FACULTY OF ENGINEERING

SCHOOL OF CHEMICAL AND ENERGY ENGINEERING

UNIVERSITI TEKNOLOGI MALAYSIA

SKKC 3761
SEPARATION PROCESSES LABORATORY II

Experiment 7 – CLIMBING FILM EVAPORATION

Lab Instructor Dr Hashim Bin Hassan

Group Number 5

Group Members Sharmeendran A/L Muniandy A15KK0142

Muhammad Aiman Bin Mohd Kamal A15KK0220

Muaz Bin Zakaria B16KT0002

Tay Zhi Xin A15KK0164

Section 02

Date of Experiment 24th October 2018

Date of Submission 31st October 2018

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ABSTRACT

Evaporation is a type of separation technique where it removes a liquid by boiling or

vaporizing off some of the liquid in the feed. In this experiment, climbing film evaporator was
used to separate the sugar and water from the sugar solution under single-effect evaporation. There
were two objectives in this experiment which were to study the effect of operating temperature on
the concentration profile of sugar solution and also the effect of feed flowrate on the final
concentration of sugar solution. The sugar solution was prepared by dissolving 1 kg of sugar in 10
litres of water and served as the feed in the evaporator to undergo evaporation. Valves were closed
every 5 minutes to collect the products at each different operating temperature, while every 5
minutes for 30 minutes for each feed flow rate to determine the refractive indices of the solutions.
The results were then compared to the theoretical values from references to obtain the
concentration profile of the sugar solution product. It showed that concentration of the sugar
solution increased when operating temperature increased. However, the concentration of sugar
solution decreased when feed flow rate increased. The results were tabulated and graphs were
plotted following with discussions. Some experimental errors and precaution steps were also
mentioned in this report.
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TABLE OF CONTENTS

CHAPTER TITLE PAGE

TITLE PAGE i
ABSTRACT ii
TABLE OF CONTENTS iii

1 INTRODUCTION 1
1.1 Background of Experiment 1
1.2 Objectives 2
1.3 Scope of Experiment 3

2 LITERATURE REVIEW 4
2.1 Introduction 4
2.2 Evaporation process 4
2.3 Factors Affecting an Evaporation Process 6
2.4 Types of Evaporator 7
2.4.1 Open Kettle or Pan 7
2.4.2 Horizontal-tube Natural Circulation Evaporator 7
2.4.3 Vertical-tube Natural Circulation Evaporator 7
2.4.4 Falling Film Type Evaporator 8

3 METHODOLOGY 9
3.1 Equipment 9
3.2 Materials 9
3.3 Experimental Procedures 9
 iv

4 EXPERIMENTAL RESULTS 11
4.1 Results of Concentration of Sugar Solution versus 11
Operating Temperature
4.2 Results of Concentration of Sugar Solution versus Feed 12
Flowrate

5 DISCUSSION 14

6 CONCLUSION 16

REFERENCES 17

APPENDICES 18
 1

1.0 INTRODUCTION

1.1 Background of Experiment

Evaporation is a type of vaporization that occurs on the surface of a liquid as it changes

into the gas phase after reaching its boiling point. It involves removal of volatile solvent from an
aqueous solution consisting of non-volatile solute by vaporization, in a vessel known as
evaporator. Evaporation process begins with a liquid product and ends up with a more concentrated
liquid as the main product. In some cases, the evaporated, volatile component is the main product,
for instance in water desalination the vapor obtained by the evaporation process are condensed and
used for drinking purposes. Similarly, the water that contains minerals is evaporated to obtain solid
free water which can then be used in boilers.

Evaporation is conducted by vaporizing a portion of the solvent to produce a concentrated

solution or a thick liquor. Evaporation differs from drying in that the residue is a liquid that
sometimes a highly viscous one rather than a solid; it differs from distillation in that the vapor is
usually a single component, and even when the vapor is a mixture, no attempt is made in the
evaporation step to separate the vapor into fractions; it differs from crystallization in that emphasis
is placed on concentrating a solution rather than forming and building crystals.

There are different types of evaporators such as batch fan evaporators, falling film tubular
evaporators, rising film tubular evaporators, natural circulation evaporators, forced circulation
evaporators, and falling film tubular evaporators. Feed enters the bottom of the heating tubes and
vaporization begins at that height within the tubes where the liquor temperature exceeds the boiling
temperature at the existing pressure. As the liquor moves up inside the tubes, the liquor starts rapid
boiling and additional vapor is produced and the velocity of the liquid-vapor mixture increases.
The vapor-liquid mixture then enters to the cyclone separator where they are separated.

Industry accounts for more than one-third of all types of energy used in the world. In order
to reduce energy consumption and environmental impact, developing high efficient devices are
 2

necessary for the industry. Concentrating sugar/water solutions requires the biggest part of the total
energy consumption in sugar production. Evaporation is the mostly used process in sugar factories
and in fruit juice production. The heat and mass transfer processes take place in various devices
and procedures.

Falling film evaporators are widely used in chemical, pharmaceuticals and food industries
to concentrate the feed solutions. The thermal concentration by evaporation is commonly used for
liquid food (e.g. fruit juice, milk and sugar solutions) for three main purposes: to reduce the volume
and the weight of the product, to increase the stability of liquid food and as intermediate processing
in food industry. The boiling and evaporation effects on falling film evaporation make the study
of the mechanism more complex, because it is difficult to separate the two effects on film
evaporation when both occur in the film.

The flow of the juice through the tube with different concentration rates depends on the
sugar concentration of juice and this changes all the processing parameters continuously. To drive
the relations between heat transfer and evaporation parameters, there is a need for a mathematical
model, which requires to be supported with some experimental data. The conditions under which
evaporation is carried out in practice vary widely. The liquid to be evaporated may be less viscous
than water, or it may be so viscous that it will hardly flow. It may deposit scale on the heating
surface; it may precipitate in crystals; it may tend to foam; it may have a very high boiling point
elevation; or it may be damaged by the application of too high temperatures. This wide variety of
problems has led to considerable variation in the types of mechanical construction used.

1.2 Objectives

1) To study the effect of operating temperature on the concentration profile of sugar solution.

2) To study the effect of feed flowrate to the final concentration of sugar solution.
 3

1.3 Scope of Experiment

The main apparatus used in this experiment is climbing film evaporator. It is used to carry
out the evaporation of water from the sugar solution to concentrate the sugar solution. 9.1 wt% of
sugar solution is fed into the evaporator. Different operating temperature is set to investigate the
effect of operating temperature on the concentration of sugar solution product. For each of the
operating temperature set, the volume and refractive index of product samples of water and sugar
solution are taken after 5 minutes of evaporation process.

Besides, the same experiment is carried out at different feed flowrate to study effect of feed
flowrate on the final concentration of sugar solution obtained. The volume and refractive index of
product samples of water and sugar solution are measured at interval of 5 minutes for half an hour.
The outcome of the result is discussed by the data collected.
 4

2.0 LITERATURE REVIEW

2.1 Introduction

Evaporator is basically used widely in various process, including pharmaceuticals, food and
beverages, chemicals, pulp and paper, polymers and resins, inorganic salts, acids, bases and a
variety of other material. Evaporation is one of the process that can be used in order to concentrate
the solution. There are three methods always used in concentrating the solution which are reverse
osmosis (RO), evaporation and freeze concentration. Based on these three methods, evaporation
is the leading and earliest technology been used widely in various industry. There are various types
and variations of evaporators, and the best for its application based on the product characteristics
and desired results.

2.2 Evaporation process

In evaporation, the vapour from a boiling point solution is removed and a more
concentrated solution remains. In most of the cases, evaporation can be refers to the removal of
water from an aqueous solution. According to Monceaux and Kuehner (2009), evaporation can be
described as a process which involve the thermal energy in order to separate the substances, which
the concentration of targeted solution is increased which caused by the separation of volatile
component such as water in the original solution. Based on the difference in vapour pressure
between the components, the volatile phase (water) is removed.

In evaporation process, evaporator is the device used to aid the process. The basic principle
of evaporator is simple, which remove water from a solution or slurry through evaporation process.
Evaporator is different from dryer because the concentrate discharge from evaporator is always in
liquid phase. While, the discharge from a dryer is in solid form, usually a flowable powder or meal.
The feed to an evaporator is always in liquid phase and still in liquid form even after the water is
evaporated.
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The physical process of evaporation need the input of energy in form of heat in order to
convert a liquid into vapour. Since most of the evaporators use the method of evaporation to
remove water, so it is must for the evaporators have a source of heat to operate its system. The
heat source for most of the evaporators is water vapour, either in the form of boiler steam or waste
vapour from other processes. Besides that, evaporators require a means to transfer heat energy
from the heat source into the evaporator liquid. Most of the evaporators use a tubular heater known
as shell and tube heat exchanger for this purpose. In the shell part, water vapour is condensed on
the outside of the tube which giving up its heat energy. The evaporator liquid, which is inside the
tubes, absorbs the heat given up by the water vapour. Increasing in heat cause the water in the
evaporator liquid to boil and produce bubbles of water vapour in the liquid. When these bubbles
reach the surface of the evaporator and burst, the escaping water vapour carries some of the
evaporator liquid with it.

Some examples of evaporation are concentration of aqueous solution of sugar, sodium

chloride, sodium hydroxide, glycerol, glue, milk and orange juice. For these cases, the
concentrated solution is the desired product and the evaporated water is usually neglected.
 6

2.3 Factors Affecting an Evaporation Process

The physical and chemical properties of the solution being concentrated and the vapour
being removed depends mainly on the type of evaporator used besides the pressure and
temperature of the process. Several properties which affect the evaporation process is describe
below.

1. Concentration in the Liquid

The liquid feed to an evaporator is usually dilute, means low in viscosity, similar to that of
water and relatively high heat-transfer coefficient are achieved. As evaporation proceeds, the
solution may become very concentrated and quite viscous which lead to the mark drop in the heat-
transfer coefficient.

2. Solubility

When the solutions are heated and the concentration of solute increases, the solubility limit
of the material in solution may be exceeded and crystals may form. This can limit the maximum
concentration in solution which can be obtained by evaporation. Most of the time the solubility of
the salt increases with temperature. So, during hot temperature, concentrated solution from an
evaporator is cooled to room temperature and this can cause crystallization.

3. Pressure and Temperature

The boiling point of the solution is related to the pressure of the system. The higher the
operating pressure of the evaporator, the higher the temperature at boiling. Furthermore, as the
concentration of the dissolved material in solution increases by evaporation, the temperature would
rise. In order to keep the temperatures low in heat-sensitive materials, it is must to operate under
1 atm pressure which is under vacuum.
 7

2.4 Types of Evaporator

In evaporation, the type of equipment used depends on the configuration of the heat-
transfer surface and on the means employed to provide agitation or circulation of the liquid. The
general types of equipment are discussed below.

2.4.1 Open Kettle or Pan

Known as the simplest evaporation which consists of an open pan or kettle which the liquid
is boiled. The heat is supplied by condensation of steam in a jacket or in coils immersed in the
liquid. This type of evaporator is inexpensive and simple to operate but the heat economy is poor.

2.4.2 Horizontal-tube Natural Circulation Evaporator

Relatively cheap evaporator and suitable for non-viscous liquids with high heat-transfer
coefficients and liquids that do not deposit scale. It is unsuitable for viscous liquids since poor in
liquid circulation. Figure 2.1 below shows the diagram of this type of evaporator.

2.4.3 Vertical-tube Natural Circulation Evaporator

In this type of evaporator, vertical rather than horizontal tubes are used. The liquid is inside
the tubes while the steam condenses outside the tubes. The liquid rises in the tubes by natural
circulation because of boiling and decreases in its density. This type of evaporator is not suitable
for viscous liquids. Figure 2.2 below shows the diagram of this type of evaporator.
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Figure 2.1: Horizontal-tube type

Figure 2.2: Vertical-tube type

2.4.4 Falling Film Type Evaporator

The liquid is fed to the top of the tubes and flows down the walls as a thin film. Usually,
the separation of vapour-liquid happens at the bottom part. This type of evaporator is suitable for
concentrating heat-sensitive materials such as orange juice and other fruit juices. This is because
the holdup time is very small around 5 to 10 s, besides having high in the heat-transfer coefficients.
 9

3.0 METHODOLOGY

3.1 Equipment

Climbing film evaporator, 250mL measuring cylinders, collecting jars, refractometer

3.2 Materials

1kg of sugar, 10L of water

3.3 Experimental Procedures

At the beginning of experiment, 9.1% of sugar solution was prepared by dissolving 1kg of
sugar in 10L of water. Before starting the experiment, every equipment was ensured to be in place
as well as in good condition. Firstly, V7 and V9 valve were opened and V1, V8 and V10 valve
were closed. The switch of steam boiler was turned on. After this, the capacity of feeding pump
was adjusted to 40% to manipulate the feed flowrate at 6.48 L/hr and the operating temperature
was set at 115°C. After the boiler pressure increased to 5.4 bar which is indicated by the red line
on the gauge, the feeding pump was turned on. The vacuum pump was switched on in order to
speed up the evaporation process.

Next, the product sugar solution and water condensed were collected separately by adjusting
the position of the valves. For collecting the product sugar solution sample, V7 was closed and V8
was opened simultaneously. At the same time, V9 was closed and V10 was opened simultaneously
to collect the condensed water sample. Then, the volume and refractive index of the collected
product were measured. The valve controlling steps (V7, V8, V9, V10) were repeated every 5
minutes and the data collected was recorded. The same steps were repeated for 60% and 80%
feeding pump capacity which represent 9.72L/hr and 12.96L/hr respectively. After this, the
 10

experiment was continued by adjusting different operating temperature such as 105°C, 110°C and
115°C. The product sugar solution sample and condensed water sample were collected after 5
minutes for each temperature adjusted. The volume and refractive index of the collected product
were measured and recorded.
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4.0 EXPERIMENTAL RESULTS

4.1 Results of Concentration of Sugar Solution versus Operating Temperature

Feed flowrate set: 8.1L/hr (50% of the full capacity of the feeding pump)

Table 4.1: Experimental results of concentration of sugar solution with the changes of operating
temperature

Volume Sugar Solution Obtained

Volume
Operating of Sugar Refractive Index of
of Water Concentration
Temperature Solution Water Obtained Refractive
Obtained of Sugar
(°C) Obtained (nD) Index
(mL) Solution
(mL) (nD)
Obtained (%)
105 490 96 1.33295 1.34908 10.495
110 284 316 1.33296 1.35476 14.037
115 260 310 1.33296 1.36123 18.071

Concentration of Sugar Solution vs Operating Temperature

20
Concentration of sugar solution

18
16
14
12
10
(%)

8
6
4
2
0
104 106 108 110 112 114 116
Operating Temperature (°C)

Figure 4.1: Graph of concentration of sugar solution versus operating temperature

 12

4.2 Results of Concentration of Sugar Solution versus Feed Flowrate

Operating temperature set: 105°C

Full capacity of the pump: 16.2L/hr

Table 4.2: Experimental results of concentration of sugar solution with the changes of feed
flowrate
Volume Refractive
Volume Sugar Solution Obtained
Feed of Sugar Index of
Time of Water
Flowrate Solution Water
(min) Obtained Refractive Concentration
(L/hr) Obtained Obtained
(mL) Index (nD) (%)
(mL) (nD)
6.48 5 391 89 1.33295 1.34385 7.234
10 378 86 1.33295 1.34789 9.753
15 384 83 1.33296 1.34848 10.121
20 358 82 1.33295 1.34896 10.421
25 364 80 1.33296 1.34928 10.620
30 394 81 1.33293 1.34947 10.739
9.72 5 630 62 1.33297 1.34807 9.866
10 584 72 1.33297 1.34809 9.878
15 500 73 1.33297 1.34825 9.978
20 645 64 1.33297 1.34838 10.059
25 615 62 1.33298 1.34855 10.165
30 590 72 1.33298 1.34855 10.165
12.96 5 914 82 1.33302 1.34783 9.716
10 867 62 1.33297 1.34781 9.703
15 888 66 1.33298 1.34775 9.666
20 890 64 1.33297 1.34796 9.797
25 882 64 1.33297 1.34792 9.772
30 826 62 1.33297 1.34798 9.809
 13

Final Concentration of Sugar Solution vs Feed Flowrate

Final Concentration of Sugar Solution (%) 10.8

10.6

10.4

10.2

10

9.8

9.6
0 2 4 6 8 10 12 14
Feed Flowrate (L/hr)

Figure 4.2: Graph of final concentration of sugar solution versus feed flowrate
 14

5.0 DISCUSSION

Before starting the experiment, the sugar solution feed was prepared by dissolving 1 kg of
sugar in 10 litres (10 kg) of water to achieve a concentration of 9.1 percent by weight. The graph
in Figure 4.1 shows the final concentration of sugar solution against operating temperature. It
illustrated that the concentration of sugar solution increased when the operating temperature
increased. This is because of the increasing temperature had led to a higher heat transfer rate. Since
more heat had transferred to the feed, evaporation occurred faster. A higher evaporation rate caused
more water being evaporated and then condensed, resulting in a more concentrated sugar solution.

The data shown in Table 4.1 supports the explanation above. The table data shows that a
greater volume of water was collected at high operating temperature because more water has
evaporated. Meanwhile, the volume of sugar solution obtained decreased when the operating
temperature increased, indicating that the concentration of sugar solution increased along the
operating temperature. This followed the material balance equation which is

F= L + V
where F = flow rate of feed
L = flow rate of sugar solution (concentration liquid)
V = flow rate of water (vapor)

Therefore, the volume of sugar solution collected at a fixed flow rate of feed will decrease if the
volume of water increased.

The graph in Figure 4.2 shows the final concentration of sugar solution against the feed
flow rate. The trend of graph shows that the concentration of sugar solution decreased when feed
flow rate increased. This is because when feed flow rate increased, the residence time of the feed
in the evaporator decreased, which means that the feed had lesser exposure time to the heat
provided by the steam. Hence, the rate of evaporation was lower when the feed flow rate was
higher. This can also be proven from the data in Table 4.2 which shows that a higher volume of
sugar solution and a lower volume of water were obtained when the feed flow rate was higher. It
 15

can be explained that when the evaporation rate was lower, the water evaporated and condensed
was lesser, while most of the water was still retaining in the sugar solution thus causing a lower
final concentration of sugar solution was obtained. Apart from that, from the results data collected,
it also shows that the water distillate collected from both experiments was relatively pure as the
refractive index was in the range between 1.33293 and 1.33302 which corresponded to its
theoretical value, 1.333.

Although the both experiments were considered successful, it was observed in the results
that there were some volume losses after the evaporation process. This was because of some errors
occurred when conducting the experiments. First, the solution was unable to be drained out
completely from the evaporator. Besides, the valves were not closed on time during every 5
minutes to collect the products. There was also parallax error when students were reading the scale
on the measuring cylinders. Besides, there might be some solution still left in the beaker after
transferring to the measuring cylinder.

There are some precaution steps and recommendations to be taken in order to reduce the
errors, which are:
a) Evaporator should be cleaned before experiment starts to avoid any impurities.
b) The eyes of observer should be perpendicular to the scale of the measuring cylinder when
taking readings.
c) The student assigned to turn off each valve should be the same person as different
individual has different time of reaction.
d) Experiments with more sets of different operating temperatures should be carried out to
further determine the trend of the results.
e) Experiments should be repeated to obtain the average readings for the volume of the
products.
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5.0 CONCLUSION

The technique used to separate both sugar and water in this experiment was evaporation
technique and the apparatus used was the double effect evaporator. The objectives of this
experiment were to study the effect of operating temperature on the concentration profile of sugar
solution and the effect of feed flowrate on the final concentration of sugar solution. Based on the
results and analysis, it was concluded that when operating temperature increased, the concentration
of the sugar solution also increased. A higher volume of water and a lower volume of sugar solution
were collected as operating temperature increased. Besides, when feed flow rate increased, the
concentration of sugar solution decreased. A higher volume of sugar solution and a lower volume
of water were also obtained.
 17

REFERENCES

1. Geankoplis, C.J. (2014). Transport Processes & Unit Operations, 4th edition, Pearson
Education Limited.
2. Weast, R. C. (1984). Handbook of Chemistry and Physics, 64th edition, CRC Press.
3. Monceaux, D. A., &Kuehner, D. (2009). The Alcohol, 5th edition, Lallemand Ethanol
Technology and Nottingham University Press, United Kingdom.
4. Miyawaki, O., Liu, L., Shirai, Y., Sakashita, S., &Kagitani, K. (2005). Tubular ice system
for scale-up of progressive freeze-concentration.J. Food Eng. 69(1): 107–113.
5. Badger, L. W., &BancheroJ. T. (1955). Introduction to Chemical Engineering, McGraw-
Hill, New York.
6. Perry, R. H., & Green, D. (1988). Perry’s Chemical Engineers’ Handbook, 6th edition,
McGraw-Hill.
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APPENDICES

Appendix A: Temperature of different parts of evaporation system when collecting the product
samples

Figure 7.1: Schematic diagram of climbing film evaporator

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Table 7.1: Temperature of different parts of evaporation system for different feed flowrate
adjusted when collecting the product samples
Temperature (°C)
Feed Flowrate Time (min)
TT1 TT2 TT3 TT4 TT5 TT6 TT7 TT8
5 26.9 97.3 98.2 28.5 28.0 29.4 103.0 28.0
10 26.9 97.3 98.4 28.7 28.0 29.3 104.3 28.0
15 27.0 97.4 98.4 28.8 28.0 29.2 104.9 28.2
40%
20 27.1 97.4 98.3 29.1 28.0 29.5 104.5 28.5
25 27.1 97.3 98.4 29.2 28.0 29.3 103.0 28.6
30 27.2 97.4 98.3 29.3 28.1 29.2 105.0 28.7
5 27.4 97.2 98.1 29.2 28.1 28.8 104.5 29.3
10 27.7 97.3 98.3 29.3 28.2 29.0 104.6 29.5
15 27.8 97.2 98.4 29.5 28.2 29.1 103.9 29.4
60%
20 27.7 97.2 98.4 29.9 28.2 29.1 104.4 29.5
25 27.8 97.3 98.4 29.8 28.2 29.1 104.9 29.6
30 28.0 97.3 98.4 29.9 28.2 28.9 105.0 29.7
5 28.0 97.2 98.1 29.8 28.3 29.6 105.0 30.0
10 28.0 97.2 98.2 29.8 28.3 29.5 104.7 30.2
15 28.0 97.2 98.2 29.9 28.3 29.6 104.8 30.2
80%
20 28.0 97.2 98.2 29.9 28.3 29.5 104.7 30.2
25 28.0 97.2 98.2 29.9 28.3 29.5 104.6 30.2
30 28.0 97.2 98.2 29.9 28.3 29.5 104.4 30.2
 20

Table 7.2: Temperature of different parts of evaporation system for different operating
temperature (TT7) adjusted when collecting the product samples
Operating Temperature (°C)
Temperature
TT1 TT2 TT3 TT4 TT5 TT6 TT8
(°C)
105 28.3 97.3 98.4 29.5 28.4 29.9 29.3
110 28.3 97.1 98.4 29.5 28.4 30.3 29.6
115 28.5 97.2 98.4 29.5 28.4 29.7 29.7
 21

Appendix B: Concentration of sugar solution with respect to the refractive index

Table 7.3: Refractive index for sugar concentration

Sugar Concentration (%) Refractive Index (nD)
0 1.3330
5 1.3403
10 1.3479
15 1.3557
20 1.3639
25 1.3723
30 1.3811
35 1.3902
40 1.3997
45 1.4096
50 1.4200
55 1.4307
60 1.4418
65 1.4532
70 1.4651
75 1.4774
80 1.4901
85 1.5033
 22

Sugar Concentration vs Refractive Index

35

30 y = 623.54x - 830.71
Sugar Concentration (%)

25

20

15

10

0
1.33 1.34 1.35 1.36 1.37 1.38 1.39
Refractive Index (nD)

Figure 7.2: Graph of sugar concentration versus refractive index

Sample calculation:

The linear equation of the graph plotted for sugar concentration versus refractive index is:

y = 623.54x - 830.71

For operating temperature of 105°C, the refractive index of sugar solution product is
1.34908nD. The sugar concentration with respect to 1.34908nD can be calculated by inserting the
value into the equation obtained from the graph.

y = 623.54 (1.34908) - 830.71

y = 10.495%

Thus, the concentration of sugar solution product is obtained, which is 10.495%. Same
equation is applied for calculation of concentration of other sugar solution products.