International Journal of Engineering and Technology Volume 2 No.

11, November, 2012

ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
1854

Breaking of Oil -Water Emulsion for the Improvement of Oil Recovery
Operations in the Niger Delta Oilfields

C. Ijogbemeye Oseghale
1
, Akpabio E. J
2
and Udottong, G
1
1
Department of Chemical Engineering, University of Port Harcourt,
Port Harcourt, Nigeria.
2
Depaertment of Chemical & Petroleum, University of Uyo, Nigeria.

ABSTRACT

Emulsified water is generally present in crude oil as a result of mixing occurring during production operations. The formation
of emulsion leads to problems in production and also transportation. Therefore the need to break oil/water emulsions system
through demulsification process using chemical surfactants for improved oil recovery operations. Selected cationic
surfactants were effective in separating oil-water emulsions expected during a surfactant/polymer (SP) process for improved
oil recovery. The aqueous phase of the emulsion contained an anionic surfactant blend, alcohol and partially hydrolyzed
polyacrylamide. Brine composition was a suitable mixture of formation brine with brine from polymer drive. The crude oil
had an API gravity of 47.2. Bottle tests were conducted at ambient temperature, which is near the reservoir temperature. Both
oil and water phases of acceptable quality were obtained after settling upon addition of 200ppm of octytrimethylammonium
bromide (C
8
TAM) at ambient temperature. Microscopy image showed significant coalescence after only 1 minute in C
8
TAM
system as the cationic surfactant reduced electrostatic repulsion among drops and shifted system behavior towards the
balanced state between hydrophilic and lipohilic effect well-known to reduce emulsion stability. The amount of cationic
surfactant may be reduced by reduced by adding it simultaneously with anionic demulsifier resin.

Keywords: Oil-water emulsion, Demulsification process, Surfactant/polymer process, Enhanced oil recovery

1. INTRODUCTION

In the petroleum industry, emulsion of oil and water is
one of many problems encountered (Swindle, Wang and
Kuznik, 2010). These emulsions have wide spread
occurrence in petroleum recovery. The evaluation of
stability of emulsion systems and selection of optimal
conditions for oil recovery process must be closely
scrutinized to achieve effective separation (Poindexter, et
al, 2003).

Crude oil is a continuous, multi-component solution of
light and heavy hydro carbons which can be classified as
asphaltenes, hetero atomic species, high molecular weight
saturated alkanes and light gases. The light gases keep the
heavy components in solution and the solubility of these
components depends on the composition of the crude oil
and the operating conditions of pressure and temperature
during oil production. Crude oil is seldom produced alone
because it generally is commingled with water. The water
creates several problems and usually increases the unit
cost of oil production. The produced water must be
separated from the oil, treated, and disposed of properly.
All these increase costs. Moreover, sellable crude oil must
comply with certain product specifications, including the
amount of basic sediment and water (BS&W) and salt,
which means that the produced water must be separated
from the oil to meet crude specifications. Emulsions occur
in almost all phases of oil production and processing such
as inside reservoirs, wellbores, wellheads and also at wet-
crude handling facilities and gas/oil separation plants; and
during transportation through pipelines, crude storage,
and petroleum processing (Kokal, and Al-Dokhi, 2007).

Selecting the best demulsify for crude oil emulsion is very
important as it will aid in the development of cost-
effective separation of such an emulsion, providing an oil
phase containing no more than 0.3-0.5% water by volume
and an aqueous phase containing no more than 200 ppm
oil, preferably 100 ppm, reducing treatment cost on
emulsion resolution and generate revenue from the
residual quantities of oil, help overcome pumping
production encountered during the crude oil transportation
and processing, increase the Net Present Value of the
residual oil and minimize cost of treatment to maximize
profit. The work will be strictly based on experimental
treatment of emulsion form during by chemical enhanced
oil recovery process. Recovering (i.e displacing) trapped
oil will become increasing prevalent and important as
assets age and producers want to recover their remaining
reserves which in most cases are well in excess of what
they have produced to date (i.e over the current life of the
field) (Nguyen and Sadeghi, 2011).

Many analysts agree that around half the worlds original
proven oil reserves of around 2.2 trillion barrels of
conventional oil have now been produced, with about 1
International Journal of Engineering and Technology (IJET) Volume 2 No. 11, November, 2012
ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
1855

trillion remaining. Although estimates vary considerably,
the fact is that producing the second half of the worlds
ultimate recovery of conventional oil will be more
difficult than producing the first half. Oil production
growth is forecast to decline within the next few years, as
illustrated by Campbell-Laherrere; their predictions
suggest that production will soon be unable to keep up
with demand.

2. ENHANCED OIL RECOVERY

During the past 40 years, a variety of Enhanced Oil
Recovery(EOR) methods have been developed and
applied to mature and mostly depleted oil reservoirs (Fu
and Mamora, 2010). These methods improve the
efficiency of oil recovery compared with primary
(pressure depletion) and secondary (water flooding) Oil
methods. Each of these EOR methods are highly energy
intensive.

Enhanced Oil Recovery (EOR) is a term applied to
methods used for recovering oil from a petroleum
reservoir beyond that recoverable by primary and
secondary methods. Primarily recovery normally refers to
production using the energy inherent in the reservoir from
gas under pressure or a natural water drive. Secondary
recovery usually refers to injection of water or water
flooding. Thus, enhanced oil recovery is often
synonymous with tertiary recovery, although sometimes
Enhanced Oil Recovery methods can be used earlier in the
sequence. In some older discussions, water flooding was
considered as enhanced oil recovery, but now EOR is
generally thought to follow water flooding.

These groups of methods; 1 3 are well established while
4 is under developmental study. We have total of eleven
EOR methods grouped under four types:

(1) Thermal recovery methods are cyclic steam
stimulation, steamflooding, and insitu combustion.

(2) Gas miscible recovery methods are cyclic carbon
dioxide stimulation, carbon dioxide flooding, and
nitrogen flooding.

(3) Chemical flooding methods are polymer flooding,
micellar-polymer flooding and alkaline flooding.

(4) Microbial flooding methods include cyclic microbial
recovery and microbial flooding.

3. CHEMICAL ENHANCED OIL
RECOVERY METHOD

Due to a growth of petroleum demand and price, more
and more planned or anticipated EOR projects will
become reality. Chemical enhanced oil recovery (EOR)
methods are expected to play a major role in future global
crude oil production (Watkins, 2009; Hirasaki et al,
2009). While recovering the oil can be a challenge,
treating production that results from chemical EOR
projects can be an even greater challenge (Poindexter, et
al, 2003). During the application of chemical enhanced oil
recovery (EOR) floods, breakthrough of the injection
chemicals periodically occurs resulting in stable
emulsions. It is generally not possible to predict when
chemical breakthrough will occur and flood designs try to
eliminate this unwanted event from occurring. Some
Enhanced Oil Recovery recommendations use a
combination of surfactant and polymer (SP), alkaline,
surfactant and polymer (ASP), and variations on these two
themes.

In the event that chemical breakthrough does occur, it is
critical to have processes in place that can handle the ever
changing conditions that evolve during the course of
crude oil recovery. The emulsions from such floods can
yield both stable water-in-oil (normal) and oil-in-water
(reverse) emulsions particularly if the return of injection
chemicals is higher than expected. Injection chemical
packages often use surfactant-polymer (SP) or alkaline-
surfactant-polymer (ASP) mixtures (Nguyen and Sadeghi,
2011). These chemical cocktails are injected into the
formation, and by their very nature, facilitate the removal
of trapped oil. Surfactants lower the crude oil water
interfacial tension (IFT), polymers increase the viscosity
of the water phase which raises the capillary number and
alkali saponifies naturally occurring acids which can
increase their water solubility and further reduce the IFT.
All physical factors above that enhance oil recovery can
also greatly contribute to the formation of very stable
emulsions which are ultimately quite different from
naturally occurring emulsions which are stabilized by
asphaltenes and resins. Traditional demusifiers are often
not effective on emulsions created by chemical floods
Efeovbokha, et al, (2010). Like any emulsion, these
induced (i.e basically synthetic) EOR based emulsions
need to be resolved or broken. Producing dry oil
(generally < 0.5 BS&W), and clean water are
requirements that all producers must achieve (Kokal,
2005).

However, breaking dilute oil-in-water (O/W) emulsions
produced during surfactant/polymer (SP) and
alkaline/surfactant/polymer (ASP) processes for
Enhanced Oil Recovery is important for process success.
These emulsions can be very stable, for example, as
discussed by Li et al, 2006 for ASP processes. Emulsions
for SP processes may have continuous aqueous phases
containing an anionic surfactant blend and high
molecular-weight, partially hydrolyzed polyacrylamide.

Owing to dilution by mixing with reservoir brine and the
polymer drive, surfactant concentrations vary during the
process and may range from below 0.1 to perhaps 0.5%
by weight, depending upon such factors as injection
concentration, reservoir heterogeneity, and process
International Journal of Engineering and Technology (IJET) Volume 2 No. 11, November, 2012
ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
1856

design. Polymer concentrations up to about 0.1% by
weight may be expected. Total dissolved solids may be 1-
5% by weight with some hardness. A cosolvent, such as
an alcohol, may also be present in the EOR chemical
blend. The surfactant is preferentially soluble in the
aqueous phase for these conditions and solubilizes some
oil. That is, the aqueous phase is an Oil/Water
microemulsion. A typical process requirement is to
develop a cost-effective separation of such an emulsion,
providing an oil phase containing no more than 0.3-0.5%
water by volume and an aqueous phase containing no
more than 200 ppm oil, preferably 100 ppm (Bryan and
Kantzas, 2009).

Much effort has been devoted to breaking crude oil-brine
emulsions from normal production operations (Angle,
2001; Sjoblom et al, 2003; Kilpatrick, 2009; Watkins,
2009; Hirasaki et al, 2009). Emphasis has been on
breaking brine-in-crude oil emulsions and, thereby,
reducing the brine content of the oil phase to acceptable
values. Asphaltene layers at the surfaces of the brine
drops are the chief source of emulsion stability in most
cases.

Many compounds have been proposed or used as
demulsifiers. One type of widely used demulsifier capable
of displacing significant portions of the asphaltene layers
in such emulsions and promoting coalescence consists of
ethoxylated and/or propoxylated alkylphenol
formaldehyde resins with molecular weights of a few
thousand daltons. Experiments have indicated that, for a
given emulsion, there is an optimal ratio of hydrophilic
and lipophilic properties for these non-ionic demulsifiers,
which provides the best separation (Berger et al, 1987,
Smith and Covatch, 1989, Paulis et al, 1997). This
behavior is consistent with observations that both oil- and
water-continuous emulsions stabilized by surfactants of
low molecular weight are least stable near conditions
where hydrophilic and lipophilic properties of the
surfactant film are balanced and spontaneous curvature is
zero.

Rondn et al (2007) perform experiment on breaking of
water-in-oil emulsions formed during oil slicks or
petroleum production operations. He stated that the
natural surfactant molecules (principally asphaltenes) that
are present in the crude oil are the cause of emulsion and
these persistent emulsions may be broken by adding a
suitable demulsifier at the proper concentration to attain a
so-called optimum formulation at which the stability of
the emulsion is minimum. In his report, the concentration
of asphaltenes was varied by diluting the crude oil with a
solvent such as cyclohexane, toluene, or mixtures of them.
His experimental evidence showed that there exists some
critical asphaltene concentration at which the interfacial
zone seems to be saturated. Beyond this threshold, which
is typically around 1000 ppm of asphaltenes, the
demulsifier concentration necessary to attain the
emulsions quickest breaking is constant. Below it i.e.
when the crude is highly diluted with a solvent, the
optimum demulsifier concentration is found to be
proportional to the asphaltene concentration. He went
further to establish a map of emulsion stability versus
asphaltene and demulsifier concentrations which exhibits
a typical pattern for different demulsifiers and diluents
and contributes to improving the interpretation of the
demulsifying action.

4. MATERIALS AND METHODS

The materials used for the experiment are crude oil, pure
cationic surfactants of the type:
Al kyl t r i met hyl ammoni umbr omi des (C
6
-C
18
),
Al kyl di met hyl benzyl ammoni umbr omi des (C
10
-
C
18
), Polymer (partially hydrolyzed polyacrylamide,
HPAM), Alcohol propoxylate sulphate and alkyl sulfonate
surfactants, brine solution and Diethylene glycol
monobutyl ether (DGBE) and Iso-butanol co-solvent.

4.1 Experimental Methods

The experimental methods is divided into three steps to
generate raw data to show the effectiveness of the
chemical demulsifiers listed above as capable of breaking
oil/water emulsions for improved oil recovery operations.

4.2 The Properties of Crude Oil

The physical and chemical properties of crude oil used for
the experiment such as API gravity, viscosity, the
asphaltene content and the mass of KOH/g of oil were
obtained and listed in table 1.

4.3 Preparation of SyntheticProduced Brine

A 5-gallon bucket (19.08 litres) was used to prepare a
solution of synthetic produced brine by adding
deionized water and brine solution. Then, polymer
(partially hydrolyzed polyacrylamide,HPAM) was added.
The solution was slowly stirred for about 30min so as not
to form clumps commonly known as fisheyes. The mixing
continues for about 1hour. Thereafter, the preweighed
surfactants (0.05 wt%) of alkyl-trimethyl ammonium
bromides (C
6
-C
18
),
alkyldimethylbenzylammoniumbromides (C
10
-C
18
), were
added with alcohol propoxylate sulpahate and
alkylsulfonate surfactants and the resulting solution was
stirred with a rod at 8rpm for another 30 min for proper
blending.

4.4 Emulsion Preparation

The emulsion was prepared in (177 ml) glass prescription
bottles by mixing the produced water (synthetic
produced brine) with oil. The mixture of the brine
solution and crude was done in the ratio of 7:3, 70 ml of
synthetic produced brine using prescription bottles
marked at 100 ml levels. A funnel plastic beaker was used
International Journal of Engineering and Technology (IJET) Volume 2 No. 11, November, 2012
ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
1857

to pour 30 ml of crude oil into each of the prescription
bottle to the 100 ml mark. The prescription bottle samples
of emulsions were placed on the Eberbach shakers on
high speed for 10 min to mechanically mix the mixture
together.

4.5 Demulsification Tests

The demulsification tests were conducted in graduated
177 ml glass prescription bottle to allow for rapid water
drop readings. About 200 ppm of demulsifiers (chemicals
for demulsification) Separol NF-36 was added on the
basis of the total weight of emulsion about 50 ppm. The
resulting mixture in the sample bottles was then placed on
Eberbach shakers on high speed for a 240 shakes/min for
10 min after which they were removed and emulsion
separation noticed in the emulsion samples were recorded
at various time intervals and water drop readings were
recorded in milliliters as a function of time. Water drop
values were equally used to gauge emulsion stability.
Water samples were withdrawn from the bottom of the
bottles using a syringe and the oil concentrations in water
were measured from the turbidity measurements to
indicate the slug grindout number. After the water drop
readings, the resolved or partially resolved oil from each
bottle was analyzed for water content. Using a syringe
with a blunt-tipped needle, a small portion of the oil
(about 6 ml) was withdrawn off with the tip of the syringe
which was set to 15-20 ml above the theoretical oil-water
interface as determined by the slug grind out value (a
procedure that measures the water content of the
emulsion). The treated emulsion of oil of about 200 ppm
was added to a graduated API centrifuge tube containing
an equal volume of an aromatic solvent (Iso-butanol co-
solvent), and the contents was shaken by hand. The
centrifuge tubes were then centrifuged at high speed of
2700 rpm for 3 min. After centrifugation, the percent
residual emulsion, typically referred to as basic sediment
(BS), and the percent water (W) were noted for each
bottle. After recording BS&W values, an akylsulfonate
surfactant (a chemical known to resolve the remaining
emulsion) was added to completely knockout remaining
water from the emulsion at a higher dosage of about 300
ppm to the centrifuge tube. Such chemicals are generally
called slugging or knockout chemicals and are typically
low-molecular-weight sulfonate-based materials. After
slugging, the tube was again shaken and centrifuged as
previously described. The basic sediment was therefore
completely eliminated and only water remained in the
bottom part of the. Lastly, the slug grindout number (a
measure of the water content of the emulsion) was
prepared as a percentage while smaller values of BS&W
and slug indicate drier oil.

5. RESULTS AND DISCUSSIONS

The results of this work are presented in tables 1 to 4 and
figures 1 to 5. The tables 1 to 4 shows the properties of
crude oil used, slug grindout (BS&W), Oil content in
water and effects of the cationic demulsifier dosage and
settling time on BS&W for emulsions respectively, while
figures 4 and 5 shows the effects of the cationic
demulsifier dosage and settling time on BS&W for
emulsions and relationship between the oil concentration
and settling time with and without a cationic demulsifier
for emulsions respectively.

The cationic surfactants of the type
akyltrimethylammonium bromide were used to determine
the effect on water and oil separation of produced
emulsions resulting from surfactant-polymer floods. A
clear separation of aqueous phase was found upon
addition of around 200 ppm n-octyltrimethyammonium
bromide (C
8
TAB). The addition of this demulsifier to the
produced brine did not appear to produce any
precipitation, even when heated to about 40
0
C.
Precipitation can occur in mixtures of cationic and ionic
surfactants. With 200 ppm of added C
8
TAB, the
cationic/anionic surfactant mole ratio is about 1:3,
significantly lower than the 1:1 molar ratio where
precipitation usually occurs. These surfactants are soluble
in water but combine with anionic surfactant present in
the brine of the initial emulsion to form ion pairs and
reduce electric charge at the oil-water interfaces, thereby
shifting phase behaviour of the oil/brine/surfactant system
in the desired direction. C
8
TAB seemed particularly
effective at concentrations of 200 and 300 ppm. It
produced clear brine phases (by visual inspection) after
several hours and reduced water content in the oil to 0.8
per cent by volume after 2.75 h as shown in figure 1
below.

Preliminary Experiments, 18 Hours Equilibration

1 2 3 4 5

Figure1. Preliminary screening experiments for emulsions
with 30% oil cut at ambient temperature

1 - 200ppm EO/PO Demulsifier A; 2 - 200ppm C
8
TAB; 3 -
100ppm C
8
TAB; 4 - 2000ppm C
8
TAB; 5 - 200ppm Cationic
Demulsifier V
Results of the bottle tests of figure 2 shown below
indicate that the clearest aqueous phases were obtained
with the combination of 50 ppm of demulsifier A and 50
ppm C
8
TAB, followed by 50 ppm demulsifier A with 30
ppm C
14
TAB respectively. These combined systems all
have improved clarity of aqueous phases compared to 200
ppm C
8
TAB alone. The results indicate a basis at 50 ppm
C
8
TAB for effective demulsification when used with 50
ppm demulsifier A for this system.

International Journal of Engineering and Technology (IJET) Volume 2 No. 11, November, 2012
ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
1858

Bottle Tests: Cationic Surfactants &
Demulsifier A, 21 Hours Equilibration


1 2 3 4 5

Figure 2. Separation produced by demulsifier A and
different chain length of surfactant combinations after 21
hours for emulsions with 30% oil cut and ambient
temperature

1 No added chemicals; 2 Demulsifier A + C
8
TAB; 3
Demulsifier A + C
12
TAB; 4 Demulsifier A + C
14
TAB; 5
Demulsifier A + C
16
TAB

Similarly, microscopy studies showed large oil droplets
separating from the emulsion shortly after the addition of
C
8
TAB, with larger droplets found at higher doses as
shown in figure 3 below.

Microscopy of Emulsions after 1 Minute


Untreated 50ppm C
8
TAB


100ppm C
8
TAB 200ppm C
8
TAB

Figure 3. Microscopy of emulsions with 30% oil cut at
ambient temperature

Table 1: Properties of Crude Oil

Properties SP Oil
API (at 20
0
C) 47.2
0
Viscosity (at 20
0
C, cP) 2.2
Specific gravity (S.G) 0.7918
Pour Point 3
0
C
Wax, wt% 1.53
Sand content 15.4
BS&W % vol. 30.0

Table 2: Slug Grindout (BS&W) Percent

Emulsion Grindout (BS&W) per
cent
Untreated 30
Emulsion + C
6
TAB 3.0
Emulsion + C
8
TAB 0.4
Emulsion + C
16
TAB 1.0

From the analysis of table 2 above, the slug grindout
number (a measure of the water content of the emulsion)
greatly reduced from the initial 30% by volume to 0.4%
by volume by addition of C
8
TAB surfactant.

Table 3: Oil Content in Water (ppm)*

Emulsion Oil Content in Water
(ppm)*
Untreated 224
C
6
TAB 172
C
8
TAB 112
C
16
TAB 204

From table 3 shown above, it was observed that the lowest
value of oil content in water was obtained when C
8
TAB
was added to the emulsion showing the effectiveness of
this surfactant at resolving emulsion problems.

Table 4: Effects of the Cationic Demulsifier Dosage on
BS&W for emulsions with 30% oil cut at ambient
temperature and 40 min settling time

Cationic Demulsifier
Dosage (ppm)
BS&W (%)
Untreated 13.8
50 8.8
100 0.9
200 0.6
300 0.6

From the observation of table 4 above rapid separation did
not occur below 200 ppm, which is consistent with the
observation that aqueous phase had reduced clarity below
that dosage level as shown in table 4. It was found that the
value of BS&W decreased with an increase in demulsifier
dosage and settling time. At a demulsifier dosage of 200
ppm, BS&W decreased from 13.8 (untreated) to 0.6 per
cent after 40 min of settling time. Similarly, figure 4
shown below indicates the effect of dosage and settling
time on BS&W and oil content of the water phase for the
cationic demulsifier. The oil content was reduced from
550 to 70 ppm after 4 h. These results showed that oil-
water separation was improved with the use of the
demulsifier.

International Journal of Engineering and Technology (IJET) Volume 2 No. 11, November, 2012
ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
1859


Figure 4. Relationship between the oil concentration and
settling time with and without a cationic demulsifier for
emulsion with 30% oil cut at ambient temperature

6. CONCLUSION

In this research work, the addition of 200 ppm of suitable
surfactants accelerated the separation of oil-water
emulsions representative of produced emulsions expected
during chemical enhanced recovery operations and
yielded oil and water phases with highly improved quality
compared to the initial emulsions. Microscopy test
confirmed that 200 ppm n-octyltrimethyammonium
bromide (C
8
TAB) produced significant coalescence
shortly after it was added to the emulsions. This is in
agreement with an increase of the oil droplet size in the
presence of the demulsifier. While these results were
obtained in connection with emulsion treatment studies
specific for surfactants/polymer (SP) flooding, it is
expected that the basic principle of using cationic
surfactants demulsifier will be applicable to other similar
processes employing anionic surfactants.

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International Journal of Engineering and Technology (IJET) Volume 2 No. 11, November, 2012
ISSN: 2049-3444 2012 IJET Publications UK. All rights reserved.
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