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Patent 2196522 Summary

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(12) Patent: (11) CA 2196522
(54) English Title: TREATMENT OF OIL, WATER AND SAND MIXTURES
(54) French Title: METHODE DE TRAITEMENT DES MELANGES D'EAU, DE SABLES ET DE PRODUITS HUILEUX
Status: Expired and beyond the Period of Reversal
Bibliographic Data
(51) International Patent Classification (IPC):
  • B01D 21/02 (2006.01)
  • B01D 17/00 (2006.01)
  • B01D 21/00 (2006.01)
(72) Inventors :
  • SAIK, LARRY (Canada)
(73) Owners :
  • 1303365 ALBERTA LTD.
(71) Applicants :
  • LARRY SAIK (Canada)
(74) Agent: J. GORDON THOMSON
(74) Associate agent:
(45) Issued: 2004-06-29
(22) Filed Date: 1997-01-31
(41) Open to Public Inspection: 1998-08-01
Examination requested: 2001-02-05
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data: None

Abstracts

English Abstract

The invention comprises a method and apparatus for treating oil, water and sand mixtures to separate the components. The apparatus comprises an arrangement of four sequential treatment cells, each comprising an agitation chamber including a rotating paddle and agitation baffles and a settlement chamber. The mixture is agitated in the first agitation chamber and transferred to the first settlement chamber where the sand settles to the bottom. Means are provided for transferring sand from each settlement chamber to the agitation chamber of the next cell. The transfer means may comprise pressurized water jets which dislodge the sand allowing it to fall through an opening in the bottom of the settlement chamber and into the next agitation chamber. The agitation and settlement steps are repeated in each cell. There are four transfer tanks associated with each cell where the oil and water drawn from the settlement chamber are separated. The treated sand is washed with fresh water in the fourth cell and collected and dried by a basket centrifuge. Means are also provided to recirculate the water, which may include an added surfactant and/or a demulsifier, from each transfer tank backward through the treatment cells.


French Abstract

L'invention comprend un procédé et un appareil de traitement de mélanges de produits huileux, d'eau et de sable en vue d'en séparer les composants. L'appareil comprend un arrangement de quatre cellules séquentielles de traitement, chaque cellule comprenant une chambre d'agitation, qui possède une palette tournante et des déflecteurs d'agitation, et une chambre de décantation. Le mélange s'agite dans la première chambre d'agitation et est transféré à la première chambre de décantation au fond de laquelle le sable se dépose. Des moyens sont fournis pour transférer le sable entre les chambres de décantation et jusqu'à la chambre d'agitation de la cellule suivante. Les moyens de transfert peuvent comprendre des jets d'eau sous pression qui déloge le sable, ce qui lui permet de tomber dans une ouverture au bas de la chambre de décantation jusque dans la chambre d'agitation suivante. Les étapes d'agitation et de décantation sont répétées dans chaque cellule. Quatre réservoirs de transfert sont associés à cellule, où les produits huileux et l'eau sont retirés de la chambre de décantation et sont séparés. Le sable traité est nettoyé avec de l'eau pure dans la quatrième cellule et est amassé et séché par une centrifugeuse à bol perforé. Des moyens sont également fournis pour faire recirculer l'eau, moyens qui peuvent comprendre un surfactif et/ou un désémulsifiant, pour une recirculation de chaque réservoir de transfert jusqu'aux cellules de traitement.

Claims

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


The embodiments of the invention in which an exclusive property or privilege
is
claimed are defined as follows:
1. An apparatus for separating solids comprising sand from oil in a feedstock
comprising the solids and oil, the apparatus comprising:
a. first, second, third and fourth cells each comprising an agitation chamber
and a settling
chamber, wherein each agitation chamber comprises an inlet, an outlet and
agitation
means and wherein each settling chamber comprises an inlet, a fluid outlet and
a solids
outlet, wherein the agitation chamber outlet communicates with the settling
chamber
inlet, and wherein the solids outlet of the first settling chamber leads to
the inlet of the
second agitation chamber, the solids outlet of the second settling chamber
leads to the
inlet of the third agitation chamber and the solids outlet of the third
settling chamber
leads to the fourth agitation chamber;
b. means to introduce said feedstock and an aqueous phase comprising water
through the
inlet of the first agitation chamber;
c. means for adding an effective amount of surfactant into each of the
agitation chambers;
d. means for collecting the solids associated with the solids outlet of the
fourth settling
chamber;

e. transfer means associated with each of the solids outlet of the settling
chamber for
transferring solids from the settling chamber to the next agitation chamber or
the solid
collection means.
2. The apparatus of claim 1 wherein the agitation means comprises a rotatable
paddle having
an axis of rotation and at least one baffle member.
The apparatus of claim 2 wherein there are two baffles.
4. The apparatus of one of claims 2 or 3 wherein the baffle member is elongate
and is
oriented parallel to the axis of rotation of the paddle.
5. The apparatus of claim 1, 2 or 3 further comprising first, second, third
and fourth transfer
tanks associated with the fluid outlets of the first, second, third and fourth
settling chambers
respectively, wherein the transfer tanks receive the oil and aqueous phase
from the corresponding
settling chamber and at least one transfer tank comprises skimming means to
collect oil which
coalesces and floats to the top of the fluid within the transfer tank.
6. The apparatus of claim 5 wherein the first, second and third transfer tanks
each comprise
skimming means to collect oil which coalesces and floats to the top of the
fluid within the transfer
tank.

The apparatus of claim 5 or 6 further comprising a fresh water supply
associated with the
fourth agitation chamber, a disposal tank and aqueous phase circulation means
for introducing
fresh water into the fourth agitation chamber and circulating the aqueous
phase from the fourth
transfer tank to the third agitation chamber, from the third transfer tank to
the second agitation
chamber, from the second transfer tank to the first agitation chamber and from
the first transfer
tank to the disposal tank.
The apparatus of claim 1, 2 or 3 wherein the solid transfer means comprises at
least one
pressurized fluid jet.
9. The apparatus of claim 8 wherein each chamber has a bottom end which
defines a bottom
opening and comprises a door associated with the bottom opening and moveable
between a closed
position and an open position and wherein the bottom opening is positioned
above the inlet of the
next agitation chamber in the case of the first, second and third settling
chambers or the solid
collection means in the case of the fourth settling chamber, whereby solids
passing through the
bottom opening enter the next agitation chamber or the solid collection means.
10. The apparatus of claim 9 wherein the at least on pressurized fluid jet
causes solids settled at
the bottom of each settling chamber to pass through the bottom opening when
the door is in the
open position.
11. The apparatus of claim 10 wherein there are at least two pressurized fluid
jets, one above
the other, and control means to activate the fluid jets sequentially with the
opening and closing of
the door in the following sequence:

(a) once the level of solids settled at the bottom of the settling chamber
exceeds a
predetermined level above the upper fluid jet, the door is opened;
(b) the lower fluid jet is activated;
(c) the door is closed; and,
(d) the upper fluid jet is activated;
whereby the activation of the lower fluid jet causes a portion of the settled
solids to be displaced
and pass through the opening and the activation of the upper fluid jet causes
the remaining settled
solids to take the place of the displaced settled solids.
12. The apparatus of claim 11 wherein there are a plurality of lower fluid
jets arranged in one
or more substantially horizontal row and there are a plurality of upper fluid
jets arranged in one or
more substantially horizontal row.
13. The apparatus of claim 12 further comprising first, second, third and
fourth transfer tanks
associated with the fluid outlets of the first, second, third and fourth
settling chambers
respectively, wherein the transfer tanks receive the oil and aqueous phase
from the corresponding
settling chamber and at least one transfer tank comprises skimming means to
collect oil which
coalesces and floats to the top of the fluid within the transfer tank.

14. The apparatus of claim 13 wherein the first, second and third transfer
tanks comprise
skimming means to collect oil which coalesces and floats to the top of the
fluid within each
transfer tank.
15. The apparatus of claim 13 or 14 further comprising a fresh water supply
associated with
the fourth agitation chamber, a disposal tank and a aqueous phase circulation
means for
introducing fresh water into the fourth agitation chamber and circulating the
aqueous phase from
the fourth transfer tank to the third agitation chamber, from the third
transfer tank to the second
agitation chamber, from the second transfer tank to the first agitation
chamber and from the first
transfer tank to the disposal tank.
16. A process for separating solids comprising sand from oil in a feedstock
comprising the
solids and the oil, the method comprising the steps of:
(a) combining the feedstock with an aqueous phase comprising water and an
effective
amount of surfactant to form a first mixture;
(b) agitating the first mixture at a temperature in the range of about 85 to
95°C to form
a first froth-like emulsion;
(c) removing the first emulsion and allowing the first emulsion to settle such
the oil
coalesces and separates from the aqueous phase and the solid particles settle;

(d) removing the settled solids from step (c) and combing the settled solids
with
additional aqueous phase to form a second mixture;
(e) repeating steps (b) and (c) as steps (e.1) and (e.2) with the second
mixture;
(f) removing the settled solids from step (e.2) and combining the settled
solids with
additional aqueous phase to form a third mixture;
(g) repeating steps (b) and (c) as steps (g.1) and (g.2) with the third
mixture;
(h) combining the settled solids from step (g.2) with additional aqueous phase
and
agitating to wash the solids;
(i) collecting the solids.
17. The process of claim 16 wherein the additional aqueous phase added to the
agitation step
(h) comprises an effective amount of a demulsifier and may or may not comprise
the surfactant
agent.
18. The process of claim 16 wherein the agitation steps occur within agitation
chambers
comprising a rotatable paddle and at least one baffle member to aid in
agitation.

19. The process of claim 16 wherein steps (d) and (f) occur within settling
chambers
comprising transfer means to remove solids accumulated at the bottom of the
settling chamber and
deposit the solids into the next agitation chamber.
20. The process of claim 19 wherein steps (c), (e.2) and (g.2) occur by
overflow over a divider
between the agitation chamber and the settling chamber.
21. The process of claims 16, 17, 18, 19, or 20 wherein the aqueous phase is
recirculated by
the following additional steps:
a, recovering the aqueous phase from the fourth settling chamber and
transferring said
aqueous phase to the third agitation chamber;
b. recovering the aqueous phase from the third settling chamber and
transferring said
aqueous phase to the second agitation chamber;
c. recovering the aqueous phase from the second settling chamber and
transferring
said aqueous phase to the first agitation chamber; and,
d. recovering the aqueous phase from the first settling chamber and
transferring said
aqueous phase to a disposal tank from where said aqueous phase may be disposed
or transferred to the first agitation chamber.

22. The method of claim 21 wherein the recirculation of aqueous phase results
in some
demulsifier being present in each of the agitation steps.
23. The method of claim 16, 21 or 22 wherein feedstock is continuously added
to the first
agitation chamber and each step of the method is substantially continuous once
the method is
initiated.

Description

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


219522
TREATMENT OF OIL. WATER AND SAND MIXTURES
TECHNICAL FIELD
The present invention relates to a method of and apparatus for the treatment
of
oil, water and sand mixtures and more particularly to the treatment of storage
residues
comprising oil, water and sand.
BACKGROUND ART
Oil storage tanks are used to store the mixture of fluids that is immediately
pumped from oil wells in the field. In such tanks, the oil, water and solid
phases separate and
the solids settle to the bottom of the tank and the oil rises to the top. As
oil is drawn from
the top of the tank, sand and water may accumulate at the bottom of the tank.
Other
particulate matter such as shale or clay may also accumulate. A significant
amount of oil may
remain emulsified in the water and adsorbed on the surface of the solid
particulate matter.
This is especially true for the heavy oils which are produced in certain
regions of Alberta and
Saskatchewan, Canada. The water may have significant concentrations of
chlorides in
solution.
The oily sand is occasionally removed from storage tanks by a process known
as "stinging" where a jet of water is used to stir up the sand at the same
time suction is
applied by a vacuum truck to remove the oily sand and water. The oily sand and
water may
then be disposed of or utilized in applications such as dust control on gravel
roads. An

219652
analysis of a sample taken from a storage tank in Innisfree, Alberta
demonstrates the
following composition of the non-aqueous components:
Table 1 lw:w~
Oil/Paraffin 17.65%
Asphaltene 1.81%
Carbonates 0.34%
Iron Salts 0.68%
Insolubles 79.52%
The insolubles consisted primarily of high silica sand.
Conventional techniques for separating the sand such as settling pits or
centrifuging do not effectively remove and recover all of the non-sand
components. Nor are
such conventional techniques cost-effective or environmentally sound. Of
course it is well
known that certain surfactants will remove the oil from the sand, however,
there is no known
process for doing so and economically recovering both the oil and the sand.
There is a need in the art for a new method and apparatus of recovering clean
sand and refinable oil from such mixtures which is effective in completely
separating these
components in an economical and convenient manner. It would further be
advantageous if
-2-

21~ss2~
such a method were continuous and could be performed by an apparatus that is
self contained.
DISCLOSURE OF INVENTION
The present invention relates to an apparatus for separating solids comprising
sand from oil in a feedstock comprising the solids, the oil, and an aqueous
phase. In one
aspect of the invention, the apparatus comprises:
(a) first, second, third and fourth cells each comprising an agritation
chamber and a
settling chamber, wherein each agitation chamber comprises an inlet, an outlet
and agitation
means and wherein each settling chamber comprises an inlet, a fluid outlet and
a solids outlet
and wherein the solids outlet of the first settling chamber leads to the inlet
of the second
agitation chamber, the solids outlet of the second settling chamber leads to
the inlet of the
third agitation chamber and the solids outlet of the third settling chamber
leads to the fourth
agitation chamber;
(b) means to introduce the solids, the oil and the aqueous phase through the
inlet
of the first agitation chamber;
(c) solid collection means associated with the solids outlet of the fourth
settling
chamber;
-3-

219632
(d) transfer means associated with each of the solids outlet of the settling
chambers
to transfer solids from the settling chamber to the next agitation chamber or
the solid
collection means.
The agitation means may comprise a rotatable paddle having an axis of rotation
and at least one baffle member. In a preferred embodiment, there are two
baffle members
which are elongate and oriented parallel to the axis of rotation of the
paddle.
There may also be first, second, third and fourth transfer tanks associated
with
the fluid outlets of the first, second, third and fourth settling chambers
respectively, wherein
the transfer tanks receives the oil and aqueous phase from the corresponding
settling chamber
and at least one transfer tank comprises skimming means to collect oil which
coalesces and
floats to the top of the fluid within each oil skimmer tank. The first, second
and third
transfer tanks may comprise skimming means to collect oil which coalesces and
floats to the
top of the fluid within each transfer tank.
In a preferred embodiment, a fresh water supply is provided which is
associated
with the fourth agitation chamber along with a disposal tank and aqueous phase
circulation
means for introducing fresh water into the fourth agitation chamber and
circulating the
aqueous phase from the fourth transfer tank to the third agitation chamber,
from the third
transfer tank to the second agitation chamber, from the second transfer tank
to the first
agitation chamber and from the first transfer tank to the disposal tank.
-4-

~ns~2z
In a preferred embodiment, the solid transfer means comprises at least one
pressurized fluid jet. Further, each settling chamber has a bottom end and
defines a bottom
opening and comprises a door associated with the bottom opening and moveable
between a
closed position and an open position and wherein the bottom opening is
positioned above the
inlet of the next agitation chamber in the case of the first, second and third
settling chambers
or the solid collection means in the case of the fourth settling chamber,
whereby solids
passing through the bottom opening enter the next agitation chamber on the
solid collection
means.
The at least one pressurized fluid jet causes solids settled at the bottom of
each
settling chamber to pass through the bottom opening when the door is in the
open position.
There may be a plurality of upper and lower pressurized fluid jets and control
means to
activate the fluid jets sequentially with the opening and closing of the door
in the following
sequence:
(a) once the level of solids settled at the bottom of the settling chamber
exceeds a
predetermined level above the upper fluid jet, the door is opened;
(b) the lower fluid jets are activated;
(c) the door is closed; and
-5-

219~~N~
(d) the upper fluid jets are activated;
whereby the activation of the lower fluid jets causes a portion of the settled
solids to be
displaced and pass through the opening and the activation of the upper fluid
jets causes the
remaining settled solids to take the place of the displaced settled solids.
In a second aspect of the invention, its method form, the invention comprises
a
method for separating solids comprising sand from oil in a feedstock
comprising the solids
and the oil, the method comprising the steps of:
(a) combining the feedstock with an aqueous phase comprising water and an
effective amount of a surfactant to form a first mixture;
(b) agitating the first mixture at a temperature in the range of about 85 to
95°C to
form a first froth-like emulsion;
(c) removing the first emulsion and allowing the first emulsion to settle such
that
the oil coalesces and separates from the aqueous phase and the solid particles
settle;
(d) removing the settled solids from step (c) and combining the settled solids
with
additional aqueous phase to form a second mixture;
-6-

296522
(e) repeating steps (b), (c) and (d) as steps (e. l), (e.2) and (e.3) with the
second
mixture;
(f) removing the settled solids from step (e.3) and combining the settled
solids
with additional aqueous phase to form a third mixture;
(g) repeating steps (b), (c) and (d) as steps (g.1), (g.2) and (g.3) with the
third
mixture;
(h) combining the settled solids from step (g.3) with additional aqueous phase
and
agitating to wash the solids;
(i) collecting the solids.
The additional aqueous phase added to the agitation of step (h) comprises an
effective amount of a demulsifier and may or may not comprise the surfactant
agent. The
agitation steps occur within agitation chambers of the apparatus described
herein. The settling
steps occur within settling chambers of the apparatus described herein. The
settling chambers
comprise transfer means to remove solids accumulated at the bottom of the
settling chamber
and deposit the solids into the next cell.

2196522
~.
The aqueous phase is recirculated by the following additional steps:
(a) recovering the aqueous phase from the fourth settling chamber and
transferring
said aqueous phase to the third agitation chamber;
(b) recovering the aqueous phase from the third settling chamber and
transferring
said aqueous phase to the second agitation chamber;
(c) recovering the aqueous phase from the second settling chamber and
transferring
said aqueous phase to the first agitation chamber; and
(d) recovering the aqueous phase from the first settling chamber and
transferring
said aqueous phase to a disposal tank from where said aqueous phase may be
disposed or
transferred to the first agitation chamber.
As a result of the recirculation of aqueous phase, some demulsifier is present
in
each of the agitation steps. Feedstock is continuously added to the first
agitation chamber and
each step of the method is substantially continuous once the method is
initiated.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a schematic diagram of a preferred embodiment of the invention.
_g_

219622
Figure 2 is a cross-sectional view of a settling chamber of the invention.
Figure 3 is a cross-sectional view of an agitation chamber of the invention.
Figure 4 is a plan view of a treatment cell.
Figure 5 is a cross-sectional view of a skimmer tank of the invention.
BEST MODE OF CARRYING OUT INVENTION
Referring to Figure 1, the invention in its apparatus form is an apparatus for
separating an inert, solid inorganic fraction comprising sand from oil in a
feedstock
comprising the solid fraction, oil and an aqueous phase. The apparatus
comprises four cells
each comprising an agitation chamber and a settling chamber. In the preferred
embodiment of
the apparatus, the four cells are arranged in a cascading fashion to assist in
the flow of
feedstock through the apparatus. Feedstock is received in the first cell and
moves through the
cells in sequential order, as described hereinafter. The preferred embodiment
is hereinafter
described in relation to an apparatus where each agitation chamber is
approximately 3 metres
long, 2.5 metres wide and 2 metres deep, with a capacity of approximately 50
barrels. Each
corresponding settling chamber has an approximate capacity of 10 barrels. Of
course, the
invention described herein is not limited to an apparatus of those dimensions
and may be
practised on a larger or smaller scale.
-9-

CA 02196522 2003-11-03
In a second aspect of the invention, the invention is a method for separating
an
inert, solid inorganic fraction comprising sand from oil in a feedstock
comprising the sand, oil and
an aqueous phase. The invention in its method form will be described
concurrently with the
description of the apparatus and its operation.
Referring to Figures 2, 3 and 4, each cell is comprised of an agitation
chamber and
a settling chamber which are separated by a short transfer pipe. Each cell,
and the apparatus in
general, is constructed using conventional and well-known tank fabrication
techniques. In the
preferred embodiment, the agitation chamber is substantially rectangular in
shape while the
settling chamber is cylindrical. The settling chamber has a conically tapered
bottom section. The
transfer pipe between the agitation chamber and the settling chamber allows
overflow from the
agitation chamber to enter the settling chamber.
The flow of feedstock through the invention is as follows. Oily sand to be
processed is introduced into the first agitation chamber by means of a
conveyor. The feedstock
passes through a shaker screen to separate larger particles. Feedstock is then
mixed with water
which is recycled from the process as described below and a surfactant which
is injected into the
first agitation chamber by means of a chemical pump. The oil, sand and aqueous
phase are
agitated in the agitation chamber by a paddle which is mounted on an axle for
rotation. The
agitation produces a frothy emulsion which overflows into the first settling
chamber through the
transfer pipe. The overflow of feedstock into the first settling chamber is
caused by continuous
addition of feedstock into the first agitation chamber. In the first

219~~2~
settling chamber, the sand settles to the bottom and is transferred to the
next agitation
chamber as described below. The oil and aqueous phase is drawn off and pumped
to a first
skimmer tank where the oil is allowed to coalesce and float to the surface and
is collected.
The aqueous phase from the first skimmer tank is pumped to a disposal tank
where it may
either be pumped down a disposal well or reused in the first agitation
chamber. The process
of agitation with chemical treatment and settling is repeated in the second,
third and fourth
cells. Sand from the fourth settling chamber is transferred to a basket
centrifuge to remove
water. The end product is clean, dry sand.
The paddle is rotated by conventional motor means which produces sufficient
power to effectively agitate the feedstock. In the preferred embodiment, an
electric motor
having a peak capacity of 30 h.p. is effective. The agitation process is aided
by baffles
which run longitudinally across the agitation chamber, parallel to the axle
and paddle. The
baffles are preferably cylindrical and placed on either side of the paddle.
In the preferred embodiment, the paddle is centrally located within the
agitation chamber and rotates about a horizontal axis which is centred in the
horizontal plane,
as shown in Figure 2, and is located just below centre in the vertical plane,
as shown in
Figure 3. The paddle comprises two blades affixed to the axle in a planar
manner. The
blades are shaped to be wider at the two ends of the paddle as illustrated in
Figure 3.
Agitation is also aided by a sloping floor as shown in Figure 3. In the
preferred embodiment,
the floor is sloped in stages to approximate a curve which steepens as it
approaches the lateral
-11-

2I9G~2~
walls of the agitation chamber which are parallel to the rotation axis of the
paddle. The
radius of the curve is perpendicular to the rotation axis of the paddle. The
purpose of the
curve is to eliminate corners in the agitation chamber to ensure that
feedstock does not get
trapped where it might not be effectively agitated.
As shown in Figure 2, each settling chamber has a comically tapered bottom
portion and hydraulically actuated bottom doors. Water jets are provided at
four levels along
the bottom portion to approximately midway up the settling chamber. As the
sand settles to
the bottom, it compacts slightly under its own weight and may not move even
when the
bottom doors open. To displace the sand into the next cell, water is jetted
into the settling
chamber from the lower two rows of jets which dislodges the bottom level of
sand up to the
second row of jets. The dislodged sand falls through the open bottom doors and
into the next
agitation chamber. The doors are then closed. Next, the upper two rows of jets
are activated,
dislodging the sand level with the upper rows and allowing that sand to settle
to the bottom of
the settling chamber. Once enough sand settles to again reach past the
uppermost row of jets,
the process may be repeated. If the settlement rate of sand in the settling
chamber is known,
the sequential operation of the doors and water jetting may be operated by a
timer.
Alternatively, sensors (not shown) may be placed within the settling chamber
to determine the
level of settled sand and sequentially activate the doors and water jets.
As shown in Figure 1, first, second, third and fourth skimmer tanks are
provided to receive the fluid component comprising the oil and aqueous phases
which is
-12-

2191522
recovered from the first, second, third and fourth settling chambers
respectively. The first,
second and third skimmer tanks include means to skim off the oil which
coalesces and floats
to the top and pumps to draw off the aqueous phase for recycling within the
system. The
fourth skimming tank in the preferred embodiment does not require skimming
means to
collect oil as there is insufficient oil in that tank to coalesce and float to
the surface.
As shown in Figure 5, the skimmer tanks are of conventional construction,
having a skimming chamber, a water chamber, a baffle separating the two
chambers, an inlet,
an oil outlet and a water outlet. The baffle is raised approximately 30
centimeters off the
skimming tank floor to allow passage of the aqueous phase into the water
chamber while the
oil remains in the skimming chamber.
The aqueous phase from the first skimmer tank is pumped to a disposal tank
which acts as a reservoir for the system. Excess fluid in the disposal tank
may be pumped
down a disposal well. If additional fluid is required in the first agitation
chamber, it may be
drawn from the disposal tank. Aqueous phase from the second skimmer tank is
pumped into
and reused in the first agitation chamber. Similarly, aqueous phase from the
third skimmer
tank is pumped into the second agitation chamber and aqueous phase from the
fourth skimmer
tank is pumped into the third agitation chamber.
Each agitation chamber is heated by a conventional steam coil to a temperature
of approximately 90° Celsius. It has been found that effective results
are obtained in the
-13-

219u52~
range of 85° to 95° Celsius. In the first agitation chamber, the
paddle is rotated at
approximately 60 rpm which produces a froth-like emulsion of oil, sand and the
aqueous
phase. A surfactant is added to the first agitation chamber to aid in the
separation of the oil
from the sand.
In the second agitation chamber, the agitation step is repeated under
identical
conditions to the first agitation chamber. Aqueous phase containing surfactant
from the third
skimmer tank is added as described above. Additional surfactant is added if
necessary to
bring the concentration of surfactant in the aqueous phase to an effective
level. As in the first
cell, a froth-like emulsion is produced which is drawn off through the
transfer pipe into the
second settling chamber. There again, the sand settles to the bottom. When the
second
settling tank fills to capacity, the step of jetting the sand to the next
(third) agitation chamber
is repeated. From the second settling chamber, the oil and the aqueous phase
are pumped to
the second skimmer tank. After sufficient oil has accumulated in the second
settling tank, it
is skimmed off and collected. The aqueous phase is pumped back to the first
agitation
chamber to be reused in the system.
The agitation step is repeated in the third agitation chamber with sand from
the
second settling chamber and aqueous phase from the fourth skimming tank. It is
unnecessary
to agitate this mixture as vigorously as in the first two agitation chambers
as most of the oil
has been removed from the feedstock by this point in the process. In the
preferred
embodiment agitation in the range of 20 to 40 rpm is sufTicient. Again, the
agitated mixture
-14-

2~9G52~
i
feeds into the third settling chamber where the sand settles to the bottom and
is transferred to
the fourth agitation chamber. The aqueous phase and oil is removed to a third
skimming tank
where the oil skimming step is repeated. The aqueous phase from the third
skimming tank is
reintroduced into the system in the second agitation chamber.
The fourth cycle is primarily a wash cycle to remove all traces of treatment
chemicals and soluble components from the initial feedstock. Sand from the
third settling
chamber is combined with fresh water and agitated in the fourth agitation
chamber. No
surfactant is added because the sand is substantially free of oil. As in the
third agitation
chamber, vigourous agitation is unnecessary: rotation of the paddle in the 20
to 40 rpm range
is sufficient. A demulsifier is added to the fourth agitation chamber to
clarify the aqueous
phase. As in the previous three cycles, the sand mixture enters the fourth
settling chamber
where the sand settles out. The sand is jetted with fresh water to a
centrifuge basket which
removes the water, leaving clean dry sand. Other means to dry the sand may be
used in place
of the centrifuge basket, however, it is preferable that the water recovered
from the drying
means be recycled in the system. The water removed by the centrifuge basket
may be
recycled into the fourth agitation chamber.
As in the previous three cycles, the aqueous phase is collected in the fourth
skimming tank. No oil is recovered from the fourth settling tank because there
is very little
oil associated with the sand entering the fourth cell and also because no
surfactant is used in
the fourth cell.
-15-

219GS2)
1
Because the aqueous phase is recycled from each cell to the previous cell, the
demulsifier added to the fourth cell fords its way back to the first cell, in
diminishing
concentration through the cells. Therefore, in the first cell, the demulsifier
is present,
although significantly more dilute than in the fourth cell, along with the
surfactant which is
added to the first agitation chamber. The demulsifier should not interfere
with the efficacy of
the surfactant in the first agitation chamber. The concentration of the
surfactant is such that
the oil is effectively removed from the sand in the first agitation chamber
but is not so high
as to interfere in any appreciable way with the separation of the oil from the
aqueous phase in
the first skimming tank. The same may be true of the second and third skimming
tanks.
A surfactant which is suitable and effective for this process is X-TOL XT-
85'"'
which is available commercially from Petrolite Canada Inc., Calgary, Alberta.
According to
the manufacturers description, XT-85~ is a water soluble, acidic surfactant
which disperses
and suspends organic and inorganic acids and solubilizes heavy hydrocarbons. A
suitable and
effective demulsifying agent is Reaction 11104'M which is available
commercially from
Edmonton Chemical Distributors Inc., Edmonton, Alberta. According to the
manufacturer's
description, Reaction 11104T"' is a solution of cationic polyamines which
effectively clarifies
water by resolving oil in water emulsions.
The surfactant and the demulsifier are used in accordance with the
manufacturer's specifications. In the preferred embodiment of the present
invention, XT-85T°'
is injected into the first, second and third agitation chambers to achieve a
concentration of 100
-16-

21g~~2z
ppm ( I litre per 100 barrels) continuous. Reaction 11104'M is introduced at a
rate of 25 ppm
continuous into the fourth agitation chamber.
Once the preferred process has been initiated, only small amounts of the
surfactant need be added to the first and second agitation chambers to
maintain an effective
concentration because of the recirculation of the aqueous phase from the third
cell. However,
because the aqueous phase in the third cell is free of surfactant, greater
amounts of the
surfactant should be added to the third agitation chamber to achieve an
effective
concentration.
Testing of the inventive process on a bench scale prototype apparatus was
performed on a variety of samples to determine the oil content remaining on
the sand.
Dichloromethane (DCM) extractions were performed on dried samples of sand
produced by
each wash cycle and the results are shown in the following table:
-17-

219G~22
TABLE 2
DCM EXTRACTION OF COMPARTMENT CONTENTS
Sample No. W1% Oil in Wt% Oil in Wt% of OriginalWt% of Original
Feed Extracted Oil ExtractedOil in Sand
Sand Sand
54.4(R1-C1) 1.89 0.202 89.31 10.69
54.4(R1-C2) 1.89 0.137 92.75 7.25
54.4(Rl-C3) 1.89 0.133 92,96 7.04
54.4(R1-C4) 1.89 0.036 98.10 1.9
54.4(R2-CI) 1.89 0.212 88.78 11.22
54.4(R2-C2) 1.89 0.157 91.69 8.31
54.4(R2-C2) 1.89 0.135 92.86 7.14
54.4(R2-C4) 1.89 0.018 99.05 0.95
54.9(Rl-C2) 11.22 0.201 98.21 1.79
54.9(Rl-C3) 11.22 0.150 98.66 1.34
54.9(Rl-C4) 11.22 0.106 99.06 0.94
Note: Cl, C2, C3, C4 denote compartment numbers
R1 denotes the first run and R2 denotes the second ran.
As may be seen sample, 54.4 was subjected to two runs: Rl and R2. In Rl, the
sample
began at 1.89% oil (w:w). The first wash cycle reduced oil content to 0.202%.
Further wash
cycles reduced oil content to 0.036%. In R2, a reduction to 0.018% was
achieved. Sample
54.9 began at 11.22% oil, which was reduced to 0.106% after four wash cycles.
Another sample (54.11) began with 7.79% oil and was reduced to 1.29% oiI
after four wash cycles. This was an unacceptable result and was found to have
resulted from
-18-

219522
a high level of polar compounds which were resistant to the surfactant action
of XT-85'~"I. In
such a case, it is likely necessary to vary the surfactant to deal with the
chemical composition
and nature of the feedstock.
In the first, second and third settling tanks, very fine solids, less than 5
microns
in diameter such as clay and shale, settle out and must be periodically
removed from the
bottom of the tank. A convenient method of removal is use of a "stinging" and
vacuum
process, which is well known in the art.
The test data was obtained using a process which did not feature the recycling
and recirculation of the aqueous phase, however, the concentrations of the
surfactant and the
demulsifier were such that similar results should be achieved in both
instances.
Those skilled in the art will readily appreciate that modifications can be
made
in the arrangement of the present invention while remaining within the scope
of the present
invention.
-19-

Representative Drawing
A single figure which represents the drawing illustrating the invention.
Administrative Status

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Event History

Description Date
Time Limit for Reversal Expired 2016-02-01
Letter Sent 2015-02-02
Inactive: Office letter 2014-10-01
Inactive: Adhoc Request Documented 2014-10-01
Appointment of Agent Request 2014-09-25
Revocation of Agent Request 2014-09-25
Inactive: Office letter 2014-03-21
Inactive: Adhoc Request Documented 2014-03-21
Revocation of Agent Request 2014-03-05
Appointment of Agent Request 2014-03-05
Inactive: Late MF processed 2009-02-23
Letter Sent 2009-02-02
Letter Sent 2008-03-14
Letter Sent 2008-03-14
Inactive: Single transfer 2008-02-11
Letter Sent 2007-04-16
Inactive: Office letter 2007-03-07
Inactive: IPC from MCD 2006-03-12
Inactive: IPC from MCD 2006-03-12
Grant by Issuance 2004-06-29
Inactive: Cover page published 2004-06-28
Letter Sent 2004-04-27
Final Fee Paid and Application Reinstated 2004-04-01
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 2004-02-02
Inactive: Final fee received 2004-01-05
Pre-grant 2004-01-05
Inactive: Office letter 2003-12-30
Notice of Allowance is Issued 2003-12-23
Letter Sent 2003-12-23
Notice of Allowance is Issued 2003-12-23
Inactive: Approved for allowance (AFA) 2003-12-10
Amendment Received - Voluntary Amendment 2003-11-10
Appointment of Agent Requirements Determined Compliant 2003-11-07
Revocation of Agent Requirements Determined Compliant 2003-11-07
Inactive: Office letter 2003-11-07
Inactive: Office letter 2003-11-07
Amendment Received - Voluntary Amendment 2003-11-03
Amendment Received - Voluntary Amendment 2003-11-03
Revocation of Agent Request 2003-11-03
Appointment of Agent Request 2003-11-03
Inactive: S.30(2) Rules - Examiner requisition 2003-07-31
Inactive: Adhoc Request Documented 2002-11-04
Inactive: Office letter 2001-03-27
Letter Sent 2001-03-23
Inactive: Delete abandonment 2001-03-20
Inactive: Delete abandonment 2001-03-20
Letter Sent 2001-03-05
Request for Examination Requirements Determined Compliant 2001-02-05
All Requirements for Examination Determined Compliant 2001-02-05
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 2001-01-31
Letter Sent 2000-03-30
Inactive: Adhoc Request Documented 2000-03-24
Inactive: Reversal of dead status 2000-03-24
Inactive: Office letter 1999-11-08
Inactive: Office letter 1999-11-08
Revocation of Agent Requirements Determined Compliant 1999-11-08
Appointment of Agent Requirements Determined Compliant 1999-11-08
Appointment of Agent Request 1999-10-25
Revocation of Agent Request 1999-10-25
Inactive: Cover page published 1999-10-01
Reinstatement Request Received 1999-08-12
Inactive: Correspondence - Formalities 1999-08-12
Inactive: Compliance - Formalities: Resp. Rec'd 1999-08-12
Reinstatement Requirements Deemed Compliant for All Abandonment Reasons 1999-08-12
Inactive: Dead - Application incomplete 1999-08-12
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 1999-02-01
Deemed Abandoned - Failure to Respond to Notice Requiring a Translation 1998-08-12
Application Published (Open to Public Inspection) 1998-08-01
Inactive: Application prosecuted on TS as of Log entry date 1998-07-14
Inactive: Status info is complete as of Log entry date 1998-07-14
Inactive: Incomplete 1998-05-12
Small Entity Declaration Determined Compliant 1997-01-31

Abandonment History

Abandonment Date Reason Reinstatement Date
2004-02-02
2001-01-31
1999-08-12
1999-02-01
1998-08-12

Maintenance Fee

The last payment was received on 2004-04-01

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  • the reinstatement fee;
  • the late payment fee; or
  • additional fee to reverse deemed expiry.

Please refer to the CIPO Patent Fees web page to see all current fee amounts.

Fee History

Fee Type Anniversary Year Due Date Paid Date
MF (application, 2nd anniv.) - small 02 1999-02-01 1997-01-31
MF (application, 3rd anniv.) - small 03 2000-01-31 1997-01-31
MF (application, 4th anniv.) - small 04 2001-01-31 1997-01-31
MF (application, 5th anniv.) - small 05 2002-01-31 1997-01-31
1999-08-12
1999-08-12
MF (application, 6th anniv.) - small 06 2003-01-31 2001-02-05
Request for examination - small 2001-02-05
Final fee - small 2004-01-05
MF (application, 8th anniv.) - small 08 2005-01-31 2004-04-01
MF (application, 9th anniv.) - small 09 2006-01-31 2004-04-01
Reinstatement 2004-04-01
MF (application, 7th anniv.) - small 07 2004-02-02 2004-04-01
MF (patent, 10th anniv.) - small 2007-01-31 2007-01-26
MF (patent, 11th anniv.) - small 2008-01-31 2008-01-31
Registration of a document 2008-02-11
MF (patent, 12th anniv.) - small 2009-02-02 2009-02-23
Reversal of deemed expiry 2009-02-02 2009-02-23
MF (patent, 13th anniv.) - small 2010-02-01 2009-12-18
MF (patent, 14th anniv.) - small 2011-01-31 2010-12-13
MF (patent, 15th anniv.) - small 2012-01-31 2011-12-28
MF (patent, 16th anniv.) - small 2013-01-31 2012-09-19
MF (patent, 17th anniv.) - small 2014-01-31 2014-01-24
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
1303365 ALBERTA LTD.
Past Owners on Record
LARRY SAIK
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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