SPE-198666-MS

Enhanced Oil Recovery for Carbonate Oil Reservoir by Using

Nano-Surfactant:Part II

Ali K. Alhuraishawy, Iraqi Ministry of Oil; Ramzy S. Hamied and Hajir A. Hammood, University of technology;
Waleed Hussien AL-Bazzaz, Kuwait Institute for Scientific Research

Copyright 2019, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Gas & Oil Technology Showcase and Conference held in Dubai, UAE, 21 - 23 October 2019.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
Excellent attempts have been made worldwide to improve oil recovery. Nano technology features in EOR
have been the focus of attention over the past century. The introduction of nanotechnology began in the
late 1980s and was created to synthesize fresh nano-materials by rearranging atoms and molecules. Based
on the small partition size of NPs (1-100) nm, the optical, thermal, chemical and structural properties of
the nanomaterial differ completely from those shown by either its atoms or bulk materials. It is also clear
that surfactants contribute to the stability of nanoparticles and emulsions with the aim of reducing IFT and
changing rock wettability to water-wet.
The main objective of this study is to investigate the effects of nano particles and surfactant on improving
oil recovery in carbonate reservoirs. Two key parameters were examined: silica nano particles and silica
nano particles with Sodium Dodecyl sulfate (SDS) as an anionic surfactant. Finally, flooding test showed
that using 0.03wt% SiO2 with 0.158 wt% SDS can improve oil recovery by 15.1% and minimize residual
oil saturation to 25.6%. X-ray powder diffraction (XRD) and field emission scanning electron microscope
(FESEM) were also done for thin core samples and the results have been discussed.

Introduction
Despite the fact that millions of barrels are obtained daily from the petroleum fields, common petroleum
recovery techniques (primary or secondary) are capable of removing only about 40 percent of the total oil
in a reservoirs (Rosestolato, et al., 2019). Increased oil recovery (EOR) or tertiary recovery is the use of
several physical and chemical methods to enhance crude oil production (Cheraghian, et al., 2017). Chemical
methods are an alternative for overcoming limitations by using miscible floods. It is based on water injection
into the wellbore with chemicals of various natures. There are two aims to add these chemicals, first, to
achieve a reduction in the interface tension between crude oil and water, and second, to reduce the difference
in viscosity between crude oil and liquid displacement by increasing viscosity. In this type of flooding,
alkaline and polymers or surfactants are used (De Compostela, S., 2016). A lot of studies has been published
on the effects of NPs as additives in surfactant flooding. The use of NPs can change the surfactant properties
and thus increase the effect of surfactant solution on oil recovery operations (Sun, et al., 2017).
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Experiments of flooding on unconsolidated sandstone sand packs were carried out by (Zargartalebi, et al.,
2014) when they used silica nanoparticles in combination with anionic surfactant called Sodium Dodecyl
Sulfate (SDS) to explore the ability of these particles to improve oil recovery. The improvement of oil
recovery from surfactant / nanoparticles flooding was from (10.78 % to 20.41%).
Also, (Ahmadi and Shadizadeh, 2017) presented the application of a combination of hydrophilic nano-
silica and extracted surfactant from the leaves of Ziziphus spina-christi, for EOR process, carbonate core
samples were used, and nano-silica concentrations were (500,1000,2000) ppm. Results gained from this
study demonstrate that with increasing concentration of hydrophilic nano-silica in the surfactant solution,
surfactant concentration in the solution is 8 wt%, ultimate oil recovery increases from 81.08% to 83.45%
OOIP. Cheraghian, et al., (2017) used five spot glass micromodel to study the effects of Silica nanoparticles
(Si-NPs) in combination with sodium dodecyl sulfate (SDS) surfactant for enhanced oil recovery (EOR)
process, The results showed that Si-NPs/SDS solutions made a significant improvement to oil recovery
values up to 13%.
S, et al., (2017) used sandstone core plug to study the interfacial-Tension (IFT), contact angle by
using silica nanoparticles (NPs) and SDS surfactant. The results showed that the oil recovery for water
flooding, surfactant flooding, and optimum nano-solution flooding was around 53%, 73%, and 80%
respictevely. Then, (Abdel-Fattah, et al., 2017) a new class of surfactants (STRX-NS) has been created for
enhanced oil recovery (EOR) applications in the form of dispersions of petroleum sulfonate nanoparticles in
seawater. These NanoSuractants (NS) are particles of 10-60 nm. The results of flooding process showed an
incremental oil recovery of 7% beyond water flooding. Also, (Arab, et al., 2018) used silica NPs and anionic
surfactants (sodium alkane sulfonate) to enhance the efficiency of heavy oil. Chemical floods showed that
silica NP with surfactant yielded an incremental oil recovery of 48 % OOIP, which is remarkably higher
than that of either surfactant or NP floods with incremental recoveries of 16 and 36 % OOIP, respectively.
Adeniyi and Olafuyi, (2018) fount that an improvement of additional 10% of OOIP was obtained by used
a new silicate based surfactant prepared from silicate with highest percentage of silica. (Pillai, P., 2019)
used grafted silica nanoparticle (LGS) and (Methyl ester sulfonate) surfactant to show their effect on Sand
pack flooding. The results showed a greater recovery in the presence of LGS with an additional recovery
of 24.6% which was much better the surfactant itself.
Rezk and Allam, (2019) explored the use of zinc oxide nanoparticles (ZnO NPs) to enhance an organic
liquid (n-dodecane) extraction from a porous medium (sandstone) based on surfactants. The results show
that the ZnO NPs / SDS flooding showed an 8% rise in oil recovery relative to standard SDS flooding.
Alhuraishawy et al. (2018a) study the combined ionically modified seawater and microgel to improve oil
recovery in carbonate reservoirs. They found that modified seawater improved the oil recovery factor when
used with gel treatment in fractured carbonate reservoirs. Alhuraishawy et al. (2018b) investigate the effect
of low salinity waterflooding on improve oil recovery in low permeability sandstone reservoir. They pointed
out that the low salinity waterflooding redistributes the flowing paths by releasing sand particles and some
fine minerals causing the flow path to narrow and; therefore, oil recovery factor improved. Pillai, et al.,
(2019) demonstrated whether the combination of surfactants (Methyl ester sulfonate), and silica grafted
lysine nanoparticles (LGS) could provide a more stable emulsion for EOR applications. The results showed
a higher recovery in the presence of LGS with an extra recovery of 24.6 % which was much better for
the surfactant itself. Hammood et al., (2019) (Part I of this study, SPE-198662-MS) measured the surface
tension, interfatial tension, and dynamic light scattering (DLS) tests for fluids in part I of this study to be
ready to use in this paper (Part II).

Experiments
Materials. Two types of brine (formation water and low salinity water) were used in this study (Table 1).
Synthetic formation water with (1.148) gr/cc density was used to saturate the core sample initially while low
SPE-198666-MS 3

salinity water containing nano silica provided by (US Research Nanomaterial's, Inc.) [Porous type, general
properties are listed in Table 2] and Sodium Dodecylsulfate [SDS, Mol.wt= 288.38 g.mol-1] was used as
anionic surfactant (Fig.1) which used to flooding test. A light crude oil was used with the properties as in
(Table 1). Four plugs from a carbonate oil reservoir in the west of Iran/Sarvak formation were used in this
study. The blocks were primarily composed of limestone carbonate.

Table 1—The composition and properties of used crude

Table 2—Brine compositions used in the experiments.

Table 3—Properties of SiO2 nanoparticles

Figure 1—Structure of Sodium Dodecylsulfate surfactants (SDS) (Al-Ansari et al., 2017).

4 SPE-198666-MS

Fluids Formulation. DI- water was used to prepare brine, injection fluid wich include surfactant and
nano particles. SiO2 concentration range based on the result of dynamic light scattering (DLS) method,
while CMC value of SDS based on surface tension test. Nine injection fluid prepared, 500ppm NaCl brine,
brine 500ppm NaCl with (0.01, 0.03, 0.05, 0.08) wt% of SiO2 respectively, and brine 500ppm NaCl with
(0.01, 0.03, 0.05, 0.08) wt % of SiO2 respectively with SDS surfactant. To prepare the surfactant solution
according to (S, et al., 2017), the surfactant was placed in the brine using the magnetic stirrer for 30 minutes.
After that, nanoparticles were added and stirred to prepare the nano-surfactant solution. Nanoparticles were
then dispersed with the ultrasonic device in the solution for more 30 minutes.
Core preparation. Four plugs were cut, cleaned by using standard soxhlet method (with toluene and
methanol solvents) for two weeks to remove any contamination, and subsequently dried in a conventional
oven at temperature (80°C) for 24 hours. Porosity and permeability were measured for core samples, the
cores dimensions and properties are summarized in Table (4). Also, Nine thin sections (slabs) were cut
from core plugs in cylindrical slices with less than two-millimeter thickness which used for Contact angle
measurement as in the first part of this study, cleaned by using standard soxhlet method (with toluene and
methanol solvents) for two weeks to remove any contamination, and subsequently dried in a conventional
oven at temperature (80°C) for 24 hours. This thin section used for (SEM) and (FESEM) tests.

Table 4—Cores dimensions and properties used in this study

Establishing Swi and Soi by Centrifuge. Four saturated plug samples with synthetic formation water
were placed in a core centrifuge. The water was replaced by cyclohexane (colored by Sudan red to
distinguish from water) at ambient temperature and 9,000 rpm for 12 hours. Then, water extracted from this
process was collected in graduated cylinders to calculate Swi and Soi as seen in (Fig.2)

Figure 2—colored cyclohexane and formation water separation in graduated cylinders.

Dynamic Aging in Core-holder. Four plug samples were placed in vertical core-holder, filtered crude oil
was injected through them to displace cyclohexane at 70 °C and 1000 psi confining pressure. Dynamic aging
SPE-198666-MS 5

was done by low rate injection (0.025 cc/min) of crude oil for three days, crude oil was filtered in a vertically
setup at 70 °C by using 7 and 2 microns’ steel filters prior to core flood in order to avoid core damage.

Core-flooding Experiments Procedure.

Four aged plug samples in crude oil were placed in horizontal core-holder (as in Fig.3) separately to do
water, Nano, and surfactant flooding tests consecutively. Twelve injection cycles were done at ambient
temperature, no back pressure, and 1000 psi confining pressure. Injection flow rate was constant (0.07) cc/
min for each plug sample which is near to typical reservoir fluid velocity (1-2 ft/day), according to (Brodie
and Jerauld, 2014), (Mahani, st al., 2011) and (Zang and Sarma, 2012). Injection of each fluid (water,
Nano, surfactant) was continued two pore volume or until no oil was produced from plug sample. (Table
5) explained the procedure for core flooding tests:

Figure 3—Plug flooding apparatus

Table 5—the procedure for core flooding tests

After finishing flooding tests, oil recovery factoran and differential pressure results were calculated and
plotted against injected pore volume.

(XRD) and (FESEM) tests

X-ray powder diffraction (XRD) and field emission scanning electron microscope (FESEM) tests were done
for nine thin sections after contact angel measuring in the first section of this study (SPE-198662-MS).
XRD was taken for the carbonate limestone samples before and after aging slabs with different SiO2/SDS
concentrations fluids to find the compositional analysis for samples and FESEM was used to investigate
6 SPE-198666-MS

the migration of fine mineral particles in order to explain the effect of nano silica /SDS on carbonate core
samples that had aged by different SiO2 concentrations.

Results and Discussions

Flooding test results
Figures (6 to 9) illustrates the effect of 500ppm brine, nano-silica, and SDS surfactant on the oil recovery
factor for four plugs during three injection cycles by measuring produced oil volume. For all plugs as in these
figures and (Table 6), the results show that nano silica flooding resulted in increasing oil recovery factor
from(47.3 % to 59.8), (47.6 % to 62.7), (43.9% to 55.6), (41 % to 52.6) and the displacement efficiency(ED)
improved to (23.7%, 28.8%, 20.9%, 19.6%) for plugs (1, 2, 3, 4) respectively. The reason behind this is that
nano-silica has the ability to reduce the interfacial tension between oil and brine, decrease the contact angle
that leads to change the wettability of plugs towards water wettability, as well as increasing the viscosity of
solution that lead to reduced mobility ratio between brine and oil.

Figure 6—Oil recovery performance for core No.(1)

Figure 7—Oil recovery performance for core No.(2)

SPE-198666-MS 7

Figure 8—Oil recovery performance for core No.(3)

Figure 9—Oil recovery performance for core No.(4)

8 SPE-198666-MS

Table 6—Oil recovery factor results

Furthermore, adding 0.158 wt% of SDS surfactant to nano silica can increase the ultimate recovery up
to by (66.8%, 68.4%, 61.4%, 60.2%) and (ED) improved by (17.5%, 15.3%, 13.2%, 16%) for plugs (1,
2, 3, 4) respectively. That is because the SDS/Si-NPs solution reduces the IFT between the oil and brine
more than using NP alone and could change the reservoir rock wettability to be water-wet (Hammood et al.,
2019). Also, SDS/Si-NPs solution form more uniform sweeping during the injection and reduces fingering
that lead to improved displacement efficiency.
As seen in Figures (10 and 11), 0.03wt% nano silica shows the maximum recovery factor up to 62.7%
with an improvement of 15.1% and the mixture of 0.03 wt % nano silica and SDS shows the maximum
recovery factor up to 68.4 % with an improvement of 5.7%. Also, the same behavior is shown in (Fig.12)
when 0.03 wt% silica gives the minimum residual oil saturation from 42.5 % down to 25.6 %. In the sense,
0.03 wt% NP gives a better recovery than 0.05 wt% and 0.08 wt%, from this result we conclude that it
does not necessarily increase the concentration of silica in order to obtain maximum production. The reason
beyond that may be the high concentration of NP has the ability to block the pore throats and prevent oil
flooding through porous media.
SPE-198666-MS 9

Figure 10—Ultimate oil recovery comparison for all plugs

Figure 11—Improved oil recoveryfor all plugs.

Figure 12—Residual oil saturation for all plugs.

The results of oil recovery are close to researches as (Li, et al., 2013) which found that the oil recovery
increased from (61.7% to 67.02%) when 0.05 wt % of SiO2 was injected. Also, Jiang and Li, (2017) found
that 10% oil recovery improved when Sio2 injected with the brine. Finally, Abdel-Fattah et al., (2017) found
10 SPE-198666-MS

an incremental oil recovery of 7% by beyond water flooding by injecting nano-surfactant at a concentration

of 0.2 wt%.

Differential pressure results

For all plugs, results show that differential pressure increases in the case of brine flooding. At the instance of
brine breakthrough, differential pressure goes down and becomes stable. All plugs have a breakthrough time
before 0.5 PV injected, and then differential pressure stabilization means than the properties of plugs remains
as it and no core damage accrue because of nano- surfactant flooding. This is why silica concentrations have
been tested by DLS test and ignored the unstable concentrations to preserve the properties of the rock from
damaging. Differential pressure results in (Fig. 13) and (Table 7).
SPE-198666-MS 11

Table 7—Breakthrough time and Average stabilized pressure for plugs

Figure 13—Differential pressure results and breakthrough time

(XRD) and (FESEM) results

XRD figures (14 to 19) and table (8) shows that the compositional analysis for the original core sample after
cleaning and shows that the highest peak that was observed at 29.295° which mean that the rock sample
was composed of pure calcite (100%). And this analysis is consistent with (Horeh et al., 2018) when they
found that the XRD analysis of carbonate core was 100% calcite. And the XRD analysis after aging core
samples with different brines shows that the mineral quantitative remains 100 % Calcite and that means
there is no core damage and there is no silica deposition on the pores of the core sample and these results
consistent with injection pressure profiles.
12 SPE-198666-MS

Table 8—XRD results

Figure 14—Original XRD result for reservoir rock core sample (1),
(the red line is pure calcite, and the black line is the rock sample).

Figure 15—XRD result for core sample No.(2).

SPE-198666-MS 13

Figure 16—XRD result for core sample No.(3).

Figure 17—XRD result for core sample No.(4).

Figure 18—XRD result for core sample No.(5).

14 SPE-198666-MS

Figure 19—FESEM results (3 nm scale)when (a) original core sample, (b) core sample aged with
0.01 wt% SiO2, (c) core sample aged with 0.03 wt% SiO2, and (d) core sample aged with 0.03 wt
% SiO2 +SDS, (e) core sample aged with 0.05 wt% SiO2, and (f) core sample aged with 0.08 wt% SiO2.

(FESEM) was used to investigate the migration of fine mineral particles in order to explain the effect of
nano silica /SDS on carbonate core samples that had aged by different SiO2 concentrations, (a) original core
sample, (b) core sample aged with 0.01 wt% SiO2, (c) core sample aged with 0.03 wt% SiO2, and (d) core
sample aged with 0.03 wt% SiO2 + SDS, (e) core sample aged with 0.05 wt% SiO2, and (f) core sample aged
with 0.08 wt% SiO2 As shown in Fig.(24). SEM images assure that SiO2 nanoparticles coating the surface
SPE-198666-MS 15

of rock and distribution homogeneously and that lead to change the plug wettability towards water. Also,
FESEM shows that there is no SDS adsorption because surfactant adsorption on the surface of plugs reduces
in the presence of silica nanoparticle. FESEM results are close to the authors' conclusion (Cheraghian and
Hendraningrat, 2016) and (Al-Ansari, et al., 2017).

Conclusions
A series of tests were performed to select the best EOR technique in the presence of nanoparticles and
surfactants as in the first part of this study. Core flooding results showed the following conclusions:

• The ultimate recovery of 0.03 wt% nano-silica and the 0.158 wt% surfactant is about 68.4% OOIP,
and this value shows a significant change from 62.7 % OOIP when using 0.03 wt% nano silica only.
• Nano-silica/surfactant combination can reduce IFT, improve rock wettability, and increase in the
viscosity of the solution and then a reduced mobility ratio between the solution and crude are
reasons for improving oil recovery factor.
• The optimum concentration of nanoparticle injection for carbonate cores was approximately 0.03
wt%. Nanoparticles' deposition on pore walls of porous media could lead to a wettability alternation
toward water-wet and improve oil recovery, whereas at higher concentration it has a tendency to
block pore throats.
• XRD and FESEM results showes the efficiency of nano- surfactant on core samples without core
damaging and negative effect on their composition.

Acknowledgment
The authors would like to thank Petroleum Department /University of technology and Petroleum Institute/
University of Tehran for their support. Also, the authors would like to express their appreciation to Petro
Vision Pasargad (PVP) Company in Tehran/Iran to provide opportunities to carry out flooding tests. Last
but not the least, a sincere thanks to Dr. Negahdar Hosseinpour and Dr. Bahaloo horeh /University of Tehran
for their great support to carry out all the experiments needed.

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