Fundamentals of Distillation

A Sunrise Project for a Sunshine Future
PARADEEP REFINERY PROJECT

Faculty
M Elamaran
PNM-CG
Prepared by
Production-CG Team
CONTENTS
Introduction

Basics of distillation

History of distillation

Types of distillation

Videos

Fractionating equipments
INTRODUCTION TO REFINERY
Hydrocarbon molecules in crude do NOT meet customer needs
SEPARATION PROCESSES
(Primary Processes)
CONVERSION PROCESSES
(Secondary Processes)
FINISHING PROCESSES
(Secondary Processes)

Segregate the molecules
Rearrange the molecules
Remove Contaminants
MARKETABLE PRODUCTS
UNIT OPERATIONS
1.Fluid flow processes, including fluids transportation, filtration, and solids
fluidization.

2. Heat transfer processes, including evaporation, condensation, and heat
exchange.

3. Mass transfer processes, including gas absorption, distillation, extraction,
adsorption, and drying.

4.Thermodynamic processes, including gas liquefaction, and refrigeration.

5.Mechanical processes, including solids transportation, crushing and
pulverization, and screening and sieving.
UNIT OPERATIONS
1. Combination.

2. Separation Distillation comes under this.

3. Reaction.
BASICS OF DISTILLATION
EVAPORATION
ORDINARY EVAPORATION IS A SURFACE PHENOMENON - SOME MOLECULES
HAVE ENOUGH KINETIC ENERGY TO ESCAPE FROM THE LIQUID.
THE PROCESS OF EVAPORATION IN A CLOSED CONTAINER WILL PROCEED
UNTIL THERE ARE AS MANY MOLECULES RETURNING TO THE LIQUID AS
THERE ARE ESCAPING.
AT THIS POINT THE VAPOUR IS SAID TO BE SATURATED AND THE PRESSURE
OF THAT VAPOUR (EXPRESSED IN mmHg) IS CALLED SATURATED VAPOUR
PRESSURE.
IF THE LIQUID IS OPEN TO THE AIR, THEN THE VAPOUR PRESSURE IS SEEN AS
PARTIAL PRESSURE ALONG WITH OTHER CONSTITUENTS OF THE AIR.
THE TEMPERATURE AT WHICH VAPOUR PRESSURE IS EQUAL TO THE
ATMOSPHERIC PRESSURE IS CALLED THE BOILING POINT.
SINCE THE VAPOUR PRESSURE IS LOW IN ORDINARY EVAPORATION AND THE
PRESSURE INSIDE THE LIQUID IS EQUAL TO ATMOSPHERIC PRESSURE PLUS
THE LIQUID PRESSURE, BUBBLES OF VAPOUR CAN NOT FORM INSIDE THE
BULK LIQUID.
AT BOILING POINT, VAPOUR PRESSURE IS EQUAL TO ATMOSPHERIC
PRESSURE, BUBBLES FORM AND VAPORIZATION BECOMES A VOLUME
PHENOMENA.
SINCE THE MOLECULAR KINETIC ENERGY IS GREATER AT HIGHER
TEMPERATURE, MORE MOLECULES CAN ESCAPE THE SURFACE AND THE
SATURATED VAPOUR PRESSURE IS CORRESPONDINGLY HIGHER.

VAPOUR PRESSURE OF A LIQUID AT A PARTICULAR TEMPERATURE IS THE
EQUILIBRIUM PRESSURE EXERTED BY MOLECULES LEAVING AND ENTERING
THE LIQUID SURFACE.

SOME IMPORTANT POINTS REGARDING VAPOUR PRESSURE:

ENERGY INPUT RAISES VAPOUR PRESSURE
VAPOUR PRESSURE IS RELATED TO BOILING
A LIQUID IS SAID TO BOIL WHEN ITS VAPOUR PRESSURE EQUALS THE
SURROUNDING PRESSURE
THE EASE WITH WHICH A LIQUID BOILS DEPENDS ON ITS VOLATILITY
LIQUIDS WITH HIGH VAPOUR PRESSURES (VOLATILE LIQUIDS) WILL BOIL AT
LOWER TEMPERATURES
THE VAPOUR PRESSURE AND HENCE THE BOILING POINT OF A LIQUID MIXTURE
DEPENDS ON THE RELATIVE AMOUNTS OF THE COMPONENTS IN THE MIXTURE
DISTILLATION OCCURS BECAUSE OF THE DIFFERENCES IN THE VOLATILITY OF
THE COMPONENTS IN THE LIQUID MIXTURE

THE BOILING POINT DIAGRAM SHOWS
HOW THE EQUILIBRIUM COMPOSITIONS OF
THE COMPONENTS IN A LIQUID MIXTURE
VARY WITH TEMPERATURE AT A FIXED
PRESSURE.
CONSIDER AN EXAMPLE OF A LIQUID
MIXTURE CONTAINING 2 COMPONENTS (A
AND B) - A BINARY MIXTURE.
IN THIS EXAMPLE, A IS THE MORE VOLATILE
COMPONENT AND THEREFORE HAS A
LOWER BOILING POINT THAN B.
THE DEW-POINT IS THE TEMPERATURE AT
WHICH THE SATURATED VAPOUR STARTS
TO CONDENSE.
THE BUBBLE-POINT IS THE TEMPERATURE
AT WHICH THE LIQUID STARTS TO BOIL.
FOR EXAMPLE, WHEN A SUBCOOLED LIQUID
WITH MOLE FRACTION OF A=0.4 (POINT A) IS
HEATED, ITS CONCENTRATION REMAINS
CONSTANT UNTIL IT REACHES THE BUBBLE-
POINT (POINT B), WHEN IT STARTS TO BOIL.
THE VAPOURS EVOLVED DURING THE BOILING
HAS THE EQUILIBRIUM COMPOSITION GIVEN
BY POINT C, APPROXIMATELY 0.8 MOLE
FRACTION A.
THIS IS APPROXIMATELY 50% RICHER IN A
THAN THE ORIGINAL LIQUID.
THIS DIFFERENCE BETWEEN LIQUID AND
VAPOUR COMPOSITIONS IN EQUILIBRIUM IS
THE BASIS FOR DISTILLATION OPERATIONS.
DISTILLATION IS ACHIEVED BY THE APPLICATION AND REMOVAL OF HEAT.
THE SEPARATION OF COMPONENTS FROM A MIXTURE BY DISTILLATION DEPENDS ON
THE DIFFERENCE IN BOILING POINTS OF THE INDIVIDUAL COMPONENTS, CALLED
RELATIVE VOLATILITY.
WHEN A MIXTURE OF TWO OR MORE LIQUIDS IS HEATED AND BOILED, THE VAPOR HAS
A DIFFERENT COMPOSITION THAN THE LIQUID. FOR EXAMPLE, IF 10% MIXTURE OF
ETHANOL IN WATER IS BOILED, THE VAPOR WILL CONTAIN OVER 50% ETHANOL.
DISTILLATION IS BASED ON THE FACT THAT THE VAPOUR OF A BOILING MIXTURE WILL
BE RICHER IN THE COMPONENTS THAT HAVE LOWER BOILING POINTS. THE
CONDENSATE WILL CONTAIN MORE VOLATILE COMPONENTS.
AT THE SAME TIME, THE ORIGINAL MIXTURE WILL CONTAIN MORE OF THE LESS
VOLATILE MATERIAL.
THE VAPOR CAN BE CONDENSED AND BOILED AGAIN, WHICH WILL RESULT IN AN
EVEN HIGHER CONCENTRATION OF ETHANOL. DISTILLATION OPERATES ON THIS
PRINCIPLE.
REPEATED BOILING AND CONDENSING IS A CLUMSY PROCESS, HOWEVER, THIS CAN
BE DONE AS A CONTINUOUS PROCESS IN A DISTILLATION COLUMN.
IN THE COLUMN, RISING VAPORS WILL STRIP OUT THE MORE VOLATILE
COMPONENT, WHICH WILL BE GRADUALLY CONCENTRATED AS THE VAPOR CLIMBS
UP THE COLUMN
DISTILLATION CONSUMES ENORMOUS AMOUNTS OF ENERGY . BOTH IN TERMS OF
COOLING AND HEATING REQUIREMENTS IT CAN CONTRIBUTE TO MORE THAN 50%
OF PLANT OPERATING COSTS.

HISTORY OF DISTILLATION
USE OF DISTILLATION DATES BACK IN RECORDED HISTORY TO ABOUT 50 B.C.

INDUSTRIAL EXPLOITATION OF THIS SEPARATION PROCESS STARTED IN 12TH
CENTURY WHEN IT WAS USED TO PRODUCE ALCOHOLIC BEVERAGES.

BY THE 16TH CENTURY, DISTILLATION WAS BEING USED IN THE MANUFACTURE OF
VINEGAR, PERFUMES, OILS AND OTHER PRODUCTS.

EARLY DISTILLATION WAS BASICALLY BATCH STILLS TO PRODUCE ETHANOL.

NEXT WAS A SERIES OF STILLS WITH A CONTINUOUS FEED THAT FLOWED THROUGH
THE SERIES.
THE NEXT PROGRESSION WAS TO PLACE THE STILLS IN A COLUMN AND
INTERCHANGE THE VAPOUR AND LIQUID TO IMPROVE RECOVERY.

EARLY SMALL TOWERS HAD ONE OR TWO LARGE BUBBLE CAPS PER
TRAY.

THE LIQUID AND VAPOUR TRAVELLED THROUGH THE CENTRE OF
COLUMN AND MIXED ON THE OUTER RING OF BUBBLE CAP.

LATER WHEN THE TRAY EFICIENCY BECAME MORE IMPORTANT, FLOW
ON THE TRAY BEGAN TO BE STUDIED AND SEVERAL TYPES OF TRAYS
AND CHANGED FLOW PATTERNS WERE DEVELOPED.

TRAY COLUMNS APPEARED IN THE SCENE IN THE 1820s ALONG WITH
FEED PREHEATING AND USE OF INTERNAL REFLUX.
TYPES OF DISTILLATION
Based on system composition:

Binary distillation
Multi component distillation

Based on Operation Mode:

Batch distillation
Continuous distillation
TYPES OF DISTILLATION
Based on Extra feed:

Extractive distillation: Extra feed component leaves with the
bottom product.
Azeotropic distillation: Extra feed component leaves with the top
product.

Based on Separation:

Stripping Removes lighter from heavier component
Rectification Removes heavier from lighter component
Fractionation Separates lighter and heavier.
Complex fractionation separates into 3 or more components.
VIDEOS

Faculty
M Elamaran
PNM-CG
Prepared by
Production-CG Team
COMPONENTS OF FRACTIONATION EQUIPMENT
Distillation columns are made up of several components, each of which
is used either to transfer heat energy or enhance material transfer. A
typical distillation contains several major components:

A vertical shell where the separation of liquid components is carried out.

Column internals such as trays/plates and/or packings which are used to
enhance component separations.

A reboiler to provide the necessary vaporization for the distillation
process .

A condenser to cool and condense the vapour leaving the top of the
column

A reflux drum to hold the condensed vapour from the top of the column
so that liquid (reflux) can be recycled back to the column

The 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.

The condenser, reboiler and the column internal are termed as
Stages, where ideally vapour and liquid equilibrium is established, if
given enough residence time.

A vessel filled with a mixture of two components is said to be in
equilibrium if the number of light molecules escaping from the
liquid is equal to the number returning to the liquid.
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.

REBOILER TYPES
Types of Reboiler:

1. Vertical Thermo-Syphon Reboiler.

2. Horizontal Thermo-Syphon Reboiler

3. Kettle Reboiler.

4. Furnace

CONDENSER
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.
CONDENSER TYPES
A. Partial Condenser
The partial condenser is best used when there is a
large difference in the overhead vapour composition.
For e.g. when there is a small amount of methane
and hydrogen mixed in a gasoline stream, the partial
condenser condenses the gasoline and leaves the
methane and hydrogen as a vapour to be vented
from the overhead reflux drum.
B. Total Condenser
The total condenser is best used when there is small
difference in the overhead vapour composition. The
overhead vapour can be condensed at approximately
same temperature.
CONDENSER TYPES
C. Hot vapour bypass condenser
The hot vapour bypass condenser is best utilized
when there is a potential for large changes in the
overhead vapour composition. The vapour
bypass can be used to maintain the pressure in
the tower system when the light components are
lower than design.

COLUMN INTERNALS
TRAYS PACKINGS
TRAYS
Trays

A tray essentially acts as a mini-column, each
accomplishing a fraction of the separation
task.

The more trays there are, the better is the
degree of separation .

Overall separation efficiency will depend
significantly on the design of the tray.

Trays are designed to maximize vapour-liquid
contact by considering the liquid distribution
and vapour distribution.

TRAYS
Vapour and liquid mixes to form a froth.

Mass transfer occurs within the froth.

The froth overflows across a weir.

The vapour disengages and move to the
tray above.

The bulk liquid flows down the down
comer to next tray.

The steps are repeated in the next tray.

LIQUID AND VAPOR FLOW IN TRAY COLUMN
Each tray has 2 conduits called down
comers: one on each side. Liquid falls
by gravity through the down comers
from one tray to the tray below.
A weir ensures there is always some
liquid (holdup) on the tray and is
designed such that the holdup is at a
suitable height, e.g. such that the
bubble caps are covered by liquid.
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.
LIQUID FLOW
Single pass Double Pass
TRAY TYPES
1. BAFFLE TRAYS

2. SIEVE TRAYS

3. VALVE TRAYS

4. BUBBLE CAP TRAYS

5. HIGH EFFICIENCY TRAYS
TRAY TYPES- BAFFLE TRAYS
Baffle Tray

Baffle trays are trays of low fouling
potential with low efficiency. They have
open areas approaching 50 % where a
high efficiency tray will have open area
less than 15 %.

Three major types of baffle trays are

A. Shed decks
B. Side to side trays
C. Disc and Donut trays
TRAY TYPES- SIEVE TRAYS
Flat perforated plate

Vapor issues from holes to give
multi-orifice effect

Simple in structure easy to
fabricate

Turn down ratio is around 2:1

Pressure drop is moderate

Not suitable for operation under
variable loads

TRAY TYPES- VALVE TRAYS
Valve can be round or rectangular
with or without caging structure

Vary high capacity tray

Turndown ratio5:1

pressure drop Moderate (earlier
designs somewhat higher recent
design same as sieve tray)

Around 20%higher cost then sieve
tray

TRAY TYPES- VALVE TRAYS
CAGED VALVE
FIXED VALVE FLOATING VALVE
TRAY TYPES- BUBBLE CAP TRAYS
Perforated plate with riser around
the hole

Cap in the form of inverted cups
over the riser

excellent turn down ratio

Good at extreme low liquid rates

Pressure drop is high
TRAY TYPES- BUBBLE CAP TRAYS
PACKED COLUMNS
Random and structured Packed columns generate a mass transfer area by providing
a large surface area over which the liquid can transfer heat and mass to the vapour.

Packing utilizes a continuous contacting principle to separate products. A major
advantage to packed column is the reduction in pressure across the column.

Typically the column pressure drop for a packed column is less than that of a trayed
column because of % open area.

Typical percent open area of a trayed column is 8 to 15 %, whereas a packed column
can approach 50 %. Liquid accumulation for a packed column is lower than a trayed
column.

Another advantage of packed column is reduced foaming. Packing generates thin
films instead of fine droplets for mass and heat transfer, reducing entrainment when
foaming agents are present.

The introduction of vapour and liquid to the packing is very important. Trays will
normally equalize whatever mal-distribution is developed by vapour and liquid feeds.
PACKED COLUMNS
TRAY VS PACKED COLUMNS
Sl. No Description Trays Random
Packing
Structured
Packing
1 Pressure Drop High Low Lower
2 Fouling Service Yes No No
3 Feed Point Flexibility Yes Difficult Difficult
4 Liquid Hold up Considerable Small Small
5 Cleaning Easy Difficult difficult
6 Cost Low Low/Medium High
COLUMN PROBLEMS
Foaming

Foaming refers to the expansion of liquid due to passage of
vapour or gas. Although it provides high interfacial liquid-vapour
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.

COLUMN PROBLEMS
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
detrimental because tray efficiency is reduced: lower volatile
material is carried to a plate holding liquid of higher volatility. It
could also contaminate high purity distillate. Excessive
entrainment can lead to flooding.
COLUMN PROBLEMS
Weeping/Dumping

This phenomenon is caused by low vapour flow. The pressure
exerted by the vapour is insufficient to hold up the liquid on the
tray. Therefore, liquid starts to leak through perforations.
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.
COLUMN PROBLEMS
Flooding

Flooding is brought about by excessive vapour flow, causing liquid
to be entrained in the vapour up the column. The increased
pressure from excessive vapour also backs up the liquid in the
down comer, causing an increase in liquid holdup on the plate
above. Depending on the degree of flooding, the maximum
capacity of the column may be severely reduced. Flooding is
detected by sharp increases in column differential pressure and
significant decrease in separation efficiency.
QUERIES

Fundamentals of Distillation

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PARADEEP REFINERY PROJECT

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