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Separation study of BS-4 emulsions and evaluation of the HTVIEC


technology from Aibel

Contact person from Marketing and Sales, Aibel T&P (name/email/telephone)

Runar Sunde Olsen, Sales Manager, Aibel Technology and Products,


Runar.Sunde.Olsen@aibel.com
Responsible from Aibel T&P:

Andreas Hannisdal, Sr. Engineer, Aibel AS Technology and Products.


Andreas.Hannisdal@aibel.com, +47 47453384
Author(s)/Source(s):

Date issued:

A. Hannisdal

16.04.2008

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TABLE OF CONTENTS

1.

INTRODUCTION......................................................................................................... 3

2.

EXPERIMENTAL ........................................................................................................ 6

2.1
2.2
2.3

Materials ................................................................................................................................6
Experimental setup ................................................................................................................6
Experimental design...............................................................................................................8

3.

RESULTS ................................................................................................................... 9

3.1

Screening phase ....................................................................................................................9

4.

DISCUSSION............................................................................................................ 20

4.1
4.2

Comparing results from different studies..............................................................................20


Expectations and extrapolations...........................................................................................21

5.

CONCLUSIONS AND RECOMMENDATIONS ......................................................... 22

6.

REFERENCES.......................................................................................................... 24

7.

APPENDICES........................................................................................................... 25

7.1
7.2
7.3

Level sensors .......................................................................................................................25


Raw data for droplet size analyses.......................................................................................26
Raw data for separation tests...............................................................................................26

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INTRODUCTION

Separation tests with the BS-4 crude oil from Shell were done at high temperatures and pressures
to conclude on the efficiency of gravitational and electrostatic destabilization processes at relevant
conditions.
Electrocoalescers are the working horses in heavy oil process trains. Even when the first and
second stage separators are operated properly, the separation efficiency is greatly limited by the
slow sedimentation velocity of small droplets in the viscous heavy oil. The electrostatic fields
between the electrodes in the electrocoalescer can provide considerable droplet growth and
dramatically increase the sedimentation velocity of water droplets. Traditional electrocoalescers (oil
treaters) have non-isolated electrodes and are for that reason placed downstream of normal gravity
separators to avoid too high water loading and short-circuiting followed by collapse of the electrical
field. Recently, other non-traditional electrostatic coalescer units have appeared in the market,
including the CEC from Aker Kvaerner (Norway), the Dual Polarity treater from Natco (US), and the
VIEC from Aibel (Norway). All these products have completely or partially isolated electrodes to
avoid short-circuiting at high water cuts. Here, the Vessel Internal Electrostatic Coalescer (VIEC)
technology from Aibel has been evaluated since it will be particularly applicable for heavy oil
processing with the new spin-off product for high temperatures, the HTVIEC.

Figure 1: Principle of electrostatic coalescence.

In all alternating current (AC) electrocoalescers with isolated electrodes, droplet-droplet attraction
occurs as a result of the interaction between dipoles induced on water droplets. When a nonuniform field (set up by the presence of nearby droplets) is in alignment with the dipole, one end of
the dipole will be in a weaker field, resulting in a net force pulling the dipole towards the place of
greatest field intensity. As the inter-droplet distance decreases, the attractive force between droplets
increases until the contact occurs in a point which becomes a region of very intense localized

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electric field. Two droplets merge together to form a bigger droplet which will settle faster (according
to Stokes law). As mentioned already, the HTVIEC is a high temperature version of the classic
VIEC. The VIEC has been presented previously (Less, 2008, Fjeldly, 2006). Shortly, the High
Temperature Vessel Internal Electrostatic Coalescer (HTVIEC) technology introduces the
electrocoalescence process into conventional upstream separation vessels to enhance the speed
and effectiveness of water-oil separation. The system is built as a wall of coalescer modules, sitting
vertically across the cross-section of the vessel (Figure 2). Each stainless steel module consists of a
matrix of 1 inch ceramic tubes (20 cm long), placed between horizontal electrodes in a unit which
can be introduced into the separator through a standard manhole. Unlike conventional electrostatic
coalescers, the system thus has electrical isolated electrodes that make the HTVIEC functional in all
kinds of fluids without short-circuiting. Low voltage is supplied to the system and converted to high
voltage in the transformer inside each individual module. Emulsion is flowing inside the tubes in the
module. The resulting high voltage AC field applied across the tubes forces the water droplets in oil
to coalesce due to polarisation effects. Due to the increase in droplet size, the sedimentation speed
is increased and hence the separation is improved. HTVIEC can be installed as a retrofit or in new
built separators to enhance/ensure downstream performance (proper conditions for conventional oil
treaters). The separation process will be improved dramatically without an additional footprint. The
advantage of this improved separation can be realised in several possible ways like e.g. higher
liquid production, better oil quality, better water quality, improved level control, reduced chemical
consumption or reduced heating requirement. It is clear how the process train will benefit from
installing the HTVIEC in the first stage separator. By increasing the water discharge, the oil quality
from the first stage separator will be improved. Both the flow rate and the viscosity of the water-in-oil
emulsion will be reduced, which will enhance the heat transfer process and reduce the demand for
interstage heating. With improved overall separation performance, it will be possible to reduce the
temperature in the process train and still reach the performance that was achieved without HTVIEC.

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Figure 2: HTVIEC wall covering the cross-section of a separator. Each module has a matrix of tubes (emulsion
flows inside these) and a transformer (lower left corner of each module). A standard perforated plate has been
indicated in the section below the HTVIEC wall.

The oil/water separation process may be simulated in a flow loop if a sufficiently large sample is
available. The flexibility and availability of such tests are usually low. Therefore other separation
tests in earlier stages are necessary. Usually, one or several smaller scale tests are done in a
laboratory, either at ambient pressure or in more advanced separation rigs. The philosophy is to get
preliminary separation characteristics for design purposes. The following results show that the
emulsions with the BS-4 crude oil were very stable. Attempts were done to reduce the overall
stability of the system by increasing droplet sizes of the emulsion, increasing temperature, changing
or increasing dosages of demulsifiers. Still, the emulsions were too stable to show significant dropout of free water within realistic separation times. However, with applying the electrostatic HTVIEC
technology from Aibel, efficient phase separation was achieved within minutes. The results have
been discussed with results from the previous phase of the test program.

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2.

EXPERIMENTAL

2.1

MATERIALS

26

Crude oil from BS-4 (13 L) was left from the 1st phase of the testing (week 37, 2006). The sample
was free of water. The water phase for separation tests was prepared from tap water (pH 7) and
NaCl (30 g/L). The pH was adjusted by HCl addition. Demulsifier CC3737 from Servo, a demulsifier
from Petrobras and a non-specified demulsifier (Dem. X) was used during the study. Generally, the
oil-continuous demulsifiers were added to a toluene solution to have an accurate dosage. The
CC3737 demulsifier was also tested in a mutual dissolving phase (ethanol). Some separation tests
were done on diluted crude oil systems with toluene (p.a) or heptane (p.a).
2.2

EXPERIMENTAL SETUP

2.2.1

STABILITY TO ELECTRICALLY INDUCED SEPARATION SMALL SCALE VIEC TEST

Crude oil and water was heated to the specific temperature in a clima chamber. 250 ml emulsion
was produced by continuously adding more water to the oil phase and shake by hand. Droplet size
distributions were measured with a Vipa from JORIN Inc. Demulsifier (diluted in toluene) was then
added with a pipette and distributed in the emulsion sample by carefully shaking the sample for 1
minute. One half of the prepared emulsion (100 ml) was allowed to separate without applying
electrical forces. The other half of the w/o emulsion (100 ml) was subjected to an alternating
electrical field for 15 seconds. The emulsions were monitored to see the drop-out of a free water
phase. A scheme of the small scale test setup is showed in Figure 3.

Step-by-step test procedure:


1. Keep oil and water at the correct temperature, T
2. Mix in water by hand-shaking (or with a static mixer)
3. Measure the droplet size distribution (Vipa JORIN)
4. (Add demulsifier w.r.t total volume)
5. Divide the emulsion in two graded tubes
6. Subject one of the emulsions to an electrical field
7. Put both samples in an oil bath at T
8. Monitor the separation of free water

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100 ml

HV AC

Figure 3: Small scale separation test setup

2.2.2

STABILITY TO ELECTRICALLY INDUCED SEPARATION LARGE SCALE HIGH TEMPERATURE


VIEC TEST

A scheme of the test setup is showed in Figure 4 and 5. The vertical height of each sensor in the
level detection system can be found in the appendices. Droplet size distribution profiles are
presented in the appendices.
Step-by-step test procedure:
1. Keep oil and water at 90oC
2. Mix in water gradually by hand-shaking (external mixing to ensure w/o emulsion type)
3. Measure the droplet size distribution (Vipa JORIN)
4. Load the emulsion in the HP system, pressurize
5. Transport the system for 6 minutes while heating (dP = 0.2-0.3 bar over valve) or heat the
system without transport (static)
6. Measure the droplet size distribution (Vipa JORIN)
7. Add demulsifier and distribute for 1 minute
8. Pass the emulsion through the HT VIEC segment with power ON/OFF
9. Record separation with level detection system
10. Drain system when test is completed. Record the amount of free water phase for validation
of signal from level detection system

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Pressure release

PI
3 valve

Computer
Cleaning
PI
Gear pump

TI

Electrodes

Separator

To droplet size
analyser

VIEC Power supply

Multiplexer

T-contol reservoir

N2

PI

T-contol separator

Chemical
injection
point

Reservoir

PI

TI

HV
trafo

waste

Figure 4: High temperature separation test scheme. Heat tracing, internal heating and pressure release valves
are not included in the figure. Tubing diameters are 1 inch (from reservoir to separator), 12 mm (mixing loop),
and 10 mm (gas loop).

Figure 5: High temperature separation test rig.

2.3

EXPERIMENTAL DESIGN

According to the contract: document EPP-2007-XXXX from the client 27 data points were planned.
The planned data points were in the following ranges: Temperatures = {170, 230, 300 F}, Watercut
= {30, 50, 70}, Particle size = {50, 200, 500}. No tests with electrical fields were included. Aibel

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stated that the proposed test matrix was limited by the amount of crude oil left (reported to be 13 L).
The 27 tests required more than 13 L. It was not an option to get more sample. Moreover, it was
explained before approving the contract that the maximum size in the lab would be from 100-200
m. Shell was continuously informed about all variations to the experimental design.
Table 1: Deliverables

Type of result

3.

Presented

Planned

HP tests

15

< 27

LP tests

12

Droplet size determination

yes

yes

Rawdata

yes

yes

Expectations on real performance

yes

yes

RESULTS

Very stable emulsions were observed even at high temperatures and large droplet sizes. For that
reason, the planned test scheme including experiments at low temperature and small droplet sizes
had not the same relevance. These would produce too stable emulsions. The contractor had to
deviate from this scheme and provide experiments at conditions were the potential for achieving
separation was the best: as large droplets as possible, as high temperature as possible, increased
dosage of demulsifier. To understand the progress of the study, the test program is described
chronologically below. The results will be presented and discussed with reference to the separation
profiles attached.
3.1

SCREENING PHASE

The screening showed a clear tendency for phase inversion even at low water cut when water was
present in the mixture initially. To have control over the emulsion process, a step vise introduction of
water to the oil phase seemed to be a good solution. Water-in-oil emulsions were achieved for 30%
and 50% water cuts. It was decided that the mixing process was going to be performed externally at
90oC; the emulsion was then loaded into the test reservoir, heated it to the desired temperature;
demulsifier was added, and the separation performance was analyzed. The emulsion type was
properly controlled and the droplet size distribution of the emulsion could be analyzed before
loading the emulsion into the test rig. The droplet size distribution was in the 10-130 m range as
presented in Figure 7. To avoid separation during the heating time (6 minutes), the emulsion was

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26

transported in the mixing loop with a full valve opening of the needle valve. The resulting pressure
drop was only 0.2 bar. It seemed reasonable to expect a certain separation at 110oC and 30%
water, even without electrostatic treatment. At this condition, the oil viscosity was about 58 cP.
TEST A, 110oC VIEC OFF, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. Result: No separation after 60 minutes. Ref. Figure 6 (and 8).
A sample from the bottom of the separator, collected after 60 minutes verified that no free water
was present in the separator. Since no separation was achieved during the first 60 minutes, the
corresponding test at 135oC was performed. The preparation method was identical to test A, and
the droplet size distribution was in the 10-130 m range.
TEST B, 135oC VIEC OFF, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. Result: No separation after 50 minutes. Ref. Figure 6 (and 8).

Again, sampling from the separator showed no separated water after 50 minutes. Without
separation even at 135oC and with 100 ppm of demulsifier, we got an indication of the great stability
of these emulsions. At 135oC the crude oil viscosity was about 25 cP. To test the efficiency of
electrostatic treatment, the test at 135oC and 30% water was done by subjecting the emulsion to an
electrical field when flowing through the 1 inch tube from the reservoir to the vertical separator. The
corresponding tests at 50% water were also performed, with and without applying the VIEC
technology. Moreover, the separation test with VIEC ON at 110oC was performed to complete this
part of the test scheme and to compare with the test done without subjecting the emulsion to an
electrical field (Test A). The separation profiles are presented in Figure 6. For all tests, the amount
of free water collected from the separator after the test matched perfectly with the signals of the
level detection system.
TEST C, 135oC VIEC ON, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. Ref. Figure 6 (and 8).
TEST D, 135oC VIEC ON, 50% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. Ref. Figure 6 (and 8).

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TEST E, 135oC VIEC OFF, 50% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. Result: No separation after 30 minutes. Ref. Figure 6 (and 8).
TEST F, 110oC VIEC ON, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. Ref. Figure 6 (and 8).
70

60

Remaining water in oilphase (%)

VIEC OFF 50% 135C


50
no separation

40

VIEC OFF 30% 135C


30

VIEC ON 30% 110C

20

VIEC ON 50% 135C


10
VIEC ON 30% 135C

0
0

10

15

20

25

30

Time (min)

Figure 6: Separation profiles from experiments in the HT separation system (Test A F)

Figure 6 clearly shows the dramatic improvement in separation performance by subjecting the
flowing emulsion to an electrical field. The profiles indicated a sudden knock-out of emulsified water
droplets, followed by a certain phase separation during the first 10 minutes of gravitational
separation. No further separation was observed. The results gave optimism with respect to the
efficiency of electrostatic treatment methods for the BS-4 crude oil emulsions. However, it was
important to also have separation of the emulsions which were not subjected to electrostatic fields.
The efficiency of the process train could not rely only on the efficiency of the VIEC technology. A
separation of the VIEC OFF experiments would also be beneficial to get a proper base case for the
VIEC ON experiments. With this in mind, attempts were done to produce a coarser emulsion
characterized by even larger droplets than in the 10-130 m range. The standard preparation

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26

procedure involved adding water corresponding to 5% of the emulsion, then shaking 20 times. The
process was repeated until all water was emulsified. A coarser w/o emulsion could be expected by
either reducing the mixing energy (fewer shakes) or increasing the amount of water added each
time. However, these attempts (see TESTS G) produced inverted emulsions of the o/w type. With a
partial separation of the excess water, the emulsions gave an oil-continuous upper phase with
droplet sizes in the 10 to 130 m range. A droplet size of 130 m seemed to be the upper limit of
what we could produce in a laboratory scale experiment.
TESTS G:
50% water, Mixed by handshaking (10%, 20 shakes); Result: not properly emulsified, o/w. Droplet
size in oil phase [10,130] m

50% water, Mixed by handshaking (5%, 10 shakes); Result: not properly emulsified, o/w. Droplet
size in oil phase [10,130] m

50% water, Mixed by handshaking with all the water present initially; Result: not properly emulsified,
o/w. Droplet size in oil phase [10,130] m

In test F, droplet analyses were performed both before and after subjecting the emulsion to a 6
minutes transport in the loop. Unfortunately, the droplet size distribution was shifted to slightly
smaller droplets during the transport process, even though the pressure drop over the needle valve
was minimal (0.2-0.3 bar). The distribution is presented in Figure 7 (green) whereas all distribution
profiles are presented in the appendices. To analyse the validity of previous separation tests, a new
test was performed at 135oC by heating and pressurizing the emulsion without any mixing (to have
the demulsifier distributed properly, the system was mixed for a couple of seconds). A droplet size
analysis verified that the distribution was unchanged. Still, no separation was achieved during the
first 75 minutes of gravitational separation.
TEST H, 135oC VIEC OFF, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
added after mixing. NO TRANSPORTATION IN LOOP. Result: No separation after 75 min.

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100 %
90 %
80 %

Cumulative Volumetric .

70 %
Large scale before transport

60 %

Large scale after transport


Small scale

50 %
40 %
30 %
20 %
10 %
0%
0

20

40

60

80

100

120

140

160

d (microns)

Figure 7: Examples of cumulative volumetric droplet size distributions from large and small scale experiments.
The two profiles from large scale experiments represent the droplet size distribution after the external mixing
procedure (blue) and after additional mixing in the mixing loop (green).

This emulsion was the most unstable system tested (highest temperature, largest droplets). With
this result, the outcome of the previous test with VIEC OFF was validated. No separation was
achieved. A slightly better separation of the VIEC ON experiment could be expected by increasing
the size from about 10-80 m to about 10-130 m. However, as the experiments already showed
good separation, it was decided not to redo these analyses. The major challenge was to achieve
some separation without electrical fields.

A next approach was to study the stability of emulsions with very high water cuts (70%). From the
previous tests (TEST G) a phase inversion phenomenon was expected during the preparation of the
emulsion. It was still decided to follow the same procedure as used for previous analyses and load
the emulsion system into the HP test system. A water-continuous system would have to flip over to
oil-continuous with the separation of water.
TEST I, 135oC VIEC OFF, 70% water, Mixed by handshaking (5%, 20 shakes), Inversion at 5560%, Droplet size in oil phase [10,130] m, 100 ppm CC3737 added after mixing. Ref. Figure 8.

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TEST J, 135oC VIEC ON, 70% water, Mixed by handshaking (5%, 20 shakes), Inversion at 60-65%,
Droplet size in oil phase [10,130] m, 100 ppm CC3737 added after mixing. Ref. Figure 8.

Phase inversion from w/o to o/w type was identified at 55-60% and 55-60% water for test I and J,
respectively. Droplet size distributions of the top layers were in the usual range from 10 to 130 m
before loading the emulsions into the test rig. Droplet size distributions from the HP rig was not
possible in this case because of partially water-continuous and partially oil-continuous regions in the
sample. The separation profiles are presented in Figure 8. Interestingly, the VIEC OFF experiment
at 70% water cut showed an instantaneous dropout of water to about 58% remaining water. This
matched perfectly with the observed phase inversion phenomenon during emulsion preparation. No
additional separation was observed after the initial dropout of free water. With electrostatic fields
water could be knocked-out immediately to a remaining 35% of water in oil emulsion. The VIEC ON
experiment was not allowed to separate before passing it through the VIEC segment. For that
reason, we can expect some water bridges to steal some of the field set up over the electrodes. For
that reason, the efficiency of this test was not as god as the oil-continuous tests at 30 and 50%
water. The effect of the electrostatic field was still prominent.

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Aibel WBS 004610-09


Separation tests BS-4 HP

15

26

70

60

VIEC OFF 70% 135C Water continuous initially

Remaining water in oilphase (%)

VIEC OFF 50% 135C


50
no separation

40

VIEC ON 70% 135C Water continuous initially


VIEC OFF 30% 135C

30

VIEC ON 30% 110C

20

VIEC ON 50% 135C

10

VIEC ON 30% 135C


0
0

10

15

20

25

30

Time (min)

Figure 8: Separation profiles from experiments in the HT separation system (Test A F, I-J)

With the objective of improving the separation of water from the emulsions, the dosage of
demulsifier was increased from 100 to 400 ppm. Moreover, the demulsifier was added upstream of
the point of mixing to see if the presence of demulsifier initially would change the picture. The
demulsifier molecules have usually much faster adsorption kinetics to the oil/water interface than
amphiphilic crude oil components. By being present before droplets were created, we could expect
that the demulsifier would contribute more importantly to the overall character of the interfaces. The
produced droplet size distribution was in the 10-130 m range and the emulsion was heated without
transportation to keep that particular distribution during the test. The separation profile is presented
in Figure 9. Again, very little separation occurred, from 30% to 22%, during the first 60 minutes of
gravitational separation. It seemed like the transition from totally stable to partially stable emulsions
had been reached.
TEST K, 135oC VIEC OFF, 30% water, Mixed by handshaking (5%, 20 shakes), 400 ppm CC3737
added before mixing. NO TRANSPORTATION IN LOOP. Ref. Figure 9.

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Separation tests BS-4 HP

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26

To check the effect of the particular Servo CC3737 demulsifier, another demulsifier was selected for
a test run. The Petrobras demulsifier had previously showed good performance for the coalescing
process for stable emulsions. 100 ppm of the demulsifier was added. Again, a certain separation of
water was observed during the first hour. The separation profile is presented in Figure 9. A test
where the CC 3737 demulsifier was added in ethanol was also performed to rule out any effect of
the solvent used for diluting the chemical to an accurate dosage. The change did not seem to affect
the effect of the demulsifier. No separation was observed during the first 70 minutes.
TEST L, 135oC VIEC OFF, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm Petrobras
demulsifier added after mixing. NO TRANSPORTATION IN LOOP. Ref. Figure 9.
TEST M, 135oC VIEC OFF, 30% water, Mixed by handshaking (5%, 20 shakes), 100 ppm CC3737
demulsifier diluted in ethanol added after mixing. NO TRANSPORTATION IN LOOP. Result: No
separation after 70 min.

70
30% BS&W 400 ppm 135 degC
60

Remaining water in oilphase (%)

30% BS&W 100 ppm Petrobras demulsifier, 135 degC

50

40

30

20

10

0
0

10

20

30

40

50

60

Time (min)

Figure 9: Separation profiles from experiments in the HT separation system (Test K and L)

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Separation tests BS-4 HP

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With this, the high temperature/pressure testing was ended. The most favourable conditions for
efficient separation had already been tested: high temperatures, large dosage of demulsifier, large
droplets. The emulsions were still very stable. The only successful separation methodology was
electrostatic treatment. It was decided to proceed in smaller scale because of the limited amount of
sample left. Moreover, we had to address the deviation between HT/HP tests on undiluted crude oil
and results from phase 1 where the BS-4 crude oil was diluted in naphtha (Tb:160-180oC, 0.86-0.88
g/cm3, 1mm2/s) to a viscosity of 30 mPas at the test temperature. As seen from Figure 12, these
experiments had showed separation even without electrostatic means, particularly at higher water
cuts.
The BS-4 crude oil was diluted with toluene to a viscosity of about 25 mPas at 77oC (13 wt.%
solvent). Toluene would be the optimum solvent for the heavy BS-4 crude oil with respect to the
solvency of asphaltene molecules. The emulsions were produced similarly to the experiments in
large scale, but with lower mixing. By shaking the smaller sample volume 10 times instead of 20
times, comparable droplet size distributions were produced. An example of the cumulative
volumetric distribution profile is presented in Figure 7 (dark blue). Figure 10 shows 3 replicated
separation tests with the diluted BS-4 crude oil diluted in toluene. Again, it was a huge difference
between experiments with and without applying the VIEC technology. These tests were done on
identical emulsions (divided in 2). It was some scattering between replicated experiments with VIEC
OFF, but the main trend was clear: the oil quality could be improved from 30% to better than 5%
during the first 10 minutes after being subjected to the electrical field. As a comparison, experiments
with undiluted oil at 135oC (Figure 6, similar viscosity of oil phase) gave a 30 to 10% during the first
10 minutes (5% after 17 minutes). The results matched very well. By comparing results from VIEC
OFF experiments in Figure 10 and Figure 6, it was clear that the diluted emulsions were less stable
than the undiluted emulsions. A separation from 30% to 23% was observed during 60-80 minutes of
gravitational separation. The effect of changing to another demulsifier was not significant.
TESTS (8) N, Crude oil diluted in toluene to 25 cP, 77oC VIEC ON/OFF, 30% water, Mixed by
handshaking (5%, 10 shakes), Ref. Figure 10.

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Separation tests BS-4 HP

18

26

30

Remaining water in oilphase (%)

25

20

15

10

0
0

20

40
Time (min)

60

VIEC OFF 100 ppm CC3737

VIEC ON 100 ppm CC3737

VIEC OFF 100 ppm Dem X

VIEC ON 100 ppm Dem X

80

Figure 10: Separation profiles from experiments in the small scale separation system (Tests N). The crude oil
was diluted in Toluene to 25 cP at 77oC. Tests were performed at 77oC.

The same drill was done for a crude oil system diluted in heptane. Heptane is a low viscous aliphatic
solvent with poor solvency of asphaltene molecules. Again the crude oil was diluted to about 25
mPas at 77oC. Figure 11 shows the separation profiles of 30 and 70% water-in-oil emulsions. The
30% emulsions were more stable than the emulsions with oil diluted in toluene (Figure 10).
Increasing the amount of demulsifier from 100 to 200 ppm resulted in improved separation (Figure
11).
TESTS (6) O, Crude oil diluted in heptane to 25 cP, 77oC VIEC ON/OFF, 30%/70% water, Mixed by
handshaking (5%, 10 shakes), Ref. Figure 11.

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Separation tests BS-4 HP

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Finally, a test at 70% water was performed to see the effect of increasing the water cut. The 70%
emulsion in Figure 11 was viscous and showed no tendency to invert. The emulsion was a stable
w/o emulsion. The inversion point was shifted to greater values by the dilution process. For the
preparation of undiluted crude oil emulsions, the inversion point was about 60% (See text to Figure
8). When 100 ppm of demulsifier was added, the emulsions produced a separation profile as seen
in Figure 12. Half of the emulsion sample was subjected to an electrical field and showed an
instantaneous knock-out of water from 70 to 18 % WiO. The other half of the emulsion was left for
normal gravitational separation and was completely stable for 40 minutes, before showing a slow
separation to 40% water-in-oil after 100 minutes.

70

Remaining water in oilphase (%)

60

50

40

30

20

10

0
0

20

40

60

80

100

Time (min)
VIEC OFF 100 ppm CC3737 30%

VIEC ON 100 ppm CC3737 30%

VIEC OFF 200 ppm CC3737 30%

VIEC ON 200 ppm CC3737 30%

VIEC OFF 100 ppm CC3737 70%

VIEC ON 100 ppm CC3737 70%

Figure 11: Separation profiles from experiments in the small scale separation system (Tests O). The crude oil
was diluted in Heptane to 25 cP at 77oC. Tests were performed at 77oC.

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Aibel WBS 004610-09


Separation tests BS-4 HP

4.

DISCUSSION

4.1

COMPARING RESULTS FROM DIFFERENT STUDIES

20

26

Generally, the experiments performed on undiluted crude oil (135oC: 25 cP, Test C and Test H,
Figure 6) gave similar results to those performed with crude oil in toluene (77oC, 25 cP, Test N,
Figure 10). Without electrical fields, both the undiluted and the diluted crude oil emulsions gave little
separation of water during the first hour of separation (slightly better for diluted emulsions). With
electrical fields, the separation was instantaneous and resulted in 3-7 vol.% remaining water after
15 minutes of separation. The separation process was slightly better for diluted emulsions. These
emulsions (VIEC ON) were characterized by bigger droplets (<10, 130> m) than the undiluted
emulsions (<10, 80> m). As highlighted previously, the 30% emulsions of crude oil diluted in
heptane (Figure 11) were more stable than the emulsions with oil diluted in toluene (Figure 10).
Since the separation performance of BS-4 crude oil emulsions was analysed previously, it was
necessary to compare the results to the current study. The first study was done on BS-4 crude oil
diluted with naphtha to a viscosity of 30 cP. Results are showed in Figure 12. The results from tests
at atmospheric pressure with BS-4 crude oil diluted in heptane were presented in Figure 11. The
viscosity of the diluted crude oil was 25 cP at 77oC. The results in Figure 11 were not very different
from the results from phase 1 of the study (Figure 12). Both showed very little destabilization of the
VIEC off experiment and an important improvement by applying the VIEC technology. The
separation of water with electrostatic means was more efficient in phase 2 than in phase 1.
However, the droplet sizes in phase 2 tests were also much greater than in phase 1 tests. Tests at
70% water were performed to see the effect of increasing the water cut. In phase 1, an increase of
the water to 70% resulted in a collapse of the emulsions when demulsifier was present. The 70%
emulsion in Figure 11 was viscous and showed no tendency to invert. This difference in phase
inversion point influenced the performance at high water cut.

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Aibel WBS 004610-09


Separation tests BS-4 HP

21

26

60

35
30

50

VIEC OFF
20

Water in Oil (%)

Water in Oil (%)

25

VIEC ON

15

40

VIEC OFF
VIEC ON

30

20
10

10

0
0

10

20

30

40

50

10

20

30

40

50

Time (min)

Time (min)

70
60

Water in Oil (%)

50
VIEC OFF
40

VIEC ON

30
20
10
0
0

10

20

30

40

50

Time (min)

Figure 12: Figure 11, 12, and 13 from previous study on BS-4. The oil phase was diluted with naphtha to 30 cP at
70oC. Tests were performed at 70oC. 100 ppm CC3737 demulsifier.

4.2

EXPECTATIONS AND EXTRAPOLATIONS

Predicting separation performance in large scale from laboratory scale experiments is a challenge,
and can only be done after experience from several fields. From previous studies and comparison
with other laboratories, Aibel confirm that the results from the HP separation rig are on the
conservative side regarding oil quality. However, the experimental conditions and setup cannot
explain the extreme stability observed in the tests of the BS-4 emulsions. During the previous 2
years, the VIEC technology by Aibel has been successfully qualified (with similar studies as this) for
more than 30 crude oils in onshore and offshore test facilities. The crude oils range from API 11 to
36 with viscosities up to 100 cP. The BS-4 oil is among the most viscous crude oils being tested,
and the most stable one. Figure 13 shows results form the separation of an API 11.5 crude oil in the
same separation system as used for BS-4. Aibel propose that further testing, preferably on a new
BS-4 sample, is done to get the necessary confidence for designing and developing the field.

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Separation tests BS-4 HP

35

22

26

90 C

Remaining water in oilphase (%).

30

90 C

25
o

110 C
20
o

125 C

110 C
15
100 PPM DEMULSIFIER
o

VIEC OFF 125 C

10

125 C
5
NO DEMULSIFIER
VIEC ON

NO DEMULSIFIER
VIEC OFF

0
0

10

15

20

25

30

35

40

Time (minutes)

Figure 13: Example of results from another heavy oil (API 11.5) with the following viscosity of the oil phase: 100
mPas at 90oC; 60 mPas at 110oC; 35 mPas at 125oC.

5.

CONCLUSIONS AND RECOMMENDATIONS

The BS-4 crude oil produced very stable w/o emulsions with good reproducibility. The separation
performance was analyzed under pressure in 1 L experiments and with temperatures up to 135oC.
The gentle mixing procedure gave a lognormal droplet distribution function with a maximum of 130
m. Attempts to produce larger droplets were not successful. These formulations were either not
emulsified or produced inverted emulsions (o/w). Even with large water droplets, long separation
times, and with addition of demulsifier, very little free water was observed from the emulsions with
normal gravitational separation. However, with electrostatic separation methodology the separation
of water was dramatic from 30 to 20% at 110oC, and from 30 to 5%, 50 to 10% and 70 to 35% at
135oC. These results strongly support the use of electrostatic devices in early stages of the
separation trains and traditional electrocoalescers for the polishing stage. According to the scope of
work (EPP-2007-XXXX) phase 3 of the BS-4 project will involve Treater testing.

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Separation tests BS-4 HP

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26

Tests performed with diluted crude oil (toluene or heptane) at 77oC confirmed the results done
under pressure. The effect of electrostatic treatment was dramatic. Crude oil diluted in heptane
gave more stable emulsions than the corresponding emulsions produced with crude oil diluted in
toluene. The stability of the emulsions to normal gravitational separation was great, the large droplet
sizes taken into account.
We know from other studies of heavy crude oils that the BS-4 crude oil sample analyzed in Sept
2007 produced particularly stable water-in-oil emulsions. Figure 13 shows an example of an API
11.5 crude oil analyzed similarly to the BS-4 crude oil. The API 11.5 sample has a viscosity of 35,
60, and 100 cP at 90, 110, 125oC, respectively. An addition of 100 ppm of the same demulsifier
used for the BS-4 study dramatically changed the separation performance (VIEC OFF).

The results from Phase 2 suggest that it is difficult to design a crude dehydration process for BS-4
without including electrostatic treatment methods. To have a different separation character than
reported here, the crude oil or the demulsifier has to be different from the one used for this phase of
the test program. Aibel propose to initiate furter testing, preferably on a different sample from BS-4,
to see if the sample analysed in the current study was representative for the actual wellstream at
BS-4.

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Separation tests BS-4 HP

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26

REFERENCES

T. A. Fjeldly, E. B. Hansen, P. J. Nilsen, Novel Coalescer Technology in First-Stage Separator


Enables One-Stage Separation and Heavy-Oil Separation, OTC 18278, Houston, Texas, 2006.

S. Less, A. Hannisdal, E. Bjrklund, J. Sjblom, Electrostatic Destabilization of Water-in-Crude Oil


Emulsions: Application to a Real Case and Evaluation of the Aibel VIEC Technology, Fuels, 2008.

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Aibel WBS 004610-09
Separation tests BS-4 HP

7.

APPENDICES

7.1

LEVEL SENSORS
800

Sensor

700

600

500
Volume (ml)

V(ml)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41

400

300

200

100

25

26

h(cm)
20
20
23
25
30
30
35
40
47
50
58
67
78
90
102
110
128
143
160
180
200
220
240
265
290
319
350
377
404
435
465
493
518
547
578
609
638
664
690
720
750

4.0 *
4.6
5.2
5.8
6.4
7.0
7.6
8.2
8.8
9.4
10.0
10.6
11.2
11.8
12.4
13.0
13.6
14.2
14.8
15.4
16.0
16.6
17.2
17.8
18.4
19.0
19.6
20.2
20.8
21.4
22.0
22.6
23.2
23.8
24.4
25.0
25.6
26.2
26.8
27.4
28.0

41
40
39
38
37
36
35
34
33
32
31
30
29
28
27
26
25
24

9 10 11
5 6 7 8
1 2 3 4

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10

12 13

14 15

15

16

17

18

20

19

21

22

23

20

25

30

35

40

45

Sensor (no.)

Figure A-1: Vetical position of level sensors in the separator (top). Level rod (lower).

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Separation tests BS-4 HP

26

26

RAW DATA FOR DROPLET SIZE ANALYSES


1.2

Cumulative distribution frequency.

1.0

0.8
Test A before mixing
Test B before mixing

scattering

0.6

Test E before mixing


Test F before mixing
Test F after mixing
Test G -1

0.4

Test I before mixing


Test J before mixing
Test K before mixing
Test N

0.2

Test O 30%

0.0
0

20

40

60

80

100

120

140

Droplet size (microns)

Figure A-1: Droplet size distribution profiles.

7.3

RAW DATA FOR SEPARATION TESTS

Raw data for HP separation tests is attached as Excel files.

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