Colloids and Surfaces A 550 (2018) 245–255

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Colloids and Surfaces A

journal homepage: www.elsevier.com/locate/colsurfa

Mobility control in carbon dioxide-enhanced oil recovery process using T

nanoparticle-stabilized foam for carbonate reservoirs
⁎
Omeid Rahmania,b,
a
Department of Petroleum Engineering, Mahabad Branch, Islamic Azad University, Mahabad 59135-433, Iran
b
Department of Natural Resources Engineering and Management, School of Science and Engineering, University of Kurdistan Hewlêr (UKH), Erbil, Kurdistan Region, Iraq

G R A P H I C A L A B S T R A C T

A R T I C LE I N FO A B S T R A C T

Keywords: Recent developments in the subject of using silica-nanoparticles (SiNPs) for stabilizing carbon dioxide (CO2)-
Mobility control foam have led to a renewed interest in the enhanced oil recovery (EOR) in oilfields. This study investigates the
Carbon dioxide mobility control in the process of CO2 EOR through unfractured and fractured limestone cores. Toward this aim,
Nanoparticle laboratory tests were performed by co-injection of CO2 and 12 nm methyl-coated SiNPs solution to generate
Enhanced oil recovery
stable CO2 foam in the cores. In addition, sodium chloride (NaCl) and decane were used to examine the sen-
sitivity of foam generation to salinity and to signify hydrocarbon (HC) phase in the experiments, respectively.
The results revealed that SiNPs were able to generate stabilized CO2 foam in both unfractured and fractured
limestone cores. A critical shear rate was established in the generation of foam with different conditions in the
core-flood experiments. The cores with lower matrix permeability had a lower value of critical shear rate for
foam generation. Moreover, the magnitude of apparent viscosity was found to be a crucial factor for mobility
control and to obtain an optimum quality of foam. The results indicated that increasing NaCl concentration to
3 wt.% causes a decrease in the value of critical shear rate at applied temperatures. Furthermore, the findings
revealed that a real mobility control in CO2 EOR process can only be reached when the generated foam still
interacts with HC in the reservoir.

⁎
Corresponding author at: Department of Petroleum Engineering, Mahabad Branch, Islamic Azad University, Mahabad 59135-433, Iran.
E-mail addresses: omeid.rahmani@iau-Mahabad.ac.ir, omeid.rahmani@ukh.edu.krd.

https://doi.org/10.1016/j.colsurfa.2018.04.050
Received 5 February 2018; Received in revised form 21 April 2018; Accepted 23 April 2018
Available online 25 April 2018
0927-7757/ © 2018 Elsevier B.V. All rights reserved.
O. Rahmani
1. Introduction
In recent years, both field applications and laboratory tests of foam
flooding have shown a well-established mobility control notion in the
enhanced oil recovery (EOR) process with positive prospects and effects
[1], predominantly for the injection of carbon dioxide (CO2) into the
reservoir [2–5]. Further, CO2 flooding has been widely used as an EOR
technique [5–7], CO2 EOR has become even more attractive recently
due to a way of utilizing the CO2 available through advance in CO2
sequestration process, a very substantial fraction of residual oil in re-
servoirs [8], and likely increasing crude oil price in the upcoming years.
Miscible CO2 EOR has grown in importance in which the molecules of
carbon dioxide are able to contact the residual oil in the reservoir. In
the CO2 flooding, the estimated recovery of oil may be reduced due to
poor sweep efficiency [9,10] and the CO2 channeling problem (CCP).
The extent to which CO2 flooding has been successful in light of the
reservoir the estimated recovery of oil is poorly understood. The poor
sweep efficiency is related to a high mobility ratio between CO2 and
water. This challenge is considered as one of the most frequently stated
problems in the reservoirs whenever associated with the presence of
natural fractures. These natural fractures provide high permeability
passages for CO2 in order to bypass oil-bearing zones with low per-
meability. The mobility ratio, which is the ratio between mobility of
displacing fluid (i.e. CO2) and the displaced fluid (i.e. oil), is defined as:
Mobility of displacing fluid (CO2) Kr CO2/ μ CO2
Mobility ratio = =
Mobility of displaced fluid (oil) Kr oil/ μ oil (1)
where kr and μ are the relative matrix permeability (mD) and the
viscosity (cP), respectively. At the reservoir condition, the μ CO2 ranges
from ∼0.05 to 0.1 cP, which is considerably lower than the μ oil . It
leads to mobility ratio higher than 1. Therefore, sweep efficiency can be
improved through reducing the mobility of CO2 and lowering the mo-
bility ratio [9,11]. On the other hand, the CCP stands as an operational
problem in which the amount of CO2 recycling significantly increases
after early CO2 breakthrough. According to Balan et al. [12] and Gau-
glitz et al. [13], the presence of foam in the reservoirs lowers the mo-
bility of CO2 phase by increasing the resistance of gas to flow and mi-
tigating the CCP [14].
Conventional foam, extensively used in the oil industry, is defined
as a dispersion of gas in a continuous liquid phase where thin liquid
films (called lamellae) separate the gas flow paths [10,15]. The foam is
produced and stabilized with surfactants, the amphiphilic molecules
that have an affinity both to CO2 and water [16]. When referring to
high temperature or salinity in the reservoirs, these surfactants lack the
capability to provide enduring foam stability. Recent studies have de-
monstrated the ability of nanoparticles (NPs) in stabilizing CO2 foam
and improving the mobility ratio of CO2 and oil as displacing and dis-
placed fluids, respectively [10,17,18]. Nguyen et al. [4] demonstrated
that NPs adsorb more energy at the interface between liquid and gas
than the surfactants; therefore, they are a more stable agent for foam
formation. Furthermore, this process is most effective when the surface
of NPs is modified to minimize their aggregation [19–21].
So far, there has been little discussion about the behavior of nano-
particle-stabilized (NP-St) CO2 foam in the presence of oil
[16,17,22,23]. While extensive studies have been carried out on the
generation of foam with NPs in unconsolidated porous media [24–27],
no research has been conducted to test the ability of surface-modified
SiNP to stabilize CO2 foam in consolidated rock such as limestone. To
date, Aroonsri et al.’s study is one of the rare investigations that ex-
amined the conditions for forming the NP-St CO2 foam in unfractured
and fractured sandstone cores [16]. However, they do not take account
of the experimental evidence to prove the CO2 foam stability while it
could be determined through a half-life time as a crucial procedure
[4,17]. Additionally, in their study, the core samples were considered
vertically rather than horizontally in which the core-flood experiment
246
Colloids and Surfaces A 550 (2018) 245–255
will be more relevant to a real reservoir that is usually developed
horizontally. Therefore, the main objectives of this study are to in-
vestigate the transmission and stability of SiNP-St CO2 foam in un-
fractured and fractured limestone cores to improve the mobility control
and attain insight into the behavior of foam while the hydrocarbon
(HC) is present in the CO2 EOR process.
2. Materials and methods
2.1. Materials
In order to study the ability of NPs to stabilize CO2 foam, two types
of surface-modified silica nanoparticle (SiNP) coated by poly ethylene
glycol (PEG) and methyl were considered. In comparison, methyl-
coated SiNP has an excessive stability for enduring of mobility control
in CO2 EOR process [4,22]. Therefore, a 12 nm spherical methyl-coated
SiNP received from Wacker Chemicals Korea Inc., with 0%, 50%, and
75% coverage of dichlorodimethylsilane (C2H6SiCl2) in purity of 99.5%
and specific surface area of 129 m2/g, was used in unfractured and
fractured limestone core-flood experiments. The limestone samples
were taken from an oilfield in the Zagros Basin, Iran. To prepare the
NPs solution, they were dispersed in ethanol (C2H6O) to wet their
surface during one day. The solution was then centrifuged to remove
the ethanol [4,22]. Deionized (DI) water was also applied to dilute NPs
dispersion to preferred concentration. Pressurized CO2, with a purity of
99.99% in cylinders equipped with a valve for gas and liquid with-
drawals, was obtained from ATDM Gas. Sodium chloride (NaCl, Thermo
Fisher Scientific) was introduced to the aqueous phase to maintain the
permeability of cores and to examine the sensitivity of foam generation
to salinity. Decane (C10H22), with more than 99% purity from Thermo
Fisher Scientific, was utilized to signify HC phase in oil recovery ex-
periments with CO2 foam [23].
2.2. Experimental apparatus
A schematic of the apparatus used for the generation of foam is
shown in Fig. 1. A core holder, manufactured by Core Lab’s Reservoir
Optimization, was used in the core-flood experiments to handle a 3 cm
diameter core sample, with a length up to 30 cm. The core was sealed
by a silicone rubber sleeve to prevent flow along its outer surface. To
establish a seal around the core and provide a confining pressure, a
hydraulic lightweight hand pump (Enerpac P-141, 327 cm3, 2.4 kg) was
applied. The hydraulic oil was injected into the annulus between the
core holder and the rubber sleeves. The provided confining pressure
could be recorded through the installed pressure gauge. Teledyne ISCO
500D syringe pump, with its 500 ml cylinder capacity at pressures up to
3750 psi, was used to inject brine (with different concentration from 1
to 3 wt.% NaCl) or aqueous dispersion of NPs. A floating piston accu-
mulator (FPA1000-10 1/8" FLP) provided by Nano-lab at IAU-Mahabad
Branch was applied to store the liquid phase of CO2. The fluid flow was
isolated from the driving water and liquid CO2 via the FPA that by
virtue of its design minimizes friction and reduces pressure load. To
keep the decane and assemble the effluent during CO2 EOR process, two
FPA, each with a capacity of 500 ml, were also supplied by the Nano-lab
at IAU-Mahabad Branch. Moreover, an Autoclave Engineers O-ring self-
sealing closure was designed specifically for low pressure and moderate
temperature applications, where O-ring seals are permissible. Further-
more, a CO2 flow-meter regulator (HPT-GAR-398CR Hero) was in-
stalled to the CO2 gas cylinder to control the flow rate of injected CO2
and calculate the net volume (%) of inlet gas. The desired pressure at
the experiments was maintained with the CO2 flow-meter regulator. In
addition, a hose (W.P. 400 bar, 6-SAE 100 at ¼˝) of 6.4 mm diameter
and 2 m length was connected to both the CO2 cylinder and the flow-
meter regulator. A capillary tubing of 1 mm internal diameter and
24 cm length was also utilized to measure the apparent viscosity of
fluids flowing. Finally, an oven embedded to a digital set controller
O. Rahmani Colloids and Surfaces A 550 (2018) 245–255

Fig. 1. A schematic of the set-up used for the generation of foam.

with a Hall sensor feedback (input power supply: 220 V; 50 Hz) was Q .μapp .. L
k=
utilized to provide and control the desired temperatures. Before car- Acore . ΔP (4)
rying out the core-flood experiments, the fluids (i.e. CO2 and water)
were pre-heated in the water bath for 45 min. By carrying out this where Acore, ΔL, and ΔP are the core cross-sectional area to flow (cm2),
function, the set-up inside the oven allows for achieving the desired core length (cm), and pressure drop (Pa.), respectively. μapp stands for
temperatures in the core-flood experiments. apparent viscosity (Pa.s) of aqueous phase.
For the experiment of fractured core-flood, the limestone core was
loaded to crack its frame. Similar to the experiment of unfractured
2.3. Experimental procedure
limestone core-flood, the limestone sample was first cut into a cylind-
rical core 30 cm in length and then wrapped thoroughly with the PTFE
A core-flood experiment was carried out to study the foaming ability
tape to prevent it from breaking down while loaded. Towards this aim,
of SiNP by direct co-injection of CO2 and NP dispersion through the
a regular load frame provided by an axial force was applied to fracture
unfractured and fractured limestone cores. To prepare for the ex-
the core. Based on compressive strength of the limestone core (i.e.
amination of unfractured core-flood, the limestone sample was first cut
85 MPa), the load frame was set to run at a loading rate of 1000 psi/
into a cylindrical core of 3 cm in diameter and 30 cm in length. The core
min. The load frame was then run from the bottom plate to the top one.
sample was then wrapped with a polytetrafluoroethylene (PTFE) tape
After contacting the core with the top plate, the run of load frame was
and heat-shrink tubing (UL224-2010 ASTM D 2671) to prevent flow
continued until the core was failed in its compression. Under tensile
along the core wall and decrease the contact between CO2 and rubber
loading, the limestone core was fractured into two pieces and then
sleeves [16]. Next, the limestone cores were vacuumed twice in order to
removed immediately to avoid more squeezing. The fractured limestone
prove all trapped air is removed. Afterwards, the core samples were
core was next thoroughly wrapped by the shrink tube and PTFE tape,
saturated with NaCl brine as an early stage before carrying out the core-
respectively. The heat shrink tubing prevents the crushing of the core
flood experiments. The samples were then placed in the oven and he-
by providing confining pressure while it is fractured. The two pieces of
ated to the temperature of 200 °C. By the heating of the samples, the
fractured core were put back together with some offset to keep the
shrink wrap tubing was activated [23]. After completing the wrapped
fracture open and, therefore, to extract the fractured core. In doing so,
process, the weight of the wrapped cores were measured. The core
the same process used in the unfractured limestone core was applied to
samples were placed in a sealed chamber and vacuumed for 24 h. In the
prepare the sample for further experiment.
following step, the 3-way valve at the top of the chamber was opened to
In addition, Fig. 2 shows a schematic of fractured core indicating the
introduce the NaCl brine into the vacuumed chamber. After submerging
width (W) and height (H) of fracture along the length (L) of the core.
the limestone core into the NaCl brine, any remaining trapped air that
The fracture in the core-flood experiment was considered as a narrow
in the sample was vacuumed out. The wet weight (Ww) of the saturated
fissure that the W is extremely larger than the H. In view of all that has
cores were also measured and compared with dry weight (Wd) to de-
been mentioned so far, one may suppose that a single phase Newtonian
termine pore volume (PV) and porosity (Φ ) of the cores applying the Eq.
fluid flows through the narrow fissure and, therefore, the fracture
(2) and (3). In addition, the permeability (k) was measured through an
aperture size (H in cm) is calculated from the Eq. (5). The H was cal-
injection of brine to the core sample at different flow rates (Q in cm3/s),
culated in the basis of the matrix permeability (km) and the average
from the low to the high, and calculated using Darcy’s law (Eq. (4)).
permeability of the core (kave.) and used to determine the fracture
Ww−Wd permeability (kfr) [16,28]. By knowing the kfr, a model of parallel flow
PV = permeability (MPFP), adopted from Odling et al. [29], was applied to
Density of saturated brine (2)
determine the fractions of flow in both fracture (Ffr) and matrix (Fm).
PV 1
Φ= H = (12 × kfr ) 2
Acore . L (3) (5)

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O. Rahmani Colloids and Surfaces A 550 (2018) 245–255

2.5. Determination of the quality of CO2 foam (Fg)

Fg, which determines the volume fraction of CO2 in the generation

of foam, is defined as the volumetric ratio of carbon dioxide (VCO2 in
cm3) to the aqueous phase (VL, liquid volume in cm3) at the core-flood
conditions (Eq. (9)). CO2 and DI water were co-injected at the same
volumetric flow rate at core-flood conditions.
VCO2
Fg =
Vw + VCO2 (9)

2.6. Estimation of oil saturation (So)

As pointed out in subsection 2.1, decane was utilized as the re-

presentative of HC phase in the experiment due to its miscibility with
Fig. 2. A 3D schematic of fractured core indicating the width (W) and height CO2. With the aim to estimate the oil saturation residing in the cores,
(H) of fracture alongside the core.
the So was measured through the difference between wet weight of the
limestone core (Wm ) containing the oil (Wso ) and when it was saturated
[km × (Acore −HW )] + (kfr × HW ) with brine (Wsw ). This discrepancy was a result of the difference be-
kave . =
Acore (6) tween the density of decane ( ρd ) and brine ( ρb ) in the aqueous phase.
Wsw = Wm + PV . ρb (10)
kfr × HW
Ffr = Wso = Wm + PV . [ρb . (1−So) + ρd . So] (11)
kave . × Acore (7)
Wsw−Wso = PV . So. (ρb −ρd ) (12)
Furthermore, to evaluate the effect of injected pressure on the
change in fracture aperture, the fractured limestone core was placed Wsw−Wso
So =
under a compression cycle and significantly the provided confining PV . (ρb −ρd ) (13)
pressure did not affect the fracture aperture size.

3. Results and discussion

2.4. Mobility reduction factor (MRF)
MRF is the ratio of the measured ΔP across the core for the foam
experiment with NPs to the aqueous phase that does not contain the
NPs [23]. During co-injection of CO2 and NP dispersion to the both
unfractured and fractured limestone cores, the ΔP depends on (and also
converted to) the μapp of aqueous phase with and without NPs. There-
fore, the MRF is the ratio of the μapp of generated foam (with NPs) to the
μapp of the CO2-water mixture (without NPs) at the same flow rate [16].
μapp . generated foam
MRF =
μapp . aqueous phase without NPs
3.1. Foam generation in unfractured limestone core
To test the ability of NPs for stabilizing CO2 bubbles, CO2 and NP
dispersion were co-injected directly into the unfractured limestone
cores with average petrophysical properties of ∼17.75% porosity and
10–60 mD permeability. To infer the MRF, the ΔP drop measured across
the core was converted into the μapp (see Eq. (4)) and compared with
the aqueous phase without NPs.
Initially, CO2 and DI water at a volumetric ratio of 1:1 were co-
injected into the unfractured limestone core to establish the μapp of
(8) baseline experiment (without NPs). The measured ΔP converted to the
μapp at different PV and Q is shown in Fig. 3. The results of this baseline
experiment show that the μapp first approaches to a certain amount

•
Fig. 3. The plotted measured baseline μapp (81.6 < γ < 980 s−1) vs. injected PV in the unfractured limestone core (without NPs) at an equal ratio (1:1) of CO2 and DI
water and an operating pressure of 1000 psi.

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O. Rahmani Colloids and Surfaces A 550 (2018) 245–255

Table 1 Table 1 (continued)

The experiment of foam generation in unfractured limestone cores with NPs
dispersion from 0.1 to 1 wt.%. Experiment k (mD) Q (ml/ ΔP (psi) μapp (cP) MRF •
γ (s−1)
min)
Experiment k (mD) Q (ml/ ΔP (psi) μapp (cP) MRF •
γ (s−1)
min) CNP-12 60 1 1.15 4.479 2.488 33.333
NPs = 1 wt.% 3 4.96 6.439 3.577 99.998
CNP-1 10 1 0.47 1.830 1.017 81.648 NaCl = 3 wt.% 6 10.44 6.777 3.765 199.997
NPs = 0.1 wt.% 3 1.44 1.869 1.039 244.945 Φ = 17.75% 8 14.29 6.957 3.865 266.662
NaCl = 1 wt.% 6 2.91 1.889 1.049 489.890 10 15.37 5.986 3.326 333.328
Φ = 17.75% 8 3.94 1.918 1.066 653.186 T = 75 °C 12 18.22 5.913 3.285 399.993
T = 25 °C 10 4.97 1.936 1.075 816.483 P = 2000 psi
P = 1000 psi 12 5.98 1.941 1.078 979.779

CNP-2 25 1 0.5 1.947 1.082 51.639

NPs = 0.1 wt.% 3 1.6 2.077 1.154 154.917 (1.45 cP) and then reaches the steady state while the flow rate changes.
NaCl = 3 wt.% 6 3.7 2.402 1.334 309.833 The highest amount of μapp is 1.92 cP at the Q of more than 8 ml/min. It
Φ = 17.75% 8 5.05 2.458 1.366 413.111
can be noted that the amount of μapp in the baseline experiment is es-
T = 25 °C 10 5.94 2.313 1.285 516.389
P = 1000 psi 12 7.09 2.301 1.278 619.667 sentially unaffected by the injection rates and is about 1.8 cP in
average. Eq. (14) [30] was applied to calculate the amount of shear rate
CNP-3 45 1 0.55 2.142 1.190 38.489 •
NPs = 1 wt.% 3 1.91 2.480 1.378 115.468
(γ , measured in s−1) on the fluid flowing through unfractured lime-
NaCl = 1 wt.% 6 3.95 2.564 1.424 230.936 stone cores.
Φ = 17.75% 8 5.46 2.658 1.477 307.915
4Q
T = 25 °C 10 6.44 2.508 1.393 384.894 γ̇ (s−1) = 1
P = 1000 psi 12 7.61 2.470 1.372 461.872 A (8k ∅) 2 (14)
CNP-4 60 1 0.69 2.687 1.493 33.333
In doing so, NPs (with different dispersion from 0.1 to 1 wt.%) were
NPs = 1 wt.% 3 2.13 2.765 1.536 99.998
NaCl = 3 wt.% 6 4.61 2.992 1.662 199.997
dispersed into the NaCl (with different concentration from 1 to 3 wt.%)
Φ = 17.75% 8 6.52 3.174 1.763 266.662 brine to investigate the feasibility of foam generation of high quality in
T = 25 °C 10 7.26 2.827 1.571 333.328 unfractured limestone core (Table 1). According to Worthen et al. [22],
P = 1000 psi 12 8.53 2.768 1.538 399.993 foam stabilization is promoted by increasing the salinity of aqueous
CNP-5 10 1 0.49 1.908 1.060 81.648 phase through increasing the affinity of NPs between the CO2 and
NPs = 0.1 wt.% 3 1.54 1.999 1.111 244.945 aqueous phase. A gradual increase in the MRF between the Q of 3 and
NaCl = 1 wt.% 6 3.11 2.019 1.122 489.890
8 ml/min increases the quality of generated foam. This result can also
Φ = 17.75% 8 4.38 2.132 1.185 653.186
T = 50 °C 10 5.56 2.165 1.203 816.483 be approved through the view cell observation where the small texture
•
P = 1500 psi 12 6.61 2.145 1.19 979.779 of generated foam was detected at the γ of above 100 s−1. With respect
CNP-6 25 1 0.51 1.986 1.103 51.639
to high quality of foam (i.e. 0.8), CO2 bubbles were distributed in larger
NPs = 0.1 wt.% 3 1.8 2.337 1.298 154.917 size. These bubbles are formed by the coalescence of unstable foam.
NaCl = 3 wt.% 6 4.16 2.700 1.500 309.833 Because the unstable foam has lower μapp, it is necessary to increase the
•
Φ = 17.75% 8 6.33 3.082 1.712 413.111 value of γ to improve the texture of foam.
T = 50 °C 10 7.23 2.816 1.564 516.389
Additionally, the measurement of internal pressure taps provides a
P = 1500 psi 12 8.32 2.700 1.500 619.667
perceptive information about the foam generation at different sections
CNP-7 45 1 0.75 2.921 1.623 38.489
of the core. For example, after converting the sectional ΔP drops to the
NPs = 1 wt.% 3 2.54 3.297 1.832 115.468
NaCl = 1 wt.% 6 5.61 3.641 2.023 230.936 μapp, the value of μapp at the top part of the core remains consistent with
Φ = 17.75% 8 8.36 4.070 2.261 307.915 the baseline level, while it increases at the bottom part (e.g. at the Q of
T = 50 °C 10 9.1 3.544 1.969 384.894 3 ml/min). Although the μapp of the baseline experiment is about 1.8 cP
P = 1500 psi 12 10 3.246 1.803 461.872 at the top and bottom parts of the unfractured limestone core at every
CNP-8 60 1 0.9 3.505 1.947 33.333 injection rate, this value is not considered for the generation of foam.
•
NPs = 1 wt.% 3 2.96 3.843 2.135 99.998 Therefore, the low value of γ at the Q of 3 ml/min causes to move the
NaCl = 3 wt.% 6 6.81 4.420 2.456 199.997
Φ = 17.75% 8 9.85 4.795 2.664 266.662
NPs to the interface of the fluids at the top part of the core (see #10 in
T = 50 °C 10 11.21 4.366 2.425 333.328 Fig. 1). As a result, a lower surface of NPs was covered. Accordingly, a
P = 1500 psi 12 13.01 4.222 2.346 399.993 small portion of lamellae remains at the top part of the unfractured
CNP-9 10 1 0.53 2.064 1.147 81.648 limestone core. By following these lamellae, they were accumulated to
NPs = 0.1 wt.% 3 2.1 2.726 1.515 244.945 the central part of the core and more surfaces of NPs were covered. At
NaCl = 1 wt.% 6 5.1 3.310 1.839 489.890 the central part, the μapp became greater than the top part. As a result, it
Φ = 17.75% 8 7.52 3.661 2.034 653.186 can be extended to the bottom part of the core, having the most amount
T = 75 °C 10 9.01 3.509 1.949 816.483
P = 2000 psi 12 10.66 3.460 1.922 979.779
of the μapp among other parts of the core.
The results obtained from the unfractured limestone cores show that
CNP-10 25 1 0.56 2.181 1.212 51.639 •
NPs = 0.1 wt.% 3 2.15 2.791 1.551 154.917
the presence of NPs below than the value of the critical shear rate (γ crit)
NaCl = 3 wt.% 6 6.31 4.096 2.275 309.833 and does not affect the measured ΔP across the core [16]. As shown in
Φ = 17.75% 8 9.16 4.459 2.477 413.111 Fig. 4, the MRF values are about 1 in the unfractured limestone cores
T = 75 °C 10 11.12 4.331 2.406 516.389 with NPs dispersion of 0.1 wt.%, which means that the measured ΔP at
P = 2000 psi 12 13.03 4.229 2.349 619.667
these conditions is the same as that of without NPs. In addition, the
•
CNP-11 45 1 0.9 3.505 1.947 38.489 MRF value increases by increasing the γ across the unfractured lime-
NPs = 1 wt.% 3 4 5.193 2.885 115.468
stone core. Therefore, the increase in the value of MRF cause to increase
NaCl = 1 wt.% 6 8.1 5.258 2.921 230.936
Φ = 17.75% 8 10.95 5.331 2.962 307.915
the μapp of generated foam as the fluids flow across the core.
T = 75 °C 10 13.06 5.086 2.826 384.894 By increasing the Q to the rate of 8 ml/min, the μapp increased
•
P = 2000 psi equally at the whole parts of the core. Because the amount of γ was
NPs = 1 wt.% 12 14.95 4.852 2.696 461.872 sufficient at this rate and caused enough NPs to move to the interface,
the foam was generated in the top part of unfractured limestone core

249
O. Rahmani
Fig. 4. The amount of MRF vs. shear rate for unfractured limestone cores with different dispersion of NPs from 0.1 to 1 wt.% and different concentration of NaCl from
1 to 3 wt.% at temperatures of 25, 50, and 75 °C.
Fig. 5. The measured apparent viscosity at the top, central, and bottom parts (see # 10 in Fig.1) of the unfractured limestone cores with flow rates from 1 to 12 ml/
min.
where the highest rank of lamellae was earlier accumulated. For this
reason, the μapp of foam remained at the same level in the other parts,
while the generated foam was transmitted to the central and bottom
parts of the core. In the higher quality of generated foam (i.e. 0.9), the
amount of μapp significantly differed among the parts of core (Fig. 5).
This result is enhanced when the Q of more than 8 ml/min is applied in
the experiment of foam generation. This result is also significant at the
Q of ≥10 ml/min.
3.2. Foam generation in fractured limestone cores
Similar to the experiment of foam generation in the unfractured
limestone core, the brine containing NPs dispersion with 1 wt.% was
first prepared through injection of CO2 and NaCl (with concentration of
1 wt.%) simultaneously into the fractured core with aperture size (or
fracture height) of 85 μm. Then, the experiments were conducted using
higher concentration of NaCl to 3 wt.% into the cores with aperture size
of 102 and 164 μm. The obtained data of baseline apparent viscosity
(i.e. 1.8 cP) from the previous experiment were used to deduce the
proportion of limestone matrix in the foam generation (Table 2). De-
spite the previous results, the significant increase of the μapp only
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Colloids and Surfaces A 550 (2018) 245–255
occurred at the Q of > 8 ml/min in the fractured limestone core
(Fig. 6). Therefore, in this section, both limestone matrix and fracture
were used to evaluate the generation of foam. Additionally, the MPFP
was applied to estimate the amount of Q across the fractured limestone
•
core and hence the value of γ on the fluid flowing was calculated
through Eq. (15).
6Q
γ˙ (s−1) =
H 2W (15)
•
Fig. 6 shows the measured μapp vs. γ in the fractured limestone core.
•
It can be inferred that the notion of γ crit also applies for the fractures in
• •
the core. As shown in Fig. 6A, by reaching the γ to γ crit at 221.1 s−1, the
μapp increases to 2.53 cP. This is in accordance with forming the fine
texture of foam at the limestone matrix. Regarding the generation of
foam, the results reveal that the limestone matrix reached the value of
• •
γ crit before the fracture (i.e. γ crit 1011.3 s−1, Fig. 6B). This occurred
when 52% of injected fluid was passed through the fracture. It is
somewhat surprising that further injected fluid was allocated to the
limestone matrix, while the foam was generated in the fracture.
•
At the Q of < 8 ml/min, the γ in both fracture and matrix were
below the critical value and no foam was thus generated. At this stage,
O. Rahmani Colloids and Surfaces A 550 (2018) 245–255

Table 2
The experiment of foam generation in fractured limestone cores with different dispersion of NPs from 0.1 to 1 wt.%. The width of fracture equals to the core diameter
(i.e. 3-cm).
Experiment ϕ (%) kfr (mD) km (mD) kave.(mD) Q (ml/ min) ΔP (psi) μapp (cP) MRF •
γ fracture (s−1)
•
γ matrix (s−1)

FNP-1 21 6.02 × 10−6 25 24.91 1 0.47 1.830 1.017 470.588 47.561

NPs = 0.1 wt.% 3 1.47 1.908 1.060 1411.765 142.683
NaCl = 1 wt.% 6 3.01 1.954 1.085 2823.529 285.365
H = 85 μm 8 4.35 2.118 1.176 3764.706 380.487
T = 25 °C 10 5.47 2.130 1.184 4705.882 475.609
P = 1000 psi 12 7.01 2.275 1.264 5647.059 570.730

FNP-2 21 6.02 × 10−6 25 24.91 1 0.53 2.064 1.147 470.588 47.561

NPs = 0.1 wt.% 3 1.65 2.142 1.190 1411.765 142.683
NaCl = 1 wt.% 6 3.39 2.200 1.222 2823.529 285.365
H = 85 μm 8 4.78 2.327 1.293 3764.706 380.487
T = 50 °C 10 6.06 2.360 1.311 4705.882 475.609
P = 1500 psi 12 7.43 2.411 1.340 5647.059 570.730

FNP-3 21 6.02 × 10−6 25 24.91 1 0.51 1.986 1.103 470.588 47.561

NPs = 0.1 wt.% 3 1.62 2.103 1.168 1411.765 142.683
NaCl = 1 wt.% 6 3.39 2.200 1.222 2823.529 285.365
H = 85 μm 8 4.58 2.230 1.239 3764.706 380.487
T = 75 °C 10 8.9 3.466 1.926 4705.882 475.609
P = 2000 psi 12 11.59 3.762 2.090 5647.059 570.730

FNP-4 26 8.67 × 10−6 45 44.81 1 0.57 2.220 1.233 326.797 33.884

NPs = 1 wt.% 3 1.77 2.298 1.277 980.392 101.652
NaCl = 3 wt.% 6 3.61 2.343 1.302 1960.784 203.304
H = 102 μm 8 4.89 2.381 1.323 2614.379 271.072
T = 25 °C 10 6.24 2.430 1.350 3267.974 338.840
P = 1000 psi 12 7.66 2.486 1.381 3921.569 406.608

FNP-5 26 8.67 × 10−6 45 44.81 1 0.57 2.220 1.233 326.797 33.884

NPs = 1 wt.% 3 1.75 2.272 1.262 980.392 101.652
NaCl = 3 wt.% 6 3.56 2.311 1.284 1960.784 203.304
H = 102 μm 8 4.81 2.342 1.301 2614.379 271.072
T = 50 °C 10 6.1 2.376 1.320 3267.974 338.840
P = 1500 psi 12 7.49 2.431 1.350 3921.569 406.608

FNP-6 26 8.67 × 10−6 45 44.81 1 0.55 2.142 1.190 326.797 33.884

NPs = 1 wt.% 3 1.75 2.272 1.262 980.392 101.652
NaCl = 3 wt.% 6 3.58 2.324 1.291 1960.784 203.304
H = 102 μm 8 4.93 2.400 1.333 2614.379 271.072
T = 75 °C 10 9.14 3.560 1.978 3267.974 338.840
P = 2000 psi 12 11.86 3.849 2.138 3921.569 406.608

FNP-7 35 2.24 × 10−5 60 59.58 1 0.57 2.220 1.233 126.413 27.638

NPs = 1 wt.% 3 1.78 2.311 1.284 379.239 82.915
NaCl = 3 wt.% 6 3.6 2.337 1.298 758.477 165.829
H = 164 μm 8 4.97 2.420 1.344 1011.303 221.105
T = 25 °C 10 6.35 2.473 1.374 1264.128 276.382
P = 1000 psi 12 7.77 2.522 1.401 1516.954 331.658

FNP-8 35 2.24 × 10−5 60 59.58 1 0.57 2.220 1.233 126.413 27.638

NPs = 1 wt.% 3 1.78 2.311 1.284 379.239 82.915
NaCl = 3 wt.% 6 3.67 2.382 1.323 758.477 165.829
H = 164 μm 8 5.11 2.488 1.382 1011.303 221.105
T = 50 °C 10 6.52 2.539 1.411 1264.128 276.382
P = 1500 psi 12 7.89 2.561 1.423 1516.954 331.658

FNP-9 35 2.24 × 10−5 60 59.58 1 0.58 2.259 1.255 126.413 27.638

NPs = 1 wt.% 3 1.79 2.324 1.291 379.239 82.915
NaCl = 3 wt.% 6 3.69 2.395 1.331 758.477 165.829
H = 164 μm 8 5.19 2.527 1.404 1011.303 221.105
T = 75 °C 10 9.36 3.645 2.025 1264.128 276.382
P = 2000 psi 12 11.98 3.888 2.160 1516.954 331.658

68% of injected fluid was allocated to the fracture. In contrast, the foam
was generated in both matrix and fracture, while the Q of ≥8 ml/min
was applied and, therefore, 52% of injected fluid was allocated to the
fracture. Together these results provide important insights into the ef-
fect of the concentration of NP and NaCl on the quality of generated
foam.
3.3. Factor affecting the generation of CO2 foam
3.3.1. Effect of the Fg
The μapp, as an essential factor of foam generation, seems to affect
the Fg, which determines the volume fraction of CO2 in foam. Worthen
et al. [22] indicated that increasing the foam quality reaches the μapp to
a maximum level. There appears to be a maximum level of the Fg (i.e.
0.8) that obtained the highest μapp (i.e. 6.96) in the experiments (see
Table 1). While producing a significant μapp as a result of sufficient
lamellae needs considerable volume fraction of CO2 [16], the amount of
CO2 fraction was critically checked as it may reduce the lamellae and
decrease their stability. In the case of too high foam quality (i.e. 0.9),
there is not a sufficient amount of liquid to form lamellae and they are
too thin. Moreover, it is easier to coalesce the thin lamellae as there is
possibly only a monolayer coverage of NP. Additionally, sometimes lack

251
O. Rahmani Colloids and Surfaces A 550 (2018) 245–255

Fig. 6. The measured apparent viscosity vs. shear rate at both limestone matrix (A) and fracture (B).

Table 3
The quality of generated foam in unfractured and fractured limestone cores with 1 wt.% dispersion of NPs and 3 wt.% NaCl concentration.
Experiment T (°C) P (psi) K (mD) μfoamCO2 (cP) •
γ crit (s−1) ρCO2 (g/cm3) VCO2
VCO2 + VL

CNP-4 25 1000 25 3.17 266.66 0.88 0.45

CNP-8 50 1500 45 4.79 266.66 0.67 0.64
CNP-12 75 2000 60 6.96 266.66 0.43 0.80
FNP-3 25 1000 24.91 1.15 5647.06 0.88 0.31
FNP-6 50 1500 44.81 2.12 3921.57 0.67 0.56
FNP-9 75 2000 59.58 2.59 1516.95 0.43 0.74

of aqueous phase to support the generation of foam decreases its
quality. As a result of smaller lamellae proportion at high quality, there
is a possible transfer of foam from discontinuous- to continuous-gas
foam. In the continuous-gas foam, the unrestricted CO2 route caused a
considerable growth in the mobility of gas phase and consequently the
large CO2 bubbles were yielded (Table 3).
Moreover, the value of permeability affects the foam quality in
which it is dropped from a high value to a lower one, therefore, caused
to decrease the Fg. As a result, a continual decline in the Fg occurs while
the value of permeability decreases from 60 mD to 25 mD. What is
curious about this result is that the foam with the low quality resists
flow as permeability decreases [31].
Furthermore, the Fg was investigated at different temperatures of
25, 50 and 75 °C. For instance, the highest value of μapp obtained when
a foam quality of 0.8 generated at 75 °C rather than at T of 25 and 50 °C.
Considering these conditions at two unfractured and fractured core-
•
flood experiments, the γ crit decreased from 1516.95 s−1 to 266.66 s−1
as a consequence of the growth of foam quality from 0.45 to 0.8
(Table 3). To test these results, further analyses were conducted at a
consistent rate of injection on the limestone cores in order to establish
their optimum quality of foam. The results showed that there seems to
be a correlation between the value of μapp and the quality of foam in all
the experiments, which tends to be flat. The quality of foam below the
value of 0.31 did not has a significant effect on the μapp. At higher
values, the μapp of foam began to decline. The declination of μapp can be
elucidated through shifting from discontinuous-gas to continuous-gas
foam when further volume of CO2 is applied. Hence, this change was
determined as the ideal quality of foam since it produced the highest
μapp at a temperature of 75 °C. In contrast to earlier finding, Aroonsri
et al. [16] did not find any relation between the increasing T and the Fg.
They concluded that the T does not seem to affect the Fg and the trends
for all temperatures are the same.
In order to the feasibility of methyl-coated SiNPs to stabilize CO2
foam in the carbonate reservoirs, the effect of temperature was also
evaluated at higher temperatures of 75 °C. At these elevated tempera-
ture, the physical properties of carbon dioxide is changed from liquid
phase to supercritical one, therefore, this can affect the stabilization of
CO2 foam. The results showed that no foam was generated while CO2
and 1 wt.% methyl-coated SiNP in 3 wt.% NaCl were co-injected. These
•
data suggest that the γ crit may be increased higher than 266.66 s−1 as

252
O. Rahmani
the temperature increased to the upper than 75 °C. These results are in
line with those of previous studies. Sun et al. [17] reported that in-
creasing temperature has two functions on the foam quality. First, in-
creasing temperature to 60 °C increases the foam volume until the
maximum foam quality is reached and then the foam volume decreases
with temperature higher than 60 °C. In addition, an experimental de-
monstration of temperature effect was carried out by Bacho and Ben-
nion [32] who declared that the interfacial tension (IFT) between CO2
and water molecules at T of higher than 75 °C is about 25% greater than
the T of 50 °C. On the other words, a 25% more energy is needed to
move the NPs to the interface at the T of higher than 75 °C.
•
3.3.2. Effect of the γ crit
•
The effect of the γ crit on the generation of foam was demonstrated in
the experiments using unfractured and fractured limestone cores. The
•
μapp of NPs below the γ crit remains consistently similar to the experi-
•
ment without NPs. By overwhelming the γ crit, the rapid increase of the
μapp occurred as foam continued to refine its texture (see Figs. 4 and 6).
• methyl-coated SiNPs were used for all subsequent experiments.
A comparison of two experiments revealed that the value of γ crit varies
with the presence of fractures. In addition, the μapp and k affected the
• 3.4. The behavior of NP-St CO2 foam in the presence of HC
value of γ crit. In unfractured limestone core, a thinned layer of NPs-St
foam observed at low matrix permeability (e.g. 25 mD), however, in-
creasing the μapp to the peak value (i.e. 2.12 cP) at fractured limestone
core caused the NPs-St foam to have this behavior (see Fig. 6B).
3.3.3. NaCl concentration
The concentration of NaCl in the aqueous phase has a positive effect
on the generation of foam. According to Binks et al. [33], the addition
of salt to an aqueous phase increases the hydrophobicity between the
NPs. As a result, the affinity of NPs at their interfaces enhances when
the concentration of NaCl changed from 1 wt.% to 3 wt.% in the ex-
periments. Worthen et al. [22] demonstrate that increasing the con-
centration of NaCl improves the contact angle at CO2-water interfaces.
This improvement helps to adsorb more NPs at the CO2-water interface,
generate additional lamellae, and cause higher μapp. As shown in
Fig. 6B, it can be concluded that the increasing NaCl to 3 wt.% increases
• that the miscibility of decane and carbon dioxide proves the ability of
the μapp at the T of 75 °C and then decreases the value of γ crit to generate
the foam. The results revealed that adding further NaCl (e.g. 5 wt.%) to
the aqueous phase induced to aggregate the NPs, according to the
findings established by Worthen et al. [22].
3.3.4. Matrix permeability
The results, as shown in Table 1, indicate that the value of perme-
•
ability can affect both the μapp and γ crit. A comparison of the experi-
ments reveals that the μapp measured in the limestone core with higher
permeability (e.g. 60 mD) is greater than the core with lower value of
permeability (e.g. 10 mD); considering the same experimental condi-
tions in the temperature and salinity. It is also worth noting that the
•
value of γ crit for generation of foam is lower when the sample with
higher matrix permeability is used. These values were 266.66 s−1 and
about 653.19 s−1 in the limestone cores with matrix permeability of 60
and 10 mD, respectively.
3.3.5. NPs concentration
When the concentration of NP increases, the μapp of foam succes-
sively increases. A possible explanation for this result might be related
to improve the stability of lamellae. From the data in Tables 1 and 2, it
is apparent that increasing the dispersion of NPs from 0.1 to 1 wt.% into
the unfractured and fractured limestone cores (at the Q of 8 ml/min)
caused an increase of the value of MRF from 1.71 to 3.86 and 1.18 to
1.4, respectively. These findings indicate that increasing plentiful dis-
persion of NPs in the aqueous phase result in covering more surface of
CO2 bubbles and prohibit the coalescence of lamellae. Fig. 4 shows a
clear trend of generating foam at different concentration of NPs. From
these data, it can be seen that the foam is not generated while the
253
Colloids and Surfaces A 550 (2018) 245–255
concentration of NPs is low.
3.3.6. Effect of SiNPs coating
The properties of NPs surface are essential to the function of gen-
erated foam [4]. Because the NPs behaviors vary from the hydrophilic
to hydrophobic when they are dispersed to water and accumulated at
the CO2-water interphases, respectively. Nguyen et al. [4] indicated
that the strong attraction between methyl-coated SiNPs and CO2-water
interface reduces the NPs loss to the surface of the core rather than PEG-
coated nanoparticles. In addition to this benefit, the methyl-coated
SiNPs were more compatible at the carbonate reservoirs with high
temperature and pressure conditions. Therefore, 12 nm SiNPs with
three coating conditions of 0%, 50%, and 75% by C2H6SiCl2 were used
in the core-flood experiments. The findings indicated that no CO2 foam
was formed with uncoated SiNPs while both the 50% and 75% methyl-
coated SiNPs formed the stable foam. However, there was a significant
difference between 50% and 75% methyl-coated SiNPs and referred to
the aggregation of 75% methyl-coated SiNPs in water. Therefore, 50%
According to the stability and ability of foam to improve the re-
covery of oil, the behavior of NP-St CO2 foam was determined in the
unfractured and fractured limestone cores. Returning to the discussion
in subsection 3.3, it is now possible to state that a real mobility control
in CO2 EOR process can only be reached when the generated foam still
interacts with HC in the reservoir. To achieve this, decane with the
residual saturation (So) of 30% was applied to study the effect of HC on
CO2 EOR process in the aqueous phase associated with 3 wt.% NaCl and
CO2. The results revealed that decane is miscible with bubbles of CO2 in
both experiments with and without NPs and the So reduces from 30% to
4%. Referring to the miscibility of decane and CO2 bubbles, it was
unexpected to remain the So value in the cores. This result may be
explained by the fact that the water phase might have prevented the
miscibility between HC phase and CO2 bubbles. It can thus be suggested
the NP-St CO2 foam to reduce the So and control the mobility. Another
reason why these experiments were conducted is to measure the re-
covery of oil and the μapp. Fig. 7 shows the plots of μapp vs. PV injected
for the experiments with and without NPs. From the data in Fig. 7, it is
apparent that foam still provides a considerable amount of resistance
while the residual oil is present in the core. Considering the same
condition of residual oil, the highest value of measured μapp in the ex-
periment with and without NPs was 5.35 and 1.55 cP, respectively. The
presence of residual oil at the highest value of μapp declined the re-
sistance of foam against to flow.
In the experiment without NPs, the generated foam was transmitted
slightly faster (PV = 0.4) than the experiment with NPs (PV = 1.2)
across the core. Comparing the lack of residual oil, its presence also
supported the fast spread of generated foam. On the other hand, the
transmitted time of generated foam in the experiments with and
without NPs was 0.45 and 2.91 PV, respectively. It could be concluded
that there is a delay to transmit of foam in the lack of HC (see Figs. 3
and 5). It is also worth noting that the transmitted time is recorded with
a prompt response in the presence of HC. This finding suggests that the
interaction between the bubbles of CO2 and the residual oils may mo-
bilize the HC across the core.
3.5. Foam stability analysis
The stability of NP-St CO2 foam was measured by determination of
its half-life time through filling a cylinder with a bulk foam. Due to
decomposition of the foam stability at reservoir condition with high
temperatures [17], the half-life time of CO2 foam for both PEG- and
methyl-coated SiNPs was studied at different temperatures from 25 °C
O. Rahmani
Fig. 7. The plots of μapp vs. PV injected for the experiments with (a, b) and without (c) NPs in the presence of decane with the So of 30%.
Fig. 8. The analysis of foam stability measured by half-life time at different temperatures from 25 °C to more than 75 °C.
to more than 75 °C. In addition, the concentrations of PEG-coated and
50% methyl-coated SiNPs were ranged from 0.1 wt.% to 1 wt.%. The
results showed that the increasing temperature to 75 °C first increases
the bulk foam and then it decreases with applying further temperatures
(Fig. 8). These results are in agreement with those obtained by Nguyen
et al. [4] and Sun et al. [17]. They indicated that the half-life time of
NP-St CO2 foam decreases with increasing the temperature when the
bulk foam reaches to the maximum value. Although the half-life time of
PEG-coated SiNP was increased considerably, its bulk foam was about
25% lower than that methyl-coated SiNP in the same concentration. As
shown in Fig. 8, the value of half-life time for methyl-coated SiNPs is
about 3.11 times that of PEG-coated at T of 75 °C. As a result, the 50%
methyl-coated SiNPs have higher thermal stability.
4. Conclusions
The present study was designed to determine the mobility control in
CO2 EOR process using 12 nm methyl-coated SiNP in unfractured and
fractured limestone core-flood experiments. The results revealed that
the stable CO2 foam was successfully generated through direct co-in-
jection of CO2 and NP dispersion into the cores. The significant factor in
generating stabilized CO2 foam was the value of critical share rate in
•
the experiments with and without NPs. The value of γ crit referred to the
factors affecting the quality of CO2 foam. By increasing the quality of
•
foam in unfractured limestone core, the γ crit was decreased. The results
254
Colloids and Surfaces A 550 (2018) 245–255
suggest that changing the amount of matrix permeability from a high to
a lower one changes the optimum quality of foam. Therefore, the
limestone samples with higher matrix permeability had a lower value of
•
γ crit for foam generation. Taken together, these results suggest that the
pore throats simplifies the formation of bubbles and decreases the value
•
of γ required to generate the foam.
In addition, the amount of apparent viscosity was crucial for ob-
taining an optimal quality of foam. Establishing a condition similar to
the typical reservoir by posing the optimum quality of foam (i.e. 0.8) at
75 °C caused some difficulties in applying NP-St CO2 foam. It might be
preferable to apply high quality foam (i.e., 0.9) in the oilfields because
there the process demands less water, provides the reservoir with more
CO2, and increases foam mobility. It needs to be noted that the μapp
affected foam quality and was considered as the most crucial factor for
the aim of mobility control. Therefore, a logical relation between two
these factors (i.e. the μapp and foam quality) was required in order to
efficiently apply mobility control utilizing NP-St CO2 foam.
It was also shown that the increasing of NaCl concentration caused
to drive NPs to the interface of CO2 bubbles and brine. Although the
NPs was aggregated at NaCl concentration of 5 wt.%, this increasing to
•
3 wt.% decreased the value of γ crit for the foam generation thus the μapp
of foam was increased at temperature of 75 °C. On the other hand, in-
creasing the dispersion of NPs from 0.1 to 1 wt.% resulted to cover more
surface of CO2 bubbles and prohibited the coalescence of lamellae.
O. Rahmani Colloids and Surfaces A 550 (2018) 245–255

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