Journal of Dispersion Science and Technology

ISSN: 0193-2691 (Print) 1532-2351 (Online) Journal homepage: http://www.tandfonline.com/loi/ldis20

Influence of Asphaltene Concentration on the

Interfacial Properties of Two Typical Demulsifiers

Yali Zhang, Shenwen Fang, Tao Tao, Yan Xiong & Ming Duan

To cite this article: Yali Zhang, Shenwen Fang, Tao Tao, Yan Xiong & Ming Duan
(2015): Influence of Asphaltene Concentration on the Interfacial Properties of
Two Typical Demulsifiers, Journal of Dispersion Science and Technology, DOI:
10.1080/01932691.2015.1111147

To link to this article: http://dx.doi.org/10.1080/01932691.2015.1111147

Accepted author version posted online: 09

Nov 2015.

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 Influence of Asphaltene Concentration on the Interfacial Properties of Two Typical
Demulsifiers

Yali Zhang1, Shenwen Fang1,2, Tao Tao1, Yan Xiong1,2, Ming Duan1,2

1
School of Chemistry and Chemical Engineering, Southwest Petroleum University,
Chengdu, Sichuan, China, 2Oil& Gas Field Applied Chemistry Key Laboratory of
Sichuan Province, Chengdu, Sichuan, China

Corresponding Author: Shenwen Fang, E-mail: 1104680134@qq.com

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Present Addresses: † 8 Xindu Avenue, Xindu District, Chengdu, Sichuan 610500, P. R.

China

Abstract

Oil-in-water emulsion is an innovate manner by which heavy crude oil can be transported

from producing sites to transforming sites through pipelines. The effect of emulsifier on

the interfacial properties and demulsification performance of demulsifier for heavy crude

oil–in-water emulsion has been studied by many researchers. However, the influence of

asphaltene in heavy crude oil on the interfacial properties of demulsifier has not been

investigated yet. In this paper, the influence of asphaltene concentration of two typical

demulsifiers (straight-chained SP-1 and branch-chained AE-1) was systematically studied

in terms of absorption thermodynamics, absorption kinetics and coalescence kinetics. The

results revealed that the demulsifier adsorption was a ΔS controlled spontaneous process.

The absolute value of ΔG of SP-1adsorption was found to decrease with asphaltene

concentration, whilst the asphaltene concentration had no significant influence on that of

1
 AE-1. With the increase of asphaltene concentration, the demulsifiers’ adsorption rates

increased, but the reorganization rates on the interface decreased. Coalescence speed of

asphaltene droplet decreased with asphaltene concentration in spite of demulsifier type.

Additionally, AE-1 had higher absolute value of ΔG, adsorption speed and coalescence

speed than that of SP-1 at the same condition.

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Graphical Abstract:

KEYWORDS: Heavy crude oil–in-water; Asphaltene; Demulsifier; Interfacial properties

1. INTRODUCTION

Heavy crude oil accounts for a large fraction of the world’s potentially recoverable oil

reserves, which reaches 20% of the economically recoverable oil in China. The viscosity

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 of heavy crude oil at 250C varies from 1000 cP to more than 100,000 cP1,2. With the

depletion of the low viscosity crude oil, the production of heavy crude oil is expected to

increase significantly in future 3. Numerous literatures have revealed the he increasing

importance of heavy crude oil in the outlook of world energy demands4,5.

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Conventional pipelining is not suitable for transporting heavy crude oil because of its

high viscosity. Generally, crudes with viscosities less than 500 cP are suitable for

pipelining6. The methods to decrease the viscosity includes diluting with lighter crudes,

preheating the crude with subsequent heating of the pipeline, and injecting of a water

sheath around the viscous crude7. However, the logistic, technical, and economic draw

backs limit the applications of these methods greatly.

Another favorable transportation strategy is using an oil-in-water (O/W) emulsion, which

could adjust the viscosity of the heavy crude oil to less than 500 cP. The emulsion

transport seems to be an ideal method, providing that it can be carried out

appropriately8-10. For this method, hot heavy crude is emulsified with the appropriate

ratio of surfactant, producing a heavy crude O/W emulsion containing≈ 70 v.t. % heavy

crude oil. The emulsion is allowed to be stored till pipeline transportation. Once the

emulsion arrives at the end of the pipeline, it could be broken by changing the

temperature or adding demulsifier11, 12. Adding demulsifier is the most popular method

for its simplicity and finding suitable adequate demulsifiers attracted great attention for
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 the researchers13,14. Mostly, the heavy crude oil-in-water emulsion is stabilized by

asphaltene (natural surfactant for heavy crude oil) and emulsifier, which locate at

interfaces and tend to inhibit or delay the interdrop film drainage 15,16. The effect of

emulsifier on the interfacial properties and the demulsification performance have been

reported by several papers17,18. However, the influence of asphaltene on the interfacial

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properties and demulsification performance of demulsifier has not been published so far.

The objective of the current research is to investigate the influence of asphaltene

concentration on interfacial properties. Two typical demuslifiers that have straight chain

and branch chain were studied respectively. The interfacial properties were studied in

terms of absorption thermodynamics, absorption kinetics and the coalescence kinetics,

which are important to analyze demulsifier’s performance.

2. MATERIALS AND METHODS

2.1 Materials

Asphaltenes was extracted from heavy crude (9°API, density of 1.0). The extraction has

been made as follows: the heavy crude was first stirred with an excess of n-pentane (1g of

heavy crude and 30ml of pentane). The precipitated fraction was filtered, dried, and

grinded.

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 The demulsifiers were SP-1 and AE-1. They were used as received from Energy

Technology & Services Oilfield Technology Services Co., China National Offshore Oil

Crop. They are, respectively, a branch chain demulsifier (AE-1) and a straight chain

demulsifier (SP-1), as shown in Fig.1. In addition, the number-average molecular weight

(Mw) of AE-1 and SP-1 are 3710g/mol and 5540g/mol, respectively.

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2.2 Methods

Usually, the process of demulsification of O/W emulsion includes four steps: (1)

demulsifier absorption, demulsifier diffuses from bulk phase to interface; (2) demulsifier

displaces the active agents on the interface; (3) oil droplets collision and coalescence; (4)

oil droplets aggregation. Fig.2 shows the step (1), step (2) and step (3). In this paper, the

influence of asphaltene concentration on absorption thermodynamics, absorption kinetics

and the coalescence kinetics was studied.

2.2.1 Absorption Thermo Dynamics Method

An equilibrium state is always reached when the demulsifier diffuses from water to the

interface. At this equilibrium state, the ratio of the demulsifier concentration in the

aqueous phase Cw to its concentration in the oil phase Co is defined as partitioning

coefficient (K). According to Equation (1)19,20, RT ln K is the Gibbs free energy change

(ΔG)of transfer of demulsifier from water to interface.

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 Cw
RT ln K  2.303RT lg K  RT ln  G *o  G *W
Co (1)
 G *
W O  G   H  T  S

Where, G*w is the initial state Gibbs free energy of demulsifier in the water phase, G*o is

the final state Gibbs free energy of demulsifier in the oil phase or at the interface. ΔH and

ΔS are the enthalpy change and entropy change in the process of adsorption, respectively.
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A linear function relationship between lgK and 1/T can be obtained from Eq.(2), which is

transformed by Eq.(1):

lg K  H / 2.303RT  S / 2.303R (2)

If we know the relationship of lgK versus 1/T, ΔH and ΔS can be obtained according to

Eq.(2). The measurement of relationship of lgK versus 1/T was described as below:

(1) Measurement of relationship between equilibrium IFT and ln (demulsifier

concentration) (lnC).

Firstly, asphaltene solution was prepared by using mixture of toluene and heptanes (50:50

by volume). Demulsifier aqueous solutions were also prepared with concentration of

50mg/L, 80mg/L,100mg/L, 150mg/L and 200mg/L.

Then, IFT between asphaltene solution and demulsifier aqueous solution was measured at

300C by a University of Texas spinning drop tension meter (Model TX500, CNG USA

CO.). The variation of IFT with time was monitored and equilibrium IFT was obtained
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 when IFT had no change. The relationships between equilibrium IFT and lnC at different

asphaltene concentrations are shown in Fig.3.

(2) Adsorption experiment

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Firstly, 30 mL asphaltene solution and 70 mL demulsifier aqueous solution (C=200mg/L)

were added into the bottle. The bottle was allowed to reach desired temperature via a

water bath. Once reached the desired temperature, the bottle was shaken 200 times and

then returned to the water bath.

Then, the bottle was shaken 100 times per hour and 2 mL demulsifier aqueous solution

was taken from the bottom of bottle to measure the equilibrium IFT. When the adsorption

reached the equilibrium state, the equilibrium IFT would have no change with time and

the value was recorded.

At last, a series of adsorption experiments were conducted with changing the asphaltene

concentration and temperature.

(3) Calculation of K

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 Cw was calculated by using the recorded equilibrium IFT and the relationships were

shown in Fig.3. The Co was the difference between initial demulsifier concentration and

Cw. K was calculated according to Eq.(1).

2.2.2 Adsorption Kinetics Method

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Due to the slow diffusion of demulsifier from water to the interface and molecular

rearrangement at the interface, the IFT between asphaltene solution and demulsifier

aqueous solution was time-dependent.

To investigate adsorption kinetics of demulsifier at asphaltene solution-water interface,

the dynamic IFT was studied by monitoring of the IFT variation with time(as shown in

Fig.4) at 30 0C. A series of dynamic IFTs were studied by changing the asphaltene

concentration and demulsifier concentration.

To compare the adsorption kinetics, the experimental data was fitted to a biexponential

(four-parameter) decay curve,

  ae( bt )  ce(  dt ) (3)

Where is the IFT as a function of time t. The constants b and d describe the rate at

which the interfacial tension decays, respectively. The fast decay is described by decay

constant b while the slower decay is described by decay constant d.This equation has also

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 been used by Fossen21,22 for fitting the IFT curves of asphaltene solution in toluene. The

curve fitting was performed using OriginPro 8.0.

2.2.3 Coalescence Kinetics Method

The droplet-to-planar coalescence experiment was used to study the coalescence kinetics

at 60 0C. The asphaltene solution droplets were released from a droplet extrusion device
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and coalesced at an asphaltene solution-water interface23-25. As shown in Fig.5, 1 mL

asphaltene solution was added on top of demulsifier aqueous solution and an oil-water

interface was formed. An asphaltene solution droplet was squeezed out through micro

injector and entered into the water phase. When the droplet reached the interface, timing

was triggered. Timing was stop until droplets coalesced with asphaltene solution planar

and disappeared. The measurements were repeated for 32 droplets. The relationship

curves between ln(N/N0) –t were draw, where N is the number of droplets which do not

coalesce within time t, N0 is the total number of determined droplets, namely N0=32 and t

is coalescence time. According to Cockbain’s theory, coalescence kinetics parameters

were calculated.

With a given system the stabilities of individual drops were not constant, but if thirty or

more were examined separately, a distribution curve was obtained sufficiently

reproducible for analysis and the examination curve at rupture stage can be expressed as

follows23,24:
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  N
ln    kt  C (4)
 N0 

Where k is coalescence rate constant and C is regression factor.

The coalescence speed of asphaltene solution droplets can be determined by half life

timet1/2, that is, half the time droplets disappear. Then, the following relationship can be
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obtained.
ln2  C
t1/2   (5)
k
The coalescence speed increased with decreasing t1/2.

3. RESULTS AND DISCUSSION

3.1 Absorption Thermodynamics

The relationships between lgK and 1/T at different asphaltene concentrations are shown

in Fig.6. All of them had good linear relationships. According to the Eq.(1) and Eq.(2),

ΔG, ΔH and ΔS were calculated and listed in Table 1, respectively.

As shown in Table 1, ΔG was less than 0, which means the asphaltene adsorb via a

spontaneous process. ΔH>0 and ΔS>0 indicated that this spontaneous process was

controlled by ΔS.

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 For SP-1, as asphaltene concentration increasing from 0.2% to 1.0%, both ΔH and ΔS

decreased, while ΔG increased. The result revealed that asphaltene concentration had a

great influence on the adsorption thermodynamics of SP-1 and the driving force of

SP-1adsorption (indicated by the absolute value of ΔG) decreased with asphaltene

concentration. For AE-1, ΔG, ΔH and ΔS changed slightly but not significant as
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asphaltene concentration increased, which indicated that asphaltene concentration had

moderate influence on the adsorption thermodynamics.

Since the ΔH > 0, it can be concluded that the demulsifier adsorption was an

endosthermic process. Therefore, the absolute value of ΔG would increase with

temperature. In addition, the absolute value of ΔG of AE-1 was more than that of SP-1,

which indicated the AE-1 adsorption may be easier than SP-1 adsorption.

3.2 Adsorption Kinetics

The parameters obtained from the fitting of IFT versus time of SP-1 and AE-1 are listed

in Table 2 and Table 3, respectively. It was noticed that the fast decay constant b of both

demulsifiers increased with asphaltene concentration and slow decay constant d exhibited

an opposite result. The fast decay is usually due to the diffusion and adsorption of

demulsifier from bulk phase to the interface, and the slow decay corresponds to the

demulsifier reorganization at the interface. The results indicated that the adsorption rates

to the interface of both demulsifiers increased with asphaltene concentration, but their
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 reorganization rates on the interface decreased. Both the constant band constant d of

AE-1 were larger than that of SP-1, which may be attributed to its higher driving force of

adsorption.

3.3 Coalescence Kinetics

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Results from the coalescence kinetics experiments at different asphaltene concentrations

are shown in Fig.7. t1/2s of AE-1 and SP-1 increased with asphaltene concentration. The

result indicated that coalescence speed of asphaltene solution droplet decreased with

asphaltene concentration in spite of demulsifier type. It may be attributed to the lower

reorganization rate at the interface with increasing asphaltene concentration. In addition,

the t1/2 of AE-1 was much smaller than that of SP-1 and the effect of asphaltene

concentration on t1/2of SP-1 was much greater than that of AE-1. The results were in

agreement with the result of adsorption kinetics and adsorption thermodynamics.

4. CONCULSION

In this study, we firstly and thoroughly investigated the influence of asphaltene

concentration on interfacial properties of two typical demuslifiers (straight-chained SP-1

and branch-chained AE-1). The interfacial properties including absorption

thermodynamics, absorption kinetics and the coalescence kinetics were systemically

investigated. Absorption thermodynamics results showed that the demuslifiers adsorb via

a ΔS controlled spontaneous process. The driving force of SP-1adsorption (indicated by

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 the absolute value of ΔG) decreased with asphaltene concentration, whilst the asphaltene

concentration had no great influence for AE-1. The adsorption kinetics results indicated

that the adsorption rates to the interface of both demulsifiers increased with asphaltene

concentration, but their reorganization rates at the interface decreased. Coalescence

kinetics indicated that coalescence speed of asphaltene solution droplet decreased with
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asphaltene concentration in spite of demulsifier type. In addition, AE-1 had higher

absolute value of ΔG, adsorption speed and coalescence speed than that of SP-1 at the

same condition.

ACKNOWLEDGEMENTS

The authors of this work wish to gradefully acknowledge the financial support from the

Sichuan Youth Science & Technology Foundation for Innovation Team (2015TD0007)

and National Natural Science Foundation of China (Project No: 21376193) and Program

for New Century Excellent Talents in University (NCET-13-0983).

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 Table 1 ΔG, ΔH and ΔS during the demulsifier adsorption

0.2% 0.5% 0.8% 1.0%

ΔS(J.K-1.mol-1) SP-1 AE-1 SP-1 AE-1 SP-1 AE-1 SP-1 AE-1

219.33 242.28 169.42 238.07 148.00 248.40 69.03 231.57

ΔH(KJ.mol-1) SP-1 AE-1 SP-1 AE-1 SP-1 AE-1 SP-1 AE-1

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51.70 54.80 34.74 42.54 33.07 56.93 8.03 52.07

ΔG(KJ.mol-1) 303K -14.79 -18.22 -16.53 -17.79 -11.26 -18.30 -12.88 -17.98

313K -16.48 -21.87 -18.10 -19.96 -13.72 -20.26 -13.54 -19.84

323K -18.80 -23.00 -19.67 -21.77 -14.97 -23.13 -14.41 -23.13

333K -22.06 -26.46 -22.12 -23.12 -16.00 -26.40 -14.98 -25.25

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 Table 2. Parameters obtained from the fitting of IFT of SP-1 versus time

a b c d R2

0.2% 2.0993 0.1244 1.7747 0.0089 0.9968

0.5% 2.2007 0.1148 2.0861 0.0042 0.9948

0.8% 1.7079 0.1348 2.8172 0.0032 0.9951

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1.0% 2.3625 0.2137 2.0626 0.0013 0.9922

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 Table 3. Parameters obtained from the fitting of IFT of AE-1 versus time

a(mN/m) b(s-1) c(mN/m) d(s-1) R2

0.2% 3.8285 0.1250 7.1776 0.0092 0.9830

0.5% 2.7638 0.3996 6.3828 0.0059 0.9934

0.8% 2.5417 0.4693 7.1187 0.0048 0.9899

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1.0% 3.3093 0.5040 6.6169 0.0041 0.9910

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Fig. 1. Schematic diagram for the molecular structure of SP-1and AE-1
 Fig. 2. Schematic diagram of demulsifier adsorption and oil droplet coalescence
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 Fig. 3. The relationships between quilibrium IFT and lnC at different asphaltene

concentrations (a) 0.2%; (b) 0.5%; (c) 0.8%; (d) 1.0%

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 Fig. 4. IFT between demulsifier aqueous solution (C=200mg/L) and 0.2% asphaltene

solution versus time at 30 0C. The line is the fit with Eq. (3).
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 Fig. 5. Setup for studying the droplet-to-planar coalescence experiment (oil is asphaltene

solution and water is demulsifier aqueous solution)

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 Fig. 6. The relationships between lgK and 1/T at different asphaltene concentrations (a)

0.2%; (b) 0.5%; (c) 0.8%; (d) 1.0%

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 Fig. 7. Results from the coalescence kinetics experiments at different asphaltene

concentrations
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