USER’S MANUALS

For

 COMPUTER OPERATED DISTILLATION COLUMN

(PILOT PLANT)

Printed in India  August 2018

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 Table of Contents

1. INTRODUCTION TO DISTILLATION COLUMN ....................................................... …2

1.1 Distillation........................................................................................................................... 2

1.2 Bubble Cap Plates ............................................................................................................... 3

2. SAFETY ISSUES ..................................................................................................................4

3. PROCESS DESCRIPTION ..................................................................................................5

4. SIEVE TRAY PLATE DISTILLATION COLUMN OPERATION...................................8

5. START UP PROCEDURE ...................................................................................................9

5.1 The sequence for startup of operator consoles is as follows:- ............................................... 9

5.2 Pre- Start- Up Inspection ..................................................................................................... 9

5.3 Cold Start ............................................................................................................................ 9

5.4 Establishing Vapor Flow ................................................................................................... 10

5.5 Starting Reflux to the Column ........................................................................................... 10

5.6 Placing the Column on Auto .............................................................................................. 11

6. SHUT DOWN PROCEDURE ............................................................................................ 12

6.1 Shut down Procedure ......................................................................................................... 12

7. EXPERIMENT.................................................................................................................... 13

7.1 Objective ........................................................................................................................... 13

7.2 Pre- Start- Up Inspection ................................................................................................... 13

7.3 Procedure .......................................................................................................................... 13

7.4 Observation ....................................................................................................................... 15

7.5 Result ................................................................................................................................ 15

 1. INTRODUCTION TO DISTILLATION COLUMN

1.1 Distillation
It is a process of separating component substances from liquid mixtures through vaporization and
condensation, based on different volatility (vaporization point) of components in the mixture.
Distillation is a unit operation, or a physical separation process, and not a chemical reaction.
Commercially, distillation has a number of applications. It is used to separate crude oil into more
fractions for specific uses such as transport, power generation and heating. Air is distilled to
separate its components—notably oxygen, nitrogen, and argon—for industrial use. Liquid chemicals
for diverse uses are distilled after synthesis to remove impurities and unreacted starting materials.
Distillation of fermented solutions can produce distilled beverages with higher alcohol content. The
premises where distillation is carried out, especially distillation of alcohol are known as a distillery.
A still is the equipment used for distillation.

The unit operation distillation is used to separate the components of a liquid solution, which
depends upon the distribution of these various components between a vapor and a liquid phase. All
components are present in both phases. The vapor phase is created from the liquid phase by
Vaporization at the boiling point. If a homogeneous liquid solution is boiled, the vapor is rich in
the more volatile components than in the liquid, whereas the remaining liquid is richer in the less
volatile components. The separation of crude petroleum into gasoline, kerosene, fuel oil and
lubricating stock and the separation of a mixture of Methanol-water and Benzene-Toluene into its
components are examples of distillation.

Distillation may be carried out by either of two principal methods:

1. Based on the production of a vapor by boiling the liquid mixture to be separated and condensing
the vapors without allowing any liquid to return to the still in contact with the vapors.

2. Based on the return of part of the condensate to the still under such conditions that this returning
liquid is brought into intimate contact with the vapors on their way to the condenser.

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1.2 Bubble Cap Plates
Consider a column constructed with “plates” along its entire length as shown in figure. Liquid
introduce into the plate-type column form a shallow pool on each plate. The liquid flows across the
plate, while the gas bubbles up through the risers in the plate (called Bubble Cap). Each plate or
tray has a short section of tubing cut through the plate

Fig. - Schematic representation of bubble cap plate.

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 2. SAFETY ISSUES

 In this experiment methanol-water mixture is used in the distillation process.

 It is hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion,

& of inhalation. Since methanol is very volatile, cover the beaker right after taking
sample and avoid inhale. Collect the sample in the waste container.

 Make sure to turn off the cooling water pump and the electricity at the end of the
experiment.

 In case of skin or eye contact, flush contacted areas with plenty of water remove
contaminated clothing or contact lenses.

 In case of ingestion, do not induce vomiting unless directed to do so by medical

personnel.

 Never give anything by mouth to an unconscious person. Loosen tight clothing such as
collar, tie or waistband.

 In case of inhalation immediately, get a breath of fresh air.

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 3. PROCESS DESCRIPTION

The DISTILLATION COLUMN OPERATIONS program uses conventional Bubble Cap Plate
Distillation system. These are so named because they have a number of horizontal plates or trays,
which are usually equally spaced in the upright column shell. These trays provide time for mixing
and interchange of vapor and liquid flows required for carrying out distillation separation. The
relatively large number of trays used generally produces tall and upright structure, and is the
reason for the term "column" or “tower”.

The physical arrangement of the distillation column used in this training and its auxiliary
equipment, are shown in the graphics. The column contains 7 trays, which are required to achieve
desired separation. Liquid feed enters from the feed pump to some point way down the column.
The tray on which feed enters is called "Feed tray". The part of the column above the Feed tray is
called Rectifying Section and that below including the Feed tray is called Stripping Section.
Preheater is provided with electric immersion heater for heating the liquid upto desired set point.
Reboiler is provided at the bottom with the electric immersion heater for heating the liquid at the
bottom of the column to its boiling point. Vapor leaves from the top of the column and passes
through the Overhead Condenser, where large part of it is condensed. The condensed liquid flows
into the Reflux Drum. The High boiling material leaves the bottom of the column as Bottom
Product.

The liquid in the Reflux Drum, which has high percentage of "fraction" of low boiling material, is
pumped out by Reflux Pump. A large part of pump flow is returned directly to the column as
"liquid reflux". The remaining liquid leaves the tower as "overhead liquid" product.

NOTE: The arrangement of this auxiliary equipment and manner in which vapor and condensed
liquid are used as reflux, or removed as product, vary greatly with different installation, with
material being separated, and with the purity of product desired.

The working of the individual parts of tower and the auxiliary equipment, as mentioned below,
should help you in understanding the operation of this equipment.

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Liquid passes through the column from plate to plate by means of suitable down-flow pipes. The
entrance of the down-flow pipes acts as weir over which liquid must flow. The height of this weir
determines the height of the liquid that is to be maintained on the plate. The lower ends of the
down-flow pipes are sealed in the liquid of tray to which they empty.

The vapor rise through each tray of the tower is series path. In passing through each plate, the
vapor is deflected beneath the surface of the liquid and is distributed into the liquid by means of
Bubble Caps. Intimate mixing of the two streams of liquid and vapor, throughout their
countercurrent flow paths, is maintained.

The hot vapors entering the plate give up the heat to the liquid. Some of high boiling material in
the vapors is condensed and passes to the lower plate as liquid. The heat supplied condensing hot
vapor causes some of the low boiling material to vaporize and passes upward to the tray above.
The combined action of all the trays causes the low boiling material to works its way up the
column as vapor, while the high boiling material drops to the bottom of the column as liquid.

You can think of the individual tray as being specially designed hold up tank, with liquid in from
the tray above (and the feed in the case of feed tray), vapor flow in from the tray below, and liquid
flow out to the tray below plus vapor flow out to the tray above. With the column in continuous
balanced operation, the holdup of the boiling liquid is nearly constant due to the action of the
down-flow pipe weir and a material balance is always maintained. That is, the total material
flowing into the tray from all the sources must be equal to the total material leaving the tray. It
follows that a similar increase or decrease in the liquid rates out accompanies an increase or
decrease in one of the liquid rates into the trays.

The temperature of the boiling liquid is fixed by the column pressure and liquid composition and
heat balance is always maintained. For the continuous balanced operation, the sensible heat of the
liquid and vapor flows into the plate plus the latent heat of the condensing vapor must equal the
sensible heat of the liquid and the vapor flow out, plus the heat loss and the heat of mixing. Since
the temperature change from one tray to another is usually small, the heat balance effectively
reduces the balance between the heat given up by condensing vapor and the heat required to
vaporize the liquid leaving the plate. And as the heat of vaporization and condensation have
similar values, the vapor rate out of the tray is nearly equal to the vapor rate into the tray.
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Liquid enters the bottom part of the column from the bottom tray down-flow pipe. Part of this
liquid flows into the reboiler section, where heat is applied to raise the liquid temperature to its
boiling point and produce a vapor flow. The vapor from the reboiler reenters the bottom tray and
proceeds upward in distillation column. Liquid containing high percentage of boiling material is
drawn off as the bottom's liquid product.

The heat required to raise the liquid at its bubble point temperature depends upon the tower bottom
pressure and the nature of the liquid mixture. More heat tends to boil off the low boiling mixture,
producing the vapor flow to the bottom of the tower. The more vapor produced, the richer the
bottom liquid becomes, in high boiling material. Therefore, for reasonably constant column
pressure, the bottom plate temperature can be used to adjust the fraction of high boiling material in
the bottom product flow. Increasing the bottom tray temperature will increase the bottom fraction
of boilers.

Vapor containing a high percentage of low boiling material leaves the top tray and goes to the
overhead condenser, where it is condensed. Part of the condensed vapors are drawn off as
overhead liquid product, and remainder is returned as liquid reflux. This reflux becomes the liquid
input to the top tray and flows from the top of the column down to the feed tray. Note that the
liquid reflux contains about the same fraction of low boiling material as the vapor from the top
tray.

The reflux rate effectively determines the time that the feed material remains in the column. A
large reflux rate means high portion of the overhead vapors are returned to the column giving the
material a longer time exposure to the separation operation, making it richer (higher percentage) in
low boiling material. A smaller reflux flow will produce a less pure overhead product.

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4. SIEVE TRAY PLATE DISTILLATION COLUMN OPERATION
4.1.1 Operation from the panel

Main power supply to all the equipments and control instruments provided on panel. All the rotary
equipments can be operated only from the SCADA which includes different pumps such as
cooling water, reflux, feed, and Bottom Product. Electrical supply for electric heater on panel
which is to be operated, while the electric heater output can be varied from the operator control
station (SCADA).

Sr. No. Instruments No. Description

1 ELCB Mains Power Switch
1 P - 01 Cold Water Pump
2 P – 02 Bottom Product Pump
3 DP – 01 Reflux Pump
4 DP – 02 Feed Pump
5 HE – 02 Chiller
6 Heater - 01 Preheater Tank Heater
7 Heater - 02 Reboiler Tank Heater

4.1.2 Operation from the computer operation station:

The system being digitally controllable thereby most of the control operation can be done from the
operator console station which gives the liberty to operate various instruments and to understand
process control schemes those been applied such as temperature control system for reboiler etc.

4.1.3 Operation from the field:

There are manually controllable valves (Hand valves) are provided for tank drain, pump
recirculation, which is to be operated through field.

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 5. START UP PROCEDURE
5.1 The sequence for startup of operator console is as follows:-
1. Start the computer.
2. To start the program double click on the icon named “TSSS200”. Now program will be
started.
3. Dialog box will be displayed with the facility for selecting the model.
4. Select Distillation Column and click ok to start the software

5.2 Pre- Start- Up Inspection

Prior to start-up, the following plant system and services should be available.

1. Electric power, control panel power and control system

2. Compressed Air for service and instrumentation Air
3. Cooling Water Supply
4. No leakage in the system pipe line and instruments like pump, pneumatic valve, column
etc. if any leakage found attend it.
5. Make sure all instruments vents and drains are operating properly.

5.3 Cold Start

1. The Column should be cold that is:
a. Cold water control valve should be closed.
b. Feed pump and reflux pump should be switched off.
c. All controllers should be in manual mode.
d. All controller outputs should be zero (control valves closed & heater off).

2. Start the Main Earth Leakage Circuit Breaker (ELCB) from panel and then start all
switches from panel.

3. Start Cold Water pump by clicking on switch from SCADA (computer).

4. Open the Condenser HE-01 by giving 100% output to cooling water control valve PCV 04.

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 5. Add feed in feed tank (T-01), open hand valve to take the feed to preheater tank (T-02)
from feed tank (T-01).

6. Switch TIC 101 to auto mode, Preheat the feed up to desire value by giving set point
TIC101 controller.

7. Switch on the feed pump (DP-02) and give the required output (flow rate) from SCADA
for loading the Reboiler Tank with feed.

8. Check the Reboiler level, as indicated by LIC-01.

5.4 Establishing Vapor Flow

1. Using the TIC - 103 control in manual mode, slowly increase heater output to heat the feed
in the Reboiler to its boiling point. After achieving the desired temperature at column top
and bottom put the TIC-03 controller in Auto mode. As the vapor generated in the Reboiler
reaches the top of the column, the condenser (HE-01) will condense it. The vapors
condensed to liquid flows into the Reflux Tank (T-04) causing the drum level to rise as
indicated by LIC-02.

2. If the level in the Reflux Tank rise too fast, reduce the vapor flow rate by cutting the
Reboiler heater load (reducing the output/set point of controller TIC-03).

5.5 Starting Reflux to the Column

1. When the level in the Reflux Drum reaches 20-30% switch on the Reflux pump (DP-01)
from SCADA.
2. Using the controller TIC-102, adjust the reflux flow rate to maintain the top temperature of
distillation column and use controller LIC-02 in auto mode to maintain the level of the
reflux tank.
3. Maintain a level of about 30% in the reflux tank T-04.

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5.6 Placing the Column on Auto
1. To obtain the desired product split requires:

a) Periodic monitoring of recorded and indicated variables for spotting trends in column
Operation.
b) Avoiding extra large changes in operating conditions.
c) Avoiding operation that leads to emptying or overflowing the re-boiler and reflux drum.
d) Maintaining a constant column top pressure.
e) Adjusting the re-boiler temperature to change the fraction of the higher boiling point
component in the bottom product flow. Maintaining the re-boiler temperature below the
boiling point of the component with a higher boiling point will increase the fraction of
high boiling material in bottom product flow and vice-versa.
2. Adjust the reflux rate to obtain the desired fraction of low boiling material in the operating
point.
3. Continue these small adjustments until the column is operating at or near the specified point.

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 6. SHUT DOWN PROCEDURE

6.1 Shut down Procedure

1. After Complete separation, when all distillate product and bottom product separate out
switch off heaters and all pump except cooling water pump from SCADA
2. Do not turns off cooling water pump from SCADA until re-boiler temperature get back to
ambient temperature
3. Close all the pneumatic valve and hand valve except recirculation valve of all tanks.
4. Shut down all pumps and air supply.
5. Take out the sample from distillate tank and bottom product tank, and send it for analysis.
6. Turn off the electric supply.

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 7. EXPERIMENT
7.1 Objective

The objective of this experiment is to demonstrate Distillation Separation Process for a binary
mixture of methanol-water

7.2 Pre- Start- Up Inspection

Prior to start-up, the following plant system and services should be available.

1. Electric power, control power and control system

2. Compressed Air for service and instrumentation Air
3. Cooling Water Supply
4. No leakage in the system pipe line and instruments like pump, pneumatic valve, glass
column etc. if any leakage found attend it.
5. Make sure all instruments vents and drains are operating properly.

7.3 Procedure
1. Check to ensure the drain and vent valves are closed for all tanks before filling.
2. Turn on the cold water pump (P-01) and chiller from SCADA. The flow rate of cooling
water will be operated manually using hand valve.
3. Fill the preheater as per requirement, operate TIC-101 in Auto Mode & Maintain its
temperature up to 50˙C.
4. Fill the re-boiler up to 20-40% of its Capacity from Pre-heater (T-01) through feed dosing
pump DP-02.
5. If the liquid level is OK and the valves are in the correct positions continue with startup.
6. If you want to collect data during the column warm up period note down start time and
Start Collecting data for temperature and flow as mentioned below. You should make a
note in your notebooks of the time in seconds whenever you make any changes in the
heater or controller set points from here to the end of the experiment.

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 7. Click on the TIC-103 controller on the computer. Initially operate the TIC-103 Controller
in manual mode and when re-boiler temperature achieves the desired temperature then put
controller in auto mode. You can monitor the temperature of the re-boiler liquid by
monitoring TIC-103 controller.
8. When the temperature of re-boiler reaches to set point it may go a little higher you should
see some movement of vapor up the column. You may also see movement of liquid in
some of the down comers. You will probably see the temperature of column, bottom and
middle temperature rise to their steady state temperature.
9. Depending on the concentration of high volatile component in the re-boiler accordingly
adjust the temperature of the column top.
10. Maintain the temperature of the Reboiler by operating TIC-103 controller as required.
Observe the re-boiler temperature and the tray temperatures to see where the vapor is at.
Experiment should progress such way, temperature profile reaches same value at all the
stages which can be observed in column temperature indicators
11. After maintaining the temperature in the column between (85-90°C) vapors generated will
get condense in the condenser. Reflux tank provided for collection of condensate from
condenser and level in the reflux tank start increasing which can be observed on mimic
screen (LIC-102) in computer. If you still do not see any condensate from condenser in the
reflux tank, slowly raise the temperature in the reboiler up to 3-5°C more and let it heat up.
12. By this time you should see a stable temperature in the reboiler and vapor being condensed
in the reflux tank.
13. When you have the column operating correctly, after collecting sufficient amount
condensate in the reflux tank (2-3 liters) then start reflux pump to maintain reflux ratio. To
maintain reflux flow to the column, operate the Dosing Pump - 01 and distillate tank flow
by operating the (PCV-02)
14. After complete separation turn off the Reboiler heater.
15. When Reboiler temperature decrease below 50°C then start bottom product pump and
collect low volatile component in the bottom product tank.
16. Collect samples from the bottom product tank, Distillate tank, and feed tank.

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7.4 Observation Chart

1. Amount of (Methanol) = _________ Lit

2. Amount of (Water) = _________ Lit
3. Total Quantity of Feed = _________ Lit
4. Feed Flow rate = _________ LPH
5. Density of (Methanol) =__________ Kg/M3
6. Density of (Water) =__________ Kg/M3
7. Density of Feed Mixture =__________ Kg/M3
9. Experiment Start Time =__________
10. Experiment End Time =__________

7.5 Result

1. Purity of Final Product = ________

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