REE171539 DOI: 10.

2118/171539-PA Date: 21-August-15 Stage: Page: 387 Total Pages: 13

Experimental Study of Enhanced-Heavy-

Oil Recovery in Berea Sandstone Cores by
Use of Nanofluids Applications
Osamah A. Alomair, Khaled M. Matar, and Yousef H. Alsaeed, Kuwait University

Summary esses, and chemical flooding. Miscible flooding is a general term

The application of nanotechnology in the oil industry has become for injection processes that introduce miscible gases into the reser-
a useful approach in oil production. The main objective of this voir. Poor reservoir-volumetric-sweep efficiency is the major prob-
study is to investigate the effect of nanofluids on the recovery of lem associated with this type of flooding (Xiangling and Michael
heavy crude oil compared with waterflooding. The nanofluids are 2010). Thermal processes provide a driving force by adding heat
prepared by the addition of pure and mixed nanoparticles—silicon to the reservoir, which increases oil production by reducing the oil
oxide, aluminum oxide, nickel oxide, and titanium oxide—at dif- viscosity. This method includes steamflood and cyclic steam injec-
ferent concentrations to the formation water. The prepared nano- tion. The main disadvantage of this method is the heat loss during
fluids were screened to determine the suitable type for the heavy the injection process, which negatively impacts its applicability for
oil and rock samples subjected to the study. The effect of nano- deep reservoirs (Holm and Josendal 1982). Chemical flooding is
fluids on the interfacial tension and viscosity of emulsion were performed by the addition of chemicals (polymer, surfactant, or
also investigated. Nanofluid-flooding tests were performed on a alkaline fluid) to increase oil recovery, mainly by decreasing inter-
heavy-oil sample of 17.45  API by use of Berea sandstone core facial tension (IFT) or increasing oil mobility (Gates 2010). These
samples with average air permeability of 184 md, liquid perme- chemicals are less effective at high water salinity or high hardness,
ability of 60 md, and porosity of 20%. After selection of the opti- and there might be some damage or distortion for them at high res-
mum type of nanofluid, additional tests were performed including ervoir temperature (Dong et al. 2008). Therefore, new technologies
effect on asphaltene precipitation by use of a flow-assurance sys- are necessary to establish an EOR method that should lead to
tem. Results from the experiments show that the aluminum oxide appropriate spread of fluid deep inside the formation, minimum
nanofluid at concentration of 0.05 wt% reduced the emulsion vis- chemical adsorption onto the reservoir rock, fluids and/or chemi-
cosity by 25%. The mixed nanofluid of silicon and aluminum cals that can withstand high water salinity and well performance in
oxides at 0.05 wt% has shown the highest incremental oil recov- high reservoir temperature, and high reduction of IFT between the
ery among the other nanofluids. It is expected to be the best type injected fluid and oil (Manirique et al. 2010).
of chemical flooding because of its performance in reservoir con- Wang et al. (2009) observed that the addition of nanoparticles
dition (high pressure, temperature, and water salinity) and its to the injected fluid can enhance the oil recovery by altering the
capability to oppose asphaltene precipitation. wettability pattern of the reservoir rock. This study reveals that
nanoparticles may also serve as inhibitors for asphaltene precipi-
tation. The main mechanism for the spreading of the nanofluid to
produce oil was investigated by Wasan and Nikolov (2003),
Introduction Chengara et al. (2004), and Wasan et al. (2011), and it is called
The oil industry is facing challenges in terms of materials and the structural-disjoining-pressure gradient (Dc), which is
safe environmental operations, because energy consumption directed toward the wedge from the bulk solution. McElfresh
worldwide is expected to increase in coming years. It is important et al. (2012) described the force of this phenomenon, which is
to use improved-oil-recovery methods because large amounts of driven by Brownian motion and electrostatic repulsion between
the original oil in place is left after the production through pri- the nanoparticles. The electrostatic-repulsion force depends on
mary recovery (Wittle et al. 2008). Currently, studies of the effect the size and amount of nanoparticles. Disjoining pressure is
of nanotechnology in the oil industry are significantly increasing related to the ability of a fluid to spread along the surface. This
because of its ability to improve some of the important factors force will be stronger when nanoparticles are smaller, and it will
that have a positive effect on the oil recovery (Hascakir et al. increase as the quantity of nanoparticles increases. A wedge/film
2008; Hamedi and Babadagli 2010; Ayatollahi and Zerafat 2012; structure could be created when the nanoparticles are present in
Haroun et al. 2012; Ogolo et al. 2012; Shahrabadi et al. 2012). In the three-phase-contact region (oil/water/solid). The wedge/film
spite of the positive achievements with nanoparticles, some appli- will separate formation fluid such as oil, water, and gas from the
cations are still under laboratory study and research development. formation surface.
However, other nanoparticles can be used in the oil and gas indus-
try to overcome the issues caused by conventional recovery mech-
anisms, such as adsorption, chemical thermal degradation, and Experiments
working in extreme conditions of temperature and salinity (Choi Materials. The physical properties of the four nanoparticles used
and Eastman 1995; Abdelrahman and Adel 2013; Franco et al. in this study are reported in Table 1. Aluminum oxide (Al2O3)
2013). Also, they can be used to increase oil recovery, improve and nickel oxide (NiO) were provided by Skyspring Nanomateri-
water disposition, break emulsion, change hydrophilic and hydro- als Inc. (Houston, Texas). Silicon oxide (SiO2) and titanium oxide
phobic behavior of waterflood applications, and maintain the res- (TiO2) were supplied by MKnano (Missisauga, Ontario, Canada).
ervoir pressure above bubblepoint (Fletcher and Davis 2010). The microscopic structures were observed by use of a field-emis-
Enhanced-oil-recovery (EOR) processes are mainly classified sion scanning-electron microscope (FESEM) with a magnification
into three major categories: gas miscible flooding, thermal proc- of 25,000X, as shown in Fig. 1. The raw materials were used
without any future treatment. The heavy-crude-oil sample was
collected from an oil field in specially designed glass-stoppered
Copyright V
C 2015 Society of Petroleum Engineers
bottles of 2.5-L capacity and was stored at 20  C. The oil sample
This paper (SPE 171539) was accepted for presentation at the SPE Asia Pacific Oil & Gas was mixed with an emulsion breaker (commercial-grade Nalco
Conference and Exhibition, Adelaide, Australia, 14–16 October 2014, and revised for
publication. Original manuscript received for review 13 August 2014. Revised manuscript
demulsifier) and centrifuged to remove the traces of basic sedi-
received for review 7 February 2015. Paper peer approved 3 April 2015. ments and water by use of ASTM D4007 (1995) and finally

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Table 1—Properties of the nanoparticles.

Fig. 1—FESEM images of (a) titanium oxide, (b) aluminum oxide, (c) nickel oxide, and (d) silicon oxide.

maintained in an oven at 25  C. As soon as the bottles were Preparations. Preparation of 30,000 ppm Brine Water.
opened, the water contents of the samples were measured with a Formation water (FW) sample of 160,000 ppm salinity and 217.4-
Metrohm KF (Model 832-Thermoprep). Several important physi- ms/cm conductivity supplied from an oil field was used for sam-
cal and chemical properties (density, kinematic and dynamic vis- ple preparation with standard procedures. Produced water con-
cosities, molecular weight, and elemental components) were tains various impurities and pollutants, including organic and
measured, and the results are reported in Tables 2 and 3. inorganic particles and hydrocarbon droplets. Therefore, the filtra-
tion process was performed in two steps to reduce the concentra-
tion of total suspended solids (TSS) in water before injection. The
Porous Medium. The laboratory-flooding experiments were per- first step was performed by use of Whatman inorganic-membrane
formed on Berea sandstone core plugs purchased from Kocurek syringe filter capable of removing 0.7 lm of the suspended-solid
Industries (Houston); 21 core samples with average length, diame- particles. Sterile polyethersulfone syringe filters with four total
ter, and pore volume (PV) of 6.73 cm, 3.8 cm, and 15.34 cm3, layers were used as a second step to remove up to 0.45 lm of the
respectively, were used in this study. Fig. 2 indicates a core-sam- suspended particles. The prepared FW sample was diluted by
ple-surface morphology under FESEM. The permeability and po- Millipore (Merck Millipore, GmbH) ultrapure water with conduc-
rosity of the samples were measured by use of KA-210 gas tivity of 0.06 lscm and total dissolved solids 0.5 ppm until the
permeameter and PHI-220 helium porosimeter (Coretest System conductivity reached 46.9 ms/cm (30,000 ppm). The quality of
Incorporated), respectively. The results of the petrophysical prop- water was checked by Janway portable conductivity meter model
erties are tabulated in Table 4. 4071. To evaluate the quality of water and to understand the

Table 2—Physical properties of crude-oil sample.

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Table 3—Crude-oil composition. The total wt% of the components is 100.

distribution of the solid particles in water samples, a dynamic SiO2, and TiO2) of average diameters of 40, 50, 15, and 50 nm,
light scattering (DLS) Zetasizer Nano ZS-ZEN3600 was used as a respectively, which were dispersed with the treated FW of 3 wt%
technique that measures the fluctuations of the intensity of scat- salinity to create from each type the weight concentrations of 0.01,
tered light caused by the motion of the molecules in solution. The 0.05, and 0.1 wt%. Therefore, the suspension was stirred on the
results of DLS are presented in Fig. 3. It can be noticed that the digital stirring plate IKA C-Mag-HS 7 for 300 rev/min for 8 hours
average size of the TSS in the FW sample before and after the fil- at a temperature of 30  C; was left for 2 hours to observe the possi-
tration process decreased from 2470 to 685 nm. Particle move- bility for particle agglomeration; and then was sonicated by means
ment in porous media is a very-complex process because of the of an ultrasonic bath U300H (Ultrawave U300H Ultrasonic Bath)
complexity of porous media and forces governing the movement for a period of 4 hours at 40  C to obtain homogeneous suspen-
of solids through it. Because of this, the filtration process was sions. The nanofluids were left to rest overnight, and afterward,
conducted because these suspended-solid particles might affect each nanofluid was subjected to ultrasonication by Hielscher
the mechanisms of nanoparticles. The density and viscosities of GmbH ultrasonic mixture model UP200S for approximately 8
the 30,000 ppm brine sample were measured as shown in Table 5. hours to ensure uniform dispersion of nanoparticles as well as to
Nanoparticle Stability. To perform the laboratory experi- prevent the nanoparticles from the initial agglomerating in the
ments closer to the real enhanced-oil-recovery (EOR) operating base fluid. After preparation of each nanofluid, the solution was
conditions. After the nanofluids preparation, the samples were placed in a sealed transparent bottle and used immediately. To
kept for 48 hours at temperature 30–40 C and pressure 450 psi in determine that there was a complete dispersion of nanoparticles in
specially design Stainless Steel containers, then observation from the solution, the n-potential was measured for nanofluids of aver-
the side glass were recorded (color, turbidity, sedimentation) of age measured pH value equal to 5.92 and a concentration of 0.1
each prepared nanofluid to assure sample stability. The nanofluids wt% for the aforementioned nanoparticles by use of the DLS appa-
preparation included hydrophilic nanoparticles (Al2O3, NiO, ratus. The measured values were –13.2, –28.3, þ 25.3, and –23.4
for TiO2, SiO2, Al2O3, and NiO, respectively. The magnitude of
the n-potential indicates the degree of electrostatic repulsion
between adjacent and similarly charged particles. The results were
satisfactory because the colloids with high n-potential (negative or
positive) are electrically stabilized and in dispersion, and it is a
key indicator of the stability of colloidal dispersions (the solution
or dispersion will resist aggregation) (Xu 2008). Table 6 shows
the densities of the nanofluids at different temperatures.
Nanofluid Preparation. The four nanofluids were used with-
out any further treatment. Each nanofluid was prepared by mixing
the treated saline water with nanoparticles to obtain three concen-
trations of 0.01, 0.05, and 0.1 wt% from each type. A digital stir-
ring plate at 300 rev/min followed by ultrasonic mixing was used
to obtain a high dispersion of the nanoparticles in the solution. Ta-
ble 6 shows the densities of the nanofluids at different tempera-
tures. After preparing the nanofluid, the solution was placed in a
sealed transparent bottle and used immediately to ensure a com-
plete dispersion of nanoparticles in the solution and to prevent the
nanoparticles from settling down.
20 µm EHT = 20.00 kV Signal A = SE2 Date: 8 Dec 2013
Mag= 1.00 K X WD = 17 mm Photo No. = 3408 Time: 13:40:59 Coreflood Experimental Work Flow. The laboratory experi-
ments consist of recovery processes by both routine waterflood-
ing and nanofluid flooding. In the routine waterflooding, the FW
Fig. 2—Core-sample-surface morphology under FESEM. was used as injected fluid, whereas in the nanofluids case, stable

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Table 4—The measured dimension and average petrophysical properties of core samples at initial conditions.

5000
Zeta-Potential Average Size (d·nm)

4500
4000
3500
3000
2500
Formation water
2000 Formation water after filtration
1500 Deionized water
Crude oil
1000
500
0
0 200 400 600 800 1,000 1,200
Time (minutes)

Fig. 3—DLS results for formation water, crude oil, and deionized water.

colloidal solutions of FW mixed with individual nanoparticles were studied. Stage 1 included the use of the four nanoparticles
(TiO2, SiO2, Al2O3, and NiO) at different concentrations were with three different concentrations of 0.01, 0.05, and 0.1 wt% for
used as injection fluid. The coreflood experiments were con- each type as a secondary-recovery process to be compared with
ducted in five main stages. Through a work flow of the five waterflooding on the basis of oil recovery. The effect of nano-
stages, the behaviors of the nanofluids and blank FW injection fluids and brine on emulsion viscosity and IFT were also studied.
In Stage 2, a new testing approach was applied that included mix-
ing the two types of nanoparticles (ratio of 1:1) to indicate the
best influence on the three criteria mentioned in Stage 1, to be
implemented as a secondary-recovery method and compared
with outcomes in Stage 1. The best nanofluid on the basis of
Table 5—Physical properties of 30,000 ppm brine sample at 25 º C. incremental oil recovery was selected as the recommended

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to ensure complete saturation. This was followed by the oil-satu-

ration process at an injection rate of 0.5 cm3/min until no more
water was produced. At this point, the core is at connate water
and initial oil saturations. The core was then flushed by use of
nanofluid or brine (as secondary method) at a flow rate of
0.2 cm3/min until no more oil is produced [approximately 2.5 PV
injected (PVI)]. Vetter et al. (1987) conducted particle-filtration
tests to study the effects of particle sizes, flow rates, particle con-
centration, and particle charges. The test conditions concluded
that particles of sizes from 0.05 to 7 lm cause formation damage.
The lower injection rate (less than or equal to 0.5 cm3/min) will
minimize the possibility of formation damage. The higher the lin-
ear flow rate, the less severe the damage to the core plug. In addi-
tion, high particle concentration will cause more-severe damage.
Consequently, the particle retention in the core is often affected
by the nanofluid-flow rate. It is suggested that higher velocity in
narrow areas can cause heavier particles to accumulate and
retain, or in the worst case block pore throats. Keeping all other
parameters constant (particle size, viscosity, and temperature of
the nanofluids constant), nanofluid was injected with different
flow rates (0.2 or 0.5 cm3/min) at constant value of 0.75 PVI
(breakthrough). The pressure-drop variation occurred at the same
nanoparticle concentration and the same type even at low particle
Table 6—Experimental nanofluid-density results at different temper- size (Table 7). This behavior could be a result of rock morphol-
atures. ogy, FW salinity, and/or caused by increase of the nanofluid-flow
rate. Consequently, all preventive measures were taken in consid-
eration of the constant low injecting flow rate of 0.2 cm3/min to
nanofluid and was used in the next stages. Stage 3 included the ensure stability and the homogeneous nature of the nanofluid. In
use of the recommended nanofluid as tertiary recovery. From this Stage 3 only, nanofluid injection as the tertiary method followed
stage, a recommendation can be concluded on the appropriate re- after the injection of 2 PVI of waterflooding at flow rate of
covery method for this nanofluid. Stage 4 studied the effect of 0.2 cm3/min. Fig. 4 shows the schematic of the coreflood setup. It
water salinity on the performance of the recommended nanofluid. consists of the core holder, positive-displacement pump, transfer
Formation water of 160,000 ppm was used as injection fluid and vessels, and high-pressure steel piping (1=8-in. inner diameter).
the oil production was determined. Then, the recommended The produced fluids were carried through the outlet regulator into
nanoparticles will be dispersed in the FW (same salinity) to esti- an accumulator.
mate its potential by estimating the incremental oil recovery.
Stage 5 tested the performance of the recommended nanofluid
under reservoir conditions. IFT. The IFT between crude oil and brine/nanofluid as aqueous
phase was measured by the Vinci Technologies IFT 700. The de-
vice uses a pendant-drop IFT-measuring system. The oil drop is
Coreflood Setup and Procedure. Waterflooding is commonly generated from the end of a capillary needle in a bulk fluid at
used as a secondary-recovery method in which water is injected required pressure and temperature conditions. With a calibrated
into reservoir, displacing the oil in front of it. This assumes that and accurate video-lens system, the complete shape of the drop is
the reservoir is initially at irreducible water saturation and only analyzed with the drop-shape-analysis software. Then, the nonlin-
oil is produced until breakthrough, the time when water first ear system of differential equations is solved (Laplace equation)
appears at the production well. After breakthrough, increasing numerically over the complete shape. The measurements are per-
the amount of water decreases the amount of oil that is produced. formed at room temperature and pressure of 450 psi. This pressure
The process continues until the water/oil ratio is so high that the represents the average inlet pressure of the coreflood experiments
well becomes uneconomical to produce. On the basis of the nor- in Stage 1.
mal operation in the oil fields, we designed our coreflood experi-
ments by use of nanofluids instead. The clean core sample was Emulsion Viscosity. The four types of nanoparticles at different
placed inside a sleeve of rubber and set inside the core holder. concentrations have been used to estimate their ability on reduc-
Then the core was vacuumed by use of an Edwards model RV3 ing emulsion viscosity by use of an electromagnetic viscometer at
vacuum pump to evacuate the air inside the core holder. A pre- 45  C. The viscometer consists of two coils that move the piston
caution should be taken so that the coffering pressure around the back and forth magnetically at a constant force. The instrument
sleeve is applied and there is no leak when the vacuum pump is was calibrated by measuring in triplicate the three reference sam-
working. The confining-pressure regulator was set at 900 psi for ples, N600, N2000, and N4000, supplied by Canon Instruments.
Stages 1 through 4 and at 1,600 psi for Stage 5, to prevent any The calibration was performed for the temperature range of inter-
leakage events that may occur between the sleeve and the core est with a reproducibility of 60.95%.
inside it. For Stage 5 only, the coreflood experiments were per-
formed at 80  C with the outlet pressure regulator at 1,100 psi;
the other stages were performed at ambient temperature and with Asphaltene Precipitation Through Solid-Detection System
outlet regulator of 450 psi. The water-saturation process was per- (SDS). The pressure/volume/temperature (PVT) cell is equipped
formed by transferring the brine through a pipe that has one side with SDS for screening the stability of asphaltene in the fluid sam-
connected to the inlet valve and the other side inside a beaker ple by detecting the solid particles by use of a laser spectroscopy
filled with the brine. This saturation process was performed by SDS, which uses near-infrared light to probe fluids as asphaltenes
gravity force to remove the possibility of air compressibility. The precipitate isothermally with decreasing pressure (for live oil) or
PV was measured from this process by subtracting the readings by injecting n-heptane to the sample at a specific rate (for dead
of brine inside the beaker before and after opening the inlet oil). In the oil-phase SDS fluid sampling and analysis laboratory
valve. Afterward, the water vessel was filled with the same brine setup, the PVT cell used for this technique is a transparent glass
and the core was flushed at a flow rate of 0.5 cm3/min by use of tube containing a magnetically driven mixer. A near-infrared light
the Vinci Technologies model SP 65 positive-displacement pump source on one side of the cell generates light at specific

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Table 7—Effect of nanofluid-flow rate on differential pressure (DP) along the core plugs at constant
pore volume 5 0.75 (breakthrough) and injecting pressure of 450 psi.

transmittance power, and fiber-optic sensors on the other side are throat (Ravera et al. 2006). From the average measurement of IFT
used to detect the light. When asphaltenes precipitate, the scatter results, it can be observed that measured values between crude oil
light reduces the transmittance power of the light detected by the and nanofluids undergo the same exponential decrease of up to
sensors. An average pressure of 3,000 psi and temperature of 0.05 wt% of the nanoparticle concentration, and no change can be
45  C were applied for the experiments. Injection rate of n-hep- seen at 0.1 wt% (Fig. 5). This suggests that the reduction in oil/
tane was held constant at 20 cm3/h. water IFT may be related to the interactions between oil phase/
nanofluid. Karnanda et al. (2013) indicated that IFT values
undergo an exponential decrease with the increase of surfactant
Results and Discussion concentration, and Bin Dahbag et al. (2014) indicated the same
Stage 1: Evaluation of the Individual Nanoparticles. Effect of behavior when using ionic liquids instead of surfactant. Li et al.
Nanofluids on Interfacial Tension (IFT). The IFT is the surface (2013) also found similar performance by studying the effect of
tension at the surface separating two immiscible liquids. Reduc- silicon oxide (SiO2) nanoparticles on IFT; the study indicated a
tion of IFT demonstrated the nanofluids’ potential to mobilize reduction in IFT caused by the effect of specific-surface area
immobile oil and improve oil recovery (Munshi et al. 2008). This (SSA). This complies with our study, in which high SSA of nano-
leads to easy flow of the trapped oil because it reduces the work particles has a great effect on decreasing IFT, as shown in the
of deformation needed for oil droplets to move through the pore behavior of SiO2 (650 m2/g), which caused a reduction in IFT up

Conferring-pressure regulator
Connection valve

Outlet regular

Inlet valve Outlet valve

Air cylinder

Accumulator
Core holder

Stand
Oil vessel Water/nanofluid vessel
Pump

Fig. 4—Schematic of the coreflood experimental setup.

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most-effective concentration of nanoparticles: 0.05 wt% in FW.

2.9 HNF of SiO2
The result shows a pseudoplastic (non-Newtonian) behavior up to
HNF of TiO2
2.7
20 shear rates. As the shear rate increased, the nanofluids behave
HNF of NiO
in a Newtonian manner. Similarly, the dynamic viscosities of
Interfacial Tension (mN/m) HNF of Al2O3
crude oil with 5 wt% of FW and nanoparticles were measured by
2.5 SiO2 + Al2O3
use of the electromagnetic viscometer. The results of blank-crude-
2.3 oil viscosities before and after addition of FW at 45  C were 65.81
and 71.3 cp, respectively. This increase in viscosity may be caused
2.1 by the water-in-oil emulsion, as stated by Farah et al. (2005); they
indicated that this increase in viscosity may be caused by the pseu-
1.9 doplastic and non-Newtonian behavior (more nonlinear shear-
stress/shear-rate relations). Table 9 shows the results of emulsi-
1.7
fied-crude-oil viscosity before and after adding the optimum con-
1.5 centration of 5 wt% of FW and nanoparticles. According to the
studies of Dan and Jing (2006) and Chong et al. (1971), as the con-
1.3 centration of the dispersed phase increases, the effect of droplet-
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.1 0.11 0.12 size distribution on water-in-oil emulsion viscosity will increase.
Nanofluid Concentration (wt%) Fig. 6a shows the droplet size of blank 5 wt% FW in oil is
16.65 lm, but with 5 wt% of FW and 0.05 wt% of Al2O3 nanopar-
Fig. 5—Effect of nanoparticles on IFT between nanofluid and ticles, the droplet size decreased by 38.44% to 10.25 lm, as indi-
crude oil. cated in Fig. 6b. This behavior indicates that Al2O3 nanoparticles
have the tendency to destabilize the water drops, which facilitates
to 37.6% from the original value, and also in the behavior of NiO the coalescence of water droplets and so reduces the emulsion vis-
(6 m2/g), which caused the lowest effect with a reduction up to cosity by 25.15% at 0.05 wt% of Al2O3 and to 3.23% at 0.1 wt%
28.11%. Comparisons between the IFT reduction for the individ- of Al2O3. The same behavior could be seen for NiO at concentra-
ual nanoparticles—aluminum oxide (Al2O3), nickel oxide (NiO), tions of 0.01, 0.05, and 0.1 wt% with a decrease in emulsion-vis-
SiO2, and titanium oxide (TiO2)—and the mixture of SiO2/Al2O3 cosity values ranging from 0.6 to 1.22%. This performance also
were performed at concentration of 0.05 wt%. The comparison could be seen at 0.01 wt% of SiO2 and at 0.01 and 0.1 wt% of
showed that the mixture had stronger impact on the reduction of TiO2 for the decrease in emulsion viscosity by 2.88, 6.6, and
IFT than individual nanoparticles. As shown in Fig. 5, the IFT of 13.32%, respectively. It is suggested that the nanoparticles may
the mixture of the blank crude oil and the low-salinity formation have an effect on emulsion, which can form a compact, well-struc-
water (FW) was reduced from 2.92 mN/m to 1.7 mN/m (41.31%) tured monolayer at the aqueous/nonaqueous-phase interface to
when mixed with 0.05 wt% concentration of the SiO2/Al2O3 mix- make the emulsion extremely stable even under high temperatures,
ture. The results of these experiments showed how dispersed and offer the possibility of the controlled destabilization of the
nanoparticles in an aqueous phase (FW and nanofluid) can modify emulsion. Also from Table 8, it can be observed that each type of
the interfacial properties of the liquid/liquid systems if their sur- nanoparticle had its own influence on the emulsion viscosity
face is modified by the presence of nanoparticles. because of the heterogeneity in the physical properties of each
Effect of Nanofluids on Crude-Oil Viscosity. In the present nanoparticle. Ogolo et al. (2012) concluded that Al2O3 nanopar-
study, the effects of different nanofluids on oil viscosity and recov- ticles have the tendency to produce oil through their ability to
ery processes were investigated experimentally. Viscosity of the reduce oil viscosity when used with fresh water and brine as the
displacing fluid is an important parameter in enhanced oil recovery dispersing fluid. The rheological characteristics of these emulsions
(EOR). Therefore, the increase in viscosity of the displacing fluid have the potential to facilitate the conformance control during oil
to a certain extent improves the mobility ratio, which increases the recovery. Therefore, a common problem is that water injected to
overall displacement of oil by increasing the sweep efficiency. The displace oil toward production wells flows preferentially through
viscosities of nanofluids were measured just after reultrasonication high-permeability, already-swept portions of the reservoir.
by use of a Brookfield viscometer CAP 2000 þ of low torque, with Effect of Nanofluids on Oil Recovery. 30,000-ppm salinity
CAP-01L cone-type spindles at different shear rates, 1/s to 100/s, water without and with nanoparticles SiO2, Al2O3, NiO, and TiO2
and temperature of 25  C. The calibration was conducted by use of was tested to determine the best choice for increasing the oil re-
NIST fluid S60 supplied by the manufacturer. Table 8 shows the covery rather than the typical waterflooding process. Table 10
results of the measured viscosity data of the nanofluids with the shows the results obtained from the coreflood experiments. From

Table 8—Nanofluid viscosity as a function of shear rate of SiO2, Al2O3, NiO, and TiO2 at 0.05 wt% concentrations in FW of 3 wt% salinity
(after reultrasonication).

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Table 9—Experimental viscosity data of blank-crude-oil emulsion with different concentrations of

nanoparticles. gblank(oil) = Dynamic viscosity of blank crude oil with no nanofluid. gblank(oil) = Dynamic
viscosity of crude oil with nanofluid (FW+ nanoparticles).

Fig. 7, it can be observed that 0.01 wt% of SiO2 hydrophilic nano- alteration and the reduction on the IFT. The IFT influences capil-
fluid (HNF) in Core A1 produced the highest incremental oil re- lary pressure, capillary number, and adhesion tension. The capil-
covery compared with the other concentrations of the same lary number increases as IFT decreases, and consequently the oil
nanoparticle (5.903% more than the blank low-salinity water- recovery will increase, whereas as the nanoparticles’ concentra-
flooding). This is mainly because of the excessive reduction effect tion changes from 0.05 to 0.1 wt%, the recovery decreased
on the IFT as shown in Fig. 5, and the particles that have high slightly. The main suggested reasons for this performance are that
SSA providing an excess pressure in the wedge/film. Buckley and concentration changes increased the viscosity of emulsion,
Fan (2005) suggested that the hydrophilic silica nanofluids can plugged the pore channels, or both occurred in the core. Hendra-
give a high performance on oil recovery because of wettability ningrat et al. (2013) concluded that higher concentration of

Fig. 6—Particle-size analysis of crude oil under optical microscope with 200X magnification: (a) injecting 5 wt% of blank
30,000 ppm saline water and (b) injecting 5 wt% (4.95 wt% saline water and 0.05 wt% Al2O3) nanofluid.

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Table 10—Drainage processes and nanofluids/improved-oil-recovery scenarios.

45

40

35
Oil Recovery (%)

30
SiO2 0.01 wt%
25 SiO2 0.05 wt%
SiO2 0.1 wt%
Al2O3 0.01 wt%
20 Al2O3 0.05 wt%
Al2O3 0.1 wt%
15 NiO 0.01 wt%
NiO 0.05 wt%
10 NiO 0.1 wt%
TiO2 0.01 wt%
TiO2 0.05 wt%
5 TiO2 0.1 wt%
Waterflooding
0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
Pore Volume Injected

Fig. 7—Nanofluid oil recovery vs. PVI (Stage 1).

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45
40
35

Oil Recovery (%)

30
25
20 SiO2/Al2O3 0.01 wt%
15 SiO2/Al2O3 0.05 wt%
10 SiO2/Al2O3 0.1 wt%
5 Waterflooding
0
0 0.5 1 1.5 2 2.5 3 3.5
Pore Volume Injected

Fig. 8—SiO2/Al2O3-nanofluid oil recovery vs. PVI (Stage 2).

45 45
40 40
35
Oil Recovery (%)

35

Oil Recovery (%)

30 30
25
25
20
20
15
Waterflooding 15
10 Waterflooding 160,000 ppm
SiO2/Al2O3 0.05 wt% 10 SiO2/Al2O3 0.05 wt%
5
0 5
0 1 2 3 4 5 6
0
Pore Volume Injected 0 0.5 1 1.5 2 2.5 3 3.5
Pore Volume Injected
Fig. 9—SiO2/Al2O3 oil recovery vs. PVI as tertiary process
(Stage 3). Fig. 10—SiO2/Al2O3 oil recovery vs. PVI under high salinity
(Stage 4).
nanoparticles has a tendency to block pore throats because of the
aggregation of these particles around the pores, which could pre- film. The results of flooded Cores D1 and D2 by TiO2 HNF at
vent additional oil recovery. The Al2O3 nanofluid of 0.05 wt% in 0.01 and 0.05 wt%, respectively, indicated low effect on the incre-
Core B2 obtained an oil recovery of 38.5% at 2 pore volumes mental oil recovery. However, a severe reduction by 16.95% of
injected (PVI), whereas at the same PVI, concentration of 0.1 incremental recovery was obtained for Core D3 (0.1 wt%)
wt% in Core B3 reached an oil recovery of 25%. Therefore, a because of the plugging of pore channels as a result of the injec-
selection was made to consider 0.05 wt% the most-practical con- tion at high concentration.
centration for Al2O3 nanoparticles. The main expected reasons for From Stage 1, it can be noticed that SiO2 indicated the best
the performance of 0.05 wt% of Al2O3 nanofluid are the reduction influence on IFT and Al2O3 exhibited the most reduction in emul-
of IFT and its effect on emulsion viscosity. In case of Cores C1 sion viscosity (25.147% reduction at 0.05 wt%). SiO2 at 0.01 wt%
and C2 injected with 0.01 and 0.05 wt% of NiO nanofluids, and Al2O3 at 0.05 wt% obtained the highest incremental oil recov-
respectively, it can be observed that there was a negative effect on ery of 5.903 and 6.02%, respectively, among the other nanofluids.
the incremental oil recovery. However, there was an increase by Therefore, these two nanoparticles were selected to be used in the
3.56% for 0.1 wt% of NiO (Core C3). This performance might be next stage.
because of the low SSA value of NiO nanoparticles. It is sug-
gested that nanoparticles with very-low SSA values need to be
Stage 2: SiO2/Al2O3-Nanofluid Flooding As Secondary-
injected at high concentrations to have the ability to increase the
disjoining pressure and provide an excess pressure in the wedge/ Recovery Process. From Fig. 8, it can be observed that the per-
formance of the mixed SiO2/Al2O3 nanofluids (ratio of 1:1) had a
substantial enhancement on the incremental oil recovery, which
60 was measured at 7.52 and 9.65% for concentrations of 0.01 and
0.05 wt%, respectively. The main suggested reason for this
50
improvement is that mixed SiO2 and Al2O3 will have a high SSA
Oil Recovery (%)

40 value that might positively affect the oil recovery, because SiO2
reduces IFT and Al2O3 reduces both emulsion viscosity and IFT.
30 For 0.1 wt%, the anticipated reason for the low amount of oil pro-
duction is that the pore channels were plugged because of the
20 high concentration injected. The mixed SiO2/Al2O3 nanofluid at
10 Waterflooding 160,000 ppm 0.05 wt% provided the highest incremental recovery in Core E2
SiO2/Al2O3 0.05 wt% among all the other nanofluids. Therefore, it was chosen as the
0 recommended nanofluid and will be used in the next stages.
0 1 2 3 4 5 6
Pore Volume Injected
Stage 3: SiO2/Al2O3-Nanofluid Flooding As Tertiary Recovery
Fig. 11—SiO2/Al2O3 oil recovery vs. PVI at reservoir conditions Process. The performance of the recommended nanofluid was
(Stage 5). tested as a tertiary-recovery method on Core F1 to conclude the

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(a) Stage 5: SiO2/Al2O3-Nanofluid Flooding Under Reservoir

0.25 Conditions. As previously discussed, the use of polymer, surfac-
0.20 tant, or alkaline as chemical-flooding materials is not applicable
0.15 at high water salinity and they might be degraded at high reservoir
0.10 temperature. Therefore, studying the performance of the mixed
0.05 nanofluid under reservoir conditions is essential. Core H1 at pres-
0.00 sure of 1,600 psi and temperature of 80  C was injected with FW
0.5 1.0 1.5 2.0 2.5 3.0 3.5 of salinity of 160,000 ppm in this stage to determine whether
(b)
nanofluid injection is applicable at near-reservoir conditions. Core
H2 was also placed under the same conditions of pressure and
0.25 temperature and injected with nanofluid of mixed nanoparticles
0.20 SiO2 and Al2O3 at concentration of 0.05 wt%. The results of
0.15 flooding with FW of high salinity and with nanofluid of mixed
0.10 nanoparticles provide oil recovery of 32.99 and 56.7%, respec-
Normalized Power

0.05 tively. Fig. 11 compares both cases. The incremental increase in

0.00
0.5 1.0 1.5 2.0 2.5 3.0 3.5
recovery of 23.724% when injecting mixed nanofluid provides
clear evidence of the advantage of the use of mixed-nanofluid
(c) flooding vs. traditional waterflooding.
0.25
0.20 Effect of SiO2/Al2O3 Nanofluids on Asphaltene Precipitation.
0.15
Asphaltene adsorption plays an enormous role in enhancing oil re-
0.10
covery. Therefore, studying the effect of nanoparticles on asphal-
0.05
tene precipitation is vital. Abu Tarboush and Husein (2012) and
0.00
0.5 1.0 1.5 2.0 2.5 3.0 3.5 Mohammadi et al. (2011) concluded that nanoparticles have the
ability to stabilize asphaltene precipitation. From the knowledge
(d)
gained, the recommended nanofluid study was not yet tested for
0.25 effect on asphaltene precipitation; therefore, this is the first
0.20 experiment that has been performed by use of this type of nano-
0.15 particles. Fig. 12 shows the response of the solid-detection-system
0.10 light transmittance during the injection of n-heptane. With addi-
0.05 tion of n-heptane to the total volume of the solution, saturated
0.00 hydrocarbon will increase, resulting in aggregation of the asphal-
0.5 1.0 1.5 2.0 2.5 3.0 3.5 tene particles that are dissolved in the oil. The density of these
Volume Ratio (Cc of C7 of Oil sample) particles will increase with time and cause precipitation, accord-
ing to Stokes’ law. Fig. 12a represents the behavior of a crude-oil
Fig. 12—(a, b, c and d) Onset point of asphaltene from blank sample with 5 wt% of FW (3% salinity). As the volume ratio of n-
heavy crude oil with saline water (3 wt%) and 0.01, 0.05, and 0.1 heptane increased, the light transmission stabilized up to 0.825
wt% of SiO2/Al2O3 mixture, respectively, at 45 º C. volume ratio of n-heptane, showing that no asphaltene is being
precipitated yet; afterward, the light transmission decreased
because of asphaltene precipitation. Figs. 12b, 12c, and 12d ex-
hibit the behavior of a heavy-crude-oil sample mixed with 5 wt%
appropriate recovery method for this type of nanofluid. An insig-
of nanoparticles and FW. The nanofluids were SiO2/Al2O3 at con-
nificant increase of 0.959% of oil recovery above the secondary
centrations of 0.01, 0.05, and 0.1 wt% in FW. It can be observed
baseline was obtained after 2.96 PVI of the recommended nano-
that as the concentration of nanofluids increases, greater delay of
fluid was used in the tertiary-recovery process, as shown in Fig. 9.
asphaltene precipitation will be achieved. The light transmission
A difference of 8.69% can be obtained between the use of SiO2/
was stabilized until 1.23 and 1.55 volume ratio for 0.01 and 0.05
Al2O3 nanofluid as secondary- and tertiary-recovery processes.
wt%, respectively, and then it decreased steeply and stabilized to
Therefore, it can essentially be noticed from this experiment that
the end of the tests. When the concentration increased up to 0.1
the favorable flooding method for the recommended nanofluid is
wt%, asphaltene precipitation was delayed during the entire test,
to be injected as the secondary-recovery method. Hendraningrat
suggesting that this concentration is the most recommended one
et al. (2012) also observed that nanofluid flooding has more poten-
to overcome the asphaltene phenomenon, as shown in Fig. 12d.
tial in improving oil recovery as a secondary-recovery process
This shows that the SiO2/Al2O3 nanofluid has a tendency to delay
than a tertiary method.
the precipitation and deposition of asphaltene. However, as men-
tioned previously in this study, 0.1 wt% of SiO2/Al2O3 might
Stage 4: SiO2/Al2O3-Nanofluid Flooding in High-Salinity block the pore throats when used for flooding.
Water. The performance of the SiO2/Al2O3 nanofluid was tested
under the influence of high water salinity. Saline water of
160,000 ppm was injected in Core G1. The mixed nanoparticles Conclusions
were dispersed in the same water salinity and injected in Core G2. Owing to the unique properties of the metal oxide nanoparticles
In Stage 1, 30,000 ppm of low-salinity water was injected in Core that are different from their bulk counterparts, nanoparticles have
W1 given an oil recovery of 32.639%, whereas in this stage, considerable potential applications as adsorbents and catalysts for
160,000 ppm formation-water (FW) flooding obtained an oil re- upgrading heavy oil and enhancing recovery. However, the appli-
covery of 24.469%, as shown in Fig. 10. This performance was cation of nanoparticle technology in the oil industry is facing a
expected because as the salinity of the injected water decreased, number of limitations and challenges. The presence of nanopar-
more oil will be produced because of wettability alteration (Agba- ticles inside the injected fluid has provided the ability to improve
laka et al. 2009). The SiO2/Al2O3 nanofluid has shown an incre- oil recovery as a secondary-recovery method vs. the typical water-
mental oil recovery of 4.895%, lower than the value in Stage 2 by flooding process. The dispersed nanoparticles in an aqueous phase
4.751%. That was also expected for the previously mentioned rea- [formation water (FW) and nanofluids] can decrease the viscosity
son. After comparing the results of both stages, it can be noticed or modify the interfacial properties of the liquid/liquid systems if
that the mixed nanoparticles are preferred to be dispersed in low their surface is modified by the presence of controlled-nanopar-
water salinity. ticle concentration. This study sheds some light on the potential

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application of nanoparticle technology in heavy-oil upgrading and Dan, D. and Jing, G. 2006. Apparent Viscosity Prediction of Non-Newto-
recovery. The effect of the tested nanoparticles on interfacial-ten- nian Water-in-Crude Oil Emulsions. J. Pet. Sci. Eng. 53 (1–2):
sion (IFT) values undergoes an exponential decrease with the 113–122. http://dx.doi.org/10.1016/j.petrol.2006.04.003.
increase of nanoparticle concentration up to 0.05 wt% in FW, but Dong, M., Ma, S. and Liu, Q. 2008. Enhanced Heavy Oil Recovery
the opposite behavior could be seen at high concentration of nano- Through Interfacial Instability: A Study of Chemical Flooding for
particles, near 0.1 wt%. Thus, the hydrophilic silicon oxide (SiO2) Brintnell Heavy Oil. Fuel 88 (6): 1049–1056. http://dx.doi.org/
and aluminum oxide (Al2O3) nanofluids yield higher performance 10.1016/j.fuel.2008.11.014.
on oil recovery compared with nickel oxide and titanium oxide Farah, A. M., Oliveira, C. R., Caldas, N. J., et al. 2005. Viscosity of
because of their high ability to reduce the IFT. However, it could Water-in-Oil Emulsions: Variation with Temperature and Water Vol-
be more useful to use the nanoparticles SiO2 and Al2O3 in low ume Fraction. J. Pet. Sci. Eng. 48 (3–4): 169–184. http://dx.doi.org/
concentrations with FW of low salinity than with high salinity. 10.1016/j.petrol.2005.06.014.
On the other hand, the proposed mixed nanoparticles SiO2/Al2O3 Fletcher, A. J. P. and Davis, J. P. 2010. How EOR Can be Transformed by
at the optimum concentration of 0.05 wt% in low-salinity FW Nanotechnology. Presented at the SPE Improved Oil Recovery Sym-
incrementally enhance the recovery by 9.6% more than blank posium, Tulsa, Oklahoma, 24–28 April. SPE-129531-MS. http://
low-salinity water. Furthermore, highly promising results were dx.doi.org/10.2118/129531-MS.
obtained with the SiO2/Al2O3 nanoparticles mixture with FW by Franco, A., Nassar, N., Ruiz, M., et al. 2013. Nanoparticles for Inhibition
enhancing the stability of asphaltene in the fluid, and delay in as- of Asphaltenes Damage: Adsorption Study and Displacement Test on
phaltene precipitation can be achieved. Porous Media. Energ. Fuel. 27 (6): 2899–2907. http://dx.doi.org/
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Acknowledgments Thin Oil Sand Reservoirs. J. Pet. Sci. Eng. 74 (3–4): 138–146. http://
The authors would like to appreciate the support received from dx.doi.org/10.1016/j.petrol.2010.09.003.
Kuwait University Research Grant No. GE 01/07. The authors Hamedi, S. and Babadagli. T. 2010. Effects of Nano-Sized Metals on
also acknowledge the support received from Research Grants Viscosity Reduction of Heavy Oil/Bitumen during Thermal Applica-
Nos. GS 01/01 and GS 01/05. The authors extend their apprecia- tions. Presented at the Canadian Unconventional Resources and
tion to Kuwait Institute of Scientific Research for assistance with International Petroleum Conference, Calgary, Alberta, Canada,
conducting of interfacial-tension tests. Thanks are also extended 19–21 October. SPE-137540-MS. http://dx.doi.org/10.2118/137540-
to Abdulhaq Abdullatif, Sony Ninan, and Raju Jose for their tech- MS.
nical and theoretical support. We appreciate Abdullah Alenezi for Haroun, M., Al-Hassan, S., Ansari, A., et al. 2012. Nano-EOR Process
his contribution to the study. for Abu Dhabi Carbonate Reservoirs. Presented at the Abu Dhabi
International Petroleum Conference and Exhibition, Abu Dhabi,
UAE, 11–14 November. SPE-162386-MS. http://dx.doi.org/10.2118/
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Investigation of HLP Nanofluid Potential to Enhance Oil Recovery: A
Mechanistic Approach. Presented at the SPE International Oilfield Nano- Osamah A. Alomair is an associate professor in the Petroleum
technology Conference and Exhibition, Noordwijk, The Netherlands, Engineering Department at Kuwait University. He has been
12–14 June. SPE-156642-MS. http://dx.doi.org/10.2118/156642-MS. with Kuwait University for more than 14 years. Alomair’s current
Vetter, O. J., Kandarpa, V., Stratton, M., et al. 1987. Particle invasion interests include enhanced oil recovery (EOR), application of
into porous medium and related injectivity problems. Presented at the nanotechnology, fluid behaviors, and asphaltene studies. He
holds a PhD degree in petroleum engineering from Colorado
SPE International Symposium on Oil Field Chemistry, San Antonio,
School of Mines.
Texas, 4–6 February. SPE-16255-MS. http://dx.doi.org/10.2118/
16255-MS. Khaled Matar is a graduate student from Kuwait University in
Wang, K., Liang, S. and Wang, C. 2009. Research of Improving Water 2014. He worked on this technical paper as an extension of
Injection Effect by Using Active SiO2 Nano-powder in the Low-Per- senior project when he was a senior student in the Petroleum
Engineering Department. Matar’s current interests include
meability Oilfield. Adv. Mater. Res. 92 (January): 207–212. http://
acidizing optimization, fracturing of unconventional reservoirs,
dx.doi.org/10.4028/www.scientific.net/AMR.92.207. and studies of nanotechnology. He holds a bachelor’s degree
Wasan, D. T. and Nikolov, A. D. 2003. Spreading of Nanofluids on Solids. in petroleum engineering from Kuwait University.
Nature 423 (8 May): 156–159. http://dx.doi.org/10.1038/nature01591.
Wasan, D., Nikolov, A. and Kondiparty, K. 2011. The Wetting and Yousef Alsaeed is a graduate student from Kuwait University in
2014. He worked on this technical paper as an extension of
Spreading of Nanofluids on Solids: Role of the Structural Disjoining
senior project when he was a senior student in the Petroleum
Pressure. Curr. Opin. Colloid In. 16 (4): 344–349. http://dx.doi.org/ Engineering Department. Alsaeed’s research interests are
10.1016/j.cocis.2011.02.001. nanotechnology and enhanced oil recovery using steam
Wittle, J. K., Hill, D. G. and Chilingar. G. V. 2008. Direct Current Electri- injection. He holds a bachelor’s degree in petroleum engi-
cal Enhanced Oil Recovery in Heavy-Oil Reservoirs to Improve Recov- neering from Kuwait University.

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