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DISTILLATION
PRESENTED BY
NABEEL SHAN
TRAINEE ENGINEER
ATTOCK REFINERY LTD
CONTENTS
 Refinery
 Separation Process
 Crude oil
 Types of crude oil
 Distillation
 Distillation column
 Atmospheric distillation
 Components of column
 Types of column
 Trays and packing's
 Vacuum distillation
 How vacuum created
 Uses of distillation products
 Steps in distillation
 Other types of distillation
 Factors affecting distillation operation
 Vapors flow rates
REFINERY
A set of equipment's used for making various
Useful Products by processing Crude Oil (Which
directly cannot be used as a beneficial product).
ARL receives crude from 80-85 different oil fields
throughout Pakistan
 Crude is received through Pipeline as well as
Bowsers to Refinery
 After receiving, blends of different fields are
prepared in respective tanks so that a proper
crude may be charged to respective plant. e.g. a
heavy density blend is charged to the heavy
crude distillation unit
REFINERY FLOW DIAGRAM
REFINING FACILITY IN PAKISTAN
 BYCO 12,0000 bbl/day
 PARCO 100,000 bbl/day
 NRL 65,000 bbl/day
 PRL 50,000 bbl/day
ARL 53,400 bbl/day
SEPARATION PROCESS
 A process that converts a mixture of substances
into two or more distinct product mixtures (which
may be referred to as fractions), which differ from
each other in composition.
SEPARATION PROCESS
Generally, separation processes may be classified
as either mechanical-physical separation processes
or mass transfer operations.
 Mechanical-physical separation processes (do not
require a mass transfer gradient for the
separation)
 Mass transfer operations (based on diffusion and
require a mass transfer gradient for the
separation)
Examples of mechanical-physical separation
processes are:
 Size reduction
 Size enlargement
 Size separation (screening, etc.)
 Filtration
 Sedimentation
 Centrifugation
Examples of mass transfer operations are:
 Distillation
 Drying
 Liquid-liquid extraction
 Leaching
HYDRO-CARBONS
Chemical compounds which consist of Hydrogen &
Carbon essentially. Other elements like Oxygen,
Nitrogen, Sulfur and some metals may also be
present.
Crude oil contains various kinds of hydro carbons.
CRUDE OIL
 A mixture of various hydrocarbons formed by
Decay and Decomposition of animals as well as
forest plants under Earth crust at High Pressure
and Temperature millions of years ago
 Crude oil contains hundreds of different
hydrocarbons, present in different proportions &
compositions
 Crude oil also contains small quantities of water
and salts depending on the source from where it
is extracted
 Impurities include salts of Ca & Mg, sand,
drilling mud, iron oxide, leaves, trashes, water
and sulfur
COMPOSITION OF CRUDE OIL
TYPES OF CRUDE (W.R.T DENSITY)
Light Crude:
Crude having Specific gravity (Rel.
density) less than 0.86 or which contains more
quantity of lighter fractions.
Heavy Crude:
Crude having Specific gravity 0.86 or
greater is called heavy crude or which contains
more heavier fractions.
TYPES OF CRUDE (W.R.T. SULFUR)
Sweet Crude:
The Crude having sulfur contents less
than 0.5wt %.
Sour Crude:
Crude having sulfur contents 0.5wt %
or more.
DISTILLATION
Distillation is a Separation technique in Unit
Operations, in which a mixture is separated into
various components due to difference in their
boiling point/ Relative Volatility by application of
heat.
The Separation Technique in Unit operations
which leads to “ Partial Vaporization & Partial
Condensation”
No Chemical Reaction in Distillation, only physical
separation.
What is Partial Condensation and Vaporization?
 Suppose we have a mixture of 50% pentane (B.P
36 C)& 50% hexane (B.P 69 C) in a close
container. Now we want to separate it out.
 So for separation, we have to first maintain temp
of vessel at 36 C. At this temp, all pentane will
vaporize and collect at receiver, while all hexanes
remain in vessel. So we have separate these
hydrocarbons.
 This is called Partial condensation & Partial
vaporization
Equipments used in small scale distillation are:
 A Still having a reboiler or pot in which the
source material is heated
 A Condenser in which the heated vapors is cooled
back to the liquid state
 A Receiver in which the concentrated or purified
liquid is collected
LAB. SCALE DIAGRAM
WHAT IS DISTILLATION COLUMN?
 A tower consisting of Trays in which liquid and
vapors contact, mass transfer occurs and mixture
is divided into its components physically
 The Hot Feed enters the Flash zone of distillation
column
 The heavy oil like furnace or bitumen which
remain in liquid form, go to the bottom of tower,
while the lighter molecules travel towards top as
these are in vapor form
ATMOSPHERIC DISTILLATION
 Distillation generally occur at a pressure greater
than atmospheric pressure. This may be done for
pressure drop considerations, to flow the vapors
from one location to the desired location
 Desalted crude oil is flashed in the atmospheric
distillation unit and the crude oil is fractionated
into various fractions
 Light gases, light and heavy naphtha, kerosene,
light and heavy gas oils, and atmospheric residue
COMPONENTS OF COLUMN
 Vertical Shell where the separation of liquid
components is carried out
 Trays/Plates column internals such as
trays/plates or packing's at which vapor liquid
contact/mass transfer takes place
 Re-boiler to provide the necessary vaporization
for the distillation process
 Condenser to cool and condense the vapor
leaving the top of the column
 Reflux drum to hold the condensed vapor from
the top of the column so that liquid (reflux) can
be recycled back to the column
DISTILLATION COLUMN
REFLUX
 Reflux refers to the portion of the condensed
overhead liquid product from a distillation or
fractionation tower that is returned to the upper
part of the tower
 Maintain the proper temperature profile in the
column
 Maintain the purity of the fractions
 Maintain the proper specifications of the
products
INTERNAL VIEW:
DISTILLATION PRODUCTS
TYPES OF COLUMN
Tray column - where trays of various designs are
used to hold up the liquid to provide better contact
between vapor and liquid, hence better separation.
Packed column - where instead of trays,
packing's are used to enhance contact between
vapor and liquid
TRAY VS PACKING
TYPES OF TRAYS
 Bubble Cap Trays
 Valve Trays
 Sieve Trays
BUBBLE CAP TRAYS
 Better vapor liquid contact
 Maximum Pressure Drop
VALVE TRAY
 Lift able caps
 Vapor flows lifts the caps
 Provide better mixing
SIEVE TRAYS
 Simply Metal Plates with holes
 Less Pressure Drop
 Ease Of Maintenance
 Low Cost
STRIPPER
 To remove the lighter ends from the side
products by adding steam
 To maintain the product purity
 Product is then pumped, exchange the heat and
then stored in the tank
SIDE STRIPPERS
STRIPPING
(REMOVING LIGHTER ENDS FROM BOTTOM / SIDE
PRODUCTS)
 The bottom product is not pure and may contain
some lighter ends
 Removal of these lighter molecules from product
is necessary
 Steam contacts with down coming product like
Furnace oil, kerosene etc. and vaporize the
lighter molecules trapped in it.
 The fractionators' bottom product is used for two
purposes:
 Some Residue, as it is sent to storage after
cooling through feed exchangers and called as
Furnace oil.
 Some residue send to Vacuum Tower after
heating in a heater for making Bitumen.
 Some lighter ends remain in bottom residue,
because efficiency of any process be never 100%.
So these are removed in vacuum section.
Some compounds have very high boiling points. To
boil such compounds, it is often better to lower the
pressure at which such compounds are boiled
instead of increasing the temperature.
So we need Vacuum Distillation
VACUUM DISTILLATION
 In vacuum distillation, pressure in the column is
less than atmospheric pressure
 Decreasing pressure of a component decreases
the boiling point and vice versa
 Atmospheric residue is the feed and vacuum gas
oil and vacuum residue may be the products
 Pressure less than the surroundings is Vacuum
HOW IS VACUUM CREATED
 Pressurized steam passes through ejectors.
 An ejector has a nozzle, through which steam
passes with its highest velocity.
 A process line is attached to this high velocity
point.
 Hence the high velocity steam carry process
vapors with it and produces vacuum behind its
system
STEAM EJECTOR
BAROMETRIC CONDENSER
VACUUM TOWER
ADVANTAGES OF VACUUM
 Energy saved as less fuel is required for a lower
Temperature
 As vapors forms easily, so overhead diesel and
other products are recovered in this way
 Crude does not crack thermally (mean if no
vacuum, then high temp required, crude may
crack thermally)
USES OF DISTILLATION PRODUCTS
Naphtha:
 Used as Motor fuel
LPG:
 Used as domestic fuel
Kerosene:
 Used as Domestic heater fuel, Jet fuel.
MTT: (Mineral Turpentine Oil)
 Paints of homes/offices is done by mixing of
MTT with Paint
JP-1/JP-8:
 Used as jet fuel
Diesel
 Used as fuel in cars and heavy Automobiles
JBO:
 Used for making Jute batches in jute industry
 Also used for making lubricating oils
Furnace oil:
 Used as fuel in Power Plant Generators
Bitumen/Asphalt:
 One of the Raw material in Road making
STEPS IN DISTILLATION UNITS
1. 1st Pre-heat train of heat exchangers
2. De-salters
3. Charge Heater
4. Distillation Tower
5. Stabilizer section
6. Vacuum Distillation (in case of heavy
crude)
7. Product cooling
OTHER TYPES OF DISTILLATION
(ON THE BASIS OF MIXTURES)
STEAM DISTILLATION
 Steam distillation is a method for distilling compounds
which are heat-sensitive.
 High rate of heat transfer without heating at a very high
temperature.
 This process involves bubbling steam through a heated
mixture of the raw material.
 Some of the target compound will vaporize (in accordance
with its partial pressure).
 The vapor mixture is cooled and condensed, usually
yielding a layer of oil and a layer of water
Extractive distillation
Reactive distillation, etc.
FACTORS AFFECTING DISTILLATION
OPERATION
1. State of feed
2. Composition of feed
3. Internal and external reflux
4. Trays or packing's
REFLUX
 It is necessary to remove heat from some parts of
tower to control the temperature as well as
pressure of tower, this is actually controlling the
quality of different products
 A line from tower goes directly to a pump, then
through pump, it passes through cold crude
(Feed) exchangers, transfer its heat to crude and
then send back to column
 When up-coming vapors in tower come in contact
with that plate, the desired components condense
and can be extracted as a product
 Hence the temp & quality is achieved.
 Without reflux, the product will be too heavy or
off grade
 Inside the tower, the down flowing reflux liquid
provides cooling and condensation of the up
flowing vapors thereby increasing the efficiency
of the distillation tower
 More reflux that is provided for a given number
of plates the better the tower's separation
 Alternatively, the more reflux that is provided for
a given desired separation, the fewer the number
of plates required
SOME IMPORTANT RELATIONS
 Tower Top Temperature α End Point of Product
 Tower Top Temperature α IBP of Product
 Tower Top Temperature α 1/External Reflux
(Cold Reflux)
 With Draw Flow Rate of Product α End Point
VAPOR FLOW CONDITIONS
 Foaming
 Entrainment
 Weeping
 Flooding
FOAMING
 Expansion of liquid due to passage of vapor
 Provides high interfacial liquid-vapor contact
 Depends upon properties of liquid mixtures
 Separation efficiency is reduced
ENTRAINMENT
 Liquid carried by vapor up to the tray caused by
high vapor flow rates
 Efficiency is reduced
 Excessive entrainment can lead to flooding
WEEPING
 Caused by low vapor flow
 Insufficient pressure exerted by the vapor to
hold up the liquid on the tray
 Liquid starts to leak through holes
 Excessive weeping will lead to dumping
 Indicated by a sharp pressure drop in the column
 Reduced separation efficiency
FLOODING
 Excessive vapor flow
 Liquid to be entrained in the vapor up the
column
 Flooding is detected by sharp increases in column
differential pressure
 Significant decrease in separation efficiency.
ANY QUESTION?

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Nabeel Shan

  • 1.
  • 3. PRESENTED BY NABEEL SHAN TRAINEE ENGINEER ATTOCK REFINERY LTD
  • 4. CONTENTS  Refinery  Separation Process  Crude oil  Types of crude oil  Distillation  Distillation column  Atmospheric distillation  Components of column  Types of column  Trays and packing's  Vacuum distillation  How vacuum created  Uses of distillation products  Steps in distillation  Other types of distillation  Factors affecting distillation operation  Vapors flow rates
  • 5. REFINERY A set of equipment's used for making various Useful Products by processing Crude Oil (Which directly cannot be used as a beneficial product). ARL receives crude from 80-85 different oil fields throughout Pakistan  Crude is received through Pipeline as well as Bowsers to Refinery  After receiving, blends of different fields are prepared in respective tanks so that a proper crude may be charged to respective plant. e.g. a heavy density blend is charged to the heavy crude distillation unit
  • 7. REFINING FACILITY IN PAKISTAN  BYCO 12,0000 bbl/day  PARCO 100,000 bbl/day  NRL 65,000 bbl/day  PRL 50,000 bbl/day ARL 53,400 bbl/day
  • 8. SEPARATION PROCESS  A process that converts a mixture of substances into two or more distinct product mixtures (which may be referred to as fractions), which differ from each other in composition.
  • 9. SEPARATION PROCESS Generally, separation processes may be classified as either mechanical-physical separation processes or mass transfer operations.  Mechanical-physical separation processes (do not require a mass transfer gradient for the separation)  Mass transfer operations (based on diffusion and require a mass transfer gradient for the separation)
  • 10. Examples of mechanical-physical separation processes are:  Size reduction  Size enlargement  Size separation (screening, etc.)  Filtration  Sedimentation  Centrifugation
  • 11. Examples of mass transfer operations are:  Distillation  Drying  Liquid-liquid extraction  Leaching
  • 12. HYDRO-CARBONS Chemical compounds which consist of Hydrogen & Carbon essentially. Other elements like Oxygen, Nitrogen, Sulfur and some metals may also be present. Crude oil contains various kinds of hydro carbons.
  • 13. CRUDE OIL  A mixture of various hydrocarbons formed by Decay and Decomposition of animals as well as forest plants under Earth crust at High Pressure and Temperature millions of years ago  Crude oil contains hundreds of different hydrocarbons, present in different proportions & compositions  Crude oil also contains small quantities of water and salts depending on the source from where it is extracted  Impurities include salts of Ca & Mg, sand, drilling mud, iron oxide, leaves, trashes, water and sulfur
  • 15. TYPES OF CRUDE (W.R.T DENSITY) Light Crude: Crude having Specific gravity (Rel. density) less than 0.86 or which contains more quantity of lighter fractions. Heavy Crude: Crude having Specific gravity 0.86 or greater is called heavy crude or which contains more heavier fractions.
  • 16. TYPES OF CRUDE (W.R.T. SULFUR) Sweet Crude: The Crude having sulfur contents less than 0.5wt %. Sour Crude: Crude having sulfur contents 0.5wt % or more.
  • 17. DISTILLATION Distillation is a Separation technique in Unit Operations, in which a mixture is separated into various components due to difference in their boiling point/ Relative Volatility by application of heat. The Separation Technique in Unit operations which leads to “ Partial Vaporization & Partial Condensation” No Chemical Reaction in Distillation, only physical separation.
  • 18. What is Partial Condensation and Vaporization?  Suppose we have a mixture of 50% pentane (B.P 36 C)& 50% hexane (B.P 69 C) in a close container. Now we want to separate it out.  So for separation, we have to first maintain temp of vessel at 36 C. At this temp, all pentane will vaporize and collect at receiver, while all hexanes remain in vessel. So we have separate these hydrocarbons.  This is called Partial condensation & Partial vaporization
  • 19. Equipments used in small scale distillation are:  A Still having a reboiler or pot in which the source material is heated  A Condenser in which the heated vapors is cooled back to the liquid state  A Receiver in which the concentrated or purified liquid is collected
  • 21. WHAT IS DISTILLATION COLUMN?  A tower consisting of Trays in which liquid and vapors contact, mass transfer occurs and mixture is divided into its components physically  The Hot Feed enters the Flash zone of distillation column  The heavy oil like furnace or bitumen which remain in liquid form, go to the bottom of tower, while the lighter molecules travel towards top as these are in vapor form
  • 22. ATMOSPHERIC DISTILLATION  Distillation generally occur at a pressure greater than atmospheric pressure. This may be done for pressure drop considerations, to flow the vapors from one location to the desired location  Desalted crude oil is flashed in the atmospheric distillation unit and the crude oil is fractionated into various fractions  Light gases, light and heavy naphtha, kerosene, light and heavy gas oils, and atmospheric residue
  • 23. COMPONENTS OF COLUMN  Vertical Shell where the separation of liquid components is carried out  Trays/Plates column internals such as trays/plates or packing's at which vapor liquid contact/mass transfer takes place  Re-boiler to provide the necessary vaporization for the distillation process  Condenser to cool and condense the vapor leaving the top of the column  Reflux drum to hold the condensed vapor from the top of the column so that liquid (reflux) can be recycled back to the column
  • 25. REFLUX  Reflux refers to the portion of the condensed overhead liquid product from a distillation or fractionation tower that is returned to the upper part of the tower  Maintain the proper temperature profile in the column  Maintain the purity of the fractions  Maintain the proper specifications of the products
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  • 29. TYPES OF COLUMN Tray column - where trays of various designs are used to hold up the liquid to provide better contact between vapor and liquid, hence better separation. Packed column - where instead of trays, packing's are used to enhance contact between vapor and liquid
  • 31. TYPES OF TRAYS  Bubble Cap Trays  Valve Trays  Sieve Trays
  • 32. BUBBLE CAP TRAYS  Better vapor liquid contact  Maximum Pressure Drop
  • 33. VALVE TRAY  Lift able caps  Vapor flows lifts the caps  Provide better mixing
  • 34. SIEVE TRAYS  Simply Metal Plates with holes  Less Pressure Drop  Ease Of Maintenance  Low Cost
  • 35. STRIPPER  To remove the lighter ends from the side products by adding steam  To maintain the product purity  Product is then pumped, exchange the heat and then stored in the tank
  • 37. STRIPPING (REMOVING LIGHTER ENDS FROM BOTTOM / SIDE PRODUCTS)  The bottom product is not pure and may contain some lighter ends  Removal of these lighter molecules from product is necessary  Steam contacts with down coming product like Furnace oil, kerosene etc. and vaporize the lighter molecules trapped in it.
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  • 39.  The fractionators' bottom product is used for two purposes:  Some Residue, as it is sent to storage after cooling through feed exchangers and called as Furnace oil.  Some residue send to Vacuum Tower after heating in a heater for making Bitumen.  Some lighter ends remain in bottom residue, because efficiency of any process be never 100%. So these are removed in vacuum section.
  • 40. Some compounds have very high boiling points. To boil such compounds, it is often better to lower the pressure at which such compounds are boiled instead of increasing the temperature. So we need Vacuum Distillation
  • 41. VACUUM DISTILLATION  In vacuum distillation, pressure in the column is less than atmospheric pressure  Decreasing pressure of a component decreases the boiling point and vice versa  Atmospheric residue is the feed and vacuum gas oil and vacuum residue may be the products  Pressure less than the surroundings is Vacuum
  • 42. HOW IS VACUUM CREATED  Pressurized steam passes through ejectors.  An ejector has a nozzle, through which steam passes with its highest velocity.  A process line is attached to this high velocity point.  Hence the high velocity steam carry process vapors with it and produces vacuum behind its system
  • 46. ADVANTAGES OF VACUUM  Energy saved as less fuel is required for a lower Temperature  As vapors forms easily, so overhead diesel and other products are recovered in this way  Crude does not crack thermally (mean if no vacuum, then high temp required, crude may crack thermally)
  • 47. USES OF DISTILLATION PRODUCTS Naphtha:  Used as Motor fuel LPG:  Used as domestic fuel Kerosene:  Used as Domestic heater fuel, Jet fuel. MTT: (Mineral Turpentine Oil)  Paints of homes/offices is done by mixing of MTT with Paint JP-1/JP-8:  Used as jet fuel
  • 48. Diesel  Used as fuel in cars and heavy Automobiles JBO:  Used for making Jute batches in jute industry  Also used for making lubricating oils Furnace oil:  Used as fuel in Power Plant Generators Bitumen/Asphalt:  One of the Raw material in Road making
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  • 50. STEPS IN DISTILLATION UNITS 1. 1st Pre-heat train of heat exchangers 2. De-salters 3. Charge Heater 4. Distillation Tower 5. Stabilizer section 6. Vacuum Distillation (in case of heavy crude) 7. Product cooling
  • 51. OTHER TYPES OF DISTILLATION (ON THE BASIS OF MIXTURES)
  • 52. STEAM DISTILLATION  Steam distillation is a method for distilling compounds which are heat-sensitive.  High rate of heat transfer without heating at a very high temperature.  This process involves bubbling steam through a heated mixture of the raw material.  Some of the target compound will vaporize (in accordance with its partial pressure).  The vapor mixture is cooled and condensed, usually yielding a layer of oil and a layer of water Extractive distillation Reactive distillation, etc.
  • 53. FACTORS AFFECTING DISTILLATION OPERATION 1. State of feed 2. Composition of feed 3. Internal and external reflux 4. Trays or packing's
  • 54. REFLUX  It is necessary to remove heat from some parts of tower to control the temperature as well as pressure of tower, this is actually controlling the quality of different products  A line from tower goes directly to a pump, then through pump, it passes through cold crude (Feed) exchangers, transfer its heat to crude and then send back to column  When up-coming vapors in tower come in contact with that plate, the desired components condense and can be extracted as a product  Hence the temp & quality is achieved.  Without reflux, the product will be too heavy or off grade
  • 55.  Inside the tower, the down flowing reflux liquid provides cooling and condensation of the up flowing vapors thereby increasing the efficiency of the distillation tower  More reflux that is provided for a given number of plates the better the tower's separation  Alternatively, the more reflux that is provided for a given desired separation, the fewer the number of plates required
  • 56. SOME IMPORTANT RELATIONS  Tower Top Temperature α End Point of Product  Tower Top Temperature α IBP of Product  Tower Top Temperature α 1/External Reflux (Cold Reflux)  With Draw Flow Rate of Product α End Point
  • 57. VAPOR FLOW CONDITIONS  Foaming  Entrainment  Weeping  Flooding
  • 58. FOAMING  Expansion of liquid due to passage of vapor  Provides high interfacial liquid-vapor contact  Depends upon properties of liquid mixtures  Separation efficiency is reduced
  • 59. ENTRAINMENT  Liquid carried by vapor up to the tray caused by high vapor flow rates  Efficiency is reduced  Excessive entrainment can lead to flooding
  • 60. WEEPING  Caused by low vapor flow  Insufficient pressure exerted by the vapor to hold up the liquid on the tray  Liquid starts to leak through holes  Excessive weeping will lead to dumping  Indicated by a sharp pressure drop in the column  Reduced separation efficiency
  • 61. FLOODING  Excessive vapor flow  Liquid to be entrained in the vapor up the column  Flooding is detected by sharp increases in column differential pressure  Significant decrease in separation efficiency.
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