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Summary. Phase behavior, interfacial tension (1FT), viscosity, and density data were determined for the system 2% CaCl 2
brine/isopropyl alcohol (IPA)/isooctane. Liquid pairs from this system were used in a test of capillary number as a correlating
function for mobilization of residual oil in geometrically similar porous media as provided by bead packs. Close correlation of
results was obtained for a more than five-fold variation in permeability and a more than six-fold variation in 1FT. Extensive
investigation was also made of the change in trapped oil saturation given by vertical upward flooding; the ratio of gravity to
capillary forces varied more than 100-fold. A correlation between trapped oil saturation and Bond number was obtained that was in
good agreement with previous results obtained for gas entrapment. However, capillary numbers for entrapment of a given reduced
residual oil saturation (ROS) were found to be slightly higher than those for entrapment of gas.
Relative permeabilities were independent of whether the trapped phase was oil or gas and were determined mainly by the
magnitude of the trapped nonwetting-phase saturation.
Capillary numbers for mobilization of residual oil from bead packs were much higher than typical values for sandstones. For
bead packs that had been consolidated by sintering, capillary numbers for prevention of entrapment increased and those for
mobilization decreased. The net result was that differences in capillary numbers for mobilization and entrapment were greatly
reduced and results became more akin to relationships observed for consolidated sandstones.
r'
I
O~45 O~5O
,
2 I'w
0.'60
3
l'o' 0.70
~
tl Composition Path r I i I i I
e Composition Anolysis 40
20.
E
~ 10
E S
6
z
a
If)
z
W
I-
.....I
~ I
~ 08
0:: O.t.
w
;Z 0.4
b 0..2
o..llf~-o.::-':.I:J..uLW..l...W.~o.2u......J...L.1</L..U-':o.:-:3w..J.:LU..J..uo.""4
(a) 2% ISOOCTANE (b) IIp . DENSITY DIFFERENCE(g/ml)
Fig. 1-Propertles of Isopropyl alcohol/isooctane/2% CaCI 2 brine system used in displacement studies. (a) Phase envelope for
2% CaCI 2 brine, Isooctane, and isopropyl alcohol showing compositions, tie-lines, and 1FT's of equilibrated liquid pairs. (b) Rela-
tionships between fluid properties at 25C (numbers Indicated correspond to tie-line compositions shown in Fig. 1a).
, ..
Q .....
.'
,-:'
~ .
(a) LOWER END PLUG (b) COLUMN (c) ARRANGEMENT FOR PER-
MEABILITY MEASUREMENTS
Fig. 2-Apparatus for measurement of capillary number relationships and relative permea-
bllitles at reduced residual saturation In unconsolidated bead packs.
system fell very close to that for the CaCl 2 system. A slight in- (232C [73.43.6F]) that displacement experiments could be
crease in tie-line slopes observed for the NaCI/CaCl 2 system was conducted at ambient temperature without significant effect on OAW
in the direction to be expected because hydration of sodium ions fluid properties.
is greater than for calcium; this causes a small increase in the amount Contact angle measurements showed that there was strong wet-
of alcohol that partitions into the oil phase. Increase in tempera- ting of silica by the aqueous phase for all liquid pairs used in the
ture from 25 to 30C [77 to 86F] caused a small shift in tie-lines displacement experiments. For convenience in discussion, the aque-
but little change in the position of the phase envelope. It was con- ous and oleic phases will be referred to as water (W) and oil (0)
cluded that laboratory temperatures were sufficiently well controlled phases, respectively.
Residual
Bead Radius, a ilp Saturation Standard Number of
Mesh r (ltm) (mN/m) (g/cm 3 ) ~ ~ (%) Deviation Runs vitIa + 0.001412(ilpgr 2 Ia)
---
70/80 97.2 22.37 0.318 0.00132 759.47 15.15 0.61 6 1.2 x 10- 5
80/100 81.9 11.53 0.300 0.00171 585.05 15.19 0.51 6 1.25x 10- 5
45/50 163 21.05 0.315 0.0039 256.23 15.16 1.11 8 1.56x 10- 5
35/40 230 21.05 0.315 0.0078 128.69 14.06 0.55 6 2.11xl0- 5
30/35 274 21.53 0.317 0.0109 91.74 13.53 1.6 10 2.55x 10- 5
30/35 274 6.65 0.288 0.0319 31.35 10.94 1.12 7 5.51 x 10- 5
18/20 463 10.1 0.300 0.0624 16.03 7.84 0.81 5 9.82xl0- 5
18/20 463 6.5 0.289 0.093 10.75 6.42 0.71 6 1.41xl0- 4
16/18 545 6.65 0.288 0.126 7.82 4.3 1.09 8 1.88x 10- 4
18/20 463 2.5 0.274 0.23 4.35 3.12 0.88 9 3.35 x 10- 4
Experimental Procedures for Displacement Work quired for the presence of the frit compared with that for a wire
Unconsolidated Bead Packs. Bead packs were contained in a glass screen used in previous work. 12 The experimental procedure for
chromatographic column with internally threaded glass ends (see tests in which relative permeabilities are reported was therefore
Fig. 2). The column had an internal diameter of2.5 cm [1 in.] and modified as follows so that the frit could be removed after the bead
length of 30 em [12 in.]. The column was fitted with threaded teflon pack was drained to irreducible saturation. The packing was first
end pieces. A glass frit of pore size 10 to 20 ~m was sealed into saturated with the beads held in place by a wire mesh. The end
the lower end with epoxy resin. A circular polytetrafluorethylene piece containing the fritted glass was then screwed into the upper
screen and polyethylene washer were inserted in the upper end. end of the column, the height of the column being such that the
The column could withstand pressure differences of up to 1.379 frit bore down on the packing. After the upper part of the column
MPa [200 psi] across the bead pack and glass frit. assembly was fully saturated through the packing, the column was
All liquids used in displacement experiments were deaerated be- inverted and drained to irreducible wetting saturation. After
fore use. The empty column was first flooded with the W phase drainage, the column was restored to its original position, and the
at high capillary number to ensure removal of all air from the frit. end piece containing the frit was removed and replaced by the origi-
The upper portion of the glass tube was wiped dry, and the column nal end piece containing the wire screen. The column was then
was weighed with the W phase in and below the frit. More W phase waterflooded at low capillary number to establish normal ROS,
was added, and a known weight of beads was slowly and carefully S~r' After permeability at saturation S~r was measured, the column
added to avoid trapping of air while the column was vibrated to was flooded at high capillary number to a reduced ROS. The falling-
aid uniform packing. Sufficient beads were added to make the pack- head technique was then used to measure permeability under con-
ing essentially fixed when the upper end cap was screwed down. ditions where the correction for the resistance of the column in the
The fIlled column was disconnected and weighed at initial and sub- absence of beads was quite minor. These measurements provided
sequent stages of displacement. relationships between relative permeability to water at S~r and re-
duced residual saturation, Sor'
Establishing Irreducible Wetting-Phase Saturation. The W phase
was displaced with the 0 phase by gravity. Fluid levels were set Entrapment. In experiments on entrapment of oil by water, the
so that the hydrostatic head at the membrane provided sufficient column was set up and drained to irreducible water saturation by
suction for drainage of all the given bead pack to irreducible wetting- the method described previously. The column was then flooded at
phase saturation. The suction was well below that needed for some selected capillary number, and the volume of oil trapped was
penetration of the glass frit. The column was allowed to drain for determined gravimetrically. Next, the column was flushed with
about 24 hours. The space below the frit remained completely filled about 8 to 10 PV of IPA and then resaturated with the W phase.
with lower phase at all times. The procedure of draining to irreducible wetting-phase saturation
was then repeated with subsequent flooding carried out at increased
Mobilization. The column was flooded with W phase at low capil- capillary number. This cyclic procedure was used to obtain a rela-
lary number to give an S~r of about 15 %. Because the W phase tionship between capillary number and reduced residual saturation
is more viscous than the 0 phase, viscous instabilities should not achieved by entrapment for a given packing.
occur during the establishment of S~r' The column was then The effect of buoyancy forces on entrapment was investigated
flooded with W phase at increasingly higher flow rates (i.e., in- by carrying out a series of floods at constant and comparatively
creased capillary numbers). All runs were carried out with a spe- low capillary number with bead size, 1FT, and density difference
cially constructed pump that was driven through mechanical linkage as variables.
by an air piston. After steady-state flow conditions had been estab-
lished, flow rate was measured at the set pressure acting on the Sintered Bead Packs. Cylinders of artificial consolidated media
air piston of the displacement pump. The pump capacity was about were made from bead packs by light sintering at about 700C
200 cm 3 . About 2 PV was passed through the column at each [l,300F]. The cylinders were 7 cm [2* in.] long and 3.8 cm [llh
selected flooding rate. After flooding at a given rate, residual satu- in.] in diameter and were encapsulated in epoxy resin of about
ration was determined by weighing. Bead size, 1FT's, and density 1.3-cm [lh-in.] thickness with metal end plates tapped for inlet and
differences in this series of experiments were such that the effect exit flow lines. It was found that the epoxy-confined core could
of buoyancy on ROS was very small. withstand pressures of at least 250 kPa [36 psi]. This method of
Relative permeabilities were measured at reduced ROS achieved confining the test specimen was chosen so that saturations could
after mobilization of trapped oil. Permeability to the flowing water be determined accurately by weighing. However, difficulties were
phase was determined by a falling-head technique for which the experienced in obtaining satisfactory gravimetric and volumetric
rate of volumetric displacement was proportional to the hydrostatic material balances for OA W systems, so only one preliminary set
head. For a given saturation, plots of volumetric displacement vs. of data is presented for this system.
logarithm oftime yielded straight-line relationships, with permea- In a second approach to studying the effects of consolidation, a
bility being related to slope. The resistance of the column was meas- packing of lightly sintered glass beads was formed between two
ured in the absence of the packing to allow correction for the rectangular glass plates separated by a distance of about six bead
resistance of the fritted glass and the inlet and outlet ports. In ob- diameters. The spacing was set by two strips of glass set at the ends
taining reproducible measurements, however, some difficulty was of the plates and temporarily glued in place. After a third side was
experienced that appeared to be related to the large correction re- closed with masking tape, the space between the plates was filled
LEGEND z
o Legend
20 ---
-- . . --
BRINE-ISO-OCTANE-IPA SYSTEM-I Nc
SOLTROL OILAIR SYSTEMI Nc = 2.82xI0") 12
=1.01 x 10")
~
a::
f Experimental Data 13
10
... -- - ------ ------ ----- - --. ---- ...J
:5 '-
o If)0
If) I
W .~
a::lf)
5 z~
- 001
w
l.!)
0L---~25-----5~0-----7L5----~IOO~--~12-5----IL50-----. z
I LJ \~r-'>{)r) U.li61J loq(N ) - 0.26637
B
INVERSE BOND NUMBER --.- u lr)rt'l'ldt liHl (r)f'ff l( ll'nt Ll.993
dpgr 2
.,.t'
.
..&
I _,,'6
sealed with epoxy resin. Finally, flow ports were drilled at each .0
'-
(f)
end of the model. Variation in time of fusion and temperature could
be used to vary the degree of consolidation as judged from the o o
decrease in the porosity of the model. The prepared micromodels
of this type had dimensions of 10 x 20 cm [4 x 8 in.] and an overall
thickness of 0.45 cm [0.18 in.]
In the displacement experiments, air was used as the nonwetting
phase and a 50/50 mixture of styrene and xylene as the wetting
phase. Use of these liquids, which happened to be on hand, gave
a close match in refractive index with the glass; the distribution Fig. 4-Comparison of the effect of Bond number on the
change in ROS: (a) experimental data for OAW systems and
of residual nonwetting-phase blobs could be observed directly and
(b) air/oil and OAW systems.
recorded by photography or videotaping.
Model PV was determined from the difference in dry and liquid-
saturated weights of the model. Displacements at low capillary num- all displacement is conducted. Apart from the tendency for OAW
ber were carried out with constant-rate syringe pumps. Constant- systems to retain somewhat higher residuals, there is close agree-
pressure injection pumps were used to obtain capillary numbers up ment in the correlations obtained for trapping of gaseous and oleic
to about 8 x 10 -4. Changes in fluid saturation within a model were nonwetting phases.
determined gravimetrically. Experiments were run with the plane The effect of Bond number on the magnitude of residual non-
of the model in both horizontal and vertical positions. wetting phase l2 was recently modeled by Wilkinson 13 by use of
a so-called invasion percolation approach. Predictions were made
Results and Discussion for the reduction in ROS, S~r-Sor' as a function of Bond number
Unconsolidated Bead Packs. when the capillary number is very low (e.g., < 10- 7 ). In the pres-
Buoyancy vs. Capillary Forces. Extensive investigation was made ent work, the effect of Bond number at fixed capillary number con-
of the effect of the ratio of gravity to capillary forces expressed ditions on the ROS was determined (see Table 1) for OAW systems.
as the Bond number on entrapment using OA W systems. For bead Comparisons of results with theory are shown in Fig. 4a and b.
packs, it is convenient to express the Bond number as Apgr2 /a, When the mean values of Sor and S~r of the OAW systems are
where Ap is the density difference. A summary of results and test used, the experimental results at a capillary number vfJ.la=
conditions is given in Table 1. These results largely reflect the ef- 1.01 x 10- 5 follow the trend predicted by theory 13 (Fig. 4a). The
fect of Bond number on residual oil, the capillary number being regression line gave a slope of - 0.78, which is in agreement with
low and constant for all displacement tests. Data for entrapment the value of 0.77 predicted by theory. 13 However, the range of
of 0 phase and standard deviations are presented in Fig. 3. Also Bond number values over which S~r-Sor values can be measured
shown are data for trapping of air by Soltrol at slightly higher with accuracy is very narrow, 0.03<NB <0.15. For N B < 10- 2 ,
capillary number (2.82XlO- 5 ) and an estimate of results (based the reduction in ROS is difficult to measure. For NB > 10- 1 , the
on a correlation 12 of the combined effect of viscous and buoyan- experimental results for trapping of air by oil deviate from the the-
cy forces on trapping of gas) that would be given by the lower capil- oretical prediction. Thus, theory is supported by experiment for
lary number (1.01 x 10 - 5 ). Standard deviations were approx- values of Bond number 10 - 2 < N B < 10 -1 even for capillary num-
imately proportional to the inverse of phase-density differences and ber conditions that are higher than lO -7 by two orders of magni-
for the oill air system were therefore only about 1,4 of those shown tude. Because of the many simplifications used in development of
for the OAW system. It is concluded that the small increase in the theory, however, it is possible that the agreement is fortuitous.
residual oil of about 1 'h % PV is significant and may be associated A further test of theory will follow once measurements of residual
with the effect of nonwetting-phase viscosity on the outcome of saturation vs. Bond number become available for consolidated media
capillary instabilities, which occur no matter how slowly the over- such as sandstones.
930 SPE Reservoir Engineering, August 1988
200 TTTnj iii ii'''1 I ' i 111111 i i Ii jilll ,i i i lill
IB.O 18.0
160 160
r .. 97 microns
(],.. 6.6 dynes/em
14.0 r .. 162 microns 14.0 +-------+------ ..... ~
".17.0 dynes/em
,
12.0 12 0 't
\
TEST I mae
TEST Z 6064
TEST 3 + + +
10.0 10 a
B.O 8.0
6.0 60
40 40
2.0
2.0
0.0 0.0
000001 0.00001 0.0001 0.001 0.01 0.1 1.0 0.000001 000001 0.0001 0001 0.1 1.0
CAPILLARY NUMBER
CAPILLARY NUMBER
(b)
(0 )
20.0 20.0
18.0 18.0
16.0 16.0
r-115 microns
14.0 14.0
u= 11.8 dynes/em r - 70 microns
(J,.. 2.8 dynes/em
12.0 .. 12.0
TEST I BIDe -'
TEST 2 ...... + TEST I 000
10.0 <5 10.0
TEST 3 ,.",,, TEST 2 .. ++
...-'=>
8.0 0 8.0
in
w
6.0 '" 6.0
4.0 4.0
2.0 2.0
0.0 0.0
0.00001 0.01 0.1 1.0 0.000001 0.00001 0.0001 0.1 1.0
CAPILLARY NUMBER CAPILLARY NUMBER
(C) (d)
Fig. 5-Relatlonshlps between residual 011 saturation and capillary number for bead packs.
Viscous vs. Capillary Forces. Mobilization and Entrapment. It is also of interest to compare
Mobilization of Residual Oil. Results obtained for four sizes of capillary numbers for prevention of entrapment with those deter-
beads at 1FT's ranging from 17.0 to 2.8 mN/m [17.0 to 2.8 mined for mobilization. Results for prevention of air entrapment
dynes/cm] were obtained for mobilization of discontinuous oil (Fig. by oil (unlike results obtained for mobilization) are believed to be
5). Excellent reproducibility was obtained for a given system, as generally reliable because close correlation of results was obtained
can be seen from the data shown in Fifi' 5b, c, and d. These data for a range of bead sizes and displacement rates. 12 Results of at-
are also available in tabular form. I Plots of reduced ROS tempts to check the previously obtained correlation for air/oil with
(Sor/S*or' where S*or is the normal waterflood residual for a given oleic/aqueous fluid pairs are presented in Fig. 7.
run) vs. capillary number, shown in Fig. 6, demonstrate that all Although capillary numbers for initial reduction in oil saturation
results could be closely correlated. agree with results for gas entrapment, it appears that generally higher
Attempts to measure capillary numbers for mobilization were capillary numbers are required for prevention of entrapment of liquid
made previously with air as the nonwetting phase. 12 However, nonwetting phase. Wardlaw and McKellar l4 report even higher
from the dependence of residual gas saturation on volume throughput capillary numbers for trapping at a given oil saturation in bead packs
and direct observation of a shock front marked by change from very where the initial water saturation was about 18 rather than 8 %. The
low to high gas saturation in the direction of displacement, it was correlation between trapped gas saturation and a linear combina-
clear that results were severely affected by gas passing into solu- tion of Bond and capillary numbers 12 apparently does not hold for
tion at the upstream end of the column. Thus, at best, it was con- trapping of oil. However, the results shown in Fig. 7 confirm that
cluded that these results corresponded to a lower limit for recovery by prevention of trapping is much easier than mobiliza-
mobilization caused by increase in capillary number. tion of either oil or air as the nonwetting phase.
The correlation between capillary number and reduced ROS ob- Mobilization at Less-Than-Normal ROS. In further investigation
tained with variation in bead size, 1FT, and viscosities provides of the differences between mobilization and entrapment, displace-
definitive experimental support for use of the capillary number as ment of continuous oil was carried out at a capillary number of
a correlating group for tertiary oil recovery. The correlation should 4.5 X 10 -4, which established a reduced residual saturation of
be of value in assessing the behavior of systems of, for example, 7.4% (Sor/S*or=O.5). This value was anticipated from previous
much lower 1FT. Deviations from the correlation will likely pro- relationships for entrapment. The capillary number was then raised
vide an indication of significant changes in displacement mecha- incrementally to determine the conditions required for additional
nism that might arise from the effects on microscopic flow behavior oil recovery. It can be seen from the results included in Fig. 7 that
of initial water saturation, viscosity and viscosity ratio, coalescence the curve for subsequent mobilization falls below, but close to, the
rater" wettability, 1FT, swelling clays, and dispersable fines. range of values observed for mobilization beginning at normal water-
~
I "I
x '- i!o
"6'!J"~
1 . 0 1 - - < > - = : - - - - - - - -_ _
0.8
t,'!f. 0.'
C 0.8
0.6
r (J' 1<h 07
+-
Q 162fLm 17.0 diem 06
o
'" '"
0
0.4
0 J!5}Lm I! 8 diem to\X J!:? 0.5 - CORRELATION FOR
X 97JLm 6.6 diem o,xx MOBILIZATION {See fiQ.5)
04
x 000 TRAPPING OF CONTiNUOUS AIRI2
(;; 70JLm 28 dIem X
0,>< 0' (:]88 TRAPPtNG OF CONTINUOUS OIL
60 x
01<
Ql(
02 VI\"l\"l TRAPPING OF CONTINUOUS Oil AT
0.2 NC : 45 x 10-'4 FOLLOWEO BY
t 01
MOBILIZATION
flood residual saturations (see Fig. 5). It appears that distributions Consolidated Beads.
associated with mobilization from reduced residual saturations given Sintered Cores. A variety of experimental difficulties were ex-
by displacement of continuous fluid are similar to those attained perienced in obtaining results for epoxy-encapsulated sintered cores.
after displacement of discontinuous fluid. The most plausible set of results obtained by this procedure is shown
Relotive Permeabilities. Relative permeabilities to the aqueous in Fig. 9. Even these are regarded as providing little more than
phase in 40/45- and 70/80-mesh bead packs at reduced ROS qualitative guidance on the effects of consolidation. However, all
achieved by mobilization are shown in Fig. 8. The results are seen results obtained with epoxy-encapsulated cylindrical cores formed
to be in fair agreement and fall within the range defined by 40 data from sintered beads indicated that consolidation caused a decrease
points obtained previously for displacement of continuous air by in capillary numbers required for mobilization (see Fig. 9). Also
oil. 12 Relative permeabilities at reduced residual saturation will be included in Fig. 9 is a general correlation for sandstones based on
determined to some extent by the manner in which residual oil is a correlation 4 with the capillary number expressed as kwAp/Lu.
distributed. The overlap of results given for saturations achieved A correlation of relative permeabilities at ROS and reduced
by mobilization compared with entrapment suggests that differences ROS,15 with 35% ROS, S~r' as a basis, was used to convert
in detailed structure and distribution caused by the manner in which kwAp/Lu values to vp./u. In general, results for cores formed from
residual nonwetting-phase saturation is achieved in bead packs are sintered beads fell between the widely separated correlations shown
minor with respect to their effect on permeability to the wetting in Fig. 9 for sandstones and bead packs. The results in sintered
phase. This is consistent with previous observations on strongly cores are in agreement with results of sintered micromodels present-
water-wet sandstones that the magnitude of oil saturation rather ed next.
than its distribution largely determines the wetting-phase permea- Sintered Micromodels. Three sets of results are shown in Fig.
bility.IS 10 for displacement of air by a xylene/styrene mixture from thin
layers of sintered beads. Initial wetting-phase saturations were about
10 to 12%. A well-defined residual air saturation of about 25%
1.0 could be established by flooding the model vertically from the bot-
tom. Once established, capillary numbers for mobilization were
>-
I- 0.9 measured with the model horizontal; they were about an order of
.J k rw d (MOBILIZATION)
aJ
<! 0.8
lJJ
X 70-80 MESH BEADS
~ 0 40-45 MESH BEADS 1.0
a: 0.7
lJJ
Cl. D.
0.6 k rw c (ENTRAPMENT)
lJJ
> x 08
I-
<t
...J
lJJ
0.5 - - FROM REF. II
(WIDE RANGE OF
X
0.7
0.6
Sor
.
SANDSTONE
CORRE LAT I ON
~ 0.35
a: BEAD SIZES)
0.4
1 ~I'~ 05
-"'~
0,3 "'''' 04
<; 0,2 03
u
-; 0,1
0.2
oX 0.1
0
50 60 70 80 90 100 10- 6
2
Concluding Remarks
Numerous laboratory studies of oil recovery processes have been
.~
conducted with packings of spheres or close-sized sands . The con- CA P llLr, R'I' NUI.lOER. ~u
~ ~
0 . 1 mm O.lmm
(a)
Fig. 11-Dlstrlbution of residual nonwettlng phase (air) in a pack of 35/40mesh slntered beads at low and high capillary numbers.
Phase behavior and physical property measurements were carried 51 Metric Conversion Factors
out by Lindley Paul and the displacement measurements by Vijaya
cp x 1.0* E-03 Pa's
Dandge, Sandra Nordman, and Mary Paneral. Funding was provid-
dynes/cm x 1.0* E+OO mN/m
ed by the U.S. DOE Contract No. DE-AS19-80BC1031O and the
in. x 2.54* E+OO cm
New Mexico Research and Development Inst., Project No.
2-70-3304.