SPE-197774-MS

Improvement in Rheological Features, Fluid Loss and Swelling Inhibition of

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Water-Based Drilling Mud by Using Surfactant-Modified Graphene

Azeem Rana and Tawfik A. Saleh, King Fahd University of Petroleum and Minerals; Mohammad K. Arfaj, Saudi
Aramco, EXPEC Advanced Research Center, Drilling Technology Division

Copyright 2019, Society of Petroleum Engineers

This paper was prepared for presentation at the Abu Dhabi International Petroleum Exhibition & Conference held in Abu Dhabi, UAE, 11-14 November 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
of the paper have not been reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect
any position of the Society of Petroleum Engineers, its officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written
consent of the Society of Petroleum Engineers is prohibited. Permission to reproduce in print is restricted to an abstract of not more than 300 words; illustrations may
not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.

Abstract
The improved rheological properties of the drilling fluid are very critical for the oil well drilling operation.
The present work reports the effect of sodium dodecyl sulfate modified graphene (SDS-Gr) on the
rheological features, fluid loss and swelling inhibition mechanism of clay. The rheology and filtration test
of drilling mud were conducted after being hot rolled for 16 h at 150oF and under 500 Psi pressure. The
inhibition characteristics were evaluated by the dispersion test and shale inhibition durability test, where
SDS-Gr modified drilling mud shows the highest recovery as compared to KCl and traditional drilling
mud. The inhibition mechanism was investigated by various kind of techniques such as thermogravimetric
analysis, scanning electron microscopy, and energy dispersive X-Ray spectroscopy. The outcomes revealed
that the addition of SDS-Gr to the traditional drilling mud clearly affect the rheological properties and make
it more suitable for the drilling. Moreover, SDS-Gr additive reduces fluid loss by 20% as compared to the
mud without SDS-Gr. The Fourier transform infrared spectroscopic study also confirms the adsorption of
SDS-Gr on clay. SDS carries the negatively charged functional group that help SDS-Gr to binds to the
cations present on the clay surface and graphene plug the pores in the clay. The intercalation and adsorption
of SDS-Gr on to the surface of clay hinder water molecules from invading the clay that helps in mitigation of
swelling due to hydration. We report for the first time the SDS modified graphene (SDS-Gr) that successfully
binds to the clay surface. In order to combine the features of SDS and graphene, the graphene surface is
factionalized with SDS that modify the drilling mud rheology, control fluid loss and inhibit the clay swelling.
Keywords: Water-based drilling mud, anionic surfactant, rheological properties, swelling inhibition, fluid
loss control

Introduction
The search and production for oil and gas do not remain the easy task due to the continuously decreasing
pressure of mature oil reservoir fields. Additionally, the depletion of oil reserves reaches to the level that oil
drilling became extravagantly unfeasible. Therefore, the industry is exploring the more challenging areas to
fulfill the energy needs of the world. [1–3]. While drilling these depleted fields many problems are faced,
2 SPE-197774-MS

such as fluid loss, differential sticking and instability of the wellbore [4,5]. The cause of borehole instability
can be mechanical and chemical. The drilling operation itself is the key cause of mechanical instability,
while the interaction between the drilling fluid system and the shale is the chemical cause of borehole
instability [6–8]. When the shale encounters the water-based mud (WBM), the active clay swells with the
absorption of water. The swelling of the shale can cause borehole instability that in the worst case can lead
to the stuck pipe, loss of drilling equipment or abandonment of the well [9,10]. Therefore, a lot of research

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efforts has been made to control shale swelling inhibition issues.
On account of the long-term interaction of WBM with the shale, there are chances of water diffusion and
swelling of shale that can cause the wellbore instability [11]. Without overcoming this wellbore stability
issues no WBM can be considered for the drilling operation. The surfactant-based drilling fluids are
widely employed to control the rheological features, fluid loss and maintain borehole stability [12,13]. The
surfactant-based drilling fluid (SBDF) could help to control the fluid seeping and transport the cuttings.
The higher viscosity with low density makes the SBDF as a foreseeable candidate for the challenging
drilling operation of depleted wells [14,15]. There are various studies reported in the literature where sodium
dodecyl sulfate (SDS) is used to affect the rheology of the drilling mud [16,17].
Graphene is widely explored material that has atom-thick two-dimensional conjugated structure, large
surface area, and high conductivity. Kosynkin and coworker utilized the graphene as the additive for fluid
loss control. The report demonstrated that the graphene displayed better fluid loss control as compared to the
polymer-based materials [18]. Some of the patents also report the utility of the graphene to control the shale
swelling [19–21]. Graphene has the plugging capacity to the shale surface due to flexible nanosheet like
structure, that prevents the interaction of water with shale and hinders the shale swelling [18]. In the present
study, we report for the first time the SDS modified graphene (SDS-Gr) as the fluid loss control and swelling
inhibitor for the shale material. In order to combine the features of SDS and graphene, the graphene surface
is factionalized with SDS. The inhibitive effect of SDS-Gr was also inspected by utilizing various kinds of
inhibition evaluation methods such as mud making tests, % dispersion recovery, shale inhibition durability,
filter loss, scanning electron microscopy (SEM), and thermal gravimetric analysis (TGA). Finally, Fourier
transforms infrared spectroscopy (FT-IR) analysis was carried out to prove the adsorption of SDS on clay.

Experimental section
Materials
In order to compare the swelling inhibition performance of the developed shale inhibitors, KCl was used
as the baseline and purchased from Beantown chemicals, Hudson, USA. The bentonite was obtained from
Delmon group of companies, Al-Khobar, KSA. Resinex, Xanthan gum (XC) biopolymer and poly aluminum
chloride (PAC-L) were acquired from Haliburton, Houston, USA. Sodium sulfite was purchased from Sigma
Aldrich (USA). The tap water was utilized in all the experimentations. Shale cuttings were collected from
one of the Aramco drilling sites and employed to estimate the impression of shale inhibitor on shale integrity.

Material characterization
Field emission scanning electron microscopy (FE-SEM) (Lyra3 TESCAN) was used to characterize the
surface features of the materials under study. X-ray photoelectron spectroscopy (V.G. Scientific ESCALAB
Mk (II) spectrometer using a non-monochromatic Al source (Kα, 1486.6 eV) was used. The FTIR spectra
were acquired by employing a Nicolet 6700 FT-IR (Thermo Electron Corporation) Fourier transform
infrared spectroscopy (FTIR). Thermogravimetric study (SDT Q 600, TA Instruments, New Castle, DE)
was carried out by heating the samples at increment frequency of 10°C / min with flow of nitrogen (75 ml/
min) up to 800°C.
SPE-197774-MS 3

Methods
The swelling inhibition features of the modified WBM was demonstrated by extensive experimental
evidence. In order to test the various features of the shale inhibitor, the water-based mud (WBM) was
prepared by utilizing the components depicted in table 1. The experimental procedures are reported in the
following section.

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Table 1—The composition of water-based muds with and without SDS-Gr shale inhibitor.

Formulation (g) Traditional drilling mud Modified drilling mud

Water (ml) 281.4 281.4

Bentonite 5 5

XC-polymer 0.8 0.8

Resinex 4.5 4.5

PAC-L 1.5 1.5

KCl 29 29

Sodium sulfite 0.3 0.3

SDS-Gr 0 3

The viscometer model 35A (FANN instrument company, Houston, USA) was utilized for the rheology
testing of the unmodified and modified muds. For this purpose, 350 ml of the WBM was prepared containing
5 g of bentonite, various concentrations of surfactants, 3 g shale inhibitor, and coalesced for 30 min. The
dispersion was hot rolled at 100 oC for 16 h under 500 Psi pressure. After hot rolling the rheological features
such as apparent viscosity (AV), plastic viscosity (PV) and yield point (YP) were estimated by using 600
rpm and 300 rpm dial reading of viscometer in the subsequent formulas took from standard procedure for
assessment [22,23]. The mud balance (OFI testing equipment, Inc. Houston, USA) was employed for the
density approximation of the bentonite-based inhibitive mud. For this purpose, 350 ml of the WBM was
prepared containing 5 g of bentonite, various concentrations of surfactants, 3 g SDS-Gr as shale inhibitor,
and commingled for 30 min. The rheological properties of the WBM were estimated before and after hot
rolling to compare the effect of temperature and pressure.
The fluid loss testing was done by utilizing water loss press unit (OFI testing equipment, Inc. Houston,
USA). Bentonite based drilling mud was prepared by adding bentonite along with various additives in the
water. The WBM was mixed for the 30 min then the amount of fluid loss was measured by utilizing water
loss press under pressure of 100 psi according to the standard procedure.
For dispersion recovery test, the shale was crushed and sorted by sieve shaker (W.S. Tyler Mentor, Ohio,
USA) between mesh No. 10 and No. 5. In order to measure the dispersion of shale, the 20 g of the shale
cuttings were added to the 350 ml of WBM with and without shale inhibitor. The aging cell was hot rolled
at 25 rpm and 66oC for 16h in the rolling oven (OFI testing equipment, Inc. Houston, USA)) to mimic a
borehole environment. Afterward, the cell was cool down to room temperature. The shale cuttings were
sieved with mesh No. 35 and then washed thoroughly with running water to eliminate the small shale
particles. The shale cuttings on the sieve were desiccated at 105oC for 24 h in oven. Lastly, the cuttings were
weighed and the % recovery was calculated by using the following equation.
Shale dispersion recovery = Wc/20 x 100
Where Wc is the weight of shale cuttings
4 SPE-197774-MS

Results and discussion

Material characterization
The SEM images and EDX data demonstrate the eminent difference in the shale surface before and after
treatment with SDS-Gr. The figure 1a is the SEM image of the original shale surface, where the pores
are visible, and the surface is not smooth with small broken chunks of shale. The 1b is the graphene
surface modified with SDS material. Once the surface of shale is treated with SDS-Gr the unseamed surface

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appeared in SEM micrograph (1c). The EDX confirms the composition of the shale (1d) is similar to that
is reported in the literature [24,25]. The EDX of SDS-Gr (1e) shows higher content of carbon with sodium,
oxygen, and sulfur. The SDS-Gr modified shale demonstrates that the % of the carbon content prominently
increased as compared to shale material (1f).

Figure 1—FE-SEM images of shale (a), SDS-Gr (b) and shale modified with SDS-
Gr (c). EDX spectra of shale (d), SDS-Gr (e) and shale modified with SDS-Gr (f).

Figure 2 revealed the FTIR spectrum of graphene (Gr), SDS-Gr, shale, and SDS-Gr modified shale was
measured to confirm the structural characteristics. In the FTIR spectra of graphene two prominent bands
appear at 2846 and 2916 cm-1 are attributed to symmetric and asymmetric stretching of -CH2- groups [26].
A characteristic stretching vibration peak of hydroxyl group appear on the 3430 cm-1 [27]. The FTIR spectra
of SDS-Gr revealed that the SDS modified the surface of graphene and variations can be observed. Figure 2
demonstrated the broad peak due -OH stretching vibration disappear due to functionalization by SDS. The
absorbance bands at 2912 and 2840 cm-1 in curve SDS-Gr were attributed to C-H stretching vibrations of
the -CH2- of SDS [28]. The angular vibration of O-H groups of the adsorbed and hydration water in shale
give rise to the absorption band at 1640 cm-1 [29]. The study of FTIR spectra of the shale material match
with that of kaolinite and these outcomes suggested that shale is formed by kaolinite [30]. When SDS-Gr
was added to the shale sample the shale inhibitor interacted with shale surface and plug the nanopores. The
FTIR spectra of SDS-Gr modified shale demonstrate all the characteristics of the clay. However, the broad
peak due to OH stretching at 3416 cm-1 prominently reduced. The peak arises due to adsorbed and hydration
water at 1640 cm-1 was also reduced that confirms the attachment of SDS-Gr to shale induce hydrophobicity.
SPE-197774-MS 5

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Figure 2—FTIR spectra of graphene, PEI-Gr, shale, and shale modified with SDS-Gr.

Figure 3 demonstrates the thermogravimetric analysis of SDS-Gr, shale, and shale modified with SDS-
Gr. The initial weight loss of SDS-Gr can be accredited to the loss of moisture [31]. Afterward, relatively
faster mass loss was observed after 200oC due to degradation of SDS and the hydroxyl functional group
on graphene [32,33]. Finally, a total of 71 % of the residue was obtained from SDS-Gr. The physically
adsorbed water and the water molecules around cations in shale play vital role in mass loss before 200oC.
Therefore, the mass loss before 200oC can be accredited to the dehydration of water molecules [34]. As
shown in figure 3 that from ambient temperature to 200oC the mass loss in the shale sample was 11 % of
its initial weight. On the other hand, SDS-Gr modified shale demonstrated just 3.8 % weight loss that was
much lower as compared to the unmodified shale material. The difference in the % water loss confirms the
intercalation of the SDS-Gr with shale that makes the surface hydrophobic and reduces the water content.
Till 800oC the shale and SDS-Gr modified shale display 36 % and 17 % weight loss correspondingly.

Figure 3—TGA data of SDS-Gr, shale, and shale modified with SDS-Gr.

Mud making test

The measurement of the apparent viscosity (AV), plastic viscosity (PV), yield point (YP) and fluid loss
are presented in table 2. The rheological features can provide crucial information about the drilling mud.
When SDS-Gr is applied to the traditional drilling mud, a prominent decrease in AV of pre and post hot
rolled drilling mud was observed. For a good drilling mud, the PV should be kept low. The temperature is a
crucial factor that affects PV. The table indicates that the PV of the drilling mud conspicuously decrease after
addition of SDS-Gr (0.85 wt %) and by increasing the temperature. The rheological study of the drilling
mud exposed introduction of SDS-Gr to the drilling mud before and after hot rolling increase the YP value.
6 SPE-197774-MS

The traditional inhibitive mud seems to be more affected by the temperature and pressure as compared to
SDS-Gr modified WBM.

Table 2—Rheological properties, and fluid loss measurements.

Pre-hot rolling Post-hot rolling Pre-hot rolling Post-hot rolling

Drilling mud Traditional drilling mud SDS-Gr modifed drilling mud

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Rheology tests (49°C)

PV 15.5 6.5 12 8.9

AV 25 12.25 22.5 16

YP 19 11.5 21 14.2

Gel strength (49°C)

10 s (lb/100ft2) 10 4 9 6

Pascal 4.788 1.915 4.309 2.87

10 min (lb/100ft2) 23 9 22 14

Pascal 11.012 4.31 10.533 6.7

Fluid loss

Spurt loss (ml) 0.6 0.8 0.25 0.5

Total fluid loss (ml) 10 8.33 8.2 8.5

Filter mud cake (mm) 0.397 1.191 1.191 1.191

In order to evaluate the plugging capacity of the SDS-Gr, the filter loss method is used. The SDS-Gr
modified mud display a considerable decrease in the fluid loss due to the SDS-Gr film formation of on the
surface of filter paper that plug the pores and hinder the water flow from filter paper. The formation of a
less permeable film can be confirmed from the formation of the filter cake. The gel strength quantifies the
attractive forces within the drilling mud system under no-flow conditions. The outcomes revealed that the
addition of the SDS-Gr reduces the gel strength G10s and G10 min of traditional drilling mud. Consequently,
resultant modified mud becomes more favorable for drilling by consuming less energy.

Dispersion and swelling test

The dispersion test assesses the fragmentation and attrition of the shale material when exposed to the drilling
fluid. The quantity of shale cuttings recovered after hot rolling indicates the quality of inhibition against
dispersion. The SDS-Gr modified mud demonstrates higher shale cutting recovery that can be ascribed by
adsorption of the SDS-Gr to the surface of shale that hinders the interaction of water with shale surface
and increases the resistance of shale materials against the effects of the aqueous medium as demonstrated
in figure 4.
SPE-197774-MS 7

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Figure 4—Dispersion test of shale in the presence of H2O, KCl, traditional mud, and SDS-Gr modified mud.

The linear swelling rate measurement demonstrates the inhibition capacity of the SDS-Gr shale inhibitors
in figure 5. For this purpose, the linear swelling of the clay materials were also observed in the water and
KCl and SDS-Gr shale inhibitor. The 0.85 wt. % of the inhibition matrix was used to form an aqueous
solution. The outcomes demonstrate that water displays the highest percentage of linear swelling i.e. 27%.
However, an aqueous solution of KCl and SDS-Gr considerably decrease the swelling rate that drops down
to 22 % and 20% correspondingly. The swelling test also confirms the better performance of SDS-Gr as
compare to KCl.

Figure 5—% linear swelling test of shale in the presence of H2O and SDS-Gr aqueous solution.

Swelling and inhibition mechanism

The interaction of SDS-Gr with the clay and swelling inhibition mechanism is schematically depicted in
figure 6. The clay consists of layers of negatively charged aluminosilicates that are held together by the
electrostatic forces arise due to positive ions figure 6a. The Na+, Ca+2, and Mg+2 act as intercalating ions and
make the clay surface hydrophilic. Once the water molecules approach the cations, due to their interaction
the interlayer d-spacing started to increase and commence the clay swelling as illustrated in figure 6b.
Consequently, the volume, number and the surface area of clay particle of wet clay increase several times
as compared to the dry clay. The anionic surfactant modified graphene (SDS-Gr) can limit the swelling by
interaction with clay as illustrated in figure 6c. The negatively charged hydrophilic head interacts with the
oppositely charged edges of the clay [17]. On the other hand, the alkyl chain makes the surface hydrophobic.
In addition to the SDS, the graphene plugs the pores of clay to eliminate the chances of osmotic swelling of
clay particles. Consequently, the SDS-Gr hinder the water molecules to reach the surface of clay by making
it hydrophobic and also change the rheological properties. The description of the mechanism is in good
agreement with the outcomes obtained in SEM, FTIR, rheological and dispersion studies.
8 SPE-197774-MS

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Figure 6—schematic demonstration of (a) dry clay, (b) clay interaction
with water and (c) clay swelling inhibition mechanism of SDS-Gr.

Conclusion
The adsorption of SDS-Gr occurs through the interaction of the negative charges of SDS with the positive
charges on clay. On the other hand, graphene plugs the pores present on the surface and interlayer spacing
of clay. Subsequently, the clay is protected from the destructive action of water. The study of rheological
features, gel strength, fluid loss, and dispersion test revealed the better performance of SDS-Gr modified
drilling mud as compared to the traditional drilling mud. Additionally, SDS-Gr demonstrates better swelling
inhibition performance due to the synergetic effect of anionic surfactant and graphene. Consequently, the
SDS-Gr proves to be a good additive for the drilling mud with promising control of swelling rate.

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