Pet. Sci.

(2016) 13:340–346
DOI 10.1007/s12182-016-0080-y

ORIGINAL PAPER

Investigation of asphaltene deposition under dynamic

flow conditions
Farhad Salimi1 • Javad Salimi2 • Mozafar Abdollahifar1

Received: 25 June 2015 / Published online: 16 March 2016

Ó The Author(s) 2016. This article is published with open access at Springerlink.com

Abstract Asphaltene deposition is one of the most seri- 1 Introduction

ous problems, which usually occurs in oil wells, petroleum
production, oil processing, and transportation facilities. The formation of asphaltene deposits during petroleum
Deposition of heavy organic components, especially production can cause several operational issues including
asphaltene, can lead to wellbore blockage and impacts well total or partial blocking of pipelines and wellbores, changes
economics due to reduction in oil production. Therefore, it in wettability, and damage to equipment (Islam 1994).
is necessary to pay more attention to finding some solution Asphaltene deposition inside the oil reservoirs and pro-
to overcome this problem. In this study, a pipe-loop duction facilities is known as the main flow assurance
apparatus for investigation of oil stability was employed to problem in the oil industry.
measure deposition thickness using a thermal method. The In general, asphaltenes, which are regarded as part of the
effects of many factors such as oil type, oil temperature, oil crude oil, are insoluble in normal alkanes such as pentane
velocity, inhibitors, and solvents on asphaltene deposition and heptane; however, they are soluble in aromatics like
were investigated. The results showed that the deposition toluene and benzene. Also asphaltenes are known to have a
increased with the increasing value of the colloidal insta- high molecular weight and number of polar oil components
bility index. Besides, the deposition thickness increased (Ali and Al-Ghannam 1981; Hirschberg et al. 1984;
with the decreasing velocity of oil, but did not change with Speight 1999).
oil temperature. In addition, n-heptane could result in more There are many methods for identifying the stability of
deposition; however, toluene had no effect on the deposi- asphaltene in crude oil. These methods can approximately
tion. Branched dodecyl benzene sulfonic acid (Branched determine oils with the potential of asphaltene precipita-
DBSA) and Linear DBSA as inhibitors decreased the rate tion. Some of the older, but more popular, methods have
of asphaltene deposition. been employed for the stability of asphaltenes, including
asphaltene–resin ratio, Oliensis spot test, light scattering,
Keywords Asphaltene  Deposition  Dynamic flow  measurement of particle size, colloidal instability index
Pipe-loops  Inhibitors (CII), microscopic observations, and refractive index (RI).
The latter (RI) was first introduced and used by Buckley
(1999 for predicting the asphaltene precipitation onset. The
results showed that the RI was independent of asphaltene
& Farhad Salimi
content and occurred at a characteristic RI of 1.42–1.44.
f.salimi@iauksh.ac.ir; farhadsalimi348@gmail.com
Another method- used to predict asphaltene deposition CII
1
Department of Chemical Engineering, Faculty of Basic was presented by Yen et al. (2001) as CII = (Satu-
Sciences, Kermanshah Branch, Islamic Azad University, rates ? Asphaltene)/(Aromatics ? Resin). They found
Kermanshah, Iran
that, if CII is less than 0.7, the oil would be stable, and
2
Young Research and Elite Club, Kermanshah Branch, Islamic asphaltene precipitation would not occur. However, if this
Azad University, Kermanshah, Iran
index is higher than 0.9, the oil would be very unstable, and
Edited by Xiu-Qin Zhu

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Pet. Sci. (2016) 13:340–346 341

thus asphaltene precipitation would occur. Finally, if it is criterion for inhibitor selection. The result obtained from
between 0.7 and 0.9, the oil would be moderately unstable. this section is not sufficient to choosing a suitable inhibitor.
Asphaltene composition, structure, and stability depend Therefore, it is important to examine the inhibitors in real
on its source, type of solvent used for oil extraction, flow conditions. Besides, a literature study reveals that
pressure, and temperature (Soorghali et al. 2014; Groenzin there are only few reports on asphaltene deposition in real
and Mullins 2000; Alboudwarej et al. 2002; Akbarzadeh pipe conditions (De Boer et al. 1995; Alboudwarej 2003;
et al. 2002). Asphaltenes as colloidal with various sizes or Wang et al. 2004; Zougari et al. 2006; Jamialahmadi et al.
as individual molecules can be absorbed on solid surfaces 2009; Vargas et al. 2009).
by the virtue of their weak phenolic and carboxylic acid In this work, we report the effects of oil, oil velocity,
groups (Kokal et al. 1995). These materials can also be temperature, and inhibitors on asphaltene deposition in
strongly deposited on mineral surfaces and reservoir rocks, dynamic conditions by flow loop apparatus using a thermal
and hence cause formation damage, and hinder oil recovery approach.
from the reservoirs (Dubey and Doe 1993; Kord et al.
2012; Zanganeh et al. 2012). Furthermore, the absorption 1.1 Asphaltene deposition measurement
and deposition of asphaltenes on steel surfaces would
restrict oil flow in transportation pipelines (Faus et al. Direct and indirect methods are used to measure asphaltene
1984; Mochida et al. 1988). The remediation of asphaltene deposition in the pipe. In the direct method, depositions are
is very costly, which limits the production design of many measured directly such as the weight method, with ultra-
asphaltenic crude oil reserves (Hammami and Ratulowski sonic sensors, and caliper. In the indirect method, after the
2007; Akbarzadeh et al. 2012; Buckley 2012). formation of a deposition layer on the internal pipe wall,
Asphaltenes have inherent positive or negative charges, convection heat transfer occurs at the interface between the
depending on the composition of crude oil. Resins have a flowing fluid and the deposited layer. A thermal resistance
strong desire to link asphaltenes and attract opposite term is added to the total resistance due to heat conduction
charges; consequently, they make a protective layer for through the layer (Fig. 1). Hence, the deposit’s thickness
asphaltenes. When this protective layer is removed, can be determined from the measurements of the relevant
asphaltene precipitation occurs. The force balance between thermal parameters by solving the heat transfer equations.
the adsorbed resins and asphaltenes is the most important Heat transfer from the internal flowing fluid to the outside
factor for crude oil instability (Mullins et al. 2007). Resins environment is described by the following equation (Chen
naturally act as inhibitors, group contribution of which is a et al. 1997):
factor which connects the polar (asphaltenes) and non-po- 1 1 ro ro ri ro ro 1
lar (oil bulk) media. ¼ þ ln þ ln þ ð1Þ
Ub ho ri  dd kdep ri  dd kp ri hg
In the stabilization of asphaltene micelles, resins can be
helpful; however, when a paraffinic solvent is added to the where Ub is the overall heat-transfer coefficient, ri and ro
crude oil, the stability between resins and asphaltenes is are the inside radius and outside radius of pipe, respec-
demolished, and the amount of asphaltene monomers tively, and kdep, kp, ho, and hg are the deposit’s thermal
increases in the bulk phase. In some quantities, asphaltene conductivity, pipe’s thermal conductivity, convection
concentration reaches the concentration of the onset point, coefficient of oil, and convection coefficient of the bath,
and deposition occurs (Al-Sahhaf et al. 2002). respectively. The total heat-transfer rate in the test section
Amphiphilic molecules are among the inhibitors, often is given by
known as dispersants which are used to prevent the
aggregation of the micelles of asphaltenes. The perfor-
mance of inhibitors is mainly dependent on their structural
and chemical characteristics. Therefore, many inhibitors
Toil-in Toil-in
have been investigated as dispersants. To prevent asphal-
tene precipitation, amphiphils, which are soluble in oil, can Oil
rdep
be more efficient than aromatics. There are many works ho ri r
o

that have investigated the effects of various inhibitors on

the stability of asphaltenes (Hirschberg et al. 1984; Al- d

Sahhaf et al. 2002; González and Middea 1991; Chang and

P, L
Fogler 1994; Shadman et al. 2014; Rocha Jr et al. 2006; Tbath hg Tbath
Boukherissa et al. 2009; Ghloum et al. 2010; Ramos 2001). Bath of DEG
Most of these methods are done under static conditions,
and the onset point of asphaltene precipitation is the main Fig. 1 The pipe cross sections and related parameters

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342 Pet. Sci. (2016) 13:340–346

Q ¼ Ub Ab DTlm ¼ mo Cpo ðTo;in  To;out Þ ð2Þ and placed inside the bath. The bulk temperatures of the oil
were measured with K-type thermocouples, located in the
where, Ab = pd0L; and mo, Cpo, and DTlm are the mass tank and in the mixing chambers, before and after the test
flow rate, specific heat capacity, and logarithmic mean section. The temperature of the bath was controlled within
temperature difference in the heat-exchange, respectively. ±0.1 °C. The absolute pressure at the outlet of the tube was
At the beginning of the experiment, asphaltene thickness is controlled with a back pressure control regulator (model
zero, and the heat transfer equation is as follows: BP-66). The oil flow rate was controlled by the constant
1 1 ro ro ro 1 rate pump. A data acquisition system was used to monitor
¼ þ ln þ ð3Þ
Ubo ho ri kp ri hg the temperature at various points of both the bath and the
tube.
If Eq. (3) is subtracted by Eq. (1), the following equa-
tion is obtained: 1.3 Error analysis
1 1 1 r o dd ro ri
Y¼  ¼ þ ln ð4Þ
Ub Ubo ho ri ðri  dd Þ kdep ri  dd The experimental error in the measurement of the mass of
asphaltene deposition may result from the errors in the
The overall heat-transfer coefficient, Ub is calculated by measurement of bulk temperature and bath temperature of
Eq. (2), and the deposition thickness is calculated by the test section. The temperatures were measured with
Eq. (4). PT100 thermocouples located in the bulk of the oil flow
The inside (oil) convective heat-transfer coefficient (ho) before and after the test section. The inaccuracy in tem-
is obtained using the Hausen correlation (Eq. (5) (Hausen perature measurements due to the calibration errors of the
1943): thermocouples may lead to a deviation of approximately

0:8
0:19 NPe dLw ±0.1 °C. The maximum error in the mass of asphaltene
NNu ¼ 3:66 þ 
0:467 ; ð5Þ deposition measurements was estimated to be less than
1 þ 0:117 NPe dLw
±2.5 % by taking into account the temperature and flow
where NPe = NReNPr, NPr = lCpo/ko, and dw and ko are the rate measurement errors.
diameter of the pipe open to flow and thermal conductivity
of oil, respectively. Finally, ho is obtained by Eq. (6): 1.4 Experimental materials and procedure
NNu ko
ho ¼ ð6Þ Two different samples of Iranian crude oil were used for
dw investigation of asphaltene deposition. The results of
SARA test for these oils are shown in Table 1. To establish
a relationship between the composition and the stability
1.2 Experimental apparatus behavior of the crude oils, their main constituents, namely
saturates, aromatics, resins, and asphaltenes, were deter-
Figure 2 shows a schematic view of the novel designed mined following the procedure that has already been used
flow assurance test loop, which was used to measure the by Carbognani (Carbognani and Izquierdo 1989). Resins
thickness of asphaltene deposition as a function of time at were obtained through chromatographic fractionation of
different conditions. The apparatus is made of a well- the deasphalted oil. Silica was used as a packing material,
controlled temperature bath containing a long stainless and the different fractions were sequentially eluted with
steel tube in coil shape. The temperature of the bath was hexane (saturates), toluene (aromatics), and a 10 %
maintained constant using a heat source, controlling unit methanol/toluene mixture (resins). The solvents were
and stirrer. The long test tube was equipped with accurate removed by distillation, and the resins were further dried
pressure transducers and thermocouples at several inter- under vacuum.
vals, transferring all the information into a data acquisition In order to measure the viscosity and density of oil, an
system. The feedstock was prepared and transferred into Anton Paar SVM 3000 viscometer was used. The solvent
the feed storage, and its temperature was maintained at pre- used as precipitant in the viscometric method was normal
set temperature prior to flow through the pump into the heptane, and toluene, linear dodecyl benzene sulfonic acid
flowing loop. (Linear DBSA), and branched dodecyl benzene sulfonic
In this study, the pipe test section was made of a acid (Branched DBSA) were used as the inhibitors. Table 2
stainless steel tube (seamless, Fitok Company) of 1 m in presents the chemical structure of inhibitors used. The
length and 3.74 mm in inner diameter, which was coiled properties of these inhibitors are presented in Table 3.

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Pet. Sci. (2016) 13:340–346 343

Temperature controlled
DEG bath
’’ tubing
Coiled tube
Back pressure

’’ tubing
regulator

’’ tubing Data acquisition

system

Mixing-
preheating the feed High pressure pump
with adjustable flow

Fig. 2 Schematic of the experimental apparatus

Table 1 Analysis of SARA Oil 1 Oil 2 Table 2 Chemical structure of the inhibitors
Chemical structure Inhibitors
Asphaltenes 13.84 3.75
Resins 13.46 0.49 CH3 Toluene
Saturates 30.31 43.67
Aromatics 42.40 52.09
O Linear DBSA
HO S
The oil samples were weighed, mixed with certain O
amounts of inhibitor, and then put in a closed container O Branched DBSA
(preheating reactor) for 0.5 h. HO S
The experiment was conducted as follows: oil and sol- O
vent solutions were poured into the feed tank, then the
stirrer was turned on, and the temperature of preheater was
set to allow the feed to reach the specified temperature.
Simultaneously, the temperature of the bath, which con- experiment was set by a back-pressure control (BPCR)
tained the pipe, was set at the test temperature. After outlet valve. Next, the temperature data were gathered by
reaching the desired temperatures of the bath and pre- data-acquisition system. Then, the correlations related to
heater, the flow rate of the pump was set and turned on. deposition measurement were applied for the collected
After the fluid circulated inside the pipe, the pressure of the data.

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344 Pet. Sci. (2016) 13:340–346

Table 3 Properties of inhibitors used

Water, % Molecular weight, g/gmol Free sulfuric acid, % Free oil, % Acidity, mg (KOH)/g Anionic active, % Inhibitor

– 92.14 – – – – Toluene
0.41 322 1.35 1.89 183.9 96.4 Linear DBSA
– 321 1.8 2.2 180 96 Branched DBSA

After the experiments, 2 l of gasoline was added to the According to the CII definition, n-heptane increases CII,
feed tank, and the pump was initiated for an hour to wash and toluene decreases CII. Comparison between the results
the pipes. Finally, nitrogen gas was used to dry the of adding n-heptane (n-C7) to Oil 2 indicated that the
pipeline. thickness of asphaltene deposit increased, and the initiation
time, when asphaltene deposition occurs, was decreased.
Adding n-heptane to the oil led to an increased amount of
2 Results and discussion asphaltene particles in the oil and increased the deposition
rate of asphaltene particles. The flow rates (q) of solvent
The solubility of asphaltene in oil is reduced by adding for this test was equal to 220 cc/min, and the temperatures
normal alkanes to the oil. At this point, known as the onset, of oil and bath were adjusted to 50 and 70 °C, respectively.
more solvent will lead the asphaltene to begin to separate Toluene is an aromatic solvent; thus, its addition to the oil
from the oil. Further addition of solvent will lead to led to decreased CII index, and stabilized the oil. To study
increased asphaltene precipitation. the effect of toluene, 15 % volume percent of the solvent
The CII index for Oils 1 and 2 is equal to 0.79 and was added to Oil 2 at the flow rate of 220 cc/min at 50 and
0.902, respectively, and the results show that the oils are 70 °C of oil and bath, respectively, and the obtained results
within the moderately unstable range. are shown in Fig. 4.
According to the CII index calculated for Oil 1 and Oil Regarding the toluene solvent, as shown in Fig. 4
2, Oil 2 is in instability zone; however, Oil 1 is in the addition of toluene had very little effect on the amount of
transition zone. So, the amount of asphaltene deposit asphaltene deposit. There are two possible reasons for this:
formed in Oil 2 is expected to be greater than that in Oil 1. Addition of toluene solvent decreased the viscosity of oil
To investigate this issue, two experiments were carried out and the asphaltene particles in the oil, causing them to
for both oils at the same flow rate, bulk temperature, and easily move and stick to the wall. Besides, reducing the
wall temperature. The results (see Fig. 3) showed that more viscosity of oil led to decreased shear stress on the wall,
asphaltene deposited from Oil 2 than from Oil 1, indicating and increased the formation of deposits on it. Although
Oil 2 was more unstable than Oil 1. Another important adding toluene reduced the CII index, these two factors
point was related to the time of deposition formation, could cause toluene to have almost no effect on the amount
occurring at the later time for Oil 1. of asphaltene deposition.

120

Oil 1 120
100
Oil 2 q=220cc/min-0% sol(v/v)-Toil=50°C
100
Thickness, µm

80 q=120cc/min-0% sol(v/v)-Toil=56°C
Thickness, µm

80
60 q=220cc/min-0% sol(v/v)-Toil=50°C

60
40
40
20
20
0
0 20 40 60 80 100 120 140 160 0
Time, hr 0 20 40 60 80 100
Time, hr
Fig. 3 The effect of oil on the thickness of asphaltene deposit versus
time in pipeline for laminar flow. q = 220 cc/min, Toil = 50 °C, Fig. 4 The effects of flow rate (q) and oil temperature on the
Tbath = 70 °C thickness of asphaltene deposit versus time for Oil 2, Tbath = 70 °C

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Pet. Sci. (2016) 13:340–346 345

For calculating the laminar flow inside the pipe, the Effect of solvent on deposition
120
following Hagen Poiseuille equation (Sutera and Skalak q=120cc/min-0% sol(v/v), Toil=50°C
1993) was used: 100 q=120cc/min-0.5%B-DBSA(v/v), Toil=50°C
32L  l  m q=120cc/min-0.5%L-DBSA(v/v), Toil=50°C
DP ¼ ð7Þ

Thickness, µm
80
d2 q=120cc/min-1%B-DBSA(v/v), Toil=50°C

In the above equation, DP is the pressure loss, L, d, and m 60

are the length of pipe, diameter, and dynamic viscosity,
respectively 40

If the momentum balance is written for the pipe’s cross

20
section, the following equation is derived:
DP  p  r 2 ¼ s  2p  r  L ð8Þ 0
0 20 40 60 80 100
where s and r are the shear stress and radius, respectively. Time, hr
After inserting Eq. (7) in Eq. (8), the following equation is
Fig. 6 The effects of inhibitors on the deposit thickness versus time
obtained for the shear stress: for Oil 2, Tbath = 70 °C
32l  m
s¼ ð9Þ
d
According to Eq. (9), the increases of velocity and vis- Effect of oil temperature on asphaltene deposition was
cosity led to the increase of shear stress on the wall, which studied in this work. The results demonstrated that a rise of
could cause a reduction in the amount of asphaltene oil temperature (up to 56 °C) decreased the initiation time,
deposition. when the deposition occurs; however, it had no effect on
The effect of flow rate (velocity) on asphaltene depo- the amount of deposit after 100 h (Fig. 5).
sition was another parameter which was studied, and the A decreased viscosity of oil was the most important
results are shown in Fig. 5. As indicated, the deposition factor for reducing the initiation time of deposition to 5cp,
thickness was strongly dependent on this parameter. When which could decrease the shear rate on the inner pipe
the flow rate reduced to half, the thickness of deposition surface, and increase the deposit.
increases to about 2.5 times after 100 h. Besides, the ini- Figure 6 shows the effects of type and amount of inhi-
tiation time for the deposition formation declined from bitors on asphaltene deposition formed on the pipe surface.
about 40 h to 20 h, because the shear stress on the wall, It can be seen that the presence of inhibitors can decrease
which was directly proportional to the fluid velocity, might the initiation time, when the deposition occurs, and
have caused a reduction in the erosion of the deposition accelerate asphaltene deposition. However, an important
layer. point, which was found while adding inhibitors to the crude
oil, was the reduction of slope related to the formation of
asphaltene deposition or deposition rate on the inner pipe
surface. Comparison of different inhibitors indicated that
L-DBSA had greater influence on decreasing of deposition
70
rate than B-DBSA. It can be explained that the existence of
q=220cc/min-0% sol(v/v), Toil=50°C
60 branches on B-DBSA could lead to the reduced effect of
q=220cc/min-15% sol-nC7(v/v), Toil=50°C inhibitors in comparison to the inhibitors without branches
50 on its structure. Nevertheless, the deposition rate decreased
Thickness, µm

q=220cc/min-15% toluene(v/v), Toil=50°C

with increasing concentration of B-DBSA.
40

30
3 Conclusions
20

In this study, asphaltene deposition stability was success-

10
fully investigated under dynamic flow conditions. The
0 effects of many factors such as oil, temperature, solvent,
0 20 40 60 80 100
inhibitor, and velocity on the rate of deposition inside the
Time, hr
pipe were studied. It was found that the presence of oil with
Fig. 5 The effect of solvent on the thickness of deposition versus more CII led to the increased asphaltene deposition. The
time for Oil 2, Tbath = 70 °C deposition thickness increased with the decreasing velocity

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346 Pet. Sci. (2016) 13:340–346

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