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Patent 2512324 Summary

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(12) Patent: (11) CA 2512324
(54) English Title: TREATMENT OF AQUEOUS SUSPENSIONS
(54) French Title: TRAITEMENT DE SUSPENSIONS AQUEUSES
Status: Granted
Bibliographic Data
(51) International Patent Classification (IPC):
  • B09B 3/00 (2006.01)
(72) Inventors :
  • WHITHAM, LOUISE ELIZABETH (Canada)
  • DYMOND, BRIAN (United Kingdom)
  • HARMAN, RONALD L. (United States of America)
  • SCHAFFER, RONALD J. (Canada)
(73) Owners :
  • BASF SE (Germany)
(71) Applicants :
  • CIBA SPECIALTY CHEMICALS HOLDING INC. (Switzerland)
(74) Agent: GOWLING WLG (CANADA) LLP
(74) Associate agent:
(45) Issued: 2015-11-24
(22) Filed Date: 2005-07-18
(41) Open to Public Inspection: 2007-01-18
Examination requested: 2010-05-11
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data: None

Abstracts

English Abstract

A process in which material comprising an aqueous liquid with dispersed particulate solids is transferred as a fluid to a deposition area, then allowed to stand and rigidify, and in which rigidification is improved whilst retaining the fluidity of the material during transfer, by combining with the material an effective rigidifying amount of aqueous solution of a water-soluble polymer. The process is particularly suitable for the treatment of the tailings underflow resulting oil sands processing operation and the co-disposal of fine and coarse tailings fractions. In addition, liquor released during the rigidification step is of high clarity.


French Abstract

Un procédé dans lequel un matériau comprenant un liquide aqueux renfermant des solides particulaires dispersés est transféré comme fluide dans une zone de dépôt, puis laissé au repos et rigidifié, et dans lequel la rigidification est améliorée et la fluidité du matériau maintenue pendant le transfert, en combinant au matériau une quantité rigidifiante efficace d'une solution aqueuse d'un polymère hydrosoluble. Le procédé convient particulièrement au traitement des sous-écoulements de résidus provenant de l'opération de traitement des sables bitumineux et le co-dépôt de fractions fines et brutes de résidus. De plus, la liqueur libérée pendant l'étape de rigidification est de grande clarté.

Claims

Note: Claims are shown in the official language in which they were submitted.


45
Claims
1. A process for treating oil sands tailings being transferred to a
deposition area, the
process comprising the steps of:
(a) adding the combination of a clarifying polymer and an aqueous solution
of
a water-soluble polymer to the oil sands tailings during transfer to create a
mixture;
(b) maintaining the fluidity of the mixture during transfer to the
deposition
area;
(c) dispensing the mixture in the deposition area; and
(d) allowing the mixture to rigidify in the deposition area.
2. The process defined in Claim 1, wherein the aqueous solution of the
water-soluble
polymer and the clarifying polymer are added simultaneously to the oil sands
tailings.
3. The process defined in Claim 1, wherein the aqueous solution of the
water-soluble
polymer and the clarifying polymer are added sequentially to the oil sands
tailings.
4. The process defined in Claim 3, wherein the aqueous solution of the
water-soluble
polymer is added to the oil sands tails prior to addition of the clarifying
polymer.
5. The process defined in Claim 3, wherein the aqueous solution of the
water-soluble
polymer is added to the oil sands tails after addition of the clarifying
polymer.
6. The process defined in any one of Claims 1-5, wherein the clarifying
polymer has
a molecular weight in the range of from about 10,000 to about 1,000,000 g/mol.
7. The process defined in any one of Claims 1-5, wherein the clarifying
polymer has
a molecular weight in the range of from about 10,000 to about 500,000 g/mol.
8. The process defined in any one of Claims 1-7, wherein the clarifying
polymer is
anionic.

46
9. The process defined in any one of Claims 1-7, wherein the clarifying
polymer is
neutral.
10. The process defined in any one of Claims 1-7, wherein the clarifying
polymer is
cationic.
11. The process defined in any one of Claims 1-10, wherein the clarifying
polymer is
naturally derived.
12. The process defined in any one of Claims 1-11, wherein the clarifying
polymer is
synthetic.
13. The process defined in any one of Claims 1-8, wherein the clarifying
polymer is
selected from the group consisting of starch, gum, cellulose and any mixture
thereof.
14. The process defined in any one of Claims 1-8, wherein the clarifying
polymer is
selected from the group consisting of a homopolymer of sodium acrylate, a
copolymer
with acrylamide, a hydrolysed polyacrylamide, a hydrolysed acrylamide and any
mixture
thereof.
15. The process defined in any one of Claims 1-14, wherein the clarifying
polymer is
used in an amount of from about 5 to about 500 g/tonne of dry solids in the
oil sands
tailings.
16. The process defined in any one of Claims 1-14, wherein the clarifying
polymer is
used in an amount of from about 5 to about 100 g/tonne of dry solids in the
oil sands
tailings.
17. The process defined in any one of Claims 1-16, wherein the clarifying
polymer is
added as a clarifying polymer solution.
18. The process defined in Claim 17, wherein the clarifying polymer is
present in an

47
amount of at least 10% by weight of the clarifying polymer solution.
19. The process defined in any one of Claims 17-18, wherein the clarifying
polymer
solution is added in an amount of at least about 0.01% by weight of the water-
soluble
polymer.
20. The process defined in any one of Claims 17-18, wherein the clarifying
polymer
solution is added in an amount in the range of from about 0.05% to about 5% by
weight
of the water-soluble polymer.
21. The process defined in any one of Claims 17-18, wherein the clarifying
polymer
solution is added in an amount in the range of from about 0.1% to about 2% by
weight of
the water-soluble polymer.
22. The process defined in any one of Claims 17-18, wherein the clarifying
polymer
solution is added in an amount in the range of from about 0.1% to about 3% by
weight of
the water-soluble polymer.
23. The process defined in any one of Claims 17-18, wherein the clarifying
polymer
solution is added in an amount in the range of from about 0.25% to about 1% by
weight
of the water-soluble polymer.
24. The process defined in any one of Claims 17-18, wherein the clarifying
polymer
solution is added in an amount in the range of from about 0.25% to about 1.5%
by
weight of the water-soluble polymer.
25. The process defined in any one of Claims 1-24, wherein the aqueous
solution of
the water-soluble polymer is added to a conduit containing a flow of oil sands
tailings.
26. The process defined in any one of Claims 1-25, wherein Step (d)
comprises co-
immobilizing fine and coarse fractions in the mixture so as to rapidly release
water and
cause the mixture to rigidify in the deposition area.

48
27. The process defined in any one of Claims 1-26, comprising the further
step of:
(e) recycling water released in the deposition area to an oil sands
processing
operation.
28. The process defined in any one of Claims 1-26, comprising the further
step of:
(e) recycling water released in the deposition area to an oil sands
processing
operation without further processing of the recycled water.
29. The process defined in any one of Claims 1-28, wherein the oil sands
tailings
comprising fine tailings.
30. The process defined in any one of Claims 1-29, wherein the oil sands
tailings
have a fines fraction consisting of a particle size of less than about 45
microns.
31. The process defined in any one of Claims 1-29, wherein the oil sands
tailings
have a 70% fraction consisting of a particle size of less than about 45
microns.
32. The process defmed in any one of Claims 1-29, wherein the oil sands
tailings
have a 95% fraction consisting of a particle size of less than about 20
microns.
33. The process defined in any one of Claims 1-29, wherein the oil sands
tailings
have a 75% fraction consisting of a particle size of less than about 10
microns.
34. The process defined in any one of Claims 1-33, wherein the oil sands
has a solids
content in the range of from about 10% to about 80% by weight.
35. The process defined in any one of Claims 1-33, wherein the oil sands
has a solids
content in the range of from about 20% to about 70% by weight.
36. The process defined in any one of Claims 1-35, wherein the water-
soluble
polymer has a intrinsic viscosity of at least 3 dl/g and is formed from
ethylenically
unsaturated water-soluble monomer or blend of monomers.

49
37. The process defined in any one of Claims 1-36, wherein the water
soluble
polymer is anionic.
38. The process defined in Claim 37, wherein the polymer is formed from
monomers
selected from the group consisting of (meth)acrylic acid, ally! sulphonic acid
and 2-
acrylamido-2-methyl propane sulphonic acid as the free acids or salts thereof,
optionally
in combination with non-ionic co-monomers, selected from the group consisting
of
(meth)acrylamide, hydroxy alkyl esters of (meth)acrylic acid and N-vinyl
pyrrolidone.
39. The process defined in any one of Claims 1-36, wherein the water-
soluble
polymer is non-ionic.
40. The process defined in Claim 39, wherein the polymer is formed from
monomers
selected from the group consisting of (meth) acrylamide, hydroxy alkyl esters
of (meth)
acrylic acid and N-vinyl pyrrolidone.
41. The process defined in any one of Claims 1-36, wherein the water-
soluble
polymer is cationic.
42. The process defined in Claim 41, wherein the polymer is formed from
monomers selected from the group consisting of dimethyl amino ethyl(meth)
acrylate -
methyl chloride, (DMAEA.MeCl) quat, diallyl dimethyl ammonium chloride
(DADMAC), trimethyl amino propyl (meth) acrylamide chloride (ATPAC) optionally
in
combination with non-ionic co-monomers, selected from the group consisting of
(meth)
acrylamide, hydroxy alkyl esters of (meth) acrylic acid and N-vinyl
pyrrolidone.
43. The process defined in any one of Claims 1-42, wherein Step (c)
comprises
dispensing the mixture on the surface of previously rigidified material in the
deposition
area.
44. The process defined in any one of Claims 1-42, wherein Step (c)
comprises
dispensing the mixture on the surface of previously rigidified material in the
deposition

50
area to form a stack.
45. The process defined in any one of Claims 1-44, wherein Step (a) is
conducted
prior to a pumping stage for the oil sands tailings.
46. The process defined in any one of Claims 1-44, wherein Step (a) is
conducted
during a pumping stage for the oil sands tailings.
47. The process defined in any one of Claims 1-44, wherein Step (a) is
conducted
subsequent too a pumping stage for the oil sands tailings.
48. A process according to any one of Claims 1-44, in which an effective
rigidifying
amount of the aqueous solution of the water-soluble polymer is mixed with the
oil sands
tailings.

Description

Note: Descriptions are shown in the official language in which they were submitted.



CA 02512324 2005-07-18
MP/3-22373/P 1
Treatment of Aaueous Suspensions
The present invention relates to the treatment of mineral material, especially
waste mineral slurries. The invention is particularly suitable for the
disposal
of tailings and other waste material resulting from mineral or oil sands
processing and beneficiation processes, including the co-disposal of coarse
and fine solids, as a homogenous mixture.
Processes of treating mineral ores or oil sands in order to extract mineral
values or in the case of oil sands to extract bitumen will normally result in
waste material. Often the waste material consists of an aqueous slurry or
sludge comprising particulate mineral material, for instance clay, shale,
sand,
grit, oil sand tailings, metal oxides etc admixed with water.
In some cases the waste material such as mine tailings can be conveniently
disposed of in an underground mine to form backfill. Generally backfill waste
comprises a high proportion of coarse large sized particles together with
other smaller sized particles and is pumped into the mine as slurry where it
is
allowed to dewater leaving the sedimented solids in place. It is common
practice to use flocculants to assist this process by flocculating the fine
material to increase the rate of sedimentation. However, in this instance, the
coarse material will normally sediment at a faster rate than the flocculated
fines, resulting in a heterogeneous deposit of coarse and fine solids.
For other applications it may not be possible to dispose of the waste in a
mine. In these instances, it is common practice to dispose of this material by
pumping the aqueous slurry to lagoons, heaps or stacks and allowing it to
dewater gradually through the actions of sedimentation, drainage and
evaporation.


CA 02512324 2005-07-18
2
For example in oil sands processing, the ore is processed to recover the
bitumen fraction, and the remainder, including both process material and the
gangue, constitutes the tailings that are not valuable and are to be disposed
of. In oil sands processing, the main process material is water, and the
gangue is mostly sand with some silt and clay. Physically, the tailings
consist of a solid part (sand tailings) and a more or less fluid part
(sludge).
The most satisfactory place to dispose of these tailings is, of course, in the
existing excavated hole in the ground. It turns out, however, that the sand
tailings alone from the one cubic foot of ore occupy just about one cubic
foot.
The amount of sludge is variable, depending on ore quality and process
conditions, but average about 0.3 cubic feet. The tailings simply will not fit
back into the hole in the ground.
There is a great deal of environmental pressure to minimise the allocation of
new land for disposal purposes and to more effectively use the existing
waste areas. One method is to load multiple layers of waste onto an area to
thus form higher stacks of waste. However, this presents a difficulty of
ensuring that the waste material can only flow over the surface of previously
rigidified waste within acceptable boundaries, is allowed to rigidify to form
a
stack, and that the waste is sufficiently consolidated to support multiple
layers of rigidified material, without the risk of collapse or slip. Thus the
requirements for providing a waste material with the right sort of
characteristics for stacking is altogether different from those required for
other forms of disposal, such as back-filling within a relatively enclosed
area.
In a typical mineral or oil sands processing operation, waste solids are
separated from solids that contain mineral values in an aqueous process.
The aqueous suspension of waste solids often contain clays and other
minerals, and are usually referred to as tailings. These solids are often
concentrated by a flocculation process in a thickener to give a higher density
underflow and to recover some of the process water. It is usual to pump the
underflow to a surface holding area, often referred to as a tailings pit or
dam.
Once deposited at this surface holding area, water will continue to be


CA 02512324 2005-07-18
3
released from the aqueous suspension resulting in further concentration of
the solids over a period of time. Once a sufficient volume of water has been
collected this is usually pumped back to the mineral or oil sands processing
plant.
The tailings dam is often of limited size in order to minimise the impact on
the environment. In addition, providing larger dams can be expensive due to
the high costs of earth moving and the building of containment walls. These
dams tend to have a gently sloping bottom which allows any water released
from the solids to collect in one area and which can then be pumped back to
the plant. A problem that frequently occurs is when fine particles of solids
are carried away with the run-off water, thus contaminating the water and
having a detrimental impact on subsequent uses of the water.
In many mineral and oil sands processing operations, for instance a mineral
sands beneficiation process, it is also common to produce a second waste
stream comprising of mainly coarse (> 0.1 mm) mineral particles. It is
particularly desirable to dispose of the coarse and fine waste particles as a
homogeneous mixture as this improves both the mechanical properties of
the dewatered solids, greatly reducing the time and the cost eventually
required to rehabilitate the land. However, this is not usually possible
because even if the coarse waste material is thoroughly mixed into the
aqueous suspension of tine waste material prior to deposition in the disposal
area, the coarse material will settle much faster than the fine material
resulting in banding within the dewatered solids. Furthermore, when the
quantity of coarse material to fine material is relatively high, the rapid
sedimentation of the coarse material may produce excessive beach angles
which promote the run off of aqueous waste containing high proportions of
fine particles, further contaminating the recovered water. As a result, it is
often necessary to treat the coarse and fine waste streams separately, and
recombine these materials by mechanically re-working, once the dewatering
process is complete.


CA 02512324 2005-07-18
4
Attempts have been made to overcome all the above problems by treating
the feed to the tailings dam using a coagulant or a flocculant to enhance the
rate of sedimentation and/or improve the clarity of the released water.
However, this has been unsuccessful as these treatments have been applied
at conventional doses and this has brought about little or no benefit in
either
rate of compaction of the fine waste material or clarity of the recovered
water.
It would therefore be desirable to provide treatment which provides more
rapid release of water from the suspension of solids. In addition it will be
desirable to enable the concentrated solids to be held in a convenient
manner that prevent both segregation of any coarse and fine fractions, and
prevent contamination of the released water whilst at the same time
minimise the impact on the environment.
In the process for recovery of heavy oil and bitumen from oil sand deposits,
when using open cast mining, the oil or bitumen is extracted either by a hot-
water process in which oil sands are mixed with 65 °C (150 °F)
water and
caustic or by a low-energy extraction process run at lower temperatures
without caustic. However, both processes generate large volumes of tailings
which consist of the whole oil sand ore body plus net additions of process
water less only the recovered bitumen product.
These oil sand tailings can be subdivided into three categories; viz.: (1 )
screen oversize, (2) coarse or sand tailings (the fraction that settles
rapidly),
and (3) fine or tailings sludge (the fraction that settles slowly). Thus the
oil
sands tailing are made up of particles of different sizes.
Typically these oil sand tailings are piped to a tailings pond for disposal.
The
coarse sands settle first with fine particles settling only very slowly. These
fine particles form highly stable fines suspensions in water containing as
much as about 30 percent by weight solids. Over time these fine particles


CA 02512324 2005-07-18
settle to form a substantially solid clay sediment thus filling the lagoon and
requiring the creation of new lagoons.
It is well known to concentrate these oil sand tailings in a thickener to give
a
5 higher density underflow and to recover some of the process water as
mentioned above.
For example, Xu.Y et al, Mining Engineering, November 2003, p.33-39
describes the addition of anionic flocculants to the oil sand tailings in the
thickener before disposal.
The underflow can be disposed of and/or subjected to further drying for
subsequent disposal in a oil sand tailings stacking area.
In the Bayer process for recovery of alumina from bauxite, the bauxite is
digested in an aqueous alkaline liquor to form sodium aluminate which is
separated from the insoluble residue. This residue consists of both sand, and
fine particles of mainly ferric oxide. The aqueous suspension of the latter is
known as red mud.
After the primary separation of the sodium aluminate solution from the
insoluble residue, the sand (coarse waste) is separated from the red mud.
The supernatant liquor is further processed to recover aluminate. The red
mud is then washed in a plurality of sequential washing stages, in which the
red mud is contacted by a wash liquor and is then flocculated by addition of a
flocculating agent. After the final wash stage the red mud slurry is thickened
as much as possible and then disposed of. Thickening in the context of this
specification means that the solids content of the red mud is increased. The
final thickening stage may comprise settlement of flocculated slurry only, or
sometimes, includes a filtration step. Alternatively or additionally, the mud
may be subjected to prolonged settlement in a lagoon. In any case, this final


CA 02512324 2005-07-18
6
thickening stage is limited by the requirement to pump the thickened
aqueous suspension to the disposal area.
The mud can be disposed of and/or subjected to further drying for
subsequent disposal on a mud stacking area. To be suitable for mud
stacking the mud should have a high solids content and, when stacked,
should not flow but should be relatively rigid in order that the stacking
angle
should be as high as possible so that the stack takes up as little area as
possible for a given volume. The requirement for high solids content conflicts
with the requirement for the material to remain pumpable as a fluid, so that
even though it may be possible to produce a mud having the desired high
solids content for stacking, this may render the mud unpumpable.
The sand fraction removed from the residue is also washed and transferred
to the disposal area for separate dewatering and disposal.
EP-A-388108 describes adding a water-absorbent, water-insoluble polymer
to a material comprising an aqueous liquid with dispersed particulate solids,
such as red mud, prior to pumping and then pumping the material, allowing
the material to stand and then allowing it to rigidify and become a stackable
solid. The polymer absorbs the aqueous liquid of the slurry which aids the
binding of the particulate solids and thus solidification of the material.
However this process has the disadvantage that it requires high doses of
absorbent polymer in order to achieve adequate solidification. In order to
achieve a sufficiently rigidified material it is often necessary to use doses
as
high as 10 to 20 kilograms per tonne of mud. Although the use of water
swellable absorbent polymer to rigidify the material may appear to give an
apparent increase in solids, the aqueous liquid is in fact held within the
absorbent polymer. This presents the disadvantage that as the aqueous
liquid has not actually been removed from the rigidified material and under
certain conditions the aqueous liquid could be desorbed subsequently and


CA 02512324 2005-07-18
7
this could risk re-fluidisation of the waste material, with the inevitable
risk of
destabilising the stack.
WO-A-96/05146 describes a process of stacking an aqueous slurry of
particulate solids which comprises admixing an emulsion of a water-soluble
polymer dispersed in a continuous oil phase with the slurry. Preference is
given to diluting the emulsion polymer with a diluent, and which is preferably
in a hydrocarbon liquid or gas and which will not invert the emulsion.
Therefore it is a requirement of the process that the polymer is not added in
to the slurry as an aqueous solution.
WO-A-0192167 describes a process where a material comprising a
suspension of particulate solids is pumped as a fluid and then allowed to
stand and rigidify. The rigidification is achieved by introducing into the
suspension particles of a water soluble polymer which has an intrinsic
viscosity of at least 3 di/g. This treatment enables the material to retain
its
fluidity as being pumped, but upon standing causes the material to rigidify.
This process has the benefit that the concentrated solids can be easily
stacked, which minimises the area of land required for disposal. The
process also has the advantage over the use of cross linked water absorbent
polymers in that water from the suspension is released rather than being
absorbed and retained by the polymer. The importance of using particles of
water soluble polymer is emphasised and it is stated that the use of aqueous
solutions of the dissolved polymer would be ineffective. Very efficient
release
of water and convenient storage of the waste solids is achieved by this
process, especially when applied to a red mud underflow from the Bayer
alumina process.
However, despite the improvements brought about by WO-A-0192167,
particularly in the treatment of red mud and treatement of oil sands tailing,
there is still a need to further improve the rigidification of suspensions of
materials and further improve upon the clarity of liquor released. In
particular,


CA 02512324 2005-07-18
an objective of the present invention is to find a more suitable method for
treating coarse and/or fine particulate waste material from mineral sands,
alumina, oil sands or other mineral processing operations in order to provide
better release of liquor and a more effective means of disposing of the
concentrated solids. Furthermore, there is a need to improve the dewatering
of suspensions of waste solids that have been transferred as a fluid to a
settling area for disposal and provide improvements in the clarity of run-off
water. In particular, it would be desirable to provide a more effective
treatment of waste suspensions transferred to disposal areas, for instance
tailings dams, ensuring fast, efficient concentration and more
environmentally friendly storage of solids and improve clarity of released
liquor.
In one aspect of the present invention, we provide a process in which
material comprising an aqueous liquid with dispersed particulate solids is
transferred as a fluid to a deposition area, then allowed to stand and
rigidify,
and in which rigidification is improved whilst retaining the fluidity of the
material during transfer, by combining with the material an effecfiive
rigidifying amount of aqueous solution of a water-soluble polymer.
In a preferred embodiment the dispersed particulate solids are in all or in
part
oil sands tailings. The dispersed particulate solids are produced from
extraction of the oil or bitumen from oil sands.
In a second aspect of the present invention, we provide a process in which
the aqueous liquid contains dispersed particulate solids with a bimodal
distribution of particle sizes and following treatment with an effective
amount
of aqueous solution of a water soluble polymer, on standing, rigidifies
without
significant segregation of the coarse and fine fractions of particulate
solids.


CA 02512324 2005-07-18
9
The addition of the aqueous solution of water-soluble polymer to the material
allows it to retain sufficient fluidity during transfer and then once the
material
is allowed to stand it will form a solid mass strong enough to support
subsequent layers of rigidified material. We have unexpectedly found that
the addition of the aqueous solution of polymer to the material does not
cause instant rigidification or substantially any settling of the solids prior
to
standing.
Generally suspended solids will be concentrated in a thickener and this
material will leave the thickener as an underflow which will be pumped along
a conduit to a deposition area. The conduit is any convenient means for
transferring the material to the deposition area and may for instance be a
pipe or a trench. The material remains fluid and pumpable during the transfer
stage until the material is allowed to stand.
Desirably the process of the invention is part of the mineral or oil sands
processing operation in which an aqueous suspension of waste solids is
optionally flocculated in a vessel to form a supernatant layer comprising an
aqueous liquor and an underflow layer comprising thickened solids which
form the material. The supernatant layer will be separated from the under
flow in the vessel and is typically recycled or subjected to further
processing.
The aqueous suspension of waste solids or optionally, the thickened
underflow is transferred, usually by pumping, to a deposition area, which
may for instance be a tailings dam or lagoon. The material may consist of
only mainly fine particles, or a mixture of fine and coarse particles.
Optionally, additional coarse particles may be combined with the aqueous
suspension at any convenient point prior to discharge at the deposition area.
Once the material has reached the deposition area it is allowed to stand and
rigidification takes place. The aqueous polymer solution may be added to the
material in an effective amount at any convenient point, typically during
transfer. In some cases the aqueous suspension may be transferred first to a
holding vessel before being transferred to the deposition area.


CA 02512324 2005-07-18
Suitable doses of polymer range from 10 grams to 10,000 grams per tonne
of material solids. Generally the appropriate dose can vary according to the
particular material and material solids content. Preferred doses are in the
5 range 30 to 3,000 grams per tonne, while more preferred doses are in the
range of from 60 to 200 or 400 grams per tonne.
The material particles are usually inorganic and/or usually a mineral. For
example, the material particles are sand, oil sands tailings, clay, shale,
grit,
10 silt, metal oxides etc admixed with water.
Typically the material may be derived from or contain filter cake, tailings,
thickener underflows, or unthickened plant waste streams, for instance other
mineral tailings, oil sand tailings or slimes, including phosphate, diamond,
gold slimes, mineral sands, tails from zinc, lead, copper, silver, uranium,
nickel, iron ore processing, coal, or red mud. The material may be solids
settled from the final thickener or wash stage of a mineral or oil sands
processing operation. Thus the material desirably results from a mineral or
oil sands processing operation. Preferably the material comprises tailings.
The fine tailings or other material which is pumped may have a solids
content in the range 10% to 80% by weight. The slurries are often in the
range 20% to 70% by weight, for instance 45% to 65% by weight. The sizes
of particles in a typical sample of the fine tailings are substantially all
less
than 25 microns, for instance about 95% by weight of material is particles
less than 20 microns and about 75% is less than 10 microns. The coarse
tailings are substantially greater than 100 microns, for instance about 85% is
greater than 100 microns but generally less than 10,000 microns. The fine
tailings and coarse tailings may be present or combined together in any
convenient ratio provided that material remains pumpable.


CA 02512324 2005-07-18
11
The dispersed particulate solids may have a bimodal distribution of particle
sizes. Typically this bimodal distribution may comprise a fine fraction and a
coarse fraction, in which the fine fraction peak is substantially less than 25
microns and the coarse fraction peak is substantially greater than 75
microns.
For example, the particles in oil sands tailings may have a fine fraction of
less than about 45 microns. For instance about 70 percent of the particles
may be less than about 45 microns.
We have found better results are obtained when the material is relatively
concentrated and homogenous. It may also be desirable to combine the
addition of the polymer solution with other additives. For instance the flow
properties of the material through a conduit may be facilitated by including a
dispersant. Typically where a dispersant is included it would be included in
conventional amounts. However, we have found that surprisingly the
presence of dispersants or other additives does not impair the rigidification
of
the material on standing. It may also be desirable to pre-treat the material
with either an inorganic or organic coagulant to pre-coagulate the fine
material to aid its retention in the rigidified solids.
Thus in the present invention the polymer solution is added directly to the
aforementioned material. The polymer solution may consist wholly or
partially of water-soluble polymer. Thus the polymer solution may comprise a
blend of cross-linked polymer and water soluble polymer, provided sufficient
of the polymer is in solution or behaves as though it is in solution to bring
about rigidification on standing.
This may be a physical blend of swellable polymer and soluble polymer or
alternatively is a lightly cross-linked polymer for instance as described in
EP202780. Although the polymeric particles may comprise some cross-
linked polymer it is essential to the present invention that a significant


CA 02512324 2005-07-18
12
amount of water soluble polymer is present. When the polymeric particles
comprise some swellable polymer it is desirable that at least 80% of the
polymer is water-soluble.
Preferably the aqueous solution of polymer comprises polymer which is
wholly or at least substantially water soluble. The water soluble polymer may
be branched by the presence of branching agent, for instance as described
in WO-A-9829604, for instance in claim 12, or alternatively the water soluble
polymer is substantially linear.
Preferably the water soluble polymer is of moderate to high molecular
weight. Desirably it will have an intrinsic viscosity of at least 3 dl/g
(measured
in 1 M NaCI at 25°C) and generally at least 5 or 6 dl/g, although the
polymer
may be of significantly high molecular weight and exhibit an intrinsic
viscosity
of 25 dl/g or 30 dl/g or even higher. Preferably the polymer will have an
intrinsic viscosity in the range of 8dl/g to 25 dl/g, more preferably 11 dl/g
or
12 dl/g to 18 dl/g or 20 dl/g.
The water soluble polymer may be a natural polymer, for instance
polysaccharides such as starch, guar gum or dextran, or a semi-natural
polymer such as carboxymethyl cellulose or hydroxyethyl cellulose.
Preferably the polymer is synthetic and preferably it is formed from an
ethylenically unsaturated water-soluble monomer or blend of monomers.
The water soluble polymer may be cationic, non-ionic, amphoteric, or
anionic. The polymers may be formed from any suitable water-soluble
monomers. Typically the water soluble monomers have a solubility in water
of at least 5g/100cc at 25°C. Particularly preferred anionic polymers
are
formed from monomers selected from ethylenically unsaturated carboxylic
acid and sulphonic acid monomers, preferably selected from (meth) acrylic
acid, allyl sulphonic acid and 2-acrylamido-2-methyl propane sulphonic acid
(AMPS), and their salts, optionally in combination with non-ionic co-


CA 02512324 2005-07-18
13
monomers, preferably selected from (meth) acrylamide, hydroxy alkyl esters
of (meth) acrylic acid and N-vinyl pyrrolidone.
Preferred non-ionic polymers are formed from ethylenically unsaturated
monomers selected from (meth) acrylamide, hydroxy alkyl esters of (meth)
acrylic acid and N-vinyl pyrrolidone.
Preferred cationic polymers are formed from ethylenically unsaturated
monomers selected from dimethyl amino ethyl (meth) acrylate - methyl
chloride, (DMAEA.MeCI) quat, diallyl dimethyl ammonium chloride
(DADMAC), trimethyl amino propyl (meth) acrylamide chloride (ATPAC)
optionally in combination with non-ionic co-monomers, preferably selected
from (meth) acrylamide, hydroxy alkyl esters of (meth) acrylic acid and N-
vinyl pyrrolidone.
In some instances, it has been found advantageous to separately add
combinations of polymer types. Thus an aqueous solution of an anionic,
cationic or non-ionic polymer may be added to the above mentioned material
first, followed by a second dose of either a similar or different water
soluble
polymer of any type.
In the invention, the water soluble polymer may be formed by any suitable
polymerisation process. The polymers may be prepared for instance as gel
polymers by solution polymerisation, water-in-oil suspension polymerisation
or by water-in-oil emulsion polymerisation. When preparing gel polymers by
solution polymerisation the initiators are generally introduced into the
monomer solution.
Optionally a thermal initiator system may be included. Typically a thermal
initiator would include any suitable initiator compound that releases radicals
at an elevated temperature, for instance azo compounds, such as azo-bis-


CA 02512324 2005-07-18
14
isobutyronitrile. The temperature during polymerisation should rise to at
least
70°C but preferably below 95°C. Alternatively polymerisation may
be
effected by irradiation (ultra violet light, microwave energy, heat etc.)
optionally also using suitable radiation initiators. Once the polymerisation
is
complete and the polymer gel has been allowed to cool sufficiently the gel
can be processed in a standard way by first comminuting the gel into smaller
pieces, drying to the substantially dehydrated polymer followed by grinding to
a powder. Alternatively polymer gels may be supplied in the form of polymer
gels, for instance as neutron type gel polymer logs.
Such polymer gels may be prepared by suitable polymerisation techniques
as described above, for instance by irradiation. The gels may be chopped to
an appropriate size as required and then on application mixed with the
material as partially hydrated water soluble polymer particles.
The polymers may be produced as beads by suspension polymerisation or
as a water-in-oil emulsion or dispersion by water-in-oil emulsion
polymerisation, for example according to a process defined by EP-A-150933,
EP-A-102760 or EP-A126528.
Alternatively the water soluble polymer may be provided as a dispersion in
an aqueous medium. This may for instance be a dispersion of polymer
particles of at least 20 microns in an aqueous medium containing an
equilibrating agent as given in EP-A-170394. This may for example also
include aqueous dispersions of polymer particles prepared by the
polymerisation of aqueous monomers in the presence of an aqueous
medium containing dissolved low IV polymers such as poly diallyl dimethyl
ammonium chloride and optionally other dissolved materials for instance
electrolyte and/or multi-hydroxy compounds e. g. polyalkylene glycols, as
given in WO-A-9831749 or WO-A-9831748.


CA 02512324 2005-07-18
The aqueous solution of water-soluble polymer is typically obtained by
dissolving the polymer in water or by diluting a more concentrated solution of
the polymer. Generally solid particulate polymer, for instance in the form of
powder or beads, is dispersed in water and allowed to dissolve with
5 agitation. This may be achieved using conventional make up equipment.
Desirably, the polymer solution can be prepared using the Auto Jet Wet
(trademark) supplied by Ciba Specialty Chemicals. Alternatively, the
polymer may be supplied in the form of a reverse phase emulsion or
dispersion which can then be inverted into water.
The aqueous polymer solution may be added in any suitable concentration.
It may be desirable to employ a relatively concentrated solution, for instance
up to 10 % or more based on weight of polymer in order to minimise the
amount of water introduced into the material. Usually though it will be
desirable to add the polymer solution at a lower concentration to minimise
problems resulting from the high viscosity of the polymer solution and to
facilitate distribution of the polymer throughout the material. The polymer
solution can be added at a relatively dilute concentration, for instance as
low
as 0.01 % by weight of polymer. Typically the polymer solution will normally
be used at a concentration between 0.05 and 5% by weight of polymer.
Preferably the polymer concentration will be the range 0.1 % to 2 or 3%.
More preferably the concentration will range from 0.25% to about 1 or 1.5%.
In a mineral or oil sands processing operation where a suspension
containing solids is flocculated in a thickener in order to separate the
suspension into a supernatant layer and an underflow material, the material
can typically be treated at any suitable point after flocculation in the
thickener
but before the material is allowed to stand. A suitable and effective
rigidifying
amount of the water-soluble polymer solution can be mixed with the material
prior to a pumping stage. In this way the polymer solution can be distributed
throughout the material. Alternatively, the polymer solution can be
introduced and mixed with the material during a pumping stage or


CA 02512324 2005-07-18
16
subsequently. The most effective point of addition will depend upon the
substrate and the distance from the thickener to the deposition area. If the
conduit is relatively short any may be advantageous to dose the polymer
solution close to where the material flows from the thickener. On the other
hand, where the deposition area is significantly remote from the thickener in
may be desirable to introduce the polymer solution closer to the outlet. In
some instances in may be convenient to introduce the polymer solution into
the material as it exits the outlet.
When aqueous suspensions of fine and coarse particulate materials are
being combined for the purposes of co-disposal, the effective rigidifying
amount of the water-soluble polymer solution will normally be added during
or after the mixing of the different waste streams into a homogeneous slurry.
Preferably the material will be pumped as a fluid to an outlet at the
deposition area and the material allowed to flow over the surface of
rigidified
material. The material is allowed to stand and rigidify and therefore forming
a stack of rigidified material. This process may be repeated several times to
form a stack that comprises several layers of rigidified material. The
formation of stacks of rigidified material has the advantage that less area is
required for disposal.
The rheological characteristics of the material as it flows through the
conduit
to the deposition area is important, since any significant reduction in flow
characteristics could seriously impair the efficiency of the process. It is
important that there is no significant settling of the solids as this could
result
in a blockage, which may mean that the plant has to be closed to allow the
blockage to be cleared. In addition it is important that there is no
significant
reduction in flow characteristics, since this could drastically impair the
pumpability on the material. Such a deleterious effect could result in
significantly increased energy costs as pumping becomes harder and the
likelihood of increased wear on the pumping equipment.


CA 02512324 2005-07-18
17
The rheological characteristics of the material as it rigidifies is important,
since once the material is allowed to stand it is important that flow is
minimised and that solidification of the material proceeds rapidly. If the
material is too fluid then it will not form an effective stack and there is
also a
risk that it will contaminate water released from the material. It is also
necessary that the rigidified material is sufficiently strong to remain intact
and
withstand the weight of subsequent layers of rigidified material being applied
to it.
Preferably the process of the invention will achieve a heaped disposal
geometry and will co-immobilise the fine and course fractions of the solids in
the material and also allowing any released water to have a higher driving
force to separate it from the material by virtue of hydraulic gravity
drainage.
The heaped geometry appears to give a higher downward compaction
pressure on underlying solids which seems to be responsible for enhancing
the rate of dewatering. We find that this geometry results in a higher volume
of waste per surface area, which is both environmentally and economically
beneficial.
It is not possible to achieve the objectives of the invention by adapting the
flocculation step in the thickener. For instance flocculation of the
suspension
in the thickener to provide an underflow sufficiently concentrated such that
it
would stack would be of a little value since it would not be possible to pump
such a concentrated underflow. Instead we have found that it is essential to
treat the material that has been formed as an underflow in the thickener. It
appears that separately treating the thickened solids in the underflow allows
the material to rigidify effectively without compromising the fluidity during
transfer.
A preferred feature of the present invention is the release of aqueous liquor
that often occurs during the rigidification step. Thus in a preferred form of
the


CA 02512324 2005-07-18
18
invention the material is dewatered during rigidification to release liquor
containing significantly less solids. The liquor can then be returned to the
process thus reducing the volume of imported water required and therefore it
is important that the liquor is clear and substantially free of contaminants,
especially migrating particulate fines. Suitably the liquor may for instance
be
recycled to the thickener from which the material was separated as an
underflow. Alternatively, the liquor can be recycled to the spirals or other
processes within the same plant.
Furthermore clarifying polymers may optionally be added after the thickener
to the underflow but before disposal by rigidification. This may enhance the
clarity of the water released from the rigidifying stack.
The clarifying polymers are typically low molecular weight, polymers.
For the purposes of the invention low molecular weight means an average
molecular weight ranging from about 10,000 to about 1,000,000 g/mol. For
example, anionic polymers in the range of about 10,000 to about 500,000
g/mol may be used.
These can be anionic, non-ionic or cationic. They can be synthetic or
naturally derived, eg from starch, gums or cellulose, eg carboxymethyl
cellulose. Preferably they are anionic, eg a homopolymer of sodium acrylate,
or as a copolymer with acrylamide, or hydrolysed polyacrylonitrile or
hydrolysed acrylamide.
The amount of clarifying polymer will be determined by the composition of
the oil sands tailings but generally about 5 to about 500 g/tonne of dry
solids.
For example the amount of clarifying polymer may be about 5 g to about 100
g/tonne of dry solids.


CA 02512324 2005-07-18
19
The clarifying polymer may be added as a solution or powder and may be
added in any suitable concentration. It may be desirable to employ a
relatively concentrated solution, for instance up to 10 % or more based on
weight of polymer in order to minimise the amount of water introduced into
the material. The clarifying polymer solution can be added at a relatively
dilute concentration, for instance as low as 0.01 % by weight of polymer.
Typically the clarifying polymer solution will normally be used at a
concentration between 0.05 and 5% by weight of polymer. Preferably the
polymer concentration will be the range 0.1 % to 2 or 3%. More preferably
the concentration will range from 0.25% to about 1 or 1.5%.
The clarifying polymer may be added before, simultaneously, or after the
rigidifying amount of the water-soluble polymer solution.
It is equally possible to treat the tailings without the thickener step if the
feed
is at a sufficiently high solids concentration and suitable sands/ fines
ratio.
In a further aspect of the present invention we provide a process in which
material comprising an aqueous liquid with dispersed particulate solids is
transferred as a fluid to a settling area, then allowed to dewater to release
liquor containing dissolved mineral values, and in which dewatering is
improved whilst retaining the fluidity of the material during transfer, by
combining with the material an effective dewatering amount of aqueous
solution of a water-soluble polymer.
In this form of the invention the aqueous polymer solution is applied to the
material in a similar manner as described above. In this case, the polymer
solution is applied in an effective dewatering amount and in the same way as
a first aspect of the invention it is important that the fluidity of the
material is
retained during transfer. The material is transferred to a settling area,
which
can for instance be a tailings dam or a lagoon. The dewatering step must


CA 02512324 2005-07-18
proceed as quickly as possible such that the solids are allowed to
concentrate and aqueous liquor is released. It is important that the liquor is
of high clarity and not contaminated by solids, particularly fines, which
would
impair further processing.
5
Typically in a mineral or oil sands processing operation, a suspension of
solids is flocculated in a vessel to form a supernatant layer comprising an
aqueous liquor and an underflow layer comprising thickened solids, which
forms the material. The underflow-suspension flows from the vessel, is
10 optionally combined with additional coarse particulate material, and in
which
the material is then pumped to a settling area where it is allowed to dewater.
The aqueous polymer solution is mixed into the material after flocculating the
suspension and before the material is allowed to rigidify and dewater.
15 The aqueous polymer solution may comprise any of the polymers and be
used in a similar manner as that described above.
The following examples are intended to demonstrate the invention.


CA 02512324 2005-07-18
21
EXAMPLE 1
Polymer preparation
The polymer samples shown in Table 1 have been prepared by the gel
polymerisation method. The polymers were stirred into water to provide an
aqueous solution at a concentration of 0.25%.
Table 1
Intrinsic
Sample Polymer (% wt/wt) Viscosity
i
dl/


A 100% acrylamide homopolymer 16


B 15/85 sodium acrylate/acrylamide copolymer 18


C 30/70 sodium acryiate/acrylamide copolymer 12


D 30/70 sodium acrylate/acrylamide copolymer 24


E 45/55 sodium acrylate/acrylamide copolymer 16


F 75/25 sodium acrylate/acrylamide copolymer 19 I


G 100% sodium acrylate homopolymer 18


H 10/90 sodium AMPS/acrylamide copolymer 16


I 40/60 sodium AMPS/acrylamide copolymer 14


J 25/75 DMAEA.MeCI/acrylamide copolymer 14


K 60/40 DMAEA.MeCI/acrylamide copolymer 12


L 80/20 DMAEA.MeCI/acrylamide copolymer 12


M 35/60/5 DMAEA.MeCI/acrylamide/sodium acrylate20
pol mer


Experimental Details
Test were carried out according to the following procedures using a tailings
slurry obtained from a mineral sands operation.
Table 2
Solids Content (% 53.1


wt/wt


Solids < 75 um (% 10.9


wt/wt


Specific Gravity 1.51




CA 02512324 2005-07-18
22
A) A Slump Test is conducted using the following method:
1. A collar, measuring in equal diameter and external diameter was
placed on a metal surface of adequate size, with drainage holes to
facilitate the collection of free water.
2. This collar is filled with the aqueous mineral slurry to the brim and
levelled off.
3. The collar is lifted vertically off the tray, at speed, allowing the slurry
to
slump outwards.
4. The diameter of the resultant solids and the height, both at the edge
and in the centre, is then recorded, allowing the height to be
calculated as a percentage of the radius, denoted as the slump.
slump (%) = c - a x 100
r
where:
c = slump height at centre
a = slump height at edge
r = radius
5. Where applicable, the water released from the solids over a period of
one minute is collected and both the volume and clarity or turbidity
measured.
B) Treatment tests, employing samples A to M above were conducted using
the following method.
1. A known volume of the tails slurry was sampled into an adequate size
plastic beaker.


CA 02512324 2005-07-18
23
2. The slurry was then subjected to low shear mixing by pouring the
sample from one beaker to another to ensure that the sample was
homogeneous.
3. The required dose of aqueous polymer solution was added to the
tailings slurry and mixing continued until a consistent material was
produced.
4. The treated slurry was evaluated using the slump test as described in
section "A" above.
Table 3
Dose r c a Slump Released
Water


Sample ~gpt~ (mm) (mm) (mm) (%) Volume Turbidity
ml NTU


Blank 0 80 4 3 1 25 > 1000


125 24 52 14 158 95 23
A


250 33 32 13 58 89 57


125 28 41 16 89 43 23


B
250 23 52 6 200 46 116


62 28 42 17 89 57 23


C
125 24 51 22 121 25 24


62 30 41 17 80 50 19


D
125 25 47 18 116 54 20


62 30 38 18 67 27 72


E
125 24 50 13 154 61 179


62 38 27 12 39 47 119


F
125 23 51 27 104 56 51


125 25 50 18 128 57 25


250 23 51 22 126 47 95


125 35 33 12 60 41 119


250 24 52 19 138 71 69


62 48 23 6 35 45 108


I
125 24 53 10 179 85 29


125 58 13 4 16 45 547


J
250 23 53 21 139 80 21


125 25 49 19 120 52 14


K
250 24 52 19 138 75 14




CA 02512324 2005-07-18
24
62 40 25 7 45 35 117
L


125 23 51 20 135 68 20


125 34 33 15 53 51 208
M


250 25 51 18 132 60 108


The increased rigidification of the mineral tailings through the addition of
the
water soluble polymer is evident by the reduced slump radius and increased
stacking height compared to the untreated material. In almost all tests,
increases in the quantity, and significant increases in the clarity of the
released liquor are also observed.
EXAMPLE 2
Polymer preparation
The polymer samples shown in Table 1 have been prepared by a number of
different polymerisation methods. The polymers were stirred into water to
provide an aqueous solution at a concentration of 0.25% active polymer.
Table 4
Intrinsic


Sample Form Polymer (% wt/wt) Viscosity


dl/


N Bead 30/70 sodium acrylate/acrylamide12


co of mer


p Inverse 30/70 sodium acrylate/acrylamide17


Emulsion co of mer


P Dispersion30/70 sodium acrylate/acrylamide16


co of mer


Q Solution 100% mannich derivatised 14


of ac lamide


Inverse 25/75 DMAEA.MeCI/acrylamide 16


Emulsion copol mer


S Bead 25/75 DMAEA.MeCI/acrylamide 8


co olymer


T Dispersion80/20 DMAEMA.MeCI/acrylamide 8


co of mer


U Gel 5/95 APTAC/acrylamide copolymer 16


V powder polyethylene oxide n/a


W solution dextran polysaccharide n/a


X powder guar gum n/a




CA 02512324 2005-07-18
Experimental Details
Tests were carried out according to the procedures and using the tailings
slurry detailed in example 1.
Table 5
Dose r c a Slump Released
Water


Sample ~gpt~ (mm) (mm) (mm) (%) Volume Turbidity
ml NTU


Blank 0 83 4 2 2 10 > 1000


62 28 37 12 89 38 23
N


125 23 52 16 157 73 31


44 40 28 9 48 38 181


87 24 54 51 13 60 44


62 23 52 7 196 36 124


P
125 24 53 51 8 40 48


55 48 22 6 33 52 285


90 25 49 21 112 76 26


175 29 39 17 76 44 32


R
350 24 51 23 117 52 158


125 48 22 7 31 36 124


S 250 26 50 26 92 57 10


125 30 38 17 70 38 34


T
250 23 52 40 52 44 72


250 29 37 19 62 33 24


U
375 24 53 23 125 71 18


250 29 39 15 83 53 29


V
500 28 34 15 68 32 113


W 375 65 10 5 8 35 271


5
EXAMPLE 3
Sample C from example 1 was tested according to the procedures and using
the tailings slurry detailed in example 1 in conjunction with some additives
which may be added to the slurry for other purposes.
10 Table 6
Sample ~ Additive


CA 02512324 2005-07-18
26
X organic coagulant - poly DADMAC


Y inorganic coagulant - poly aluminium chloride


Z organic dispersant - sodium polyacrylate


Table 7
Sam Dose Sam Dose r c a Slump
le pt le t mm mm mm
p p


Blank 0 Blank 0 93 7 3 4


X 250 C 94 23 52 29 100


C 94 X 250 24 51 26 104


Y 250 C 94 28 43 11 114


C 94 Y 250 30 45 17 93


Z 250 C 125 23 49 19 130


C 125 Z 250 23 51 21 130


J 62 C 62 28 43 15 100


C 62 J 62 23 51 26 109


EXAMPLE 4
Selected samples taken from example 1 were evaluated according to the
procedures detailed in example 1 using a tailings slurry obtained from a
lateritic nickel, acid leach process.
Table 8
Solids Content (% 26.7
wt/wt)


Solids < 75 um (% 22.5
wt/wt)


Specific Gravity 1.21




CA 02512324 2005-07-18
27
Results
Table 9
Dose r c a Slump Released
Water


Sample (gpt) (mm) (mm) (mm) (%) Volume Turbidity
ml NTU


Blank 0 > 100 2 n/a < 0.5 44 > 1000


330 80 11 3 10.0 59 > 1000


A 495 50 17 6 22.0 69 169


660 30 34 17 56.7 100 49


330 68 11 3 11.8 38 369


C 495 30 29 15 46.7 70 82


660 25 47 44 12.0 98 40


330 58 11 4 12.1 45 1000
E


660 25 43 23 80.0 92 27


EXAMPLE 5
Selected samples taken from example 1 were evaluated according to the
procedures detailed in example 1 using a red mud tailings slurry obtained
from a alumina refinery.
Table 10
Solids Content (% 27.4
wt/wt)


Solids < 75 um (% 26.7
wt/wt)


Specific Gravity 1.25




CA 02512324 2005-07-18
28
Results
Table 11
Dose r c a Slump Released
Water


Sample (gpt) (mm) (mm) (mm) (%) Volume Turbidity
ml NTU


Blank 0 85 2 n/a < 0.5 240 > 1000


C 874 83 5 4 0.6 10 > 1000


292 45 19 8 24.4 55 800


E 438 48 16 7 18.8 19 604


729 63 12 5 11.1 35 NT


584 73 8 3 6.8 19 > 1000


720 34 31 17 41.2 80 349
F


875 31 28 13 48.4 97 233


1022 31 32 12 64.5 92 222


583 68 12 5 10.3 91 > 1000
J


874 45 17 8 20.0 79 950


W 874 47 16 3 27.7 29 143


EXAMPLE 6
Selected samples taken from example 1 were evaluated according to the
procedures detailed in example 1 using a tailings slurry obtained from a gold
CIL/CIP processing operation
Table 12
Solids Content (% 53.3
wt/wt)


Solids < 75 um (% 35.4
wt/wt)


Specific Gravity 1.58




CA 02512324 2005-07-18
29
Results
Table 13
Dose r c a Slump Released
Water


Sample (gpt) (mm) (mm) (mm) (%) Volume Turbidity
ml NTU


Blank 0 > 100 2 n/a < 0.5 22 > 1000


119 49 14 7 14.3 32 38


A 238 52 12 7 9.6 48 95


356 45 18 7 24.4 20 266


238 40 22 8 35.0 20 256
C


356 28 38 21 60.7 28 42


238 39 22 8 35.9 18 497
F


356 25 40 23 68.0 45 22


119 39 22 8 35.9 18 497


J 238 25 40 23 68.0 45 22


356 39 22 8 35.9 18 497


EXAMPLE 7
Selected samples taken from example 1 were evaluated according to the
procedures detailed in example 1 using a tailings slurry obtained from a
lead/zinc mineral processing operation.
Table 14
Solids Content (% 53.4
wt/wt)


Solids < 75 um (% 45.8
wt/wt)


Specific Gravity 1.52




CA 02512324 2005-07-18
Results
Table 15
Dose r c a Slump Released
Water


Sample (gpt) (mm) (mm) (mm) (%) Volume Turbidity
ml NTU


Blank 0 104 5 4 1.0 0 n/a


123 95 6 3 3.2 0 n/a


A 246 93 6 4 2.2 0 n/a


370 83 7 4 3.6 0 n/a


62 85 7 4 3.5 0 n/a


123 63 13 7 9.5 0 n/a
C


246 45 20 9 24.4 0 n/a


370 34 29 24 14.7 0 n/a


62 98 6 4 2.0 0 n/a


E 123 93 6 4 2.2 0 n/a


246 57 9 7 3.5 0 n/a


370 35 29 18 31.4 0 n/a


EXAMPLE 8
5 Selected samples taken from example 1 were evaluated according to the
procedures detailed in example 1 using a tailings slurry obtained from a coal
preparation plant. Due to the low solids of content of this sample, the slump
cylinder size was increased to 50 mm diameter x 100 mm height and 500 ml
aliquots of substrate used. A clarity wedge was also used to assess the
10 clarity of the released water.
Table 16
Solids Content (% 18.5
wt/wt)


Solids < 75 um (% 10.9
wt/wt)


Specific Gravity 1.09




CA 02512324 2005-07-18
31
Results
Table 17
Dose r c a Slump Released
Water


Sample (gpt) (mm) (mm) (mm) (%) Volume Clarity
ml 0-48


Blank 0 > 100 2 n/a < 0.5 46 0


124 > 100 3 n/a < 0.5 163 43


A 371 53 16 10 11.3 290 > 48


494 29 44 36 27.6 300 > 48
I


124 40 22 10 30.0 285 48


C 247 34 33 19 41.2 315 47


371 26 45 40 19.2 300 45


124 33 31 14 51.5 290 > 48


E 247 30 40 25 50.0 320 47


371 29 41 26 51.7 300 47


EXAMPLE 9
Laboratory Evaluation
Product 1 is an inverse emulsion containing a 80/20 sodium
acrylate/acrylamide copolymer.
Product 1 was inverted into water to provide an aqueous solution containing
0.35% active polymer. The product was evaluated on a combination of fine
and coarse tailings from a mineral sands operation according to the methods
outlined in Example 1 above.
Fine solids fraction: thickener underflow @ 27.7% wt/wt
Coarse solids fraction: cyclone rejects @ 96.4% wt/wt
Where possible, the blend of coarse and fine solids were diluted with water
to a target solids of 43 - 47% wt/wt.
Results




Image


CA 02512324 2005-07-18
33
The photographs show the improved stacking of the treated compared to the
untreated tailings. This is especially true for co-disposal of coarse and fine
material with higher proportions of the coarse fraction.
EXAMPLE 10
Product 2A is an gel product consisting of a 30/70 sodium
acrylate/acrylamide copolymer.
Product 2A was dissolved into water to provide an aqueous solution
containing 0.25 % product as supplied. The polymer was evaluated on a
combined fine and coarse tailings from a coal preparation operation at a
dosage of 740 gpt. The total solids content of the combined tails was
approximately 19% wt/wt and approximately 1.4:1 fines/coarse ratio.
Treatment tests, employing the solution of Product 2B, were conducted using
the following method:
1. 500 ml of the tails slurry was sampled into a 600 ml plastic beaker.
2. The slurry was then subjected to low shear mixing by pouring the sample
from one 600 ml beaker to another to ensure that the sample was
homogeneous.
3. The required dose of aqueous polymer solution was added to the tailings
slurry and mixing continued until a consistent material was produced.
4. The material was transferred into a 500 ml measuring cylinder and left to
compact for several days, after which the liberated water was decanted
and discarded.
5. Sections were taken from the top and the bottom of the compacted solids
and analysed to determine the particle size distribution of the solids in
each section.

CA 02512324 2005-07-18
34
Results
The particle size distribution in each section are represented graphically in
Figure's 1 and 2.
Figure 2: Treated Coal Tailings - 740 gpt of Polymer 2A


CA 02512324 2005-07-18
Figure 1 shows that for the untreated material, a high degree of segregation
in the compacted solids has occurred with the majority of the coarse particles
only present in the bottom section of the sample. Figure 2 shows that for the
5 material treated with 740 gpt of Polymer 2A, the particle size distributions
in
both the top and the bottom sections are very similar, and only minimal
segregation has occurred during compaction.
EXAMPLE 11
Product 2A was evaluated according to the procedures detailed in example
10 10 on a combined fine and coarse tailings from a gold CIL/CIP processing
operation at a dosage of 240 gpt. The total solids content of the combined
tails was approximately 53% wt/wt with approximately 2:1 fines/coarse
ratio.
Results
15 The particle size distribution in each section are represented graphically
in
Figure's 3 and 4.
Figure 3: Untreated Gold Tailings

CA 02512324 2005-07-18
36
Figure 4: Treated Gold Tailings - 240 gpt of Polymer 2A
Figure 3 shows a high degree of segregation of the coarse solids to the
bottom section for the untreated material where as for the material treated
with Polymer 2A, Figure 4 shows that the top and bottom sections contain
similar amounts of both coarse and fine particles.
EXAMPLE 12
Product 2B is an inverse emulsion containing a 30/70 sodium
acrylate/acrylamide copolymer.
Product 2B was inverted into water to provide an aqueous solution
containing 1.0% product as supplied. The polymer was evaluated on a
combined fine and coarse tailings from a mineral sands operation. The total
solids content of the combined tails was 53% wt/wt with a fines/coarse ratio
of approximately 1:5.
Laboratory Evaluation
Treatment tests, employing the solution of Product 2B, were conducted using
the following method:


CA 02512324 2005-07-18
37
1. Tails slurry is sampled into a 1 litre plastic bottle up to the graduation
mark.
2. The slurry is then subjected to high shear mixing of ~1500rpm using
an overhead stirrer and a suitably machined marine impellor, in order
to produce a vortex.
3. The required amount of polymer solution is added to the vortex of the
slurry created by the high shear mixing.
4. The contents of the plastic bottle is allowed to mix for 1 minute.
5. After this period had elapsed, slurry is sampled into 250m1 plastic
bottles, full to the neck, and these are subsequently tumbled at 25rpm
for X minutes.
6. At the appropriate times, Slump tests are carried out as per Example
1.
Results
Table 19
Dose Rate Mixing Time Sump Slump
Product ( gpt ) ( min ) Radius ( % )
(mm)


5 146 0


Blank 0 10 152 0


15 145 0


5 80 12.5


50 10 85 7.1


15 130 0.4


5 45 53.3


Product 2B 100 10 73 13.8


15 90 2.8


5 35 97.1


150 10 48 50.5


15 83 8.5




CA 02512324 2005-07-18
38
Plant Evaluation
The tails from the Mineral Sands process is pumped uphill out of the lagoon-
covered mining area to a raised tailings disposal area. The low viscosity of
the waste stream together with the high flow rates means that solids are
deposited over a great distance, and a long way from the discharge point.
Scouring by the tailings stream also creates deep channelling in the disposal
area. The fluidity of the flow endangers the operation of the mine since at
maximum flows, the tails can flow back down into the mining area, swamping
the lagoon and interfering with mining efficiency.
The application of this invention via the introduction of a 0.5% (as supplied)
aqueous solution of a 30% anionic inverse emulsion polymer (Product 2B),
at a dosage of 100g/tonne of dry solids, into the pipeline feeding a mixed
fines (thickener underflow) and coarse rejects slurry fractions at a rate of
20
and 50 Ips respectively to the disposal area. Based on the above laboratory
evaluation, a dosing point close (20 meters or 11 seconds) to the discharge
point was chosen to minimise shearing of the treated material. This achieved
a heap of treated material with a stacking angle of 8-10 degrees (measured
using a surveyors inclinometer), clean water release and samples from the
stack showing a high sub 75 micron content confirming a retention of the fine
material within the heap disposal.


CA 02512324 2005-07-18
39
Fi-gure 5: Untreated Fi_~ ug re 6: Treated @ 100gpt (Product
2B)
Figure 5 and Figure 6 show the discharge of the mineral sands tailings
without and with treatment. In Figure 5, the tails are highly mobile and there
is no deposition of solids at the point of discharge. Figure 6 shows stacking
of the treated tailings underneath the discharge point and the liberation of
clean water in the foreground.
EXAMPLE 13
Product 2B is an inverse emulsion containing a 30/70 sodium
acrylate/acrylamide copolymer as used in Example 12 above. Product 3 is a
solution grade, sodium polyacrylate homopolymer.
Product 2B was inverted into water to provide an aqueous solution
containing 1.0% product as supplied. Product 3 was used as supplied with
no further dilution necessary. The polymers were evaluated on a combined
fine and coarse tailings from a mineral sands operation. The solids of the
combined tails was 67% wt/wt with a fines/coarse ratio of approximately 1:7.
Laboratory Evaluation
Treatment tests, employing the solution of Product 2B, and Product, 3 were
conducted using the following method:


CA 02512324 2005-07-18
1. A 250 ml aliquot of the homogenous combined tails slurry is placed into a
500 ml beaker.
2. The slurry is then subjected to mixing of ~500rpm using an overhead
stirrer and a suitably machined paddle impellor.
5 3. The required dose of polymer is added to the slurry and mixing continued
for either 10, 20 or 30 seconds.
4. Approximately 150 ml of the treated slurry is transferred to a 200 ml
beaker and the yield stress measured using a vane viscometer.
Further tests were also carried out on Product 2B and 3 to evaluate the
10 effect of different fines/coarse tailings ratio, using the above procedure
and a
constant mixing time of 20 seconds.
Results
Table 20
Dose field
Stress
(Pa)
After
Mixing


Product
(g/t) 10 sec 20 sec 30 sec


Blank 0 5 4 3


53 109 103 90


Product 2B 107 217 183 115


160 356 90 211


22 97 105 95


Product 3 888 181 200 168


1155 78 351 73


15 The results show that both products increased the yield stress of the
combined mineral sands tails. Free water drainage was present at high
doses.
The effect of different fines to coarse ratios are represented graphically
below. At all ratios tested, both Product 2B and Product 3 significant
20 increased the yield stress of the mineral sands tailings.

CA 02512324 2005-07-18
41
Fi-g_ure 7: Fi ure 8:
Plant Evaluation
The underflow of a thickener in which slimes are compacted is combined
with the waste sand fraction from the Mineral Sands operation. The ratio of
sand to slimes varies with ore type, and the rheology and drainage rates of
the deposited combination vary as a result.
The mining operation is mobile and follows the line of the ore body. The
combined waste material is pumped to a series of pits that are filled
sequentially and re-vegetated afterwards. It is desirable for the mining
company to operate in as small a footprint as possible at any one time.
Faster dewatering rates would allow the rehabilitation process to be started
earlier. Additional drainage water could be returned to the process plant for
improved efficiency's and reduced imported water costs.
The application of this invention at the site described above is as follows:
Product 3 was dosed at dosage was 1050 gpt over a three day period,
added after the screw conveyer and before the small centrifugal pump. The
result was an improved slump angle and much greater release of water from
the slurry. Figures 9, 10 and 11 show the slump angle at discharge into the
dam for untreated tails, and tails treated with 513 gpt and 1050 gpt
respectively.


CA 02512324 2005-07-18
42
Figure 9: Untreated Fi ure 10: Product 3 @ 513gpt
The dosing point was modified and Product 3 added directly after the
centrifugal pump. The dosage was reduced to 726g/T with the alternative
position. The same sand consistency was generated using this point.
24hours later the free drainage and porosity on the surface of the dam was
apparent. Figures 12 and 13 show the discharge characteristics and the dam
surface respectively.
Figure 12: Discharge Pipe Figure 13: Surface Area
Figure 11: Product 3 @ 1050gpt


CA 02512324 2005-07-18
43
EXAMPLE 14
Selected samples taken from example 1 were evaluated according to the
procedures detailed in example 1 using a tailings slurry obtained from a oil
sands processing operation. Facility was included for the collection and
measurement of the quantity and residual suspended solids content of the
released water. Due to the poor turbidity of the release water, a water
clarifies was added to the tailing treatment process. Clarity was assessed by
percentage solids (water can be accepted straight into the plant if the water
solids are below 0.5%).
Tests were conducted using a 70mm by 70mm collar. Rheology modifier
products were prepared and used at a concentration of 0.3% and the water
clarifies was prepared and used at a concentration of 1 %. Clarifies solution
is
added several seconds after the rigidifying polymer is added.
Water quantity and quality were evaluated after 30 minutes. All test work was
conducted at 40 °C.
Table 20
Solids Content (% 51.8
wt/wt)


Sand to fines ratio 6.05:1


Specific Gravity 1.45


Results
Table 21
Released
Water


d c a Slump AvaliableSus ended
Sample Dose (gpt) p


(mm) (mm) (mm) (%) solids


release (%)


%)




CA 02512324 2005-07-18
44
Blank 0 >200 - - 0 - -


155 160 20 4 20.0 25.1


D 130 180 22 4 20.0 44.7 1.12


104 121 14 3 18.2 55.7 1.39


130 +
' 150 29 5 32.0 36.9 0.29


45 clarifies


104 +
' 90 45 0 100.0 47.9 25
0


D + 45 clarifies .


water 78+


clarifies43 clarifies'140 50 0 90.9 52.5 0.35


104+


21.5 120 40 0 66.7 52.0 0.59


clarifier~


D + 104+ 180 42 0 46.7 47.3 0.93
43 clarifier2


t


wa 104+ 17 40 0 72.7 63.1 0.26
er 86 clarifierz0
clarifies


1. Low molecular weight anionic polymer.
2. Low molecular weight cationic polymer.
The results shows that stacking can be achieved when using Product D.
However results indicate that the water release when using Rheology
modifier D alone is improved when a water clarifies is employed in
combination with a Rheology modifier. The water released is of suitable
quality for re-use in the plant without the need for further water polishing.

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Administrative Status

Title Date
Forecasted Issue Date 2015-11-24
(22) Filed 2005-07-18
(41) Open to Public Inspection 2007-01-18
Examination Requested 2010-05-11
(45) Issued 2015-11-24

Abandonment History

Abandonment Date Reason Reinstatement Date
2014-08-04 FAILURE TO PAY FINAL FEE 2015-07-30

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Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $400.00 2005-07-18
Registration of a document - section 124 $100.00 2005-11-24
Maintenance Fee - Application - New Act 2 2007-07-18 $100.00 2007-05-16
Maintenance Fee - Application - New Act 3 2008-07-18 $100.00 2008-06-05
Maintenance Fee - Application - New Act 4 2009-07-20 $100.00 2009-05-13
Request for Examination $800.00 2010-05-11
Maintenance Fee - Application - New Act 5 2010-07-19 $200.00 2010-07-13
Maintenance Fee - Application - New Act 6 2011-07-18 $200.00 2011-06-17
Maintenance Fee - Application - New Act 7 2012-07-18 $200.00 2012-06-22
Registration of a document - section 124 $100.00 2012-07-10
Registration of a document - section 124 $100.00 2012-07-10
Registration of a document - section 124 $100.00 2012-07-10
Maintenance Fee - Application - New Act 8 2013-07-18 $200.00 2013-07-17
Maintenance Fee - Application - New Act 9 2014-07-18 $200.00 2014-07-09
Maintenance Fee - Application - New Act 10 2015-07-20 $250.00 2015-07-15
Reinstatement - Failure to pay final fee $200.00 2015-07-30
Final Fee $300.00 2015-07-30
Maintenance Fee - Patent - New Act 11 2016-07-18 $250.00 2016-07-04
Maintenance Fee - Patent - New Act 12 2017-07-18 $250.00 2017-06-23
Maintenance Fee - Patent - New Act 13 2018-07-18 $250.00 2018-06-25
Maintenance Fee - Patent - New Act 14 2019-07-18 $250.00 2019-06-21
Maintenance Fee - Patent - New Act 15 2020-07-20 $450.00 2020-06-23
Maintenance Fee - Patent - New Act 16 2021-07-19 $459.00 2021-06-21
Maintenance Fee - Patent - New Act 17 2022-07-18 $458.08 2022-06-21
Maintenance Fee - Patent - New Act 18 2023-07-18 $473.65 2023-06-21
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
BASF SE
Past Owners on Record
BASF SPECIALTY CHEMICALS HOLDING GMBH
CIBA HOLDING INC.
CIBA SPECIALTY CHEMICALS HOLDING INC.
DYMOND, BRIAN
HARMAN, RONALD L.
MCCOLL, PHILIP
SCAMMELL, STEPHEN ROSS
SCHAFFER, RONALD J.
WHITHAM, LOUISE ELIZABETH
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 2005-07-18 1 18
Claims 2005-07-18 4 165
Description 2005-07-18 44 2,443
Cover Page 2007-01-09 1 30
Claims 2012-10-15 6 194
Claims 2013-09-26 6 205
Cover Page 2015-10-21 1 28
Correspondence 2005-08-26 1 26
Assignment 2005-07-18 2 81
Assignment 2005-11-24 7 193
Office Letter 2018-03-23 1 23
Prosecution-Amendment 2010-05-11 1 44
Prosecution-Amendment 2012-04-13 4 148
Correspondence 2013-01-14 5 133
Assignment 2012-07-10 6 239
Prosecution-Amendment 2012-10-15 11 472
Correspondence 2012-10-19 1 14
Correspondence 2012-10-19 1 18
Correspondence 2013-01-25 1 15
Prosecution-Amendment 2013-03-26 2 46
Fees 2013-07-17 1 163
Prosecution-Amendment 2013-09-26 8 277
Fees 2014-07-09 1 33
Reinstatement 2015-07-30 2 57
Final Fee 2015-07-30 2 52
Correspondence 2015-09-17 1 26