SPE-191922-MS

Kaolinite Mobilisation in Unconsolidated Porous Media: Effect of Brine

Salinity and Salt Type Na- and Ca Salts

Thomas Russell, Duy Pham, Genna Petho, Mahdi Tavvakoli Neishaboor, and Alexander Badalyan, University of
Adelaide; Aron Behr, Luis Genolet, and Patrick Kowollik, Wintershall Holding GmbH; Abbas Zeinijahromi and Pavel
Bedrikovetsky, University of Adelaide

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Asia Pacific Oil & Gas Conference and Exhibition held in Brisbane, Australia, 23–25 October 2018.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
Existence of clay particles in reservoir rock plays a major role in both oil recovery and formation damage.
Clay mobilisation and consecutive formation damage have been observed during injection of low-salinity
water in oil fields and laboratory coreflood experiments. Hence, this research aimed at understanding and
quantifying the effect of clay type, clay content and composition of injected brine on clay mobilisation.
In order to study the effect of clay content, several unconsolidated cores using kaolinite and sand are
prepared. The clay content of each sample is controlled by mixing an accurately measured mass of kaolinite
with sand. A new procedure is developed to assure: a uniform distribution of kaolinite along the core length,
reproducible preparation of sand-clay mixture, identical compaction of the mixture in all experiments using
axial and overburden stresses, and reproducible permeability data. Each core is initially saturated with high
salinity brine (equivalent to sea water salinity) by creating a constant flow rate of 0.6 M solution through the
core. The experiments continue with stepwise reduction of salinity of the injected solution (6 steps down to
DI water). Around 150 PV of solutions is injected at each step until permeability stabilization. This indicates
that no more kaolinite particles are mobilised. Differential pressure across the core is measured continuously
and particle concentration and the conductivity of the effluent samples are also measured
The kaolinite concentration, solution salinity and valency of ionic species (salt type) are found to be the
controlling factors for clay mobilisation.
The following correlations are established: relationships between initial kaolinite concentration and initial
core permeability, initial kaolinite concentration and degree of permeability damage, and salt type and
permeability damage due to salinity reduction. Experimental data show that a core with lower kaolinite
content has higher undamaged/initial permeability. It is also observed that the lower is kaolinite content the
higher is permeability damage during injection of low salinity water. Significant permeability decline during
low-salinity corefloods is due to mobilization of the kaolinite particles and their capture in pore throats. The
results also show that injection of solution containing divalent ions (Ca) stabilises the kaolinite particles and
prevents their migration during low salinity brine injection.This study is novel in several aspects including:
developing a new methodology for unconsolidated core preparation with desired clay content, studying the
2 SPE-191922-MS

effect of clay content on initial permeability and severity of formation damage and studying the effect of
divalent ions on clay behaviour during low salinity brine injection. The results of this study could be used
to engineer the composition of injected water to minimise formation damage based on rock clay content.

Introduction
Fines migration is the process encountered in porous media in which small particles detach from pore
surfaces and travel through the pore space. The migration path of a detached particle is often terminated
when the particle meets a pore throat smaller than its size. This is referred to as straining and reduces the
permeability of the porous medium. Fines migration plays a critical role in several important processes such
as contaminant transport (Kretzschmar, Borkovec, Grolimund, & Elimelech, 1999) as well as injectivity/
productivity decline in petroleum wells (Civan, 2007).
Understanding and quantifying fines migration relies on knowledge of particle detachment mechanics
as well as the probability of, and permeability damage caused by, particle straining. Technologies designed
to control fines migration, either by inhibiting or inducing it, are based on the detachment mechanics of
fine particles within the pore space. While particle transport and capture are present in deep bed filtration
problems, where particles are suspended in the injected fluid (Sacramento et al., 2015), the discussions in
this text will be limited to the behavior of particles initially attached to the pore grains in the porous media.
Particle detachment is often investigated using a torque balance and a simplification of particle geometry
to that of a sphere. A schematic of an attached particle with the primary acting forces is presented in Figure 1.
While particle detachment could occur by lifting, sliding, or rolling, studies have shown that for the particle
sizes, as well as hydrodynamic and electrostatic conditions encountered by fines in porous media, rolling is
the most likely detachment mechanic (Sharma, Chamoun, Sarma, & Schechter, 1992). The primary forces
acting on the particle are the hydrodynamic drag force, FD, the lifing force, FL, the gravitational force, Fg, and
the electrostatic force, Fe. The drag and lifting force will generate detaching torques, the electrostatic force
will generate an attaching torque, and the gravitational force will generate either a detaching or attaching
torque based on the particles placement within the pore space. Studies have shown that for typical conditions
in porous media, the gravitational and lifting forces are several orders of magnitude smaller than the drag
and electrostatic forces (You, Bedrikovetsky, Badalyan, & Hand, 2015).

Figure 1—Schematic of an attached particle with the primary acting forces with their respective lever arms
SPE-191922-MS 3

As such, detachment is primarily dictated by the strength of the torques generated by the electrostatic
and hydrodynamic drag forces. The equation which governs particle detachment is:

Where ld and ln are the drag and normal lever arms respectively. Both are shown on the schematic
presented in Figure 1. While only a brief description of the forces will be given here, the torque balance
above can be used to quantify the degree of particle detachment due to changes in salinity, fluid velocity,
and temperature (You et al., 2015, Yang et al., 2016).
The drag force is based on Stokes law and was generalised by (Goldman, Cox, & Brenner, 1967) for
various separation distances,h, between the sphere and surface. The expression given by these authors is

Where μ is the fluid viscosity, r is the particle radius, h is the distance between the particle and surface,
is the shear rate, and is the dimensionless shear force.
The torque resulting from this force is:

Where is the dimensionless torque. Tabulated values for and can be found in the publication by
Goldman et al. in 1967.
This equation demonstrates the dependencies of the drag force on the fluid viscosity and flow rate, as
well as the particle radius. The linear velocity dependence explains the presence of fines migration in the
near wellbore region around production and injection wells in petroleum and geothermal reservoirs (Byrne
& Waggoner, 2009) (P. Bedrikovetsky a, A. Vaz b, F. Machado c, A. Zeinijahromi a & S.Borazjani: Skin
Due to Fines Mobilization,
Migration, and Straining During Steady-State Oil Production), where the fluid velocity is high.
The electrostatic force is primarily dependent on the electrostatic properties of fine particles within the
rock and the solution chemistry. Most clays and sand particles are negatively charged (Marshall, 1964) and
ions surround the particles in the form of double layers in aqueous solutions (Graham, 1947). Due to the
sign of the surface charge, more cations are present in these double layers than anions to counteract the
negative surface charges of the particles (Krebs, Thomas, & Moore, 1960).
When a clay particle, such as kaolinite, is in the vicinity of a sand particle, they exhibit a net electrostatic
attraction, despite the similar sign of their surface charges. This attraction is due to the Van der Waals
component of electrostatic interaction which is solely attractive in this context. The two remaining
components of the electrostatic force, being the Born repulsion and the interaction of the double layers
(Electrostatic Double Layer interaction) are both repulsive. The Electrostatic Double Layer interaction
(EDL) is repulsive here due to the similar sign of the surface charges noted above.
Quantifying the total electrostatic interaction involves summing the individual contributions to the
potential energy of the particle-grain system. Relationships for each component are as follows (Derjaguin
& Landau, 1993; Elimelech, Gregory, Jia, & Williams, 2013; Gregory, 1981; Ruckenstein & Prieve, 1976):
4 SPE-191922-MS

Where

Where V is the potential energy, A132 is the haymaker constant, h is the distance between the particle and
the grain surface, λw is the characteristic wavelength of interaction, rs is the particle radius, rg is the pore
grain radius, n∞ is the bulk number density of ions, kB is the Boltzmann constant (4.116 × 10−21 J), T is the
absolute temperature, κ is the Debye-Huckel parameter, ψ1 is a parameter related to the surface potential
of the particle, ψ2 is a parameter related to the surface potential of the pore grain, ρc is the atomic collision
diameter, z is the valence of the cation in solution, e is the elementary charge (1.602 × 10−19 C, and ζparticle
and ζgrain are the zeta-potentials of the particle and grain respectively.
The primary components determining the magnitude and attractive or repulsive nature of the total
electrostatic force are the two zeta potentials, ζparticle and ζgrain, which are dependent on the solution chemistry
and fluid temperature (You et al., 2015, You et al., 2016). Here, as is commonly done (Elimelech, 2013),
the zeta potentials have been used as an approximation of the surface potentials, as the zeta potentials are
more easily measured.
The zeta-potential is based on the theory of the electric double layer. The theory states that at a certain
boundary, referred to as the slipping layer, adsorbed ions will no longer remain adsorbed if the particle
begins moving. By inducing electrophoresis, wherein the particle moves relative to the surrounding fluid,
the potential at this layer can be measured experimentally. This potential is termed the zeta-potential and can
provide insight into the impact of cation type and concentration on the electrostatic force that the particle
experiences.
When the salinity of the solution saturating a rock decreases, less cations will be present to mask the
negative charge of the particles and thus the repulsive EDL component will increase in magnitude. This
change in surface potential is measured through changes in the zeta potential for each solution. Disregarding
the effect of salinity on other components of the interaction potential, the larger the magnitude of the zeta
potential, the larger the repulsive EDL component. The consequence of an increase in the double layer
repulsion is a decrease in the net attraction between fine particles and the rock surface. Given this change,
hydrodynamic forces acting on the particles may become sufficient to detach the particles, inducing fines
migration.
Kia, Fogler, and Reed (1987) investigated the role that the type of cation plays in fines migration. The
authors found that fines migration was more pronounced when the injected cation was primarily sodium and
less pronounced when it was calcium. They related the permeability decline ratio to the ratio of sodium and
calcium in the injected solution. The corefloods were performed on Berea sandstones, which are generally
considered to be representative of typical sandstone reservoir rocks. While compositional analysis was done
on these cores, the complexity of sandstone cores does not allow a direct study of individual mechanisms
of particle detachment. In this study, artificially made cores that contain only kaolinite and chemically pure
silica sand grains are used to reduce number of affecting parameters and significantly simplify the situation.
While this simplification risks the representative nature of the cores, it does allow for a relation between
individual constituent properties and the behaviour of the core.
SPE-191922-MS 5

The current study aims to provide insight into the mechanisms of fines migration and explain the
differences between fines migration in the presence of Na and Ca cations. Coreflood experiments as well as
measurements of the properties of individual constituents are performed to study the aforementioned effects.
The structure of this paper is as follows. Following the introduction, an overview of the methodology of
the experiments is given in Section 2. The results of the experimental corefloods and SEM are presented
and discussed in Section 3, followed by some concluding remarks in Section 4.

Experimental study
Materials.
Cores: The study of kaolinite particle mobilisation was carried out on unconsolidated kaolinite-silica sand
mixtures (artificial cores).
Kaolinite powder, Al2(Si2O5)(OH)4, was washed in deionised (DI) water and dried in an oven at 60 °C
for 24 hours before mixing with sand.
Silica sand with > 99% of silica was sieved to a grain size range such that both particle migration and
straining could occur simultaneously. In order to remove organic and inorganic impurities, the sand was
washed with hexane, then with acetone, later with deionised (DI) water, dried in an oven at 60 °C for 24
hours, washed with 0.5 M HCl and, finally, washed again in DI water. Monitoring of supernatant water pH
during the final wash with DI water ensured complete removal of traces of HCl. Following this, the sand was
dried in an oven at 60 °C for 24 hours. This procedure follows the work of Shani et al. who demonstrated
the importance of impurities on colloid mobilisation (Shani, Weisbrod, & Yakirevich, 2008).
Two identical sand-kaolinite mixtures were prepared with 5% kaolinite mass fraction (w/w). During
compaction, these mixtures were wet slightly with 0.6 M NaCl (0.6 M CaCl2 for test 2) solution. Note that,
unless specified, all molar concentrations presented in this text are the calculated ionic strengths of those
particular solutions.
Solutions: The corefloods were performed to investigate the mobilisation of fine kaolinite particles during
injection of NaCl and CaCl2 solutions of the same ionic strength. NaCl and CaCl2 analytical grade salts were
used to prepare the solutions (purity of 96.7% and 99.0%, respectively). The salt solutions were prepared
by dissolving a desired amount of salt in DI water. The ionic strength of the prepared solutions are: 0.6 M,
0.3 M, 0.1 M, 0.05 M, 0.01 M, 0.001 M. This corresponds to solution salinity of NaCl – 0.6 M, 0.3, 0.1 M,
0.05 M, 0.01 M, 0.001 M and CaCl2 – 0.2 M, 0.1 M, 0.0333 M, 0.0167 M, 0.0033 M, 0.00033 M. In grams
per litre these are: NaCl – 35.06 g/L, 17.53 g/L, 5/84 g/L, 2.922 g/L, 0.584 4g/L, 0.05844 g/L, and CaCl2
– 29.40 g/L, 14.70 g/L, 4.896 g/L, 2.455 g/L, 0.4896 g/L, 0.04852 g/L.

Experimental setup.
Experimental studies of kaolinite mobilisation in unconsolidated sand-kaolinite mixtures were carried out
using a setup schematically shown in Figure 2. An unconsolidated core (1) is placed inside a Viton sleeve
(2) of internal diameter 1.5". The sleeve and core are placed inside a standard RCH-series Hassler-type
coreholder (3). The core is then compacted and compressed using two stainless steel stoppers/distributors
on both sides of the coreholder.
6 SPE-191922-MS

Figure 2—Schematic of laboratory setup. See Section 2.2 for specific references to each component.

An overburden pressure is then developed by a manual HiP piston pressure generator (4). A high
performance HPLC pump (6) is used to pump the solutions through the core. A K-type thermocouple
(8) is used to measure the temperature of injected solutions and absolute pressure transmitters (9) and
(10) measure inlet and outlet pressures continuously. Four differential pressure transmitters (12-15) with
measuring ranges 0-1, 0-10, 0-100 and 0-1000 psi are used to measure the pressure drop across the core
sample during the tests. Effluent suspensions are collected continuously using a fraction collector (20).
Kaolinite concentration in effluent streams is measured in real-time using UV-Vis spectrophotometer (17).
The flowthrough electrolytic conductivity sensor (18) coupled with an electrically isolated signal amplifier
(19) used to measure electrolytic conductivity of effluent streams in real-time and convert them into ionic
strength. A data acquisition software records all experimental parameters.
Standard solutions with known properties were prepared and tested to generate calibration curves for
both the spectrophotometer and the electrolytic conductivity meter. This ensures that the results are accurate
to within reasonable experimental uncertainty.

Methodology.
Core floods: The experimental setup is used to study kaolinite mobilisation in unconsolidated cores with
real-time measurements of pressure drop, effluent pH, electrolytic conductivity, and suspended particle
concentration.
Conditioning of unconsolidated sand-kaolinite cores is carried out by saturating them with 0.6 M NaCl
or 0.6 M CaCl2 solutions at 0.2 mL/min (superficial velocity 2.93×10−6 m/s). Core saturation with high ionic
strength solution at low superficial velocity favours kaolinite fines attachment to sand grains. In parallel,
calibration of the spectrophotometer and conductivity sensor is carried out. During calibration, effluent from
the coreholder is directed to a glass bottle. A flowrate of 2 mL/min is then established and measurements
of all test parameters begin. The first "high-ionic strength" coreflood continues until stabilisation of core
permeability within experimental uncertainty of 3.2 % (Badalyan et al., 2012). Subsequently, injection of
the next solution, with lower ionic strength, begins, and the all parameters are measured until permeability
stabilization. This procedure is repeated for all solutions. Fluid viscosity is corrected in real-time for changes
in salt concentration, temperature and pressure according to (Aleksandrov, Dzhuraeva, & Utenkov, 2012;
Kestin, Khalifa, & Correia, 1981).
SPE-191922-MS 7

SEM-EDX: SEM-EDX analyses on kaolinite powder (as received and collected from coreflood effluents)
were conducted. Imaging was carried out using operating conditions of 20 kV and a spot size of 4 in the
secondary and backscattered electron modes. Energy dispersive X-ray (EDX) analysis was used to identify
the elemental composition of particles of interest identified in SEM image from EDX spectra. SEM analysis
can provide confirmation of the platelet form of the kaolinite particles used in this study.

Experimental Results and Discussions

Stability and reproducibility test.
Stability and reproducibility of permeability data is a necessary component in performing a comparative
analysis on the results in unconsolidated corefloods. During the experiments, two separate, but identical
coreflooding setups were used in parallel to further investigate the reproducibility of the procedure.
Two Coreflood tests were performed on two sand-only cores (no kaolinite) on the separate setups. A
duration of approximately 100 PVI was given to allow complete permeability stabilisation. The results of
these tests is given in Figure 3. The stability of permeability data for setup-A is 0.49% (standard deviation)
and 0.20% for setup-B (standard deviation). Taking into account that the experimental uncertainty is 3.2%
for the permeability, this variation can be regarded as acceptable.

Figure 3—Permeability tests run to evaluate the reproducibility of the experimental procedure

The error bars for permeability values for both setups overlap, meaning that permeabilities agree within
their experimental uncertainties, which implies that the method has produced reproducible results. Mean
permeability values obtained from both setups (1477 mD for setup-A and 1517 mD for setup-B) agree
within 2.6% which again is below the experimental uncertainty.

Coreflood tests.
Coreflooding tests using either sodium chloride or calcium chloride solutions with a stepwise decreasing
salinity, exhibit significantly different results.
Figure 4a shows the permeability of the first core, which underwent coreflooding with NaCl solutions.
Figure 4b shows the corresponding suspended particle concentration at the outlet of the core. The x-axis on
both of these graphs is time, presented here as the dimensionless quantity, Pore Volumes Injected (PVI)
8 SPE-191922-MS

where U is the fluid velocity, t is the time, ϕ is the porosity, and L is the core length.

Figure 4—Permeability (a) and outlet suspended particle concentration (b) results for a 5%
kaolinite (w/w) – 95% silica sand core flooded with NaCl solutions of varying ionic strength

Minor increases in permeability were observed during the injection of 0.6 M NaCl which was explained
by Russell et al (2016) as being the result of particle re-attachment due to favourable electrostatic conditions
at high salinities. For all solutions following the 0.6 M NaCl solution, permeability declines monotonically
due to fine release flowed by straining. The permeability decline is relatively minor until the injected solution
is changed to 0.001 M NaCl. At this salinity, the permeability of the core declines moderately, to a final
value of 379 mD 79.7% of its original value. Upon injection of deionised water, the permeability declines
significantly to a final stabilised value of 50 mD only 10.5% of the core's initial permeability. On Figure 4b,
the observed permeability decline aligns with a significant suspended outlet concentration. These results
suggest that the injection of DI water has induced detachment of kaolinite within the core. A portion of
SPE-191922-MS 9

these detached particles have consequently strained and damaged the permeability of the core, while the
remainder were collected at the core outlet.
Figure 5a and Figure 5b show the permeability and outlet suspended concentration graphs for the second
core, which underwent coreflooding with CaCl2 solutions. The first stage of this experiment mirrored the
NaCl experiment, inasmuch as CaCl2 solutions of decreasing ionic strength were injected in a step-wise
manner. The minor decreases in permeability present in the NaCl test are absent in the first stage of this
experiment Perhaps the most striking difference is the relative invariance of the second core to injection of
deionised water. While injection of DI water caused a 7.58 fold decrease in permeability in the NaCl test,
the injection of the same fluid resulted in a negligible change in permeability in the CaCl2 test. On Figure
5b it is clear that a negligible concentration of suspended particles was collected at the outlet during this
injection period.

Figure 5—Permeability (a) and outlet suspended particle concentration (b) results for a 5%
kaolinite (w/w) – 95% silica sand core flooded with CaCl2 solutions of varying ionic strength

As described in the methodology, the CaCl2 tests involved a second stage wherein a high salinity NaCl
solution was injected following the stepwise salinity reduction. The permeability was relatively constant
10 SPE-191922-MS

during this injection, as was expected. Following re-injection of DI water into the core, a 51.99 fold reduction
in permeability was observed and a significant volume of particles were collected in the effluent. These
features, as with the NaCl coreflood, suggest that the DI water induced particle detachment and fines
migration within the core.
The stabilised permeability decline curves are presented in Figure 6. The difference between the extents
of permeability decline in the two cases can be explained by the different injection schedules. The injection
schedule for the NaCl experiment would have caused small volumes of particles to detach for several
solutions prior to deionised water injection. This was not the case for the CaCl2 experiment. Particle capture
is a highly non-linear process and the sudden detachment of a large volume of particles can induce particle
bridging, wherein multiple particles block a pore throat more completely. This is a likely explanation for
the differences in permeability decline factors upon injection of DI water for the two cases.

Figure 6—Stabilised permeability values for the two experimental corefloods

SEM.
Results for SEM-EDX analyses for particles from effluent streams are presented in Figure 7. A vast majority
of fine particles visible on the high magnification SEM photograph (see Figure 7a, positions 1, 2, 4 and
5) showed nearly equal "peak height ratios" for Al and Si on EDX spectra (Figure 7b-1, b-2, b-4 and b-5)
confirming the identification of these particles as kaolinite, Al2(Si2O5)(OH)4. Differentiation of kaolinite
from muscovite was made on the basis of the relative absence of a K peak (Ulery & Drees, 2008).
Another key concern is whether the washing procedure removed any ions that were adsorbed prior to the
experiment. Removal of pre-existing ions is critical in establishing the ion exchange reactions prescribed
above for study. While trace volumes of these ions may still be present (see Figure 7b-3) due to ion fixation
or blocking (Scott, Hunziker, & Hanway, 1960), most of the previous ions seem to have been removed
through washing.
SPE-191922-MS 11

Figure 7—SEM image (a) and EDX spectra (b) for kaolinite particles from effluent stream

Conclusions
Coreflooding tests have confirmed that fines detachment by electrolyte solutions in porous media is
dependent on the type of cation present.
These results indicate that the water sensitivity of rocks is not only dependent on the injected solution,
but also on the previous saturation history of the rock.
The two main applications of this technology in petroleum waterflooding projects would be:
1. The injection of a high salinity plug with added CaCl2 prior to waterflooding to increase the fraction
of calcium on the clays within the reservoir. This would reduce the probability of particle detachment
and hence inhibit injectivity and productivity decline.
2. The injection of a high salinity plug with added NaCl prior to waterflooding to increase the fraction of
sodium on the clays within the reservoir. This would increase the sensitivity of clays to detachment by
injection of low-salinity water and may prove to be a useful tool in enhancing the volumetric sweep
efficiency and reducing the water relative permeability by induced fines migration.
12 SPE-191922-MS

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