Separation Technology/CKD 20103/EXP2B/Jan2015

Experiment 2B : Packed Column Distillation Process

1. Objective(s)

The students should be able to:

 Operate vapour – liquid separation experiment using a Packed Column Distillation Process Unit.
 Prepare a calibration curve for Refractive Index (RI) vs Concentration of Ethanol-Water mixtures.
 Analyze the sample of top and bottom product by using Refractometer to obtain the Refractive Index
(RI) in order to determine their respective composition.
 Obtain the time when the distillation process is nearly finish.

2. Introduction

Distillation is one of the important unit operations in many chemical industries and has been used from
the inception of chemical and process industry. Distillation is used for the separation of components in a
liquid mixture of volatile constituents. The Distillation Column is usually a vertical column where the liquid
and vapour phases of the mixture are made to mix and approach equilibrium. Packed Bed Distillation
Columns are sometimes used to carry out the Distillation in the industry.

Distillation is a process of separating the components of a solution by the application of heat

when the vapour produced by boiling the solution has a different composition to that of the solution. If the
vapour formed is condensed and subsequently reboiled it will produce, yet again, a vapour of different
composition. Repeated boiling of condensed vapours will ultimately produce a product of desired quality
rich in concentration of one of the components of the original solution.

Distillation takes place in a Distillation Column which, in essence, comprises a Boiler, a Column
and a Vapour Condensed. The Boiler provides the heat for vapour generation; within the column rising
vapours continually mix with liquid flowing down the column, condense and are reboiled until vapour of
required composition leaves the column and condenses in the Vapour Condenser to be removed as
Liquid Product. A certain proportion of this condensate is returned to the column, called Reflux, the
proportion being a major influence on the quality of the product achieved.

Since this experiment use Batch Distillation plant, therefore, it can be said that this is a process
whereby a specific quantity of a liquid mixture is separated into its components. The technique is used
extensively in laboratories and small scale production plants where the equipment is often used for
separating several different mixtures of where if only one mixture is separated, the mixture is not
produced continuously. The relatively high capital cost of Continuous Distillation Plants with their
sophisticated control systems, often results in smaller companies operating Batch Distillation plants.
Batch Distillation is particularly useful for separating liquid mixtures contaminated with solids which would
otherwise foul a continuous plant.

This unit comprises of a Reboiler operating on the Thermosyphon principle heated by either
steam or electrically. Process vapours enter at the base of the column which contains a Packed Column
containing 10 mm Raschig Rings, (the vapour temperatures entering and leaving the column are
measured by temperature indicators TI 3 and TI1 respectively as shown in the Process Flow Diagram of
this unit.) and are condensed at the top of the column in a Condenser. The Distillate is separated into
Reflux, which is passed back to the column and Product, which passes through a Product Cooler and
then through a Graduated Pipe Section. The Product may then be collected or returned back to the
Reboiler. Vapours leaving at the top of the column are totally condensed to Liquid Distillation in the
Overhead Condenser and pass to the Reflux Control Flow Meters RI 1A and RI 1B. RI 1A indicates the

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quantity of Distillate returned to the column via the three-way valve while RI 1B indicates the quantity of
Distillate removed as Product.

Figure 1: Process Flow Diagram for Packed Column Distillation Process Unit

3. Chemicals and Ancillary Equipments

a) Chemicals required:

Industrial grade Ethanol

Water

b) Ancillary Equipments required:

TWO (2) 2000ml beakers

TWO (2) 250ml beakers
Refractometer (measuring sample concentrations)

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4. Operating Instructions

4.1 Safety Considerations

 You must familiarize yourself with each item such as the Reboiler, Condenser, Distillation Unit
and the flow paths and apparatus before conducting of the experiment. This distillation operation
usually deals with very hot and highly flammable materials. Extreme care must be taken when
handling the apparatus, in taking readings and collecting samples.
 The Flow Meters should be operated smoothly in order to avoid pressure surges within the
equipment.
 Inspect the equipment visually for any damaged components or glass breakage. If any such
defects are noticed, please report them to your instructor / technician.
 Goggles must be worn at all times in the laboratory.
 Appropriate rubber gloves must be worn when Organic Solvents are handled.
 Avoid wearing clothes which can easily catch fire.
 The flow rates of liquids should not exceed the maximum of the rates shown in the flow meter.
 Do not allow the water pressure to exceed 2.0 bar maximum as indicated by PI.2. Always
maintain V8 in the open position during atmospheric operation (avoid system pressurizing).
 Don’t isolate cooling water until the heating has been shut down (at least 10 minutes).
 Don’t switch on the immersion heater with the level in the reboiler below the heater elements or
when the reboiler is empty.
 Don’t return the product distillate collected to the reboiler vessel when the equipment is in
operation.
 Do not allow the liquid level to rise much above the top graduation on the tube before the stop
valves V2 and V3 are opened.
 Don’t drain the liquid in reboiler vessel until is cold.
 Do not touch the hot components of the unit.

4.2 Calibration Curve Curve for Refractive Index vs concentration of Ethanol-Water mixtures

1. Prepare a 5% v/v ethanol-water solution in a test tube.

2. Using a refractometer, obtain the refractive index reading for the solution.
3. Repeat step 1 to 2. Using increments of 5%, obtain refractive index readings for ethanol-water
mixtures up to 100 %.
4. Record the RI reading for each of 5% v/v concentration in Table 1.

4.3 General Start-up Procedures

Materials needed:

a. Ethanol industrial grade

b. Water

 Prepare between 30 litres of 10% v/v (volume/volume) mixture of Ethanol in Water by mixing
appropriate quantities of the Industrial Grade of Ethanol in Distilled Water.
 Using the Refractive Index (RI) method, check the RI of pure ethanol and pure water and
record at Time “0” in the Table 2.
 Refer to the diagram of the equipment in the lab for better / accurate view.
 Ensure that the concentration of feed in the reboiler vessel is correct and that the liquid level is at the
vessel equator.
 Ensure valves V1, RCV1, V3, V4, V5, V6, V7, V9 and FCV2 are closed. Ensure valves V2, V8 and
V10 are open.
 Start fill in Ethanol / Water mixture up to the desired level (Ask Lecturer / Technician).

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 Slowly open the cooling water to the condenser (max 2.0 bar). Make sure water is indeed flowing
through it.
 Check water flows to the drain from the Cooling Water outlets.
 Do not start the experiment until the Cooling Water flow is visible in the outlets to the drain.
 Ensure that the Bottom Product sampling valve V5 and Top Product sampling valve V4 is closed.
 Ensure that the Reboiler Vessel is already charged with the Ethanol – Water mixture through the
Charge Port (Refer to the diagram).
 Otherwise top up with the Ethanol – Water mixture through the Charge Port (Refer to instructor /
technician).
 Ensure that the concentration of feed in the Reboiler vessel is correct and that the liquid level is at
the Vessel Equator (Refer to Lecturer / Technician).
 The Reboiler Vessel should never be filled with liquid above the maximum level indicated.
 The level should never recede below the minimum level while on operation.
 Close the Reflux Adjustment Valve RCV 1 and valve below Product Cooler V2.
 Obtain a sample of Ethanol – Water mixture from the Reboiler through the Sampling Port and test its
composition using Refractometer.
 Turn on the main power control switch. Turn on the power switch of the heater.
 Switch on electrical supply (green ‘heater on’ button).
 Set heater controller HC.4 to maximum setting (About 200 V).
 Allow a period of 15 minutes for the equipment to maintain thermal equilibrium with surroundings.
 Observed the temperature readings of all Temperature Indicator (TI). Record the temperature
reading every 5 minutes (from Time “0” onwards).
 When distillate liquid is seen to flow through RI.A1, reduce the heat input and set HC.4 (About 150V).
 During this period observe HC.4.
 The unit is now ready to be used for an experiment.

4.4 Experiment: Operation under Partial Reflux Conditions

 Ensure that the valve for Reflux Ratio adjustment RCV 1 is opened.
 Adjust both valve for Reflux Ratio RCV 1 and valve below Product Cooler V2 so that both readings
on R1 and R2 provide a Reflux Ratio of 1.0 for the operation.
 Wait for about 15 minutes until the flow rate shown by R1 and the temperature readings at the top
and bottom of the columns are steady ( Refer to instructor / technician ).
 Collect samples from the Reboiler and the overhead from the Sampling Port for every 5 minutes.
 Observe Temperature of the Reboiler TI 4. If the temperature is already 90ºC, reduce the current of
the Reboiler to between 150V to 160V.
 Observe the flow rate at R1. Adjust the valve for Reflux Ratio adjustment to ensure that the
Reflux Ratio is maintained at 1.0.
 The concentration of the samples drawn is measured using the Refractive Index method.
 Record the reading of temperatures for every 5 minutes.
 Readings are recorded in the provided table of results.

4.5 General Shut – Down Procedures

 Adjust heater controller HC.4 to minimum setting.

 Switch off electrical supply (red ‘heater off’ button).
 Turn off the power switch of the reboiler.
 Turn off the main power control switch.
 Do not drain the hot liquid from the Reboiler. If necessary, the liquid within the system could be
drained only when the liquid is already cooled.
 Allow the Cooling Water to run for some time (Ask Lecturer / Technician).

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5. Result (Please attach this part in your report)

Standard Refractive Index (RI):

Ethanol :______________
Water : _______________

Table 1
% v/v Ethanol RI Value

Table 2
Time Temperature Readings ( º C ) RI RI
(Min) TI 1 TI 2 TI 3 TI 4 TI 5 TI 6 Top Bottom
Product Product
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
105
110
115
120