Distillation

Distillation Dynamics: Equipment, Techniques, and

Troubleshooting

Prepared by
Bahgat Negm
Distillation
Overview of Distillation Process

Table of Contents
Distillation .............................................................................................................................1
Distillation Dynamics: Equipment, Techniques, and Troubleshooting .............................................1
Distillation ...................................................................................................................................2
Introduction ........................................................................................................................4
1. Basics of Distillation ........................................................................................................5
2. Distillation Equipment .....................................................................................................5
3. Types of Distillation .........................................................................................................7
1) Simple Distillation: .......................................................................................................7
2) Fractional distillation....................................................................................................7
3) Vacuum Distillation ......................................................................................................9
4) Azeotropic Distillation ..................................................................................................9
5) Extractive Distillation:................................................................................................. 10
4. Types of distillation columns:........................................................................................ 12
1) Tray Columns ............................................................................................................. 12
2) Packed Columns ........................................................................................................ 14
3) Hybrid Columns ......................................................................................................... 15
5. Key Differences in Operation Between Packed and Tray Distillation Columns ......... 15
Comparison of Different Types of Distillation Column Internals: Advantages,
Disadvantages, Cost, Efficiency, Capacity, and Maintenance ....................................... 16
6.Trays Efficiency and Performance................................................................................... 17
Factors Affecting Tray Efficiency .......................................................................................... 17
7.Downcomers: ................................................................................................................. 18
8.Flooding.......................................................................................................................... 19
Here are some key factors related to downcomer designs that affect flooding risk: ......... 19
1. Downcomer Area and Capacity .................................................................................. 19
2. Weir Height and Downcomer Clearance ...................................................................... 20
3. Liquid and Vapor Flow Rates ....................................................................................... 21
4. Tray Spacing and Number of Stages ............................................................................ 21
5. Reflux Ratio and Pressure Drop ................................................................................... 21
9.Other Common Distillation Problems ............................................................................ 24
1. Flooding .................................................................................................................... 24
2. Fouling ...................................................................................................................... 24
2. Weeping .................................................................................................................... 25
4. Dumping .................................................................................................................... 26
5. Foaming ..................................................................................................................... 26
6. Jet Flood /Entrainment ............................................................................................... 26
7. Conning ..................................................................................................................... 27
8. Pulsation ................................................................................................................... 28
9. Mechanical Issues...................................................................................................... 28
Interpretation of a Dew point and Bubble Point curve ........................................................... 29
Why control tower pressure ................................................................................................. 30
list of important concepts and terms ................................................................................... 31
Sources /references ............................................................................................................ 34
Introduction

When we need to separate a solid from a liquid in a mixture, we typically use a method
like filtration. Filtration involves passing the mixture through a filter, which allows the liquid to pass
through while retaining the solid particles.

If we need to separate one solid from another in a mixture, we can dissolve one of the solids in a
suitable solvent. This creates a solution that can be filtered to separate the dissolved solid from the
undissolved one. Alternatively, we can use other solid-solid separation techniques based on the
physical or chemical properties of the solids, such as their size, density, or magnetic properties.

For separating a mixture of liquids based on their boiling point, we often use distillation.
Distillation relies on the different boiling points of the liquids. By heating the mixture, the liquid with
the lower boiling point evaporates first and can be collected separately from the liquid with the
higher boiling point.

Are there other methods to separate liquid-liquid, solid-liquid, and solid-solid mixtures?!
Consider exploring additional techniques.
Distillation is a widely used separation process in the chemical industry, primarily for
purifying liquids or separating liquid mixtures based on differences in boiling points. This
presentation will cover the fundamentals of distillation, distillation equipment’s, various
distillation types, distillation column internal packing types, and common distillation
problems.

1. Basics of Distillation
Distillation is a thermal separation process that involves heating a liquid to create vapor and then
cooling the vapor to obtain a liquid.

The process relies on the differences in boiling points of components in a mixture. The component
with the lower boiling point vaporizes first, allowing for separation.

2. Distillation Equipment
The previous figure is the arrangement used in laboratory for obtain Distillate water and it is
single stage, in industrial settings, the same basic principles apply, but the process is
continuous and involves multiple stages to improve purity and separate more complex
mixtures, like crude oil in refineries.
Equipment:
1. - Distillation Column: The main component where the separation occurs. A distillation
column is a tall vertical cylinder filled with trays or packing materials. It allows for multiple
vaporization-condensation cycles, improving the separation efficiency.
2. - Reboiler: Heats the liquid at the bottom of the column, providing vapor to rise through the
column.
3. - Condenser: Cools and condenses the vapor back into liquid, allowing for collection as
distillate.
4. - Receiver: Collects the distillate after condensation.

5. Process:
1. Feed Introduction: The mixture (feed) is introduced into the column.
 2. Heating: The reboiler at the bottom heats the mixture, causing the component with the
lowest boiling point to vaporize first.

3. Vapor Rise: The vapor rises through the column, passing through multiple trays.

4. Trays: Each tray acts like a mini-distillation unit, where vapor and liquid come into
contact and exchange components.

5. Condensation: The vapor reaches the top of the column and passes through the condenser,
where it cools and turns back into liquid.

6. Collection: The distillate is collected at different stages, and the remaining liquid (bottoms)
is collected at the bottom of the column.

3. Types of Distillation
Let us go over the different types of distillation, why we use them, and how each one works in
simple terms:

1) Simple Distillation: The most basic form of distillation. Used to separate liquids with
significantly different boiling points (more than 25°C difference).

2) Fractional distillation is a process used to separate a mixture into its individual

components based on differences in their boiling points. This method is particularly useful
when the boiling points of the components are close to each other (less than 25°C apart). One
of the most common examples of fractional distillation is the refining of crude oil. Crude oil is a
complex mixture of hydrocarbons, and fractional distillation is used to separate it into useful
products like gasoline, diesel, kerosene, and jet fuel.

How Fractional Distillation Works

Uses a fractionating column, Different components condense at different heights in the column,
allowing for separation.

The mixture is heated, and vapor rises through the column, which is filled with trays or packing
material. This column provides a large surface area for repeated vaporization and condensation. As
the vapor rises through the column, it cools and condenses on the trays or packing. The condensed
liquid then re-vaporizes, and this cycle repeats multiple times. Each time the vapor condenses
and re-vaporizes, the concentration of the more volatile component increases. This process
continues until the vapor reaches the top of the column, where it is collected as a distillate, The
distillate is collected in a receiver, while the less volatile components collected at different points
along the column and the heaviest component remain at the bottom.

Temperature Gradients: The temperature in the column decreases from bottom to top. This
gradient is crucial for the separation process, as it ensures that components with different boiling
points are separated efficiently.

The range of temperatures from the top of the column to the bottom is called the "Temperature
gradient." The temperature gradient can reveal a great deal about how well the column is
performing. The temperature on each tray in a distillation column is different. So, the composition
of the fraction on each tray in a column is different. Heat is added to a tray by hot vapors rising the
column. Heat is removed from a tray by reflux flowing across it and down the column.

in a distillation column, there is a countercurrent flow of fluids. A stream of hot vapors rises in the
column and a stream of cooler liquid flows downward. The vapors bubble up through the liquid on
each tray inside the tower. As a result of this contact, light materials in the liquid tend to vaporize
and heavy materials in the vapor tend to condense. The highest temperatures occur at the bottom
of a column, where hot vapors are generated. The high temperatures vaporize most of the light
material out of the liquid, so a heavy fraction is formed at the bottom of the column.

The lowest temperature occurs at the top of a column where reflux is added to the system. The
cooler reflux condenses most of the heavy material out of the rising vapors, so a light fraction is
isolated at the top of the column
3) Vacuum Distillation
It Is distillation under reduced pressure. It used for components with extremely high boiling points
that might decompose at elevated temperatures.

How It Works:

The pressure in the system is reduced, lowering the boiling points of the components, The mixture
is heated, and the components vaporize at lower temperatures, The vapor is condensed and
collected.

4) Azeotropic Distillation
Azeotropic distillation is a special type of distillation used to separate mixtures that form
azeotropes. An azeotrope is a mixture of two or more liquids that boils at a constant temperature
and behaves like a single substance. This means that the vapor has the same composition as the
liquid, making it impossible to separate the components using simple distillation.

Why Do We Use Azeotropic Distillation?

We use azeotropic distillation to break the azeotrope and separate the components. This is done by
adding another substance called an entrainer, which changes the boiling points of the
components, allowing them to be separated.
How Does Azeotropic Distillation Work?

Adding an Entrainer: An entrainer is added to the mixture. This substance forms a new azeotrope
with one or more components of the original mixture.

Distillation Process: The new azeotrope has a different boiling point, allowing it to be separated
from the other components.

Separation: The new azeotrope is then separated, and the entrainer can be recovered and reused.

To simplify this, think of azeotropic distillation like trying to separate two friends
who always stick together (ethanol and water). You cannot separate them by just pulling
them apart (simple distillation). So, you introduce a third friend (entrainer) who convinces
one of them to leave with them, making it easier to separate the original pair. 😊

5) Extractive Distillation:
Extractive distillation is a specialized distillation process used to separate mixtures with
very similar boiling points, which makes them difficult to separate using conventional
distillation methods. Here is a brief overview:

How It Works
Addition of a Solvent: A high-boiling, non-volatile solvent is added to the mixture. This
solvent does not form an azeotrope with the components of the mixture.
Change in Relative Volatility: The solvent interacts differently with the components of the
mixture, altering their relative volatilities. This makes it easier to separate the components
through distillation.
Distillation Process: The mixture is then distilled. The component with the greatest
volatility separates out as the top product.
Separation of Solvent: The bottom product, which consists of the solvent and the other
component, can be separated easily since the solvent does not form an azeotrope with it.
 Applications
Extractive distillation is commonly used in the chemical and petrochemical industries. For
example, it is used to separate:
Benzene and cyclohexane using aniline as the solvent.
Acetone and methanol using water as the solvent.

Note:

Solvent Selection: The choice of solvent is important. It must significantly alter the relative
volatility of the components and be easily separable from the bottom product, The solvent
should be cost-effective and readily available and should not react chemically with the
components or cause corrosion in the equipment.
 4. Types of distillation columns:
Distillation columns can be classified based on their internal components to:

1) Tray Columns
Tray columns use trays to facilitate contact between the rising vapor and the descending liquid. The
main types of trays include:

is the section where the rising vapor

is enriched in the more volatile
component. This area is located
above the feed point and involves
multiple stages or trays where the
vapor and liquid phases repeatedly
contact each other, enhancing the
separation of components.

is the section below the feed

point where the descending
liquid is stripped of its more
volatile components by the
rising vapor. This process
helps to concentrate the less
volatile components in the
liquid phase.

Bubble Cap Trays: These have risers over each hole, covered with caps. The vapor passes through
the risers and bubbles through the liquid on the tray.
Sieve Trays: These are metal plates with holes drilled into them. The vapor passes through the holes
and contacts the liquid on the tray.

Valve Trays: These have holes covered by caps that can lift, allowing vapor to pass through. The
caps can move or fixed, adjusting to the vapor flow rate.
 2) Packed Columns
Packed columns use packing materials to enhance the contact between the vapor and liquid. The
main types of packing include:

Random Packing:

Includes materials like Raschig rings, Pall rings, and Berl saddles. They provide a large surface area
for vapor-liquid interaction.

Structured Packing:

Designed with specific geometries to enhance flow and mass transfer, offering lower pressure
drops
3) Hybrid Columns
Hybrid columns combine trays and packing to optimize performance. They might use trays in one
section and packing in another, depending on the specific separation requirements.

Each type of internal has its advantages and disadvantages, and the choice depends on factors like
the nature of the feed, desired separation efficiency, pressure drop, chemical compatibility and
cost considerations.

5. Key Differences in Operation Between Packed and Tray Distillation

Columns
Packed and tray distillation columns differ in their mode of operation and internal design:

Aspect Packed Columns Tray Columns

Contact Continuous vapor-liquid contact as vapor and liquid flow Discrete vapor-liquid contact stages provided
Mechanism counter currently through the packing material. by horizontal trays.

Liquid Flow Liquid flows down over the packing, spreading over the Liquid flows across trays and down through
large surface area. downcomers to the next tray below.

Vapor Flow Vapor rises up through the spaces between the packing Vapor flows upward through openings or
pieces. perforations in the trays.

Packing/Tray Uses random packings (e.g., Raschig rings, Pall rings) or Common tray types include bubble cap, valve,
Types structured packings with specific geometries. and sieve trays.

Liquid Requires effective liquid distributors at the top to ensure Not applicable.
Distribution even liquid distribution over the packing.

Feed Entry Feed mixture enters at a specific point, typically in the Feed mixture enters at a specific feed tray,
middle of the column, dividing the column into a dividing the column into a rectifying section
rectifying section above and a stripping section below. above and a stripping section below.

The choice between packed or tray columns depends on factors like feed composition, flow rates,
pressure drop, and cost.
Comparison of Different Types of Distillation Column Internals: Advantages,
Disadvantages, Cost, Efficiency, Capacity, and Maintenance
Type Advantages Disadvantages Relative Efficiency Capacity Maintenance
Cost

Bubble Cap - Excellent - High-pressure High Moderate Moderate High (complex to

Trays mixing drop to High clean and
- Operates at low - Expensive replace)
vapor and liquid - Complex
rates construction
- No weeping

Sieve Trays - Simple design - Prone to weeping Low Moderate High Moderate (easier
- Low cost at low vapor rates to clean)
- High vapor - Less efficient at
handling low liquid rates
capacity

Valve Trays - Flexible - Moderate cost Moderate High High Moderate (valves
operation - Can be prone to can be replaced)
- Low-pressure fouling
drop
- High capacity

Random - Low cost - Less efficient than Low Moderate Moderate Low (easy to
Packing - Good for small structured packing replace)
columns - Can settle
- Low pressure unevenly
drop

Structured - High efficiency - High cost High High High Moderate (can be
Packing - Low pressure - Complex difficult to clean)
drop installation
- High capacity

Additional Notes:

Bubble Cap Trays: Ideal for applications requiring precise control of vapor-liquid interaction, such as vacuum distillation.

Sieve Trays: Commonly used in large-scale distillation processes, particularly in refineries and chemical plants.

valve Trays: Suitable for applications where operational flexibility and energy savings are critical.

Random Packing: Often used in stripping, distillation, and liquid-liquid extraction.

Structured Packing: Provides more surface area for heat and mass transfer, making it suitable for high-efficiency separations.
 6. Trays Efficiency and Performance
Stage Efficiency: Each tray represents a theoretical stage of separation. The efficiency of a tray
determines how close it comes to achieving complete separation at that stage.

Distillation trays in a fractionator operate between 10 and 90 percent efficiency. It is the process
person’s job to make trays operate as close to 90-percent efficiency as possible. Calculating tray
efficiency is sometimes simple. Compare the vapor temperature leaving a tray to the liquid
temperature leaving the trays. For example, the efficiency of the tray shown in Fig. 3.3 is 100
percent. The efficiency of the tray in Fig. 3.4 is 0 percent.

Factors Affecting Tray Efficiency

Liquid and Vapor Flow Rates: High flow rates can lead to insufficient contact time between
phases, reducing efficiency.

Tray Design: The type of tray (e.g., sieve, valve, bubble cap) and its design impact efficiency.

Mixing and Contact Time: Better mixing and longer contact time between liquid and vapor phases
improve efficiency.

Operating Conditions: Temperature, pressure, and feed composition can influence efficiency.
 7. Downcomers:
A downcomer in a distillation column is a channel that directs liquid from one tray to the next lower
tray. It works by allowing the liquid to flow down due to gravity while preventing vapor from
bypassing the trays. The purpose of the downcomer is to ensure proper liquid distribution and
maintain the efficiency of the separation process. Vapor is prevented from passing through the
downcomer by maintaining a liquid seal at the bottom, which acts as a barrier.

Design considerations for downcomers include ensuring adequate liquid flow capacity,
minimizing pressure drop, and preventing vapor bypass. The downcomer must be sized to handle
the maximum liquid flow rate and maintain a liquid seal to prevent vapor from escaping. Proper
liquid distribution and residence time are crucial for efficient operation. The design should also
consider ease of maintenance and cleaning to prevent fouling and ensure long-term reliability And
managing the risk of flooding in distillation columns.
 8. Flooding
occurs when the liquid flow rate exceeds the column's capacity, leading to a buildup of liquid that
disrupts the normal vapor-liquid flow dynamics.

Here are some key factors related to downcomer designs that affect
flooding risk:

1. Downcomer Area and Capacity

The downcomer must have enough cross-sectional area to handle the maximum expected
liquid flow rate, ensuring that liquid flows smoothly from one tray to the next without
causing excessive liquid holdup, as insufficient area can lead to liquid backup and flooding.

Downcomer B is Flooding due to

lack of downcomer seal, this
permits vapor to flow up
downcomer B. The up-flowing
vapor displaces the downflowing
liquid
 2. Weir Height and Downcomer Clearance
Weir Height: The height of the weir (a barrier at the edge of the tray) affects the liquid level
on the tray. A higher weir can increase the liquid holdup, potentially leading to flooding if not
properly managed.

Downcomer Clearance: The clearance between the bottom of the downcomer and the tray
below must be sufficient to allow liquid to flow freely. Inadequate clearance can cause
liquid to accumulate, increasing the risk of flooding.

Liquid built up in downcomer B cause

tray #2 to flood and then downcomer
C will flood, and tray above will also
flood till all trays above tray#1 flood

Flooding caused by Inadequate

downcomer clearance. the bottom
edge of the downcomer is too close
to the tray below

Note:

Generally, when flooding starts on a tray, all the trays above that point will also flood, but
trays below that point will go dry.

• An early indication of flooding in a distillation column is loss of liquid level in the bottom
of the column.

• If the downcomer clearance—which means the distance between the bottom edge of the
downcomer and the tray below—is too great, the downcomer becomes unsealed. Vapor
flows up the downcomer, and the trays above flood.
 • If the downcomer clearance is too small, then liquid backs up in the downcomer, and the
trays above flood.

To guarantee a proper downcomer seal, the bottom edge of a downcomer should be

about 0.5 inch below the top edge of the outlet weir. This dimension should be carefully
checked by process personnel when a tower is opened for inspection. It is quite easy
for sloppy tray installation to distort this critical factor

3. Liquid and Vapor Flow Rates

Vapor/Liquid V/L Ratio: A high vapor/liquid ratio can increase the risk of flooding as more
liquid is condensed on the trays. Proper downcomer design helps manage this ratio to
prevent excessive liquid buildup.

While the typical V/L ratio for distillation columns ranges from 1.0 to 1.5, the ideal ratio for a
specific operation should be determined through detailed process analysis and
optimization. This ensures that the column operates efficiently and meets the desired
separation objectives.

The V/L ratio is often optimized through process simulations and economic evaluations.
This involves balancing energy consumption, separation efficiency, and operational costs to
determine the most cost-effective and efficient operating conditions.

Practical Considerations

• High V/L Ratios: Higher V/L ratios can improve separation efficiency but may lead to
increased energy consumption and potential flooding issues.

• Low V/L Ratios: Lower V/L ratios can reduce energy consumption but may compromise
separation efficiency and product purity.

4. Tray Spacing and Number of Stages

Tray Spacing: Adequate spacing between trays allows for proper vapor-liquid contact and
reduces the risk of flooding. Too close spacing can restrict vapor flow and increase liquid
holdup.

Number of Stages: More stages can increase the residence time of liquid on each tray,
potentially leading to flooding if not properly managed

5. Reflux Ratio and Pressure Drop

Reflux Ratio: The ratio of liquid returned to the column versus the liquid collected as
distillate affects the liquid load on the trays. A high reflux ratio can increase the risk of
flooding.

As a general A low reflux ratio, typically ranging from 0.5 to 1.0, is characterized by lower
energy consumption and fewer theoretical stages, but it may result in lower product purity.
A moderate reflux ratio, which falls between 1.0 and 2.0, offers a balanced approach,
 providing a good compromise between energy efficiency and product purity, and is
commonly used in many industrial applications. On the other hand, a high reflux ratio,
ranging from 2.0 to 5.0 or higher, achieves higher product purity and better separation
efficiency, but this comes at the cost of increased energy consumption and more
theoretical stages.

Important concept, always Remember that reflux comes from the reboiler

Incipient flood point: The above figure illustrates this point. Point A is called the incipient flood
point, that point in the tower’s operation at which either an increase or a decrease in the reflux rate
results in a loss of separation efficiency. You might call this the optimum reflux rate; that would be
an alternate description of the incipient flood point

How to identify the incipient flood point which is the best efficiency point?!

As per Norman P. Lieberman in his book AWORKING GUIDE TO PROCESS EQUIPMENT, we

can use the following formula:

where DP = pressure drop across a tray section, psi

NT = the number of trays

TS = tray spacing, inches

s.g. = specific gravity of clear liquid, at flowing temperatures

On the basis of hundreds of field measurements, we have observed

K = 0.18 to 0.25: Tray operation is close to its best efficiency point.

K = 0.35 to 0.40: Tray is suffering from entrainment—increase in reflux rate noticeably

reduces tray efficiency.

K = ≥0.5: Tray is in fully developed flood—opening a vent on the overhead vapor line will
blow out liquid with the vapor.

K = 0.10 to 0.12: Tray deck is suffering from low tray efficiency, due to tray deck leaking.

K = 0.00: The liquid level on the tray is zero, and quite likely the trays are lying on the bottom
of the column.

K = 1.00: Tower is completely full of liquid.

Pressure Drop: High pressure drops across the column can indicate excessive liquid
holdup and potential flooding. Proper downcomer design helps manage pressure drop to
prevent flooding:

As shown in the diagram, the pressure at tray #2 is lower than the pressure in the tray below
due to a pressure drop. This drop occurs because vapor flows through the tray deck. As
vapor passes upwards through the tray openings, its velocity increases and pressure
decreases. A common example of this is the pressure drop across an orifice plate.

The question is, how does liquid flow from tray #2 with lower pressure to the tray below
with higher pressure?

The answer is gravity. If the pressure drops increases, the liquid height in the downcomer
will rise to overcome this pressure drop, potentially leading to flooding.
 9. Other Common Distillation Problems
Here are some common problems in distillation columns, along with their descriptions,
causes, and ways to avoid them:

1. Flooding
We already discussed flooding in detail in the previous section

2. Fouling
• Description: Accumulation of unwanted materials on the column's internal surfaces.

Fouling in distillation columns can occur due to several factors. Polymerization, where
unwanted polymers like polyethylene, polystyrene, and polypropylene form due to chemical
reactions within the column, leads to reduced capacity and unit outages. Sedimentation,
crystallization, and precipitation involve the accumulation of suspended solids, metal
oxides, salts, coke fines, and catalyst fines, occurring when the system is supersaturated,
especially at the surfaces of mass transfer. Corrosion, caused by the presence of corrosive
substances like acids or chlorides in the feed or process streams, degrades column
materials. Scaling, the formation of hard deposits on surfaces, occurs due to the
precipitation of dissolved salts when the solubility limit is exceeded.

To avoid fouling, regular cleaning and maintenance, proper material selection, optimized
operating conditions, use of anti-fouling agents, and proper column design are essential.
These strategies help prevent the buildup of fouling materials and ensure efficient column
operation.
2. Weeping

Weeping in a distillation column occurs when liquid leaks through the perforations of the
trays instead of flowing across them. This happens when the vapor flow rate is too low to
hold the liquid on the tray, causing the liquid to drip down to the tray below. Weeping
reduces the efficiency of the distillation process because the liquid does not have enough
contact time with the vapor.

Common reasons for weeping include improper tray design, low vapor velocity, and high
liquid rates. To avoid weeping, ensure the column is properly designed with the correct tray
spacing and hole size, maintain appropriate vapor and liquid flow rates, and regularly
monitor and adjust the column's operating conditions.
4. Dumping
Dumping in a distillation column occurs when the liquid on the trays falls through the
perforations to the bottom of the column instead of flowing across the trays. This happens
when the vapor flow rate is too low to support the liquid on the trays, leading to a complete
loss of liquid hold-up and separation efficiency. Causes of dumping include low vapor
velocity, improper tray design, and excessive liquid flow rates. To avoid dumping, ensure the
column is properly designed with adequate tray spacing and hole size, maintain appropriate
vapor and liquid flow rates, and regularly monitor and adjust the column's operating
conditions.

5. Foaming
Description: Formation of stable foam that disrupts the liquid-vapor contact.

Cause: High liquid velocity and improper tray spacing.

Avoidance: Use anti-foaming agents, optimize tray design, and control liquid velocities.

6. Jet Flood /Entrainment

The below figure shows realistic picture of what we would see if our towers were made of
glass. In addition to the downcomers and tray decks containing froth or foam, there is a
quantity of spray, or entrained liquid, lifted above the froth level on the tray deck. The force
that generates this entrainment is the flow of vapor through the tower. The spray height of
this entrained liquid is a function of two factors:
• The foam height on the tray
• The vapor velocity through the tray

High vapor velocities, combined with high foam levels, will cause the spray height to hit the
underside of the tray above. This causes mixing of the liquid from a lower tray with the liquid
on the upper tray. This back mixing of liquid reduces the separation, or tray efficiency, of a
distillation tower.
 When the vapor flow through a tray increases, the height of froth in the downcomer draining
the tray will also increase. This does not affect the foam height on the tray deck until the
downcomer fills with foam. Then a further increase in vapor flow causes a noticeable
increase in the foam height of the tray deck, which then increases the spray height. When
the spray height from the tray below hits the tray above, this is called the incipient flood
point, or the initiation of jet flooding.

7. conning

Coning in a distillation column occurs when the rising vapor pushes the liquid back from the
top of the tray holes, causing poor vapor-liquid contact. This typically happens when the
liquid flow rate is too low compared to the vapor flow rate, resulting in the vapor forming a
cone shape as it passes through the liquid. Coning reduces the efficiency of the distillation
process because the liquid does not spread evenly across the tray. To avoid coning, ensure
the liquid and vapor flow rates are balanced, maintain proper tray design, and regularly
monitor and adjust the operating conditions of the column.
 8. pulsation
Pulsation in a distillation column refers to the periodic fluctuations in pressure and flow
rates within the column, which can disrupt the steady operation and efficiency of the
separation process. This phenomenon is often caused by irregularities in the feed rate,
vapor flow, or reboiler duty, leading to unstable vapor-liquid contact on the trays or
packing. To avoid pulsation, it is crucial to maintain consistent feed and vapor flow rates,
ensure proper column design, and use control systems to stabilize the operating
conditions. Regular monitoring and adjustments can help mitigate the effects of
pulsation and maintain optimal column performance

9. Mechanical Issues
• Description: Damage to internal components due to vibrations or misalignment.

• Cause: Equipment vibrations and mechanical wear.

• Avoidance: Regular inspections, proper installation, and maintenance.

Interpretation of a Dew point and Bubble Point curve

There are two curved lines on this graph. One represents the dew point; the other represents the
bubble point. A temperature scale is on the left side of the graph. The bottom scale shows the
composition of the mixture of compounds ‘A’ (Light one) and ‘B’ (Heavy one).

This graph tells us how much of ‘A’ and how much of ‘B’ is in the vapor and how much of each is in
the liquid at any given temperature.

For example, to find the composition of the vapor at a tray whose temperature is 250º F, first find
250º F on the temperature scale at Point ‘a’. Then, follow the line over to the dew point curve at
Point ‘b’. Now, drop straight down to the composition scale at Point. ‘c’ The composition scale reads
that the vapor at 250º F consists of approximately 60% ‘A’ and 40%. ‘B’. To find the composition of
the liquid on the same tray, start at 250º F on the temperature scale at Point ‘a’. Then, move over to
Point ‘d’ on the bubble point curve.

Finally, drop straight down to Point ‘e’ on the composition scale. The composition of the liquid on
that tray is 25% ‘A’ and 75% ‘B’. There will be a higher percentage of lighter components ‘A’ in the
vapor above a liquid than in the liquid itself.
Why control tower pressure
Why are distillation towers designed with controls that fix the tower pressure? Naturally, we do not
want to overpressure the tower and pop open the safety relief valve. Alternatively, if the tower
pressure gets too low, we could not condense the reflux. Then the liquid level in the reflux drum
would fall and the reflux pump would lose suction and cavitate. But assuming that we have plenty
of condensing capacity and are operating well below the relief valve set pressure, why do we
attempt to fix the tower pressure? Further, how do we know what pressure target to select?

How can an operator select the optimum tower pressure to maximize the benefits of
enhanced relative volatility, and reduced tray deck dumping without unduly promoting jet
flooding due to entrainment?

Point A is the incipient flood point. In this case, the incipient flood point is defined as the operating
pressure that maximizes the temperature difference across the tower at a particular reflux rate.
How, then, do we select the optimum tower pressure to obtain the best efficiency point for the
trays?

(Answer: Look at the temperature profile across the column.)

list of important concepts and terms

1. Distillation: A separation process that involves heating a liquid to create vapor and then
cooling the vapor to create a liquid. It is used to separate components based on differences
in their boiling points

2. Boiling Point: The temperature at which a liquid's vapor pressure equals the external
pressure, causing it to turn into vapor

3. Tray: A horizontal plate inside a distillation column where vapor and liquid interact to
enhance separation. Trays can be perforated or have bubble caps to facilitate contact

4. Packing: Materials used inside a distillation column to provide a large surface area for
vapor-liquid contact, enhancing separation efficiency

5. Reflux: The portion of condensed vapor that is returned to the distillation column to
improve separation by providing additional contact between vapor and liquid

6. Reboiler: A heat exchanger at the bottom of the distillation column that provides the
necessary heat to generate vapor from the liquid mixture

7. Condenser: A heat exchanger that cools the vapor exiting the top of the distillation column,
turning it back into liquid

8. Weeping: Occurs when liquid leaks through the perforations of the trays due to low vapor
flow rate, reducing separation efficiency

9. Dumping: Happens when liquid falls through the trays to the bottom of the column due to
insufficient vapor flow to support the liquid, leading to loss of separation efficiency

10. Coning: Occurs when vapor flow pushes the liquid back from the tray holes, forming a cone
shape and reducing vapor-liquid contact

11. Pulsation: Periodic fluctuations in pressure and flow rates within the column, disrupting
steady operation and separation efficiency

12. Latent heat This is the number of BTUs needed to change 1 lb of liquid into 1 lb of vapor. For
water, this is about 1000 BTU per pound, for diesel oil, about 100 BTU per pound.

13. Sensible heat This is the heat associated with the temperature of the material. This does
not include latent heat.

14. Specific heat This is the number of BTUs needed to heat 1 lb of liquid 1°F; for water, 1.0
BTU; for diesel oil, 0.5 BTU.

15. Enthalpy This is sensible heat plus latent heat.

16. Vapor pressure This is a key concept. As we heat a liquid, the molecules in the liquid try to
escape into the vapor phase. The hotter the liquid, the harder they try to escape. The
pressure that the molecules of liquid create as they push out into the vapor space is the
liquid vapor pressure. More volatile liquids such as LPG have a higher vapor pressure than
less volatile diesel oil.

17. Boiling point Heat a liquid and its vapor pressure increases. When the liquid’s vapor
pressure equals the pressure in the vessel, the liquid starts to boil. The temperature at
which this boiling start is the liquid’s boiling temperature.

18. Bubble point This is the same as boiling point. When a liquid is at its bubble point, it is also
said to be a saturated liquid at the temperature and pressure. If we raise the pressure, the
liquid’s bubble point temperature also goes up.

19. Dew point A vapor at its dew point temperature is on the verge of starting to condense to a
liquid. Cool the vapor by 1°F, or raise its pressure by 1 psi, and it will form drops of liquid. Air
at 100 percent relative humidity is at its dew point temperature. Cool it by 1°F and it starts to
rain.

20. Relative volatility Divide the vapor pressure of a lighter material by the vapor pressure of a
heavier material. The bigger the resulting number, the larger the relative volatility. It’s easier
to separate two components in a distillation tower if they have a larger relative volatility.

21. Theoretical stage This stage is created when vapor and liquid mix perfectly and then
separate without entraining any drops of liquid into the vapor or retaining any foam in the
liquid.

22. Tray efficiency A tray in a distillation tower will work at some percentage of efficiency
compared to a theoretical stage. This is mostly a function of how well the vapor and liquid
are mixed on the tray deck, and how well they are then separated.

23. Flooding Massive entrainment of liquid caused by high-level or high velocity of the up-
flowing vapor. A vapor-liquid separator (KO or Knock Out drum) that floods can wreck a
downstream compressor in a few seconds.

24. Tapped-out This is a mechanism of flooding due to a high liquid level caused by flawed
calibration of the level indicator. The liquid level has risen above the upper-level indication
connection point.

25. Thermosyphon circulation (or natural circulation) Partially vaporizing a liquid causes it to
flow to a higher elevation. The driving force is the density difference between the denser
liquid feed and the less dense, partly vaporized effluent.

26. Bernoulli’s equation Conservation of energy. If we want higher fluid velocity, that extra
energy must come from heat, pressure, or external work.

27. Kettle reboilers Also called a gravity feed reboiler. It has only a vapor outlet nozzle venting
back to the tower.
28. Grid tray Similar to a sieve tray. A perforated distillation tray deck, but with no movable
valve caps. Represents modern distillation tray design.

29. Equilibrium Stages An equilibrium stage is a hypothetical zone in which the liquid and
vapor phases of a mixture come into contact and reach equilibrium. At this point, the
composition of the vapor phase is in equilibrium with the composition of the liquid phase.

30. Raoult’s Law: Describes the vapor pressure of an ideal mixture.

31. Dalton’s Law: Relates to the total pressure exerted by a mixture of non-reacting gases.

32. Mole fraction: is a way of expressing the concentration of a component in a mixture. It is

defined as the ratio of the number of moles of a particular component to the total number
of moles of all components in the mixture.

33. Molar Mass: The mass of one mole of a substance is called its molar mass, usually
expressed in grams per mole (g/mol). For example, the molar mass of water (H₂O) is
approximately 18 g/mol, meaning one mole of water weighs 18 grams.
34. Mass=moles X molar mass.

Thank You
Bahgat Negm
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