Colloids and Surfaces A 598 (2020) 124833

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Colloids and Surfaces A

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

Mechanistic study on silica nanoparticles-assisted guar gum polymer T

flooding for enhanced oil recovery in sandstone reservoirs
Achinta Bera*, Subhash Shah, Maunish Shah, Jatin Agarwal, Rakesh Kumar Vij
Drilling, Cementing, and Stimulation Research Center, School of Petroleum Technology, Pandit Deendayal Petroleum University, Raisan, Gandhinagar, 382007, Gujarat,
India

GRAPHICAL ABSTRACT

⁎
Corresponding author.
E-mail address: achinta.bera@spt.pdpu.ac.in (A. Bera).

https://doi.org/10.1016/j.colsurfa.2020.124833
Received 5 December 2019; Received in revised form 11 March 2020; Accepted 6 April 2020
Available online 17 April 2020
0927-7757/ © 2020 Elsevier B.V. All rights reserved.
A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

ARTICLE INFO ABSTRACT

Keywords: Nanoparticles-assisted polymer flooding has attracted the attention of researchers for its enhanced rheological
Silica nanoparticles properties and stability of the chemical slugs. The present work deals with the rheological properties of guar gum
Guar gum with and without silica nanoparticles in the temperature range from 25 °C to 75 °C. It is found that the viscosity
Polymer flooding of guar gum solution increases significantly with increasing concentration of silica nanoparticles. Imbibition
Enhanced oil recovery
experiments were performed with waxy crude oil-saturated sandstone cores using 2000 ppm brine, 4000 ppm
Imbibition
guar gum solution, 0.2 wt% silica nanoparticles in distilled water, and 4000 ppm guar gum containing 0.2 wt%
Phase behaviour
silica nanoparticles as test fluids for understanding the mechanism of wettability alteration in the presence of
silica nanoparticles and guar gum. Mixture of 0.2 wt% silica nanoparticles and 4000 ppm guar gum shows higher
oil recovery (∼36 % original oil-in-place) compared to other test solutions in imbibition experiments. Contact
angles between crude oil and sandstone rock were measured in presence of 2000 ppm brine, 0.025 wt% silica
nanoparticles in water, and guar gum (2000 ppm)-silica nanoparticles (0.025 wt%) mixture. Guar gum con-
taining silica nanoparticles are effective in changing the contact angle towards water-wet state (Contact angle
∼115°) from oil-wet state (contact angle ∼72°). No significant phase change is observed during the phase
behavior experiment except for light emulsion formation. Finally, core flooding experiments were conducted
with guar gum, silica nanoparticles solution, and mixture of silica nanoparticles and guar gum for additional oil
recovery to verify the effectiveness of the chemical slugs. Results showed that the addition of silica nanoparticles
to guar gum solution improves the effectiveness of guar gum polymer by recovering 44.3 % of original oil-in-
place. A comparative study was also conducted to show the performance of silica nanoparticles-assisted guar
gum solution for additional oil recovery. Most of the research works have focused on the application of silica
nanoparticles-induced polyacrylamide and xanthan gum chemical slugs in enhanced oil recovery. However,
laboratory study based on the application of silica nanoparticles-induced guar gum solution in additional oil
recovery adds some interesting findings to the literature compared to the existing information.

1. Introduction efficiency of the process. To improve the stability and viscosity of

Most oil reservoirs have reached matured stage with a decline rate
of oil production. Discovery of new oil reserves does not meet the re-
quirement significantly of increasing energy demand. Therefore, the oil
industries are attentive to the enhanced oil recovery (EOR) techniques
to extract the remaining trapped oil after primary and secondary re-
covery. Novel advanced EOR methods are required to develop for
supplying crude oil to mitigate the growing energy demand of the
twenty first century that is increasing every day. Based on the reservoir
properties, new EOR methods can be developed to extract the trapped
oil from the reservoir. Polymer flooding is one of the EOR techniques
where sweep efficiency of the EOR process by injected fluid can be
improved to recover crude oil from the reservoir. Generally, partially
hydrolysed polyacrylamide (PHPA) and Xanthan gum are used in
polymer flooding. But they are not always active to recover oil under
certain reservoir conditions. High reservoir heterogeneity and mobility
of displacing fluid can lead to viscous fingering and that can sig-
nificantly reduce the oil recovery. Polymers are considered as effective
materials to enhance the viscosity of water. They are added to a desired
concentration and the resultant viscous polymer solution is used as a
suitable displacing fluid. It reduces the mobility ratio and hence, im-
proving the sweep efficiency.
The commonly used polymers in the industry such as PHPA and
Xanthan gum are not stable at high temperature and high salinity.
Generally, PHPA is widely used due to its common commercial prospect
in the oil industry. Numerous studies on polymer flooding for EOR exist
in the literature [1–6]. Polymer properties have been modified by ad-
ditives to improve their effectiveness and stability during polymer
flooding. Surfactant-polymer blend is used to recover additional oil by
reducing the interfacial tension between oil and water and increasing
the viscosity of injected fluid [7–9]. On the other hand, alkali-polymer
blend is used to change the wettability and reduce the interfacial ten-
sion between oil and water by formation of in-situ surfactant by alkali-
crude oil reaction and the polymer increases viscosity of the injected
fluid [10–12]. However, alkali-surfactant-polymer blend is often in-
vestigated in laboratory for the effectiveness of chemical slug in EOR
[13–16]. Polymer flooding alone can be used to improve sweep
polymer and to reduce adsorption of polymer onto rock surface, na-
noparticles could play a vital role to increase the process efficiency. In
this regard, nanotechnology plays an energetic role in advancing the
chemical and thermal EOR methods [17–22].
Recently, nanoparticles-aided polymer flooding has gained the at-
tention of researchers in the field of chemical EOR. To identify the ef-
fectiveness of nanoparticles, Maurya and Mandal [23] studied the ap-
plication of nanoparticles-induced polymer suspension in EOR. They
used silica as nanoparticles and polyacrylamide as a polymer for pre-
paration of nano-polymer suspension. The results showed silica nano-
particles-induced polyacrylamide exhibited higher viscosity than poly-
acrylamide solution alone. For the development of nanoparticles-
induced polymer flooding study, Corredor et al. [24] studied the ap-
plication of surface-modified nanoparticles in polymer flooding for
improvement of the performance of polymer in oil recovery. They used
PHPA and Xanthan gum as polymers. It is reported that the addition of
1 and 2 wt% silica nanoparticles with PHPA and Xanthan gum exhibits
favourable mobility ratio and improves areal sweep efficiency. The
capillary number of flooding process was also increased by using silica
nanoparticles. However, PHPA and Xanthan gum are not suitable
polymers for application in EOR under harsh reservoir conditions such
as high salinity (100,000 ppm), high temperature (120 °C) and high
shear forces which can degrade the polymer network structure causing
a low EOR performance [25–28]. Gbadamosi et al. [29] also studied the
application of aluminium oxide nanoparticles with polyacrylamide for
additional oil recovery. They reported that addition of aluminium oxide
nanoparticles increased the efficiency of polymer and showed higher oil
recovery. Application of nanoparticles-aided polymer flooding is now
researched in laboratory to improve properties of the injected polymer
solution.
Most of the nanoparticles-induced polymer (PHPA and Xanthan
gum) flooding laboratory experiments have focused on the rheological
properties improvement, phase behaviour of produced emulsion, hy-
drodynamic radius measurement and core displacement for additional
oil recovery [30,31]. Recently, Druetta and Picchioni [32] studied the
simulation of nanoparticles-induced chemical EOR focusing on polymer
flooding. It is reported that nanoparticles-aided polymer flooding can

2
A. Bera, et al.
recover 40–45 % OOIP based on the reservoir properties. They also
stated that nanotechnology-enhanced polymer flooding could improve
oil recovery significantly based on the synergistic effect of polymer and
nanoparticles on oil displacement efficiency [33].
Imbibition test can provide a precise understanding of the me-
chanism of nanoparticles-induced polymer flooding for spontaneous oil
recovery. Oil recovery by surfactant solution by imbibition tests is very
well known to understand the associated mechanism of the process
[34–36]. To the best of our knowledge, laboratory experiments with
polymer solution containing silica nanoparticles have not been per-
formed to understand the oil displacement mechanism by spontaneous
imbibition. Nanoparticles alter the wettability of rock samples by ad-
sorption at the crude oil-rock interface through changing disjoining
pressure [37–39]. Therefore, the nanoparticles-induced polymer solu-
tion can alter the wettability of reservoir rock during core flooding.
Generally, when surface active agents are present in the oil-water
mixture, they change the phase behavior. In presence of proper driving
force, it is seen that nanoparticles can also form different phases based
upon the crude oil property [39–41]. Therefore, it is imperative to in-
vestigate the phase behavior of crude oil and nanosuspension in pre-
sence of polymer.
In purview of the current scenario of available literature on the
application of nanoparticles-induced polymer flooding for additional oil
recovery in laboratory scale, it is appropriate time to focus on the
systematic work flow on this research topic to establish a way to screen
the chemical slugs for their utilization in EOR techniques. As most past
studies have focused on PHPA and Xanthan gum, guar gum is selected
in this work to verify its effectiveness in oil recovery. Silica nano-
particles-induced guar gum application with a systematic work will be a
new addition to the literature and can document a novel comparative
work in the field of nanoparticles application in polymer flooding. The
novelty of work is the addition of phase behavior and imbibition ex-
periment with nanoparticles-induced guar gum a chemical slug which is
missing in the literature. The work is also important in that the con-
centration of polymer should be chosen based on the molecular weight
of the polymer as molecular weight is related to the viscosity of
polymer. A high concentration has been selected for core flooding ex-
periment for guar gum as its molecular weight is low and high con-
centration can achieve the higher viscosity for displacement of waxy
viscous crude oil.
In the present study, the effectiveness of silica nanoparticles-in-
duced guar gum solution has been tested for additional oil recovery at a
laboratory scale. The mechanistic study was conducted on imbibition
experiment using silica nanoparticles and guar gum polymer solution.
Contact angle measurements were performed to study the wettability
alteration. Phase behavior of silica nanoparticles/guar gum/crude oil/
brine solution was performed to investigate the participation of silica
nanoparticles for the formation of emulsion in presence of guar gum.
Finally, core displacement experiments were conducted with different
concentration of silica nanoparticles and guar gum to identify the op-
timum slug for additional oil recovery.
2. Experimental
2.1. Materials used
Guar gum (95 % purity) was purchased from a local supplier in
Ahmedabad, India and hydrophilic silica nanoparticles with 99.99 %
purity (size: 5−15 nm) was procured from Sigma Aldrich, Germany.
Crude oil was collected from GSPC (Gujarat State Petroleum
Corporation) oil field, India. Sandstone core samples used were col-
lected from Himmatnagar, India. NaCl (98 % purity) was supplied by
Merck, Mumbai, India. Deionized water was used for the preparation of
solutions.
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Colloids and Surfaces A 598 (2020) 124833
2.2. Methods
2.2.1. Characterization of crude oil
The crude oil samples from GSPC were characterized by measuring
their viscosity at different temperatures, density, API gravity, and water
content. The Anton Paar Rheometer was used to measure crude oil
viscosity as a function of temperature. The density of crude oil was
measured by pycnometer and API gravity was calculated. The water
content of crude oil was measured by centrifuge method after taking a
measured amount of crude oil in a plastic tube and centrifuged at 4000
rpm for 4 h. The settled water at the bottom of the tube after centrifuge
provided the water content of crude oil.
2.2.2. Core analysis
The core samples were 1.5 inch diameter and 3.5 inch long. The
porosity of core samples was measured by saturation method. The in-
itial weight of the core was recorded first and then placed in a beaker
filled with water. After 2 h, the weight of core was again recorded to
obtain the weight change. The change in weight divided by density of
water provided the volume of water occupied in the pore spaces. The
bulk volume of core was determined from the length and diameter of
core. The porosity was then calculated by dividing the pore volume by
bulk volume. Permeability of each core sample was measured by core
flooding with water and using the Darcy’s equation as shown in Eq. (1).
The mineralogical composition of core samples was determined by X-
ray diffractogram (XRD) study. The sample was cleaned and dried
properly before the XRD analysis. The Bragg’s law (nλ = 2d sin θ;
where n is an integer, λ is the wave length of X-ray, d is the spacing of
the crystal layer, and θ is the incident angle) was used to generate XRD
data by the interaction of incident rays with the sample by constructive
interference. This law relates the wavelength of electromagnetic ra-
diation to the diffraction angle and the lattice spacing in a crystalline
sample.
2.2.3. Measurement of rheological properties of polymer-nanoparticle
suspensions
Suspensions were prepared by adding various concentrations of
nanoparticles in distilled water and stirring the solution for 4 h. Then
guar gum powder was added to it to prepare the nanoparticles-induced
polymer solution and stirred again for 2 h. Guar gum solutions at dif-
ferent concentration were also prepared separately and using Anton
Paar Rheometer their viscosities were measured in the shear rate from 1
s−1 to 100 s−1 and temperature range from 30 to 80 °C. A small amount
of prepared chemical slug (2−3 ml) was placed on the plate and using
cone and plate geometry of the instrument, the rheological measure-
ments were made. The data generated during the experiment was
stored as excel file in the computer.
In the present study different concentrations were chosen to see the
effect of concentration on rheology. A low concentration 2000 ppm and
a high concentration 8000 ppm were chosen to understand the effect of
concentration on viscosity of guar gum polymer. The target viscosity
was below 1000 cP for core displacement study which was found in
case of 4000 ppm guar gum.
2.2.4. Imbibition experiment
Imbibition experiment was conducted to investigate the sponta-
neous displacement of oil by different test fluids at elevated pressure
and temperature. A specially designed imbibition cell as shown in Fig. 1
was used for the experiment. A saturated core sample (1.5 inch OD and
3.5 inch long) was placed inside the imbibition cell. The core was sa-
turated by injecting crude oil into the core using an ISCO pump. A
minimum 3 pore volume of crude oil was passed through the core and it
was assumed that the core was fully saturated with crude after the
process. In this case the initial weight of core was recorded and after the
saturation the weight was taken to determine the amount of crude oil
present within the core. Thereafter, the cell was filled with a test
A. Bera, et al.
Fig. 1. Schematic of imbibition cell for spontaneous oil displacement study. A
core is placed inside the imbibition cell and oil is spontaneously displaced by
the test fluid.
solution and kept for several hours to visually observe the oil released
from the saturated core as test fluid imbibed into the core. The amount
of oil accumulated at the top of graduated tube of the imbibition cell
was recorded at various time intervals.
2.2.5. Wettability alteration study by contact angle measurement
Wettability alteration of rock samples was determined by specially
designed equipment after capturing time-lapsed photographs of each oil
drop beneath the rock sample. The corresponding contact angles were
measured by drawing the angle of contact of crude oil drop to rock
surface (Fig. 2). The wettability determination through contact angle
measurement depends on the experimental protocol. If a water drop is
place on beneath the rock surface which is immersed in oil then the
wettability of the rock surface is determined by the contact angle ranges
accordingly. The rock surface is said to be water-wet if the contact angle
is less than 90°, oil-wet if the contact angle is larger than 90°, and
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Colloids and Surfaces A 598 (2020) 124833
intermediate-wet if the contact angle is ∼90°. But if an oil drop is place
beneath a rock surface which is immersed in water/test fluid then with
increasing contact angle the wettability will be shifted towards water-
wet state. Therefore, contact angle lager than 90° is considered as
water-wet and the values of contact angle would be presented in the
opposite. In the present study, the oil drop was place beneath the rock
surface immersed in the test fluid as shown in Fig. 2.
2.2.6. Phase behaviour study
In order to study the participation of silica nanoparticles in phase
formation, phase behavior study was performed by using the test tube
shaking method. A 5 ml of each crude oil and test solution (1:1) was
taken in a test tube and vigorously shaken for 30 min and kept it for 12
h to attain equilibrium. The phase volumes were visually measured as
they appeared after equilibrium. The effect of temperature in the range
from 30 to 80 °C was also studied by keeping the samples for 30 min at
a given temperature after shaking for 30 min. The phase volumes were
then measured for phase behavior study.
2.2.7. Core displacement study
The core flooding setup shown in Fig. 3 was used to conduct ex-
periments for determination of additional oil recovery by using the
prepared nanoparticles solution, guar gum polymer solution, and na-
noparticles-induced polymer solutions. The setup consists of Isco syr-
inge pump, core holder, an effluent collector with balance and five
cylinders for storing brine solution, nanoparticles suspension, polymer
slug, nanoparticles-induced polymer slug, and crude oil. The pore vo-
lume (PV) of core sample was determined by weighing method. Weight
of dry core was recorded and after immersing it in water the weight was
again taken. The change in weight is the amount of water soaked by
core. The volume of water was calculated by dividing the weight by
water density. This volume represents the PV of core and it was found
to be 13.95 ml. The full core displacement setup was monitored by
computational pressure maintenance unit.
Steps listed below were followed during the core displacement study
as discussed by Pal et al. [42]:
Step 1: Initially the brine solution was injected for 3 h at a constant
flow rate of 1 ml/min through the core sample maintained under
Fig. 2. Wettability alteration study by contact angle measurement method.
A crude oil drop is placed beneath the slice of rock sample which is im-
mersed in the test fluid and photographs are taken by a digital camera at
different time intervals to observe the change in contact angle. From the
contact angle values, wettability of rock sample is determined.
A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

Fig. 3. Setup for core displacement study for oil recovery. A crude oil saturated core is placed in the core holder and confining and back pressures are set to run the
experiment. Initially water flooding is conducted to measure the oil recovery and then different chemical slugs are injected to analyse the performance of chemical
slugs followed by chase water flooding to maintain the initial condition of core.

Table 1 overburden pressure of 300 psi and the permeability of core to water
Properties of sandstone core and crude oil used in experiments. (kw) was calculated from the data.
Rock Type Sandstone
Step 2: Once the core was saturated with brine, crude oil of 6 Pa.s
Porosity 15−17% viscosity at 30 °C @ 10 s−1shear rate was injected at a constant flow
Permeability 200−205 mD rate of 1 ml/min through the core and 300 psi of pressure for 3 h to
Density of oil (g/cc) at 25 °C 0.828 calculate the connate water saturation (Swc) and original oil in place
Stock Tank Oil density (g/cc) 0.873
(OOIP), (Soi).
API gravity of oil at 25 °C 39.57
Viscosity at 30 °C @ shear rate 15 s−1 4.95 Pa.s Step 3: Six pore volumes (PV) of brine solution was then injected
Water content 6% into the core at a constant flow rate of 1 ml/min to displace oil from
core. This oil recovery process is known as conventional water flooding
(secondary oil recovery). The remaining trapped oil in the core is

Fig. 4. Crude oil viscosity as a function of shear rate at different temperatures. Viscosity of crude oil decreases with increasing temperature and shear rate.

5
A. Bera, et al.
Fig. 5. XRD of sandstone core sample used in experiment. XRD shows that the primary composition of sandstone core is silica and a trace amount of iron oxide and
alumina oxide are present.
Fig. 6. Viscosity of 2000 ppm guar gum solution at different temperatures.
known as residual oil saturation (Sor).
Step 4: With the purpose of additional oil recovery, guar gum so-
lution, nanoparticles suspension in water and nanoparticles-induced
polymer slug (3 PV in all cases) were injected into the core (tertiary oil
recovery process) at a constant flow rate of 1 ml/min. The liquid (oil
and water) recovered by the displacement process was collected in the
effluent collector. This oil recovery obtained by reducing the residual
oil saturation is known as EOR.
Final step: When more than 95 % water cut is reached, the chase
brine solution was injected to maintain the pressure and retain the in-
itial physicochemical properties of core sample, which results in con-
stant oil recovery. The whole core displacement study was conducted at
a temperature of 50 °C as the crude oil is viscous and waxy in nature.
The flow ability of the crude oil was found at 50 °C and therefore, the
experiment can be performed properly.
The permeability of core sample was measured by the following
Darcy equation [43].
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Colloids and Surfaces A 598 (2020) 124833
kA dp
q=
µ dx (1)
where q is the volumetric flow rate (cm3/sec), A is the cross-sectional
area of core sample (cm2), μ is the fluid viscosity (cP), (dp/dx) is the
pressure gradient (atm/cm) and k is the permeability in Darcy.
The polymer and nanoparticles concentrations were selected based on
the previous work available in literature and properties of the silica na-
noparticles and guar gum. The nanoparticles concentration (0.2 wt%) used
for core displacement study is really low enough. However, the polymer
concentration is high as the molecular weight of guar gum is low. Different
concentrations of guar gum were selected and the effect of concentration
on rheology is tested. The desired concentration (4000 ppm) to achieve
targeted viscosity is chosen for oil recovery experiment. The concentration
is suitable for this study based on the permeability of the sandstone core
used in this experiment. Also the selected crude has high viscosity and
high wax content. Therefore, the high concentration of selected polymer is
important to displace the crude in the core sample.
A. Bera, et al.
Fig. 7. Viscosity of 4000 ppm guar gum solution at different temperatures.
Fig. 8. Viscosity of 6000 ppm guar gum solution at different temperatures.
3. Results and discussion
3.1. Rock and fluids properties
The conventional core analysis and fluid properties are shown in
Table 1. The mineralogical properties of core sample were determined
by XRD. Porosity and permeability of rock samples were found to be in
the range of 15−17% and 200−205 mD respectively. Fig. 4 shows the
viscosity of crude oil as a function of temperature. With increasing
temperature and shear rate, viscosity of crude oil decreases as expected.
The crude oil exhibits highest viscosity at 30 °C and lowest shear rate.
The viscosity results indicate that due to wax content the crude is
showing high viscosity even though it is light oil based on API gravity.
The composition of core sample was determined by XRD. Fig. 5
shows the X-ray diffractogram of sandstone core sample. The pre-
dominant peak indicates the single-phase present in sample. The
characteristic peaks were found at 20.8°, 26.7°, 50.2°, and 59.9°. The
JCPDS file (file nos. 851460 and 861410) indicates that silica is the
main constituent of core sample. The main peak was obtained at 26.7°
which indicates the presence of silica in sample. Peak at 20.8 also shows
the presence of amorphous silica which is main component of quartz.
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Colloids and Surfaces A 598 (2020) 124833
Another two peaks at 50.2 and 59.9 indicate the presence of small
amount of iron oxide and alumina oxide in the sample, respectively.
3.2. Effect of silica nanoparticles on rheological properties of guar gum
Effect of guar gum concentration on viscosity was studied at dif-
ferent temperatures. Guar gum concentration was varied from 2000
ppm to 8000 ppm. Guar gum solution showed a shear thinning behavior
over a wide range of temperatures from 25 °C to 75 °C. As expected, it
was found that the viscosity of guar gum solution increases with in-
creasing concentration and decreases with temperatures studied.
Furthermore, the viscosities of allguar gum solutions decreased with
increasing shear rate, suggesting non-Newtonian pseudoplastic beha-
vior of the aqueous solutions of guar polymer. This can be explained
based on the uncoiling and aligning of polymer chains upon exposure to
shear flow. Figs. 6–9 show the viscosity variation with shear rate at
different temperatures for 2000 ppm, 4000 ppm, 6000 ppm, and 8000
ppm guar gum solutions respectively. With increase in temperature, the
average speed of molecules in a liquid increases, so the time they spend
in contact with their nearest neighbors decreases. Thus, as temperature
increases, the average intermolecular forces decrease. Therefore, as the
A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

Fig. 9. Viscosity of 8000 ppm guar gum solution at different temperatures.

Fig. 10. Viscosity @ 2 s−1 shear rate of guar gum solution at different temperatures and concentrations.

Fig. 11. Viscosity @ 15 s−1 shear rate of 8000 ppm guar gum solution at different temperatures and silica nanoparticles concentrations.

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A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

Fig. 12. Spontaneous oil recovery in imbibition experiment by different test solutions: 2000 ppm brine, 4000 ppm guar gum solution, 0.2 wt% nano silica in water,
and mixture of 0.2 wt% nano silica and 4000 ppm guar gum solution.

Table 2
Properties of the rock and test fluids and additional oil recovery by spontaneous imbibition.
Experiment No. Porosity of core, Permeability (mD) Test fluid Initial water saturation, Initial oil saturation, Oil recovery, %
% % % OOIP

1 15.7 203 2000 ppm brine 19 81 7.19

2 16.2 200 0.2 wt% silica nanoparticles in water 20.1 80.9 28.77
3 16.1 202 4000 ppm guar gum solution 19.5 80.5 23.02
4 15.9 201 0.2 wt% silica nanoparticles + 4000 ppm 18.8 81.2 35.97
guar gum solution

Fig. 13. Photos of imbibition cells during the oil recovery experiments for (a) 2000 ppm brine, (b) 4000 ppm guar gum solution, (c) mixture of 0.2 wt% nano silica
and 4000 ppm guar gum solution and (d) 0.2 wt% nano silica in water.

solution temperature increases, the viscosities of polymer solutions
decrease. With increasing shear rate the viscosity of guar gum solution
decreases at all temperatures. Fig. 10 shows 2 s−1 shear rate viscosity of
guar gum solution at different concentration and temperature.
To study the effect of silica nanoparticles on the rheology of guar
gum solution, the viscosity of guar gum solution containing silica na-
noparticles was performed at temperatures from 25 °C to 75 °C.
Concentrations of silica nanoparticles used were: 0, 0.05, 0.2, 0.3, and
1.0 wt%. These silica particle concentrations were mixed with 8000
ppm guar gum solution and viscosities were measured at different
temperatures. Fig. 11 shows the variation of viscosity (at 15 s−1 shear
rate) of 8000 ppm guar gum solution with different concentration of
silica nanoparticles. The viscosity of guar gum solution increases as the
silica nanoparticles concentration increases gradually. Addition of silica

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A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

Fig. 14. Contact angle variation with time in different test fluids and photos of oil drops on the rock samples.

Fig. 15. Schematic showing the adsorption of silica nanoparticles at the oil-water contact and disjoining pressure for wettability alteration (Modified from [45]).

Fig. 16. Phase behavior of crude oil and silica nanoparticles solution at different concentrations of 0.05, 0.1, 0.2, 0.3, 0.4, and 0.5 wt% (1:1 volume ratio). It can be
seen that emulsification takes place at low temperature and demulsification occurs at high temperature.

nanoparticles also increases the viscosity at high temperature which
can help guar gum solution to perform adequately in high-temperature
reservoirs. The high viscosity of guar gum solution associated with si-
lica nanoparticles even at high temperature is due to interlink bond
established between guar gum solution and silica nanoparticles and a
stable polymer slug is formed. Van der walls force is also responsible for
the higher viscosity and stability at high temperature.
3.3. Imbibition study
Imbibition study was conducted to investigate the oil released from
saturated cores spontaneously. Experiments were conducted with
sandstone samples in brine solution, nanoparticles suspension in water,
guar polymer solution, and nanoparticle-polymer solution. Fig. 12
shows the oil recovery as a function of time for four different test so-
lutions. Table 2 shows a summary of core properties and oil recovery

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A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

Fig. 17. Phase behavior of crude oil and mixture of silica nanoparticles and polymer solution at different concentrations from left to right 0.05 wt% silica +1000
ppm guar solution; 0.1 wt% silica +2000 ppm guar solution; 0.15 wt% silica +3000 ppm guar solution; 0.2 wt% silica +4000 ppm guar solution (1:1 volume ratio).
Emulsion formed at low temperature is broken down at high temperature.

Fig. 18. Oil recovery, water cut and pressure drop during 4000 ppm guar gum solution flooding. Initially 6 PV water then 3 PV guar gum solution followed by 3 PV
chase water were injected in core displacement study.

using different test fluids. Maximum oil was released in case of the
nanoparticles-polymer solution. The mechanism of oil recovery can be
attributed to the wettability alteration of core sample by nanoparticles
[44]. When nanoparticles and polymer solution was used, the amount
of oil released was higher due to the synergistic effect of nanoparticles
and polymer. Microscopic oil displacement phenomenon occurs during
imbibition of the test solution. When polymer and nanoparticles are
present in the solution counter-current flow of imbibed fluid and
drainage fluid occurs that increases oil recovery from the core sample.
A 0.2 wt% silica nanoparticle solution shows oil recovery of 28.77 %
OOIP while 4000 ppm guar gum solution mixed with 0.2 wt% silica
nanoparticles and 4000 ppm guar gum solution show 35.97 % and
23.02 % OOIP respectively. In the case of 2000 ppm brine solution, only
7.19 % of OOIP was recovered. Fig. 13 shows oil produced at the end of
imbibition experiments, i.e. after 180 h for all cases. From the results, it
can be seen that nanoparticles-polymer solution is an effective candi-
date to recover crude oil from sandstone rock via wettability alteration
from oil-wet state to water-wet state. Imbibition will be spontaneous
when the wettability of the rock sample changes to water-wet state. As
silica nanoparticles-guar gum solution promotes the wettability al-
teration from oil-wet to water-wet, the oil recovery in the imbibition
experiment was found to be higher than the other cases. Structural
disjoining pressure change in case of silica nanoparticles-guar gum
solution is higher compared to the other test fluids; therefore, in this
case more oil is recovered and also at a faster rate.
3.4. Wettability alteration
Wettability alteration of sandstone rock was determined from con-
tact angle measurements. A 0.2 wt% silica nanoparticle in water, a
mixture of 0.025 wt% nano-silica and 2000 ppm guar gum solution,
2000 ppm brine, and distilled water were used individually as test so-
lution for wettability alteration through contact angle measurement.
Fig. 14 shows the contact angle values for different test solutions with
corresponding photographs of the oil drops. Results indicate that the
mixture of nano-silica and polymer solution is effective to alter the oil-
wet rock to water-wet. Contact angle in distilled water was measured
and found to be 60°. The values of the contact angle remained the same

11
A. Bera, et al. Colloids and Surfaces A 598 (2020) 124833

Fig. 19. Oil recovery, water cut, and pressure drop during 4000 ppm guar gum solution containing 0.2 wt% silica nanoparticles flooding. Initially 6 PV water then 3
PV nano silica-guar gum mixture followed by 3 PV chase water were injected in core displacement study.

Fig. 20. Oil recovery, water cut, and pressure drop during 0.2 wt% silica nanoparticles solution flooding. Initially 6 PV water then 3 PV nano silica in water followed
by 3 PV chase water were injected in core displacement study.

with elapsed time. On the other hand, in case of 2000 ppm brine, a
small change in contact angle (65° to 90°) was observed which indicates
the less effectiveness of brine to alter the wettability of sandstone rock.
The wettability change may be attributed to in-situ formation of the
surface-active agent via weak ionic interaction of acidic components of
crude oil and salt. In case of 0.2 wt% nano-silica in water, the wett-
ability alteration was observed from oil-wet to water-wet changing
contact angle from 70° to 108°. Nanoparticles get adsorbed at the oil
and rock interface and change the disjoining pressure as shown in
Fig. 15. When silica nanoparticles (0.025 wt%) and guar gum polymer
(2000 ppm) mixture was used to investigate the wettability change of
sandstone rock it was observed that the mixture acts very pronounc-
edly. Contact angle value was changed from 73°to 115°, indicating the
wettability change from oil-wet to water-wet. As guar gum and nano-
silica are together, the effect on contact angle is highly active due to
easy adsorption of silica nanoparticles onto sandstone rock which helps
to alter wettability prominently.
However, the concentration of silica nanoparticles and guar gum
was changed for contact angle measurement with the mixture. It was
found that the test fluid prepared with more than the selected con-
centration (0.025 wt% nanosilica and 2000 ppm guar gum) became
fully turbid. Therefore, the oil drop from the outside cannot be seen and
the proper photograph could not be captured. Therefore, the con-
centration was reduced to 0.025 wt% for silica nanoparticles and 2000
ppm for guar gum to capture clear photographs of the crude oil drop.
The main objective of the study is to investigate the effect of silica
nanoparticles on wettability alteration of sandstone rock in presence of
guar gum solution.
3.5. Phase behavior study
Phase behavior study is very important to investigate the ability of
injected chemical slug to form an emulsion or microemulsion during oil
recovery. The optimum concentration of the chemical can be identified
from the phase behavior. Surface active agents mainly change the
phases and form different phases based on the concentration of che-
micals used and condition. Generally, on the variation of salinity from
low to a high concentration of injected slug, phase is changed from

12
A. Bera, et al.
Fig. 21. Comparison of oil recovery performances of 0.2 wt% nano silica solution, 4000 ppm guar gum solution, and 0.2 wt% nano silica and 4000 ppm guar gum
solution.
Winsor-I to Winsor-II through Winsor-III [46–48]. Phase behavior of
oil-water-injected chemical slug during additional oil recovery is very
significant to understand the formation of emulsion or microemulsion
which can attain ultra-low interfacial tension. Phase behavior of nano-
silica and polymer mixture-crude oil and silica nanoparticles-crude oil
at different concentrations of silica nanoparticles and a constant guar
gum polymer concentration were investigated at temperatures of 30 °C,
70 °C, and 80 °C. Fig. 16 shows the phase behavior of crude oil and
silica nanoparticles solutions at concentrations of 0.05, 0.1, 0.2, 0.3,
0.4, and 0.5 wt%. Although some amount of crude oil remains in
emulsion form at 30 °C, no significant emulsification was observed at
80 °C as demulsification occurs at high temperature. In most cases, with
increasing concentration of silica nanoparticles, emulsified crude oil
remains in water phase. In case of silica nanoparticles-guar gum
polymer mixture-crude oil, emulsion formation was also not observed
prominently in phase behavior and polymer did not participate in the
formation of an emulsion as shown in Fig. 17. Phase behavior of crude
oil and the mixture of silica nanoparticles and polymer solution at
different concentrations from left to right as 0.05 wt% silica +1000
ppm guar solution; 0.1 wt% silica +2000 ppm guar solution; 0.15 wt%
silica +3000 ppm guar solution; 0.2 wt% silica +4000 ppm guar so-
lution are depicted in Fig. 17. However, due to the presence of silica
nanoparticles in guar gum polymer light emulsification is formed but at
80 °C emulsions start to break through demulsification as shown in
Fig. 17. The phase behavior of waxy crude oil and the mixture of silica
nanoparticles and polymer solution is very complex. Proper design of
experiments with required concentration of nanoparticles solution for
phase behavior study is very crucial to produce a three-phase emulsion.
3.6. Oil recovery by silica nanoparticles and guar gum polymer slugs
Core displacement study was conducted using sandstone samples in
order to investigate the effectiveness of the chemical slugs of 4000 ppm
guar gum solution, 0.2 wt% nano-silica solution and silica nano-
particles-polymer mixture (4000 ppm guar gum solution +0.2 wt%
nano-silica) individually. Initially, water was injected up to 6 pore
volumes (PVs) to recover the crude oil by secondary mode until the
water cut reached above 90–95 %. Results showed that more than 45 %
of OOIP was recovered by water flooding. Water flooding was con-
ducted before any chemical flooding as secondary mode. As the ex-
perimental conditions and permeability and porosity of cores are almost
the same the reproducibility of results is observed in all cases. After
13
Colloids and Surfaces A 598 (2020) 124833
that, 3 PVs chemical slugs are injected for all cases to recover additional
oil in tertiary mode. Finally, 3 PVs chase brine was injected to retain the
core properties and no significant oil recovery was obtained by chase
water flooding. The oil recovery is suddenly increases as the chemical
injection starts. As the viscosity of the injected fluid is high due to guar
gum and silica nanoparticles, the sweep efficiency is increased and the
injected fluid can push more oil towards the production side. As silica
nanoparticles are present in the chemical slug, wettability alteration
also takes place and oil-wet rock is changed to water-wet which ac-
celerates the oil recovery. Therefore, a steady increase of oil recovery is
observed until the most trapped oil is recovered and water cut reached
to 95 %.
Usually in field operation, 1 PV of chemical slug is often considered
to recover additional oil after water flooding. During injection of che-
mical slug if oil is produced even after 1 PV then injection is continued
to reach water cut more than 90 %. However, in laboratory, as the pore
volume is small and after injecting 1 PV still additional oil was pro-
duced from the core and the injection was continued to 3 PV to reach
the water cut up to 95 %. Thereafter, chase water was injected to re-
cover the initial condition of core. Figs. 18–20 show the oil recovery,
water cut, and pressure drop by three different chemical slugs such as
guar gum solution (4000 ppm), silica nanoparticles solution (0.2 wt%
nano-silica) and silica nanoparticles-polymer solution (4000 ppm guar
gum +0.2 wt% nano-silica). With increasing the injected pore volume,
pressure drop also increases in all cases. For guar gum and nano silica-
guar gum mixture the pressure drop increases gradually due to viscosity
of polymer. In case of nano silica suspension, pressure drop initially
increases and at the time of chase water flooding pressure drop de-
creases and remains almost the same throughout the chase water
flooding. Fig. 21 depicts a comparison of additional oil recovery by the
three chemical slugs. Maximum oil recovery of 44.28 % OOIP was
obtained for silica nanoparticles and polymer mixture. Additional oil
recovery for guar gum solution and silica nanoparticles was 27.23 %
and 10.73 % OOIP. Maximum oil recovery for guar gum and nano-silica
mixture can be attributed to increased viscosity of the injected fluid as
well as wettability alteration of sandstone from intermediate wetting
state to water-wet state by silica nanoparticles present in the chemical
slug. Table 3 summaries core properties and additional oil recovery
obtained by different chemical slugs used during core displacement
study.
Usually, guar gum polymer solution can increase oil recovery by
improving sweep efficiency. Silica nanoparticles are also effective in
 Table 3
Results of core displacement study for different chemical slugs.
Experiment No. Porosity of core, Permeability (mD) Design of injection scheme Initial water saturation, Initial oil saturation, Residual oil saturation, Additional oil recovery, %
A. Bera, et al.

% % % % OOIP

1 16 204 6 PV water + 3 PV 4000 ppm guar solution + 3 PV chase water 19 81 7.19 27.23
2 16.2 205 6 PV water + 3 PV 0.2 wt% nano silica solution+ 3 PV chase water 19.5 80.5 23.02 10.73
3 16.3 204 6 PV water + 3 PV mixture of 0.2 wt% nano silica and 4000 ppm 20.1 80.9 35.97 44.28
guar solution + 3 PV chase water

14
Table 4
Comparison between previous works available in literature and present work.
Polymer and Concentration (ppm) Nanoparticles and Concentration Type of Rock Porosity (%) and Viscosity Change of Wettability Additional oil recovery, %OOIP Reference
(wt%) Permeability (mD) polymer solution Alteration

Hydrolyzed polyacrylamide and Silica and 0.5 Sandstone Not reported Yes Not reported 8.68 over polymer flooding [50]
800 (Micromodel)
Polyacrylamide and 1000−3000 Silica and 0.1−5.0 Glass micromodel 33 and 2.5 Yes Not reported 11.20 over polymer flooding [19]
Polyacrylamide and 1000 Silica and 1.5 Sandstone – Yes Yes 17.53 over polymer flooding [51]
Xanthan gum Silica and 0.3 Berea sandstone 25−26 and 750−1000 mD Yes Yes 11.00 over polymer flooding [52]
Polyacrylamide and 2500−5000 Silica and 0.2−1.0 Not reported Not reported Yes Not reported Not reported [23]
Hydrolyzed polyacrylamide Silica (0.1 wt%) and aluminium Sandstone 19.76 and 204 mD Yes Yes 10.00 (for Silica) and 15.00 (for [29]
oxide (0.1 wt%) aluminum oxide) over polymer flooding
Hydrolyzed polyacrylamide and Montmorillonite nanoparticles and Sandpack 23−26 and 294−311 Yes Not reported 13.00 over polymer flooding [53]
2000 0.25
Xanthan gum and 2500 ppm Nickel nanoparticle and 0.1 Sandpack 40−42 and not reported Yes Yes 6.00 over polymer flooding [54]
Guar gum and 2000−8000 ppm Silica and 0.025−1.0 Sandstone 15−17 and 200−205 Yes Yes 17.00 over polymer flooding Present study
Colloids and Surfaces A 598 (2020) 124833
A. Bera, et al.
improving oil recovery due to the unique nature of particle size (larger
surface area) increasing the viscosity of injected fluid as well as the
ability to change the wetting properties of core samples. Once guar gum
and nanoparticles are mixed, the improved viscous properties of pro-
duced chemical slug enhance oil recovery due to synergistic effect.
Other polymers such as polyacrylamide, hydrolysed polyacrylamide,
and xanthan gum are also used with silica nanoparticles for oil recovery
experiments [19,49,50]. The comparison indicates that silica nano-
particles-induced guar gum is effective to recover more than 44 % OOIP
while other polymers can extract only up to 30 % OOIP. Therefore,
experimental work on guar gum with silica nanoparticles should be
continued to optimize the concentration of both chemicals to recover
maximum oil.
However, a high concentration of guar gum polymer is selected for
core displacement study compared to other research investigations re-
ported in literature. Viscosity increases with molecular weight and
therefore, a low concentration is considered for high molecular weight
polymer. Guar gum has molecular weight 0.2 to 0.25 million Da
whereas Xanthan gum and polymacrylamide are having 2 million Da
and 9–11 million Da respectively. Therefore, higher concentration guar
gum solution is required to achieve the desired viscosity of the injected
fluid for waxy viscous crude oil. In the present work, relatively higher
concentration (4000 ppm) is selected for core displacement study to get
high viscosity of guar gum. During the core displacement study, pres-
sure drop was monitored. No anomalous behavior was found during
polymer injection. The viscosity of 4000 ppm guar gum is not too high
and thus, there was no problem in the injection of polymer during core
displacement study. This injectivity issue can be studied further by
injecting higher concentration of guar gum (say 8000 ppm) in core
flooding for additional oil recovery. However, a comparative study is
provided in Table 4 showing results of nanoparticles-induced polymer
flooding for additional oil recovery in the present and previous work.
4. Conclusions
A detailed investigation is conducted on silica nanoparticles-in-
duced guar gum polymer solution flooding for EOR. The primary focus
of this study was on viscosity modification of guar gum solution,
wettability alteration of rock sample, imbibition, phase behavior of
crude oil and nanofluids, and additional oil recovery by silica nano-
particles-aided guar gum solution. Addition of silica nanoparticles to
the guar gum solution increases viscosity of polymer solution which
improves the sweep efficiency as well as oil recovery. A 1.0 wt% silica
nanoparticles improves the viscosity of guar gum to a greater extent
than other concentration such as 0.05 wt%; 0.1 wt%, and 0.3 wt%.
Imbibition experiments showed recovery of 28 % and 36 % OOIP for
0.2 wt% nano-silica solution and mixed silica nanoparticles-guar gum
solution respectively. As it is spontaneous imbibition nano-silica plays a
major role in oil recovery. Contact angle measurements indicated the
alteration of wettability from intermediate-wet (88°) to water-wet
(115°) state in case of silica nanoparticles and guar mixture which can
ease the oil recovery. On the other hand, silica nanoparticles (0.025 wt
%) in water alone can also change the wettability from intermediate-
wet (82°) to water-wet (108°). Brine cannot significantly alter wett-
ability. Phase behavior study showed that emulsification is possible
when silica nanoparticles are used with guar gum solution. But the
spontaneous formation of Winsor III phase was not observed in the
study. It was found that emulsification is obtained at low temperature
and emulsions were broken down at high temperature. Core displace-
ment study showed that silica nanoparticles-assisted guar gum solution
recovered the maximum additional oil of 44.28 %, followed by 10.73 %
with silica nanoparticles solution and 27.13 %with guar gum solution.
Therefore, silica nanoparticles are effective in improving oil recovery
when they are used in conjunction with guar gum polymer. Finally, a
comparative study is conducted to show the performance of silica na-
noparticles-assisted polymer flooding for additional oil recovery in
15
Colloids and Surfaces A 598 (2020) 124833
different cores and micromodel set up. Most of the research investiga-
tions have focused on the application of silica nanoparticles-induced
polyacrylamide and xanthan gum chemical slugs in enhanced oil re-
covery. The present work focuses on the silica nanoparticles-assisted
guar gum flooding for additional oil recovery from sandstone core and
it is found that the designed polymer slug has better efficiency than
other chemical slugs available in the literature.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgements
The authors would like to acknowledge Drilling, Cementing, and
Stimulation Research Center, School of Petroleum Technology, Pandit
Deendayal Petroleum University for providing the facilities to conduct
research work on enhanced oil recovery by nanoparticles-induced
polymer flooding. The authors are thankful to Mr. Hitendra Patel, Mr.
Dhrumil Patel and Mr. Bhavesh Mehta for their assistance in performing
laboratory experiments.
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