Journal of Petroleum Science and Engineering 186 (2020) 106791

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Journal of Petroleum Science and Engineering

journal homepage: http://www.elsevier.com/locate/petrol

Environmentally benign invert emulsion mud with optimized performance

for shale drilling
Roshan Tiwari a, Saket Kumar b, Maen M. Husein b, *, Pranali M. Rane a, Nitesh Kumar c
a
Department of Petroleum & Energy Studies, DIT University, Dehradun, Uttarakhand, 248001, India
b
Department of Chemical & Petroleum Engineering, University of Calgary, Calgary, AB, T2N 1N4, Canada
c
MDNK Oil & Gas Consultants, Mumbai, Maharashtra, India

A R T I C L E I N F O A B S T R A C T

Keywords: Drilling muds having less environmental footprint are highly desired, especially for drilling into sensitive for­
Shale mation. In this research, an environmentally benign invert emulsion mud having Indian mango methyl ester
Instability (IMME) continuous phase was developed for shale drilling. The properties of the mud were tuned using nanoclay
Swelling
and gum acacia in order to minimize shale instability associated with rock-fluid interactions. The effect of
Fluid loss
Drilling
nanoclay and gum acacia content on the rheological behavior and fluid loss of the developed mud was assessed.
Shear thinning Furthermore, the thermal and mechanical stability of the mud were estimated. Results obtained with nanoclay
and gum acacia were compared with the conventional bentonite and carboxymethyl cellulose additives. Muds
containing nanoclay and gum acacia outperformed conventional additive-containing muds in all measures. The
rheological properties, such as apparent and plastic viscosities, yield point and gel strength, of the mud
formulated with gum acacia and nanoclay were remarkably enhanced. Moreover, the mud containing nanoclay
and gum acacia was mechanically and thermally stable up to 100 � C. Particle size analysis of this mud confirmed
the suitability of the additives toward shale plugging. The invert emulsion with the nanoclay and gum acacia
achieved 95% weight recovery comparing with the conventionally used bentonite and CMC, which only achieved
64% weight recovery. Overall, the 40:60 (W/O) invert emulsion with IMME continuous phase and nanoclay and
gum acacia additives portrayed ideal viscosity, rheology, fluid loss, particle size distribution and stability suited
for shale drilling.

1. Introduction ranging from 0.1 to 150 mm (Dorman et al., 2015) are used in shale
drilling. The difference in size, on the other hand, compromises the
Drilling through a clay-rich shale formation often results in borehole ability of conventional, commercially available loss circulation mate­
instability issues (Jain and Mahto. 2017; Kumar et al., 2018a,b). Con­ rials (LCMs) from building effective, smooth filter cakes on shale sur­
trary to conventional drilling, in which drilling only accounts for 25% of face. Gum acacia is a bio polymer consisting of monosaccharide
the wellbore cost, drilling into shale formations makes up more than monomer with different functional groups such as hydrogen bonded OH,
75% of the cost, with more than 90% of all expenses associated with amino, C– – C and carboxylic groups (Daoub et al., 2018). Generally CMC
wellbore instability (Kang et al., 2016). The main cause of wellbore polymer are used for drilling mud formulation, which is a semi-synthetic
instability in shale formation is rock-fluid interaction, which results in polymer. It is evident from the literature that bio polymers have always
subsequent swelling, sloughing and eventually to the dispersion of the shown better shear thinning property than semi- or synthetic polymer
wellbore (Chenevert., 1970). The rock-fluid interaction generally arises (Jain and Mahto. 2017). In addition, biopolymers are biodegradable and
from the invasion of mud filtrate into the pores of shale formation. In less sensitive to H2S comparing with synthetic and semi-synthetic
principle, plugging, or seal off, the shale pore throats (10–50 nm polymers (Jamroz et al., 2019). Following particle bridging theory
([Kumar et al., 2018a,b]) while drilling helps minimizing shale swelling (Dick et al., 2000), the only possible option to tackle such challenge in
(Hayatdavoudi., 1986). Conventional filtration loss additives, e.g. shales is the use of nanoparticle (NP) LCMs (Abrams. 1970; Suri and
various bio- and synthetic polymers, bentonite, and barite, with sizes Sharma., 2001).

* Corresponding author.
E-mail addresses: [email protected] (S. Kumar), [email protected] (M.M. Husein).

https://doi.org/10.1016/j.petrol.2019.106791
Received 17 October 2019; Received in revised form 4 December 2019; Accepted 7 December 2019
Available online 11 December 2019
0920-4105/© 2019 Published by Elsevier B.V.
R. Tiwari et al. Journal of Petroleum Science and Engineering 186 (2020) 106791

Application of nanotechnology in petroleum industry has evolved Table 1

significantly over the past decade (Corredor et al., 2019). In particular, Composition of the (W/O) invert emulsion muds with IMME as the continuous
the use of NPs in drilling fluids have been reported to enhance drilling phase used in the experiments, unless otherwise stated.
fluid performance significantly. For example, Abdou et al. (2013) have Constituents Mud system 1 Mud system 2
reported that mud systems incorporating nanomaterials impart superior Water (mL) 200 200
rheological and filtration properties and enhance the mechanical and XG (g) 0.3 0.3
thermal stability of the mud. Husein and coworkers described an SLS (g) 0.3 0.3
economically viable approach for preparing highly dispersed NPs into NaCl (g) 5 5
IMME (mL) 300 300
different types of drilling fluids (Husein et al. 2013, 2017; Husein and
Nanoclay (g) 0.3 –
Hareland, 2014). They reported effective fluid loss prevention (Husein Gum acacia (g) 0.2 –
et al., 2013), lubricity improvement (Husein and Hareland, 2014) as Bentonite(g) – 0.3
well as wellbore strengthening (Husein et al., 2017), even for shale CMC (g) – 0.2
formation. Moreover, application of different nanomaterials as fluid loss
control additives tackled borehole instability issues in shales (William
conventionally employed bentonite and carboxymethyl cellulose (CMC)
et al., 2014; Akhtarmanesh et al., 2013; Li et al., 2016). The observed
rheology modifier and fluid loss control additives is made. The chemical
reduction in fluid loss was attributed to sealing off shale pore throats by
and physical properties of the IMME were detailed in our earlier pub­
virtue of the size compatibility between the mud particles and the for­
lication (Kumar et al., 2019). The effect of nanoclay and gum acacia on
mation pore throat. Nanoclay has been used as a viscosity enhancer by
formation damage potential, thermal stability and the rheological and
virtue of its small particle size comparing with the conventionally
filtration properties of the mud is assessed. Shale encapsulation prop­
employed bentonite. Hence, nanoclay may easily plug the pore throats
erties were analyzed using shale recovery test as well as careful in­
of shale and may result in less fluid loss. Nanoclays are typically
spection of photographs of the in-house synthesized shale specimens
composed of montmorillonite minerals with negative surface charges
following exposure to the mud.
leading to negative zeta potential (Teli et al., 2017; Kumar et al., 2018a,
b).
2. Experimental procedures
Water-based drilling fluids are generally used in conventional dril­
ling operations. However, when applied to shale, the rock-fluid inter­
2.1. Materials
action leads to shale swelling and disintegration (Liang et al., 2014;
Oort., 2003; Deville et al., 2011) owing to water sorption into the center
Indian mango seed oil was purchased from Satyanarayan oil mills,
of the shale structure (He et al., 2016; Kumar et al., 2017a,b). In addi­
Siwan, Bihar, India. The seed oil was converted into Indian mango
tion, these rock-fluid interactions also lead to alteration in in-situ stress
methyl ester (IMME) via transesterification, as detailed in our previous
regimes and change in properties and functions of drilling fluids (Jain
study (Kumar et al., 2019). Details on the chemical structure and syn­
and Mahto., 2015). Mahto and Sharma (2004) noted that swelling is a
thesis of IMME have been included in our earlier publication (Kumar
function of shale structure and chemical composition as well as the type
et al., 2019). The resultant IMME constituted the continuous phase of
of cations present in it. Accordingly, wellbore instability may be miti­
the (W/O) invert emulsion muds used in this study. Distilled water,
gated by proper selection of drilling fluid additives. Generally, oil-based
bentonite and carboxymethyl cellulose (CMC) were purchased from
drilling muds (OBM) lead to better shale borehole stability than the
Shankar Chemical Company Pvt. Ltd. (New Delhi, India). Nanoclay of
water-based drilling mud (WBM). Operators mostly use conventional
synthetic grade and laboratory grade xanthan gum (XG), sodium lauryl
diesel oil while formulating OBM owing to diesel’s appropriate viscosity
sulphate (SLS) and potassium chloride (KCl) were purchased from Sigma
and low flammability and cost (Mahto and Sharma., 2004). Neverthe­
Aldrich (Mumbai, Maharashtra, India). Gum acacia was procured from
less, diesel oil is not desired for offshore application due to the associ­
the Department of Pharmacy, DIT University, Dehradun, Uttarakhand,
ated risk to aquatic life and low rates of degradation (Nelson et al.,
India. All chemicals were used as received without further purification.
1984). Disposal of diesel-based OBM has been a major cause for
seawater pollution (Li and Osisanya., 2016). Many oil producing coun­
tries enact laws on offenders to protect their environment from the 2.2. Experimental methods
harmful impacts of diesel-based OBM (Agwu., 2015). For instance, the
Arabia established Corporate Regulations for Offshore Drilling Opera­ 2.2.1. Mud preparation
tions in November 18, 1987, whose motto is to haul back all drill cut­ Two 40:60 (W/O) invert emulsion muds were formulated with IMME
tings to onshore facilities and clean cuttings before exposing them to the as the continuous phase. A volume of 300 mL of IMME, 0.3 g of SLS and
sea (Kumar et al., 2019). In addition to their environmental impact, 5 g NaCl were mixed with 200 mL distilled water using a magnetic stirrer
diesel-based muds may incur high costs to the drilling operations, to achieve complete dissolution/dispersion of the additives. A mass of
especially given the required cleaning step of the drill cuttings. Subse­ 0.3 g of nanoclay and 0.2 g of gum acacia were added to one of the mud
quently, an eco-friendly OBM represents an attractive alternative (Yas­ systems, termed as mud system 1. In the other mud system, system 2, the
sin et al., 1991). Kumar et al. (2019) recently proposed (O/W) emulsion masses of nanoclay and gum acacia were replaced with the conven­
mud with IMME dispersed phase as a replacement to diesel-based mud. tionally used bentonite and carboxymethyl cellulose (CMC) LCMs,
They reported IMME to be biodegradable and non-toxic. Nevertheless, respectively. Table 1 provides detailed description of the constituents of
for shale formation swelling and dispersion due to filtrate invasion, each mud system. Other mud compositions were prepared by changing
especially at high water content, represents different challenge. the concentration of nanoclay (0.2–0.6 g), bentonite (0.2–0.6 g), CMC
Accordingly, coupling OBMs formulated with IMME as a continuous (0.1–0.6 g), gum acacia (0.1–0.6 g), NaCl (2–10 g) in such a way that
phase with nanomaterials may address the environmental concerns as 500 mL of 40:60 (W/O) emulsions mud volume was maintained for ease
well as shale instability issues. Nevertheless, another problem associated of comparison. Duplicates of some of the mud systems were prepared
with vegetable oil-based drilling muds is their relatively high viscosity and variability in the measured properties was <5%.
(Onuh., 2017). Thus, formulating (W/O) invert emulsion mud with
vegetable oil continuous phase may address the high viscosity issues. 2.2.2. Rheological and filtration property analyses
The current work explores the use of (W/O) invert emulsion having The effect of nanoclay and gum acacia on the rheological and
IMME as a continuous phase and incorporating nanoclay and gum acacia filtration characteristics of the mud were analyzed using Fann viscom­
as viable alternative LCMs for shale drilling. A comparison with the eter (Model 35, Fann Instruments Company, Houston, Texas, USA) and

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Fig. 1. Photographs of the in-house prepared shale specimens (D ¼ 6 cm and H Fig. 2. Photographs of the in-house prepared shale cuttings before soaking into
¼ 5 cm). mud system 1 or 2.

API filter press (Fann Instruments Company, Houston, Texas, USA) at Panalytical Ltd, Malvern, United Kingdom). The scattered light when the
room temperature and 100 psi. The filter paper had 0.137 mm pore size laser beam passed through the samples was collected and related to the
and 6.35 cm diameter. particle size distribution (PSD) (Kumar et al., 2019).

2.2.3. Flow behavior studies 2.2.9. Shale stability test

The consistency curve of mud system 1 for different mass fractions of
nanoclay and gum acacia was extracted from the flow behavior curves. 2.2.9.1. Preparation of shale specimen. Cylindrical shaped (D ¼ 6 cm, H
These consistency curves are obtained from the variation of the apparent ¼ 5 cm) shale specimens were prepared in the laboratory by pressing
viscosity versus shear rate as measured with Anton Paar rheometer homogenized mixtures of kaolinite (75 wt%, 50–150 mesh size), silica
(Anton Paar Analytical Instrument Company, Ashland, Virginia, USA) at (15 wt%, 60–120 mesh size), feldspar (10 wt%, 171–200 mesh size) at
80 � C (Dardir et al., 2014). The temperature for this analysis was 0.6894 MPa and keeping it to cure in an oven at 60 � C for 15 days to
controlled by a hot water bath externally attached to the motor drive of achieve solidification. Photographs of the in-house prepared shale
the rheometer. The shear rate ranged from 1 to 1000 s 1 over 50 min specimens are show in Fig. 1.
time interval.
2.2.9.2. SEM and XRD characterization of the in-house prepared shale.
2.2.4. Thermal stability Morphology and composition of the in-house prepared shale specimens
The thermal stability of mud systems 1 and 2 was analyzed with an were analyzed using SEM and X-ray diffraction (Rigaku Ultima 4, Texas,
electrically driven roller equipped with an aging cell (Fann Instrument USA). The SEM was operated as described in Section 2.2.7. XRD used Cu
Company, Texas, USA) at 130 � C, also known as the dynamic aging Ka radiation which operates at 40 kV and 44 mA with a h–2h goniom­
analysis (Jha et al., 2016). The rheological and the fluid loss properties eter. The structure of the particles was identified by comparing the
of the aged mud systems were determined as described above. patterns with database provided by JADE program, Materials Data XRD
Pattern Processing Identification & Quantification (Tarbous and
2.2.5. Emulsion stability Husein., 2012). These analyses were conducted to detail the composi­
Emulsion stability tests were performed by varying the concentration tion of the in-house prepared shale specimen as well as their surface
of SLS in systems 1 and 2, and analyzing the photographic images morphology.
collected on a digital camera (Hassan., 2015). Moreover, the effect of
SLS on the rheological and filtration characteristics of mud systems 1 2.2.9.3. Shale weight recovery test. Shale stability was analyzed using
and 2 were analyzed as described in Section 2.2.2 and compared. shale weight recovery test (Kumar et al., 2017a,b). In this method, a
mass of the in-house prepared shale cuttings was sieved through a mesh
2.2.6. Salt tolerance screen of 20 mm and weighed in a dry form (Wo). A photograph of the
The drilling contaminant tolerance was analyzed by varying the shale cuttings used in this analysis is shown in Fig. 2. The shale cuttings
concentration of NaCl (2–10 g) at fixed amounts of nanoclay (0.3 g) and were poured into mud system 1 or 2 and kept there for 10 h at room
gum acacia (0.2 g) in the mud. The effect of NaCl on the rheological and temperature. The cuttings were then recovered and dried in an oven at
filtration properties of mud system 1 was further evaluated, as described 70 � C and weighed (W1). The shale recovery percentage was calculated
in Section 2.2.2. according to 1 (Kumar et al., 2017a,b). Even though pre-hydrated
bentonite had been shown to have less impact on shale stability
2.2.7. SEM characterization (Lander et al., 2015), the bentonite used in this study (mud system 2)
The surface morphological characteristics of the nanoclay, gum was not pre-hydrated. Therefore, bentonite was thoroughly mixed with
acacia, bentonite and CMC were determined using scanning electron distilled water while preparing mud system 2 to prepare stable sus­
microscopy, SEM (Jeol JSM 5910 LV, Jeol India pvt. Ltd, New Delhi, pension before mixing the shale specimen for this analysis.
India) operated at 220 V, 110 AC, 30 A and 3KVA total load.
ðWo W1Þ
%R ¼ � 100 (1)
2.2.8. Particle size analysis Wo
Particle size analysis of the mud systems 1 and 2 was carried out in
order to reveal potential compatibility with shale pore throats. A volume 2.2.9.4. Shale specimen integrity. The in-house prepared shale speci­
of 2–10 mL of as-prepared mud system 1 or 2 was placed in Malvern mens were immersed for 4 h in mud systems 1 and 2 in order to visually
Mastersizer Particle Size Analyzer (Mastersizer 3000, Malvern evaluate the effect of rock-fluid interactions on the shale. Photographs of

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Fig. 3. A flow diagram detailing the sequence the experimental procedures involved in this study.

Fig. 4. Comparative effect of nanoclay and bentonite on the rheological and filtration loss properties of mud systems 1 and 2: a) apparent viscosity; b) plastic
viscosity; c) yield point; d) final gel strength; e) fluid loss.

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Fig. 5. Comparative effect of gum acacia and CMC on rheological and filtration loss properties of mud systems 1 and 2: a) apparent viscosity; b) plastic viscosity; c)
yield point; d) final gel strength; e) fluid loss.

the shale specimen following the 4 h soaking were compared to the as- The volume of the fluid lost during filtration decreased from 6 to 2.2
prepared specimen in Fig. 2. Appearance of defects, e.g. fractures, mL upon increasing the nanoclay content, likely due to the more effec­
dispersed structure, etc., help evaluating shale stability upon exposure tive suspension of the nanoclays within the mud when compared to
to the mud. bentonite (Fig. 4e). As such, the nanoclays readily contribute to building
A flow diagram describing the experimental work is provided as a more firm filter cake, especially by virtue of their higher extent of
Fig. 3. interaction/adsorption with the other constituents of the filter cake.

3. Results & discussions 3.1.2. Effect of gum acacia and CMC additives
The effect of varying the concentration of gum acacia and CMC on
3.1. Rheological and fluid loss properties the rheological and filtration properties of mud systems 1 and 2,
respectively, is reported in Fig. 5. The apparent and plastic viscosities
3.1.1. Effect of nanoclay and bentonite increased significantly from 33 to 42 cP and 18–30 cP for mud system 1,
The effect of the nanoclay (0.2–0.6 g) or bentonite (0.2–0.6 g) con­ containing gum acacia, comparing with mud system 2, containing CMC
tent on the rheological and filtration properties of the mud systems 1 and which varies from 23 to 40 cP and 10–28 cP. Moreover, the yield point
2 is reported in Fig. 4. The apparent and plastic viscosities increase from remained within an acceptable range i.e. 12–17 lb/100 ft2 (Kumar et al.,
29 to 48 cP and from 18 to 28 cP, respectively, upon increasing nanoclay 2019) at the higher content of gum acacia, i.e. 0.6 g. The increase in
content from 0.2 g to 0.6 g (Fig. 4a&b). However, upon increasing viscosity is attributed to effective adsorption of gum acacia onto the
bentonite content from 0.2 g to 0.6 g, the apparent and plastic viscosities nanoclay, which imparts high extent of friction with the continuous
only increase from 25 to 34 cP and from 14 to 19 cP, respectively phase as well as other constituents of the mud (Degouy et al., 1993).
(Fig. 4a&b). The superior frictional properties among the nanoclay CMC does not portray the same degree of adsorption/interaction with
particles likely contributed to higher viscosity of the mud (William et al., the constituents of mud system 2. The thixotropy of mud system 1 is also
2014). High mud viscosity provides proper suspension of the rock cut­ enhanced in presence of gum acacia comparing to the effect of varying
tings to the surface. Moreover, higher values of the yield point are CMC concentration in mud system 2, as confirmed from the gel strength
observed, from 11 to 20 lb/100 ft2, upon increasing nanoclay (Fig. 4c) data of Fig. 5d. Thus, it can be noted from Sections 3.1.1 and 3.2.2 that
comparing to bentonite, from 11 to 15 lb/100 ft2 (Fig. 4c). The increase both the gum acacia and nanoclay enhanced the rheological properties.
in viscosity and yield point is accompanied by an increase in gel Comparing the effect of nanoclay versus gum acacia on rheological
strength, as shown in Fig. 4d. Optimum gel strength corresponds to properties it can be said that at the same content, nanoclay had more
sufficient capability of cuttings suspension during down time and low impact and gum acacia further enhanced the rheology of mud system 1
energy at the start of operation (Jain and Mahto., 2017). It is anticipated through interacting with nanoclay.
that higher extent of intermolecular interactions among the mud con­ Fluid loss is significantly reduced with increasing gum acacia con­
stituents at higher nanoclay content contributed to the increased values centration in mud system 1, as depicted in Fig. 5e. It is desired to keep
of the different rheological properties comparing to bentonite. fluid loss to shale to a minimum, in order to maintain formation stability

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Fig. 6. Effect of various (a) gum acacia and (b) nanoclay content on the consistency of mud system 1.

Fig. 7. Effect of temperature on the rheology and fluid loss for mud system 1.

Fig. 8. Effect of temperature on the rheology and fluid loss for mud system 2.

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Fig. 9. Comparative effect of SLS on rheological and filtration loss properties of mud systems 1 and 2: a) apparent viscosity; b) plastic viscosity; c) yield point; d) final
gel strength; e) fluid loss. Data for concentration of SLS between 0.1 and 0.4 g has not been reported for mud system 2 due to foaming.

(Kumar et al., 2018a,b). It is highly likely that the adsorption of gum drilling operations (Tarbous and Husein., 2012; Kumar et al., 2017a,b;
acacia onto the nanoclay contributed to effective bridging between the Kumar et al., 2018a,b). The shear thinning behavior helps drawing
nanoclays contributing to filter cake. Subsequently, uniform and thin conclusions on the strength of colloidal particle interactions within mud
layer filter cake formed, which prevented further migration of fluid and system 1. Gum acacia existing as free polymer in the continuous phase, i.
low gravity solids toward the filter cake and the formation. The com­ e. IMME, is coiled up like wool in presence of nanoclays (Hassan. 2015).
bination of gum Acacia and nanoclays displayed much better degree of
interaction than conventional LCMs, i.e. CMC and bentonite.
3.3. Thermal stability

3.2. Mud consistency studies The temperature effect on mud systems 1 and 2 is reported in Figs. 7
and 8. Mud system 1 displayed persistent stability at varying tempera­
The consistency curves of mud system 1 with varying concentration tures from 25 to 100 � C, as confirmed from the constant rheological and
of gum acacia and nanoclay are depicted from Fig. 6. Mud system 1 filtration properties of this system at the various temperatures. On the
displayed strong shear thinning property also known as pseudo plastic other side, the rheological parameters are reduced with temperature for
behavior, at the different content of gum acacia and nanoclay, as mud system 2. On the other hand, the depreciation of the filtration
confirmed from the variation of apparent viscosity vs. shear rate of properties of mud system 2 formulated with bentonite and CMC
Fig. 6. Such a property is important for attaining better circulation and increased with the rise in temperature, as depicted in Fig. 8, confirms the
borehole cleaning, which have been challenging tasks to achieve during unstable nature of this mud system. Generally, the rheology of invert

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Fig. 10. Photographs of mud system 1 for SLS content varying between 0.1 and 0.5 g (no apparent phase separation or foaming).

8
Fig. 11. Photographs of mud system 2 for SLS content varying between 0.1 and 0.4 g (apparent phase separation and foaming) and SLS of 0.5 g (no signs of phase separation and little foaming).
Journal of Petroleum Science and Engineering 186 (2020) 106791
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Fig. 12. Comparative effect of KCl (2–10 g) on rheological and filtration loss properties of mud systems 1 and 2: a) apparent viscosity; b) plastic viscosity; c) yield
point; d) final gel strength; e) fluid loss.

emulsion muds degrades with increasing temperature which can be a temperature stabilizers. Hence, mud system 1 can be a better choice
severe risk while drilling sensitive formations such as shale. However, while drilling reactive shale reservoirs (Jain and Mahto., 2017).
mud system 1, with gum acacia and nanoclay, displayed enhanced sta­
bility till 100 � C as confirmed from the rheological and filtration loss
tests. This suggests that nanoclay and gum Acacia also acted as

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Fig. 13. SEM photographs for a) nanoclay, b) gum acacia, c) bentonite and d) CMC.

3.4. Emulsion stability comparison between the rheological and filtration properties for mud
systems 1 and 2 at various content of SLS is reported in Fig. 9.
The effect of varying the concentration of SLS on emulsion stability
are reported in Fig. 9 for mud systems 1 and 2 at fixed composition. For 3.5. Salt tolerance
mud system 1, Fig. 10 shows that the mud remains stable independent of
SLS content. The high stability of mud system 1 can be attributed to gum Fig. 12 summarizes the effect of NaCl on the rheological and filtra­
acacia acting as a co-emulsifier, as previously reported. On the other tion properties of mud systems 1 and 2. It can be observed that
hand, mud system 2 was not stable between SLS content of 0.1–0.4 g and increasing NaCl concentration does not have significant effect on mud
foaming was observed, as depicted in Fig. 11. Stability was, neverthe­ system 1. On the other hand, the rheological and filtration properties of
less, achieved at 0.5 g of SLS for mud system 2. Probably the low vis­ mud system 2 depreciated significantly with increasing NaCl concen­
cosity of mud system 2 contributed to its instability, since at low SLS tration. The apparent and plastic viscosity for mud system has been
content, bentonite particles were not effectively dispersed. A reduced from 28 to 33 cP and 16–11 cP which seems to be significant

Fig. 14. PSD analysis for mud systems a) 1 and b) 2.

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Fig. 15. a) SEM photographs and b) XRD finger prints of the in-house prepared shale specimens.

comparing to mud system 1 which has observed negligible effect with 3.6. Characterization of the different LCMs
increase in salt concentration. Also, no affect has been observed on gel
strength of mud system 1 compared to mud system 2 with increase in salt The surface morphologies of nanoclay, gum acacia, bentonite, and
concentration. The depreciation of the rheological and filtration prop­ CMC were investigated using SEM analysis. Fig. 13 shows SEM photo­
erties of mud system 2 as noted in Fig. 12, can be attributed to the graphs of the different LCMs. The morphology of nanoclay and gum
degradation of CMC polymer chain, which in turn affects bentonite acacia is smooth and regular, which may aid in building a smooth, thin
flocculation (Kumar et al., 2017a,b). In contrast, nanoclay and gum filter cake on the shale surface. The morphology of bentonite and CMC,
acacia showed tolerance to salt, which is desired in a drilling mud (Jha on the other hand, is non-uniform and irregular which in turn leads to a
et al., 2018). More relevant, salt tolerance is highly desired while dril­ non-uniform highly permeable filter cake. Such a cake does not protect
ling in shale, since any collapse of in mud stability may lead to major shale from the invasion of reactive components, which leads to wellbore
consequences (Buffo and Reineccius., 2000). Increase in fluid loss was instability.
also observed with mud system 2 i.e. 11.2–15.6 mL which become a
major challenge while drilling a formation like shale with such type of 3.7. Particle size analysis
mud as it is evident that salt plays an important role in encapsulating
shale swelling (Onuoha and Olafuyi, 2013). The particle size distribution (PSD) for mud systems 1 and 2 is
included in Fig. 14. Fig. 14 shows that the average particle size of mud
system 1 is 33 nm, whereas that of mud system 2 is 465 nm. As stated
earlier, majority of researchers suggested that pore size of shale lies

Fig. 16. Photographs of shale cuttings used in shale weight recovery test for mud system 1 a) before the test, b) right after the test in the wet form and c) after drying
the wet cuttings.

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was developed with Indian mango methyl ester (IMME) as the contin­
uous phase. A 40 vol% water into the invert emulsion ensured proper
viscosity. The mud system was optimized for shale drilling using nano­
clay and gum acacia. The results were compared with conventional
rheology modifiers and fluid loss agents consisting of bentonite and
carboxymethyl cellulose (CMC). In presence of nanoclay and gum acacia
the mud furnished superior rheological and fluid loss properties, likely
due to the synergy between the nanoclay and gum acacia. Fluid loss
prevention is highly desired, especially when drilling with sensitive
formation such as shale. Strong pseudo plastic characteristics suited for
cuttings circulation are observed in presence of nanoclay and gum
acacia, which could be easily tuned by adjusting the dose of either
components. The mud system was stable in presence of nanoclay and
gum acacia at any concentration of sodium lauryl sulphate (SLS) tested
Fig. 17. In-house prepared shale specimen following exposure to mud systems
in this study, KCl dose and up to 110 � C. The salt tolerance tendency of
a) 1 or b) 2 for 4 h.
mud system 1 helps in inhibiting the shale formation. The morphology of
nanoclay and gum acacia revealed strong potential to form thin smooth
between 2 and 50 nm (Kumar et al., 2018a,b). Thus, LCMs in mud sys­
layer, which prevented fluid loss into shale effectively as evident particle
tem 1, i.e. nanoclay and gum Acacia, should lead to effective plugging
size analysis. Furthermore, in presence of nanoclay and gum acacia
and much less invasion, per the optimum LCM size rule of thumb
excellent shale encapsulation property was achieved and high shale
(Whitfill., 2008). The majority of wellbore instability occurs due to
weight recovery was obtained, also owing to the use of an oil continuous
rock-fluid interaction arising from fluid loss to the formations (Kumar
phase as opposed to water-based mud.
et al., 2017a,b).
Author contributions
3.8. Shale stability analysis
Saket Kumar has conducted all the experiments other than shale
3.8.1. Characterization of the in-house prepared shale specimens stability analysis, analyzed all the experimental data and written the
The morphology of the in-house synthesized shale specimens was manuscript. Roshan Tiwari has conducted shale stability experiment and
also characterized using SEM. Fig. 15a shows evidence of microfractures some rheological tests to examine the salt tolerance tendency and
within the synthesized shale. Microfractures contribute to drilling fluid thermal stability of the mud system. Pranali Rane has analyzed the SEM
invasion and subsequent swelling of the shale formation. The composi­ and XRD analysis. Nitesh Kumar has reviewed and supervised the work
tion of the in-house prepared shale was determined using XRD, as initially. Prof. Husein reviewed the experimental results and the write-
depicted in Fig. 15b. The peak corresponding to 2θ ¼ 27.2 is charac­ up and ensured all is up to the requirements.
teristic of quartz (Jain and Mahto., 2015). The small peaks at 2θ ¼ 34.3
and 2θ ¼ 48 are characteristic of reactive clay minerals such as kaolinite Declaration of competing interest
and montmorillonite (Kumar et al., 2017a,b; Jain and Mahto, 2017). The
3 noted minerals are susceptible to swelling and dispersion when All authors declare no conflict of interest.
exposed to an aqueous environment.
Acknowledgement
3.8.2. Shale weight recovery
The shale weight recovery for shales cuttings soaked into mud sys­ The authors would like to acknowledge the laboratory support pro­
tems 1 and 2 reflects gum acacia and nanoclay versus conventional vided by the Department of Petroleum & Energy studies, DIT University,
LCMs’ ability to stabilize the shale. Percentage recovery of shale weight Dehradun, Uttarakhand, India. The authors would also like to
for shale soaked in mud system 1 was 95%, whereas that soaked in mud acknowledgeOil & Natural Gas Corporation Ltd., Dehradun, Uttarak­
system 2 was only 64%. Accordingly, it is safe to say that mud system 1, hand, India for enabling XRD and SEM analyses in their laboratory.
incorporating nanoclay and gum acacia, is much more effective in pre­
serving shale stability. Photographs of cuttings before and after soaking Appendix A. Supplementary data
in mud system 1 are shown in Fig. 16a and b, and those following drying
the cutting from Fig. 16b are shown in Fig. 16c. Supplementary data to this article can be found online at https://doi.
org/10.1016/j.petrol.2019.106791.
3.8.3. Shale specimen integrity
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