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SOCIETY OF PETROLEUM ENGINEERS OF AIME

6200 North Central Expressway


Dallas, Texas i5206
THIS

Flow

of
Oil

IS

=~~

A PREPRINT

---

SUBJECT

a Disperse
in

in

2481

TO CORRECTION

Emulsion

Water

SPE

Porous

of

Crude

Media

By
John

c.

(!artmill,U.S. Geological Survey, and Parke A.


.
American

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msmute

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of

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Iumwg,

Copyright
M..a-ll..

-Anm

Dickeyj

u.

of ~lsa~ Members Am

1969

1.1CLC9.SUX
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This paper was prepared for the khth Annual Fall Meeting of the Society of Petroleum Engineers
of AIME, to be held in Denver, Colo., Sept. 28-Ott. 1, 1969. Permission to copy is restricted to an
abstract of not more than 300 words. Illustrationsmay not be copied. The abstract should contain
conspicuousacknowledgmentof where and by whom the paper is presented. Publication elsewhere after
publication in the JOURNAL OF PETROLEUM TECHNOLOGY or the SOCIETY OF PETROLEUM ENGINEERS JCXJRNALis
usually granted upon request to the Editor of the appropriate journal provided agreement to give
proper credit is made.
Discussion of this paper is invited. Three copies of any discussion should be sent to the
Society of Petroleum Engineers office. Such discussion may be presented at the above meeting and,
with the paper, may be considered for publication in one of the two S?E magazines.
ABSTRACT
It has been suggested that oil migrates
through reservoir sands in the form of a fine,
disperse emulsion of oil in water, and that oil
accumulations occur where the stream enters
finer-grainedrock such as silt or shale. In
order to investigate the possible mechanisms,
stable emulsions of oil in water were prepared
without the use of wetting agents. They consisted of droplets 1/2 to 1-1/2 microns in
diameter, in a concentrationof 20 to 40 Parts
of oil per million of water. These emulsions
passed freely through filter paper and ordinary
sand. A plastic tube containing glass beads
of 200-microns diameter included a bed l/?-cm
thick of crushed beads 37 to 88 microns in
diameter. When the emulsion was passed through
this tube, up to 80 percent of the oil was
screened out at the coarse-fine interface. The
amount removed depended on the contrast in
grain size, the nature and the preferential
nettability of the media. Similar results
occurred when quartz sand was used as the
coarse, and crushed sand as the fine medi~.
I!his
screening did not occur as a result of
capillary effects, because the pores were manY
times the diameter of the droplets. The oil
collected as a result of flocculation of the
droplets into strings and clusters, and the oil
saturation in the pores consisted of masses of
droplets with very little coalescence. Possibly electrostatic forces are more important
than capillary in the behavior of fine,
References and illustrationsat end of paper.

disperse, oil-in-wateremulsions. Our current


ideas on multiphase flow in porous media may
not apply to disperse emulsions.
INTRODUCTION
The physical mechanisms of the migration
of oil, including the expulsion of oil from the
source rock, its migration, and its accumulation in the reservoir rock, are very poorlY
understood. Most authoritiesbelieve that the
expulsion of water from compacting shale causes
regional flows of water within the pores of the
enclosing sediments, and the water somehow
carries the oil with it. Hydrocarbons heavier
than decane have such a low volubility in water
that it is inconceivablethat large quantities
could have migrated as true solutions. Most
subsurfacewaters have near normal oil-water
interracialtension, so that migration in
solubilizedform as suggested by Bakerl is
improbable. Conventionalreservoir mechanics
require that oil occupy more than 15 percent of
the pore volume in order to exist as a continuOUS, mobile component.2 NO doubt migration in
the continuousphase has occurred frequently,
especially secondarilywhen previously formed
oil accumulationshave been shifted by tilting
of the reservoir rocks. However, such movements should leave residual oil saturationsand
staining in the flow paths. Isolated globules
of oil larger than the pore openings will not
move, because of a lack of unbalanced forces
which would be required to distort the globules

FT,(7J
OF A
I)
ISPE?,SE
------...
.- _EMKLSIONOF CRUDE CIL IN WATER IN POROUS MEDIA
in opposition to the interracial tension which
tries to maintain their sphericity.
Oil is often fountisaturating lenses of
coarse sand, while adjacent beds of finer .%md
have no detectable oil content. This situation
~QQfo~~ with the capillary behavi~rcof
immiscible fluids in porous media.~) Oil will
enter only the larger pores, and then only when
t~.e~AW~~l&Tein the oil phase is higher th~
that in the water phase.- However, it is hard
to imagine how the oil got into the lenses of
coarser sand if they are completely surrounded
by fine sand containingno oil. Oil pools
often appear to be surrounded by clean saad
with no oil staining.
It has been suggested by everal authors,
especially Hobson5 md Dickey,t that the oil
might move in the form of extremely small
dispersed droplets, fine enough to pass freely
through the pores of sands. When the migrating
water re-enters a finer medium, such as a silt
or shale, the oil would be screened out of the
flowing stream by a capillary filtering
mechanism. The oil droplets can not re-enter
the fine pores without distortion, so they tend
to pile up against the interface and coalesce
to form an accumulation. Oil accumulations
~hz~~fit+.lJs
be faud at capillary barriers
formed by updip pinchouts, and in the crests
of anticline through which large amounts of
water had to pass shortly after the deposition
of the sediments.
This mechanism is logical and seems to fit
the observed facts of both geologic structure
and what is known about the flow of mixed
fluids through porous media. However, no
experiments had been performed to show that
very fine droplets of oil are free to travel
indefinitely through porous media, and that
they are screened out at capillary interfaces.
The experiments to be described suggest that
this concept may have limited application.
Droplets much smaller than the pore diameters
do appear to be able to flow freely through
sand, but they are affected by electrostatic
rather than capillary forces.
The Emulsion
The crude oil used in the experiments was
from the Pennsylvanian Burgess sand in the
Bird Creek field, Tulsa County, Okla., and had
an API gravity of 35. It was emulsified with
tap water by heating the water to 200F and
mixing with a vibrating perforated disc. No
emulsifying agent was added, and the emulsion
had a surface tension of about 60 dynes. Sea
water and connate water would not suspend as
much oil as fresh water. Tknelarger ~r~plets
rose to the surface, but after several days
very little additional creaming occurred ad

SFE 248~

the underlying emulsion was quite stable.


The stable emulsion was almost clear, but
exhibited a strong lyndalleffect, showing the
path of a beam of light. It was examined under
the microscope on a glass hemacfiometer slide
used to count blood-corpuscles. This slide is
-...1-,4
into ~quares 200 microns [0.20 mm] on a
L-UJ.GU
side, and the cover glass is 100 microns [0.10
mm] above the slide [Fig. 11. Each square thus
has a v~lum of 4,QQQJO00 cu microns [.004 cu
mm] . The size of the droplets ranged from 0.5
to 1.5 microns, and their average abundance was
about 100 per square. Assigning the maximum
dimension of 1.5 microns to all the oil droplets, an oil concentrationof 44 ppm was
computed volumetrically. This approximate concentrationwas too high since the average oil
droplet size was less than 1.5 microns. When
the concentrationsof the several emulsions was
determined by solvent extraction and weighing
of the recovered oil, they fell between 23 and
35 PPIII
by volume. Emulsions of known concentration were diluted by known amounts of water
and the light transmitted was measured with a
photometer. The concentrationsof the
effluents from the several systems was determined by measuring their light transmission.
When observed under the microscope, the
h..,-d
RrO~iEUI
movement, but
fine oil dzmplets s..uh.w
-no tendency to coalesce, and very little tendency to attach themselves to the glass. When
a water current carried a free droplet towards
a fixed droplet on a collision course, the free
droplet made a last-minute detour to avoid
hitting the fixed one. Clearly the droplets
were fine enough that electrostaticforces
caused them to be repelled by each other and by
most solid surfaces.
The droplets passed easily through filter
paper with no retention of oil. They also
passed through nucleporefilters with holes
less than l-micron diameter when suction was
was applied. The emulsions passed through
funnels filled with sand. When mud was mixed
with the sand, water went through but most of
the oil was screened out.
The Apparatus
In order to observe the behavior of the
emulsion in porous media, a tube of transparent
plastic was constructedas shown in Fig. 2. It
was 2.48 cm in diameter and 41 cm long, with an
effective volume of 185 cc. The emulsion was
brought in at the top and moved downward by
gravity. Four holes were bored through the
tube at various elevations near the bottom, aad
to these manometer tubes were attached. By
this means the pressure drops along the tube
could be determined. The tube was packed witln
coarse-grainedmaterial, except that a layer
about 1/2 cm thick of fine-grainedmaterial was

WE 2481

JOHN C. CARTMILL i d PARKE A. DICKEY

placed between manometer holes B and C. Plugs


of glass wool were placed inside the stoppers
at either end to hold the porous media in
place.

that of the continuous component. In many


respects it behaves like a solid, and this
material plugging the pores caused the great
loss in permeability.

Various porous media were used to pack the


tube, including fine-grainedparticles of
quartz, glass, chert [novaculite],and styrofoam.

Run 2:

Experiments
Run 1:

Glass Beads

The cylinder was packed mainly with glass


beads having a diameter of 200 microns. Between nanometer holes B and C a layer 1/2 cm
thick of crushed glass beads screened to 37 to
8$ microns were placed over a 1.5-cm layer of
crushed beads sized 88 to 200 microns [Fig. 3].
Distilled water was passed through for several
hours, and the average permeability of the
coarse layer was determined to be 53 darcys,
while the interval between B and C containing
the crushed beads was 9.5 darcys. After XO
. .
~.~ flow
mmutes the emu~slon wasturned m.
rate began to decrease steadily [Fig. 4]. Oil
began to collect in the pores of the coarse
material at the top of the pack and in the fine
layer. Obviously, the oil was not being
screened out by capillary forces, for the oil
droplets were less than 2 microns in diameter
while the grains in the pack were 200 microns
iQ the coarse and 37 to 88 microns in the fine.
Presumably the pore openings were of the same
order of magnitude. The oil collected at the
interfaces between the glass wool and the
coarse beads, and between the coarse beads and
the fine beads. The maximum oil saturation was
just below the interface in the fine medium.
The collection of oil caused a marked
decrease in permeability, as shown by the
increasing pressure drop between the top and
Manometer A and between Manometers B and.C.
After 4,6oo cc of emulsion had passed through,
the interval between manometer holes A md B
had retained 74 percent of the original permeability, while the interval between B and C had
retained only 20 percent of its original
permeability.
The porous media were removed from the
tube and examined under the microscope. The
removal dispersed the grains, but many of them
had clusters of oil droplets sticking to them
[Fig. 5]. Other clusters and long chains of
oil droplets floated about in the water [Fig.
61. Some droplets had coalesced to form larger
ones, but most of them were their original size
Apparently the collection of oil occurred by
agglomeration and flocculation of droplets into
a mass. Such a mass of small drops of one
fluid in another is an emulsion wherein the
volume of the discontinuous component exceeds

Quartz Sand

The tube was filled with quartz sand


ranging between 250 and 350 microns in diameter,
A layer 0.5-cm thick of the same sand, crushed
and screened to between 37 and 8$ microns, was
included between the B and C manometers. About
5,000 cc of emulsion were passed through the
system, and results were the same as with the
glass beads. Mediately after the flow was
started, a collection of oil appeared at the
interface between the coarse and the fine media
[Fig. ~]. There was also a slight collection
of oil at the top of the sand where the emulsion first entered it. The width of the oilsaturated band increased as the flow continued.
Growth occurred in both directions from the
interface, but mostly into the fine medium.
The permeability decreased steadily. The A to
B section retained 90 percent of its original
permeability, and the C to D section retained
93 percent. The B to C interface, containing
the oil collection, retained onlY 44 Percent of
its original permeability. The effluent contained 8 ppm oil, so 75 percent was retained in
the tube.
Run 3:

Emulsion with Surfactant

~@her
Tlm was made using glass beads as
in Run 1. An emulsion was prepared using
surfactant. Its concentrationwas not measured
but it contained several times as much oil as
the regularly used emulsion. Its surface tension was 34 dynes per cm. After passing 1,750
cc, the fine layer showed no oil collection and
lost only .50percent of its permeability,
although much more oil passed through it than
in the case of Run 1. The photometer showed no
rer,ovalof oil by the porous media.
Run 4:

Oil-Wet Glass Beads

The plastic cylinder was charged with


glass beads as in Run 1. The tube was filled
with petroleum ether containing Arquad, a wetting agent. The system was then evacuated,
which removed the petroleum ether and air. The
voids were then filled with distilled water,
and distilled water was run through the system
for 100 minutes. About 2,500 cc of regular
emulsion with 61 dynes surface tension were w
through. A little oil collected at the coarsefine interfaces,but much less than when the
beads were water-wet. Some oil collected
throughout the porous medimn. The permeabilit~
of all three intervals declined; the A to B
interval retained 40 percent of its original
permeability, the B to C interval I-1percent,
and the C to D interval 10 percent.

FLOW OF A DISPERSE EMULSION OF CR1 )E OIL IN WATER IN POROUS MEDIA


Virtually all the oil was retained in the
porous media, and the effluent was quite clear.
Its surface tension remained at 61 dynes, so
the water did not pick up any wetting agent
from the beads.
Mamy other runs were made using the same
and different materials, and the restits were
generally consistent. The preceding four are
considered the most significant. They are
summarized in Table 1.
T..+......V.+D+;
~*
uucLy...w...In these experiments, oil was removed
from the flowing stream at izte~f~c?s where the
grain size abruptly decreased, but the mechanism of removal was not capillary screening.
Three possibly significantphenomena were
observed:
1. The disperse oil droplets of l-micron
diameter suspended in water were able to travel
appreciable distances in water-wet porous
media.
2. They tended to collect by attachment
to the solid surfaces and to each other whenever the pore diameter of the porous medium was
abruptly reduced.

3. They collected by means of flocculation and joined to form a very concentrated


emulsio~,with little tendency to coalesce.
The reason for this behavior is not
immediately clear. It may be that oil droplets
small enough to form a stable emulsion have an
electrical double layer at the oil-water
in%erface. These electrical charges are able
to repel other droplets and solid surfaces.
When the droplets are forced against a solid
surface by a current of water, however> they
stick to it. Possibly the sharp corners and
broken surfaces of the crushed grains had sites
of opposite charges. When a droplet stuck to a
solid surface, it might cause a concentration

SPE 2481

of the electrical charge at the point of contact, leaving a deficiency on the opPosite side
~f the droplet. This deficiency might attract
another droplet, which would cause it to attach
itself there, and to it a third, and so on.
Ihuslong strings and eventually masses of
iroplets would form. As these packed into the
pores, they would form a concentratedemulsion.
Perhaps during the course of time the droplets
would coalesce.
The results of these experiments can
hardly be applied to geological situations
without many additional experiments to verify
the phenomenon and to develop explanations for
it. They tend to confirm the possibility that
oil can migrate through sands in tklefmrm of a
fine disperse oil-in-water emulsion and be
screened out at interfaces with finer material.
However, the screening does not take place
according to the rules of capillarity as these
have been developed by students of fluid
behavior in porous media. Instead, quite a
different set of laws seems to govern the
behavior of fine disperse emulsions.
REFERENCES

1.

Baker, E. G.: Distributionof Hydrocarbons in petroleum,Bull., AAFG [1962] ~,


76-84.
2. Botset, H. G.: Flow of Gas Liquid Mixtures through ConsolidatedSands, Trans.,
[1940] 136, 91-105.
Am
ud
LeverettJ M. C.:
3. Bii&ley, S. E.
Mechanismof Fluid Displacement in Ssmds,
Trans., AIME.[1941] 146, 107-116.
4. =,
P. A.: The=fect of Underground
Waters in Localizing Oil Accumulations,
Economics of the Petroleum Industry, Gulf
Publishing co ., H~~~~~fi[19651 5@l.
5. Hobson, G. D.: Some Fundamentals of
Petroleum Geology, Oxford U. Press, London
[1954J @-99 .
6. Illing, V. C.: Some Factors in Oil
Accumulation, Inst. Pet. Tech. J. [1939]

25, 201-225.

Run
Vumber

Oi i in Water
Emulsion

,-.
.-. .1.+<.,Lulll
, n L , v=
Throuqh-put
~ubi ~ cm

~jedi ~~

Perm.
petenti
!!lnrrfmt
.Lre-,.-

e-

iiO surTactant
added

One

201M?11

A cln
-* U,

Run
Four

(Iedi um

20
?lass
Beads
and
Frushed
class
tieads

Glass
tie ads

73

Quartz
Sand

oi 1

Run
Tb re.s

on

Perm.
petenti
Percent
_

kWT

Wn
F.JIJ

c to 1)

[;to L

to F

NO surf actant
added
30/mg/l
oi 1

5 ,l)i)o

$urfactant
used in
emulsion
preparation

1 ,75U

NO surf actant
added

2,550

I:edi um

G1 ass
}]ea~~

Pern:.
Oe+c.
nti
.G!..-!!..Percent

Percent
cm
,,

79

80

75

44

and
Crushed
(!uartz

Glass
Reads
and
Crushed
lass

fllass
lieads

Glass
heads
(oil
wet)

W&tz

on

41

Glass
bea~~

51

11

and
Crushed
Glass
I;eads
(uil
Vwt)

Fig. 1 - Oil in water suspension


~~~
on menacfiometer Slide.
squares are 50 microns (0.05 mm)
on a slide.

G1ass

Sliqht

Scads

(;lass
!,eads
(nil
vet )

10

!I

*GLASS

PPPPPPPPPP?

-OIL

WOOL

STAIN
PERMEABILITY

GLASS

.33 DARCY

BEADS

193 MICRON
PERMEABILITY
53 DARCY BEFORE FLOW
~;~;;;~j~~$?;~

38,5 OARCV AFTER FLOW

*OIL
. .. ..~. ,;..
;:: ~,.....................:,.::<...;
:.::: ;: .....:.:...,.,...::
.......
:::::..::::..:...,..%::...>.
::::. . .................. ...... .1

STAIN

CRUSHEO

BEADS

37-88

MICRON

5.3 DARCV BEFORE OIL COLLECTED


0.13 OARCY AFTER OIL COLLECTED

-h
DIAGRAMMATIC SKETCH OF PLASTIC CYLINDER
FOUR MANOMETERS
A, B, C, AND D.

WITH

DIAGRAM

100

INTERVAL

C TO D

90

z
0
z
A
2
z
w

80

70
[

u
z

/
h

t
INTERVAL

1=

60

-INTERVAL

50

*\
A TO B

TOP TO A

I
B TO C INTERVAL-

-1

40L
,-*-.*-##------L

20
10

GLASS BEADS AND CRUSHED

GLASS BEADS,

Fig.
3 - Diagram of pack using glass bea3.s and crushed
glass beads (Run 1). Oil collected in the pores of the
beads at the top of the column and at the interface
between the course and fine beads.

Fi&. 2 - IIiagrav
of phstic cylintier showing manometers.
The tribewas packed xith
glass beads and quartz Santiof
about 2:0micrm size. A bed of tbe sar,ematerials
crushe6 to ,bout 50 microns was F1. c.3 between
non..xeters B ens C. Oil coilected in this bed, although
the pore openings were very much larger than the size of
the drcplets.

~.

OF PACK USING

------

+
*

FLOW

u
1-

50 z

%
K
:
u

-%---

*RAT E-*s---

.25 ;.
;

-------

--

----

~:
100
TIME, MINUTES

FLOW RATE AND PERMEABILITY

CHANGE,

RUN ONE

Fig. h - F1OW rate ad permeability change (Run 1) . After starting


ev,ulsion through flow rate declined. IJ3ssof permeability occurred
wheTe a%: collected at top of pack and between moometers B and C.

Fig. 5 - Unbroken glass bead with oil


droplets sticking to it.

Fig. 7 - Oil collecting at interface


between course and crushed sand.

Fig.

6 -

Fragments of crushed glass with


oil droplets sticking to them.

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