Egyptian Journal of Petroleum 27 (2018) 657–662

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Egyptian Journal of Petroleum

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Full Length Article

Optimum demulsifier formulations for Nigerian crude oil-water

emulsions
Olusiji Ayoade Adeyanju a,⇑, Layioye Ola Oyekunle b
a
Department of Chemical and Petroleum Engineering, University of Lagos, Nigeria
b
Department of Petroleum Engineering, Covenant University, Otta, Ogun State, Nigeria

a r t i c l e i n f o a b s t r a c t

Article history: The formation of crude emulsion during oil production and processing is a challenge of significant
Received 4 July 2017 proportions to the oil producers. Studies show that about two third of Nigerian crude oil production is
Revised 20 September 2017 in form of water in oil emulsion. For economic and operational reasons, it is necessary to separate the
Accepted 2 October 2017
water completely from the crude oil before transportation or refining.
Available online 16 October 2017
Efficiency of separation of crude emulsions is of major importance to producers. To this end, this study
primarily seeks to investigate the formulation of effective demulsifier that can be used to achieve this
Keywords:
aim; and in so doing, the optimal separation efficiency attainable by this demulsification process is deter-
Demulsifier
Variable interaction
mined. Six different samples of water and oil soluble demulsifiers were used on two different samples of
Optimal formulation synthetic emulsion (sample I and II (both water in oil emulsion) from different Nigerian oil fields). The
Emulsion destabilization bottle test method was used to determine the percentage water separation for each crude oil emulsion/
Interfacial active agent chemicals (demulsifiers) mixture. The concentrations of the combined six chemicals (demulsifier samples
A–F) in the mixture were related to the percentage water separation using response surface methodology
central composite design (RSMCCD).
Results show that the optimum concentrations of demulsifiers A–F are 59 ppm/39 ppm/29 ppm/20
ppm/29 ppm/13 ppm respectively for crude oil sample I. While 54 ppm/40 ppm/25 ppm/21 ppm/29
ppm/8 ppm respectively were observed as optimum concentration for crude oil II. The combination of
these chemical was observed to return better performance than the existing commercial demulsifiers
with percentage water separation of 92% and 94% compared to percentage water separation of 87%
and 90% returned by one of the currently available demulsifier used in the petroleum industry for crude
oil A and B respectively. Hence, the need to carry out optimization analyses on different emulsified crude
oil cannot be over-emphasize.
Ó 2017 Egyptian Petroleum Research Institute. Production and hosting by Elsevier B.V. This is an open
access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction
The mixture of two immiscible liquids always leads to the
dispersed of one liquid in the other, the dispersion of a liquid in
another liquid is defined as an emulsion. Emulsions exist between
liquids that have no solubility between them. Emulsions exist in
almost all man-made commodities such as food, paints, pharma-
ceuticals, asphalt preparation, waste water treatment and agricul-
ture chemicals [1]. Crude oils being a one of the natural and
unprocessed oil discovered in the earths subsurface exist along
with the formation water and hence during crude oil production
Peer review under responsibility of Egyptian Petroleum Research Institute.
⇑ Corresponding author.
E-mail addresses: oadeyanju@unilag.edu.ng (O.A. Adeyanju), loyekunle@unilag.
edu.ng (L.O. Oyekunle).
they are produce with the water in the form of oil and water emul-
sion [2]. Emulsions are undesirable in crude oil production because
it leads to increase operational and capital cost in production facil-
ities. Emulsion stability ranges from few minutes to few years
depending on the nature of the crude oil and water. Emulsions
increase the density from about 800 kg/m3 for original crude oil
to around 1030 kg/m3 and viscosity of crude oil from 560 mPa.s
to about 1000 mPa.s [3]. Consequently, the need for an efficient
and effective demulsifier to destabilized the emulsion and separate
the water from the crude oil cannot be over emphasized [4]. In
order to achieve this objective the demulsifiers need to be analyzed
and formulated precisely to ensure its capability in separating the
emulsion into respective phases. The demulsifiers act as emulsion
breaker [5].
Studies had established the fact that the interfacial barrier
(boundary between the oil and water phase) are responsible for

https://doi.org/10.1016/j.ejpe.2017.10.001
1110-0621/Ó 2017 Egyptian Petroleum Research Institute. Production and hosting by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
658 O.A. Adeyanju, L.O. Oyekunle / Egyptian Journal of Petroleum 27 (2018) 657–662

Nomenclature

dx
dt
rate of settling of the dispersed water phase qoil density of crude oil
d diameter of the water droplet l viscosity of the emulsion
qwater density of water

the formation of water oil emulsion. The interfacial barriers that
prevent coalescence between the phases consist of oil and water
mixture. The interfacial barriers are products of reactions between
the agitated crude oil and water resulted from the simultaneous
movement of the phases from the petroleum reservoir through
the well to the surface production facilities. Addition of demulsifier
disrupts the stability of the interfacial barrier by separating the
emulsion into their separate phases. Hence the demulsifiers need
to the properly formulated in order to meet the requirement in
breaking the emulsion with little agitation.
2. Literature review
the emulsified crude oil in order to reduce both the density and
the viscosity of the crude oil with aim of increasing the settling
velocity of the dispersed water droplets in the continuous crude
oil phase.
In this study, the objectives is to optimize the formulation of a
demulsifiers mixture using six crude oil and water soluble demul-
sifiers in order to have a wider understanding of water in oil emul-
sion behavior. Minitab-16, experimental design software, was used
to formulate the optimal demulsifier formulation in the separation
of water from the emulsified crude oil. The bottle test method
which is the most common method for the evaluation of separated
water from the emulsified crude [13] was used in the study.

Early petroleum industry operators used condensed chemicals 3. Materials and methods
such as sulphuric acid, sulphated castor oil, polyamines and poly-
hydric alcohols directly as demulsifier [6], Later in the early 3.1. Characterization of crude oil
1940, the alkoxylated polymer group derivatives such as
ethylene-, propylene-, and butylene-oxides were used [7]. A dec- Two crude oils coded crude oil-I and crude oil-II from two dif-
ade after, as a result of a large scale production of ethylene and ferent fields in the Nigerian Niger delta region were used in the
prophylene oxide, a new classes of non atomic detergents devel- study. The properties of these two crudes are shown in Table 1.
oped through condensed polyether were used as demulsifiers [8]. Overview of the properties shows that the crude oil-A is more
Presently, a polymer based hydrophilic and hydrophobic surfac- stable due to its higher content of the interfacial active agents.
tants are used as demulsifiers this is to enable the demulsifier to
permeate and destabilize the interfacial barrier between the crude
3.2. Equipment
oil and water in the emulsion. Hence it is expedient for the
designed demulsifier to contain both oil soluble (hydrophobic)
The chemicals used as demulsifiers are chosen based on their
and water soluble (hydrophilic) solvents. Daaou and Bendedouch,
potency in increasing the settling rate of water in the water in
[9] in their study on the effect of pH on Algerian crude oil emulsion,
oil emulsion, these include their solubility in water and crude oils,
confirmed the fact that neutral medium is more efficient in stabi-
their oil/water surface boundary activity, their capability in reduc-
lizing the emulsions compared to the acidic and basic solutions.
ing the density and the viscosity of the crude-oil, their ability to
The surfactants used in the petroleum industry can be grouped
increase the pour point of the crude oil and cost effectiveness.
into four groups namely, the amines, polymeric compounds, alco-
The selected chemicals (demulsifiers) are Pentylamine, polyethy-
hols and polyhydric alcohols (Krittika et al., 2014). While oil sol-
lene oxide, ethanol, butanol, polyethylene glycol and butyl acry-
uble demulsifiers such as polymeric demulsifier give outstanding
late. All the chemicals are supplied by Finlab Nigeria Limited and
performance for water in oil emulsion, water soluble demulsifiers
MON Scientific (Nigeria) Limited. The homogenizer used is the
such as amine group, alcohol and polyhydric alcohol based demul-
SAMRO SRH60-70 homogenizer manufactured by ShangHai amro
sifiers are prefer for oil in water emulsion [10].
homogenizer Company Limited.
Amines are surface active with high solubility in the continuous
water phase. However, the amine group demulsifier has an ability
3.3. Experimental methods
to alter the pH or salinity of the aqueous phase of the emulsion
thereby stabilizing the emulsion [10].
Two crude oils (Oil-I and II) with low basic sediment and water
From the Stokes’ law [11], the settling velocity of water droplet
(BS&W) of 0.6 and 0.8% respectively from two different fields in the
in a water in oil emulsion is directly proportional to the squared of
the diameter of the water droplet and the difference in densities
between the oil phase and water phases, and inversely proportional Table 1
Properties of the two crude oils and their measurement methods.
to the viscosity of the continuous oil phase. This is express as:
Properties Experimental Measurement Crude oil
dx d ðqwater  qoil Þ
2
a ð1Þ Method sample
dt l Oil-I Oil-II
where Gravity at 28°C, API ASTM-D5002-16 40.5 36.2
dx
dt
¼ rate of settling of the dispersed water phase Pour point, °C ASTM-D97-66 27 18
d ¼ diameter of the water droplet Viscosity at 28°C, cp ASTM-D445 8.5 8.1
Salt content, (g/m3) ASTM-D6470-99 (2015) 17 15
qwater  qoil ¼ relative difference in density of the emulsion Asphaltene (%) ASTM-D7-5 (06560) 0.16 0.19
phase Resin (%) ASTM-D893-69 21.5 19.4
l ¼ viscosity of the emulsion Basic Sediment and Water ASTM-D4007-02 0.6 0.8
BS&W (%)
Saturated Hydrocarbon (%) ASTM-D2786-91 (2016) 34 28
From the expression in Eq. (1), Akpobio and Ekott, [12]
Aromatic Hydrocarbon, (%) ASTM-D3238-95 (2015) 16.84 27.25
suggested the possibility of adding low boiling point diluents to
 O.A. Adeyanju, L.O. Oyekunle / Egyptian Journal of Petroleum 27 (2018) 657–662
Nigerian Niger delta from Okan and Makaraba field respectively
operated by Chevron Nigeria Limited were used in the study, the
bottle test method was used in the evaluation of the single and
combined demulsifier screening for the determination of the opti-
mal demulsifier formulations. The experiments are conducted at
room temperature of 30 °C
3.4. Emulsion preparation
The experimental studies were carried out with crude oil sam-
ples and formation water from the Nigerian Niger delta region. In
formulating the emulsion, the emulsion samples were prepared
in the ratio 2:7 water-oil volumes. In preparing the emulsion
2100 ml of each crude oil sample was mixed with 100 ml of
sodium dodecyl sulphate (SDS), homogenizer at a speed of
10,000 rpm was then used to stir the crude oil and surfactant mix-
ture in a container for a duration of 10 min.
Thereafter, the dispersed phase i.e. 600 ml of formation water
from the separator plant was introduced into the container con-
taining the crude oil and the surfactant in a slow and gentle man-
ner. After the addition of the dispersed phase the mixture is further
agitated with the homogenizer at a speed of 8000 rpm for another
10 min to facilitate homogenization between the components of
the resulting emulsion. The homogenized mixture was left for five
days to enable the free water to settle out of the emulsion. A dro-
plet of the resulting emulsion was placed on a filter paper to ascer-
tain that water-in-oil emulsion is formed [14].
3.5. Demulsifier screening
The bottle test method was used in the screening of the demul-
sifiers. Different amount of demulsifiers were added to a series of
equal amount of proposed emulsified oil to be de-emulsified in test
tubes (Mat, 2006). The de-emulsification tests were conducted at
constant room temperature (28 °C), and pH of 6.0 using varying
concentrations previously designed with a Minital-16 software.
3.6. Bottle-test
The bottle tests were performed with several 10 mL. of emulsi-
fied crude oils at the room temperature (28 °C), the designed con-
centration of each of demulsifiers mixtures from the Minital-16
software were injected in turn into each of the 10 mL of the emul-
sified according to the specify volumes from the experimental
design. A total of ninety (90) experiments were conducted on each
of the two [2] crude oils and the response was the fraction of water
that separated out of the emulsified crude oil. The bottles were
places in a centrifuge and shaken for 1 min to ensure thorough
mixing of the demulsifiers and the emulsified oil. Separation of
the water from the emulsified crude was monitored by the inter-
face between the emulsified crude oil and the separated water that
settled at the bottom. The fraction of the water separated from the
emulsified crude was recorded every 5 h. A bottle containing emul-
sified oil without any demulsifier was used as a Ref. [15]. The per-
centage of water separated is given as:
Fraction of separated water
Volume of separated water; mL
¼
Original v olume of water in the emulsified oil; mL
3.7. Optimization method
A response surface method from a Minitab-16 software was
used in designing the experiments, analyze the results and
659
optimize the demulsifiers formulation that produce optimum sep-
aration of water from the emulsified crude oil.
4. Results and discussion
4.1. Effect of the type of demulsifier
The Fig. 1 shows the plots of percentage of water separated
from each of the 10 mL. of emulsified oil in the test tubes by
the addition and mixing of 15 ppm of each of the demulsifiers
(chemicals) to the 10 mL of crude oil, and also that of blank oil
(without a demulsifier) at different periods of time (hours).
Results show that the effectiveness of the demulsifier in the sep-
aration of water from the water-in-oil emulsion from the most
effective to the least effective is in the following order: polyethy-
lene glycol, polyethylene oxide, pentylamine, butyl acrylate, etha-
nol and butanol as 57, 52, 48, 35, 32 and 28% (V/V) respectively of
water were separated from crude oil sample A after 75 h of
observations.
Emulsion destabilization being the essential mechanism for the
effective separation of dispersed phase from the continuous phase
in an emulsified liquid, the solubility of the demulsifier in the con-
tinuous phase is essential in the effectiveness of the demulsifier. In
this study, the oil being the continuous phase in the water-in-oil
emulsion, provides an avenue for the oil soluble demulsifier to
have access to the oil-water interface boundary and destabilizes
the boundary that makes the dispersed phase to be isolated. Hence
the low effectiveness of butanol as a demulsifier in the water-in-oil
emulsion is due to its low solubility in crude oil, as it is water
soluble.
4.2. Optimization of demulsifiers formulation
In an effort to formulate the optimal formulation of demulsifiers
mixture for effective separation of water from the water in oil
emulsion a total of ninety (90) experiments were designs for each
of the two (2) crude oil samples using the response surface
method. Table 2 shows the range and levels of the independent
variables for both crude oils used in the study. These are based
on the concentrations at which each demulsifier gives optimate
performance. Some of the experimental runs: showing the differ-
ent combination of the six demulsifiers (ppm) from the experimen-
tal design with the resulting response: percentage of separated
water from the two (2) water-in-oil emulsions are as shown in
Table 3.
There is noticeably dependent of the percentage of separated
water with the dosage of each demulsifiers, according to the
Table 3, the best separation occurred in run 71 (75% V/V), while
Fig. 1. Percentage of separated water by different demulsifiers at same tempera-
ture = 28 °C, Concentration = 15 ppm and pH = 6.0.
660 O.A. Adeyanju, L.O. Oyekunle / Egyptian Journal of Petroleum 27 (2018) 657–662

Table 2 The model equations relating the percentage of water separated

Experimental range and levels of independent variables selected. to the amount of each demulsifies in the formulation removing the
X-variables Variable Level (ppm) factors with insignificant influence (with P-value of less than 0.05)
2 +2 in un-coded unit for Crude oil I is given as:
Ethanol 50 60 Y ¼ 39:25 þ 13:01 B þ 12:4581 C þ 10:98 E þ 1:796 B2
Polyethylene 30 50
Pentylamine 20 40 þ 2:17 C 2 þ 0:03078 BC þ 0:3564 BE þ 0:04468 CE ð2Þ
Butanol 25 30
Polyethylene glycol 10 20 Y = percentage of the water separated from the demulsifier.
Butyl acrylate 10 15
While the model equation for crude oil II is:

Y ¼ 43:17 þ 15:15 B þ 11:2381 C þ 18:23 E þ 2:156 B2

run 27 (14% V/V) has the least separation. The average amount of
separation in these runs (run 1 to 90) was about 45% V/V.
Analyzing the results with a response surface method from the
minitab-16 software, the contour plots of the interaction between
the selected demulsifiers are shown in Figs. 2 and 3 for crude oil A.
It was confirmed from Fig. 2 that, the effect of butanol in sepa-
rating water from the emulsion is relatively very low when inter-
acting with polyethylene glycol as its effect is negligible. This
interaction is relatively as the effectiveness of the butanol in
removal of water from the emulsion when interacting with the
butyl acrylate is substantial as shown in Fig. 3. Though the percent-
age of separated water is relatively lower (less than 45%) compared
to the separated water of less than 78% in the interaction with
polyethylene glycol. Similar results were obtained with crude oil
sample II.
Representing the different demulsifier by the respective letters
as shown in Table 4:
For crude oil samples I and II, the butanol, ethanol and butyl
acrylate concentrations, their interactions and squares has no sig-
nificant influence on the percentage of water separated from the
demulsifiers, as their P-value are less than 0.05 based on confi-
dence interval of 95%. The butanol, ethanol and butyl acrylate con-
centration have antagonistic effect on the percentage of separated
water from the emulsified crude oil. While the effect of polyethy-
lene, pentylamine and polyethylene glycol are synergetic.
For crude oil I, the polyethylene has the highest effect on the
separated water, followed by pentylamine, then by polyethylene
glycol. For crude oil II, the polyethylene glycol has the highest
effect in the removal of water from the emulsified crude oil, fol-
lowed by polyethylene and then pentylamine.
þ 4:03 C 2 þ 0:02578 þ 0:5182 BE þ 0:06512 CE ð3Þ
4.3. Optimization of the demulsifiers formulation using Minitab-16
software
Using the model equations to perform the response optimiza-
tion in the minitab-16 software to maximized the amount of sep-
arated water from the water in crude oil emulsions.
Results show that the optimum concentrations of demulsifiers
(A–F) for crude oil sample I are 59 ppm/39 ppm/29 ppm/20
ppm/29 ppm/13 ppm respectively, achieving a maximum of 92%
water separation. While 54 ppm/40 ppm/25 ppm/21 ppm/29
ppm/8 ppm respectively, were observed as optimum concentra-
tions, with maximum water separation of 94% for crude oil
sample II.
4.4. Comparison of the optimum formulation with commercial
demulsifier result
Comparing the results of the percentage of the separated water
using the optimal demulsifier formulation and the separated water
using one of the currently available demulsifier in the petroleum
industry confirmed the viability of the study (design).
When the separation tests were performed in the laboratory,
using the design demulsifiers formulation, the combination of
these chemicals (demulsifiers) was observed to return better per-
formance than the existing commercial demulsifiers with percent-
age water separation of 92% and 94% compared to percentage

Table 3
Design values of each of the demulsifiers and the responses for the two crude-oils.

Run No. Ethanol (ppm) Polyethylene oxide (ppm) Pentylamine (ppm) Butanol (ppm) Polyethylene glycol (ppm) Butyl acrylate (ppm) Percentage of
Separated
water (%)
OIL I OIL II
1 60 50 20 30 10 10 31 44
2 60 30 40 25 20 15 54 55
3 55 40 30 27.5 15 12.5 37 43
11 50 30 40 30 10 10 25 34
12 50 50 20 25 20 10 54 60
16 50 30 40 25 10 10 32 35
17 60 50 20 25 20 10 58 66
27 50 30 20 30 10 15 8 14
29 50 30 20 30 20 10 27 42
33 60 50 20 25 10 10 38 44
35 60 50 20 30 10 15 26 35
36 50 30 20 25 10 10 10 18
52 60 30 20 25 20 10 35 46
53 60 30 20 30 20 10 28 45
71 50 50 40 25 20 15 73 75
72 60 30 40 30 10 10 19 28
73 50 30 40 30 20 10 51 62
88 55 40 30 27.5 15 12.5 37 43
89 60 30 40 25 20 10 58 62
90 50 50 40 30 20 15 75 59
 O.A. Adeyanju, L.O. Oyekunle / Egyptian Journal of Petroleum 27 (2018) 657–662 661

Fig. 2. Contour plot of separated water from the water-in-oil emulsion against butanol and polyethylene glycol for crude-oil I.

Fig. 3. Contour plot of separated water from the water-in-oil emulsion against butanol and butyl acrylate for crude-oil I.

Table 4
Code for each of the used demulsifiers.

Code Demulsifier
A Ethanol
B Polyethylene Oxide
C Pentylamine
D Butanol
E Polyethylene Glycol
F Butyl Acrylate

water separation of 87% and 90% returned by one of the currently

available demulsifier used in the petroleum industry for crude oil I
and II respectively as shown in Fig. 4. Hence, the need to carry out
optimization analyses on different emulsified crude oil before their
Fig. 4. Comparison of separated water from commercial and designed demulsifiers
application on the field cannot be over-emphasized.
for crude oil I and II.

5. Conclusion
To design the most effective demulsifiers formulation, a group
of demulsifiers selected from preliminary screening process were
study using the response surface method from a minitab 16
software. The bottle test method was used as the screening
process. The results of individual test show that the effectiveness
of the demulsifier in the separation of water from the water-in-
oil emulsion from the most effective to the least effective is in
662 O.A. Adeyanju, L.O. Oyekunle / Egyptian Journal of Petroleum 27 (2018) 657–662
the following order: polyethylene glycol, polyethylene oxide,
pentylamine, butyl acrylate, ethanol and butanol as 57, 52, 48,
35, 32 and 28% (V/V) respectively of water were separated from
crude oil sample I after 75 h of observations.
Application of the optimal demulsifiers formulation to the
crude sample I and II returned a percentage water separation of
92% and 94% respectively compared to percentage water separa-
tion of 87% and 90% by one of the currently available demulsifier
used in the petroleum industry.
It is expedient therefore to study and formulate the optimal
demulsifier concentrations for each crude oil as the use of same
commercial demulsifiers for all the crude-oils will not give an opti-
mum water separation performance.
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