A heat-treatment process for conditioning
waxy crude oils, developed by Burmah Oil Co.
and British Petroleum Co. Ltd.
 Principle : behavior of the wax itself.
 Conditioning of crude starts with cycles of
heating and cooling.
 Firstly, heating is done up to 950C,followed by
cooling in two stages.
 First cooling goes down to 650C followed closely by
another cooling cycle to 180C at a rate of 0.50C per
minute
 This modifies the crystal structure of wax to
permit the flow.
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 THANK YOU

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