Department of Chemical Engineering

Faculty of Materials and Chemical Engineering

Lab Manual.

Chemical Engineering Lab II (Semester III)

Particle Technology

(CH251L)

GIK INSTITUTE OF ENGINEERING SCIENCES AND

TECHNOLOGY
TOPI

1
 Preface

This manual deal with the laboratory experiments, exercises and demonstrations related to the
3rd semester chemical engineering course Particle Technology (CH251) taught to the
students.

Instructions and information

Come to the laboratory well prepared and in time.
Please read through the sheets for the particular experiment from this manual.
Observe strictly the safety precautions for handling chemicals/materials and equipment, as
well as any instructions given by the supervisors.
The worksheet joined with each exercise should be initialled by one of the instructors during
the class, and handed in as instructed: either at the end of the class, or at the start of the next.
Only worksheets signed by the instructors will be considered for assessment. And please fill
in your names, reg # etc. legibly - we can't award marks anonymously.

Grading Policy
Worksheets/lab reports: 50%
Quizzes: 30%
Viva Voce 20%

Safety Precautions
Observance of Safety Rules and the use of common sense are essential in any Laboratory.
Instructions on the manipulation of chemicals or the use of instruments should be read, or
obtained from an instructor, and strictly observed.
As apprentices in a laboratory environment you should pay particular attention to the
following rules:
No food / drinks / smoking in the Lab.
Elementary discipline: No running, observance of instructions from the instructors, no
manipulation of instruments before being instructed, attention (without interference) to others
working in the same area, are mandatory.
Care should be taken when using compressed air and particulate materials.
Mechanical testing: keep well clear (and make sure that others are clear) of any operating
machine. Manual adjustments must never be attempted during a test.

Complement to the Safety Instructions

Dealing with Electrical Systems

Don’t ever stand on or try to pinch high power cables. This may destroy their insulation and
cause electrical shock.
Don’t switch on or off the power supply of any machine without prior permission from a lab
instructor.

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Don’t try to remove the casing or cover of any electrical circuitry, even if it is not in
operation.
In case of electrical shock immediately inform the lab instructor and/or precede according to
the first aid measures.

Working with Mechanical Systems

Never touch the moving parts of any machine when in operation.
Before operating any machine, first inquire about the emergency stop button of that particular
machine
Never cross the safety-clearance distance of any machine (particularly important for the
impact testing machine)
Never try to move and/or lift any machine by yourself, it may cause physical injury to you.
Whenever you are near any moving part of machine make sure you don’t have any loose
clothes in your dress,

Fire hazards and prevention

1. In case of fire, immediately call for help/instructor and inform the fire brigade at 2333
2. If help is not available immediately reach for nearest fire extinguisher, remove its lock/pin
and use it to extinguish fire.
3. Smoking is strictly prohibited in lab premises as it can cause fire.
4. Never use lighter or match near gas equipment (e.g. oxygen, hydrogen cylinders.) as it can
cause a serious accident in form of explosion.
5. Never use water to extinguish a fire in electrical apparatus.
6. Ensure that all additions to a bath of molten metal are completely dry

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Safety Information - Chemical Lab II (CH251)
Safe laboratory practice is based on understanding and respect, not fear. Your
instructors will discuss specific safety precautions relevant to each experiment during
laboratory lecture. Your laboratory manual will point out specific hazards and precautions.
Before beginning an experiment, be sure you have this information at hand and that you
understand it.

When you have read the following information carefully and feel you understand it, please
read and sign the Chemical Lab II (CH251) Safety Regulations Agreement. At the start of
your first lab session you will submit the signed Safety Agreement to the instructor. Only
then will you be permitted to begin laboratory work.

Safety Rules

1. Working alone in the laboratory is strictly forbidden.

2. Approved safety goggles and lab coats must be worn at all times when in a laboratory.
3. Students may only perform authorized experiments and then only at the assigned time.
4. Use every precaution to keep all chemicals off your skin and clothing, out of your
nose, mouth and eyes, and away from flames. It is strictly forbidden to eat or drink
anything (including water) in the laboratory.
5. Long hair and billowy clothing must be confined when in the laboratory. Shoes are
mandatory; sandals or open-toed shoes are not allowed. Shorts are not allowed.
6. All laboratory workers must know the location and proper use of all laboratory safety
equipment.
7. All accidents, including contact with chemicals, cuts, burns, or inhalation of fumes must
be reported to an instructor immediately.
8. It is your responsibility to read and abide by the "Laboratory Safety" section of the lab
manual and to keep it with you in the laboratory.
9. Laboratory equipment and work area must be cleaned after finishing work.
10. Failure to observe laboratory safety rules and procedures may result in injury to you or to
fellow students. For a first violation, you may be asked to leave the laboratory for the day,
while for repeated violations; you may be dropped from the course with a grade of F, at
the discretion of the instructor.
11. It is in your own best interest to stay alert and to be aware of possible hazards in the
laboratory. Do not hesitate to call unsafe practices by your colleagues to the attention of
the instructors.

Important phone numbers

FIRE SECTION 2333

MEDICAL CENTRE 2434

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 Chemical Lab II (CH) Safety Regulations Agreement

1. I have received and read the "Safety Information" document for the “Chemical Lab II
(CH251)” course I am taking this semester.
2. I agree to abide by these laboratory regulations and safety procedures at all times while
working in the lab.
3. I agree not to begin an experiment until I have studied and understood the purpose of the
experiment, the procedures involved, and any particular hazards associated with the
equipment and chemicals.
4. I agree that I will not work alone in the lab and will only perform experiments if the
laboratory instructor or another member of the Chemical Engineering faculty is present.
5. I understand that if I violate the laboratory regulations I may be asked to leave the
laboratory and (for repeated violations) dropped from the course with a grade of F.

Name: _________________________
Reg. #: _________________________
Group: ________________________

Signature: ______________________
Date: _________________________

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 Contents
Table of Contents
Preface ....................................................................................................................................... 2
Safety Information - Chemical Lab II (CH251)............................................................................ 4
Chemical Lab II (CH) Safety Regulations Agreement ................................................................. 5
List of Experiments..................................................................................................................... 7
Solid Handling Study Unit .......................................................................................................... 8
Sedimentation Study Unit ........................................................................................................ 15
Computerized Controlled Fluidized Bed Study Unit ................................................................ 19
Liquid Solid Mixing Unit ........................................................................................................... 32
Computerized Controlled Filtration Unit ................................................................................. 39
Oil Extraction Screw Press ...................................................................................................... 55

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 List of Experiments

Solid Handling Study Unit ................................................................................................. 8

Granulometric analysis by sieving ........................................................................................ 11
Milling: Ball mill ................................................................................................................... 13
Sedimentation Study Unit............................................................................................... 15
Effect of the initial concentration over the sedimentation characteristics ......................... 17
Effect of the initial height over the sedimentation characteristics ....................................... 19
Computerized Controlled Fluidized bed study Unit .......................................................... 20
Pressure drop through fixed and fluidized beds (fluid: water) and fine particles ............... 24
Study of the pressure drop in fixed and fluidized beds (fluid: water) and thick particles ... 26
Study of the pressure drop in fixed and fluidized beds (fluid: air) and fine particles.......................28

Study and determination of the minimum fluidization rate.............................................................30

Liquid solid mixing Study Unit ......................................................................................... 33

Visualization of fluid fields ................................................................................................... 34
Power required in the agitation process .............................................................................. 35
Suspensions of solids in liquids.........................................................................................................37

Formation of solutions solids – liquids..............................................................................................39

Computerized Control Plate and Frame Filter Press ......................................................... 40

Obtaining the turbidity versus concentration calibration straight line ............................... 46
Study of the plate and frame filter press at constant pressure ........................................... 48
Study of the plate and frame filter press at constant flow...............................................................52

Oil Extraction Screw Press .............................................................................................. 56

To Observe and Analyze Oil extraction from Lin seeds by Screw Press Machine................ 58

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 Solid Handling Study Unit
Introduction:
Solids are, in general, more difficult to treat than liquids, vapors or gases. During the
processes, the solids may be presented in some types: big angular pieces, continuous wide
sheets or powders pulverized in a refined way. They may be hard and abrasive, resistant or
gummy, soft or fragile, dusty, plastic or sticky. Independently of its shape, it is necessary to
find ways to manipulate the solids in the way they are shown, and if it is possible, to improve
its manipulation characteristics.

Description:
The unit for the Solids Operation Study is at laboratory level, designed to study some
operations regarding the solids. And now, we show an account of the operations object of
study and the elements used for it as well:

• Size reduction: Ball mill with various sizes of balls.

• Analysis of grain measure by sieve: vibratory sieve and other sieves.
• Solids blending: V-Blender.
• Solids conveyor: Pneumatic conveyor.
• Solids separation: Cyclone.
• Solids storage: Rotational cylinder.
• Solids unloading: Hoppers and collecting tray.
• Solids properties: Graduated test tube.
• Solids weighing: Scale.

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 Solid Handling Study Unit

Theory:
The masses of solid particles, especially when the particles are dry and do not stick, have
many of the properties of a fluid. They exert pressure on the walls of a container, flowing
through a hole or coming down a hopper. However, they are different in some aspects from
the liquids and gases, as the particles are interwoven and stuck because of the pressure and
cannot glide down one to each other until the force applied reach a certain value. The
granular solids and the solids masses resist permanently the distortion when they are
subjected to a distorting and moderate force, contrary to what happens with most of the
fluids. When the force is big enough, the breaking takes place and one layer of particles
glides down over another, but among the layers situated to both sides of the fissure there is a
great deal of friction.

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The masses of solids have the following distinctive properties:

1. The pressure is not the same in all directions. In general, an applied pressure in one
direction provokes some pressure in other directions, but it is always smaller than the applied
pressure.

2. A sharp effort applied on the surface of a mass transmits itself through a whole particles
static mass as long as there are no breakings.

Depending on its flux properties, the solids in a particle shape split into two groups: cohesive
and no cohesive. The no cohesive materials like grain, sand or plastic strands flow easily
from containers or silos. The cohesive solids, like humid clay, are characterized by its
difficulty to flow through holes.

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 Experiment # 1

“Granulometric analysis by sieving”

Theory:
We use different sieves to measure the size (and the sizes distribution) of the particles for the
interval between 125 mm and 0.020 mm. The sieves, which consist of framework and mesh,
are made with wires. The openings may be square or round. Each sieve is identified by the
size of the holes called hole meshes. The particles fractions that go through the sieve are
called dust fines, and the retained fraction is called coarse grits.

Required Material:
• A scale.
• A tray.
• A vibratory sieve.
• A set of sieves with several holes meshes.
• A solid sample which is going to be studied (salt, sand, sugar, etc.).

Experimental procedure:
If we wish to analyze something, first of all we weigh the solid with a scale, which has been
previously tared. The sample will have a maximum of 250 grams to assure the correct
operation of the sieve. Afterwards, a set of normalized sieves is put, which will be fit
vertically. The sieve with the smallest hole mesh will be put at the bottom, over a rack
without openings called bottom, where we collect the solid that is not retain by the last sieve.
At the top, we put the sieve with the biggest hole mesh.

The particles are kept over the sieve, we put the lid, we fix the system with bolts and we
subject the set to vibrations for a certain time. We have a first rejection and some coarse grits
pass to the next sieve, with a smaller hole mesh than the previous one, representing its
particle. And so on.

Each rejection is removed and weighted. The total amount of the rejections (included the one
taken from the bottom) must be equal to the total mass of solids that is collected on the sieve,
with a permissible error not over 2%.

The experiment result is tabulated, showing in this table the rejection mass, the coarse grits
mass, the rejection percentage, the accumulated rejection percentage and the accumulated
coarse grits percentage.

For a better comprehension, an example of the treatment about the obtained data regarding a
false experiment of sieve has been done. In this example, we come from a particle of 200
grams. Eight sieves will be used plus the bottom that will be represented as a 0mm hole
mesh.

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We make two graphics. In first one, we represent the dust fines and coarse grits masses ratio
for each sieve. In second one, we represent the accumulated percentages of dust fines and
coarse grits for each sieve, showing the axe X the sieves sizes in a real proportion.

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 Experiment # 2

“Milling: Ball mill”

Theory:
The mill is a unitary operation that reduces the average volume of the particles in a solid
sample. We carry out the reduction dividing or fractionating the sample by mechanical ways
until we obtain the desired size. The most usual methods of reduction used on the mill
devices are: compression, impact, rubbing of metal shears and cut.

The milling operation is made in some phases: The first one consists of breaking into pieces
solids of great size. For this purpose, we use the crushers or primary mills. The more used
mills are: the hammer mill (usually used in the cement industry), and the jawbones one.

The second phase is useful to reduce the size using more control, operating intermediate and
fines sizes. For this phase, the mill more often used in the industry is the balls mill.

The balls mill carries out the most part of the reduction by impact. When it revolves round an
axis, it provokes that the balls fall down in cascade from the maximum height of the mill.
This action causes a tapping on the material that is going to be moved. Besides, we obtain the
material in good state. Thus, the mill is uniform.

At industrial scale, the balls mill works with a continuous flow, having two rooms inside; the
first one has big balls of two or three inches of diameter, whereas the second one will have
balls of 1 to 1 1/2 inches.

Required material:
• Balls mill.
• Balls.
• Vibratory shaker and a set of sieves.
• Collecting tray.
• Solid for a study.

Experimental procedure:
To establish the efficacy of the mill, the logical steps are:

• Previous sieve.
• Mill.
• Final sieve.

Weight an amount of solid between 250 grams and 1000 grams on the scale. Do several
weighing if required. We sieve the sample in pieces of 250 grams, as with greater amounts,
the effectiveness of the sieve decreases. Once the solid has been sieved, we can opt for
several practical exercises:

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Practical exercise 1: Take a mass of solid with a homogeneous size, and establish the mill
homogeneity, that is to say, if from a given size regarding the particles (previous sieve), we
can obtain one or some sizes (final sieve), changing also the mill time.

Practical exercise 2: Take a mass of solid with a heterogeneous size and establish the mill
homogeneity.

Once the practice has been decided, we fill up the mill with the sample and 3.5 kg of balls
(weighed in several times). The size and the balls proportion may be changed and be studied.

Before turning on the mill, we set the speed regulator to the minimum. Afterwards, we
increase the speed until we see the balls falling freely. The mill time can change between 10
and 30 minutes.

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 Sedimentation Study Unit
Description of the equipment:
Introduction:

The emptying of water undesired solids in suspension can be carried out in several ways,
including the use of centrifugal machinery, sedimentation receptacles, dust extractors and
sedimentary separators. The latter two equipments are the most employed in the industry, due
to the relatively low investment and working cost.

The characteristics of the small particles placed in the water are of utmost importance both in
natural systems (rivers, canals etc.) and in the transformation equipment, especially those that
include the water treatment.

The study of how the particles are laid out in a liquid is crucial for many industries, and the
sediments study equipment gives the student the opportunity of observing the deposit and
sedimentation phenomena in a simple and plain way. Likewise, the deposit rates might be
measured as a function of the particles size, as well as the density and the condensation in a
static water system.

Theoretical Basis:
Basic Principles:

When the concentration of a given suspension is low, the effects of a mutual interference are
insignificant, and the deposits index is determined according to the Stokes law:

Where: d is the equivalent spherical diameter of the particle. However, when the
concentrations are high the conditions of the suspension are remarkably modified, especially
in those in which the fluid rise velocity shown by the sedimentation particles is much bigger.
The features of the resultant fluid are importantly altered and the effect is known as “hindered
settling”.

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 Sedimentation Study Unit
Generally, there are four areas in the sedimentation of concentrated suspensions. In the zone
of constant composition, the suspension moves at a constant rate smaller than that one given
by the Stokes law (although for dilute suspensions, the Stokes law coincides almost
perfectly). In the third area, the concentration increases as the agglomeration appears, and on
the base of the column the sediment or mud is formed. The hindered settling happens in the
area of variable composition, and several correlations have been suggested to apply in this
area.

The flow of the area free from deposits is altered on the walls of the vessel, and the deposit
velocity is lower than the stipulated by the Stokes law.

While the interphase of the suspension moves downwards, the level of the sedimentation
rises. The point in which these two levels get equal is known as “critical point”, and it is a
measurement of the sedimentation volume.

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Experiment # 1
“Effect of the initial concentration over the sedimentation characteristics”

a) Select an adequate powder, such as chalk, and mix it well. Weigh five separated
quantities in order to have five equal volumes of chalk mixed with water of 2.5%, 5%,
7.5%, 10% and 12.5% concentrations per weight. Each mixture must be constituted in
a separated small barrel, and the volume of each one must be identical (more or less 1,5
liters).
b) Stir the mix well in the preparation tubes and then fill each sedimentation tube, starting
with the most concentrated one.
c) After that, the tubes must be removed from the grip brooches. Take the provided rubber
plugs that are used to close the open ends. Each tube must be shaken well but gently, in
order to obtain a suspension with consistency.
d) Then, the tubes must be placed in the grip brooches of the sustenance board, and in the
same interval of time (between the mix and the test), it is necessary to take note of the
interphase readings (between the clean liquid and the suspension that sinks).
e) Furthermore, in order to note the interphase drop in every sedimentation tube at some
suitable intervals of time, it is necessary to take notes of the interphase mix increase on
the base of the tube (This, could be observed only with concentrations relatively low).
f) Draw graphs of height against the time. For final reading it is necessary to wait 24hrs.

Observation & Calculations:

Concentration (%) 2.5% 5% 7.5% 10% 12.5%

Weight of the initial solids

employed(kg)

Height when the critical point has

been reached (m)

Sedimentation volume
3
(m /kg)=(Height in the critical
point*Tube Area)/Weight of
initial solids

Final Height of sediment (m)

Final volume (m3/kg)=Final

height*Tube area / Weight of
initial solids.

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Experiment # 2
“Effect of the initial height over the sedimentation characteristics”

1) The experiment 1 must be repeated, but instead using 5 different concentrations with
similar mixture volumes, we must use the same concentrations but with 5 different initial
volumes.
2) In the sedimentation tubes, the experiments with mixture initial heights of 30, 40, 50, 60
and 70 cm can be carried out later on.
3) The graphs referred in the Experiment 3 may be drawn again by using the values
introduced in the chart of the Experiment 1.
4) Not necessarily, there must be differences in the characteristics, for instance the graph of
V as opposed to C should be the same for the 5 different initial heights, nor in the
sedimentation ratios or in the final volumes.

Observations & Calculations:

Initial height of solutions(mm)

Concentration (5%)

Weight of the initial solids

employed(kg)

Height when the critical point has

been reached (m)

Sedimentation volume
3
(m /kg)=(Height in the critical
point*Tube Area)/Weight of
initial solids

Final Height of sediment (m)

Final volume (m3/kg)=Final

height*Tube area / Weight of
initial solids.

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 Computerized Controlled Fluidized Bed Study Unit
Description of the Unit:

Introduction:
The flow of a fluid through a particles bed is a phenomenon that normally takes place in
nature; for example, the flow of water through the ground.

As far as industrial applications are concerned, the ion exchange, the extraction of soluble
compounds from raw materials and other chemical processes can be included.

The LFF unit allows a full study about everything concerning the flow of a fluid through a
particles bed, both fixed and fluidized. The unit allows the simultaneous study of the water
and air flow through the bed.

Description:
The unit is composed of 2 transparent removable columns made of plastic for the
simultaneous study of the air and water flow through the bed. In the LFF unit each column is
connected to a manometers panel that indicates at all times the pressure drops caused by the
bed. In the LFFC unit the pressure drop is measured by a differential pressure sensor
connected to each column.

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Water is pumped from the tank, located at the back side of the unit, to the bottom of the first column,
going through a flow control valve and a flow meter(LFF) or flow sensor (LFFC).

Air is supplied to the second column through a compressor located at the back of the unit. The air
flow is measured by a flow meter (LFF) or a differential pressure sensor and an orifice plate (LFFC).

There are glass beads of two different sizes for the bed.

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Theory:

Introduction:
Fluidization is the name of a contact process that takes place between a solid and a flow (gas
or liquid), in which the bed made up of solid particles, divided in a refined way, gets up and
gets agitated using a flow rising current.

However, McCabe and Smith point out that it is about particulate fluidization when there is a
big but constant expansion of the bed at high velocities. Such expansion usually becomes
evident in flow-solid systems, for very small particles and a limited range of velocity. There
is talk of aggregative fluidization when the solids beds are fluidized with gases, as the air;
that happens where most part of the gas that passes through the bed in bubbles or in hollows
that are have almost any solid. There is only a little fraction of gas that flow through the
existent canals between the particles; such particles move erratically.

McCabe and Smith point out that although at present, the petroleum industry uses transport
reactors for the catalytic cracking instead of fluidized beds, the catalyst regeneration is made
still in fluidized bed reactors, which have until 10 meters of diameter. The fluidization is also
used in other catalytic processes, such as the acrylonitril synthesis, and to carry out gas -solid
reactions. There is a lot of interest regarding the charcoal combustion in a fluidized bed, to
reduce the costs of the boilers and to decrease the pollutants emission. The fluidized beds are
also used for minerals hardening, for fine solids drying and for gases absorption.

For the study of cakes, an important element is to know the pressure drop in it. Precisely,
McCabe y Smith point out that there are two equations to find out this value. The first one is
Ergun’s equation, which is used for packed cakes:

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For fluidized cakes, the following equation is used:

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Experiment # 1:
“Pressure drop through fixed and fluidized beds (fluid: water) and fine particles”

Objective:
This practical exercise tries to study the pressure drops generated in a fixed and fluidized bed
system, for different thickness of the bed and different flows of the liquid (water).

Necessary element:
• LFFC or LFF unit

Practical procedure:
1. Fill the filtering column at the left side with some fine glass material (170-300 microns)
up to a specific height (for example: 50mm).

2. Close the water shut-off valve (VR-1) to the column.

3. Switch on the pump (AB-1) and gradually open the flow regulation valve (VR-1) until a
low flow is obtained and the bed remains still. Record the pressure drop generated in the
column and the water flow to which it corresponds.

4. Keep on opening the valve gradually and measure the pressure drop, the flow of water and
the height of the bed several times (starting from an average between the higher and the lower
height of the bed), thus obtaining enough measurement points so as to perform the study
perfectly.

5. Repeat the experiment varying the initial height of the bed (for example: 100mm).

6. Repeat the experiment with so many heights of the initial bed as wished. Take into
account that at a certain moment the bed will not be able to fluidize because there will be too
many solids and it will be not able to expand itself or there will be too much pressure drop in
the manometers to measure it.

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Results and tables:
• Record the obtained results in the table below.

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Experiment # 2:
“Study of the pressure drop in fixed and fluidized beds (fluid: water) and thick particles”

Objective:
This practical exercise tries to study the pressure drops generated in a fixed and fluidized bed
system, for different thickness of the bed and different flows of the liquid (water).

Necessary element:
• LFFC or LFF unit

Practical procedure:
1. Fill the filtering column at the left side with some thick glass material (250-420 microns)
up to a specific height (for example: 50mm).

2. Close the water shut-off valve (VR-1) to the column.

3. Switch on the pump (AB-1) and gradually open the flow regulation valve (VR-1) until a
low flow is obtained and the bed remains still. Record the pressure drop generated in the
column and the water flow to which it corresponds.

4. Keep on opening the valve gradually and measure the pressure drop, the flow of water and
the height of the bed several times (starting from an average between the higher and the lower
height of the bed), thus obtaining enough measurement points so as to perform the study
perfectly.

5. Repeat the experiment varying the initial height of the bed (for example: 100mm).

6. Repeat the experiment with so many heights of the initial bed as wished. Take into
account that at a certain moment the bed will not be able to fluidize because there will be too
many solids and it will be not able to expand itself or there will be too much pressure drop in
the manometers to measure it.

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Results and tables:
• Record the obtained results in the table below:

26
Experiment # 3:
“Study of the pressure drop in fixed and fluidized beds (fluid: air) and fine particles”

Objective:
This practical exercise tries to study the pressure drops generated in a fixed and fluidized bed
system, for different thickness of the bed and different flows of the gas (air).

Necessary element:
• LFFC or LFF unit

Practical procedure:
1. Fill the filtering column at the right side with some fine glass material (170-300 microns)
up to a specific height (i.e. 50mm).

2. Close the air shut-off valve (VR-2) to the column.

3. Switch on the compressor (ACO-1) and gradually open the flow regulation valve (VR-2)
until a low air flow is obtained and the bed remains still. Record the pressure drop generated
in the column and the air flow to which it corresponds.

4. Keep on opening the valve gradually and measure the pressure drop, the flow of air and
the height of the bed several times (starting from an average between the higher and the lower
height of the bed), thus obtaining enough measurement points so as to perform the study
perfectly.

5. Repeat the experiment varying the initial height of the bed (for example: 100mm).

6. Repeat the experiment with so many heights of the initial bed as wished. Take into
account that at a certain moment the bed will not be able to fluidize because there will be too
many solids and it will be not able to expand itself or there will be too much pressure drop in
the manometers to measure it.

27
Results and tables:
• Record the obtained results in the table below.

28
Experiment # 4:
“Study and determination of the minimum fluidization rate”

Objective:
The objective of this practical exercise is determining and studying the minimum fluidization
point.

Necessary element:
• LFFC or LFF unit

Practical procedure:
1. Fill the filtering column at the right side with some thin glass material (170-300 microns)
up to a specific height (i.e. 50mm).

2. Close the air shut-off valve (VR-2) to the column.

3. Switch on the compressor (ACO-1) and gradually open the flow regulation valve (VR-2)
until a low air flow is obtained and the bed remains still. Record the pressure drop generated
in the column and the air flow to which it corresponds.

4. Keep on opening the valve gradually and measure the pressure drop, the flow of air and
the height of the bed several times (starting from an average between the higher and the lower
height of the bed), thus obtaining enough measurement points so as to perform the study
perfectly.

5. Repeat the experiment varying:

• The height of the bed. Take into account that at a certain moment the bed will not be able
to fluidize because there will be too many solids and it will be not able to expand itself or
there will be too much pressure drop in the manometers to measure it.
• The size of the glass material of the bed.
• The fluid (water or air) that passes through the bed. (*) NOTE: in order to visualize the
graphical representation better when performing this practical exercise with water, work
first with the regulation valve totally open, obtaining the maximum flow at the beginning
and regulating the valve to obtain lower flows then.

29
Results and tables:
1) Record the obtained results in the table below.

2) Calculate porosity of the initial bed):

The initial bed porosity can be calculated without the unit. For that purpose:

• Add a known volume of bed packing (in this case, the thin or thick glass particles, as it
corresponds).
• Record that volume and add known volumes of water until the entire added packing is
covered. So:

V’= volume of added water

V= volume of added solid

3) Calculate the rate of the fluid and Ɛ in every case and complete the table below:

• To calculate the rate, take into account the volume of flow of the fluid and the section of
the column.
• To calculate the porosity, since the area is constant:

30
4) Plot dP versus U and determine the minimum fluidization rate point (point A).

Check that the fluidization minimum rate is lower in the liquid-solid system because the
pressure drops required to equal the gravity effect on the particles is lower than in the gas-
solid system. That is due to the fact that water has viscosity and density values higher than
those of the air.

31
 Liquid Solid Mixing Unit
Introduction:
Agitation is a unit operation whose objective is to produce irregular movements in a fluid, by
mechanical devices that act on it. Agitation is often mistaken with mixture, but they are not
synonyms. Agitation refers to the movement induced in a material in a specific form,
generally with a circulatory model inside some type of container and a mixture, however, is a
random distribution of two or more phases initially separated. An only material, as water in a
tank, can never be mixed. To make it, it will be necessary to introduce water at another
temperature or another type of solid powdery material.

Description:
The mixing unit allows the study of the agitation process in order to familiarize the different
magnitudes (torque, turning speed, etc) that take part in the process.

32
 Experiment # 1: “Visualization of fluid fields”

Objective:
The objective of this practical exercise is to visualize how the fluid field evolves using a
certain tank and a certain impeller or agitator as the revolutions of the agitator are increased
and the position with regards the bottom.

Necessary elements:
• The elements required for this practical exercise are:
• Impeller of helix of = 100 mm.
• Tank of D = 300 mm and H = 300 mm, without deflector.
• Water (distilled or from the tap).
• Particles of PVC of size 10 mm.

Practical procedure:
1. Fill the tank with water until a height of 200 mm

2. Add the particles of PVC.

3. Go up the agitator and install the impeller of helix

4. Go down the agitator at a distance of 50 mm from the bottom of the tank.

5. Make the impeller rotate at very low revolutions and slowly increase the turn velocity until
the particles begin to rotate.

6. Write down the revolutions and the height of the water in the side wall of the tank h.

7. Increase the revolutions, and write it down in each case.

The experiment will conclude when the water reaches the superior border of the tank.

Analysis of the results:

For each of the tests made, represent the graph, the revolutions of the impeller in function of
the height.

33
 Experiment # 2: “Power required in the agitation process”

Objective:
The objective of this practical exercise is to demonstrate the dependence of the power
required in the agitation process in function of the turning speed of the impeller.

Necessary elements:
The elements required for this practical exercise are:

• Impeller of helix = 100 mm.

• Tank of D = 300 mm and H = 300 mm, without deflector.
• Mixture of water and glycerin (high viscosity)

Practical procedure:
1. Fill the tank with the mixture of water and glycerin to a height of ho = 210 mm.

2. Place the group in the position of work and install the impeller of helix at a distance of 70
mm from the bottom of the tank.

3. Next, cover the tank.

4. Begin the turn at low velocities, beginning at around 250 rpm and increase the revolutions
until the mixture has a homogeneous behavior.

It is advisable to stop increasing the revolutions when in the fluid we have bubbles in the
center of the dissolution, since the agitation that we produce is made in different fluid means
so that the power measured by the equipment will have a considerable variation.

5. The revolutions and the force that the torque meter shows are written down.

6. The experiment is made in a decreasing way in the turn velocity, and it is also interesting
to write down the data in an inverse way, that is, taking the velocities in a decreasing way.

7. The average would be made and we would work with these values. You can usually work
with the direct measures.

8. The experiment ends when the liquid arrives to the superior border of the tank.

34
We repeat the test using the turbine impeller of diameter 100 mm and later we use the other
blades impeller of diameter 100 mm, keeping the same characteristics.

35
 Experiment # 3: “Suspensions of solids in liquids”

Objective:
The objective of this practical exercise is to analyze how the use of different types of
impellers influences the dispersion of solid particles in liquids.

Necessary elements:
The elements required for this test are:

• Helix impeller = 100 mm.

• Tank: D = 300 mm and H = 300 mm, without deflector.
• Distilled water.
• Fine sand.

Practical procedure:
1. Pour 1/3 Kg of fine sand in a tank and fill with distilled water to a height ho = 210 mm.

2. Place it on the work place. Locate in the bench the helix impeller of 100 mm and cover the
tank.

3. Put the helix impeller of 100 mm of diameter in the bench and cover the tank.

4. Place the impeller to a distance of 150 mm from the bottom of the tank.

5. Start the turn at very low revolutions and increase it until observing that the rising of the
sand begins.

6. Write down the situation of the impeller regarding the bottom, h and the revolutions, at
which the rising of the sand takes place.

7. Put the impeller down at intervals of 25 mm and repeat the abovementioned, writing down
the same thing in the drop.

36
Results and tables:
Data will be written down in a table like the following one:

37
 Experiment # 4: “Formation of solutions solids – liquids”

Objective:
The objective of this practical exercise is to analyze how different impeller types influence in
the solutions of solid particles in liquids.

Necessary elements:
• The elements required for this test are:
• Helix, turbine and blades impellers with a diameter = 50 mm.
• Tank of D = 300 mm and H = 300 mm, without deflector.
• Distilled water.
• Salt in fine grain.

Practical procedure:
Once the best position of each agitator is defined, follow the following steps:

1. Put 1/3 Kg of salt in fine grain in the tank, fill with clear water to a height of ho = 210
mm and place it in the work place.
2. Place the helix impeller to the good distance defined in section 7.4.3.3 and cover the tank.
Begin the turn of the low revolutions and increase them until the rising of the salt is
noticeable.
3. Write down the situation of the impeller with regards to the bottom h, the revolutions and
the time that has passed by until the solution is homogeneous.
4. Proceed similarly with the turbine impeller and the blade impeller.
5. The data will be written down in a table.

Results and tables:

Write down the data in a table like this one:

Analysis of the results:

At sight of the previous table, discuss the result, pointing out the impeller that needs fewer
time and/or power.

38
 Computerized Controlled Filtration Unit
Description of the Unit:

Introduction:
Filtration is the separation of solids from liquids by forcing the liquid to flow through a
porous medium and depositing the solids on the medium. A filter aid is a finely divided
material which, when added to the liquid to be filtered, helps to control the flow and solids
removal.

Plate and frame filters, or filter presses, are batch-operated units, in which the suspension is
filtered through the surface of plates, forming a cake within the supporting frames. The
filtrate is collected through special piping and the cake is discharged when the operation is
stopped for cleaning.

Even though they are batch devices, the good washing and low cake moisture available in
plate and frame filters have kept them in wide use. These factors contribute to get long
service times and good reliability.

Filter presses are used successfully in either cake or clarifying filtration, depending on the
concentration and properties of the solids. Cake filtration is applied in the production of
chemicals, ceramics and raw materials, and in wastewater treatment, nuclear technology and
other fields.

The Computer Controlled Plate and Frame Filter Press has been designed to demonstrate the
filtration and clarification processes suitable for chemical, pharmaceutical, food and beverage
industries, etc.

Description:
Plate and frame filter presses are used in the pharmaceutical, chemical, cosmetic and food
and beverage industry (for example, to clarify intermediate products).

A suspension is prepared in a feed tank and is transferred through a centrifugal pump into the
plate and frame press. This pump ensures that the solid s remain suspended and do not settle.

The filter plates are grooved and covered over with filter clothes. Filter cloth (or filter media)
retains the solid particles of the suspension, which fills the frame plates, whilst the filtrate
passes through the filter media or filter cloth. The filtrate flows through the collecting pipe
and is collected in the filtrate tank. The solid material is separated off from the filter cloth,
where it forms a growing filter cake.

The suspension passes through three pressure sensors and one flow sensor on its way. The
initial temperature of the suspension and the final temperature of the filtrate can be recorded
with two thermocouples.

A turbidity meter allows the solid concentration of the filtrate to be determined.

39
The process control is done from the computer through the SCADA software. Such software
will allow to perform automatic controls (PID) of the variables involved in the process, thus
facilitating the work.

Darcy’s Equation:
The batch filter design equation is based on Darcy’s law. It determines the velocity of a
fluid, v, when passing through a solid bed as:

Keeping a Reynolds number smaller than 5:

Where:

• k: Darcy’s law permeability constant

• ΔP: pressure drop in the bed
• L: width of the bed
• m: viscosity of the bed
• D: diameter of the particle
• r: density of the liquid
• e: void fraction of the cake

The velocity, v, can be calculated as:

Where:

• V: total volume of filtrate since the start of the cycle

• A: transverse area of the filter
• Q: flow of liquid through the filter

Going back to equation (1), the flow resistance of the liquid can be defined as:

40
The design equation (1):

Will be then as follows:

41
Experimental Studies:

Constant pressure filtration tests:

The filtration practical exercise can be done by controlling the pressure difference, so that it
remains constant throughout the whole process. It is clear that at a constant pressure the rate
of filtration will decrease as the thickness of the cake and its resistance to filtration increases.
For the study of filtration under these conditions, we can start from the Hagen-Poiseuille law
described before, which can be written as follows:

As we have a constant pressure process:

Where:

According to the previous equation and representing Δθ / ΔV in ordinates versus the filtrate
volume, a straight line of slope K1 and ordinate K2 will be obtained, as it is shown in the
following image:

42
Once these constants are obtained, the values of α and r can be found.

In order to determine the effect of the pressure change, it is necessary to perform several tests
at different pressures and to calculate the compressibility constant S. For that purpose,
represent the log α versus log ΔP, thus obtaining a straight line of slope S and ordinate in α '
origin.

The experimental determination on a pilot scale of the parameters K1 and K2 and those of r, α,
S and α' are necessary to design or select a filter for a specific system, choose the filter
medium that provides the maximum solids retention and determine the operating conditions
(temperature, pressure, etc.).

Constant rate filtration tests:

The filtration practical exercise can be done by controlling the speed, so that it is kept
constant throughout the whole process. In this case, pressure will increase as the filtering
process takes place due to the fact that the cake thickness will increase, thus increasing the
resistance to filtration. For the study of filtration under these conditions, we can start from the
Hagen -Poiseuille law described before, which can be written as follows:

Isolate ΔP from the previous expression:

Where:

As this is a constant speed process, the previous expression will be as follows:

43
Where:

According to the previous equation and representing ΔP in ordinates versus

The filtrate volume, a straight line of slope K1 and ordinate in the origin K2, as it is shown in
the following image, will be obtained:

Once these constants are obtained, the values of α and r can be found.

44
Experiment # 1: “Obtaining the turbidity versus concentration calibration straight line”

Objective:
The objective of this practical exercise is to obtain a calibration straight line that relates the
turbidity of the filtrate with the concentration of solids in that filtrate.

Required elements:
• AFPMC unit.
• Calcium carbonate (or siliceous earth).
• Water.
• Portable turbidity meter.

Experimental procedure:
Place the filter medium and the gaskets between the plates of the filter, verifying that they fit
correctly. Close the filter press and make sure that there are no leaks between plates.

Prepare a known concentration suspension of calcium carbonate (or siliceous earth) in water.
When using calcium carbonate, the maximum amount that can be measured with the turbidity
meter is about 700 grams in 250 liters of water.

Prepare the suspension in the suspension tank. For that purpose, add a known amount of
solid to a known amount of water (for example, 150 liters) in the suspension tank. Open the
bypass of the suspension tank y close the valve of the filtration tank to keep stirring the
suspension in order to homogenize it.

Switch on the pump and continue stirring for a while. After a few minutes, take a sample of
the suspension and measure its turbidity.

After recording the turbidity, add another known amount of solute and repeat the previous
steps until the turbidity meter saturates (the reading limit is 1000 FTU).

45
Results and tables:
Complete the following tables:

Represent the turbidity (FTU) versus solute concentration in water (gr. /l) and obtain a linear
regression to obtain the corresponding calibration straight line.

46
 Experiment # 2: “Study of the plate and frame filter press at constant pressure”

Objective:
The objective of this practical exercise is to determine the operating constants of the unit
under constant pressure conditions (K1, K2, α and r).

Required elements:
• AFPMC unit
• Calcium carbonate (or siliceous earth).
• Water.
• Portable turbidity meter.

Experimental procedure:
Write down the weight of the filter frames and filtering medium when they are completely
dry.

Place the filter medium and gaskets between the plates of the filter, verifying that they fit
correctly. Close the filter press and make sure that there are no leaks between plates.

Prepare a known concentration suspension of calcium carbonate (or siliceous earth) in water
(to perform the practical exercises you can start with 0.3% of solute in water, that is to say,
about 760 grams of solute per 250 liters of water). It is important to know the proportion and
concentration of the solution with accuracy.

Check that the drain valve of the suspension tank is closed. Introduce the suspension in the
suspension tank. Open the bypass of the filtration tank and close the valve to the filtration
tank to continue stirring the suspension in order to homogenize it.

Switch on the pump (keep it to the 70-80% minimum) to stir the suspension for a few
minutes. Afterwards, switch off the pump, close the valve of the bypass and open the valve to
the filtration tank completely.

Then, introduce the suspension in the filtration tank of the unit. Close the drain valve of the
tank and open the inlet valve to the press filter. Afterwards, connect the pump to begin the
filtration process and set the pressure to a specific value to keep it constant.

The length of the process will depend on the initial concentration of the sample. The lower
the concentration is, the longer the time needed to notice a significant change in the flow will
be. Do not exceed a working pressure of 2.5 bars.

Take samples through the filtration process to check whether the filtration is correctly
performed. For that purpose, use the drain valve at the bottom of the filtration tank.
Remember that the turbidity meter must be used to analyze the turbidity of the filtered liquid.

Take the values of the flow at different points in time.

47
Carry out the filtration until there is no more liquid leaking through the filter. Then, switch
the system off.

Dismount the filter from the press.

Weight the filter on a scale and record the weight. The amount of solute retained in the filter
can be determined by knowing the weight of the dry filters.

Let the filtering medium and cake dry and weight them when they are totally dry. Record the
weight. The amount of solute retained in the filtering medium can be determined by knowing
the weight of the dry filtering media.

The final weight of the cake is obtained by summing both amounts of solute.

Perform this same procedure setting different pressures.

48
Results and tables:
Complete the following tables for different working pressures.

Plot Δt / Δv versus filtered volume (m3) and represent the regression line to obtain the value
of the slope (K1) and the ordinate (K2).

49
From these data, determine the resistance of the filter medium (r) and the specific resistance
of the cake (α).

Dry the cake after each filtration test and weight it. Calculate the number of solids that
remain in the suspension.

50
 Experiment # 3: “Study of the plate and frame filter press at constant flow”

Objective:
The objective of this practical exercise is to determine the operating constants of the unit
under constant flow conditions (K1, K2, α and r).

Required elements:
• AFPMC unit
• Calcium carbonate (or siliceous earth).
• Water.
• Portable turbidity meter.

Experimental procedure:
Write down the weight of the filter frames and filtering medium when they are completely
dry.

Place the filter medium and gaskets between the plates of the filter, verifying that they fit
correctly. Close the filter press and make sure that there are no leaks between plates.

Prepare a known concentration suspension of calcium carbonate (or siliceous earth) in water
(to perform the practical exercises you can start with 0.3% of solute in water, that is to say,
about 760 grams of solute per 250 liters of water). It is important to know the proportion and
concentration of the solution with accuracy.

Check that the drain valve of the suspension tank is closed. Then, introduce the suspension in
the suspension tank. Open the bypass of the filtration tank and close the valve to the filtration
tank to continue stirring the suspension in order to homogenize it.

Switch on the pump (keep it to the 70-80% minimum) to stir the suspension for a few
minutes. Afterwards, switch off the pump, close the valve of the bypass and open the valve to
the filtration tank completely.

Then, introduce the suspension in the filtration tank of the unit. Close the drain valve of the
tank just after starting the filtration and open the inlet valves to the pump. Afterwards,
connect the pump to begin the filtration process and set the pressure to a specific value to
keep it constant.

The length of the process will depend on the initial concentration of the sample. The lower
the concentration is, the longer the time needed to notice a significant change in the flow will
be. It is recommended not to exceed a flow of 25 l/min.

Take samples through the filtration process to check whether the filtration is correctly
performed. For that purpose, use the drain valve at the bottom of the filtration tank.
Remember that the turbidity meter must be used to analyze the turbidity of the filtered liquid.

51
Take the values of the flow at different points in time.

Carry out the filtration until there is no more liquid leaking through the filter. Then, switch
the system off.

Dismount the filter from the press.

Weight the filter on a scale and record the weight. The amount of solute retained in the filter
can be determined by knowing the weight of the dry filters.

Let the filtering medium and cake dry and weight them when they are dry.

Record the weight. The amount of solute retained in the filtering medium can be determined
by knowing the weight of the dry filtering media.

The final weight of the cake is obtained by summing both amounts of solute.

Perform this same procedure setting different flows.

52
Results and tables:
Complete the following tables for different working flows.

Plot ΔP versus filtered volume (m3) and make the regression line to obtain the value of the
slope (K1) and the ordinate (K2).

From these data, determine the resistance of the filter medium (r) and the specific resistance
of the cake (α).
53
Dry the cake after each filtration test and weight it. Calculate the number of solids that
remain in the suspension.

54
 Oil Extraction Screw Press
General Information

The Mini 40 Screw Press has been designed specifically for village industry and laboratory
applications to process a range of oilseeds with the minimum, if any pre-treatment.

The press has a nominal capacity of approximately 40 Kgs per hour input of the softer seeds
(e.g. sunflower, rapeseed, linseed) and up to 90 Kg’s per hour input when processing hard
fibrous seeds like palm kernels.

The press is normally driven by a 4 KW, (5.5 HP), 4 Pole, 3 phase electric motor that gives a
press worm shaft speed of nominally 120 R.P.M.

Starting up the Press

Before starting up the drive to the press the following check list should be observed: -

i) Ensure that all guards have been fitted and are fixed in place.

ii) That the lubrication of the machine has been carried out in accordance with the
instructions in the Lubrication Schedule.

iii) The taper choke end of the worm shaft is not fouling the taper bore of the choke ring. This
can be seen where the worm shaft emerges from the choke ring in the cake discharge area.

Mini 40 Screw Press

55
Normal Operation of the Press

When normal operating conditions have been established the aim should be to produce the
best quality of cake possible consistent with required throughput of the press. Most of the
seeds processed by the Mini 40 Press allow the machine to have a full open feed. That is, the
press will continue to operate in a uniform and steady manner gravity feeding from a full
hopper within the power range of the driving motor.

However, there are occasions when the feed is required to be metered to the press. These are:-

i) The more fibrous seeds, such as palm kernels and copra, may require to be metered to the
press as the power requirement can be much greater than that of the softer seeds and therefore
the feed rate has to be restricted to within the power limitation of the driving unit. In this
event, if it is wished to avoid laborious manual feeding, then the press may be fed by some
metering device such as a variable delivery vibrator or screw feeder from a hopper or storage
bin.

ii) Non free flowing feeds like Palm Kernels, copra and other large seeds may usually be
broken or coarsely ground before feeding to the press. In this condition they will not readily
flow into the press feed area and therefore may have to be metered as required to avoid
bridging. To obtain optimum extraction of the oil some seeds require second pressing. Again,
the first pressed cake may have a poor flow characteristic from a filled feed hopper, although
this is not always so.

56
Experiment:

To Observe and Analyze Oil extraction from Lin seeds by Screw Press Machine

Procedure:

Adjust the clearance to 20 on choke operating scale and switch on the press machine.

The motor will now drive the main worm shaft.

Slowly feed the screw press from a weighed initial mass of lin seeds.

While feeding slowly in this manner, gradually close the choke until material being
discharged is of only paper thickness.

Collect the oil and cake in separate trays.

When the thin cake has been discharged freely for few minutes, the press feed may be
increased gradually and choke gradually opened until a firm cake of 1mm thickness has been
produced.

Cake produced can be fed with seeds to optimize the output.

Calculations:

Sr No. Seeds Initial Weight Seeds Final Weight Oil extracted

(gm) (cake). (gm) (ml)

57