Journal of Petroleum Science and Engineering 157 (2017) 117–123

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Journal of Petroleum Science and Engineering

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

Flow of heavy crude oil-in-water emulsions in long capillaries

simulating pipelines
Alexander Ya. Malkin, Maria V. Mironova, Sergey O. Ilyin *
A.V. Topchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences, 29 Leninsky Prospect, 119991 Moscow, Russia

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

Keywords: We studied the rheological properties of heavy oil-in-water emulsions with the final goal of decreasing the high
Heavy crude oil viscosity of oil in pipeline transportation. The emulsions containing 3% silica or 5% montmorillonite were sta-
Oil-in-water emulsions bilized by Triton X-100. All emulsions were viscoplastic media and also demonstrated viscoelasticity. At low shear
Rotation viscometry
stresses, emulsions are in gel-like state that was reflected by the independence of the elastic modulus from fre-
Tube transportation
quency. The yield stress of basic emulsion is rather low (~1 Pa), while the introduction of solid particles leads to a
Wall sliding
remarkable increase of the yield stress. It was shown that direct transition of the rheological data for oil emulsions
measured in a rotational device to capillary rheometer appeared impossible. The apparent viscosity of the samples
estimated in tubes (as a model of a capillary viscometer) was not correlated with the shear viscosity measured on
a rotational rheometer and overall was dependent on the tube/capillary diameter. The reason for these effects
may be related to the stratified flow through a tube consisting of near-wall slippage or the existence at the stream
periphery of a low-viscosity layer. This phenomenon should be taken into account in designing pipe trans-
portation lines when viscometric data are obtained in the other conditions of flow.

1. Introduction points of view. In fact, preparing oil-in-water concentrated emulsions

Today, interest in heavy crude oils is constantly growing due to
gradual exhaustion of standard oil sources and the discovery of huge
fields of heavy oil around the world, with the latter accounting for no less
than two thirds of the explored reserves of hydrocarbons (Alboudwarej
et al., 2006; Akram et al., 2014). At the same time, prospects for a rapid
increase in heavy oil production meet serious limitations due to its high
viscosity. This leads to increased costs of transportation of crude oil and
thereby impairs economic evaluation of the use of heavy oil. To solve this
issue, various technological solutions for viscosity reduction have been
advanced. Among them, the following ideas have been discussed: heating
to the temperature at which the viscosity decreases to an acceptable
level, dilution of heavy oil with light oil to reach the necessary viscosity
level of a blend, use of drag reduction additives, arranging a multi-layer
flow by creating a low-viscosity wall layer (annular and core flow), heavy
oil deasphalting (Ilyin et al., 2016a), and transformation of crude oil into
oil-in-water emulsion. One can find the collation of all these methods as
well as numerous references to earlier publications in the review (Mar-
tínez-Palou et al., 2011).
The development of oil-in-water emulsions looks rather attractive
among the proposed methods from both technological and economic
allowed for decreasing in the viscosity of heavy crude oil by several or-
ders of magnitude (Malkin et al., 2016). Therefore, it is necessary to
stress that the evaluation of the emulsion viscosity cited in the majority of
publications is rather conditional and ambiguous. All oils and oil-based
emulsions in particular are rheologically complex media. These fluids
demonstrate not only the viscoplastic behavior, yielding effect, or non-
Newtonian flow (Foudazi et al., 2015), but primarily the heterogeneity
of the flux of multi-component fluids expressed in stratified flow and wall
effects, which depends on the geometry of the flow. For example, phe-
nomena such as the dependence of the rheological properties of waxy
crude oils on the gap between solid surfaces in a measuring rotation
device have been described (Japper-Jaafar et al., 2015). Also, the influ-
ence of the pipe diameter on the rheology of such oils has been observed
(Foissen et al., 2013).
Effects of this kind are not typical for heavy crude oil itself, which
usually contains a low quantity of paraffin wax. The behavior of these oils
is almost like Newtonian viscosity in a wide temperature range (Ilyin
et al., 2016b). However, the transformation of crude oil into emulsions
that are viscoplastic and thixotropic fluids does not allow the features of
the flow mode and the specificity of the method used for measuring the
viscosity to be neglected. Moreover, the most important point is the issue

* Corresponding author.
E-mail address: s.o.ilyin@gmail.com (S.O. Ilyin).

http://dx.doi.org/10.1016/j.petrol.2017.07.024
Received 8 December 2016; Received in revised form 28 June 2017; Accepted 11 July 2017
Available online 12 July 2017
0920-4105/© 2017 Elsevier B.V. All rights reserved.
A.Ya. Malkin et al.
Fig. 1. Principle scheme of a pressure-controlled viscometer: 1 – compressor, 2 – valve, 3
– manometer, 4 – shutoff valve, 5 – barrel with a sample, 6 – tube (capillary), 7 – open
container, 8 – analytical balance, 9 – computer.
of whether we can apply the characterization of the rheological proper-
ties obtained by the technique of rotational rheometry (commonly used
for estimating the rheology of crude oils) for predicting and designing the
performance of these systems in pipeline transportation.
This study was carried out as an attempt to answer this question. Its
main content was the correlation of data of the rotation rheometry and
the behavior of the oil-in-water emulsions during their flow through long
tubes (capillaries), which modeled the pipeline transport. We considered
such an emulsion stabilized by a common surfactant as well as these
materials with the addition of solid micro(or nano)-particles, which can
be either natural components of crude oil or stabilizers in Pickering-
type emulsions.
2. Experimental section
2.1. Materials
Heavy crude oil from Yaregskoye oil field (Lukoil, Russia) was used as
a representative sample. The density at 20
C was equal to 0.942 g/cm3,
which corresponded to API gravity ¼ 18.1. According to the classification
of the American Petroleum Institute, this oil belongs to the class of heavy
oils (heavy oils are those with API gravity < 20). The weight fraction of
sulfur was 1.24%, and the paraffin wax, asphaltene, and resin fractions
were 0.8, 5.7, and 17%, respectively. The viscosity, η, at 20
C was
approximately 2 Pa s and this value was constant in the range of shear
stress, σ, from 0.1 to 3  103 Pa.
Oil-in-water emulsions were prepared using distilled water and
nonionic surfactant Triton X-100 (4-(1,1,3,3-tetramethylbutyl)phenyl-
polyethylene glycol) supplied by AppliChem Panreac. This compound
has a rather high hydrophilic–lipophilic balance equal to 13.5. The
concentration of the surfactant in aqueous phase was 5 wt %.
Besides oil-in-water emulsions stabilized by this surfactant, addi-
tionally, samples containing micro(nano)-size particles have been stud-
ied. Two types of solid particles were used: 3 wt % silica (produced by
Aldrich) with a specific surface of 395 m2/g and 5 wt % Na-
montmorillonite clay Cloisite Naþ (Southern Clay Products, USA) with
a specific surface of 750 m2/g. The aim of using solid particles was
twofold: on one hand, they simulated natural components in crude oil,
and on the other hand, they could be an addition surfactant line in
Pickering emulsions (Chevalier and Bolzinger, 2013; Ilyin et al., 2015).
The model system (direct crude oil-in-water emulsions) contained
65 vol % oil. The emulsions were prepared by continuous addition of the
necessary volume of oil to the aqueous solution of surfactant, which
could also contain solid particles. The dispersion was performed in an
IKA Ultra-Turrax T10 rotary homogenizer. Mixing was continued for
10 min at a rotor rotation rate of 30  103 rev/min. The emulsions were
stable: precipitation of the aqueous phase did not take place for at least
several weeks.
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Journal of Petroleum Science and Engineering 157 (2017) 117–123
2.2. Methods
The rheological properties of crude oil emulsions were measured on a
RheoStress 600 rotational rheometer (Thermo Haake, Germany), a
Rosand RH10 capillary viscometer (Malvern Instruments, UK), and a
home-made pressure controlled laboratory viscometer.
The measuring device was a cone-and-plate pair
(diameter ¼ 60 mm; angle between conical surface and plate ¼ 1
grade). The rotational rheometer was used to measure the properties in
the stationary and oscillation modes of deformation. The viscosity was
measured for a rate-controlled shear rate in the range of
1  104–100 s1. Viscoelastic properties in the linear limit were
measured in the frequency range of 0.05–600 s1 at the same shear
stress amplitude of 1 Pa. The relative error in measuring the rheological
properties does not exceed 5%.
The Rosand RH10 capillary viscometer worked at a preset velocity
and was supplied with a non-standard homemade brass tube with a
length, l, of 5 m and inner diameter, d, of 0.8 mm. This long tube with l/
d ¼ 625 was considered as a model of a pipeline where the apparent
(average) shear rate varied from 10 to 1000 s1. The relative error in the
viscosity measurements does not exceed 5%.
The second capillary device used as a model of a pipeline worked in
the pressure-controlled mode. A sketch of it is shown in Fig. 1. The
viscometer consisted of a barrel, 5, containing the studied sample.
Pressure was created by compressed air supplied from a compressor, 1,
regulated by a valve, 2, and measured by a manometer, 3, with a scale of
3 atm (±0.05 atm). A shutoff valve, 4, was used for the start of the
experiment. After opening the shutoff valve, the fluid under study begins
to flowed through a rigid polypropylene tube (capillary), 6, with a known
length (l ¼ 278 mm) and diameter (d ¼ 3.25 mm) into an open container,
7, placed on an analytical balance, 8. The balance (AND EK-12Ki) was
connected through a COM-interface to the programmed computer mod-
ule 9. This allowed for continuous measurement of the rate of flow. Ex-
periments were carried out in the stress-controlled mode in the range
from 10 to 100 Pa. During the tests, the pressure uniformly acted on the
surface of a sample due to the large distance (10–15 cm) between the
injection nozzle and the sample. The relative error in the viscosity
measurements does not exceed 10%.
Experimental results were treated using the standard methods
(Malkin and Isayev, 2017), namely the shear stress in the rotation de-
vice was calculated from the torque and the shear rate was calculated
from the rotational speed. The capillary viscometry data were used for
calculation of the shear stress at the wall, σ, and shear rate, γ_ , respec-
tively, as
PR
σ¼ (1)
2l
and
4Q
γ_ ¼ ; (2)
πR3
where Р is the pressure inside the barrel with the sample (at the capillary
entrance), Q is the volume output measured by the weight method as
described above, R is the radius of a capillary (long tube), and l is
its length.
No corrections for the non-Newtonian flow and entrance effects were
introduced.
In discussing the experimental data, the Reynolds number, Re, was
also calculated by the ordinary formula:
V0 dγ 2Qρ
Re ¼ ¼ (3)
ηg πRη
Using the Hagen-Poiseuille equation for viscosity, this formula can be
rearranged and Re is expressed via measured values:
A.Ya. Malkin et al.
Fig. 2. Photomicrographs of 65% emulsions without solid particles (a) and emulsions with 3% SiO2 (b) or 5% clay (c).
1:6Q2 lρ
Re ffi
PR5
In these formulas, V0 is the average linear velocity of the flux corre-
sponding to the volume output, γ is the specific weight, ρ is density, η is
viscosity, and g is the gravitational acceleration. All values used for cal-
culations were expressed in the SI system of units.
The morphology of the prepared emulsions was observed using a
Biomed 6P optical microscope (Russia). The size distribution of the
droplets in the emulsions was found by the method of dynamic light
scattering by means of a Zetasizer Nano ZS analyzer (Malvern In-
struments, UK). Samples for the analysis were prepared by dilution of the
oil emulsion droplets in 5 ml of distilled water.
All experiments were carried out at 21 ± 1
C.
Fig. 3. The size distribution of droplets in emulsions with the addition of solid particles.
Journal of Petroleum Science and Engineering 157 (2017) 117–123
3. Results and discussion
(4)
3.1. Structure of emulsions
Photomicrographs of emulsions are shown in Fig. 2 where one can see
that droplets in emulsions are not deformed in spite of the high content of
disperse phase. The size of droplets can reach 30 μm, but in emulsions
containing solid particles, the size of droplets is smaller and lies mainly in
the range of 1–20 μm.
The droplets in emulsions with Cloisite Naþ are smaller than those in
emulsions with SiO2, which can be explained by the twofold larger
specific area of the surface of clay in comparison with silica.
The size distribution of droplets is presented in Fig. 3. As seen,
droplets with clay are smaller than droplets with silica and are charac-
terized by a narrower distribution.
Fig. 4. Dependencies of the apparent viscosity on shear stress for basic crude oil and 65%
oil-in-water emulsions.
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A.Ya. Malkin et al. Journal of Petroleum Science and Engineering 157 (2017) 117–123

3.2. The rheology of emulsions (rotational rheometry)

The basic heavy crude oil is a Newtonian fluid with high viscosity
close to 2 Pa s (Fig. 4, curve 1). Emulsion containing 65% oil is a non-
Newtonian fluid and its viscosity decreases by a factor of ~1000 along
with an increase in the shear stress (Fig. 4, curve 2). The non-linear ef-
fects may be due to the rupture of inter-droplet bonds and the orientation
of droplets in shearing. In the range of high shear stresses, the viscosity of
emulsion appears to be more than an order of magnitude higher in
comparison with basic oil.
As might be expected, emulsions demonstrate obvious viscoplastic
behavior, expressed in the sharp decrease in apparent viscosity in a
narrow stress range. If the emulsion does not contain solid particles, its
yield stress does not exceed 1 Pa (Fig. 4, curve 2), while the introduction
of solid particles results in a strong increase in the yield stress, which rises
to 10 Pa for emulsion with 5% silica (Fig. 4, curve 3) and to ~30 Pa for
emulsion with 5% clay (Fig. 4, curve 4).
Beyond the yield stress when the structure is destroyed (Malkin et al.,
2017), the apparent viscosity of emulsions becomes much lower than the
viscosity of crude oil.

3.3. Viscoelasticity of emulsions (measurements at the limit of very low

deformations)

Basic crude oil demonstrates viscoelastic properties at low tempera-

tures, possibly due to the presence of asphaltenes and other high-
molecular-weight compounds (Ilyin et al., 2016a, 2016b). To an even
greater extent, viscoelasticity is inherent for emulsions; it is only slightly
expressed in emulsion of pure oil (actually the storage modulus is not
measured by experiment) but becomes strongly expressed in emulsions
containing solid particles (Fig. 5).
The most interesting result presented in Fig. 5b is the independence of
the storage modulus from frequency in a rather wide frequency window, in
which the storage modulus is much higher than the loss modulus. Such
behavior is typical for matter in solid-like state and this means that
emulsions at low shear stresses (in the linear domain of viscoelasticity) are
gels that are unable to flow. The spatial structure of emulsions responsible Fig. 5. Dependencies of the storage modulus (filled symbols) and loss modulus (empty
symbols) on frequency for crude oil (1), oil-in-water emulsions without solid particles (2),
for such a state is formed by contacting gels with interface boundary
and emulsions with 3% silica (3) or 5% clay (4).
enriched with adsorbed solid particles. The narrower size distribution of
particles in emulsion with clay provides higher values of the storage
modulus in the same way as higher values of the storage modulus are is also worth mentioning that flow properties measured by the capillary
characteristic for monodisperse polymers in comparison with samples that method demonstrate slightly non-Newtonian behavior, although this is
are the same but polydisperse (Malkin and Isayev, 2017). not clearly noticeable when using a log scale for the viscosity.
As can be seen, the apparent viscosity estimated by the tube flow data
3.4. Viscometry in the flow through long tubes (capillaries)

Oil-in-water emulsions especially those that have been modified by

the addition of solid particles are viscoplastic non-Newtonian fluids and
the flow of such media at high shear stresses can be heterogeneous (or
stratified) (Malkin et al., 2012; Malkin and Kulichikhin, 2015). This can
occur as a well-known effect of shear banding (Møller et al., 2008;
Fielding, 2016; Divoux et al., 2016). Then the relationship between the
pressure gradient and the average velocity in the flow (as the measure of
the apparent viscosity) depends on the velocity profile and is therefore
not an objective characteristic of the rheological properties of a fluid.
So it is crucial to consider the correlation between the objective
rheological characteristic of matter obtained in the homogeneous flow
field (Fig. 4) and the peculiarities of the flow through a long capillary
(tube) as a model of a pipeline.
Appropriate experimental data are presented in Fig. 6 where the filled
symbols reproduce the rotational rheometry data and the open symbols
are the results of capillary viscometry treated by using Eqs. (1) and (2).
Comparison of the two sets of data shows that the flow curves are
Fig. 6. Dependencies of the apparent viscosity on shear stress for crude oil (1), oil-in-
equivalent for crude oil while the results of measurements appear water emulsions without solid particles (2), and emulsions with 3% silica (3) or 5%
different regardless of the level of the yield stress (low yield stress for clay (4). Rotational rheometry data are shown by filled symbols. Capillary viscometry data
pure emulsions and high yield stress for emulsions with solid particles). It (the tube with a diameter of 0.8 mm) are shown by empty symbols.

120
A.Ya. Malkin et al.
Fig. 7. Dependencies of the apparent viscosity on shear stress for 65% oil-in-water
emulsion without solid particles (1) and emulsions with 3% silica (2) and 5% clay (3).
The results have been obtained for tubes with diameters of 0.8 mm (filled symbols) or
3.25 mm (empty symbols).
is at least twofold lower than that measured in the homogeneous con-
ditions for the same shear stress.
The crucial experiment for understanding the peculiar features in the
flow of emulsions is testing long tubes with different diameters. The re-
sults of such an experiment are presented in Fig. 7 show that the data of
Fig. 8. Presentation of the experimental data using the coordinates of Eq. (6) at different shear stresses for emulsion without solid particles (a) and emulsion with 3% silica (b) or 5%
clay (c).
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Journal of Petroleum Science and Engineering 157 (2017) 117–123
the measurements do not coincide with one another because the
apparent viscosity appears higher for the tube of larger diameter. This
observation can be explained if it is supposed that the stratified flux takes
place due to wall effects (either real wall slip or formation of a thin low-
viscosity layer).
Indeed, if wall slip with velocity w happens, the volume output is
calculated as
Q ¼ Q0 þ πR2 w (5)
where the first member in Formula (5) is the volume shear flow in the
bulk of a tube and the second member is due to wall slip of fluid and
movement of the material as a whole with the velocity w. Then the
following relationship is valid:
1 1 4
¼ þ w (6)
ηapp η Rσ
where η is the real viscosity determined by shearing and ηapp is the
apparent viscosity calculated by the Hagen-Poiseuille equation for a
Newtonian fluid. Then one can see that the apparent viscosity ηapp should
increase with increasing tube radius. The numbers on the y-scale in Fig. 7
are just these apparent viscosity values and they approached the real
shear viscosity as the radius of the tube increased.
The graphs in Fig. 8 built using the coordinates of Eq. (6) give some
idea of the relationship between the real shear viscosity of emulsions and
the role of wall slip.
A.Ya. Malkin et al.
Fig. 9. Shear stress dependencies of real viscosity (a) and wall slip velocity (b) for
emulsion without solid particles (1) and emulsion with 3% silica (2) or 5% clay (3). The
slip velocities have been calculated for tubes with diameters of 0.8 mm (filled symbols) or
3.25 mm (empty symbols).
The viscosity values obtained by extrapolation to 4/Rσ ¼ 0 (i.e. R → ∞)
allow us to build the real flow curves which are the objective presentation
of the viscous properties of emulsions under study (Fig. 9a). For example
the viscosity values at shear stress of 10 Pa are equal to 0.15, 0.20, and
0.27 Pa s for emulsion without solid particles and emulsion with 3% silica
or 5% clay, respectively. The first of these values is in satisfactory agree-
ment with the viscosity at the plateau at stresses above the yield stress
obtained by the rotational rheometry method. In the other cases, such a
comparison is impossible because the level of plastic viscosity on the
rotational rheometer has not been reached (filled symbols in Fig. 6). The
slip velocities are 14.5, 5.5, and 1.0 mm/s for emulsion without solid
particles and emulsion with 3% silica or 5% clay, respectively.
These arguments emphasize the limited possibilities for application of
the rotational rheometry data for designing the flow in pipelines. Eq. (6)
shows that the wall slip can be neglected if
4η
w< <1
Rσ
This means that the slip effect can be insubstantial only for tubes of
large diameter. This inequality can be written in the following alterna-
tive form:
4η 4w
w¼ < <1
Rσ R_γ
Journal of Petroleum Science and Engineering 157 (2017) 117–123
This relationship shows the physical sense of the inequality, that is,
the relation between the shear rate in the volume of fluid ð_γ Þ and the
apparent velocity gradient (w/R) due to the wall slip.
The following example illustrates the estimation of the tube radius
when the wall slip can be neglected. For oil-in-water emulsion without
solid particles with η ¼ 0.15 Pa s, σ ¼ 10 Pa, and w ¼ 14.5 mm/s, the
strong inequality will be executed for R > 9 mm, which is much larger
than the tube with R ¼ 1.625 mm used for laboratory measurements.
For emulsions without solid particles, the slip velocity increases along
with the shear stress (Fig. 9b), while for emulsions with silica or clay, the
slip velocity passes through maxima. One can suppose that a decrease in
velocity is related to the destruction of the laminar wall-adjacent layer by
solid particles rotating in flux. It should be emphasized that the slip ve-
locity does not depend on the tube diameter but is determined only by
the pressure gradient and the nature of emulsions (i.e. the structure of
near-wall layer).
The obtained experimental results can be treated as the consequence
of stratified flow of emulsions. Indeed, it is well known that such a mode
of movement is typical for multicomponent systems (Malkin et al., 2012).
The stratified flows have been also observed for crude oil-water mixtures
as was discussed in the recent publication based on the high resolution
visualization of the flux (Loh and Premanadhan, 2016). In this study, it
has been shown that the dispersed flow regime is more typical than the
stratified regime for heavy oils in comparison with light oils. Possibly,
this is also true for the heavy oil emulsions. In this case, we meet with a
flow of a homogeneous dispersion (emulsion) with the wall slip rather
than with a real stratified flux.
In conclusion, it is worth stating that all experimental data obtained
in this study were obtained at low Reynolds numbers. Calculations show
that for the flow of heavy crude oil Re << 1 and for the emulsions under
study, Re lies in the range from 2  103 to 40. So, formally, the flow in
this study was always laminar. However, the definition of the Reynolds
number for stratified flows is rather uncertain.
4. Conclusions
The creation of oil-in-water emulsions from heavy crude oil leads to a
significant decrease in viscosity at high stresses, which is important for
the technology of pipeline transportation. Structuring concentrated
emulsions results in the appearance of viscoplasticity (yield stress) and
viscoelasticity. The presence of solid micro (or nano)-particles in emul-
sion, which can be either natural impurities or Pickering stabilizer, in-
fluences the morphology of emulsions and leads to an increase in the
yield stress and viscosity. In the domain of low stresses (linear visco-
elasticity), the storage modulus does not depend on frequency, which is
typical for emulsions in gel state or solid-like state.
The behavior of emulsions in the flow depends on the geometry of
deformation. The objective rheological properties of emulsions measured
in homogeneous shearing cannot be used directly for predicting their
behavior in flow through capillaries and designing pipelines for oil
transportation because the apparent viscosity found in the capillary
viscometer does not coincide with the viscosity measured in a rotational
rheometer. Moreover, the “capillary” apparent viscosity depends on the
diameter of the tube. These effects are evidently due to inhomogeneity of
the flux in the tube due to wall slip and the appearance of stratified flow.
These peculiarities in the behavior of concentrated oil-in-water emul-
sions should be taken into account when applying the results of the
rheological tests to real pipelines. The volume shear flow becomes
(7)
dominant only in the flow of tubes of large diameter, while whether the
diameter is large enough depends on the composition of the emulsion.
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