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Copyright 2007, AADE
This paper was prepared for presentation at the 2007 AADE National Technical Conference and Exhibition held at the Wyndam Greenspoint Hotel, Houston, Texas, April 10-12, 2007. This conference
was sponsored by the American Association of Drilling Engineers. The information presented in this paper does not reflect any position, claim or endorsement made or implied by the American
Association of Drilling Engineers, their officers or members. Questions concerning the content of this paper should be directed to the individuals listed as author(s) of this work.
Abstract
Efficient filter cake and formation clean-up is required for
production and water-injection wells drilled with synthetic/oil-
based mud (S/OBM). Most invert emulsion skin damage
removal or filter cake clean-up methods require multiple soak
treatments. Typically the first treatment is designed to break
the invert emulsion and water wet the filter cake residue. The
second step is generally designed to remove soluble particles
with acid and/or barium sulfate dissolvers. In many cases,
these steps are repeated to improve performance.
A microemulsion technology was developed for removal
of filter cake deposition, reversal of wettability and removal of
wellbore skin damage in oil wells drilled with S/OBM. These
microemulsion fluids, combined with conventional acids,
allow a single-stage S/OBM clean-up process. The
development work included formulating fluid designs,
controlling the destruction rate of the filter cake with additives
that prevent massive completion fluid losses and return water-
injection permeability.
The results of laboratory tests and field trials using the
single-stage method prove that, when using this technology to
clean-up the filter cake or skin damage by S/OBM, (1) the
invert emulsion is incorporated into the microemulsion, (2) the
solids become water-wet, and (3) the majority of acid-soluble
particles are removed. In conclusion, this technology
maximizes skin damage removal and increases hydrocarbon
recovery and water-injection rates.
Introduction
Many operators are interested in improving filter cake
clean-up after drilling into reservoirs with invert emulsion
drilling fluids. More efficient filter cake clean-up is desired
for a number of open hole completions, including stand-alone
and expandable sand screens, as well as for gravel pack
applications in both production and water injection wells.
S/OBM filter cake clean-up technology uses a single-
phase microemulsion (SPME) to incorporate the oil into the
SPME by a solubilization process1-3
(Figure 1)
In addition, the single-phase microemulsion and
conventional acid packages are used in a single blend to
solubilize the oil into the SPME, reverse the wettability of the
filter cake solids, and simultaneously decompose its acid-
soluble components. Reversing the wettability of the filter
cake, using surface active chemistry, facilitates acidizing by
preventing a sludge that could form between the acid and the
emulsified cake and by making acid-soluble particle surfaces
available to unspent acid.
In addition to the advantage of reduced skin damage,
increased hydrocarbon recovery or increased water injection
rates, a single-stage near-wellbore clean-up method will save
an operator valuable rig time.
Fundamental Theory
In the 1950s, Schulman and co-workers added alcohol to
surfactant-stabilized oil-in-water (o/w) emulsions to obtain
very stable homogeneous fluids that he called
microemulsions.4
These microemulsions had an average
droplet size of 10-100 nanometers (nm), much smaller than
conventional emulsions.
The first studies of microemulsions in the oil industry were
in the 1970’s for enhanced oil recovery (EOR) applications.5-11
Many oil operators and universities invested considerable time
to researching this topic. The research group led by Schechter
and Wade at The University of Texas at Austin made
important contributions to the understanding of the mechanism
of increased production by microemulsions. However, interest
dropped due to crude oil price decreases and because the
technology was expensive, mainly due to the high
concentrations of surfactants required. Since then, the oil
industry has conducted only a small amount of research on
microemulsions.
In the past 25 years, surfactant manufacturers, universities
and research institutes have greatly increased the knowledge
of microstructures and the phase behavior of microemulsions,
and have made surfactants available that are more efficient for
microemulsion formulations.12-18
A microemulsion is a thermodynamically-stable complex
fluid system typically composed of a non-polar oil phase, a
polar water phase, surfactant and an optional co-surfactant.
They are macroscopically homogeneous and, at the
microscopic level, heterogeneous, consisting of individual
domains of the non-polar oil phase and polar water phase,
separated by a monolayer of surfactant (amphiphile).1, 2, 14, 15
Microemulsions are typically clear solutions, because the
droplet diameter of the organized phase is approximately 100
nm or less, and contain two immiscible fluids, in contrast to
micellar solutions, which are considered to be one-phase fluids
and may be either water or oil.
The surfactant molecules in these microemulsion systems
lower the interfacial free energy to nearly zero, which induces
AADE-07-NTCE-18
Single-phase Microemulsion Technology for Cleaning Oil or Synthetic-Based Mud
Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian, Baker Hughes Drilling Fluids
2 Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian AADE-07-NTCE-18
spontaneous microemulsification when the components are
brought together. These fluids may be classified into three
categories according to Winsor definitions.16
Winsor I
microemulsions consist of oil-swollen micelles in a water
phase in equilibrium with excess oil. A Winsor II
microemulsion consists of water-swollen reverse micelles in
an oil phase in equilibrium with excess water. A Winsor III
microemulsion is a middle-phase microemulsion, with excess
water and oil. The Winsor III microemulsion systems can be
understood as an accumulation of swollen micelles, so
numerous that they touch one another, forming a perfectly
bicontinous structure.17, 18
Figure 2 shows a photograph with
Winsor I, Winsor III and Winsor II microemulsion.
A single-phase microemulsion (Winsor IV) is obtained by
increasing the surfactant concentration of a Winsor III
microemulsion fluid. 1, 2, 19
Experimental Procedures
Single-phase microemulsions were formulated with
surfactants, co-surfactants, brine and oil, and then were used
as a soak solution to remove oil-based drilling fluid filter cake.
The brines tested were calcium chloride, sodium chloride,
sodium bromide, and potassium formate. The soak solutions
were formulated in an acidic media, which was designed to
dissolve the bridging particles in the filter cake.
The clean-up tests were performed using filter cakes
obtained from oil-based drilling fluids formulated either with
barite, calcium carbonate, or barite/calcium carbonate blends.
Fluid formulations with various base oils with densities
between 9 and 11 lb/gal were formulated to evaluate the filter
cake clean-up efficiency.
The concentration of SPME in the brine was selected by a
series of screening bottle tests in which the criteria was to
incorporate all of the oil from oil-based drilling fluids into the
soak solution and change the wettability of the solids from oil-
wet to water-wet. In these tests, a certain volume of OBM is
placed in a glass bottle, and then the SPME in brine (soak
solution) is carefully added on top of the OBM. These bottles
are placed in an oven at a specified temperature to observe oil
solubilization into the SPME and wettability changes of the
solids with time.
Filtration tests were performed in a double-ended HPHT
filtration cell to evaluate the efficiency of the soak solution to
remove the filter cake. The procedure included a mud-off at
500 or 1000 psi to deposit a filter cake. Then, the excess mud
was removed and the SPME soak solution was added. Tests
were performed with the leak-off valve opened to simulate the
case for filter cake clean-up in new wells or with the leak-off
valve closed, which is the case in remediation wells.
A Sandpack Permeameter was used to evaluate the
efficiency of the OBM filter cake removal and water-injection.
A schematic diagram of the Sandpack Permeameter is shown
in Figure 3. The Sandpack Permeameter tests were run using
3, 10 or 20-micron discs, 140/270 simulated formation sand,
and 40/60 gravel.
The filter cake clean-up evaluation was based on water-
injection permeability. Injection tests were chosen instead of
production permeability tests because injection is considered a
“worst case” scenario from the viewpoint of return
permeability. The test procedure begins with the measurement
of the initial seawater injection permeability. Next, a filter
cake is deposited on a ceramic disc or Berea sandstone,
followed by treatment with the soak solution for a specified
period of time. The mud-off time for deposition of the filter
cake ranged from 3 to 16 hours. The soak time for the tests is
in the range from 3 to 20 hours. The last step of the procedure
is the water-injection measurement to determine the final
injection permeability.
Results and Discussion
Screening tests of filter cake clean-up with SPME
The first part of the filter cake clean-up study included a
series of screening bottle tests with the SPME in brine. Figure
4 shows photographs of clean-up evaluations of a 10 lb/gal
OBM using a 20% SPME in CaCl2 brine. A 1/10 proportion of
OBM/soak solution was used in these tests. In Figure 4, the
photograph on the left side was taken after initial contact of
the OBM with the soak solution. The photograph on the right
side of Figure 4 was taken after 3 hours of phase contact. The
results indicate that after contact of the soak solution and the
OBM: (1) the soak solution destabilizes the invert emulsion,
(2) the oil from the OBM is incorporated into the
microemulsion and (3) the solid particles became water-wet.
Figure 5 shows the photographs of bottle tests using a
combination of SPME with formic acid in CaCl2 brine. This
SPME/acid blend demonstrates that this combination is
capable of rapid oil-based filter cake clean-up (incorporation
of oil into the soak solution), and calcium carbonate removal.
OBM filter cake evaluation with HPHT filtration cell
Figure 6 shows the filtration rate obtained when the SPME
soak solutions were placed on the top the filter cake in the
HPHT filtration cell. The filter cakes deposited in these tests
were formed with a 10 lb/gal OBM at 1,000 psi at 150°F for 3-
hours. Even if the three SPME/brines blends achieved good
filter cake clean-up, the filtration rates obtained indicates that,
for this particular SPME, the time required to destroy the filter
cake is similar for the NaBr and CaCl2 brine-based systems,
but a longer time is required for the SPME in potassium
formate brine. This is not surprising because the behavior of
microemulsions change with changes in the types of ions and
cations in the soak solution.
The mud cake appearance after mud-off and after
treatment with the single phase microemulsion is shown in
Figures 7a and 7b. Upon removal of the filter cakes and discs
from the cell, it was observed that the filter cakes were water-
wet, as evidenced by the easy dispersion of the cake particles
in water (Figure 8). When the filter cake samples were
dispersed in water, no sheen was observed, indicating that all
of the oil was incorporated into the SPME soak solution
AADE-07-NTCE-18 Single-Phase Microemulsion Technology for Cleaning Oil or Synthetic-Based Mud 3
Injection permeability tests in the Sandpack
Permeameter
OBM filter cake clean-up and water injection was
evaluated in the Sandpack Permeameter. The first part of the
filter cake clean-up and water-injection included a series of
screening tests with the single phase microemulsion in brine
without acid in the formulation. A cake deposition time of
three-hours at 150°F and 1,000 psi was used to obtain a filter
cake with a reasonable thickness to “break” in order to verify
the cleaning efficacy.
Table 1 shows injection permeability data after tests were
performed on 20 µm ceramic discs. The soak solution,
containing 20% microemulsion mixed with a 10 lb/gal brine,
was allowed to soak at 150°F and 360 psi for up to 20 hours.
Even if the filter cake remained in place, because it cannot be
displaced due to equipment limitations, the filter cake after
treatment was very porous and loosely consolidated. As a
result, it was possible to obtain a high percentage of water
injection. The remaining filter cake residue in these tests were
water-wet
The second part of the filter cake clean-up study was the
evaluation of the single-stage soak formulation, an SPME in
conjunction with an acid package in brine. A number of
laboratory tests were performed using SPME together with
various types of acid treatments on OBM filter cakes.
Table 2 shows the injection permeability results after 3-hr
mud-offs and 3-hr or 20-hour soak times using 10 lb/gal OBM
and soak solutions formulated with 20% SPME and 10% acid
in CaCl2 brine. The injection return permeability was only
69.3% in the case of 3-hour soak time, because this was not
enough time to completely dissolve the calcium carbonate
particles. The reduced size of CaCO3 caused blockage of the
pores. This was proven when the test was repeated with a
longer soak time (20 hours), which resulted in an injection
return permeability of 177.8%. After the test, photos of the
ceramic disc with the filter cake show that the acid-soluble
particles were removed and only a small amount of barite is
observed (Figure 9)
Table 2 also shows the results of a test performed with an
in-situ acetic acid generator, which exhibited a rate of 96.7%
of the original water-injection return permeability.
Conclusions
1. The injection permeability test results prove that the
SPME clean-up technique removes OBM and OBM filter
cakes and water-wets the solid particles
2. The OBM filter cakes treated with the single-phase
microemulsion resulted in a loose, porous filter cake that
exhibited high injection permeability.
3. OBM filter cake clean-up was efficiently achieved using
SPME and acid blends in brine.
4. The single-phase microemulsion, with an acid in brine,
incorporates the oil phase of an OBM filter cake into the
aqueous soak solution and acidizes the calcium carbonate
in one step.
5. Because invert emulsion systems are the drill-in fluids of
choice to drill pressure depleted reservoirs in many global
operations, the SPME technology presented in this paper
appears to be an excellent approach to remove near
wellbore damage and prepare the reservoir for water-
injection.
References
1. Ezrahi, S., Aserin A., and Garti N.; “Aggregation Behaviour in
One-Phase (Winsor IV) Microemulsion Systems”, in Handbook
of Microemulsion Science and Technology, ed by P. Kumar and
K.L. Mittal, Marcel Dekker, Inc, New York (1999) 185.
2. Salager, J.L and Anton R.; “Ionic Microemulsions”, in Handbook
of Microemulsion Science and Technology, ed by P. Kumar and
K. L. Mittal, Marcel Dekker, Inc, New York (1999) 247.
3. Oldfield, C.; “A Method for the extraction of oil by
microemulsion”, UK 2347682, assigned to Murgitroyd &
Company on September 13, 2000.
4. Hoar T. P. and Schulman J.H., Nature (London), 152, (1943) 102.
5. Bourrel, M., Chambu, C., Schechter, R.S., and Wade, W.H., “The
Topology of Phase Boundaries for Oil/Brine/Surfactant Systems
and Its Relationship to Oil Recovery”, Soc. Pet. Eng. J., 22
(1981) 28.
6. Salager, J.L., Morgan, J., Schechter, R.S., Wade, W.H., and
Vasquez, E., “Optimum Formulations of Surfactant/Oil/Water
Systems for Minimum Tension and Phase Behavior”, Soc.
Petrol. Eng. J., 19, (1979) 107.
7. Biais, J., Bothorel, P., Clin, B., and Lalanne, P., “Theoretical
Behavior of Microemulsions: Geometrical Aspects, Dilution
Properties and the Role of Alcohol”, J. Dispersion Sci and
Technol., 2, 1 (1981) 67.
8. Scriven L.E., “Equilibrium Bicontinuous Structure”, Nature, 263,
(1976) 123.
9. Graciaa, A., Lachaise, J., Sayous, J.G., Grenier, P., Yiv, S.,
Schecter, R.S., and Wade, W.H., “The Partitioning of Complex
Surfactant Mixture between Oil/Water/Microemulsion Phases at
High Surfactant Concentrations”, J. Colloid Interfase Sci., 93, 2,
(1983) 474.
10.Reed, R.L., and Healy, R.N., “Physicochemical Aspects of
Microemulsion Flodding: A Review”, in Improved Oil Recovery
by Surfactant and Polymer Flooding, ed. by D.O. Shah and R.S.
Schechter, Academic Press, New York (1977) 383.
11.Neogi, P., “Oil Recovery and Microemulsions” in Microemulsion:
Structure and Dynamics, ed. by S.E. Friberg and P. Bothorel,
CRC Press, Inc., Boca Raton, Florida (1987) 197.
12.Prince, L.M., “Microemulsions” in Emulsions and Emulsions
Technology, Part I, Surfactant Science Series, ed by K.J.
Lissant, Marcel Dekker, Inc, New York (1974) 125.
13.Auvray, L., Cotton, J.P., Ober, R., and Taupin, C., “Evidence for
Zero Mean Curvature Microemulsions”, J. Physical Chemistry,
88, (1984) 4584.
14.Bohlen, D.S., Vinson, P.K., Davis H.T., Scriven, L.E., Xie, M.,
Zhu, X., and Miller, G.W., “Generic Patterns in the
Microstructure of Midrange Microemulsions”, in Organized
Solutions, Surfactant Science Series, ed by S. E. Friberg and B.
Lindman, Marcel Dekker, Inc, New York, (1992) 145.
15.Zana, R., and Lang, J., “Dynamics of Microemulsions” in
Microemulsion: Structure and Dynamics, ed. by S.E. Friberg
and P. Bothorel, CRC Press, Inc., Boca Raton, Florida (1987)
153.
16.Holmberg, K., “Quarter Century of Progress and New Horizons in
Microemulsions” in Micelles, Microemulsion, and Monolayers,
Science and Technology, ed. by D.O. Shah, Marcel Dekker, Inc,
4 Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian AADE-07-NTCE-18
New York, (1998) 161.
17.Scriven S., Equilibrium Bicontinous Structure, Nature, 263, 123-
124 (1976).
18.Clausse M., Peyrelasse J., Heil J., Boned C., Lagourette B.,
Bicontinous Structures in Microemulsions, Nature, 293, 636-638
(1981).
19.Winsor, P.A., “Solvent Properties of Amphiphilic Compounds”,
Butterworth, London, 1954.
Acknowledgment
The authors thank Baker Hughes Drilling Fluids for
allowing us to publish this paper. Special thanks are in order
to the Alex McKellar, and Tim Edwards who generated data
supporting development of this technology.
SI Metric Conversion factors
psi x 6.894 757 E +03 = pa
mL x 1.0* E -06 = m3
mD x 9.869 233 E -16 = m2
µm x 1.0* E -06 = m
lb/gal x 1.198 264 E +02 = kg/m3
°F (°F-32)/1.8 = °C
in. x 2.54* E +00 = m
* Conversion factor is exact.
Tables
Table 1 Water injection permeability using SPME for
clean-up OBM filter cake
Permeability
Soak density,
lb/gal/ brine Initial,
mD
Final,
mD
%
Injection
10/ CaCl2 217.3 183.3 84
9.3/ NaCl 280.7 253.8 90.4
Table 2 Water injection permeability using SPME with
acid as clean-up soak
Permeability
Soak time, hr/
type of acid Initial,
mD
Final,
mD
%
Injection
3
(formic acid)
440077 228822..11 6699..33
20
(formic acid)
201.4 358 177.8
20
(acid generator)
684 661.5 96.7
Figures
Figure 1 Mechanism of filter cake wellbore clean-up
Figure 2 Microemulsion systems according to Winsor
definition
AADE-07-NTCE-18 Single-Phase Microemulsion Technology for Cleaning Oil or Synthetic-Based Mud 5
Figure 3 Sandpack Permeameter
Figure 4 OBM/SPME soak solution contact phase tests
Figure 5 OBM/SPME with acid soak solution contact
phase tests
0
20
40
60
80
100
0 20 40 60 80 100 120 140 160
Time (minutes)
FiltrateVolume(mL)
SPME in CaCl2 brine
SPME in NaBr brine
SPME in HCOOK brine
Figure 6 Filtration rate of SPME soak placed on top of
OBM filter cake
Figure 7 OBM filter cake clean-up with SPME in CaCl2
brine
Figure 8 Filter cake placed in water after the treatment
6 Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian AADE-07-NTCE-18
Figure 9 OBM filter cake after treatment with SPME +
formic acid

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Single-stage clean-up of S/OBM filter cake

  • 1. Copyright 2007, AADE This paper was prepared for presentation at the 2007 AADE National Technical Conference and Exhibition held at the Wyndam Greenspoint Hotel, Houston, Texas, April 10-12, 2007. This conference was sponsored by the American Association of Drilling Engineers. The information presented in this paper does not reflect any position, claim or endorsement made or implied by the American Association of Drilling Engineers, their officers or members. Questions concerning the content of this paper should be directed to the individuals listed as author(s) of this work. Abstract Efficient filter cake and formation clean-up is required for production and water-injection wells drilled with synthetic/oil- based mud (S/OBM). Most invert emulsion skin damage removal or filter cake clean-up methods require multiple soak treatments. Typically the first treatment is designed to break the invert emulsion and water wet the filter cake residue. The second step is generally designed to remove soluble particles with acid and/or barium sulfate dissolvers. In many cases, these steps are repeated to improve performance. A microemulsion technology was developed for removal of filter cake deposition, reversal of wettability and removal of wellbore skin damage in oil wells drilled with S/OBM. These microemulsion fluids, combined with conventional acids, allow a single-stage S/OBM clean-up process. The development work included formulating fluid designs, controlling the destruction rate of the filter cake with additives that prevent massive completion fluid losses and return water- injection permeability. The results of laboratory tests and field trials using the single-stage method prove that, when using this technology to clean-up the filter cake or skin damage by S/OBM, (1) the invert emulsion is incorporated into the microemulsion, (2) the solids become water-wet, and (3) the majority of acid-soluble particles are removed. In conclusion, this technology maximizes skin damage removal and increases hydrocarbon recovery and water-injection rates. Introduction Many operators are interested in improving filter cake clean-up after drilling into reservoirs with invert emulsion drilling fluids. More efficient filter cake clean-up is desired for a number of open hole completions, including stand-alone and expandable sand screens, as well as for gravel pack applications in both production and water injection wells. S/OBM filter cake clean-up technology uses a single- phase microemulsion (SPME) to incorporate the oil into the SPME by a solubilization process1-3 (Figure 1) In addition, the single-phase microemulsion and conventional acid packages are used in a single blend to solubilize the oil into the SPME, reverse the wettability of the filter cake solids, and simultaneously decompose its acid- soluble components. Reversing the wettability of the filter cake, using surface active chemistry, facilitates acidizing by preventing a sludge that could form between the acid and the emulsified cake and by making acid-soluble particle surfaces available to unspent acid. In addition to the advantage of reduced skin damage, increased hydrocarbon recovery or increased water injection rates, a single-stage near-wellbore clean-up method will save an operator valuable rig time. Fundamental Theory In the 1950s, Schulman and co-workers added alcohol to surfactant-stabilized oil-in-water (o/w) emulsions to obtain very stable homogeneous fluids that he called microemulsions.4 These microemulsions had an average droplet size of 10-100 nanometers (nm), much smaller than conventional emulsions. The first studies of microemulsions in the oil industry were in the 1970’s for enhanced oil recovery (EOR) applications.5-11 Many oil operators and universities invested considerable time to researching this topic. The research group led by Schechter and Wade at The University of Texas at Austin made important contributions to the understanding of the mechanism of increased production by microemulsions. However, interest dropped due to crude oil price decreases and because the technology was expensive, mainly due to the high concentrations of surfactants required. Since then, the oil industry has conducted only a small amount of research on microemulsions. In the past 25 years, surfactant manufacturers, universities and research institutes have greatly increased the knowledge of microstructures and the phase behavior of microemulsions, and have made surfactants available that are more efficient for microemulsion formulations.12-18 A microemulsion is a thermodynamically-stable complex fluid system typically composed of a non-polar oil phase, a polar water phase, surfactant and an optional co-surfactant. They are macroscopically homogeneous and, at the microscopic level, heterogeneous, consisting of individual domains of the non-polar oil phase and polar water phase, separated by a monolayer of surfactant (amphiphile).1, 2, 14, 15 Microemulsions are typically clear solutions, because the droplet diameter of the organized phase is approximately 100 nm or less, and contain two immiscible fluids, in contrast to micellar solutions, which are considered to be one-phase fluids and may be either water or oil. The surfactant molecules in these microemulsion systems lower the interfacial free energy to nearly zero, which induces AADE-07-NTCE-18 Single-phase Microemulsion Technology for Cleaning Oil or Synthetic-Based Mud Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian, Baker Hughes Drilling Fluids
  • 2. 2 Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian AADE-07-NTCE-18 spontaneous microemulsification when the components are brought together. These fluids may be classified into three categories according to Winsor definitions.16 Winsor I microemulsions consist of oil-swollen micelles in a water phase in equilibrium with excess oil. A Winsor II microemulsion consists of water-swollen reverse micelles in an oil phase in equilibrium with excess water. A Winsor III microemulsion is a middle-phase microemulsion, with excess water and oil. The Winsor III microemulsion systems can be understood as an accumulation of swollen micelles, so numerous that they touch one another, forming a perfectly bicontinous structure.17, 18 Figure 2 shows a photograph with Winsor I, Winsor III and Winsor II microemulsion. A single-phase microemulsion (Winsor IV) is obtained by increasing the surfactant concentration of a Winsor III microemulsion fluid. 1, 2, 19 Experimental Procedures Single-phase microemulsions were formulated with surfactants, co-surfactants, brine and oil, and then were used as a soak solution to remove oil-based drilling fluid filter cake. The brines tested were calcium chloride, sodium chloride, sodium bromide, and potassium formate. The soak solutions were formulated in an acidic media, which was designed to dissolve the bridging particles in the filter cake. The clean-up tests were performed using filter cakes obtained from oil-based drilling fluids formulated either with barite, calcium carbonate, or barite/calcium carbonate blends. Fluid formulations with various base oils with densities between 9 and 11 lb/gal were formulated to evaluate the filter cake clean-up efficiency. The concentration of SPME in the brine was selected by a series of screening bottle tests in which the criteria was to incorporate all of the oil from oil-based drilling fluids into the soak solution and change the wettability of the solids from oil- wet to water-wet. In these tests, a certain volume of OBM is placed in a glass bottle, and then the SPME in brine (soak solution) is carefully added on top of the OBM. These bottles are placed in an oven at a specified temperature to observe oil solubilization into the SPME and wettability changes of the solids with time. Filtration tests were performed in a double-ended HPHT filtration cell to evaluate the efficiency of the soak solution to remove the filter cake. The procedure included a mud-off at 500 or 1000 psi to deposit a filter cake. Then, the excess mud was removed and the SPME soak solution was added. Tests were performed with the leak-off valve opened to simulate the case for filter cake clean-up in new wells or with the leak-off valve closed, which is the case in remediation wells. A Sandpack Permeameter was used to evaluate the efficiency of the OBM filter cake removal and water-injection. A schematic diagram of the Sandpack Permeameter is shown in Figure 3. The Sandpack Permeameter tests were run using 3, 10 or 20-micron discs, 140/270 simulated formation sand, and 40/60 gravel. The filter cake clean-up evaluation was based on water- injection permeability. Injection tests were chosen instead of production permeability tests because injection is considered a “worst case” scenario from the viewpoint of return permeability. The test procedure begins with the measurement of the initial seawater injection permeability. Next, a filter cake is deposited on a ceramic disc or Berea sandstone, followed by treatment with the soak solution for a specified period of time. The mud-off time for deposition of the filter cake ranged from 3 to 16 hours. The soak time for the tests is in the range from 3 to 20 hours. The last step of the procedure is the water-injection measurement to determine the final injection permeability. Results and Discussion Screening tests of filter cake clean-up with SPME The first part of the filter cake clean-up study included a series of screening bottle tests with the SPME in brine. Figure 4 shows photographs of clean-up evaluations of a 10 lb/gal OBM using a 20% SPME in CaCl2 brine. A 1/10 proportion of OBM/soak solution was used in these tests. In Figure 4, the photograph on the left side was taken after initial contact of the OBM with the soak solution. The photograph on the right side of Figure 4 was taken after 3 hours of phase contact. The results indicate that after contact of the soak solution and the OBM: (1) the soak solution destabilizes the invert emulsion, (2) the oil from the OBM is incorporated into the microemulsion and (3) the solid particles became water-wet. Figure 5 shows the photographs of bottle tests using a combination of SPME with formic acid in CaCl2 brine. This SPME/acid blend demonstrates that this combination is capable of rapid oil-based filter cake clean-up (incorporation of oil into the soak solution), and calcium carbonate removal. OBM filter cake evaluation with HPHT filtration cell Figure 6 shows the filtration rate obtained when the SPME soak solutions were placed on the top the filter cake in the HPHT filtration cell. The filter cakes deposited in these tests were formed with a 10 lb/gal OBM at 1,000 psi at 150°F for 3- hours. Even if the three SPME/brines blends achieved good filter cake clean-up, the filtration rates obtained indicates that, for this particular SPME, the time required to destroy the filter cake is similar for the NaBr and CaCl2 brine-based systems, but a longer time is required for the SPME in potassium formate brine. This is not surprising because the behavior of microemulsions change with changes in the types of ions and cations in the soak solution. The mud cake appearance after mud-off and after treatment with the single phase microemulsion is shown in Figures 7a and 7b. Upon removal of the filter cakes and discs from the cell, it was observed that the filter cakes were water- wet, as evidenced by the easy dispersion of the cake particles in water (Figure 8). When the filter cake samples were dispersed in water, no sheen was observed, indicating that all of the oil was incorporated into the SPME soak solution
  • 3. AADE-07-NTCE-18 Single-Phase Microemulsion Technology for Cleaning Oil or Synthetic-Based Mud 3 Injection permeability tests in the Sandpack Permeameter OBM filter cake clean-up and water injection was evaluated in the Sandpack Permeameter. The first part of the filter cake clean-up and water-injection included a series of screening tests with the single phase microemulsion in brine without acid in the formulation. A cake deposition time of three-hours at 150°F and 1,000 psi was used to obtain a filter cake with a reasonable thickness to “break” in order to verify the cleaning efficacy. Table 1 shows injection permeability data after tests were performed on 20 µm ceramic discs. The soak solution, containing 20% microemulsion mixed with a 10 lb/gal brine, was allowed to soak at 150°F and 360 psi for up to 20 hours. Even if the filter cake remained in place, because it cannot be displaced due to equipment limitations, the filter cake after treatment was very porous and loosely consolidated. As a result, it was possible to obtain a high percentage of water injection. The remaining filter cake residue in these tests were water-wet The second part of the filter cake clean-up study was the evaluation of the single-stage soak formulation, an SPME in conjunction with an acid package in brine. A number of laboratory tests were performed using SPME together with various types of acid treatments on OBM filter cakes. Table 2 shows the injection permeability results after 3-hr mud-offs and 3-hr or 20-hour soak times using 10 lb/gal OBM and soak solutions formulated with 20% SPME and 10% acid in CaCl2 brine. The injection return permeability was only 69.3% in the case of 3-hour soak time, because this was not enough time to completely dissolve the calcium carbonate particles. The reduced size of CaCO3 caused blockage of the pores. This was proven when the test was repeated with a longer soak time (20 hours), which resulted in an injection return permeability of 177.8%. After the test, photos of the ceramic disc with the filter cake show that the acid-soluble particles were removed and only a small amount of barite is observed (Figure 9) Table 2 also shows the results of a test performed with an in-situ acetic acid generator, which exhibited a rate of 96.7% of the original water-injection return permeability. Conclusions 1. The injection permeability test results prove that the SPME clean-up technique removes OBM and OBM filter cakes and water-wets the solid particles 2. The OBM filter cakes treated with the single-phase microemulsion resulted in a loose, porous filter cake that exhibited high injection permeability. 3. OBM filter cake clean-up was efficiently achieved using SPME and acid blends in brine. 4. The single-phase microemulsion, with an acid in brine, incorporates the oil phase of an OBM filter cake into the aqueous soak solution and acidizes the calcium carbonate in one step. 5. Because invert emulsion systems are the drill-in fluids of choice to drill pressure depleted reservoirs in many global operations, the SPME technology presented in this paper appears to be an excellent approach to remove near wellbore damage and prepare the reservoir for water- injection. References 1. Ezrahi, S., Aserin A., and Garti N.; “Aggregation Behaviour in One-Phase (Winsor IV) Microemulsion Systems”, in Handbook of Microemulsion Science and Technology, ed by P. Kumar and K.L. Mittal, Marcel Dekker, Inc, New York (1999) 185. 2. Salager, J.L and Anton R.; “Ionic Microemulsions”, in Handbook of Microemulsion Science and Technology, ed by P. Kumar and K. L. Mittal, Marcel Dekker, Inc, New York (1999) 247. 3. Oldfield, C.; “A Method for the extraction of oil by microemulsion”, UK 2347682, assigned to Murgitroyd & Company on September 13, 2000. 4. Hoar T. P. and Schulman J.H., Nature (London), 152, (1943) 102. 5. Bourrel, M., Chambu, C., Schechter, R.S., and Wade, W.H., “The Topology of Phase Boundaries for Oil/Brine/Surfactant Systems and Its Relationship to Oil Recovery”, Soc. Pet. Eng. J., 22 (1981) 28. 6. Salager, J.L., Morgan, J., Schechter, R.S., Wade, W.H., and Vasquez, E., “Optimum Formulations of Surfactant/Oil/Water Systems for Minimum Tension and Phase Behavior”, Soc. Petrol. Eng. J., 19, (1979) 107. 7. Biais, J., Bothorel, P., Clin, B., and Lalanne, P., “Theoretical Behavior of Microemulsions: Geometrical Aspects, Dilution Properties and the Role of Alcohol”, J. Dispersion Sci and Technol., 2, 1 (1981) 67. 8. Scriven L.E., “Equilibrium Bicontinuous Structure”, Nature, 263, (1976) 123. 9. Graciaa, A., Lachaise, J., Sayous, J.G., Grenier, P., Yiv, S., Schecter, R.S., and Wade, W.H., “The Partitioning of Complex Surfactant Mixture between Oil/Water/Microemulsion Phases at High Surfactant Concentrations”, J. Colloid Interfase Sci., 93, 2, (1983) 474. 10.Reed, R.L., and Healy, R.N., “Physicochemical Aspects of Microemulsion Flodding: A Review”, in Improved Oil Recovery by Surfactant and Polymer Flooding, ed. by D.O. Shah and R.S. Schechter, Academic Press, New York (1977) 383. 11.Neogi, P., “Oil Recovery and Microemulsions” in Microemulsion: Structure and Dynamics, ed. by S.E. Friberg and P. Bothorel, CRC Press, Inc., Boca Raton, Florida (1987) 197. 12.Prince, L.M., “Microemulsions” in Emulsions and Emulsions Technology, Part I, Surfactant Science Series, ed by K.J. Lissant, Marcel Dekker, Inc, New York (1974) 125. 13.Auvray, L., Cotton, J.P., Ober, R., and Taupin, C., “Evidence for Zero Mean Curvature Microemulsions”, J. Physical Chemistry, 88, (1984) 4584. 14.Bohlen, D.S., Vinson, P.K., Davis H.T., Scriven, L.E., Xie, M., Zhu, X., and Miller, G.W., “Generic Patterns in the Microstructure of Midrange Microemulsions”, in Organized Solutions, Surfactant Science Series, ed by S. E. Friberg and B. Lindman, Marcel Dekker, Inc, New York, (1992) 145. 15.Zana, R., and Lang, J., “Dynamics of Microemulsions” in Microemulsion: Structure and Dynamics, ed. by S.E. Friberg and P. Bothorel, CRC Press, Inc., Boca Raton, Florida (1987) 153. 16.Holmberg, K., “Quarter Century of Progress and New Horizons in Microemulsions” in Micelles, Microemulsion, and Monolayers, Science and Technology, ed. by D.O. Shah, Marcel Dekker, Inc,
  • 4. 4 Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian AADE-07-NTCE-18 New York, (1998) 161. 17.Scriven S., Equilibrium Bicontinous Structure, Nature, 263, 123- 124 (1976). 18.Clausse M., Peyrelasse J., Heil J., Boned C., Lagourette B., Bicontinous Structures in Microemulsions, Nature, 293, 636-638 (1981). 19.Winsor, P.A., “Solvent Properties of Amphiphilic Compounds”, Butterworth, London, 1954. Acknowledgment The authors thank Baker Hughes Drilling Fluids for allowing us to publish this paper. Special thanks are in order to the Alex McKellar, and Tim Edwards who generated data supporting development of this technology. SI Metric Conversion factors psi x 6.894 757 E +03 = pa mL x 1.0* E -06 = m3 mD x 9.869 233 E -16 = m2 µm x 1.0* E -06 = m lb/gal x 1.198 264 E +02 = kg/m3 °F (°F-32)/1.8 = °C in. x 2.54* E +00 = m * Conversion factor is exact. Tables Table 1 Water injection permeability using SPME for clean-up OBM filter cake Permeability Soak density, lb/gal/ brine Initial, mD Final, mD % Injection 10/ CaCl2 217.3 183.3 84 9.3/ NaCl 280.7 253.8 90.4 Table 2 Water injection permeability using SPME with acid as clean-up soak Permeability Soak time, hr/ type of acid Initial, mD Final, mD % Injection 3 (formic acid) 440077 228822..11 6699..33 20 (formic acid) 201.4 358 177.8 20 (acid generator) 684 661.5 96.7 Figures Figure 1 Mechanism of filter cake wellbore clean-up Figure 2 Microemulsion systems according to Winsor definition
  • 5. AADE-07-NTCE-18 Single-Phase Microemulsion Technology for Cleaning Oil or Synthetic-Based Mud 5 Figure 3 Sandpack Permeameter Figure 4 OBM/SPME soak solution contact phase tests Figure 5 OBM/SPME with acid soak solution contact phase tests 0 20 40 60 80 100 0 20 40 60 80 100 120 140 160 Time (minutes) FiltrateVolume(mL) SPME in CaCl2 brine SPME in NaBr brine SPME in HCOOK brine Figure 6 Filtration rate of SPME soak placed on top of OBM filter cake Figure 7 OBM filter cake clean-up with SPME in CaCl2 brine Figure 8 Filter cake placed in water after the treatment
  • 6. 6 Lirio Quintero, Tom Jones, David E. Clark, Cristina Torres, and Chad Christian AADE-07-NTCE-18 Figure 9 OBM filter cake after treatment with SPME + formic acid