Journal of Petroleum Science and Engineering 208 (2022) 109569

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Journal of Petroleum Science and Engineering

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

Emulsified acid systems for oil well stimulation: A review

Ahmad A. Adewunmi a, Theis Solling a, *, Abdullah S. Sultan b, Tinku Saikia a
a
Center for Integrative Petroleum Research, King Fahd University of Petroleum and Minerals, 31261, Dhahran, Saudi Arabia
b
Department of Petroleum Engineering, King Fahd University of Petroleum and Minerals, 31261, Dhahran, Saudi Arabia

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

Keywords: This review discusses the application of emulsified acids for oil well stimulation. Types of oil, aqueous solutions,
Emulsion and emulsifiers are discussed in detail along with the solid agents and inhibitors that are utilized for emulsified
Rheology acid formation. It has been found that there are at least nineteen (19) proposed ways of combining the chemicals
Kinetics
that potentially can be employed operationally. The impact of heat and viscosity on the efficiency of the acid
Stimulation
Drag
emulsions and the carbonate-decomposition kinetics are also in focus. Pumping emulsified acids through pipe­
Stability lines constitutes enormous flow challenges and this review shows that it is where the main obstacle lies. High-
level understanding of emulsification is paramount for smooth pumping and transport of emulsions through
pipes and here we show that several mechanisms are in play and that need to be considered for a smooth
operation that involves an emulsified acid. Again, pipeline design and specifications must be properly handled, as
various emulsions possess unique and distinct flow patterns. Core flooding constitutes a mode of investigation
that guides how to achieve the optimal emulsified acid volume during injection and field trials; such studies are
highlighted. More importantly, part of the objectives herein is to present some of the rheological approaches that
will assist in the assessment of drag of a specific emulsion system which is very valuable when it comes to an
assessment of how various additives impacts the drag. Further, this review shows that there is still room for
improvement when it comes to the formulation of smart acid emulsions with an emphasis on quick pumping into
the oil well without extreme pressure build-up or pressure drop. Functionalized polymers, either organic or
inorganic (here primarily organoclays), that are soluble in either water or oil and stable in strong acid can
mitigate some of the challenges while pumping acid emulsions. Novel nanomaterials with a high surface area in
combination with thermal and acid resilience have also recently gained traction when it comes to the formation
of new classes of emulsions that would prove valuable in oilfield stimulation. Overall, the application of
emulsified acid systems provides a route to better controlled and more efficient acid stimulation jobs with the
drag being the remaining challenge that should be properly managed.

1. Introduction exist; one such example is that of water-in-oil-in-water emulsions which

essentially is a multiple emulsion system. The water-in-oil-in-water
An emulsion is a disperse mixed system of two immiscible phases – emulsion system consists of tiny water droplets suspended in large oil
usually liquids. In an emulsion system, one of the phases is dispersed in droplets and this large oil droplet remain suspended in continuous water
the other via the formation of micellar structures that involve hydro­ phase (Garti and Aserin, 2013).
phobic and hydrophilic interactions between water, oil, and surfactants Emulsification requires high shear mixing and the presence of
(also referred to as emulsifiers). Emulsions can be classified based on the surface-active agents. The droplet size of the dispersed depends on
type of dispersed and continuous phases (Piacentini, 2014). The two several factors where one is the applied shear during mixing, the higher
principal classes are water-in-oil emulsions (water as a dispersed phase the shear rate the smaller the droplet size of dispersed phase; this will
in continuous oil phase) and oil-in-water emulsions (oil is dispersed in result in a tight emulsion. Another important parameter that influences
continuous water phase). The water-in-oil emulsion system is also the emulsion tightness is the type and concentration of the emulsifier.
referred to as an inverse emulsion and the oil-in-water system is referred An emulsion system with very small and closely packed dispersed
to as a direct emulsion. More complex emulsion configurations also droplets is usually considered tight where a loose emulsion results when

* Corresponding author.
E-mail address: [email protected] (T. Solling).

https://doi.org/10.1016/j.petrol.2021.109569
Received 30 July 2021; Received in revised form 10 September 2021; Accepted 26 September 2021
Available online 28 September 2021
0920-4105/© 2021 Elsevier B.V. All rights reserved.
A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

the droplets are large (Raya et al., 2020). The macro-emulsions are more and acid stimulation (Schramm, 2006). An example is acidizing which is
susceptible to coalescence as they are thermodynamically unstable. utilized to improve the productivity of the injector and producer wells.
With time, this instability becomes more pronounced because of De Groote (De Groote, Louis) first introduced the use of emulsified acids
decreasing interfacial energies. Micro-emulsions, on the other hand, are to the oil and gas industry. The choice of acid depends upon the lithology
considered to be thermodynamically stable in most cases (Eastoe et al., of the subsurface but is usually restricted to hydrochloric acid (HCl) and
2013). hydrofluoric acid (HF). The reaction between HCl and carbonates results
The mechanisms that are in play when emulsions destabilize involve in a salt, carbon dioxide, and water. In the case of sandstone, the acid of
several components such as flocculation, coalescence, sedimentation, choice is HF where the combination of acidic conditions and fluoride
Ostwald ripening, creaming, and phase inversion (shown in Fig. 1) (Shao ions leads to rupture of the Si–O–Si silicate network (Shafiq et al., 2019).
et al., 2020; Zhang et al., 2011). Flocculation results from the formation The volume of the acid that is required (volume per foot of formation) is
of flocks of emulsion droplets (without rupture of the stabilization layer assessed based on the required penetration depth in combination with
at the interface) due to attraction between the droplets (Mao and Miao, the penetration efficiency; it will vary depending upon the design ob­
2015). The influences that can lead to flocculation include (but are not jectives and characteristics of the specific formation. Volumes ranging
limited to) gravitational force, Brownian force, centrifugation and a from 10 to 500 gallons per foot are common in acidizing jobs. At the 500
reduction in repulsive energy in comparison to van der Waals energy are gallons per foot end of the interval, the quantity is indeed rather large
responsible (Payet and Terentjev, 2008). The flocculation is not a but in a matrix acidizing job with 25% porosity, the acid will penetrate
desirable property as it will promote creaming and coalescence of the no more than 20 feet into the formation from the wellbore (Treatment,
droplets (Chanamai and McClements, 2000). The gravitational separa­ 2014). In a fracture acidizing job, the acid propagation will depend upon
tion resulted in creaming or sedimentation of the emulsion droplets. the fracture length (normally under a few hundred feet) (Rabbani et al.,
When the dispersed phase is lighter than the continuous phase then the 2018). The application of acids poses a significant corrosion risk in the
droplets rise to the surface due to buoyancy; a process that is referred to well tubular and necessitates the use of a (non-metallic) coil tubing unit
as creaming. Sedimentation, on the other hand, is when the emulsion for the injection process (Condanni et al., 1997). Moreover, the rate of
droplets merge to form bigger droplets that then settle at the bottom. reaction between the formation minerals and the acid is difficult to
Upon coalescence, the smaller droplets come in contact with one control (Sidaoui et al., 2016; Johnson et al., 2016). The usual challenge
another and merge to form large droplets. The average droplet size in an is that the reactivity of the acid wears off very rapidly when transiting
emulsion increases with time due to coalescence. Ostwald ripening is the from the wellbore into the formation. Essentially, the rapid reaction
main phenomenon behind the formation of larger droplets at the between formation minerals and acid leads to depletion of the acid in the
expense of smaller droplets (Taylor, 1998). In coalescence, the droplets near-well-bore region rendering the deeper parts of the formation un­
of the dispersed phase come in direct contact with each other to form treated. The creation of long wormholes is the main objective of the
larger droplets whereas in Ostwald ripening, the external phase provi­ acidizing treatment (Fig. 3). This objective is difficult to achieve pri­
des/acts as a transfer medium (Hansen, 2020). marily because of the rapid acid-rock reaction which results in fast acid
Emulsifiers stabilize emulsions by decreasing the rate of droplet consumption. Moreover, the viscosities of acidic aqueous solutions are
coalescence (Posocco et al., 2016). Essentially, they alter the interfacial close to those of water which makes them travel through formation in­
behavior, which to a large extent is responsible for the coalescence of the tervals with high permeability just as water, leaving the (challenging)
dispersed droplets. Emulsifiers can largely be categorized into bipolar low permeable zones untreated (Zakaria and Nasr-El-Din, 2016).
organic molecules - surface-active agents in general - and solid particles All these conventional problems can be resolved by controlling the
(Fig. 2). The solid particles can be both water-wet and oil-wet; they acid reaction rate with the formation rock (Shafiq and Mahmud, 2017)
self-organize at the interface between the continuous and the disperse by, e.g., emulsification which will lower the reaction rate and in addi­
phase to provide a steric phase barrier that prevents coalescence (Gon­ tion minimize the contact between the acid and well tubular. Emulsified
zalez Ortiz et al., 2020). An emulsion that is stabilized by solid particles acid is also found to be showing good sweep efficiency, zonal coverage,
is referred to as a Pickering emulsion (Saikia and Sultan, 2020). The and acid distribution particularly in heterogeneous reservoirs (Buijse
surface-active agents, on the other hand, are soluble in both phases. and Van Domelen, 2000). The use of emulsified acid for acidizing is not
They have hydrophobic as well as hydrophilic branches with an affinity only academically interesting it also have proven its worth in a number
towards oil and water respectively and forms an interfacial film at the of field application cases and the results are also encouraging (Al-Anazi
interface of the two phases with a reduction in the interfacial tension, as et al., 1998; Kasza et al., 2006; Fatah and Nasr-El-Din, 2010; Cassidy
a result, a decrease in interfacial tension leads to enhanced droplet et al., 2012; Zakaria et al., 2015; Siddiqui et al., 2006; Norlee et al.,
dispersion and thus a larger propensity for emulsification (Binks et al., 2019; Jafarpour et al., 2017; Fredd et al., 2017; Yousufi et al., 2019;
1999). Nasr-El-Din et al., 2000; Mohamed et al., 1999; Bartko et al., 2004;
Emulsion systems have found many applications in the oil industry Nasr-El-Din et al., 2001a; Nasr-El-Din et al., 2008a; Nasr-El-Din et al.,
such as in drilling fluids, enhanced oil recovery, crude oil transportation, 2008b; Jackson et al., 2011; ZHANG et al., 2008). In
surfactant-stabilized emulsion systems, drag challenges are severe. The
reason is the presence of surfactants, which lowers the interfacial ten­
sion between the dispersed and the continuous phase because of which
smaller droplet size of the dispersed phase is obtained. Small droplets
flow along with the turbulent eddies, and consequently, the turbulence
suppression effect gets eliminated, which resulted in negligible
drag-reduction (i.e., a significant drag has to be alleviated in such cases).
This phenomenon is prominent when the droplet size is smaller than the
length scale of turbulence (Omer and Pal, 2013). An alternative expla­
nation for the drag of surfactant stabilized emulsion systems is based on
their higher viscosity (Ashrafizadeh et al., 2012). It has been pointed out
that with an increase in surfactant concentration the viscosity of the
emulsion system increases as well; the reason for this is anchored in the
smaller size of the dispersed droplets with increasing surfactant con­
centration. This leads to a stronger interaction between the droplets
Fig. 1. Different emulsion destabilization mechanisms (Shao et al., 2020). (Ashrafizadeh et al., 2012; Otsubo and Prud’homme, 1994). To phrase it

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A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

Fig. 2. Classical emulsion (surfactant stabilized) and Pickering emulsions (Chevalier and Bolzinger, 2013).

and core flooding measurements of emulsified acids for oil reservoirs

stimulations.
2. Emulsification of Aqueous Acid Diesel is commonly used as the oil
phase for the emulsification of strong mineral acids because of its
availability and cost (Sidaoui et al., 2017; Sidaoui and Sultan, 2016).
Apart from diesel, aromatics, kerosene, refined hydrocarbons, or their
mixtures are among the petroleum products that could be utilized for
acid emulsification. Traditionally, 15–28 wt% HCl is mixed with the
hydrocarbon in question and a surfactant to form a stable emulsion
(Cairns et al., 2016a). Depending on the surfactant in play, the emulsi­
fied acid system either acts as an acid being dispersed in a hydrocarbon
medium or as an aqueous solution of acid as the external phase. The
mechanism for the acid release under reservoir conditions is governed
by factors that include pressure, temperature, capillary force, and pH.
These parameters determine when the emulsified acid droplets are to
break spontaneously and slowly release the acid. The standard route to
an emulsified acid system entails mixing a suitable emulsifier with oil (e.
g., diesel). If the aim is a Pickering emulsion one would employ solid
particulate matter in the form of, for example, clay and zeolites (Cairns
et al., 2016b). An aqueous solution containing 10–28 wt% acid is then
added in a stepwise manner into the oil mixture and agitated for a
specified period. Various volume ratios of oil: aqueous (acid solution)
ranging from 10:90, 20:80, 30:70, 40:60, and 50:50 have been proposed
(Ahmed et al., 2018; Siddiqui et al., 2006; Yousufi et al., 2019; Sayed
Fig. 3. A series of wormholes that are created by different emulsified acid and Nasr-El-Din, 2013; Sayed et al., 2014; Bazin, 2001; Cairns et al.,
systems (Ahmed et al., 2018).
2016b; Aldakkan et al., 2018; Dashti et al., 2007; Al-Hassan et al., 2017;
Al-Mutairi et al., 2007; Pandya et al., 2013; Nasr-El-Din et al., 2001b;
slightly; lowering of the viscosity of an emulsion will lead to an apparent Tupã et al., 2016; Manakhayev et al., 2018; Navarrete et al., 2000;
reduction of the drag that is associated with pumping – the observable is Daeffler et al., 2018; Navarrete et al., 1998; Fatt and Chittum, 1953;
pressure, and a high-pressure drop will be seen as a reduction of the Jafarpour et al., 2019; Wadekar and Pandya, 2014) in the literature.
drag. Another method of preparation involves mixing the additives (such as
The stability and drag of a given emulsion is of course a key opera­ inhibitors, solid particle agents, etc.) with the acid solution separately
tional factor that determines pumpability and placement of the acid into and then perform emulsifier and diesel agitation in a separate container
the zone of interest. For successful implementation of an emulsified acid at high speed (Sayed et al., 2012a). Table 1 highlights the compositions
in an acidizing job it is required that the emulsion system remains stable of different emulsified acid systems developed for oil wells stimulations.
until it is successfully pumped into the target reservoir zone. In this way, It is clearly shown in this table that diesel is the mostly used crude oil
the intended depth of penetration could be achieved. The stable emul­ equivalent and cationic surfactants are preferred to stabilize emulsified
sions provide higher drag, which necessitates the use of a drag-reducing acids. Besides, corrosion inhibitors are also added to the acid solution to
agent. Incorporation of drag-reducing agents such as oil-soluble or mitigate the adverse effect of pipeline corrosion while solid particle
water-soluble polymers (Al-Yaari et al., 2009, 2012, 2013; Omer and agents are sometimes included in acid emulsions to achieve considerable
Pal, 2010; Sokhal et al., 2019) and nanomaterials (Al-Yaari et al., 2014a) thermal stability and other added favorable features such as reduction of
in the emulsion for the intent of pressure drop reduction have not been the drag. There are often challenges in making all additives play
fully solved and there is significant room for improvement. With the together and this persists to be one of the challenges in designing
help of core flooding experiments (Zakaria and Nasr-El-Din, 2016; emulsified acid systems that work in the field.
Ahmed et al., 2018; Nasr-El-Din et al., 2000; Mohamed et al., 1999;
Sayed et al., 2012a; Sayed and Nasr-El-Din, 2013; Kumar et al., 2014a; 2. Reaction kinetics of emulsified acids
Sayed et al., 2014; Bazin and Abdulahad, 1999; Sayed et al., 2018;
Cairns et al., 2016a; Bazin, 2001; Cairns et al., 2016b; Kumar et al., An essential component of the reaction between an emulsified acid
2014b; Sayed et al., 2012b; Aldakkan et al., 2018; Kumar et al., 2018; system and calcite (or dolomite) is the translocation of acid droplets in
Sayed et al., 2012c), some aspects of the problem have been investigated the oil phase to the rock surface, which eventually leads to acid droplet
with the focus on the possibilities of deploying emulsified acids for breakage and reaction with the rock surface. Usually, the surface reac­
stimulation. This review compiles that data to elucidate the mechanism tion that occurs between HCl and calcite is very fast and the rate of acid
of the emulsification process, thermal resilience, rheological properties, diffusion onto the surface is high and essentially controlling the overall

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A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

Table 1
Compositions of different emulsified acids for reservoir stimulation.
S/ Oil Acid solution Emulsifier Solid particle agents Inhibitors Ref.
No

1. Diesel, aromatics, 10-28 wt% Cationic surfactants 0.1–0.75 wt% (Clay based cationic ammonium - Cairns et al.
kerosene, refined (HCl, H2SO4, materials, organoclay, based blend (2016b)
hydrocarbon HNO3) zeolite)
2. Diesel 7% HCl Petroleum sulfonate surfactant and None none Bazin and
nonionic emulsifier Abdulahad (1999)
3. Diesel 15 wt% HCl Surfactant 1 *hlb = 4.3; surfactant 2 None none Sarma et al.
*hlb = 15 (2007)
4. Diesel 15 wt% HCl Cationic surfactants None Additive (e.g., Inhibitor) Al-Anazi et al.
(1998)
5 Diesel 15 wt% HCl cationic emulsifier (blend of cationic None Additive (e.g., Inhibitor) Sayed et al.
surfactant, isopropanol, and petroleum (2012c)
distillate)
6. Diesel 15 wt% HCl Cationic emulsifier None Additive (e.g., Inhibitor) Sayed and
Nasr-El-Din
(2013)
7. Diesel 15 wt% HCl Cationic emulsifier None Additive (e.g., Inhibitor) Al-Douri et al.
(2013)
8. Diesel 28 wt% HCl cationic surfactant None Inhibitor used Nasr-El-Din et al.
(2001a)
9 Diesel 15 wt% HCl cationic emulsifier None Inhibitor used Sayed et al.
(2013)
10 Diesel 15 wt% HCl cationic emulsifier None quaternary amine-based Al-Mutairi et al.
compound (2009)
11 Diesel 15 wt% HCl cationic emulsifier None Inhibitor: an aliphatic Nasr-El-Din et al.
amine; chelating agent: (2000)
EDTA
12 Diesel 15-28 wt%HCl Emulsifier used None Inhibitor used Navarrete et al.
(2000)
13 Waste oil 15 wt% HCl cationic emulsifier None Inhibitor used Sidaoui et al.
(2016)
14 Waste oil 15 wt% HCl cationic emulsifier None Inhibitor used Sidaoui and
Sultan (2016)
15 Waste oil 15 wt% HCl cationic emulsifier None Inhibitor used Sidaoui et al.
(2017)
16 Waste oil/Diesel 28 wt% HCl cationic emulsifier Nanoclays Inhibitor used Ahmed et al.
(2018)
17 Diesel HCl Surfactants blends (*hlb of 4.3 and 15) None none Yousufi et al.
(2018)
18 Kerosene 1.5–15 wt% HCl Alkonat L90 (nonionic surfactant) and None Inhibitor used Neuma et al.
n-butanol (co-surfactant) (2020)
19 Diesel 20 wt% HCl Surfactant Clay Inhibitor used Al Mubarak et al.
(2015)

*hlb: Hydrophilic-lipophilic balance.

reaction rate (Al-Mutairi et al., 2009). In the case of an emulsified acid (above 100 ◦ C) to avoid early release of acid into the formation (Cairns
system, diffusion starts to be the bottleneck of the stimulation process et al., 2016a).
(Navarrete et al., 2000; Wadekar and Pandya, 2014). The reason is that
proton transfer reactions normally are considered to proceed without a 3. Stability of emulsified acid systems
barrier and thereby every H3O+/carbonate collision will lead to a re­
action. The collisions are hindered when the oxonium ions need to tra­ Stability of a typical emulsified acid system that is targeted for car­
verse a range of interfaces because of being wrapped in an emulsion bonate reservoir stimulation is usually a significant challenge. The in­
(each of which is associated with a barrier). Thus, acid transport (the fluence of strongly acidic environment coupled with harsh reservoir
diffusion of H3O+) becomes the limiting factor. Rock mineralogy and the conditions is significantly reducing the emulsion stability (Singh et al.,
presence of clay traces also have an important impact on the overall 2017). An operational classification of a thermally stable emulsified acid
reaction kinetics (Sayed et al., 2013). Owing to significant retardation of system dictates that it should not separate into distinct oil and aqueous
the diffusion in the case of the emulsified acid system, its rate of reaction phases upon heating to ≥130 ◦ C for a minimum of 4 h (Cairns et al.,
with carbonate is approximately 8.5 times lower than that of regular 2016b). A stable emulsified-acid system enables deeper penetration and
acids, and this retardation paves way for deeper penetration into the inhibits localized dissolution within fractures (Singh et al., 2017). Basin
formation (Al-Mutairi et al., 2009). The reaction between the HCl and and Abdulahad (Bazin and Abdulahad, 1999) investigated the stability
calcite or dolomite (Eqs. (1) and (2)) yields products that are readily of several emulsified acid systems at ambient and slightly elevated
soluble in water. (50 ◦ C) temperatures. Their results showed that the acidic emulsion was
much more stable at ambient temperature. Sarma et al. (2007) argued
CaCO3 (s) + 2HCI(aq) CaCl2 (aq)+CO2 (g)+H2 O(1) (1a)
that the use of a stable emulsified acid system with a controlled diffusion
rate could enable proper penetration of the reactive fluid and also allow
CaMg (CO3 )2 (s) + 4HCl(aq) CaCl(aq) + MgCl(aq)+2CO2 +2H2 O(1) (2a)
an ideal wormhole propagation even at very low injection rates. They
Although, emulsification of acid in oil (e.g. diesel) lowers the reac­ further suggested that the stability of the emulsified acid system is
tion rate and favors efficient wormhole formation, the challenge is how greatly influenced by the property of the emulsifier (surfactant) as also
to enhance the stability of acid emulsions at elevated temperatures the HLB number affects the type of emulsion that is ultimately formed.

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A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

Al-Anazi et al. (1998), designed an acid-in-diesel emulsion that is stable

for more than 72 h at ambient temperature (24 ◦ C); however, the sta­
bility decreases with increasing temperature. Several studies have
actually assessed the stability of different emulsified acid systems with
very varied experimental outcomes and subsequent conclusions (Al-A­
nazi et al., 1998; Yousufi et al., 2019; Nasr-El-Din et al., 2000; Nas­
r-El-Din et al., 2001a; Sayed et al., 2018; Cairns et al., 2016a; Aldakkan
et al., 2018; Sidaoui et al., 2017; Sidaoui and Sultan, 2016; Al-Douri
et al., 2013; Al-Mutairi et al., 2009; Neuma et al., 2020; Singh et al.,
2017; Carvalho et al., 2019; Us et al., 2015). The period after emulsion
has been formed has an impact on its stability. It has been reported that
emulsion can separate into phases after long period of preparation
depending on the water content (Wong et al., 2015). Likewise, the sta­
bility of acid emulsions would largely depend on the type of oil used,
emulsifier type and concentration, and additives such as corrosion in­
hibitors. (Ahmed et al., 2018). It is also imperative to take into cogni­
zance, the fact that emulsifiers’ densities are usually higher than that of Fig. 4. Viscosity of a range of emulsified acid systems formulated from
either water or oil, therefore, there is likelihood of interfacial layers different amounts of HCl at various temperatures (250, 300, and 350 ◦ F)
increasing the droplets overall density and as such, emulsifiers that are (Navarrete et al., 2000).
tightly packed at the water-oil interface tend to create denser interface
and subsequently generate a huge impact (McClements and Jafari, scrutinized further by determining the viscosity of each HCl solution
2018). Either acidic or alkaline medium has enormous influence on the (Fig. 5) in the same temperature interval. The viscosity trend was similar
stability of emulsions generally. Emulsions exhibiting high acidity with to that of emulsified acids, whereas the absolute values for the acid
pH around 2.5 have been reported to be unstable and stability index solutions are generally lower. By and large, rheological characteriza­
decreased swiftly (Abdolmaleki et al., 2016). Anjali and Basavaraj tions (Zakaria and Nasr-El-Din, 2016; Ahmed et al., 2018; Al-Anazi et al.,
(2018) described in a study that Pickering emulsions are better formed 1998; Kasza et al., 2006; Cassidy et al., 2012; Yousufi et al., 2019;
and much stable within of pH 4 to 11. Aside emulsion’s pH, incorpo­ Nasr-El-Din et al., 2000; Mohamed et al., 1999; Nasr-El-Din et al.,
ration of salts in emulsions is another key factor that should be given 2001a; Nasr-El-Din et al., 2008b; Sayed et al., 2012a; Sayed et al., 2014;
considerable attention when designing acid emulsions for well stimu­ Cairns et al., 2016a; Sayed et al., 2012b; Kumar et al., 2018; Sidaoui and
lation. According to reports, monovalent salts had negligible effects on Sultan, 2016; Al-Mutairi et al., 2007; Nasr-El-Din et al., 2001b; Tupã
emulsion stability (Abdolmaleki et al., 2016; Anjali and Basavaraj, et al., 2016; Navarrete et al., 2000; Navarrete et al., 1998; Jafarpour
2018), however, increasing concentration of NaCl (sodium chloride) can et al., 2019; Al-Douri et al., 2013; Sayed et al., 2013; Al-Mutairi et al.,
improve emulsion stability in some instances (Adewunmi and Kamal, 2009; Neuma et al., 2020; Carvalho et al., 2019; Liu et al., 2003; Sergeev
2019). Essentially, more experimentation is needed to consistently and Kinzyabaev, 2016; Sabhapondit et al., 2012; Solares et al., 2011;
achieve robust and thermally stable emulsified acid systems particularly Appicciutoli et al., 2010; AlOtaibi et al., 2017; Maheshwari et al., 2016)
those that are also stable with the proper composition of additives being have been employed to assess the pump efficiency of emulsified acid
in play and as a recommendation, systematic and proportionate mixing systems that are to be deployed in oil well stimulation operations.
of multiple emulsifiers in the water-oil formulation could possibly pro­
duce impactful effect on the particle size distributions and stability of 5. Flow characteristics of oil-water mixtures in pipes
emulsion droplet sizes. Also, a detailed microscope screening of emul­
sified acid systems is suggested. Concurrent flow of oil and water in pipelines is a common practice in
the petroleum industry. The flow pattern of oil-water mixtures is so
4. Rheology of emulsified acid systems critical and it becomes imperative to account for the presence of water
during the flow to capture the detailed behavior and to design pipelines
The viscosity of an emulsified acid is a key factor during injection properly (Xu, 2007). The diverse properties of oil and the ability of
into carbonate reservoirs. Rheology is one of the techniques that has oil-water systems to exhibit rheological Newtonian or non-Newtonian
been used to characterize the behavior of emulsified acids. Sarma and
colleagues (Sarma et al., 2007) showed that reservoir zonal coverage is
significantly improved with increased viscosity of the emulsified acid
system in play. The viscosity largely depends on the viscosity of either
the dispersed or the continuous phase, particle size distribution, and the
nature of the emulsifying agents. A viscous acid emulsion may enhance
stability; however, highly viscous acid emulsions may give rise to a large
drag while pumping. Many skills and manipulations are therefore
necessary when formulating emulsified acid systems for applications as
oil well stimulants. Sidaoui et al. (Sidaoui and Sultan, 2016) investigated
the viscosity effect of using different surfactant concentrations in
forming the emulsified HCl. The results of their study showed that
varying surfactant concentrations had an insignificant effect on the
viscosity; conspicuous viscosity change was only noticed at a tempera­
ture of 100 ◦ C and 1.5 vol% surfactants. Al-Anazi et al. (1998) developed
an acid-in-diesel emulsion with a typical Newtonian behavior while in
another study by Navarrete et al. (2000), the viscosity of emulsified acid
system (Fig. 4) was noticed to have increased with an increased amount
of HCl (15%, 20%, and 28%) in the formulated emulsions at all tem­ Fig. 5. Viscosity of distinct HCl solutions at various temperatures (250, 300,
peratures (250, 300, and 350 ◦ F) examined. This behavior was and 350 ◦ F) (Navarrete et al., 2000).

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A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

behaviors, as well as the high-pressure gradient encountered for various understanding the flow patterns and characteristics of oil-water con­
flow patterns makes it more difficult to fully understand oil-water flow current movement in pipelines (Omer and Pal, 2010; Sokhal et al., 2019;
patterns (Izwan Ismail et al., 2015). Specifically, the mobility of emul­ Xu, 2007; Fadaei, 2012; Keleşoǧlu et al., 2012; Santos et al., 2017;
sified acid systems through pipes from the wellhead to the target zone is Tripathi et al., 2020; Pal and Hwang, 1999; Alade et al., 2020; Plasencia
a great concern during oil well stimulation activities. At certain stages et al., 2013; Trallero et al., 1997; Fan et al., 2020; Wang et al., 2011;
during the pumping of emulsified acids, friction loss increases swiftly Edwards et al., 2018; Nädler and Mewes, 1997; Masalova et al., 2003;
which constitutes a very challenging operational situation. Such chal­ Chen et al., 2006). Al-Yaari et al. (2013) found that an oil-soluble
lenges retard the efficiency of any matrix acidizing activity by lowering polymer (e.g., polyisobutylene) and water-soluble polymers (e.g.,
the penetration depth of emulsified acids (Al-Yaari et al., 2014a). To polyacrylamide and polyethylene oxide) were applied as drag-reducing
address the friction problems and enhance the throughput of emulsified agents for stable and unstable water-in-oil and oil-in-water emulsions,
acid related to oil and gas flow in pipelines, researchers have deployed and pressure drop measurements were determined under different flow
drag-reducing additives which are incorporated in formulations of rates using a flow loop methodology (Fig. 6). The results of their
emulsified acid systems. Numerous studies have focused on investigation demonstrated that the addition of a suitable polymer as a

Fig. 6. Flow loop schematic layout for pressure drop measurements of emulsions inside pipes (Al-Yaari et al., 2013). Labels: 1 and 2 – tanks, 3 and 4 – centrifugal
pumps, 5 and 6 – magnetic flow meters, 7 and 8 – pressure transducers, and 9 – Colling system with chiller.

6
A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

drag reducer also increases the stability of emulsions at ambient tem­ ΔP

× 2D
perature. Furthermore, the stability of the emulsified acid system in­ f = ΔL (2b)
creases as the molecular weight of the polymer increases. On the other ρu2
hand, the emulsion stability and polymer insensitivity to drag reduction
where f represents the Darcy friction factor, ΔP
ΔL is the pressure gradient
is retarded with increasing temperature. Finally, their results showed
that injection of specific polymers caused a pressure drop reduction in (Pa/m), D is the pipe diameter (m), ρ is the emulsion density (kg/m3),
all the emulsion types (stable water-in-oil, stable oil-in-water, and stable and u denotes emulsion average velocity (m/s). However, when emul­
concentrated water-in-oil) examined, and this reduction effect increased sions behave as single-phase Newtonian fluids, the friction factor f is
as polymer concentration increased. expressed in terms of the Reynolds number (equation (3) and equation
Apart from using polymers to control and minimize a pressure drop, (4))
Al-Yaari et al. (2014a) also carried out a detailed study to described the 16
effect of organoclay on the pressure drop that was associated with f= (3)
Re
pumping a surfactant stabilized (non-acidic, though) water-in-oil
emulsion. Their result showed that the addition of organoclay gave f = 0.079 Re− 0.25
(4)
rise to approximately a 25% reduction in the emulsion pressure drop.
Another study by Al-Yaari et al. (2012) was conducted using water where Re denotes the Reynolds number. Equation (3) is valid for laminar
holdup measurements of an oil-water flow in horizontal pipes (Fig. 7) in flow and equation (4) is termed the Blasius equation, valid for turbulent
the presence and absence of drag-reducing polymers (DPR). The result of flow in smooth pipes. The emulsion pressure drop reduction can how­
their investigation revealed that the injection of DRP into the oil-water ever be determined from equation (5).
mixture significantly influenced the water holdup, indicating the pros­ ΔPw − ΔPw’
pect of using DPR for separating and changing the distribution of PDR = (5)
ΔPw
droplets in oil-water mixtures. Flow characteristics of different emulsion
types have also been addressed in other similar studies by Al-Yaari et al., where ΔP is the emulsion pressure drop and subscript w indicates the
2013, 2014b, 2015. Determination of the pressure drop reduction (PDR) absence of drag-reducing agents (e.g., polymers, nanomaterials, etc.),
for emulsions is related to both the viscosity (η) and the friction factor (f) and the w’ subscript represents that the emulsion pressure is measured
of the emulsion. Under the pipe flow shear rate (Eq. (1)), emulsion with the incorporation of drag-reducing agents. Another key issue is the
viscosity can be extracted from the rheological measurements, which fact that different specifications of pipes (Table 2) have to a large extent
can be further applied to calculate the Reynolds number (Re) associated impacted the flow pattern of various kinds of emulsions. Realistically, to
with an emulsified acid system. The emulsion friction factor (f) can ensure decent flow inside pipes, particularly in the case of an emulsified
therefore be estimated from Eqs. (2), (3), and (4) (Al-Yaari et al., 2014a). acid system, a high degree of understanding of the relation between
Here γ˙w represents the true wall shear rate (s− 1), Q is the volumetric pumping rates and emulsification processes is required. There will be a
flow rate (m3/s), R is the pipe radius (m), τw is the wall shear stress (Pa), necessity to deploy suitable drag-reducing agents that can enhance
and emulsion viscosity could be expressed as η = τw / γ˙w . Literature emulsion stability and minimize emulsion pressure drop at elevated
studies have established that f and PDR associated with emulsions can be temperatures. Under the harsh conditions of an oil reservoir, a detailed
expressed as follows: knowledge of pipe design is pivotal, moreover, functionalization of
polymers and nanomaterials should be targeted to optimize the con­
stituents of the emulsified acid systems.

Fig. 7. Flow loop schematic layout for water holdup measurements in the case of oil-water mixtures with and without drag-reducing polymers (Al-Yaari et al., 2012).
[ ]
4 ​ Q 3 1 d(InQ)
γ˙w = 3 + (1b)
π R 4 4 d(Inτw )

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A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

Table 2 Table 2 (continued )

Different specifications for oil-water flow inside pipes. S/ Specifications for oil-water Remark Ref.
S/ Specifications for oil-water Remark Ref. No flow in pipes
No flow in pipes
m and entrance length = additive in the aqueous
1 Plexiglass pipe: D = 2.54-cm, To test water holdup with Al-Yaari 2.73–3.75-m. phase. The presence of
L = 10-m, and ID = 25.4 mm. and without DRP. Injection et al. (2012) polymer additives has a
of DRP significantly significant impact on
influenced the water turbulent drag reduction.
holdup. 9 Stainless steel pipe with ID Comparative studies of the Plasencia
2 Acrylic resin pipe: 2.54-cm The effect of DRP on the Al-Yaari = 2.2-cm and length of 6-m. pipe flow of W/O were et al. (2013)
and 1.27-cm ID, and total flow pattern of water-oil et al. (2013) investigated. No clear-cut
length of flow loop = 11-m emulsions was studied. correlation between the
Pressure drop effective viscosity and
measurements were also inversion point.
conducted. Emulsion 10 Acrylic pipe with ID = 5.08- Flow experiments were Izwan Ismail
stability enhancement and cm and length to diameter conducted for oil-water et al. (2015)
pressure drop reduction ratio = 1311 two-phase flow in a
were noticed in the presence horizontal pipe loop. Water
of DRP. holdup was noticed to be
3 Acrylic resin pipe: 2.54-cm The influence of water Al-Yaari highest at the dispersion of
and 1.27-cm ID, and total fraction and flow conditions et al. oil in water and lower when
length of flow loop = 11-m on the flow properties of (2014b) water is dispersed in oil.
stable water-oil emulsions
were investigated.
Significant increase in 6. Core flooding and field trials of emulsified acid systems
emulsion stability, viscosity,
and pressure drop was
An ideal emulsified acid system minimizes the volume that is
observed for water increase
up to 70%. required to reach a breakthrough. Core flooding experiments by Bazin
4 Acrylic pipe: D = 2.54-cm, L Effects of DRP on the flow Al-Yaari and Abdulahad (1999) revealed that acid-in-diesel emulsions could
= 10-m, and ID = 25.4 mm. behavior of oil-water in et al. (2009) provide deeper penetration with moderate injection volume at a low
horizontal pipes were flow rate. Al-Anazi (Al-Anazi et al., 1998) formulated an emulsified acid
studied. Injection of about
10–15 ppm water-soluble
system that was successfully applied in the field with a considerable
polymer resulted in about increase in oil production. In a core flood test that was conducted by
65% drag reduction in some Sayed et al., at 104 ◦ C, the optimum injection rate to pump the acid
instances. Also, a reduction emulsion (70% HCl and 30% diesel; 1 vol% emulsifier) developed was
in pressure gradient was
found to be within 5–7 cm3/min (Sayed et al., 2012c). Series of core
recorded at high mixture
velocity. flooding tests (Zakaria and Nasr-El-Din, 2016; Ahmed et al., 2018;
5 Acrylic resin pipe: 2.54-cm The effect of salinity on the Al-Yaari Nasr-El-Din et al., 2000; Mohamed et al., 1999; Sayed et al., 2012a;
and 1.27-cm ID, and total flow characteristics of et al. (2015) Sayed and Nasr-El-Din, 2013; Kumar et al., 2014a; Sayed et al., 2014;
length of flow loop = 11-m. surfactant stabilized Bazin and Abdulahad, 1999; Sayed et al., 2018; Cairns et al., 2016a;
emulsions was examined.
O/W emulsions formed at
Cairns et al., 2016b; Kumar et al., 2014b; Sayed et al., 2012b; Aldakkan
salinity ≤5kppm while the et al., 2018; Kumar et al., 2018; Sayed et al., 2012c) have been per­
stability of these emulsions formed in the laboratory to evaluate the depth penetration of emulsified
decreased with increasing acids and to ensure that volumes injected are well controlled and
salinity. Salinity ≥20kppm
conserved. Table 3 highlights the chosen oil, HCl aqueous solution, type
favored W/O emulsions and
the stability of emulsions of core samples and operating conditions employed by many researchers
enhanced with increasing to evaluate the penetration depth of emulsified acid systems when
salinity. Reduction in injected into cores during series of core flooding experiments. A variety
emulsion viscosity and of emulsified acidic chemicals have also been deployed and tested suc­
pressure drop was observed
especially when salinity
cessfully in a range of field applications across but have also revealed,
≥20kppm. challenges and lessons for further improvement. In a study conducted by
6 Horizontal pipes with The impact of organoclay Al-Yaari Manakhayev et al. (2018), a new acid stimulation protocol was designed
different IDs: 0.0254-m and (OC) on the pressure drop of et al. from hydrochloric acid with basic additives, fiber-laden diverting acid,
0.0127-m. stable W/O emulsions was (2014a)
and viscoelastic diverting acid (VDA) with the successful implementa­
studied. The addition of OC
in W/O emulsions resulted tion of these chemicals in three drilled wells.
in the decrease of emulsion
viscosity. Besides, injection 7. Conclusion
of OC in concentrated W/O
caused about a 25%
reduction in the emulsion
Emulsified acid systems that are applied for wellbore treatments and
pressure drop. reservoir stimulation are reviewed herein. Diesel and hydrochloric acid
7 The length and width of the Micro analysis of (Fan et al., (HCl) have proven successful in producing emulsified acid systems with
loop were 4-m and 0.6-m, rheological properties of 2020) the common stabilizer being a range of cationic surfactants. Thermal
respectively, the ID of the different water contents of
stability and viscosity variations of emulsified acid systems are high­
pipe was 12-mm. water-in-waxy crude oil
emulsions was analyzed lighted. The flow characteristics of oil-water systems are also buttressed
using an under flow loop. herein. It is central to carefully design the chemical composition of the
8 Stainless and PVC pipes Pipeline flow behavior of Omer and emulsified acid systems to obtain the optimal flow pattern for successful
having ID = 0.0089–0.0265- W/O emulsions was studied Pal (2010) field applications. At this stage, there is still a gap to be bridged and to a
with and without polymer
large extent, the field is dominated by trial-and-error approaches. Some
experiments are taken to indicate that the incorporation of

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A.A. Adewunmi et al. Journal of Petroleum Science and Engineering 208 (2022) 109569

Table 3
Parameters used to evaluate the penetration depth of emulsified acids in core samples during various core-flooding experiments.
S/ Oil type Acid solution Core sample Injection rate Temp. Pressure Ref.
No

1. Diesel HCl Indiana limestone - Diameter: 1.5-in, thickness: 0.5–10 cm3/min 300 ◦ F 1100 psi Sayed et al. (2012a)
0.75-in
3
2. Diesel 15 wt% HCl Dolomite - Diameter: 1.5-in, length: 6-in 0.5–10 cm /min 300 ◦ F 1100 psi Sayed and Nasr-El-Din
(2013)
3. Diesel 15 wt% HCl Indiana limestone - Diameter: 1.5-in, length: 6-in 0.5–5 cm3/min 250 ◦ F 1100 psi Zakaria and Nasr-El-Din
(2016)
4. Diesel, waste 28 wt% HCl Dolomite - Diameter: 1.5-in, length: 12-in 0.5–10 cm3/min 275 ◦ F 3000 psi Ahmed et al. (2018)
oil
3
5. Diesel 15 to 26 wt% Indiana limestone - Diameter: 1.5-in, length: 12- 0.5–5 cm /min 302 F
◦
3000 psi Aldakkan et al. (2018)
HCl in
6. Crude oil 15 wt% HCl Dolomite - Diameter: 1.5-in, length: 3-in and 6-in 0.5–20 cm3/min 200 ◦ F 1100 psi Kumar et al. (2018)
7. Diesel 15 wt% HCl Indiana limestone - Diameter: 1.5-in, length: 12- 1–5 cm3/min 300 ◦ F 3000 psi Cairns et al. (2016a)
in
8 Diesel 15 wt% HCl Indiana limestone - Diameter: 1.5-in, length: 12- 0.5–10 cm3/min 300 ◦ F 1100 psi Sayed et al. (2014)
in
3
9. Diesel 15 wt% HCl Carbonate 1–10 cm /min 220 F
◦
1100 psi Sayed et al. (2012c)
10. Diesel 15 wt% HCl Indiana limestone – Diameter: 1.5-in, length: 6- 0.5–10 cm3/min 300 ◦ F 1100 psi Sayed et al. (2012b)
in
11. Diesel 7 and 15 wt% Indiana limestone – Diameter: 5-cm, length: 20- 1.6–24.8 cm3/ 50 ◦ C 70 and 175 Bazin and Abdulahad (1999)
HCl cm min bars

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Ahmad A. Adewunmi1, Conceptualization, Writing – original draft 107741-ms.
Supervision, Theis Solling1, Conceptualization, Writing – original draft Al-Mutairi, S.H., Nasr-Ei-Din, H.A., Hill, A.D., Al-Aamri, A.D., 2009. Effect of droplet size
on the reaction kinetics of emulsified acid with calcite. SPE J. 14, 606–616. https://
Writing - Review & Editing Project administration Abdullah S. Sultan2,
doi.org/10.2118/112454-PA.
Conceptualization Project administration Funding acquisition Tinku Al-Yaari, M., Soleimani, A., Abu-Sharkh, B., Al-Mubaiyedh, U., Al-sarkhi, A., 2009. Effect
Saikia1 Writing - Review & Editing. of drag reducing polymers on oil-water flow in a horizontal pipe. Int. J. Multiphas.
Flow 35, 516–524. https://doi.org/10.1016/j.ijmultiphaseflow.2009.02.017.
Al-Yaari, M., Al-Sarkhi, A., Abu-Sharkh, B., 2012. Effect of drag reducing polymers on
Declaration of competing interest water holdup in an oil-water horizontal flow. Int. J. Multiphas. Flow 44, 29–33.
https://doi.org/10.1016/j.ijmultiphaseflow.2012.04.001.
Al-Yaari, M., Al-Sarkhi, A., Hussein, I.A., Abu Sharkh, B., 2013. Effect of drag reducing
The authors declare that they have no known competing financial polymers on surfactant-stabilized water-oil emulsions flow. Exp. Therm. Fluid Sci.
interests or personal relationships that could have appeared to influence 51, 319–331. https://doi.org/10.1016/j.expthermflusci.2013.08.015.
the work reported in this paper. Al-Yaari, M., Hussein, I.A., Al-Sarkhi, A., 2014a. Pressure drop reduction of stable water-
in-oil emulsions using organoclays. Appl. Clay Sci. 95, 303–309. https://doi.org/
10.1016/j.clay.2014.04.029.
Acknowledgments Al-Yaari, M., Al-Sarkhi, A., Hussein, I.A., Chang, F., Abbad, M., 2014b. Flow
characteristics of surfactant stabilized water-in-oil emulsions. Chem. Eng. Res. Des.
92, 405–412. https://doi.org/10.1016/j.cherd.2013.09.001.
We gratefully acknowledge our Haliburton partners, in particular,
Al-Yaari, M., Hussein, I.A., Al-Sarkhi, A., Abbad, M., Chang, F., 2015. Effect of water
Drs. Enrique Reyes and Saleh Al Mutairi for productive scientific salinity on surfactant-stabilized water-oil emulsions flow characteristics. Exp.
discussions. Therm. Fluid Sci. 64, 54–61. https://doi.org/10.1016/j.
expthermflusci.2015.02.001.
Alade, O.S., Al-Ashehri, D.A., Mahmoud, M., Sasaki, K., Sugai, Y., 2020. Evaluation of
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