University of Santo Tomas

CHE 514L:
Faculty of Engineering
Chemical Engineering Laboratory II
Department of Chemical Engineering Design of Experiment

Name of Members:
1. MOTOL, Rich Kevin C. Date Performed: Sept. 19, 2018
2. PADILLA, Demi M. Date Submitted: Sept. 26, 2018
3. PAÑA, Trisha Niña M.
Section: 5ChEB Group No: 2 Instructor: Engr. Rose Mardie Pacia

Distillation

I. Objectives
1. To be able to separate the ethanol-water mixture using batch distillation process.
2. To determine the concentration of the distillate using specific gravity.
3. To study the effect of reflux ratio and temperature to the concentration and
volume of the distillate collected.

II. Theory
Distillation is a unit operation that can be used to fractionate liquid mixtures. It utilizes
the different volatilities of the components of the mixture to be separated. To achieve
separation, the liquid mixture is brought to boiling point. The resulting vapor phase is made
up of several components, mainly the more volatile components of the mixture. The vapor
phase is separated from the liquid phase and condensed (distillate). The less volatile
components predominantly remain in the liquid phase and becomes the residue.
Distillation apparatus consists of an evaporator to heat the initial mixture and collect
the high-boiling component (residue), a condenser to condense the low-boiling component
(distillate), and one or more vessels in which to collect the distillate. Distillation does not
produce a complete separation of the initial mixture. It just divides the initial mixture into two
mixtures with different mixture ratios.
In simple distillation, all of the distillate is collected. There is also the process in which
the condensate is collected in different vessels, known as fractions, as distillation time
passes. This is known as fractional distillation. To protect temperature-sensitive substances
during distillation, their mixtures are distilled in a vacuum where boiling points are lower. This
method is known as vacuum distillation.

Figure 2: Distillation Process

 The result of the separation obtained by distillation is not sufficient in all cases. To
improve separation, the collected condensate should be distilled again. This process should
be repeated until the required material is satisfactorily purified. Multiple-stage distillation of
this type is expensive and energy-intensive. Rectification is therefore used.
In rectification, the released vapor is first passed through a vertical tube called the
column before it reaches the condenser. Instead of all of the distillate collected in the
condenser being drawn off straight away, part of it is returned to the column as the so-called
reflux.
The high-boiling component condensed first from the rising vapor. The resulting
condensation heat causes more low-boiling component to evaporate in turn. The result is that
the liquid flowing back to the bottom of the column is enriched with high-boiling components.
The vapor at the top of the column is correspondingly richer in low-boiling components.
The exchange of materials that occurs in the column can be intensified by increasing
the contact area over which the exchange can take place. Columns therefore contain suitable
internals such as trays or packed bed which increase this contact area. At the top of the
column, the distillate is divided into one-part reflux and one-part top product. The ratio of
reflux to top product is called the reflux ratio. It is an important parameter of the column.
Liquid mixtures can be almost totally separated by rectification especially mixtures whose
equilibrium curves deviate only slightly from the diagram diagonal.

Figure 4: Rectification system

III. METHODOLOGY

1 Condenser
2 Pressure Gauge
3 Hand Valve
4 Flowmeter
5 Column
6 Evaporator
7 Control Cabinet
8 Top Product Container
9 Reflux Divider 1
10 Vacuum Pump
1
 14 Emergency Stop Button
15 Reflux Divider ON/OFF
16 Reflux Ratio Display
17 Display and Measuring Point
Selector for temperature T1 – T12
18 Heater ON/OFF
19 Controller for Head
Temperature T13
20 Heater Indicator Lamp
21 Low Level Warning Lamp
22 System Diagram
23 Reflux Ratio Selector
24 Master Switch

Start-Up:
1. Ensure that all hose connections are secure and free from leaks.
2. Check that all hand valves are closed.
3. Connect the exit hose to the drain on the floor.
4. Check and drain the tank and distillate container if it contains any leftover
mixture from previous experiments.
5. Release pressure or flush trapped air or vapor.
6. Switch on the breaker.
7. Switch on the master switch.
Experimentation:
1. Prepare 5L test mixture of ethanol and water – 4L water and 1L ethanol.
Determine the specific gravity of the solution and note it.
2. Fill the evaporator with the test mixture.
3. Supply the condenser with cooling water and set the flow rate to 160L/hr.
4. Switch on the heater.
5. Set the T13 temperature.
6. Set the reflux ratio to 100.
7. After the first drop of distillate in the top product container, run the system for
10 mins to ensure that the system is in steady state.
8. Set the reflux ratio assigned to each group.
9. Collect all distillate from tank 5 every 5 minutes then measure the volume and
specific gravity using pycnometer for a 25-minute period analysis. Record the
temperature at which the density is taken.
10. Determine the concentration of distillate samples using its specific gravity.
 11. Collect all measured distillates and measure the volume and specific gravity to
compute for the concentration.
12. Turn off the heater to allow the system to cool down to 50oC or until there are
no vapor in the glass window of the evaporator.
13. Return all collected distillate samples to the evaporator.
14. Measure again the specific gravity of the sample from the evaporator (It should
be equal to the previous specific gravity of the original solution).
15. Repeat steps 5-11 using the second assigned temperature-reflux ratio
combination.

Shutdown:
1. Turn off the heater and the reflux divider button
2. Switch off the system at the master switch.
3. Shut off the water supply.
4. Allow the system to cool down to room temperature.
5. Remove the hose connections.
6. Drain the bottom tank and distillate container.
7. Close all the hand valves.
8. Switch off the breaker.

The temperature and reflux ratio assignments are as follows:

Group No. First Run Second Run

Temperature Temperature of
Reflux Ratio Reflux Ratio
of T13 T13

2 60oC 30 75oC 50

1 65oC 40 70oC 45

3 70oC 45 65oC 40

4 75oC 50 60oC 30
IV. DATA SHEET
1ST RUN:
Reflux Ratio:
Assigned T13:
Mass of empty pycnometer:
Volume of pycnometer:
Mass of pycnometer with ethanol solution:
Initial Specific Gravity:
Temperature at which density was taken:
Time (min.) Mass of Temperature Specific Gravity Concentration of
pycnometer with at which of Distillate Distillate
sample density was
taken
5
10
15
20
25

2ND RUN:
Reflux Ratio:
Assigned T13:
Mass of empty pycnometer:
Volume of pycnometer:
Mass of pycnometer with ethanol solution:
Initial Specific Gravity:
Temperature at which density was taken:
Time (min.) Mass of Temperature Specific Gravity Concentration of
pycnometer with at which of Distillate Distillate
sample density was
taken
5
10
15
20
25

V. TREATMENT OF RESULTS

1. Determine the weight percent of ethanol in the distillate for all the samples using the
specific gravity.
2. Plot the concentration of ethanol against time. NOTE: Do not include the initial
distillate, final distillate, and bottoms product in the plot.
3. Obtain the percent recovery of ethanol.
VI. QUESTIONS

1. Based on your results, is batch distillation effective on a small amount of sample base
on the purity of the final distillate? Support your answer with the data you obtained.
Will doing flash distillation instead provide us a higher yield theoretically?
2. Do you think having a higher concentration of ethanol in the feed would result to a
more concentrated distillate? Why? Why not?