Separation Technology CKD 20103/EXP2A/Jan2015

Experiment 2A : Bubble Cap Distillation Process

1. Objective(s)
The students should be able to:

Operate vapour liquid separation experiment using a Bubble Cap 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. The bubble cap distillation
column provides distinct stages at which such equilibrium can be approached.

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 reboiler, a column
and a vapour condensed. The reboiler 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.

Separation Technology CKD 20103/EXP2A/Jan2015

The unit consists of distillation column filled with bubble cap trays with a vacuum jacket and
thermo-siphon reboiler, vapour condenser, infinitely variable reflux control, distillate cooler and receiver,
all manufactured in borosilicate glass. Vapour generated in the reboiler rises through the column and is
condensed in a vertical water-cooled condenser. The condensed product leaves the column and passes
into an infinitely variable reflux ratio controller incorporating the variable area flow meters. Each column
component has five bubble cap plates with a temperature measurement nozzle on each plate. Vapour
and liquid compositions throughout are determined by respective temperatures. The unit is equipped with
the facility for liquid and gas sampling at the top and bottom of the column. A condenser consists of a coil
type heat exchanger. A reflux separator is provided at the top of the column. Reflux is returned to the
column and the product passes through a cooler and a graduated pipe section and can be passed either
to a receiving vessel, which allows product removal operating under vacuum or back to the boiler. A
sketch of a tray with bubble caps is as shown in the diagram below:

Figure 1: The cross-sectional diagram of bubble cap column

3. Chemicals and Ancillary Equipments

a) Chemicals required:
Industrial grade Ethanol
Water
b) Ancillary equipments/apparatus required:
TWO (2) 2000 mL beakers
TWO (2) 250ml beakers
Refractometer (for measuring sample concentrations)

Separation Technology CKD 20103/EXP2A/Jan2015

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.
The water supply pressure to the Condenser and the Coolers should not exceed 2 bar gauge.
Inspect the equipment visually for glass breakage and leakage.
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).
Dont isolate cooling water until the heating has been shut down (at least 10 minutes).
Dont switch on the immersion heater with the level in the reboiler below the heater elements or
when the reboiler is empty.
Dont return the product distillate collected to the reboiler vessel when the equipment is in operation.
Do not allow the liquid level to raise much above the top graduation on the tube before the stop
valves V2 and V3 are opened.
Dont 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.
2.
3.
4.

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

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

4.3 General Start-up Procedures

Materials needed:
a. Ethanol industrial grade
b. Water

Prepare 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 valves V1, RCV1, V3, V4, V5, V6, V7, V9 and FCV2 are closed.
Ensure valves V2, V8 and V10 are open.
Start fill in the Ethanol / Water mixture up to the desired level (ask lecturer / technician).
Slowly open the cooling water to the condenser (max 2.0 bars).
Make sure water is indeed flowing through it.

Separation Technology CKD 20103/EXP2A/Jan2015

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).
Check that the liquid level is satisfactory (Refer to instructor / technician).
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 RCV1 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 to roughly
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 Condition

Ensure that the valve for Reflux Ratio RCV 1 adjustment 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 the Temperature of the Reboiler TI4. If the temperature is already 90C, 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.
Continue 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).

Separation Technology CKD 20103/EXP2A/Jan2015

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

Standard Refractive Index (RI):
Ethanol :______________
Water : _______________
Table 1
% v/v Ethanol

Time
(Min)

TI 1

TI
1A

RI Value

Table 2
Temperature Readings ( C )
TI
TI 2
TI
TI
TI 4
1B
2A
2B

TI 5

TI 6

RI
Top
Product

RI
Bottom
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