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COURSE NAME: PARTICLE TECHNOLOGY 1

COURSE CODE: CHP 252


UNITS: 3
LECTURER: DR. AM MULIWA

Objective
To overall aim of this course is to equip students in disciplines requiring knowledge of the processing
and handling of particles and powders with some basic knowledge and understanding of particle
technology- the key principles, concepts and terminology. Ultimately, students should be able to
apply these concepts in process design situations involving solids.
Learning outcome
By the end of this course the student should be able to:
1. Understand particle properties and characterisation techniques
2. Select a suitable particle characterisation method
3. Manipulate particle size distribution data
4. Describe the underlying principles of several powder processing operations
5. Describe separation solid-liquid techniques e.g. sedimentation and centrifugation

Module syllabus
1. Particle characteristics: particle size and shape, density, surface area, porosity etc.
2. Size analysis: mean particle size, size distribution, shape factors.
3. Particle size classification- Classifiers: principles and equipment.
4. Size reduction: crushing and milling systems, open and closed circuit systems, equipment.
5. Solid-liquid separation: principles of gravity sedimentation and Centrifugal separation,
thickener design.
6. Size enlargement: Particle growth, wet granulation models.

Importance
 Solids used in chemical industries are most commonly in form of particles.
 Solids in general are more difficult to handle then liquid and gases.
 In process industries solid appear in variety of forms, they may be hard and abrasive, tough
and rubbery, soft and fragile, dusty and cohesive, Free flowing or sticky.
 Particulate materials, powders or bulk solids are used widely in all areas of the process
industries, for example in the food processing, pharmaceutical, biotechnology, oil, chemical,
mineral processing, metallurgical, detergent, power generation, paint, plastics and cosmetics
industries.

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 So the knowledge of their properties, handling, storage, transportation, separation and
processing is important from chemical engineering point of view.

Format/Marks distribution

1. One 3 hour lecture per week: Minimum attendance 75%


2. Two continuous assessment tests (CATs): 30% module mark
3. One 3 hour exam: 70% module mark

Books to consult
1. Coulson and Richardson’s, Particle Technology and Separation Processes, Coulson and
Richardson, volume 2, 5th Edition. Butterworth Heinemann. ISBN 0 7506 4445 1
2. Introduction to Particle Technology – Second Edition, Edited by Martin Rhodes, 2 nd Edition,
2008 John Wiley & Sons Ltd. ISBN: 978-0-470 -01427-1
3. Fundamentals of Particle Tech – free pdf book.

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1. PARTICLES AND CHARACTERSATION
1.1. Introduction to Particle Technology
-Particle technology: refers to the field of the science and technology associated with the
characterization, formation, processing, and utilization of particles. It is concerned with the systems in
which one or more of the components are in the form of particles. OR
-Study, characterisation, prediction of properties during the processing of particle dispersions ranging
down to sub-microscopic material. It is the extension of mechanics (fluids and solids) into particle
containing systems. The term 'particles' includes liquid emulsions, drops, foams, oils, dusts, bubbles,
fogs, etc.
-It is concerned with the systems in which one or more of the components are in the form of particles.
-The terms particles, powder, and particulate solids are often used interchangeably, and thus particle
technology is often also referred to as powder technology.
-Recently, the scope of particle technology has been extended to cover systems containing
nanoparticles, aerosols, liquid droplets, emulsions, and bubbles.
-This course is however limited only to solid particles.
-Industries: Energy, chemicals, petroleum, agricultural, food, minerals, pharmaceuticals,
environmental, and advanced materials.
Table 1: Examples of various particulate systems used in different industrial processes.

Types of application Examples


Physical processing powder flow, blending, separation, coating, and pelletizing
urea granulation and drying
dust/particulate collection and removal

Chemical, petrochemical, solid oxide fuel cell


metallurgical, and mineral fluid catalytic cracking
processing coal combustion, gasification, and liquefaction
fischer–tropsch synthesis of liquid fuels
uranium processing
pryolysis of oil shale
production of polyethylene and polyolefins

Biochemical, pharmaceutical, ethanol production from biomass as a renewable energy


and food processing source
treatment of municipal sewage wastewater
drug formulation for delivery via pulmonary
inhalation
calcium phosphate biomaterials used in clinical
medicine
patuline production by penicillium urticae
freeze-dried ice cream

Advanced materials chemical mechanical planarization for semiconductor


industry
electronic ink—printed circuits inks containing
metallic colloidal particles in organic solvent
synthesis of rugged nanophosphors for leds and
diagnostics

Other applications Nanoparticle synthesis (eg, carbon nanotube, mixed-metal

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oxide catalysts, nanocomposites, and quantum dots)
photonic crystal-based optical devices
emulsion templating

1.2. Solid Particle characterisation

-Individual solid particles are characterized by their size, shape and density. Size and shape are easily
specified for regular particles, such as spheres and cubes, but for irregular particles?
Why measure properties?
 Better control of quality of product (cement, urea, cosmetics etc.)
 Better understanding of products, ingredients.
 Designing of equipment for different operations such as crushing, grinding, conveying,
separation, storage etc.
Which particle properties are important to measure?
- In addition to chemical composition, the behaviour of particulate materials is often dominated by the
physical properties of the constituent particles.
-These can influence a wide range of material properties including, for example, reaction and
dissolution rates, how easily ingredients flow and mix, or compressibility and abrasivity.
-From a manufacturing and development perspective, some of the most important physical properties
to measure are: Particle size, Particle shape, Surface properties, Mechanical properties, Charge
properties, and microstructure.

Particle shape
-The shape of an individual particle is expressed in terms of the sphericity which is independent of
particle size.
-Sphericity ( ) is the ratio of surface area of sphere of same volume as particle to the surface area of
particle.

(1)
- So for spherical particle sphericity is equal to one.
- For non-spherical particle it is defined by:

(2)
Where
– : equivalent diameter of particle

– : surface area of one particle

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– : volume of one particle
Equivalent spherical diameters
-The equivalent diameter is sometimes defined as the diameter of a sphere of equal volume.

(3)

-For fine particles, is usually taken to be the nominal size based on screen analysis or microscopic
analysis.
-The surface area is found from adsorption measurements or from the pressure drop in a bed of
particles.
-For many crushed materials, Sphericity is between 0.6 and 0.8. For particles rounded by abrasion,
their sphericity may be as high as 0.95.
Exercise: Determine the sphericity of a particle of surface area 15 mm 2 and volume 2 mm3.

-Some other equivalences include projected area, surface area and mass

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Density
The bulk density of the particles is the overall density of the particulate system including the inter-
particle volumes occupied by fluid medium (eg, air or water). It is defined as the overall mass of the
material per unit volume occupied.
Particle density is the density of a particle including the pores or voids within the individual particles.
It is defined as the weight of the particle divided by the volume occupied by the entire particle.
Particle density is sometimes referred to as the material’s apparent density.
The skeletal density, also called the true density or material density, is defined as the density of a
single particle excluding the pores. Measurements of the skeletal density can be made by liquid or gas
pycnometers. Among three densities, the bulk density is smallest.

PARTICLE SIZE
-By far the most important physical property of particulate samples is particle size.
Size Definition: The size of a spherical particle is defined either by its diameter or its radius.
-Particle size measurement is routinely carried out across a wide range of industries and is often a
critical parameter in the manufacturing of many products.
Particle size has a direct influence on material properties such as:
 Reactivity or dissolution rate e.g. catalysts, tablets
 Stability in suspension e.g. sediments, paints
 Efficacy of delivery e.g. asthma inhalers
 Texture and feel e.g. food ingredients
 Appearance e.g. powder coatings and inks
 Flowability and handling e.g. granules
 Viscosity e.g. nasal sprays
 Packing density and porosity e.g. ceramics.
In general "diameter" may be specified for any equidimensional particles (e.g. emulsions or bubbles).
• Most of the solid particles used in industries are not equidimensional, therefore cannot be specified
by a single dimension i.e. “diameter”.
• In order to simplify the measurement process, it is often convenient to define the particle size using
the concept of equivalent spheres.

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• In this case the particle size is defined by the diameter of an equivalent sphere having the same
property as the actual particle such as volume or mass for example.

-The equivalent sphere concept works very well for regular shaped particles. However, it may not
always be appropriate for irregular shaped particles, such as needles or plates, where the size in at
least one dimension can differ significantly from that of the other dimensions. Such particles are often
characterized by the second longest major dimension. For example needle like particles, Dp would
refer to the thickness of the particle, not their length.
-Units used for particle size depend on the size of particles.
 Coarse particles: inches or millimetres
 Fine particles: screen size
 Very fine particles: micrometers or nanometers
 Ultrafine particles: surface area per unit mass, m 2/g

1.7. Particle size analysis (mean particle size, size distribution, shape factors)

All techniques measure property and relate it to the equivalent spherical diameter. Select your
technique to be the most appropriate for the end use of the data.
Measurement of particle size
-A wide range of measuring techniques is available both for single particles and for systems of
particles. In practice, each method is applicable to a finite range of sizes and gives a particular
equivalent size, dependent on the nature of the method. The principles of some of the chief methods
are now considered together with an indication of the size range to which they are applicable.

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Sieving (>50 μm)
-carried out using a nest of sieves, each lower sieve being of smaller aperture size
-Testing sieves are made of woven wire screens.
- Openings are square.
-Screens are identified by Mesh No. (Numbers of openings per linear inch).
-Generally, sieve series are arranged so that the ratio of aperture sizes on consecutive sieves is 2, 2 1/2
or 21/4 according to the closeness of sizing that is required.
-The sieves may either be mounted on a vibrator, which should be designed to give a degree of
vertical movement in addition to the horizontal vibration, or may be hand shaken.
-Whether or not a particle passes through an aperture depends not only upon its size, but also on the
probability that it will be presented at the required orientation at the surface of the screen.
- The sizing is based purely on the linear dimensions of the particle and the lower limit of size which
can be used is determined by two principal factors:
 The proportion of free space on the screen surface becomes very small as the size of the
aperture is reduced.
 Attractive forces between particles become larger at small particle sizes, and consequently
particles tend to stick together and block the screen.
-Sieves are available in a number of standard series and the sizes of the openings in the screen are
determined by the thickness of wire used.

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The efficiency of screening is defined as the ratio of the mass of material which passes the screen to
that which is capable of passing. This will differ according to the size of the material. It may be
assumed that the rate of passage of particles of a given size through the screen is proportional to the
number or mass of particles of that size on the screen at any instant.
Thus, if w is the mass of particles of particular size on the screen at a time t, then:

(4)
Where k is a constant for a given size and shape of particle and for a given screen.
Thus, the mass of particles (w1-w2) passing the screen in time t is given by:

()

or
- The particles retained of each screen are removed, weighed and masses of individual screen
increments are converted into mass fraction of total sample.
- Any particle that passed the finest screen are caught in the pan at the bottom of stack.
- The results of screen analysis are tabulated to show the mass fraction of each screen increment as a
function of the mesh size range of the increment.

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- The notation 14/20 means “through 14 mesh and on 20 mesh”.

Typical screen analysis is given in Table above.


 First column: mesh size,
 second column: width of opening of screen,
 third column: mass fraction of total sample that is retained on that screen xi (where i is the
number starting from the bottom of the stack),
 fourth column: averaged particle size Dpi (since the particle on any screen are passed
immediately by the screen ahead of it, the averaged of these two screen are needed to specify
the averaged size in that increment).
 Fifth column: cumulative fraction smaller than Dpi.

Size measurement with fine particles


 Dry screening is useful for sizing particles with diameter greater than about 44 μm (325
mesh).
 Wet screen analysis can be used for diameters down to 10 μm.
 Optical microscopy and gravity sedimentation are used with particles 1 – 100 μm.
 Coulter counter, a device used for sizing and measuring particles by measuring change in
resistivity of an electrolyte as it carry particle one by one through a small orifice. Light
scattering techniques, sedimentation in centrifuges and electron microscopy are other useful
method for measuring size of even smaller particles.
Students Self Study
 Microscopic analysis (1–100 μm)
 Sedimentation and elutriation methods (>1 μm)

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 Permeability methods (>1 μm)
 Electronic particle counters
 Laser diffraction analysers
 X-ray or photo-sedimentometers
 Sub-micron particle sizing

Particle size distribution

-Most particulate systems of practical interest consist of particles of a wide range of sizes and it is
necessary to be able to give a quantitative indication of the mean size and of the spread of sizes.
- The results of a size analysis can most conveniently be represented by means of a cumulative mass
fraction curve, in which the proportion of particles (x) smaller than a certain size (d) is plotted against
that size (d).
-In most practical determinations of particle size, the size analysis will be obtained as a series of steps,
each step representing the proportion of particles lying within a certain small range of size. From
these results a cumulative size distribution can be built up and this can then be approximated by a
smooth curve provided that the size intervals are sufficiently small.

-The distribution of particle sizes can be seen more readily by plotting a size frequency curve, such as
that shown in Figure 1.6, in which the slope (dx/dd) of the cumulative curve (Figure 1.5) is plotted
against particle size (d). The most frequently occurring size is then shown by the maximum of the
curve.

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For naturally occurring materials-single peak. For mixtures of particles, there may be as many peaks
as components in the mixture. Again, if the particles are formed by crushing larger particles, the curve
may have two peaks, one characteristic of the material and the other characteristic of the equipment.

Mean particle size


-A mean size will describe only one particular characteristic of the powder and it is important to
decide what that characteristic is before the mean is calculated. Thus, it may be desirable to define the
size of particle such that its mass or its surface or its length is the mean value for all the particles in
the system.
-Assuming each particle has same shape,
Consider unit mass of particles consisting of n1 particles of characteristic dimension d1, constituting a
mass fraction x1, n2 particles of size d2, and so on, then:

And

Thus

If the size distribution can be represented by a continuous function, then:

Or

And

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where is the density of particles, and

is a constant whose value depends on the shape of the particle.


Mean sizes based on volume

Volume mean diameter,

Expressing the above relation in finite difference form, then:

In terms of particle numbers other than mass fractions, we have

Mean volume diameter,

If all particles are of diameter , then the total volume of particles is the same as in the mixture.

Thus:

Substituting from Eqn gives

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=

Mean sizes based on surface

If, instead of fraction of total mass, the surface in each fraction is plotted against size, then a similar
curve is obtained although the mean abscissa ds is then the surface mean diameter.

Thus:

where , and k2 is a constant whose value depends on particle shape. ds is also known as the
Sauter mean diameter and is the diameter of the particle with the same specific surface as the powder.
Substituting for n1 gives

Mean surface diameter

The mean surface diameter is defined as the size of particle which is such that if all the particles
are of this size, the total surface will be the same as in the mixture.

Thus:

Substituting for n1 gives

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Mean dimensions based on length
A length mean diameter may be defined as:

A mean length diameter or arithmetic mean diameter may also be defined by:

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