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Department of Chemical Engineering and Energy Sustainability

Faculty of Engineering

KNC 3221 CHEMICAL ENGINEERING LABORATORY

Guided Laboratory Report

Experiment 2 – Distillation

Semester II – Session 2018/2019

Name Matric No.


1. Anthonette anak James 55514
2. Khairul Izatul Izni Binti Mohd Zin 56294
3. Shathishkomar A/L Ramesh 57831
4. Nur Farunita binti Mohamad 57217

Lecturer:
1. En Mohd Farid Atan

Submission Date: 11/04/2019

Bachelor of Engineering with Honours


(Chemical Engineering)
2018/2019
ABSTRACT

Distillation is defined as a process in which, by applying and removing heat, a liquid or vapor
mixture of two or more substances is separated into the component fractions of desired purity. A
mixture of 2L ethanol and distilled water was used in this experiment. This experiment was
conducted to differentiate the various power values and to study the relationship between the boil-
up rate with pressure drop and the degree of foaming inside the distillation column on trays. The
power was set to 900W, 1000W, 1100W and 1200W in order to observe the pressure drop in the
distillation column. The degree of foaming has been noticed with an increasing action with the
increase in power input to the equipment. Hence, the higher the heater power, the higher the boil
- up rates.

Keywords: Distillation, Boil up rate, Pressure drop, Foaming, Distillation column.


Table of Content

Topic Page

1.0 Introduction 1

1.1 Aim 1

1.2 Objectives 1

1.3 Problem statement 1

2.0 Literature review 1

3.0 Methodology 2

3.1 Experimental procedure 2

3.2 Equipment and material 4


3.3 Safety Procedure 4
4.0 Result and discussion 5

5.0 Conclusion and recommendation 8

6.0 References 8
1.0 INTRODUCTION

1.1 Aim
The aim of the experiment is to study the relationship between the boil-up rate with pressure
drop and the degree of foaming on trays.

1.2 Objective
The objectives of the experiment are
I. To observe the outcomes affected by the operating parameters.
II. To study the effect of different values of power on the pressure drop and degree of
foaming on trays in the distillation column.

1.3 Problem Statement


The distillation process is essential in chemical processes as it aids in separating the compounds
according to their boiling point (Helmenstine, 2019). As the liquid runs down the tower, vapor
will be rising. What happens to the boil-up rate and pressure drop upon heating a fluid in a
distillation column when a different power is exerted to the boiler?

2.0 LITERATURE REVIEW

According to Green (2018), distillation is a widely used technique to characterize


materials by setting an index of purity and separating selected components from a complete
matrix in chemical analysis. Distillation is the process that occurs when a liquid sample is
volatilized to produce a vapor that is condensed in the more volatile components of the original
sample to a liquid richer. The liquid mixture to be processed is known as the feed, according
to and this is usually introduced somewhere close to the middle of the column to a tray known
as the feed tray (Tham, 2016). The position of the feed divides the column into the top or
rectification section and the bottom section or also known as the section of stripping.
In traditional chemical engineering approach, distillation columns are the fundamental
unit operations mainly in the oil and gas industry. Distillation takes advantage of this by
bringing into contact phases of liquid and gas at temperatures and pressures promoting the
desired separation. The components with lower volatility typically have a lower boiling point
which will preferably move into the liquid phase during this contact meanwhile, more volatile
components move into the vapor phase. The distillation column can separate a mixture
composed of two compatible liquids. In order to operate the distillation column, one of the
dynamic elements is the pressure variation in which it was necessary to regulate. According to

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Nguyen and Moonyong (2014), pressure affects the distillation performance in a complex way
in which it affects the relative volatility between components, molar vapor flow rates, flood
limitations, and vapor density. In addition, Kister (1992) reported that one of the favorable
effects of increasing the pressure column is that it increases vapor density and capacity to
handle vapors.
Many of the studies were conducted to understand the correlation in the distillation
column between boil up rate and pressure drop. Therefore, Mauricio-Iglesias et al. (2014) are
conducted a simulation test to study the pressure drop effect on the boil-up rate by increasing
the feed flow rate by manipulating the 2-propanol from aqueous. The results showed that the
increase in the boil-up rate leads to a higher pressure drop.
The simple distillation principle is the physical process is used to separate chemicals
from the mixture by the difference in which they easily vaporize because do not interact with
each other and differ in their boiling point. Hence, the raw materials used for this experiment
are ethanol and distilled water, both of which have different characteristics. Ethanol has a
boiling point of 78.2 ᵒC — 78.5 ᵒC whereas distilled water has a boiling point of 100 C.
therefore, both of them have different characteristics such as boiling point.
The expansion of the liquid in a distillation column provides high interfacial contact
between liquid and vapor. Although one of the least common causes of malfunctions in the
distillation column, foaming may increase in a process called entrainment until the fluid in one
tray mixes with the liquid on the above tray. According to Yirka (2017), foaming can be caused
by the passage of vapor or gas in a distillation column due to too high gas velocity or too fast
evaporation rate. Hence, the presence of foam in packed columns results in a drop in high
pressure, a lack of transfer of mass and unexpected low capacity. When power increases, the
degree of foaming increases. In packed columns, the presence of foam results in a drop in high
pressure.

3.0 METHODOLOGY

3.1 Experiment Procedure

1. The Instructional Manual in the Standard Operational Procedure (SOP) is read.


2. 10 L solution of diluted ethanol, C2H5OH is prepared by diluting accurately 2L of pure
ethanol with 8L of distilled water. This is to obtain a total volume of 10L for the
distillation process.

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3. The reflux ratio timer on the console is switched “OFF” as the unit operation is set at
total reflux.
4. All valves are ensured to be closed.
5. V10 on the reflux pipe is opened.
6. Through the filter cap provided on the reboiler, the 10L of prepared solution is added
directly to the reboiler. *The filter cap on the reboiler is ensured to be replaced
firmly so that it is fully closed the reboiler.
7. The power to the control panel is turned on.
8. The temperature in the reboiler, T9 is set to 85°C. The temperature is set between the
boiling point of ethanol, 78°C and the boiling point of water, 100°C.
9. The valve V5 is opened until the cooling water flow rate F11 to the condenser is
approximately 3 L/min. (The 3L/min is the maximum flow rate that the cooling
water can be supply from the water pipe).
10. On the control panel, the power controller of the reboiler heating element is turned on
fully (anti-clockwise) and the heating element is turned “On” to “Power On” position.
11. The power controller is turned in a clockwise direction until the reading is mentioned
approximately at 0. 75 kW on the digital wattmeter. The warm-up temperature of the
reboiler content is read at readout meter. (The boiler heater power controller on the
control panel is adjusted up to a maximum of 1.0 kW due to the limitation of the
power supply).
12. V6 and V7 that connected the base and top of distillation column are opened. No
pressure difference in the column initially. V6 and V7 are closed.
13. The sieve plates of the 1 st and 5th plates in the column sections are observed. The
appearance of these trays was taken notes throughout the distillation process.
14. The rise up of vapor in the column can be seen and observed. This might due to the
increment of temperature on the temperature selector T8, T7, T6, T5, T4, T3, T2,
and T1. The vapor entered the condenser and reappeared as droplets into the glass-
walled distilled receiver vessel (11). The distillate builds up a small level in the
receiver vessel and went to the reflux regulator valve as it overflow (12) or returned
to the column as the valve is not “On” (on the control panel) and run under total reflux.
15. The cool distillate is returned to the top of the column and went down the trays forming
a liquid level on the trays and bubbling of vapor passing through the liquid. As
temperature T1, T2, T3, T4, T5, T6, T7, and T8 are constant the system is then reached
an equilibrium condition.
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16. The boil-up rate is measured by performing a timed volume collection. All the
condensate is diverted into a measuring cylinder as the V3 is opened. The time
required to collect the set quantity is recorded using a stopwatch. (The volume
collected is measured for every trial (900W, 1000W, 1100W and 1200W) to get
consistent results).
17. The reading of pressure drops over the rectifying (top) and the stripping (bottom)
sections is taken by opening valve V6 and V7 on the manometer after the samples are
taken. (V6 need to be opened first before V7 to prevent vapor from the column
entering the manometer. Pressure drops reading is taken after the valves are fully
closed).
18. The valves are closed after the pressure drop reading is taken.
19. These readings are repeated until two in a row agree fair closely. Each measurement
is set 10 minutes in between before the next set is started in order for the system to
reach equilibrium again.
20. The boiler heater power controller (on the control panel) is adjusted to step up the
boil-up rate in 100 W increments. (The power supply cannot supply the energy up to
a maximum of 1.5 kW. Thus, the experiment only did to 100 W). The column is
stabilized in 10 minutes, the boil-up rate and pressure drops are taken.
21. The shut-down procedure following in the SOP is performed after all experiment was
done.

3.2 Equipment/Materials
Equipment: Distillation Column Unit
Apparatus: Stopwatch
Materials: 1) 2L of pure ethanol, C2H3OH
2) 8L of Distilled Water

3.3 Safety Precautions


1. Flammable substances must be properly stored and handled.
2. Personal Protective Equipment (PPE) such as safety goggle, gloves and face mask are
worn during conduction the experiment.
3. The unwanted chemical is disposed of safely.
4. Do not touch the hot components of the unit.

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4.0 RESULTS AND DISCUSSION

The Taverage is calculated as the following formula:


T1+T2+T3+T4+T5+T6+T7+T8
Taverage = (1)
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The boil-up rate is calculated based on the following formula:
l volume(ml) l 60min
Boil up rate, = × × (2)
hr time(min) 1000ml hr
Example Volume = 100 ml = 0.1 L
The formula to calculate the pressure drop:
Pressure drop ( cm H 2O ) = Highest – Lowest (3)

Table 4.1 Data collection for the temperature at the distillation column
Power T1 T2 T3 T4 T5 T6 T7 T8 T9 T avg
(W) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C)
900 77.9 78.5 78.7 78.3 79.2 79.0 79.9 80.0 88.7 78.9
1000 78.1 78.3 78.9 78.4 80.0 80.3 80.4 80.1 89.0 79.3
1100 79.6 79.5 80.0 79.6 81.8 81.2 81.9 82.4 90.1` 80.8
1200 80.1 80.7 80.9 80.6 83.1 85.9 88.1 88.6 90.9 83.5

Table 4.2: The effects of boil-up rate and pressure drop of the distillation column.
Power Boil up Pressure Observation on the trays of the distillation column
(W) rate drop
(L/hr) (cm
H2O)
900 1.32 83 Bubbles are present up until the third tray. The water
circulated in a vigorous mode at the bottom of the column.
1000 5.11 135 Foaming energetically over the upper part of the trays but not
fully filled the trays.
1100 9.23 200 Foaming violently all over the trays until the upper part of the
trays. More bubbles are formed
1200 14.33 230 Vigorous water bubbles present in all trays. The water moves
until the upper section of the distillation column. The bubbles
formation is higher than when setting the pressures to 900,
1000 and 1100 W.

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Boil-Up Rate Against Average Temperature
16 y = 2.5919x - 201.48
14 R² = 0.9356

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Boil-up rate (L/hr)

10
8
6
4
2
0
78 79 80 81 82 83 84
Temperature average (°C)

Figure 4.1: The relationship between boil-up rate and the average temperature in the
distillation column.

Boil-Up Rate Against Pressure Drop


16
14 y = 0.0831x - 5.9581
R² = 0.9615
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Boil-up rate (L/hr)

10
8
6
4
2
0
0 50 100 150 200 250
Pressure drop (cm H2O)

Figure 4.2: The correlation between boil-up rate with the pressure drop of the distillation
column

Table 4.1 shows the temperature readings in the distillation column. The Temperature reading
T1 to T8 is the temperature on the top and bottom distillation column, temperature T9 is the
temperature in the heater and T avg is the temperature average of temperature T1 – T9. Table
4.2 shows the pressure drop between the top and bottom column, the boil-up rate and the

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observation on the trays of the distillation column. The data and observation were obtained
based on different power inputs of the heater which is 900, 1000, 1100 and 1200 W. Figure 4.1
shows the boil up rate against the average temperature of the distillation column. The violet
line indicates the power from 900 W to 1200 W. The dotted line indicates the linear line of the
violet line and represented by the equation y and the quadratic of the coefficient of correlation
R2. From the graph, it can be clearly seen that the boil up rate increases as the temperature
increases. There is a rapid increase in boil up rate at power 900 W to 1000 W with a temperature
increase of 78.9°C to 79.3°C. This is because the boiling point of ethanol is 78.3°C. Therefore,
the ethanol boils vigorously in this range of temperature. The bubbles are present until the third
tray only as the average temperature is not sufficient to evaporate ethanol on the first and
second tray. From temperature 79.3°C to 80.8°C, the boil up rate increases gradually because
the ethanol has already started boiling from the previous temperature difference. From
temperature 80.8°C to 83.5°C, the boil up rate increases slowly as most of the ethanol would
have been evaporated by this temperature. The R² value is 0.9356 which is near to 1. This
proves that the boil up rate increases as the temperature increases.

Figure 4.2 shows the pressure drop against the boil up rate for 4 power intensities. The
red line indicates the power from 900 W to 1200 W. The dotted line indicates the linear line of
the red line and represented by the equation y and the quadratic of the coefficient of correlation
R2. The trend of the graph gradually increases and that increases rapidly as the temperature
increases. The gradual increase of the boil up rate against the pressure drop is shown when the
pressure drop is from 83 to 200 cm H2O. The value of the pressure drop is slightly smaller
which shows that a small amount of vaporized ethanol starts to rise to the upper part of the
distillation column. There is only a small amount of vaporized ethanol although the temperature
reached above the boiling point of ethanol due to the heat loss to the surrounding from the
distillation column due to the absence of the insulator which is the aluminum foil. The rapid
increase of boil up rate can be seen from pressure drop 200 to 230 cm H2O. This is due to the
presence of the insulator to cover the distillation column which accumulates more heat energy
that caused more ethanol to boil and move upwards creating a big difference in pressure as
more vapor is in the upper part and more liquid in the lower part of the distillation column. The
R² is 0.9615 which is near to 1. Therefore, it proves that the pressure drop increases the boil up
rate.

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5.0 CONCLUSION AND RECOMMENDATION
From this experiment, it can be observed that the boil-up rate is increasing linearly to
both temperature and pressure drop as shown in the graph of Figure 4.1 and 4.2. Plus, it can
be observed that an increase in power supply would increase the temperature in the distillation
column as well as the pressure drop. The bubble formation in distillation trays would increase
in foaming as the power increases. As a conclusion, the results obtained are acceptable to that
related theory. This experiment is recommended to make a repetition in order to get a more
precise result.

6.0 BIBLIOGRAPHY

Green, J. D. (2018). Distillation In Encyclopedia of Analytical Science (Second Edition) (pp.


281-285). Beverley, United Kingdom: Elsevier Inc.
Helmenstine, A. M. (2019). What is distillation? Chemistry definition. Retrieved April 5, 2019,
from ThoughtCo.: https://www.thoughco.com/what-is-distillation-601964
Kister, H. Z. (1992). Distillation design. New York, U.S.A: McGraw-Hill.
Mauricio-Iglesias, M., Bisgaard, T., Kristensen, H., Gernaey, K. V., Abildskov, J., & Huusom,
J. K. (2014). Pressure Control in Distillation Columns: A Model-Based Analysis. .
Industrial & Engineering Chemistry Research, 53(38), 14776-14787.
doi:10.1021/ie5017514
Nguyen, V. D. L., & Moonyong, L. (2014). Review of retrofitting distillation columns using
thermally coupled distillation sequences and dividing wall columns to improve energy
efficiency. Journal of Chemical Engineering of Japan, 47(2), 87-108.
Tham, M. T. (2016). Basic distillation equipment and operation,. Retrieved April 5, 2019 from
https://www.scribd.com/document/352130128/Basic-Equipment-and-Operation-of-
Distillation-Columns
Yirka, T. (2017). What causes foaming in a distillation column? Retrieved April 6, 2019 from
https://sciencing.com/causes-foaming-distillation-column-8697646.html