SEGAS Services Training Centre

Damietta LNG Plant

DISTILLATION
DESIGN, OPERATION, TROUBLESHOOTING

COURSE OUTLINE

Course Description:
Topics include:
1. Introduction
2. Phase Behavior
3. Distillation Column, Components
4. Principles of Gas Processing Operation
5. Product Specifications
6. Distillation Column Operation
7. Distillation Column Troubleshooting

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General Objectives:
Upon completion of this course, the student shall:
1. Distillation & of Terns Definition in Gas Processing
2. Have a good understanding of vapor-liquid phase behavior and how this relates to
distillation.
Be able to describe various components on a distillation column and explain their
functions.
Understand distillation column specifications and how these are controlled.
Understand the operation of a distillation column from startup to operation to
shutdown.
Be able to understand and recognize different distillation column upsets/problems
and how to correct for them.

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An Introduction

Distillation is defined as:

a process in which a liquid or vapour mixture of two or more substances is separated into its
component fractions of desired purity, by the application and removal of heat.

Distillation is based on the fact that the

vapour of a boiling mixture will be richer in
the components that have lower boiling
points.
Therefore, when this vapour is cooled and
condensed, the condensate will contain
more volatile components. At the same
time, the original mixture will contain more
of the less volatile material.
Distillation columns are designed to achieve
this separation efficiently.

More of less Volatile

High P.P

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low P.P

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Distillation Principles
Separation of components from a liquid mixture via distillation depends on the differences in
boiling points of the individual components. Also, depending on the concentrations of the
components present, the liquid mixture will have different boiling point characteristics.
Therefore, distillation processes depends on the vapour pressure characteristics of liquid
mixtures.

Vapour Pressure and Boiling

The vapour pressure of a liquid at a particular temperature is the equilibrium pressure
exerted by molecules leaving and entering the liquid surface. Here are some important
points regarding vapour pressure:
o Energy Input Raises Vapour Pressure
o Vapour Pressure Is Related To Boiling
o A Liquid Is Said To Boil When Its Vapour Pressure Equals The Surrounding
Pressure
o The Ease With Which A Liquid Boils Depends On Its Volatility
o Liquids With High Vapour Pressures (Volatile Liquids) Will Boil At Lower
Temperatures
o The Vapour Pressure And Hence The Boiling Point Of A Liquid Mixture Depends On
The Relative Amounts Of The Components In The Mixture
o Distillation Occurs Because Of The Differences In The Volatility Of The Components
In The Liquid Mixture

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Definitions of Words and Terms

Used in the Gas Processing Industry
Absorber
A tower or column that provides contact between natural gas being processed and a liquid
solvent.
Absorption
The operation in which one or more components in the gas phase are transferred to (absorbed
into) a liquid solvent.
Absorption Oil
A hydrocarbon liquid used to absorb and recover components from the natural gas being
processed.
Acid Gas
The hydrogen sulfide and/or carbon dioxide contained in, or extracted from, gas or other
streams.
Adiabatic Expansion
The expansion of a gas, vapor, or liquid stream from a higher pressure to a lower pressure in
which there is no heat transfer between the gas, vapor, or liquid and the surroundings.
Adsorbent
A solid substance used to remove components from natural gas being processed.
Adsorption
The process by which gaseous components are adsorbed on solids because of their molecular
attraction to the solid surface.
Amine
Any of several liquid compounds containing amino nitrogen generally used in water solution
to remove, by reversible chemical reaction hydrogen sulfide and/or carbon dioxide from gas

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and liquid hydrocarbon stream

Associated Gas
Gaseous hydrocarbons occuring as a free-gas phase under original oil-reservoir conditions of
temperature and pressure.
Atmospheric Pressure
The pressure exerted on the earth by the earth's atmosphere, A pressure of 760 mm of
mercury or 101.3250 kPa is
Barrel
common English - unit measure of liquid volume which, in the petroleum industry, equals 42
U.S. liquid gallons for petroleum or natural gas liquid products measured at 60F and
Blanket Gas
A gas phase maintained in a vessel containing liquid to protect the liquid against air
contamination, to reduce the hazard of detonation, or to maintain pressure of the liquid. The
source of the gas is external to the vessel.

Blowdown
The act of emptying or depressuring a vessel. This may also refer to discarded material, such
as blow down water from a boiler or cooling tower.
Bottoms.
The liquid or residual matter which is withdrawn from the bottom of a fractionator or other
vessel during processing or while in storage.
B-P mix
A liquefied hydrocarbon product composed chiefly of butanes and propane. If it originates in
a refinery, it may also contain butylenes and propylene.

Breathing
The movement of vapor in or out of an atmospheric pressure storage tank because of a
change of level of the stored liquid, a change in the temperature of the vapor space above the

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liquid, or a change of atmospheric pressure.

Bs&w (basic sediment and water)
Waste that collects in the bottom of vessels and tanks containing petroleum products.
Bubble Point
The temperature at a specified pressure at which the first stable vapor forms above a liquid.
Butane, Commercial
A liquefied hydrocarbon consisting predominately of butane and/or butylene
Butane, Normal
Normal butane is an aliphatic compound of the paraffin series having the chemical formula
C4HlO and having all of its carbon atoms joined in a straight chain.
Calorimeter
An apparatus which is used to determine the heating value of a combustible material.

Casinghead Gas
Unprocessed natural gas produced from a reservoir containing oil. It contains heavier
hydrocarbon vapors and is usually produced under low pressure from a casing head on the
well.
Charcoal Test
A test standardized by the Gas Processors Association and the American Gas Association for
determining the natural gasoline content of a given natural gas. The gasoline is adsorbed from
the gas on activated charcoal and then recovered by distillation.
Chromatography
A technique for separating a mixture into individual components by repeated adsorption and
desorption on a confined solid bed. It is used for analysis of natural gas and NGL.
Claus Process
A process to convert hydrogen sulfide into elemental sulfur by selective oxidation.

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Compression Ratio
The ratio of the absolute discharge pressure from a compressor to the absolute intake
pressure. Also applies to one cylinder of a reciprocating compressor and one or more stages
of a rotating compressor.
Condensate
The liquid formed by the condensation of a vapor or gas; specifically, the hydrocarbon liquid
separated from natural gas because of changes in temperature and pressure when the gas from
the reservoir was delivered to the surface separators. In a steam system it may be water that is
condensed and returned to the boilers.
Copper Strip Test
A test using a small strip of pure copper to determine qualitatively the hydrogen sulfide
corrosivity of a product.
Critical Density
The density of a substance at its critical temperature and critical pressure.
Critical Pressure
The vapor pressure of a substance at its critical temperature.
Critical Temperature
For a pure component, the maximum temperature at which the component can exist as a
liquid.
Cryogenic Plant
A gas processing plant which is capable of producing natural gas liquid products, including
ethane, at very low operating temperatures, usually below minus 50C.
Cubic Meter
A unit of volume measurement commonly used in international commerce for petroleum,
petroleum products and natural gas. One cubic meter measured at 15.56C = 264.172 U.S.
gallons = 6.29 barrels = 35.315 cubic feet measured at 15.56C.
Deaerator
An item of equipment used for removing air or other non-condensible gases from a process

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stream or from steam condensate or boiler feed water.

Debutanizer
A fractionator designed to separate butane (and more volatile components if present) from a
hydrocarbon mixture.
Dehydration
The act or process of removing water from gases or liquids.
Demethanized Product
A product from which essentially all methane and lighter materials have been removed.
Demethanizer
A fractionator designed to separate methane (and more volatile components if present) from a
hydrocarbon mixture.
Depropanizer
Afractionator designed to separate propane (and more volatile components if present) from a
hydrocarbon mixture.
Desiccant
A substance used in a dehydrator to remove water and moisture. Also a material used to
remove moisture from the air.
Desulfurizationf
A process by which sulfur and sulfur compounds are removed from gases or liquid
hydrocarbon mixtures.

Dew Point
The temperature at any given pressure, or the pressure at any given temperature, at which
liquid initially condenses from a gas or vapor. It is specifically applied to the temperature at
which water vapor starts to condense from a gas mixture (water dew point), or at which
hydrocarbons start to condense (hydrocarbon dew point).
Distillation
The process of separating materials by successively heating to vaporize a portion and then

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cooling to liquefy a part of the vapor. Materials to be separated must differ in boiling point
and/or relative volatility.
Doctor Test
A qualitative method for detecting hydrogen sulfide and mercaptans in NGL. The test
distinguishes between "sour" and "sweet" products.
Dry Gas
(1) Gas whose water content has been reduced by a dehydration process. (2) Gas containing
little or no hydrocarbons recoverable as liquid product. Gas in this second definition
preferably should be called lean gas.

EP-mix (ethane-propane mix)

A product consisting of a mixture of essentially ethane and propane.
Expansion Turbine
A device which converts part of the energy content of a gas or liquid stream into mechanical
work by expanding the gas or liquid through a turbine from which work is extracted.
Extraction
The process of transferring one or more components from one liquid phase to another by
different solubility in the two liquids. It is also used to indicate removal of one or more
constituents from a stream
.
Field Separator
A vessel in the oil or gas field for separating gas, hydrocarbon liquid, and water from each
other.
Flash Point
The lowest temperature at which vapors from a hydrocarbon liquid will ignite. See ASTM D56.
Fractionation
See definition of "distillation." Generally used to describe separation of a mixture of
hydrocarbons into individual products based on difference in boiling point and/or relative
volatility.

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Gas Constant (R)

The constant multiplier in the Ideal Gas Law. Numerically, R=PV/T, if V is the volume of
one mole of an ideal gas at temperature T and pressure P.

Gas Injection
The injection of natural gas into a reservoir to maintain or increase the reservoir pressure or
reduce the rate of decline of the reservoir pressure.
Gas Lift
A method for bringing crude oil or water to the surface by injecting gas into the producing
well bore.
Gas-Oil Ratio (GOR)
The ratio of gas to liquid hydrocarbon produced from a well. This may be expressed as
standard cubic meters of gas per cubic meter of stock tank liquid.
Gas Processing T
The separation of constituents from natural gas for the purpose of making salable products
and also for treating the residue gas to meet required specifications.
Gas Processing Plant
A plant which processes natural gas for recovery of natural gas liquids and sometimes other
substances such as sulfur.
Gas-Well Gas
The gas produced or separated at surface conditions from the full well stream produced from
a gas reservoir.
Gas-Well Liquid
The liquid separated at surface conditions from the full well stream produced from a gas
reservoir.
Gathering System
The network of pipelines which carry gas from the wells to the processing plant or other
separation equipment.

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Heat Media (Heating Media)

A material, whether flowing or static, used to transport heat from a primary source such as
combustion of fuel to another material. Heating oil, steam.
Heating Value (Heat Of Combustion)
The amount of heat obtained by the complete combustion of a unit quantity of material. The
gross, or higher, heating value is the amount of heat obtained when the water produced in the
combustion is condensed. The net, or lower, heating value is the amount of heat obtained
when the water produced in the combustion is not condensed.
Heavy End
The portion of a hydrocarbon mixture having the highest boiling point. Usually hexanes or
heptanes and all heavier hydrocarbons are the heavy ends in a natural gas stream.
Hexanes Plus (Or Heptanes Plus)
The portion of a hydrocarbon fluid mixture or the last component of a hydrocarbon analysis
which contains the hexanes (or heptanes) and all hydrocarbons heavier than the hexanes (or
heptanes).
Hydrate
A solid material resulting from the combination of a hydrocarbon with water under pressure.
immiscible
Liquids that will not mix nor blend to give homogeneity are said to be immiscible.
Inerts
Elements or compounds not acted chemically by the surrounding environment. Nitrogen and
helium are examples of inert constituents of natural gases.

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Isobutene
Chemically, a hydrocarbon of the paraffin series with the formula C4HlO and having its
carbon atoms branched.
Jacket water
Water which fills, or is circulated through, a casing which partially or wholly surrounds a
vessel or machine element in order to remove, add, or distribute heat in order to control the
temperature within the vessel or element.
Joule-Thomson Effect
The change in gas temperature which occurs when the gas is expanded at constant enthalpy
from a higher pressure to a lower pressure. The effect for most gases at normal pressure,
except hydrogen and helium, is a cooling of the gas.
Lead Acetate Test
A method for detecting the presence of hydrogen sulfide by discoloration of paper which has
been moistened with lead acetate solution.
Lean Gas
(1) The residue gas remaining after recovery of natural gas liquids in a gas processing plant.
(2) Unprocessed gas containing little or no recoverable natural gas liquids.
Lean Oil
Absorption oil as purchased or recovered by the plant, or oil from which the absorbed
constituents have been removed.
Lift Gas
Gas used in a gas lift operation.
Light Ends
The low-boiling, easily evaporated components of a hydrocarbon liquid mixture.
Light Hydrocarbon
The low molecular weight hydrocarbons such as methane, ethane, propane and butanes.

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Lng (liquefied natural gas)

The light hydrocarbon portion of natural gas, predominately methane, which has been
liquefied.
loading rack
A structural and piping installation alongside a railroad track or roadway used for the purpose
of filling railroad tank cars or transport trucks.
LP-Gas (Liquefied petroleum gas)
Predominately propane or butane, either separately or in mixtures, which is maintained in a
liquid state under pressure within the confining vessel.
LNG (liquefied refinery gas)
Liquid propane or butane produced by a crude oil refinery. It may differ from LP-gas in that
propylene and butylene may be present.
LTX (low temperature extraction unit)
A unit which uses the cooling of a constant enthalpy expansion to increase liquid recovery
from streams produced from high pressure gas condensate reservoirs. Also called LTS (low
temperature separation) unit.
Mercaptan,
Any compounds of the general formula RSH. All mercaptans possess a foul odor.
Miscible Flood
A method of secondary recovery of fluids from a reservoir by injection of fluids that is
miscible with the reservoir fluids.
Natural Gas
Consisting predominately of mixtures of hydrocarbon gases. The most common component is
methane.

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Natural Gasoline
A mixture of hydrocarbons, mostly pentanes and heavier (C5+) extracted from natural gas,
Natural Gas Processing Plant
Term used for gas processing plant, natural gasoline plant, gasoline plant, etc.
Odorant
An odoriferous compound added to natural or LP-gas to impart a distinctive odor for
detection of fugitive vapors. Ethyl mercaptan is the most widely used odorant for LP-gas,
Oil-Well Gas
Gas that is produced from an oil well.
Operating Factor
The percentage of time a unit is performing the function for which it was designed.
Outage
The vapor volume in a liquid vessel left for liquid expansion. Sometimes referred to as
ullage.
Packed Column
A fractionation or absorption column filled with packing designed to give the required
contact between the rising vapors and the descending liquid.

Pentane-Plus
A hydrocarbon mixture consisting of is opentane (C5H12) and heavier components with
higher boiling points.
Pigging
A procedure for forcing a device through a pipeline for cleaning purposes, separating
products, or inspecting the line.

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Raw Gas
Unprocessed gas or the inlet gas to a gas processing plant.
Recovery
That percent or fraction of a given component in the plant feed which is recovered as plant
product.
Recycle
Return of part of a process stream to a point upstream from where it was removed to enhance
recovery or control.
Reflux
In fractionation, the portion of condensed overhead returned to the column to enhance
achievable purity of the overhead product.
Reflux Ratio
A way of giving a relative measurement to the volume of reflux. Usually referred either to the
feed or overhead product.
Relative Density
The ratio of the mass of a given volume of a substance to that of another equal volume of
another substance used as standard. Unless otherwise stated, air is used as the standard for
gases and water for liquids, with the volumes measured at 15.56C and atmospheric pressure
(101.325 kPa).
Relief System
The system for safely relieving excess pressure to avoid exceeding equipment design
pressure.
Residue
The material which remains after a separation process. (1) Residue gas is that gas remaining
after the recovery of liquid . products. (2) Residue may also be the heaviest liquid or solid
remaining after distillation or reclaiming process.

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Rich Gas
Gas feed to a gas processing plant for liquid recovery.
Rich Oil
The oil leaving the bottom of an absorber. It is the lean oil plus the absorbed constituents.
Saturated Liquid
Liquid which is at its boiling point or is in equilibrium with a vapor phase in its containing
vessel.
Saturated Vapor
Vapor at its dew point.
Shrinkage
The reduction in volume of a gas stream by removal of some of its constituents such as for
recovered products, fuel, or losses.
Solution Gas
Gas which originates from the liquid phase in an oil reservoir.
Sour
Liquids and gases are said to be "sour" if they contain hydrogen sulfide, carbon dioxide,
and/or mercaptans above a specified level. It also is used to refer to the feed stream to a
sweetening unit.
Sour Gas
Gas containing undesirable quantities of hydrogen sulfide, mercaptans, and/or carbon
dioxide. It also is used to refer to the feed stream to a sweetening unit.
Splitter
A name applied to fractionators, particularly those separating isomers
Stabilizer
A fractionation column designed to reduce the vapor pressure of a liquid stream.

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Stage Separation System

A system of separators where the liquid portion of the well effluent is separated from
formation gas and flash vapors
Still
The column where the absorbed product is recovered from the lean absorption oil. In plants
using a low molecular weight absorption oil, the still is designed as a fractionation column. In
plants using a high molecular weight absorption oil, the still may use steam or other fluids as
stripping medium. Also used to refer to regenerators in amine treating and glycol dehydration
systems.
Strapping
A term applied to the process of calibrating liquid storage capacity of storage tanks in
increments of depth.
Stream Day
A continuous 24 hour period of plant operation.
Stripper
A column wherein absorbed constituents are stripped from the absorption oil. The term is
applicable to columns using a stripping medium, such as steam or gas.
Sulfur
A yellow, non-metallic chemical element. In its elemental state, it exists in both crystalline
and amorphous forms. In many gas streams, sulfur may be found as volatile sulfur compounds, such as hydrogen sulfide, sulfur oxides, mercaptans, and carbonyl sulfide. Reduction
of the concentration of these gaseous sulfur compounds is often necessary for corrosion control and possibly for health and safety reasons.
Sulfur Dioxide (SO2)
A heavy, colorless, suffocating gas that is chemically an oxide of sulfur. Conversion of the
gaseous sulfur oxides to sulfur is necessary for corrosion control, for health and safety
reasons, and for complying with governmental standards.
Sweet
Gas containing essentially no objectionable sulfur compounds. Also, treated gas leaving a
sweetening unit.

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Sweet Gat!
Gas which has no more than the maximum sulfur and/or CO2 content defined by (1) the
specifications for the sales gas from a plant; also, the treated gas leaving a sweetening unit.
Tonne
A unit of mass measurement, commonly used in international petroleum commerce; an
expression for the metric ton, or 1000 kilograms.
Trayed Column
A vessel wherein gas and liquid, or two partially miscible liquids, are contacted, usually
concurrently on trays. Also refer to packed column.
Ullage (See Outage)
Unsaturated Compounds
Hydrocarbon compounds having one or more unsaturated valence bonds, i.e., ethylene,
propylene. These compounds are not found in natural gas streams or gas liquids because of
their relatively high chemical reactivity. Unsaturates are produced by a thermal cracking or
chemical reaction and can be found in synthetic gas (SNG) or light refinery gases (LRG).
Vapor Pressure, GPA
Vapor pressure as specified by GPA procedures.
Vapor Recovery
Equipment or process for the recovery of desired components from stock tank vapors or
vapors from some other source.
Weathering
The evaporation of liquid caused by exposing it to the conditions of atmospheric temperature
and pressure. Partial evaporation of liquid by use of heat may also be called weathering.
Weathering Test
A GPA test for LP-gas for the determination of heavy components in a sample by
evaporation under specified conditions.

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Wellhead
The assembly of fittings, valves, and controls located at the surface and connected to the flow
lines, tubing, and casing of the well so as to control the flow from the reservoir.
Wet Gas
(1) A gas containing water, or a gas which has not been dehydrated. (2) A term synonymous
with rich gas. Refer to definition of "rich gas".

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CHAPTER- 1
PHASE BEHAVIOR
Overview
This topic is aimed at all process operations staff wanting to expand their knowledge of the
behavior of gas/liquid mixtures and how this relates to the separation process of distillation.
Objectives
On completion of this topic, the trainee will:
- understand the definition and concepts for phase behavior
Contents
1.1 Vapor-Liquid Equilibrium

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Phase Behavior
Introduction:
In planning, design and operation of modem petrochemical processes, engineers,
technologists and process operators must know with- reasonable accuracy the properties of
the fluids with which they deal. If a piece of process equipment is to be designed, the
properties of the fluid which will be contained in that vessel must be determined in order to
determine the required volume of the vessel, the operating' pressure and thus the wall
thickness and even the specifications for the control devices.
1.1 Vapor-Liquid Equilibrium:
Terms/Definitions:
Property - any measurable characteristic of a substance, such as pressure, volume, or
temperature, or a characteristic that can be calculated or deduced, such as internal energy.
State - when a system possesses a unique set of properties, such as temperature, pressure,
density, and so on, at a given time. Thus the system is said to be in a particular state. A
change in the state of a system results in a change -in at least one of its properties,
Phase - a completely homogeneous and uniform state of matter.
Equilibrium - a state in which there is no tendency toward change,
Ideal Gas - is an imaginary gas which obeys exactly certain simple laws such as the laws of
Boyle, Charles, and Dalton. No real gas obeys these laws exactly over all ranges of
temperature, although "lighter" gases (hydrogen, oxygen, air, etc.) under ordinary
circumstances obey the ideal gas laws with but negligible deviations.
Ideal Gas Law - from the work of Boyle and Charles, scientists developed the relationship
now called the Ideal Gas Law. The equation used is pV = n RT. This equation can relate the
volume, pressure, temperature, and the amount of a given gas.
Vapor - a gas below its critical point which can condense (i.e change its phase).
Gas - a substance which is above its critical point and is noncondensable.
Vapor Pressure - the pressure at which vaporization and condensation are at constant
temperature and pressure under equilibrium conditions for a pure substance or mixture.

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"Normal" Boiling Point - the temperature at which boiling will take place under a pressure
of I atmosphere [101.3 kPa, 760 mm Hg].
Dew Point - the temperature at which a vapor starts to form a liquid during the process of
condensation.
Bubble Point - the temperature at which a liquid starts to from vapor during the process of
vaporization.
Saturated - when a vapor or liquid is just about to condense a drop of liquid or vaporize a
'puff of vapor respectively.
Superheated - when a substance is above its saturated vapor region.
Subcooled - when a substance is below its saturated liquid region.
Triple Point - when a substance is at a set of conditions in which the solid, liquid, and vapor
phases are all in equilibrium.

Multiphase Systems:
Water can exist in many phases, solid, liquid and vapor. These states can change from one to
another at the proper conditions with 'the addition or removal of the correct amount of
energy. For instance:
Liquid to solid : freezing
Solid to liquid
: melting
Liquid to vapor : boiling
Vapor to liquid : condensation
Sublimation
: solid to vapor
At 101.325 kPa pressure, 1 atmosphere, the boiling point of water is 100 C. This is usually
referred to as the normal boiling point of a substance and the energy required boiling that
water is referred to as the heat of vaporization. The boiling point of water changes with a
change in pressure. For example; as pressure is lowered, the boiling point of water decreases,

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CHAPTER 2
DISTILLATION COLUMN COMPONENTS

Overview
This topic is aimed at all process operations staff wanting to expand their knowledge about
the various internals and externals to a distillation column.
Objectives
On completion of this topic, the trainee will :
- know the components of a distillation column and understand their function
- understand the physical limitations of trays and packings (flooding)
- know the common process variables and understand their meaning
Contents
- Notes and diagrams on distillation column components
Components of Distillation Columns:
The modem distillation column is comprised, of a tall column with trays mounted internally,
an overhead system and a reboiler system. In some cases, packing may be used rather than
individual trays. (Figure 2)

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Condenser

Refluxing Drum
Reflux
Distillate

Tray
Distillation Sector
Feed

Packing

Stripping Section

Heat In

Heat Out

Reboiler

Bottom
Figure 2 : Distillation Column with Trays and Packing

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Basic Distillation Equipment and Operation

Main Components of Distillation Columns
Distillation columns are made up of several components, each of which is used either to
tranfer heat energy or enhance materail transfer. A typical distillation contains several major
components:
o a vertical shell where the separation of liquid components is carried out
o column internals such as trays/plates and/or packings which are used to enhance
component separations
o a reboiler to provide the necessary vaporisation for the distillation process
o a condenser to cool and condense the vapour leaving the top of the column
o a reflux drum to hold the condensed vapour from the top of the column so that liquid
(reflux) can be recycled back to the column
The vertical shell houses the column internals and together with the condenser and reboiler,
constitute a distillation column. A schematic of a typical distillation unit with a single feed
and two product streams is shown below: Figure 3

Figure 3

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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.

Liquid
Tray 2

Vapour
Tray 1

Reboiler

Bottoms
Figure 4
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.

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Figure 5

Thus, there are internal flows of vapour and liquid within the column as well as external
flows of feeds and product streams, into and out of the column.

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Column Internals
Trays and Plates
The terms "trays" and "plates" are used interchangeably. There are many types of tray
designs, but the most common ones are :
1. Bubble Cap Trays
A bubble cap tray has riser or chimney fitted over each hole, and a cap that covers the
riser. The cap is mounted so that there is a space between riser and cap to allow the
passage of vapour. Vapour rises through the chimney and is directed downward by the
cap, finally discharging through slots in the cap, and finally bubbling through the
liquid on the tray.

Figure 6

2. Valve Trays
In valve trays, perforations are covered
by liftable caps. Vapour flows lifts the
caps, thus self creating a flow area for the
passage of vapour. The lifting cap directs
the vapour to flow horizontally into the
liquid, thus providing better mixing than
is possible in sieve trays.

Figure 7

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3. Sieve Trays
Sieve trays are simply metal plates with holes in
them. Vapour passes straight upward through the
liquid on the plate. The arrangement, number
and size of the holes are design parameters.

Because of their efficiency, wide operating range, ease

of maintenance and cost factors, sieve and valve trays
have replaced the once highly thought of bubble cap
trays in many applications.
Liquid and Vapour Flows in a Tray Column

Figure 8

The next few figures show the direction of vapour and liquid flow across a tray, and across a
column.

Figure 9

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Each tray has 2 conduits, one on each side, called downcomers.

Liquid falls through the downcomers by gravity from one tray to
the one below it. The flow across each plate is shown in the above
diagram on the right.
A weir on the tray ensures that there is always some liquid (holdup)
on the tray and is designed such that the the holdup is at a suitable
height, e.g. such that the bubble caps are covered by liquid.
Being lighter, vapour flows up the column and is forced to pass
through the liquid, via the openings on each tray. The area allowed
for the passage of vapour on each tray is called the active tray area.

Figure 10 ,11

As the hotter vapour passes through the liquid on the tray above, it transfers heat to the liquid.
In doing so, some of the vapour condenses adding to the liquid on the tray. The condensate,
however, is richer in the less volatile components than is in the vapour. Additionally, because
of the heat input from the vapour, the liquid on the tray boils, generating more vapour. This
vapour, which moves up to the next tray in the column, is richer in the more volatile
components. This continuous contacting between vapour and liquid occurs on each tray in the
column and brings about the separation between low boiling point components and those
with higher boiling points.

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Tray Designs
A tray essentially acts as a mini-column, each accomplishing a fraction of the separation task.
From this we can deduce that the more trays there are, the better the degree of separation and
that overall separation efficiency will depend significantly on the design of the tray. Trays are
designed to maximise vapour-liquid contact by considering the
o Liquid distribution and
o Vapour distribution
On the tray. This is because better vapour-liquid contact means better separation at each tray,
translating to better column performance. Fewer trays will be required to achieve the same
degree of separation. Attendant benefits include less energy usage and lower construction
costs.
There is a clear trend to improve separations by supplementing the use of trays by additions
of packings.
Packings
Packings are passive devices that are designed to increase the interfacial area for vapourliquid contact. The following pictures show 3 different types of packings.

Figure 12

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These strangely shaped pieces are supposed to impart good vapour-liquid contact when a
particular type is placed together in numbers, without causing excessive pressure-drop across
a packed section. This is important because a high pressure drop would mean that more
energy is required to drive the vapour up the distillation column.
Packings versus Trays
A tray column that is facing throughput problems may be de-bottlenecked by replacing a
section of trays with packings. This is because:
o packings provide extra inter-facial area for liquid-vapour contact
o efficiency of separation is increased for the same column height
o packed columns are shorter than trayed columns
Packed columns are called continuous-contact columns while trayed columns are called
staged-contact columns because of the manner in which vapour and liquid are contacted.

Column Reboilers
There are a number of designs of reboilers. It is beyond the scope of this set of introductory
notes to delve into their design principles. However, they can be regarded as heat-exchangers
that are required to transfer enough energy to bring the liquid at the bottom of the column to
boiling boint. The following are examples of typical reboiler types.

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Figure 13
CHAPTER- 3
PRINCIPLES OF GAS PROCESSING OPERATION

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Overview
Natural gas liquids (or "NGLs), are hydrocarbons in a Liquid state. There are many reasons
for removing NGLS from the gas stream, including:
1. The hydrocarbon components may be more valuable in their liquid state, either mixed
or separated into their different individual elements.
2. Pipeline gas quality specifications may

restrict the amount of NGLS allowed.

3. Heavier NGLs can separate from the gas stream in pipelines as temperatures drop,
thus restricting flow in the pipeline.
4. The NGLs may be used for re-injection on enhanced oil recovery projects. That is,
they will be injected into a formation to help "sweep" crude Oil through the reservoir
by mixing with the oil and pushing the crude toward the well bore.
There are several different processes that can be used to separate NGLs from the natural gas
stream. The three most common are: Cryogenics, refrigeration and lean oil absorption.
1. Cryogenics
In the cryogenic process, a natural gas stream is cooled to extremely low temperatures to
liquefy the ethane and heavier hydrocarbons. When a gas stream is chilled to below -50 F

(-

45 C), heavier gas components are easily liquefied. The ethane and heavier hydrocarbons are
then separated from the methane.
EXPANDER
COMPRESSOR
COMPRESSO
METHANE

DEMETHANIZER

SEPARATO
R

NATURAL
GAS
HEAT
EXCHANGER

N. GAS

Cryogenics
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Cryogenic processing of a natural gas stream involves three basic steps: dehydration, chilling
and fractionation.
Because of the very cold temperatures in cryogenic processing, the gas stream must be almost
totally dehydrated to prevent the formation of Hydrates.
Dehydration is usually accomplished with either a liquid or solid desiccant. The method
depends on the water content of the inlet gas at your facility. Some cryogenic processes will
use only dry-desiccant dehydration. But if the water content of the inlet gas is-high, first there
would be liquid desiccant dehydration, followed by dry-desiccant dehydration.
NATURAL GAS
STREAM

WATER

DEHYDRATION
DRY GAS

CHILLING
- 150 F ( - 101 C )
GAS AND LIQUID

GAS
(METHANE)

FRACTIONATION

NATURAL GAS LIQUID

Cryogenic Processing

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Chilling of the gas is the cornerstone of the cryogenic process. The gas stream can be chilled
by heat exchange with cold gas, and by pressure reduction or pressure reduction with energy
removal. The pressure reduction method ( "J.T or Joule- Thompson), provides cold
temperatures in the range of -50 F (-45 C) to -100 F (-73 C). To obtain the lowest
temperatures, -100 F (-73 C) to -200 F (-129 C), pressure reduction with energy removal
is accomplished using an expander -compressor.

TYPICAL PERCENT
RECOVERY

METHOD

TEMPERATURE RANGE

Refrigeration

0 to 20 F
( - 18 to 29 C )

Ethane
Propane
Butanes
Heavier

25
55
93
97

Pressure Reduction
( J.T Process )

- 50 to 70 F
( - 46 to 57 C )

Ethane
Propane
Butanes
Heavier

70
80
97
99

Expander Process

- 125 to 150 F
( - 87 to 101 C )

Ethane
Propane
Butanes
Heavier

80
96
99
100

HIGH PRESSURE
GAS

HIGH PRESSURE
GAS

COMMON
SHEET
LOW PRESSURE
GAS

LOW PRESSURE
GAS

COMPRESSOR

EXPANDER

Expander Process

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Cryogenics has relatively moderate energy requirements, and is considered the most efficient
method for removing NGLS from the gas stream. .
2. Refrigeration
Refrigeration is a separation process that has been in use for many years. The principle is to
chill the natural gas stream by passing the gas through a chiller. Temperatures in this process
range from 0F (-18 C) to -20 F (-29 C). Chilling causes the heavier hydrocarbons to
liquefy, and then these NGLS can be separated from the gas.

COMPRESSOR
CONDENSER

REFIRGERANT
VAPOR

WARM NATURAL
GAS
SURGE
TANK
CHILLER
REFIRGERANT
LIQUID

COLD GAS AND

LIQUIDS

Refrigerant
The energy requirements of refrigeration are primarily for compressing the refrigerant and
driving the condenser. While the volume of heavier hydrocarbons recovered is less than with
lean oil absorption , the amount of equipment and energy used for recovery with refrigeration
is much less, making it a more economical method than lean oil absorption.

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3. Lean Oil Absorption

In lean oil absorption, lean oil is flowed through a natural gas stream, absorbing the heavier
hydrocarbons as it contacts them. The hydrocarbons are then recovered by distilling them out
of the now "rich" oil. Once the NGLs are distilled, the lean oil is recycled back through the
system.

GAS

LEAN OIL

LEAN
OIL

NATURAL
GAS
LIQUIDS

CHILLER
METHAN
E

SEPARATOR
PUMP

NATURAL
GAS

RICH OIL
STILL

ABSORBER
Lean Oil Absorption

High percentages (90-95%) of propane and heavier hydrocarbons (98-100%) can be

recovered using lean oil absorption.
Lean oil absorption is relatively expensive to operate because it requires a lot of

energy /

equipment compared to refrigeration or cryogenics.

This process was the mainstay of the industry for years. Although still in use, it is gradually
fading from the scene as cryogenics takes its place.

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Fractionation Flow

Damietta LNG Plant

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4. Fractionation ( Deethanizer & Depropanizer & Debutanizer )

Fractionation is a. downstream treatment option for NGLs after they have been separated
from the gas stream. By definition, fractionation consists of separating two components in a
mixture of two or more components. For example, a depropanizer separates propane from a
stream that contains propane and one or more heavier hydrocarbons. The propane is cooked
out of the mixture and is the overhead product from the tower. The bottom stream is
practically free of propane.

Fractionation is essentially a distillation process. As you can see by the diagram on the left,
different NGLs are cooked out in various towers. There are usually two means of control.
ling the purity of the top and bottom streams of a given tower. vary the temperature at the top
of the tower, or vary the temperature at the bottom of the tower.
Generally speaking, pressure and feed rate cannot be changed, since this would change
conditions in the rest of the plant.
Whether to fractionate is a question of economics. Is there a profitable market for the
fractionated product? Because market conditions change rapidly and often, this question must
constantly be answered to determine if fractionation will be done. There are times when the
mixed NGLs will be more valuable than their separate components.

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CHAPTER 4
PRODUCT SPECIFICATIONS

Overview
This topic is aimed at all process operations staff wanting to expand their know about the
control of distillation columns and the impact to product separation.

Objectives
On completion of this topic, the trainee will:
-understand how a distillation column is controlled (the six independent variables)

Contents
4.1 Distillate and Bottoms Specifications
4.2 Control of Product Composition

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4.1 Distillation and Bottoms Specifications:

This topic is devoted to a discussion of measurement and control techniques common is
distillation.
For purposes of discussion, it will be assumed that:
1. A column already exists.
2. Many of the control variables will be fixed by the engineering design of the
Column.
3. The column has a reboiler.
4. The feed point to the column is fixed and making only two products a
distillate and bottoms product.
If the assumptions are held for the above, there are eight (8) variables
1. Column Pressure
2. Feed Flow Rate
3. Feed Composition
4. Feed Temperature

5. Heat Added (boil-up)

6. Bottom Product Flow Rate
7. Heat Removed (reflux)
8. Distillate Product Flow Rate

only six (6) of these variables can be controlled independently. Compositions for distillate and
bottom products are called dependent variables since they are not controlled directly but
rather through the other variables mentioned above.
Pressure Control:
Most distillation columns are maintained at some kind of constant pressure. This helps in
keeping the condensation loading to the condenser as even as possible (dew point). The
specific pressure is determined from economic considerations- For example, if operating
pressure increases, the column temperature increases thus increasing the condenser cooling
requirements and decreasing the reboiler heating requirements.
Feed Control:
The first variable fixed would be the column pressure (as discussed above). If the feed
conditions were fixed, this would necessitate that three (3) more independent variables would
be determined - feed rate. feed composition. and feed temperature.
The feed flow rate can be maintained at a constant rate by using flow control. The feed
composition has a great influence upon the operation of a distillation unit. 'Unfortunately, the
feed composition is seldom subject to adjustment. For this reason, it is necessary to make
changes elsewhere to the operation of the column in order to compensate for variations in
feed composition.

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The thermal condition of the feed determines how much additional heat must be added to the
column by the reboiler. For efficient separation, it usually is desirable to ha\'e the feed at its
bubble point when it enter the column. If the feed composition varies, its bubble point also
varies. It is common practice to set the temperature control at a point which is equivalent to
the bubble point of the heaviest feed,
Reboiler Control:
Since fixing the feed conditions and column pressure determines four of the variables listed
earlier, only two other. Variables remain to be controlled in order to fix the operation of the
distillation column. Frequently, the boil-up rate is chosen as one of
the two remaining independent variables. The boil-up rate is controlled by setting the flow of
heat to the reboiler. In kettle reboilers, the heating medium (e.g. steam) is added as required
to try and achieve the bottom product specification
Reflux Control:
For total control of the distillation operation, reflux rate represents the sixth and last
independent variable to be controlled. The reflux furnishes the continuous supply of liquid to
the top and down through the column just as the boil-up from the reboiler provides a
continuous supply of vapor up through the column.
The rate of reflux is regulated by a flow controller on the reflux line.
The rate of distillate product withdrawal is controlled by the liquid level in the accumulator.
Conclusion:
By controlling the six independent variables and assuming constant feed conditions the
separation efficiency of a distillation column can be controlled. The consistent and optimum
specification for distillate and bottoms products can hence be achieved.
4.2 Control of Product Purity & Full Filling ( demands ) :
A distillation unit operates between two extremes. In one case, insufficient separation is
reflected in unacceptable product purity. In the other case, separation can be far in excess of
what is demanded so that utilities and unit capacity are wasted.
The goal of distillation then is to achieve specified product purity without causing waste. To
obtain this goal, some measure of product composition is needed.
Since distillation separates materials according to their difference in vapor pressure. and since
vapor pressure is a temperature controlled function, temperature measurement can be used to
indicate composition.

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The important consideration is to measure temperature on a tray which most reflects changes
in composition. When composition of the bottom product is the important consideration, it is
desirable to maintain a constant temperature in the lower section of the column. When
composition of the distillate product is the important consideration. It is desirable to maintain
a constant temperature in the upper section of the column
Measuring temperature in a column usually requires that the sensing device be in the liquid
on the tray. Distillation temperature is an indication of composition only when column
pressure remains constant.
In most cases, the controlling of pressures and temperatures can approximate the control of
product ( the compositions should be close to specification with a given set point of pressure
and temperature(s) in the column. Laboratory analysis can be done to confirm and/or adjust
the pressure and temperature set points.
Analytical or specific composition control is another way to sidestep the problems of
temperature control. Several types of analytical instruments can be used for distillation
column control. The most common ones used are infrared and gas .chromatographs If the
distillate and/or bottoms streams could be sampled continuously and fed lf through an
analyzer, the stream compositions could be used for column control.

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Safety Equipment, Relief Devices:

Distillation columns requires safety systems in order to function the plant environment
without creating risk to plant personal and other process equipment. These safety systems
may range in complexity from simple alarms to interlock systems.
Examples of areas That should have alarms are:
Reflux Drum

: high and low level alarms, high pressure alarm

Column Bottom : high and low level alarms

Feed Flow

: high and low flow alarms

Reflux Flow

: high and low flow alarms

Reboile

: high temperature alarm. high and low flow alarms (steam ) low flow
alarms (process).

A major concern in the operation of distillation systems is overpressure of the

Equipment and possible catastrophic failure, A partial list of the causes of
Overpressure is found below:
a) Utility failure
- Loss of coolant
- Loss of electric power
- Loss of (hot oil)
- Loss of instrument air
b) Controller failure (human error in opening valve)
- Failure of reboiler controller
- Failure of pressure controller
- Failure of feed controller
- Failure of pump around controller
c) Extraneous sources
- Valve opening to external pressure source
- Upstream upset (change in feed composition)
- Exchanger failure (tube rupture)
- Exterior fire

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d) Internal sources
- Noncondensables
- Chemical reaction
- Cosed column outlets
e) Transient sources
- Pockets of water flashing to steam
- Internal explosions

Methods of relieving overpressure which should be included in The column design are:
- Properly sized relief valves on column
- Adequate vapor vent from reflux drum
- Properly specified control valves with correct failure mode
- Manual bypass around control valves
5.2 Standard Column Control:
Distillation column control schemes may be broken into two major types, material balance
systems and heat balance systems. Of the two, the material balance system or some variation
of it, is the most common,
Material Balance System:
In a material balance control system, product composition is controlled by controlling the
flow of material into and out of the column, the column pressure is controlled by the amount
of cooling in the overhead condenser while the distillate and bottoms product are both
controlled by level control. It is common practice to have both distillate and bottoms on level
control, thus making accumulation in the column unlikely. The temperature of the bottoms is
controlled by the hot oil 0flow on temperature control while the reflux is on flow control.
This is referred to as indirect control as the tower top temperature is controlled by a flow
controller.
A variation of this is to use temperature control to manipulate the reflux. This is known as
direct control.

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Energy Balance System:

In energy balance control system, the energy balance controls the product composition while
the free variable is one of the product flows. The shortcoming of this scheme is that
variations in the material balance interact with the control system. These controls are more
sensitive to the changes in the material balance than the changes in the energy balance. For
these reasons, energy balance controls are only used if a satisfactory material balance system
cannot be implemented or in conjunction with an advanced computer control system.

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CHAPTER 6
DISTILLATION COLUMN OPERATION
Overview
This topic is aimed at all process operations staff wanting to expand their knowledge about
the operation of a distillation column.
Objectives
On completion of this topic, the Trainee will :
- Know the generic procedure of distillation column startup and shutdown
- Be knowledge in distillation column major operating variable adjustments
- Have some knowledge applicable to column energy conservation
Contents
5.1 Startup / Shutdown
5.2 Major Operating Variable Adjustments
5.3 Energy Conservation and Column Optimization

6.1 Startup / Shutdown:

Once a column is bolted up after initial construction or a shutdown, a number of operations
must occur to prepare the column for startup. These' steps, referred to as column
commissioning, are used to clear the system of undesirable materials, test the column and to
take preventative measures against performance deterioration.
Line Blowing:
Normally done with a utility service such as air and/or water. This facilitates the removal and
cleaning of any pipe scale, rust, and loose slag from weld joints. Most blowing is done to
atmosphere and not into the distillation column itself.
Pressuring and Depressuring:
This is done with the same utility mentioned above. The column, connecting equipment,
piping, along with all instrumentation is checked for leakage. The column system must be
leak proof and can be checked by monitoring the column pressure [no drop in transmitter
signal] and also by "snooping" or checking for leaks in the field.

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Purging:
This is done using an inert gas utility such as nitrogen. This is extremely' important as do not
use air [especially on vacuum systems] on the column it cause explosive mixtures to occur.
The column should be kept under a nitrogen "pad" prior to startup as not to cause any
problems on startup.
Blinding and Unblinding:
Most columns under construction and during vessel entry may have piping blind flanges or
spades inserted as not to have any utility and/or process materials enter the equipment [safety
concerns]. The removal of blinds and spades are required prior to the purging step but may be
left on during any line blowing activity if the location of the blinds and spades are connecting
equipment to piping. The removal may be done after blowing so as not to contaminant the
equipment with the blown out rust, scale, slag, etc.
Leak Testing:
Per above "pressuring and depressuring " step. A soapy water solution can be used as a
"snoop" test. Most times this solution is placed in a bottle [or can be purchased as "snoop"].
All flanges and equipment / instrument connections are squirted with the soapy water
solution. If any leaks occur, the solution will bubble vigorously.
Washing:
Some columns and equipment may need to be washed with water or a solvent prior to
operation as to eliminate any concerns with fouling, reactivity with dirt, rust, carbon, etc., as
well as any "deadspots" that cause problems with the process material to be put through the
column itself. A "water run" can be done to help calibrate instruments and check for pump
seal problems, leaks, etc..
Steaming :
Some columns can be purged with steam to exclude air. This can be done especially in warm
climates ( no freezing problems). Also, steam makes a good leak check since it can "find"
leaks better than any external testing.
Dryout:
Normally done with dry air or nitrogen utility. Can also be a solvent drying as well depending
on the application.
Once the column has been properly commissioned, the system is ready for startup. The
sequence of steps used for startup is listed below although deviations are often required for

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specific distillation columns and the hardware availab1e

1) Final elimination of undesirable materials.
The distillation column system should be clean, leak checked, and ready to run.
2)

Bringing column to normal operating pressure.

Depending on what the desired pressure is, this may be done by use of vacuum
pumps/ejectors [if vacuum column] or by allowing the pressure control system to
respond to column liquid boil up.

3)

Column heating and cooling.

The condenser cooling medium should be on and functional. The reboiler / heating
system should be ready to run once the liquid feed is introduced and a column bottoms
level established.

4)

Introduction of feed.
This is done once all the above are done.

5)

Starting up heating and cooling sources.

The cooling medium should already be running, The heating medium should be
started slowly and carefully due to the thermal stress created in the equipment during
the heatup.

6)

Bringing column to desired operating rates.

Depending on desired operating set points, the feed should be put on a minimum
setting until the entire column is up to temperature, pressure, reflux ratio [if the
distillate/forwards can be recycled], If the forwards can not be recycled, then a total
reflux can be done for a short time until the specifications are okay, then reflux ratio
can be set along with a feed increase and required reboiler/heating load increase [to
keep the bottoms on spec],

Column shutdown also follows a similar series of steps, typically:

1)

Reducing Column Rates.

Assuming all control systems are on line and at set point, the first step is to reduce
column feed -rates, This will gradually reduce heat and cooling loads as well as
forwards and bottoms rates while still on spec.. The column may be put on total reflux
so as to keep the reboiler running on a liquid inventory [i.e. no . bottoms being

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pumped forward either].

2)

Shutting Down Heating And Cooling Sources.

The feed can be stopped per step 3) below first if the heating and cooling sources are
ready to be shutdowl1. The heating source should be shutoff first as to help cool the
column with any remaining reflux.

3)

Stopping Feed.
The feed can be stopped sooner than the heating source shutdown if level rise in the
column becomes too high [alarm point]. This will help minimize the pump-out of
excess liquid inventory from the bottom of the column if required for any shutdown
activity.

4)

Draining Liquids.
Both the condenser [reflux inventory] and reboiler [bottoms inventory] can be
pumped out or drained to storage inventory prior to any column decommissioning
activities.

5)

Cooling or Heating Column.

If required for maintenance and/or vessel entry work, the column may need to be
further cooled or heated using the process material and/or utility as required.

6)

Bringing Column to Atmospheric Pressure.

For vacuum systems, nitrogen is used to repressure the column. For pressure systems,
the condenser system is often vented to a recovery and/or flare system in order to get
the column to atmospheric pressure.

7)

Eliminating Undesirable Materials.

In most cases, nitrogen is used to purge out any remaining vapors and liquids Prior to
vessel work.

8)

Prepare the Column for Opening to Atmosphere.

Hopefully the column has been purged correctly and all piping drained/blown to a
vapor/liquid recovery system.

Again, these steps may vary with each specific column or specific company procedure.

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Operations staff should be aware of any specific hazards or potential problems with the
specific column prior to startup/shutdown. Prior to startup/shutdown, there are several other
items that should be considered:
1) Prepare adequate procedures for operating, startup, shutdown and maintenance.
2) Ensure the startup/shutdown team consists of personnel who have all the required skills for
the procedure.
3) Adequate training for the startup team, supervisors and operators is required.
4) Proper startup/shutdown planning must be complete.
5) Secure any raw materials, equipment or spares required.
6) Develop adequate procedures for last minute modifications, safety checks and audits,
inspections and recordkeeping.
7) Develop adequate procedures for emergency response in case of accident
8) Develop individual tasks and objectives for each member of the startup team and ensure
these are well understood
9) Ensure proper checklists are available for each phase of the startup/shutdown.
6.2

Operation of Distillation Columns:

There are several fundamental process variables in a distillation column which must be
controlled in order to get proper separation of components:
Overhead Temperature:
The overhead temperature is determined by the composition of the liquid on the first tray, this
liquid must be at its' boiling point at the pressure of the column. The composition is
controlled by the reflux ratio. The higher the reflux ratio, the higher the concentration of the
lighter component on the top tray. As the lighter component boils, at a lower temperature, the
temperature at the top of the column will be lower. There are limits to this which are
dependent on the condenser temperature and the phase characteristics of the material in the
column.
Temperature Profile:
The temperature profile of a column is a plot of the temperature on each tray from the top of
the column to the bottom. The lowest temperature should be at the top of the column,

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corresponding to the lightest components while the highest temperature should be at the
bottom, corresponding to the heaviest component. The profile between the top and bottom of
the column should be a smooth curve with no flat spots. This indicates that the composition is
different on each tray and efficient separation is occurring. If there is a section of the column
in which the temperature profile is flat, the composition on those trays is very close and
minimal separation is taking place. The exception to this is often the feed area where a very
cold (subcooled) or very hot (superheated) feed can cause to temperature profile to flatten.
Column Pressure:
The operating pressure in the column is determined two factors, the composition of
the overhead vapor being condensed and the cooling ( both amount and temperature)
available in the overhead condenser. The condenser temperature must be cold enough to
condense the lightest component in the overhead vapor to liquid. The pressure at which this
occurs determines the operating pressure of the column. If the lightest component is not
condensed. The vapor in the overhead receiver will cause the system pressure to increase
until the temperature in the condenser is low enough to condense the light component. If this
results in a pressure which is too high for the design of the column, the light end can be
vented as vapor from the reflux drum.
Reflux Ratio:
The reflux ratio, along with the bottoms temperature, is the primary control variable for a
distillation column. The definition of -the reflux ratio is the ratio of liquid returned to the
column divided by the distillate flow, The higher the value, the more liquid that is returned to
the top of the column. The reflux ratio controls the tower top temperature, the degree of
separation of the components and the amount of liquid flowing from tray to tray. As the
reflux ratio is so important, the column is designed for a specific value known as the
optimum reflux ratio. This value is different for each application. Easy separations may
required a reflux ratio as low as 0.5 while difficult separations may require as high as 8 or 9.
Once a column is running, the reflux ratio is fine tuned for the specific operating conditions
of the plant.
Bottoms Temperature:
The temperature at the bottom of the column determines the composition of the bottom
product, the higher the bottoms temperature, the less light ends in the bottom product. The
rate of heating also determines the vapor return rate to the column. The higher the bottoms
temperature, the higher the vapor return rate. At some point the amount of vapor will become
too great for the column and jet flooding will result. As the bottoms temperature is increased,
the reflux ratio may required adjustment to maintain the same overhead temperature. The
bottoms temp is usually controlled by the amount of heating medium, such as steam of hot
oil, flowing through the reboiler.

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CHAPTER 7
DISTILLA TION COLUMN TROUBLESHOOTING
Overview
This topic is aimed at all process operations staff wanting to expand about troubleshooting
upsets in distillation columns.
Objectives
On completion or this topic, the trainee will :
- Know how to describe and know when a distillation column floods
- be knowledgeable in distillation column operation difficulties
- have some knowledgeable on control and instrumentation problems
Contents
7.l Flooding
7.2 Operation Difficulties

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7.1 Flooding:
Distillation column capacity is usually restricted by flooding.
Flooding is excessive accumulation of liquid inside the column. This accumulation is
generally caused by one of the following mechanisms:
Spray Entrainment Flooding - at low liquid flow rates, trays operate in the spray from,
where most of the liquid on the tray is in the form of liquid drops. As vapor velocity is raised,
a condition is reached where the bulk of these drops in entrained into the tray above. The
liquid accumulates on the tray above instead of flowing to the tray below.
Froth Entrainment flooding - At higher liquid rates, the dispersion of the tray is in the form
of a froth. When vapor flow rate is raised, froth height increases. When tray spacing is small,
the froth envelope approaches the tray above. As this surface approaches the tray above,
entrainment rapidly increases, causing liquid accumulation above. For large tray spacing [18 24 inches], the froth envelope seldom approaches the tray above. Given enough vapor
velocity, the froth would turn into spray and cause spray entrainment flooding per above.
Downcomer Backup Flooding - Aerated liquid is backed up into the downcomer because of
tray pressure drop, liquid height on the tray, and frictional losses in the downcomer apron.
Downcomer Choke Flooding - As liquid flow rate increases, so does the velocity of
aerated liquid in the downcomer. When this velocity exceeds a certain limit, friction losses in
the downcomer and downcomer entrance become excessive, and the frothy mixture cannot be
transported to the tray below. This causes liquid accumulation on the tray above.
Generally, at low tray spacing (less than 12 - 15 inches), froth entrainment flooding is
favored. At higher tray spacing, and when conditions do not favor vapor cross flow, the froth
regime will turn into a spray as vapor velocity increases, and spray entrainment flooding is
favored. Finally, when downcomers are small or downcomer backups are high, downcomer
flooding is favored.
Flooding can be determined by one or more of the following symptoms:
1.) Excessive column differential pressure [delta pressure is [ greater than 3 inches of water
per foot of packed bed],
2,) Sharp rise in column differential pressure
3.) Loss of bottoms
4.) Rapid rise of entrainment from column top tray [large rise in reflux vs normal]

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5.) Loss of separation as can be detected by temperature profile or product analysis,

7.2 Operation Difficulties:
Dislodging and Damage of Trays:
Most tray or packing damage comes from excessive liquid in the bottom of the column
In some cases, totally flooded trays will get damaged if vapor slugs are allowed to "bubble"
through the column. Reliable bottoms level indication is essential to safe.
column operation.
.
Some techniques for preventing tray damage due to excessive liquid levels:
1.) Pump out liquid vs boil it out.
2.) Construct the bottom seal pan to be strong.
3.) Construct the bottom 25 percent of trays for extra mechanical strength.
4.) Provide a liquid level differential pressure measurement for the bottom
5.) Provide facilities for easy diversion of bottom liquid to either the feed tank or
tank so that liquid level can be readily reduced.

storage

6.) Ensure smooth and stable automatic control of boil up to the tower.
Liquid Level in Reflux Accumulators:
An overflowing accumulator will usually backup liquid into the condenser, flooding some
tubes. Often, column pressure will rise and the relief valve may possibly lift
A low accumulator level can cause pump damage due to lack of liquid [cavitation].
Proper level indication with interlocks to pump operation or column operation should be
available.
Sources and Effects of Water Problems:
The main adverse effects of water in distillation column service are pressure surges, flooding,
cycling, corrosion, hydrates, and off-spec products.
Typical sources of water are:

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1.) The feed stream. Water may be found in the feed storage tank or from a leaking
heat exchanger.
2.) Undrained water in a stripping steam line. "Dry" steam is required prior to column
introduction.
3.) Chemical reaction. A condensation reaction forming water may occur between
organic chemicals
4.) A leaking heat exchanger [reboiler, condenser].
5.) A pre startup wash. leak -test, pr steam-water operation.
6 ) Condensate formed in previous operations. It could have remained trapped in pipelines
or pockets inside the equipment.
7 ) A water-containing stream that found its way to the column [a typical example is water
discharged from the desalter safety valve and ends up in a refinery crude column] .
Leaking Heat Exchangers:
Tube leaks may occur in the reboiler, condenser, pre heater, precooler. or any other heat
exchanger linked with the distillation column.
Effects of heat exchanger tube leaks into the column include off-spec products and/or
undesirable chemical reactions. In some cases, this reaction may lead to rapid corrosion or
plugging. It is important to realize that leaked material may cause vapor slugs and tray
damage if conditions permit.
Leaks can be detected by heat exchange equipment sampling and/or off-line drain/vent
checks. An leaking tube on an" exchanger will show the heating material on the other side of
the heat exchanger.

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