Distillation Column

Operation and Troubleshooting

 Learning Outcomes

Upon the completion of this lecture you will be able to:

01 Identify the purpose of the distillation

columns and their classification. 04 Understand the process description of
methanol-water distillation column.

Identify the control loops associated

02 Understand the working principle of
distillation column. 05 with distillation process and
understand the emergency shutdown
devices ESD.

03 Identify the main components of

Distillation Column
distillation column. 06 Apply troubleshooting techniques to
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deal with emergency operations.
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 Separation Processes

Separation Processes are essential in chemical, petrochemical,

pharmaceutical and food industries. Basically, there are many different
techniques used for separation fluid mixtures into pure substances.

1. Distillation
2. Adsorption
3. Membrane separation
4. Absorption and stripping
5. Extraction
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6. Crystallization

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 What is a Distillation Column?

A distillation column is an essential equipment used to

separate the mixture into its component parts, or fractions,
based on their boiling points (difference in volatility).

More volatile component which has low boiling point goes

to the top of the distillation column. (light keys)
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Less volatile component which has high boiling point goes

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to the bottom of the distillation column. (heavy keys)

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 What is distillation column?

Fractionating columns are used in small scale laboratory distillations as

well as large scale industrial distillations.

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 Distillation Column Principle

50% H2O
50% CH3OH

Water - BP 100oC
Methanol - BP 64.7oC

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 Distillation Column Principle

10% H2O
90% CH3OH
20% H2O
80% CH3OH
30% H2O
70% CH3OH
40% H2O
60% CH3OH
50% H2O
50% CH3OH
Distillation Column

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 Distillation Column Principle

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 Types of Distillation Column
There are many types of distillation columns, each designed to perform specific
types of separations, and each design differs in terms of complexity.
1. Batch Columns
In batch operation, the feed to the column is introduced batch-wise. That is, the column is
charged with a 'batch' and then the distillation process is carried out. When the desired task
is achieved, a next batch of feed is introduced.

Feed Output
Batch Process

Feed Output
Batch Process

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 2.1 General procedure for material balance problems

2. Continuous Columns
In contrast, continuous columns process a continuous feed stream. No interruptions occur
unless there is a problem with the column or surrounding process units. They are capable of
handling high throughputs and are the most common of the two types.

Feed Continuous Output

Process

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 Types of Distillation Column

Continuous columns can be further classified according to:

Based on the nature of the feed that they are processing
• Binary column - feed contains only two components
• Multi-component column - feed contains more than two components

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 Types of Distillation Column

Continuous columns can be further classified according to:

The type of column internals
• Tray column - where trays of various designs are used
to hold up the liquid to provide better contact
between vapor and liquid, hence better separation.

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 Types of Distillation Column

• Packed column - where instead

of trays, 'packings' are used to
enhance contact between vapor
and liquid.

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 Main Components of Distillation Column
(1) Column (Tower): a vertical shell where the
separation of liquid components is carried out.

(2) Reboiler: to provide the necessary vaporization for

the distillation process.

(3) Condenser: to cool and condense the vapor

leaving the top of the column.

(4) 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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 Tray Distillation Column

(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 vapor. Vapor 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.

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 Tray Distillation Column

(2) Sieve Trays

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

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 Tray Distillation Column

(3) Valve Trays

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

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 Distillation Column Troubleshooting

(1) What will happen if we lose the feed?

Event Column Reflux Column Column Top Product
Level Drum Pressure Temperature Composition
Level
Losing the ↓ ↓ ↑ ↑ ↑
feed

We work in total reflux operation where there is no feed and no product.

No input and no output (closed loop system)

(We can reach the maximum purity of the top product in total
reflux operation)

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 Distillation Column Troubleshooting

(2) What will happen if we lose the condenser?

Event Column Reflux Column Column Top Product
Level Drum Pressure Temperature Composition
Level
Losing the ↓ ↓ ↑ ↑ ↓
condenser

We will have Total Shutdown!

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 Distillation Column Troubleshooting

(3) What will happen if we lose the reboiler?

Event Column Reflux Column Column Top Product
Level Drum Pressure Temperature Composition
Level
Losing the ↑ ↓ ↓ ↓ ↓
reboiler

We will have TOTAL SHUTDOWN!

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 Distillation Column Troubleshooting

(4) What will happen if we lose the min pump in the

top of the column?
Event Column Reflux Column Column Top Product
Level Drum Pressure Temperature Composition
Level
Losing the ↓ ↑ ↑ ↑ ↓
pump

We will use the STANDBY PUMP!

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 Distillation Column Troubleshooting

(5) What will happen if we increase the flowrate of

the reflux?
Event Column Reflux Column Column Top Product
Level Drum Level Pressure Temperature Composition
Increasing ↑ ↓ ↓ ↓ ↑
reflux flow
rate

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 Distillation Column Troubleshooting

(6) What will happen if we decrease the flowrate of

the reflux?
Event Column Reflux Column Column Top Product
Level Drum Pressure Temperature Composition
Level
Decreasing ↓ ↑ ↑ ↑ ↓
reflux flow
rate

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 Methanol – Water Distillation Column

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 Feed Unit

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 Feed Preheater

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 Distillation Column

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 Condenser

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 Reboiler

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 Utility Unit

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 ESD

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 Distillation Column Problems
Distillation column is design to work within predetermined set of limits. However if it
works outside these limits problems can occur and effect the efficiency and the
product quality.

Operating a distillation column involves maintaining an equilibrium (or balance)

between the rising vapor and the falling liquid in the column.

Changes in feed flow rate will affect the balance ➔ it will affect the quality and
quantity

Therefore, the optimum feed rate is often determined when the system is being
designed. A range of acceptable variation is usually specified as well.

High feed rate may lead to increase in column bottom level or flooding in the column.

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 Distillation Column Problems

(1) If the feed flow rate is very high and above the optimum rate this may lead to
overloading.

Overloading is a condition where the vapor flow rate raising up the column is impeded
by liquid flowing down the column. The increase of the hydrostatic pressure restricts
the vapor raising through liquid. If overloading continues more and more liquid will
backs up in trays and raising vapor will be severely blocked (this condition is known as
flooding)

There other causes of flooding

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 Distillation Column Problems

Flooding will happen due to the following conditions:

1. Increasing the flow rate of the feed above the optimum value
2. Higher than normal reflux flowrate.
3. If the temperature of the reflux is too low
4. Excessive vapor flow rate “due to high temperature at the bottom of the
column”
5. It may occur due to scaling and trays blockage.

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 Distillation Column Problems

Indicators for flooding:

1. Column pressure and temperature.

• Pressure in the bottom will raise due to the restriction of the vapor to
move up which increases the the pressure drop. ∆P ↑
• Temperature in the bottom will increase due to the restriction of the heat
of reboiler from raising. ∆T ↑

2. Sharp decrease in column efficiency.

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 Distillation Column Problems

elimination of flooding:

1. Decrease feed rate

2. Decrease reflux rate
3. Decrease bottom temperature
4. Or in extreme cases we need to shutdown the column.

Some of the more common methods used to eliminate

flooding involve temporarily decreasing the feed rate, the reflux rate, or both, to
reduce the amount of liquid in the column, and decreasing the vapor in the
column by reducing the reboiler steam. In extreme cases, it may be necessary to
shutdown the column so that the problem can be corrected.

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 Distillation Column Problems

(2) If the feed flow rate is very low and below the optimum rate this may lead
to decrease in the performance of the distillation column

To correct the low feed problem ➔ caused must be identified

Blockage in the feedline “needs to be cleaned”
Problem in the instrumentation “reading are not identical” it should be
controlled manually.

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 Distillation Column Problems

(3) Temperature of the feed should be close to the temperature of

the feeding tray.
If the temperature much higher or lower the temperature of the feed tray
product separation will be disturbed.

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 Distillation Column Problems

More problems due to vapor flow conditions can cause:

Foaming
Entrainment
Weeping/Dumping

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 Distillation Column Problems
Foaming:
Foaming refers to the expansion of liquid due to passage of
vapor or gas. Although it provides high interfacial liquid-
vapor 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.

Foam inhibitors can be added to reduce the foaming tendency.

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 Distillation Column Problems

Entrainment:
Entrainment refers to the liquid carried by vapor up to the tray
above and is again caused by high vapor 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.

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 Distillation Column Problems

Weeping/Dumping:
This phenomenon 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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 Distillation Column Problems

Flooding:
Flooding is brought about by excessive vapor flow, causing
liquid to be entrained in the vapor up the column. The
increased pressure from excessive vapor also backs up the
liquid in the downcomer, 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.

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 Distillation Column Problems
Bottom product: The heavier components of the distillation process that flow into the bottom section and on the kettle reboiler by
gravity.

Distillation column: the separation of components in a mixture by their boiling point.

Downcomer: downspout that allows liquid to drop to lower trays.

Feed tray: point of entry of the process fluid in a distillation column under feed line.

Overhead product: the lighter components in a distillation column which rise through the column and go to the overhead line, where
they are condensed.

Overloading: operating plant at maximum conditions.

Reflux: condensed vapor from the lightest component coming off the top of the column which is cooled and condensed into a liquid so
that it can be pumped back to the top tray in the column to control product purity and temperature.

Weeping: occurs when the vapor velocity is too low to prevent liquid from flowing through the holes in the tray instead of across the
trays.

Rectifying section: a section of the distillation column above the feed line in which a higher concentration of the light components
exists.

Stripping section: a section of the distillation column below the feed line in which a higher concentration of the heavy components
exists.

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