Overview of Distillation Process

Design/Operational
Problems/Troubleshooting &
Industrial column design through
Aspen Hysis/ PRO-II-8.61

By

DHEERENDRA DUBEY

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• Distillation is defined as:
• A process in which a liquid or vapor
mixture of two or more substances is
separated into its component
fractions of desired purity, by the
application and removal of heat.

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• Distillation is the most common
separation technique
• It consumes enormous amounts of
energy, both in terms of cooling and
heating requirements
• It can contribute to more than 50% of
plant operating costs

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• 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 vapor 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
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 condenser

TOP PRODUCT
RECTIFYING
REFLUX
SECTION

FEED SCHEMATIC VIEW OF

DISTILLATION TOWER
STRIPING
SECTION
reboiler
STEAM

BOTTOM PROD

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 The lighter (lower-boiling) components tend to
concentrate in the vapor phase, while the heavier
(higher-boiling) components tend toward the
liquid phase.
The result is a vapor phase that becomes richer
in light components as it passes up the column
and a liquid phase that becomes richer in heavy
components as it cascades downward.

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 Weather Conditions
 

Most distillation columns are open to the

atmosphere. Although many of the columns
are insulated, changing weather conditions
can still affect column operation. Thus the
reboiler must be appropriately sized to
ensure that enough vapors can be generated
during cold and windy spells and that it can
be turned down sufficiently during hot
seasons. The same applies to condensers.

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BASIC DISTILLATION EQUIPMENT AND OPERATION

A typical distillation contains several major components:

• a vertical shell where the separation of liquid components is
carried out
• column internals such as trays/plates and/or packing which are
used to enhance component separations
• a reboiler to provide the necessary vaporization for the
distillation process
• a condenser to cool and condense the vapor leaving the top of
the column
• a reflux drum to hold the condensed vapor from the top of the
column so that liquid (reflux) can be recycled back to the
column

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 BASIC 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.
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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

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The vapor 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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The overall separation achieved between the
distillate and the bottoms depends primarily
on

•the relative volatilities of the components.

•the number of contacting trays, and the ratio
of the liquid phase.
•flow rate to the vapor-phase flow rate.

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 TYPES OF DISTILLATION TOWER

• TRAY COLUMN
BUBBLE CAP TRAY COLUMN
SIEVE TRAY COLUMN
VALVE TRAY COLUMN

• PACKED COLUMN
RANDOMLY PACKED COLUMN
STRUCTURE PACKED COLUMN

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WHAT FACILITATES SEPARATION

• LARGE DIFFERENCE IN BOILING

POINTS OF THE CONSTITUENTS
• LOW PRESSURE
• HIGH REFLUX RATIO
• GOOD VAPOUR LIQUID MIXING ON THE
TRAY

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 REFLUX
Vapor reaching the top of the column is cooled
and condensed to liquid in the overhead
condenser. Part of this liquid is returned to the
column as reflux to provide liquid overflow.
The remainder of the overhead stream is
withdrawn as distillate, or overhead.

REFLUX RATIO IS THE RATIO OF

REFLUX TO THE OVERHEAD
PRODUCT.

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AS REFLUX RATIO INCREASED
• TOP PRODUCT PURITY INCREASED
• NO OF PLATE DECREASED
• REBOILER LOAD INCREASED
• STEAM IN REBOILER INCREASED

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 OPTIMUM REFLUX RATIO

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 PROBLEMS IN DISTILLATION
COLUMNS
• REQUIRED PRODUCT PURITY NOT
ACHIEVED
• COLUMN PRESSURE REMAINS HIGH
• COLUMN BOTTOM TEMP REMAINS LOW
• COLUMN BOTTOM LEVEL IS
FLUCTUATING

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 COLUMN PRESSURE REMAINS HIGH

• CHECK FOR CONDENSER PERFORMANCE AND

POSSIBLE CHOCKING
• CHECK FOR POSSIBLE AIR LOCK IN CW IN
OVERHEAD CONDENSER
• CHECK FOR EXCESSIVE VAPOUR GENERATION
• CHECK FOR EXCESSIVE FEED
• CHECK FOR OVERHEAD PRESS CONTROL
VALVE

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 COLUMN BOTTOM TEMP REMAINS
LOW
• CHECK REBOILER PERFORMANCE
INCLUDING STEAM TRAPS
• CHECK FOR POSSIBLE
NONCONDENSABLE BUILD UP IN
REBOILER
• CHECK FOR BOTTOM
CONCENTRATION
• CHECK OVHD PRESSURE
• CHECK FOR EXCESSIVE FEED

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 COLUMN BOTTOM LEVEL IS
FLUCTUATING
• CHECK BOTTOM LEVEL CONTROL
VALVE AND OVHD PRESS CONTROL
VALVE HUNTING
• CHECK FOR ANY PULSATING FLOW OF
FEED OR STEAM
• CHECK FOR EXCESSIVE VAPOUR
GENERATION AT BOTTOM
• CHECK FOR STEAM TRAP
MALFUNCTIONING

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 REQUIRED PRODUCT PURITY NOT
ACHIEVED
• CHECK COLUMN OPERATION W.R.T
FOAMING,FLOODING, ENTRAINMENT
ETC
• CHECK FOR POSSIBLE TRAY DAMAGE
• CHECK FOR EXCESSIVE FEED
• CHECK FOR FEED COMPOSITION AND
CONSTITUENTS
• CHECK ALL COLUMN PARAMETERS
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 Vapour Flow Conditions

Adverse vapour flow conditions can cause

1.foaming
2.entrainment
3.weeping/dumping
4.flooding

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Foaming
Foaming refers to the expansion of liquid due to
passage of vapors or gas. Although it provides high
interfacial liquid-vapors contact, excessive foaming
often leads to liquid buildup on trays. In some
cases, foaming may be so bad that the foam mixes
with liquid on the tray above. Whether foaming will
occur depends primarily on physical properties of
the liquid mixtures, but is sometimes due to tray
designs and condition. Whatever the cause,
separation efficiency is always reduced
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Entrainment
Entrainment refers to the liquid carried by vapour
up to the tray above and is again caused by high
vapour flow rates. It is deterimental because tray
efficiency is reduced: lower volatile material is
carried to a plate holding liquid of higher volatility.
It could also contaminate high purity distillate.
Excessive entrainment can lead to flooding .

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Weeping/Dumping
This phenomena is caused by low vapor flow. The
pressure exerted by the vapor is insufficient to hold
up the liquid on the tray. Therefore, liquid starts to
leak through perforations. Excessive weeping will
lead to dumping. That is the liquid on all trays will
crash (dump) through to the base of the column (via
a domino effect) and the column will have to be re-
started. Weeping is indicated by a sharp pressure
drop in the column and reduced separation
efficiency.
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 FACTORS AFFECTING DISTILLATION
COLUMN OPERATION
The performance of a distillation is determined by
many factors, for example:
   •feed conditions
•state of feed
•composition of feed
•trace elements that can severely affect the VLE
of liquid mixtures
   •internal liquid and fluid flow conditions
   •state of trays (packings)
   •weather conditions
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 State of Trays and Packings
The actual number of trays required for a
particular separation duty is determined by the
efficiency of the plate, and the packings if
packings are used. Thus, any factors that cause a
decrease in tray efficiency will also change the
performance of the column. Tray efficiencies are
affected by fouling, wear and tear and corrosion,
and the rates at which these occur depends on the
properties of the liquids being processed. Thus
appropriate materials should be specified for tray
construction.
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 Weather Conditions
 

Most distillation columns are open to the

atmosphere. Although many of the columns
are insulated, changing weather conditions
can still affect column operation. Thus the
reboiler must be appropriately sized to
ensure that enough vapors can be generated
during cold and windy spells and that it can
be turned down sufficiently during hot
seasons. The same applies to condensers.

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 Issues in distillation malfunctions.

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 Tray spacing parameters
Tray spacing (inch) Column dia (feet)
18 2.5-4

24 4-10
30 >10

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 PROCESS CONTROL DESIGN
CRITERIA
DESIGNS FOR SPECIFIC
SERVICES

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Distillation Column Control Fundamentals

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TYPICAL ARRANGEMENT FOR DISTILLATION
PRESSURE CONTROL FOR SUB- AMBIENT
SYSTEM

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 TYPICAL ARRANGEMENT FOR
DISTILLATION PRESSURE CONTROL
FOR ABOVE AMBIENT SYSTEM

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 REFLUX CONTROL
• USE LEVEL CONTROL ON DISTILLATE
RECEIVER TO CONTROL DISTILLATE
RATE
• USE FLOW-FLOW RATIO CONTROL TO
CONTROL REFLUX RATE
• NOTE THAT THIS REFLUX RATIO
SETPOINT CAN BE ADJUSTED USING
AN ANALYZER SENSOR
• USE TEMPERATURE CONTROL FOR
CONDENSER WATER FLOW

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 BOILUP CONTROL

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BOILUP CONTROL
• THE SUMP LEVEL CONTROL SERVES
TO SET THE BOTTOMS FLOW RATE
• THE VAPORIZATION RATE CAN BE
CONTROLLED USING THE LOWER
TRAY TEMPERATURE
• OTHER OPTIONS ARE AVAILABLE

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 THANKS

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