DEFINITION

a jumbled cluster or mass of varied parts.

the act or process of agglomerating

Selection of an Agglomeration Method

By: Sara Gantner, Application Engineer
Hosokawa Bepex, Minneapolis, MN
1. ABSTRACT
Agglomeration is the process of transforming fine particles into
larger particles by the
introduction of external forces, and is a value-added step in many
processes involving powdered
materials. There are many different reasons to agglomerate,
including increased flowability and
improved product shape and appearance.
With the multitude of options available to achieve an agglomerated
product, it can be
difficult to narrow down the best method for your application. The
main factor in selecting the
right kind of equipment is to specify the type of end-product
required. The particle size
distribution, shape, hardness, solubility and dispersability, and
binder addition requirements will
point to a certain type of agglomeration equipment.
I will outline the most common options, and clarify the product
characteristics of each.
This review should be helpful for the novice, and is a good
reminder of other options for those
already proficient.
2. INTRODUCTION
Agglomeration is the process of transforming fine particles into
larger particles by the
introduction of external forces, and is a value-added step in many
processes involving finely
divided solid materials.
There are many different reasons to agglomerate. Agglomeration
will minimize or
eliminate dusting, which will improve storage and handling
characteristics as well as making the
environment safer for people working with the material. It will
improve flowability, which
improves metering and dosing characteristics. Segregation within
bulk blends is eliminated
through coagglomeration of materials. It can also be used to
increase or control bulk density, or
to produce a defined shape, size, or weight product. Some methods
of agglomeration will also
allow control of solubility and dispersibility. The end result is a
product offering more valuable
to you or your customer.
With the multitude of options available to produce an
agglomerated product, it can be
difficult to narrow down the best method. I will outline the most
common options, and clarify
the product characteristics of each. This review should be helpful
for the novice, and is a good
reminder of other options for those already proficient.
3. SELECTION OF A PROCESS
Most materials could be agglomerated using any of the methods
listed below. The main
factor in selecting the right kind of equipment is to specify the type
of end-product required. The
particle size distribution, shape, hardness, solubility and
dispersibility, and binder addition
requirements will point to a certain type of agglomeration
equipment. Having a well-defined
product specification early on will streamline the selection process.
Common characteristics for
various product types are detailed in Table 1 below.
Table 1. Product Comparison.
Product Form
/Product
Properties Onion Skin Agglomerate(Mixing) Extrudate
Hollow
Sphere Granule Briquette Flowing Properties
443143
Bulk Density 4 3 3 1 4 2
Dispersability 1 4 2-3 3 1 1
Instant
Characteristics
1 4 2-3 3 1 1
Particle Size 1-5 mm 0.2-1.2 mm 0.3-5 mm < 200μm 0.1-5 mm
5 mm+
4 – Very good / excellent
3 – good
2 – moderate
1 - poor
The initial state of the feed material to your process will point
toward certain methods, as
will any requirement on purity. If the feed is a paste, extrusion
should be considered, as an
example. If your material is very sensitive to binder addition, dry
agglomeration may be the only
viable option.
The combined capital and operating costs for any agglomeration
system are typically
quite similar. If the system does not include curing or post drying,
this would be an exception.
Therefore, it is best to narrow down the equipment choices first
through product and feed
specifications, before concentrating on the costs for the system.
4. TYPES OF AGGLOMERATION
There are four main categories of agglomeration. The first is
pressure agglomeration,
which includes briquetting, compaction granulation, tabletting, and
others. The second is
tumbling agglomeration, which includes drum, disc, cone, pin
mixer, and others. The third is
extrusion, which includes low pressure screw, gear pelletizer,
pellet mill, and others. The last is
thermal, which includes flaking, pastillating, prilling, sintering, and
others. These methods are
outlined in more detail below.
4.1 PRESSURE AGGLOMERATION
In pressure agglomeration, material masses are subjected to high
forces. The application
of high pressure causes partial crushing and realignment of the
individual particles. The pressure
can be high, in excess of 30,000 psi. This results in the particles
being forced into close
proximity, where interparticle forces result in binding.
Pressure agglomeration can be accomplished using a variety of
units, including roll
compactors, tablet presses, and piston presses. This is a dry method
of agglomeration, which
generally requires little or no binder addition, instead relying on
interparticle forces for
agglomeration. High density products are produced at a high
capacity with relatively low energy
input. Products will be of uniform size and shape, and can be
relatively large compared to other
methods. Because of the high density of these products, their
dispersability is generally limited.
One of the most common examples of high capacity pressure
agglomeration is roll
compaction. A double roll compactor is pictured in Figure 1. In
this unit, material is force fed in
the top by a feed screw. It is then drawn between the counter
rotating rolls where it is partially
crushed, and formed to the shape on the surface of the rolls.
Individual briquettes can be formed
in a variety of shapes. For granulation, a sheet of material is
produced. This is then crushed and
screened to size.
Some examples of products made with pressure agglomeration are
charcoal briquettes,
salt pellets for water softeners, pills, and fertilizers. Common
characteristics of all these
products are a high density, uniform shape, and slow dispersibility.
As a general rule, one would consider this type of agglomeration
if:
1. Binder addition is not allowed
2. High density or resistance to attrition is desired
3. Large particles (greater than 1”) or particles of controlled size
are required.

Figure 1. Double Roll Compactor

4.2 TUMBLING AGGLOMERATION
In tumbling agglomeration, material masses are combined with a
binder and subjected to
rolling or tumbling forces to form loose agglomerate structures.
Agitation can be high or low
shear, depending on the equipment. The feed to this type of system
is typically a fine powder.
Binding is generally accomplished by liquid bridges or chemical
reaction.
Tumbling agglomeration can be accomplished on a variety of
units, including drum or
cone mixers, pan or disc agglomerators, and pin mixers. This is a
wet method of agglomeration,
meaning a binder or moisture must be added to accomplish the
particle enlargement. This is a
good method for dedusting materials, or prior to waste disposal.
Tumbling agglomeration
systems typically have high capacities, and offer a low capital cost
if post drying or curing is not
necessary.
A pin or paddle mixer is a good example of a unit used to dedust
materials. Figure 3
below shows an example of a paddle mixer. This unit is fed dry
powder through the large inlet at
one end, and liquid through the couplings slightly downstream. In
this unit the paddles are
adjustable to allow one to tailor the degree of mixing to a certain
application.
Another of this type of agglomerators is the Schugi Flexomix that
is often used in
instantizing. This agglomerator is shown in Figure 2. The
Flexomix combines the powder and
liquid in a high shear environment. The granules are relatively
porous, and easily dispersed.
The agglomerates will require drying, typically in a fluid bed
dryer. The high speed contact of
the mixer yields smaller more uniform particles in a short
residence time.
Some examples of products made using tumbling agglomeration
are detergents, instant
drink mixes, fly ash dedusting, and agricultural chemicals.
Common characteristics of these
products are medium to low density, good flowability, easy
dispersion, and a rounded or
raspberry shape.
As a general rule, one would consider this type of agglomeration
if:
1. Binder addition is allowed and anticipated
2. An economical means of wetting a powder for dedusting
3. Easy dispersion is required
Figure 2. Schugi Flexomix, Instant Mixer Figure 3. Turbulizer,
Paddle Mixer
4.3 EXTRUSION AGGLOMERATION
In extrusion agglomeration, material masses are subjected to forces
pressing them
through a die plate to form pellets. Pressure ranges from low to
high depending on the type of
extruder chosen. Feed to an extruder must be formable by the die,
meaning it must be a wetcake,
paste, or dough, or form one through the mixing process in the
extruder.
Extrusion agglomeration can be accomplished on a variety of units,
including single
screw extruders, gear pelletizers, basket type extruders, and pellet
mills. Often curing or post
drying is required. The material is forced through some type of die
to form the granules, which
makes the particle size of the product very uniform. An extruder
will typically produce a
medium density product that is good for time release applications.
It will have the capacity to
handle sticky and high viscosity products.
This method of agglomeration requires the material to be formable
by the die. This
means the material must either have a melting component, or a
binder or moisture must be added
to it. Some extruders have the capability to mix the feed materials
prior to extrusion; however, it
is more common to feed a premixed material. Figure 4 shows an
extruder capable of mixing
internally. Figures 5 and 6 show a gear pelletizer, which must be
fed premixed material.
Some examples of products made using extrusion agglomeration
are animal feeds, wood
products, and polymers. Products from extrusion equipment will be
cylindrical in shape.
Typically, the diameter will be between 1 and 10 mm, and length
will be fairly uniform. The
particles will have a constant cross section due to the die forming
process. Products typically
have a density between that of tumbling agglomerates and pressure
agglomerates, and a medium
dispersibility as well.
Extrusion can be followed by spheronization, to round the edges of
the cylindrical
product and form spheres. This is accomplished on a spheronizer, a
flat bottomed bowl shaped
unit, with a spinning disc on the bottom surface. The pellets are
spheronized while still green to
allow reagglomeration of fines created during the process.
As a general rule, one would consider this type of agglomeration
if:
1. Feed is a wetcake or paste
2. Pellet or Spherical shape is required
3. Small uniform particles are required

Figure 4. Extrudomix, Mixing Screw Extruder

Figure 5. Gear Pelletizer

Figure 6. Gear Pelletizer, Material

Flow Diagram
4.4 THERMAL AGGLOMERATION
Thermal agglomeration is a wide category focusing on
agglomeration using heat transfer
processes. These processes involve sintering through heat
application, solidification through
cooling, or coagulation through melting. Examples of equipment in
this category include drum
flakers, rotary kiln nodulizers, prilling towers, etc. Since the
category is so varied, it is difficult
to generalize the characteristics of products produced.
One common example of this type of equipment is a prilling tower.
A prilling tower
requires a hot melt feed material. The feed is formed into droplets
by various methods, and the
droplets fall through the tower through a countercurrent of air. This
allows the material to
harden, and form roughly spherical products. Typical particle size
is 300 micron for this method,
larger products would require more falling distance to sufficiently
harden. This process can be
followed by a fluid bed dryer to fully dry the newly formed
agglomerates.
Some examples of products produced using thermal agglomeration
are stearic acid prills,
fatty acids, and gelatin.
5. BATCH VS CONTINUOUS PROCESSING
Most of the equipment described above operates continuously.
Another factor to
consider when choosing equipment is whether batch or continuous
processing is best for your
operation.
Batch processing is mainly used when the production rate is very
low, or product is only
required intermittently, or when material tracing is required. It can
also be a good option when
producing a wide range of different products, making frequent
cleanout necessary. Batch
processing has the advantage that off spec material can easily be
identified and separated from
the final product stream.
Continuous processing is typical for a plant with high production
rates and few different
product specifications. Continuous processing will be more
economical for these large rates due
to decreased labor demand, and more uniform end products.
6. CONCLUSIONS
Agglomeration equipment is the key part of a total agglomeration
system, which can
include mixing, size reduction, drying, and particle size
classification and recycle.1 As noted
above, there are many options available for agglomeration.
Defining the desired characteristics
of the end product is the most important step in choosing the
correct agglomeration equipment
for your process. Most materials can be agglomerated on many
types of equipment listed, but
products from each of the machines will have different
characteristics. However, once product
characteristics are defined, the choices of agglomeration equipment
can be narrowed down, and
then testing can be done to verify the machine that will produce an
end-product that meets
specifications.
7. REFERENCES
1. Gantner, S. “Condensing the Finer Points of Agglomeration.”
Chemical Engineering. May
2003.
Engelleitner, W.H. “Selection of the Proper Agglomeration
Process”, IBA Proceedings 17th
Biennial Conference. August 1981.
Holley, C.A. “Binders and Binder Systems for Agglomeration”,
IBA Proceedings 17th Biennial
Conference. August 1981.
Komarek, K.R. “Selecting Binders and Lubricants for
Agglomeration Processes”, Chemical
Engineering. December 4, 1967.
Pietsch, W. “How to Select an Agglomeration Method”, Powder
and Bulk Engineering.
February 1999.

Powder agglomeration is used in a wide variety of the chemical

process industries (CPI), and a virtually endless number of process
options are available. Selection requires engineers to make a
substantial number of design decisions, such as the choice between
wet or dry processing, the intensity of mixing and shear rates,
continuous versus batch operation, cross contamination of products
and ease of cleaning. These choices must be made in light of
desirable agglomerate end-use properties. Key agglomeration
mechanisms and their impact on agglomeration processing are
reviewed in this article. The impact on process selection is also
touched upon within the context of mechanisms
ROASTING
the use of heat for the treatment of an ore, includes smelting and
roasting. If the ore is an oxide, it is heated with a reducing agent,
such as carbon in the form of coke or coal; the oxygen of the ore
combines with the carbon and is removed in carbon dioxide, a gas
(see oxidation and reduction). The waste material in the ore is
called gangue; it is removed by means of a substance called a flux
which, when heated, combines with it to form a molten mass called
slag. Being lighter than the metal, the slag floats on it and can be
skimmed or drawn off. The flux used depends upon the chemical
nature of the ore; limestone is usually employed with a siliceous
gangue. A sulfide ore is commonly roasted, i.e., heated in air. The
metal of the ore combines with oxygen of the air to form an oxide,
and the sulfur of the ore also combines with oxygen to form sulfur
dioxide, which, being a gas, passes off. The metallic oxide is then
treated with a reducing agent. When a carbonate ore is heated, the
oxide of the metal is formed, and carbon dioxide is given off; the
oxide is then reduced.

• pyrometallurgy (in metallurgy: Roasting)

As stated above, for those instances in which a metal-bearing

compound is not in a chemical form that permits the metal to
be easily and economically removed, it is necessary first to
change it into some other compound. The preliminary
treatment that is commonly used to do this is roasting.

• uranium (in uranium processing: Roasting)

The hydrometallurgical processing of uranium ores is

frequently preceded by a high-temperature calcinations step.
Roasting dehydrates the clay content of many ores, removes
 carbonaceous materials, oxidizes sulfur compounds to
innocuous sulfates, and oxidizes any other reductants that
may interfere in subsequent leaching operations.

• zinc (in zinc processing: Roasting and sintering)

For the electrolytic production of zinc, the roasting of

concentrates is achieved in fluidized-bed roasters, in which
finely divided and heated particles of concentrate are
suspended in a rising stream of air. The sulfur content can be
reduced to less than 0.5 percent, and a high-strength (10
percent) sulfur dioxide gas is forwarded to a...

Agglomeration, whereby the moist sticky particles collide due

to the turbulence and adhere to each other forming
agglomerates, is essential for the rewet process.

As powders with different compositions do not behave in the

same way during the rewetting and agglomeration process,
different equipment is needed to obtain an optimal
agglomeration.

In principle there are two ways of performing the

agglomeration:

• Droplet agglomeration
• Surface agglomeration
Process for the agglomeration of solids
The present invention pertains to a two-stage agglomeration process for coal fines in the
form of a pumpable slurry. The slurry is selectively agglomerated in the first stage by the
addition of a hydrocarbon binder and the bulk of the water separated from the resulting
agglomerates. Improved agglomerates are obtained in the second stage where those from
the first stage are resubmitted to turbulent motion in hot water, which is drained from the
agglomerates and recirculated thus reducing energy requirements.

1. A process for the agglomeration of finely divided solids in an aqueous suspension, said
solids being selected from the group consisting of ores and coal, comprising:

passing the suspension through a first zone where it is subjected to turbulence in the
presence of a hydrocarbon binder having a softening point between 30° C. and 120° C.
which causes loose agglomerates to be formed;

substantially separating the agglomerates from the water; and,

passing the agglomerates to a second zone containing hot water and subjecting the
agglomerates to turbulence in the presence of a hydrocarbon binder having a softening
point between 30° C. and 120° C.

2. A process as claimed in claim 1 including separating the agglomerates from the heated
liquid and recirculating the heated liquid to the second zone.

3. The process as claimed in claim 1, in which the hydrocarbon binder is introduced into
the first zone in the form of an emulsion.

4. The process as claimed in claim 1, in which the temperature of the heated liquid in the
second zone is maintained between 60° C. and 85° C.

5. The process as claimed in claim 1, in which between 4 and 12%w, based on the weight
of solids to be separated, of the hydrocarbon binder is added.

6. The process as claimed in claim 1, in which a light hydrocarbon binder is introduced in

the first zone to improve the selectivity of the agglomeration of the solids over any
contaminating material present and said binder is at least partly removed from the
agglomerates in the second zone due to the higher temperature in that zone.

7. The process as claimed in claim 1, in which powdered bitumen is added in the second
zone as a binder.

8. A process for the agglomerization of finely divided solids in an aqueous suspension,

said solids being selected from the group consisting of ores and coal, comprising,
subjecting the solids to turbulence in the presence of a hydrocarbon binder to form
agglomerates and then further subjecting the agglomerates to turbulence in the presence
of a hydrocarbon binder at a higher temperature, both said hydrocarbon binders having a
softening point between 30° C. and 120° C.

9. The process as claimed in claim 8 wherein the higher temperature is above the
softening point of the hydrocarbon binder used to form the agglomerates.

10. The process as claimed in claim 8 where the first recited hydrocarbon binder has a
lower softening point than the second recited hydrocarbon binder.

Description:

BACKGROUND OF THE INVENTION

This invention relates to a process for the agglomeration of finely divided solids, and in
particular those in the form of an aqueous suspension.

In general, agglomeration is carried out by subjecting finely divided solids to turbulence

in the presence of a binder which is capable of wetting the surface of the solids. Selective
agglomeration takes place when the binder alone, or possibly in the presence of another
agent, wets the surface of the solids preferentially over that of any contaminating material
present.

Agglomeration is used for upgrading finely divided solids such as ores, and in particular
coal, and also to facilitate dewatering. Selective agglomeration is useful for the
enrichment of ores and for separating coal from gangue.

Hydrocarbon binders, such as bitumen, coal tar, short residues and the like, tend to
produce good agglomerates. In choosing a binder for selective agglomeration much more
care has to be taken. In general the most selective binders tend to be the lighter
hydrocarbons, but these do not always produce the best agglomerates.

The present invention not only seeks to provide harder agglomerates, but also to reduce
the energy input necessary for their production.

SUMMARY OF THE INVENTION

In accordance with the invention a process for the agglomeration of finely divided solids
in an aqueous suspension comprises passing the suspension through a first zone where it
is subjected to turbulence in the presence of a hydrocarbon binder which causes
agglomerates to be formed, separating the latter from water and any unagglomerated
material, passing the agglomerates to a second zone containing water at a temperature
above the softening point of the binder, where they are subjected to turbulence in the
presence of a hydrocarbon binder (which need not be the same as the one employed in the
first zone), and separating the resulting agglomerates from the hot water and recirculating
the latter to the second zone.

Broadly, the present invention pertains to forming agglomerates by vibration in the

presence of a binder in two zones, one at a higher temperature than the other, in order to
produce higher quality pellets.

DESCRIPTION OF PREFERRED EMBODIMENTS

In practice, the binder for use with the present invention is chosen so that it does not have
a viscosity in excess of 4000 mm 2 /s at the agglomeration temperature. Where this is not
possible, the binder may be emulsified as an unstable emulsion by mixing it vigorously
with water at elevated temperature according to known techniques. Stabilized emulsions
may also be used as mentioned below.

The process of the invention has the advantage that due to the elevated temperature in the
second zone pellets are formed which are hard at ambient temperature, which can be
much more easily handled, and thus have a higher market value.

The temperature of the water will advantageously be between 60° C. and 85° C. so that
the vessel does not have to be pressurized, but should it be desirable, due to, for example,
the type of bitumen to be used, to operate at a higher temperature, then it is of course
possible to pressurize the vessel so that the water remains in the liquid phase.

By using a separate charge of water in the second zone, and by recirculating it a large
proportion of its heat energy is conserved. Furthermore, a very considerable saving is
achieved by not having to heat up the whole of the water phase in which the solids are
suspended on entry into the first zone.

It also permits the optional use of a relatively more volatile binder in the first zone, which
can improve the selectivity of the agglomeration process. Such a more volatile binder can
be partially or wholly recovered in the second zone where it tends to be evaporated off
due to the higher temperature obtaining there.

The binder may be a bitumen, coal tar or short residue, whose softening point (R&B) is
between 30° C. and 120° C., but as softer binders (those having a softening point between
30° C. and 60° C.) are more effective for selective agglomeration, these tend to be
preferred if a single binder is to be used.

Normally, 6 to 12%w binder (based on the solids material to be separated) will be

sufficient.

If the binder is introduced without taking any precautions it may not be evenly distributed
over the whole of the volume of the zone in which it is introduced or the distribution may
be too slow. It is therefore advantageous to do so in the form of an emulsion which
dilutes itself rapidly in the obtaining turbulent conditions. Where an emulsifying agent is
present it can promote more rapid agglomeration of the solids, perhaps due to the
emulsifying agent improving the wetting properties of the binder on the solids or the
compaction of the particles.

Often emulsifiers used for bitumen emulsions comprise essentially alkaline soaps of
higher fatty acids but these may only be moderately suitable for this purpose. Better
results can sometimes be obtained with a special emulsion prepared with approximately
3% by weight (based on the proportion of bitumen) of alkaline naphthenate. Where more
rapid agglomeration takes place this evidently can result in additional energy and cost
savings.

Where some of the binder is to be added only in the second zone, it may be introduced in
powdered form such as powdered bitumen whose softening point (R&B) is below the
temperature obtaining in the second zone.

The invention is particularly suitable for upgrading and dewatering coal slurries either
after pipeline transport or of normal run-of-mine fines. In such slurries the fines usually
have a maximum dimension of up to, say, 1 to 2 mm and as such are difficult to handle;
they must also remain relatively wet to prevent dusting. After treatment in accordance
with the invention they are in the form of relatively hard pellets having a diameter of up
to 20 mm--the larger the pellets desired, the longer they must be submitted to the
turbulence, and thus the more expensive they are. The pellets will also have a reduced
water content which is acceptable to customers wishing to use them in conventional coal-
burning applications.

In addition, where the solids enter the agglomeration process with contaminating matter,
the resulting pellets will normally contain a significantly lower porportion of the
contaminating material due to the selectivity of the first agglomeration step. If still more
selectivity is required, an intermediate grinding step may be introduced after the first
zone, in which the loose agglomerates are reground. They are then passed to an
intermediate zone or even the above-mentioned second zone for more selective
reagglomeration to remove a proportion of the impurities.

The invention will be further described by way of example with reference to the
accompanying drawing, which is a flow scheme of an agglomeration process in
accordance with the invention for a coal slurry comprising an aqueous suspension of coal
fines and some gangue.

The slurry with a proportioned hydrocarbon binder enters a first zone or vessel 10 by
lines 12 and 13 and is subjected to turbulence by means of a stirrer 14 driven by a motor
16. Loose agglomerates so formed, together with some unagglomerated material and a
corresponding quantity of water, leave the first vessel by a line 18 and are separated by
means of a moving screen 20. The water and unagglomerated matter are removed through
a line 21 and may be recirculated to the first vessel 10 after settling and decanting the
excess water and gangue (this step is not shown the flow scheme).
The loose agglomerates are then passed via a line 24 to a second zone or vessel 22
containing hot water. The agglomerates are again stirred vigorously by means of a stirrer
26 driven by a motor 27. After remaining in the second vessel for the desired residence
time, the enlarged and hardened agglomerates in pellet form leave the vessel by line 28
with a corresponding quantity of water and are pased over a screen 30. Dewatered
agglomerates can then be stored in heaps, bins or hoppers.

The hot water drained from the agglomerates is passed via a line 31 to a reservoir 32
whence it is recirculated by a pump 34 via a heat exchanger 36 in which it is reheated to
the desired operating temperature of the second vessel 22. Ash is removed from the
reservoir 32 by a line 40 and may conveniently be recirculated to the first vessel.
Unagglomerated particles are recirculated to the second vessel with the water.

In a typical case a dilute coal slurry containing 9 m 3 of water to 3 tons of hard coal fines
having a maximum dimension of 1 mm and an ash content of 17% is introduced into a
first vessel 10 together with 20% by weight (based on the coal) of an unstabilized 50%
emulsion of bitumen having a penetration 50-60 pen at 25° C. (softening point
approximately 50° C.). After a mean residence time of 15 minutes the corresponding
quantity of loose agglomerates and water and ash are passed over the screen 20. An
amount of 8.3 tons of water are drained together with the unagglomerated ash. The
remaining 3 tons of coal agglomerates (now with 8.2% of ash) and 1 ton of water enter
the second vessel 22 and are mixed with 8 tons of water at 95° C. to produce a mixture at
80° C. After a residence time of 20 minutes the resulting pellets of 5 to 20 mm diameter
are separated from the hot water on the screen 30. They had an average water content of
approximately 10% and the ash content had fallen to 7%.

A more effective de-ashing method could have been carried out by introducing a small
quantity of a light-hydrocarbon binder such as butane into the first vessel 10, which
would necessitate sealing off from the atmosphere the solids between the first and second
vessels. Any light hydrocarbon binder remaining in the agglomerates is flashed off due to
the higher temperature obtaining in the second vessel and can be recovered. It can be
replaced by adding a corresponding quantity of powdered bitumen in the second vessel.

Improved de-ashing of the coal can also be obtained by regrinding the coal between the
first and second vessels.

Oil agglomeration process

In methods for producing agglomerate particles from aqueous slurries containing from
about 10 to about 40 weight percent solids, the solids comprising finely divided
carbonaceous solids and finely divided inorganic solids, by mixing the aqueous slurry
with oil in a first mixing zone to form a mixture and thereafter further agitating the
resulting mixture in at least one other mixing zone to produce agglomerate particles
containing the carbonaceous solids and the oil and recovering the product agglomerate
particles, an improvement comprising (a) separating finely divided inorganic solids from
the aqueous slurry after removal of the product agglomerate particles therefrom; (b)
thereafter separating smaller agglomerates of carbonaceous solids and oil from the
aqueous slurry after separation of the product agglomerate particles and the inorganic
solids therefrom; and (c) recycling the smaller agglomerates to the second mixing zone.

1. In a method for producing agglomerate particles from an aqueous feed slurry

containing from about 10 to about 40 weight percent solids, said solids comprising finely
divided carbonaceous solids and finely divided inorganic solids said inorganic solids
comprising sand, pyrites and clays by mixing said aqueous slurry containing said solids
and oil in a first mixing zone to form a mixture and thereafter further mixing said mixture
in at least one other mixing zone thereby forming product agglomerate particles
containing said carbonaceous solids and said oil and recovering said product agglomerate
particles, the improvement comprising;

(a) separating finely divided inorganic solids consisting of sand, pyrites and clays from
said aqueous slurry after separating said product agglomerate particles therefrom;

(b) thereafter separating smaller agglomerates of said carbonaceous solids and oil below
the size selected as the minimum in said agglomerate recovery step from said clay
containing aqueous slurry after separation of said product agglomerate particles and said
inorganic solids therefrom; and

(c) recycling said smaller agglomerates to said other mixing zone.

2. The improvement of claim 1 wherein said smaller agglomerates are smaller than 28
Tyler mesh.

3. The improvement of claim 1 wherein said agglomerates contain from about 10 to about
15 weight percent oil.

4. The improvement of claim 1 wherein said inorganic solids are separated in a cyclone.

5. The improvement of claim 1 wherein said smaller agglomerates are separated in a

cyclone.

Description:

This invention relates to the recovery of finely divided carbonaceous solids from aqueous
slurries.

This invention further relates to the selective recovery of finely divided carbonaceous
solids from aqueous slurries containing finely divided carbonaceous solids in mixture
with finely divided inorganic solids.
This invention further relates to the recovery of finely divided carbonaceous solids from
aqueous slurries containing finely divided carbonaceous solids and finely divided
inorganic solids by mixing the aqueous slurry with oil thereby agglomerating the
carbonaceous solids and oil into agglomerate particles which are readily recovered for
use as particulate fuel and the like.

In coal mining processes, a cleaning step is normally used to remove inorganic materials
and the like from the coal product. As a result of such cleaning steps, a by-product stream
is usually produced which contains finely divided carbonaceous solids and finely divided
inorganic solids. Such streams in the past have been passed to blackwater ponds for
storage and allowed to accumulate. Water is, in some instances, withdrawn from the
blackwater pond and recycled to the process, and in other instances the water is merely
allowed to evaporate from such ponds. Clearly, the presence of such ponds containing the
carbonaceous solids present a continuing threat of overflow and the like with the
resulting unsightly pollution of the downstream areas. Further, the carbonaceous solids
contained in such ponds represent the loss of a valuable fuel product. Accordingly,
increasing efforts have been directed to methods whereby such finely divided
carbonaceous solids can be recovered, both from such waste streams and from blackwater
ponds in a form suitable for use as fuels, coke oven feedstocks and other applications
known to those in the art for coal.

One such process comprises the mixing of aqueous slurries containing finely divided
carbonaceous solids and finely divided inorganic solids with oil to thereby selectively
agglomerate the carbonaceous solids and oil to produce particulate fuels. In such
processes, varying amounts of carbonaceous material are produced as very small
agglomerates, i.e. less than 28 Tyler mesh and is eventually lost at a screening operation
or the like where the larger product agglomerates are separated and passed to use as a fuel
or the like. The amount of carbonaceous material lost at the screening operation is of
course dependent upon the effectiveness of the agglomeration process, the nature of the
aqueous slurry passed to the process and the like. In any event, it is highly desirable that
such small agglomerates which have been through the process already, be recovered
since they constitute a potentially valuable fuel.

It has now been found that such small carbonaceous agglomerates which have already
been through the process and, as a result, treated with oil, are readily recovered by
subjecting the underflow stream from the screening operation to cycloning. A first
cyclone is used to separate sand, pyrites, clays and the like from the aqueous underflow
stream with the overflow from the cyclone being passed to a second cyclone which is
adapted to recover such small carbonaceous agglomerates for recycle to the
agglomeration process.

FIG. 1 is a schematic diagram of a process utilizing the improvement of the present

invention.

In FIG. 1, an inverter 10 including a stirrer 12 is shown. A coal slurry is charged to

inverter 10 through a line 14 with oil being charged to inverter 10 through a line 16. It is
understood that while the addition of the coal slurry is shown through a single line, that
the coal and water could be added separately if desired for any reason. In inverter 10, the
mixture is vigorously stirred and inversion occurs. The term `inversion` is used to refer to
the phenomenon wherein the carbonaceous solids become coated with oil and begin to
agglomerate and separate from the aqueous medium. After inversion, the mixture is
passed through a line 18 to a first agglomerator vessel 22 which includes a stirrer 24
where the mixture is agitated further to result in the production of larger agglomerates
which are then passed as an aqueous slurry through a line 26 to a second agglomerator 30
including a stirrer 32 where the mixture is further agitated although optionally at a lower
rate to produce still larger agglomerates which are then passed as a slurry through a line
34 to a screen 40 where the product agglomerates are recovered and passed to product via
a suitable conveyor 42 with the underflow from the screen being passed to further
processing through a line 44. The screen may be of any suitable size, although it is
preferred that a 28 Tyler mesh be used. As a result, the product agglomerates will be
larger than 28 Tyler mesh with those solids which are smaller than 28 Tyler mesh being
found in the underflow from the screen. The underflow from the screen flowing through
line 44 is passed to a first cyclone, shown as a hydroclone 50, which is designed to
separate sand, pyrites, clays and other inorganic solids from the underflow stream. The
underflow from first cyclone 50 is discharged via a line 52 to waste or the like and the
overflow from first cyclone 50 is passed through a line 54 to second cyclone, shown as a
hydroclone, 56 wherein the small carbonaceous agglomerates are separated and passed
through a line 58 back to join the aqueous slurry flowing through line 18 to agglomerator
22. The overflow from second hydroclone 56 is passed through a line 60 to a thickener
and optional water recycle or the like.

As is known to those skilled in the art, the coal slurry passed to inverter 10 desirably
contains from about 10 to about 40 weight percent solids and oil is normally added to
vessel 10 in an amount equal to from about 10 to about 20 weight percent based on the
amount of carbonaceous solids contained in the aqueous slurry charged to inverter 10.
The agglomerates produced from screen 40 typically contain from about 10 to about 15
weight percent oil. The agitation in inverter 10 is at a relatively high mixing rate, with
mixing rates from about 0.1 to about 1.25 hp/ft. 3 being suitable. Values from 0.15 to
about 0.5 hp/ft. 3 are more typical. The agitation rates in first agglomerator 22 and second
agglomerator 30 are normally somewhat lower than values from about 0.1 to about 0.4
hp/ft. 3 being typical. Typically, the agitation rate in second agglomerator 30 is somewhat
lower than in first agglomerator 22. First hydroclone 50 is designed to selectively
separate sand, pyrites, clays and other heavy finely divided inorganic materials without
removing the small carbonaceous agglomerates from the aqueous stream. Similarly,
second hydroclone 56 is designed to selectively remove the small carbonaceous
agglomerates from the clay-containing water.

The design of cyclones to accomplish such objectives is known to those skilled in the art
and would be determined by the internal design of the cyclone, the fluid velocity in the
cyclone, the differential pressures used across the cyclone, and the like. Such design
parameters are well known to those skilled in the art and need not be discussed further.
Cyclones are widely used in the cleaning of fine coals, etc. and are of a variety of types
such as hydroclones, triclones and the like as known to the art.

Desirably, the stream containing the small carbonaceous agglomerates is recycled to first
agglomerator 22 since this stream has already been subjected to the inversion step
occurring in vessel 10. The loss of such small agglomerates is particularly undesirable
since they have already been treated with oil and are suitable for agglomeration. Upon
recycle to first agglomerator 22, these small agglomerates are placed back into the
process at a point where their further agglomeration is readily accomplished. It is pointed
out that the steps of the improvement must be accomplished in the sequence shown since
it is highly undesirable that the finely divided inorganic solids, sands, pyrites and the like
be recycled to the process. It is particularly undesirable that these materials be returned to
the process after the inversion step. Accordingly, it is clear that the first separation step is
necessary in order to achieve the desired objectives of the present improvement. The use
of the present improvement is particularly effective in eliminating the loss of desirable
materials during start-up operations, during process upsets wherein the composition of
the incoming coal slurry may be rapidly varied, and the like. It is undesirable that
substantial quantities such small agglomerates be permitted to pass to the thickener and to
waste if such can be prevented. The improvement of the present invention presents a
method whereby the loss of such materials is eliminated by recycling such materials back
to the process prior to passing the aqueous stream from the screen to thickening, recycle
or the like. While the aqueous stream may have formerly been passed to recycle,
normally most, if not all, of the solid materials and any excess oil would have been
removed in the thickener.

Having thus described the present invention by reference to certain of its preferred
embodiments, it is pointed out that many variations and modifications are possible within
the scope of the present invention and it is believed that many such variations and
modifications may appear obvious and desirable to those skilled in the art upon a review
of the foregoing description of preferred embodiments.

Industrial applications of the

agglomeration process
Environmental, technological and economic problems caused by utilization of low
quality and low rank coals and serious concerns related to a growing number of polluted
industrial waste sites have significantly increased interest in further development and
application of oil agglomeration technology. Study performed at the Alberta Research
Council on the various applications of the spherical agglomeration process led to the
development of different technologies applicable for coal cleaning, upgrading,
handleability improvement or moisture reduction. The other important applications were
recovery of combustible material from rejects and settling ponds and remediation of soils
contaminated with various hydrocarbons.
The preparation and handling of fine coal is a key issue to many coal mine operators and
the efficient recovery of coal from fines streams could have a profound effect on
increased plant productivity and reduction of the potential environmental liabilities
associated with waste generation, accumulation and disposal.
To overcome the problems associated with coal fines and hydrocarbon-contaminated
soils, ARC researchers have, over the last 20 years, placed particular emphasis on the
development and testing of improved coal preparation and soil remediation technologies.

Wet agglomeration of powders: from

physics toward process optimization
A general method to optimize a wet powder agglomeration process for achieving
desired properties of granulated products is suggested. The different states of a wet
powder are characterized by a cohesion function, i.e. the evolution of the torque of the
stirred system as a function of the moisture content. Two different types of
agglomeration behaviours are shown: Stepwise Growing Behaviour (SGB) and
Continuous Growing Behaviour (CGB). The influence of various parameters such as the
particle-size distribution and the wettability of the solid surface on the cohesion function
are highlighted. Such functions are shown to be very helpful to define the granulation
process and the properties of the granulated products, revealing a promising
methodology.

An interdisciplinary approach to size

enlargement by agglomeration
Agglomeration is a natural phenomenon which has been in existence since solids first
formed on earth. Soon, animals and later humans made use of agglomeration for a
variety of activities. During the two most recent centuries, as technical development
accelerated, empirical improvements of old mechanical techniques still yielded methods
and procedures in each of the emerging industries, which solely solved problems within a
specific technological field. This resulted in the design of different equipment and
systems for similar tasks. They were defined, described and executed in ways that are
typical for that particular industry, often with independent attempts to explain the
principles and using their own nomenclature.
Only after the elaboration of a common theory, the collection of know-how from many
different disciplines and the unbiased evaluation of data did the application of this
combined knowledge to the needs of all industries lead to the recognition that size
enlargement by agglomeration is a unit operation in its own right and qualifies as an
independent field of science.
The paper describes the history of size enlargement by agglomeration, the various
developments and applications that have emerged over the years as well as the new,
interdisciplinary approach to consistently and uniformly solve agglomeration problems
in the different industries.

Electrostatic charging during a melt

agglomeration process
Lactose monohydrate was melt agglomerated in an 8-l high shear mixer using stearic
acid, polyethylene glycol (PEG) 3000, and a mixture of stearic acid and glycerol
monostearate as meltable binders. Electrostatic charging during processing at relative air
humidities of 35 and 75%, respectively, was estimated from the voltage of a monitoring
probe inserted into the mixer. Stearic acid produced a high level of electrostatic charges,
whereas PEG 3000 gave rise to a markedly lower level. Addition of glycerol
monostearate to the stearic acid reduced the level of electrostatic charges. A correlation
was found between the resistivity of the binder and the level of electrostatic charges in
the material. With the stearic acid and the binder mixture, the level of electrostatic
charges was higher at a low air humidity. The amount of adhesion to the bowl was found
to depend on the level of electrostatic charges.