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1 s2.0 S1004954122000313 Main PDF
1 s2.0 S1004954122000313 Main PDF
a r t i c l e i n f o a b s t r a c t
Article history: Injecting CO2 into the underground for oil displacement and shortage is an important technique for car-
Received 9 November 2021 bon capture, utilization and storage (CCUS). One of the main problems during the CO2 injection is the
Received in revised form 3 January 2022 channeling plugging. Finding an effective method for the gas channeling plugging is a critical issue in
Accepted 4 January 2022
the CO2 EOR process. In this work, an acid-resistance microgel named dispersed particle gel (DPG) was
Available online 31 January 2022
characterized and its stability was tested in the CO2 environment. The microgel size selection strategies
for the homogeneous and heterogeneous reservoirs were respectively investigated using the single core
Keywords:
flooding and three parallel core flooding experiments. Moreover, the comparison of microgel alternate
Carbon dioxide
Microgels
CO2 (MAC) injection and water alternate CO2 (WAC) injection in the dual core flooding experiments were
Enhanced oil recovery presented for the investigation of the role of microgel on the conformance control in CO2 flooding process.
Conformance control The results have shown that the microgel featured with ANH and CAN groups can keep its morphology
Porous media after aging 7 days in the CO2 environment. Where, the small microgel with unobstructed migration and
large microgel with good plugging efficiency for the high permeability zone were respectively featured
with the higher recovery factor in homogeneous and heterogeneous conditions, which indicate they
are preferred used for the oil displacement and conformance control. Compared to WAC injection,
MAC injection had a higher incremental recovery factor of 12.4%. It suggests the acid-resistance microgel
would be a good candidate for the conformance control during CO2 flooding process.
Ó 2022 The Chemical Industry and Engineering Society of China, and Chemical Industry Press Co., Ltd. All
rights reserved.
⇑ Corresponding author.
E-mail address: yiqiangli@cup.edu.cn (Y. Li).
https://doi.org/10.1016/j.cjche.2022.01.011
1004-9541/Ó 2022 The Chemical Industry and Engineering Society of China, and Chemical Industry Press Co., Ltd. All rights reserved.
Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334 325
found CO2 channeling reduce the sweep efficiency in the immisci- [33,34]. To expand this idea, microsphere with smaller sizes are
ble flooding using MRI technique. Ren et al. (2015) [17] believed proposed to implement conformance control in the low permeabil-
the gas channeling leads the miscibility instability and near- ity reservoir.
miscible flooding is preferred for the CO2-EOR. How to control Acid-resistance and the particle size selection are two key
the gas channeling is a critical issue for the successful CO2-EOR issues for conformance control by microgel in the reservoir of
projects application. multi-layered heterogeneous CO2 flooding. Conventional polymer
Water alternated gas (WAG), CO2 foam and hydrogel treatment in the gel is easy to degrade under the acidic conditions which cre-
are commonly used methods to control profile in CO2 flooding. The ated by CO2 dissolved in the formation water. But this problem has
existence of the free gas phase and various gas and water satura- been solved by the constant efforts. Abbasy et al. (2008) [35]tested
tion in the reservoir during WAG injection will cause the fluid the long-term stability and plugging efficiency of polyacrylamide
redistribution and increase the swept volume [18,19]. Christensen synthetic polymer, chloroprene rubber and nitrile rubber under
et al. [20] reviewed the WAG field experience in about 60 projects the H2S and CO2 environments and concluded all three materials
and concluded a 5 to 10% incremental oil recovery could be can bear H2S and CO2. Albidrez et al. [36] reported a crystallized
achieved with WAG injection. Ghahfarokhi et al. [21] reported superabsorbent copolymer with the sizes range from 1 to 14 mm
compared to the less-heterogeneous zone of SACROC, WAG injec- featured the ability of CO2-resistance and bacteria-resistance,
tion was more favorable to enlarge swept volume in more- which was used in the Permian Basin for the treatment of high-
heterogeneous zones. Song et al. [22] investigated the effect of permeability channeling during CO2 injections. Zhou et al. [37]
reservoir properties and operation parameters on WAG perfor- added dimethyldiallylammonium chloride as the acid resistance
mance using the numerical simulation and found WAG injection monomer and synthesized an acid-resistant preformed particle
has a higher incremental recovery factor of 17.64% as compared gel. It exhibited the good plugging performance in the supercritical
to water flooding. Shakiba et al. [23] and Yu et al. [24] respectively CO2 flooding. Since the plugging efficiency of these granular micro-
tested active carbonated water alternating gas (ACWAG) injection gels is determined by the relationship between microgel sizes and
in the cores with permeability of 10 mD and 0.1 mD (1 pore throats sizes, how to choose the microgel sizes based on pore
mD = 10 3 lm2). They found more than 30% original oil in place throat sizes in high-permeability channeling has been attracting
(OOIP) were recovered for both tight cores and low permeability lots of attentions. Yao et al. [38] found it can balance the microgel
cores using ACWAG injection. These reports indicate WAG seems plugging and migration ability when the ratio of particle size to
to be an effective technique in CO2 EOR process. However, the loss pore throat diameter is 1.35–1.55 using sand pack model. Chen
of injectivity, wax deposits and corrosion caused by the dissolved et al. [39] believed microgel had the best plugging efficiency when
CO2 in water are common issues in WAG projects, which may matching factor ranged from 1 to 1.3 via the resistance factor and
restrict the application of WAG injection. Using CO2 soluble surfac- plugging rate test. However, Dai et al. [40] optimized the matching
tants to generate CO2 foam for conformance control is also pro- factor from 0.21 to 0.29 based on the injection pressure and the
posed and investigated by a series of study. Ren et al. [25] found plugging rate by considering the in-depth migration and plugging
CO2 foam generated by adding two kinds of 2-ethyl-1-hexanol into ability of microgel. Yang et al. [41] proposed the plugging efficiency
aqueous phase will increase recovery factor from CO2 flooding of was affected by the elasticity of microgel and our previous work
24% to CO2 foam flooding of 71% and 92%. The surfactant parti- also presented the microgel had four migration and plugging pat-
tioned more to the CO2 phase leads a higher recovery factor. Zhang terns in the porous medium, which were separately corresponded
et al. [26] used two nonionic surfactants mixing to increase the sol- to different matching factors [39,42]. These works clarified the
ubility of single surfactant in CO2, which can significantly improve microgel size selection method for conformance control to a cer-
CO2 foam performance for its blockage. Norris et al. [27] reported tain extent, but there are several flowing channelings in the
the application of CO2 foam in the Salt Creek Field can successfully multi-layered heterogeneous reservoir. It is still unclear how to
decrease the gas–liquid ratio and expand swept volume during CO2 use microgel to simultaneously realize plugging in the large size
flooding process. Using foam as the conformance control agent in channeling and displacing in the porous medium in this condition.
the pilot also faced huge challenges. Unlike the foam generation The objective of this work is to investigate microgel size selec-
by co-injection of surfactant and CO2 in the laboratory, gas and sur- tion strategy for conformance control in the multilayer heteroge-
factant are usually separately injected in the pilots in the form of neous reservoir and test plugging efficiency by an acid-resistance
multi-slug to avoid too high injection pressures. The complicated microgel during the CO2 flooding process. Single core and three
operation process makes the application of CO2 foam more diffi- cores in parallel flooding experiments are performed to optimize
cult. Meanwhile, gas and surfactant are unable to meet in the the ratios of microgel sizes to pore throat sizes via the ultimate
severely heterogeneous reservoir, which may fail to generate foam oil displacement efficiency. The plugging efficiency of an acid-
in this condition [28]. resistance microgel was tested by the comparison of the injection
Hydrogel treatment has overcome the above problems in WAG pressure of water alternate supercritical CO2 (WAC) injection and
injection and CO2 foam flooding, which make it become a promis- microgel alternate supercritical CO2 (MAC) injection in the cylin-
ing, cost-efficient method for conformance control in the heteroge- drical core. The proposed size selection strategy is also verified
neous reservoirs [29,30]. Hydrogel treatment can be classified into by the oil displacement efficiency of dual core flooding experiment.
the in-situ gelation and preformed particle gel (PPG). In-situ gel This work will provide an insight for the microgel size selection for
treatment refers injecting monomer, crosslink agents and some conformance control in CO2 utilization for EOR.
additives into the reservoir to block preferential flow channels
after these components reaction and gelation [31]. Unfortunately, 2. Experimental
the chromatographic separation of the components and shear
degradation during its injection make the in-situ gels only work 2.1. Materials
near the wellbore [32]. PPG is an already crosslinked gel which is
made in the dry powder form. The range of PPG sizes are usually The brine used in this work was a simulated formation water
from several microns to several millimeters. Moreover, it can swell with the salinity of 9374 mg.L 1. The brine composition was listed
up to dozens of times in the brine. The good performance in shear in Table 1. The mineral oil dyed with Sudan red had a viscosity of
resistance and simple injection operation makes PPG has widely 45 mPa.s and a density of 0.835 gcm 3 at 30 °C. Two microgels
used in the water treatment in the high water cut oilfield were used in this work are both organic polymer gel. One was
326 Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334
Table 1
Composition of the simulated formation water
synthesized with various sizes in our previous work [42] and the were frozen at 80 °C for 6 h, tableted and sputtered with gold and
second named dispersed particle gel (DPG) was provided by Pro- then observed with a SEM measurement (Hitachi S-4800, Hitachi,
fessor Dai’s group at China University of Petroleum (East China) Japan).
[43]. CO2 with a purity of 99% were purchased from an agent in
Beijing. To highlight differences of each scheme, a hydrolyzed poly- 2.3. Microgel acid-resistance test
acrylamide polymer commercialized used in Dagang oilfield with
an average molecular weight of 20 million Da and a degree of The DPG morphology and size distribution before and after
hydrolysis of 25% was added into the microgel solution as the aging in the CO2 environment were compared to show its acid-
mobility control agent in core flooding experiments for microgel resistance ability. The CO2 was added into a sealed accumulator
sizes selection. The compound system had a viscosity of 32 mPa.s which contained DPG solution and then increased its internal pres-
which was measured using a Brookfield DV II viscometer at the sure to the reservoir pressure of 22 MPa with a booster pump. The
shear rate of 6 s 1 with the polymer concentration of 1500 mg.L 1. microgel was taken out for the morphology observation with ESEM
Synthesized resin cores with a size of 4.5 cm 4.5 cm 30 cm and and size distribution test with dynamic light scattering (DLS) appa-
cylindrical outcrop cores with a diameter of 2.5 cm and length of ratus (Malvern Instruments Ltd., UK) after aging 7 days.
30 cm were respectively used in the microgel size selection exper-
iments and CO2 channeling plugging experiments. Three synthe-
2.4. One-dimensional core flooding and parallel core flooding
sized cores with the gas permeability of 2800 mD, 780 mD and
experiments for microgel size optimization
360 mD were in parallel to mimic a heterogeneous reservoir. Since
the high permeability zone and middle permeability zone were the
One-dimensional cores flooding experiments were used to
treatment targets for conformance control, the pore sizes distribu-
investigate the displacement efficiency of compound systems with
tion of the synthesized cores with the permeability of 2800mD and
different sizes microgel in the homogeneous reservoir. The two
780mD were tested by nuclear magnetic resonance (NMR) as
sizes of microgel with the median diameter of 18.7 lm and
shown in Fig. 1. The outcrop with a permeability of 15 mD was
42.8 lm mixed with the polymer were respectively injected into
served for microgel plugging efficiency test and then paralleled
the cores with the permeability of 2800 mD after water flooding,
with another outcrop with a permeability of 5 mD as the dual core
which corresponded the ratio of microgel diameter to pore throat
model for microgel conformance control study in the CO2 flooding
diameter of 0.45 and 1.03. The polymer flooding was conducted
process with the optimized microgel size.
after water flooding as a comparison. The detailed experimental
procedure is as follow: vacuum the core and saturated with brine
for the porosity measurement, then used oil displacing aqueous
2.2. Characteristic of microgel that used for conformance control in
phase to create the irreducible water saturation. The prepared core
CO2 flooding
samples were flooded with water until water cut reached 90%, then
separately conduct three kinds of tertiary oil recovery methods,
The synthesis method and characteristic of microgel used in the
including 0.8 PV(pore volume, PV, unit is cm3) of two compound
size optimization experiments were introduced in our previous
systems of polymer microgels and 0.8 PV of polymer solution, fol-
work [42]. Herein, the characteristic of an acid-resistance microgel
lowed by post water flooding until the water cut reached 98%. An
named DPG which was provide by China University of Petroleum
accumulator with stir was used for the microgel injection. The
(East China) [43] was investigated with Fourier transform infrared
pressure, oil production, and water production were continuously
spectroscopy (FTIR), element analysis and scanning electron micro-
recorded.
scope (SEM). The characteristic functional groups of DPG in the
The permeability of three cores were 2800 mD, 780 mD and 360
400–4000 cm 1 range was analyzed by a TENSORIIFTIR spectrom-
mD in the parallel core flooding experiments. The ratios of two
eter (Bruker, Germany). Vario EL Cube elemental analyzer (Ele-
microgel diameters to pore throat diameter of 780 mD core are
mentar, Germany) and Rapid OXY Cube elemental analyzer
0.97 and 2.22. Unlike the scheme in one-dimensional cores flood-
(Elementar, Germany) were respectively used for C, N, H and O
ing experiments, 0.3 PV of microgel of two sizes without mixing
quantitative detection. To obtain the DPG morphology, the samples
with polymer were separately injected after water flood to the
water cut reached 90%, then followed by 0.4 PV of polymer flood-
ing. The experiments were shut off until the water cut reached 98%
during the post water flooding. The concentration of polymer and
microgel were both 1500 mg.L 1 in both one-dimensional core
flooding and parallel core flooding experiments. The schematic dia-
gram of two experiments were shown in Fig. 2.
Fig. 2. Schematic diagram of single core and parallel core flooding experiments for microgel size optimization.
with crude oil at this condition. CO2 was continuously injecting till These elements were identical to the interpreted elements of peaks
CO2 breakthrough. Then, three rounds of WAC and MAC were pre- in FTIR spectra.
formed and compared. Each alternate round contains 0.5 PV of The microscopic morphology of DPG in the original status was
aqueous phase (water or microgel solution) and 1 PV of CO2. The observed with SEM and its size distribution was counted via the
oil production and injection pressure of WAC and MAC were image identification using the IMAGE J package. The DPGs were
recorded in the whole displacing process. The schematic diagram tightly packed together and presented regular spherical in Fig. 4
of dual core flooding experiments was shown in Fig. 3. (c). The range of the DPG sizes were from several hundred nanome-
ters to several micrometers, and its median diameter was around
1 lm. Since DPGs had shaded each other, the statistics of DPG sizes
3. Results and Discussion in Fig. 4(d) can only be used for reference.
3.1. Characteristic of microgel (DPG) used in CO2 flooding 3.2. Morphology and size distribution of DPG in the acid environment
FTIR data of microgel was acquired via the 32 scans accumula- The microgel morphologies obtained from SEM in Fig. 5(a) and
tion and presented in Fig. 4(a). The broad peak at about 3322 cm 1 (b) presented the effect of acid environment on its stability. With
indicated the presence of ANH groups in secondary or tertiary car- the aging in the CO2 environment, the uniform and dispersed par-
bon amine. The peak around 1477 cm 1 revealed the presence of ticles began coalescence because of their large surface energy. Dis-
CAN in the microgel. The peak around 1642 cm 1 is ascribed to solved metallic ion in brine will also neutralize the negative charge
the presence of C@O in bond. The peaks at 3009 cm 1 and of DPG surface, which lead to the coalescence [44]. The median
2913 cm 1 were related to the stretching vibration peak of unsat- diameter of DPG increased from the initial size of 1 lm to 4 lm
urated and saturated CAH bond. The peaks at 1609 cm 1 and after 7 days aging was found from DLS measurement in the Fig. 5
1212 cm 1 were caused by the stretching vibration of C@C bond (c). The size increasing was caused by the particle coalescence
and CAC bond in DPG sample. Fig. 4(b) showed C and O were the rather than the degradation. The aggregated DPG would contribute
most abundant element in the microgel, followed by N and H. to the plugging in gas channel, which resulted in an effective con-
Fig. 3. Schematic diagram of dual core flooding experiments for the comparison of WAC and MAC during CO2 flooding process.
328 Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334
Fig. 4. (a) FTIR spectra, (b) element analysis and (c) SEM of an acid-resistance microgel (DPG) (d) Size distribution analysis of DPG via image identification.
Fig. 5. Effect of acid environment on DPG morphology and size distribution. (a) DPG morphology before aging in the acid environment; (b) DPG morphology after aging in the
acid environment; (c) Size distributions of DPG before and after aging in the acid environment using DLS measurement.
Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334 329
Fig. 6. Oil recovery curves and incremental oil recovery factor of polymer with and without microgel.
the tertiary oil recovery stage. Oil recovery factors of three exper-
iments during water flooding stage were similar, which indicated
the good repeatability of these experiments. With the chemical
solution injection, the oil recovery factors rapidly increased and
gradually became smoothly. The incremental recovery factor of
polymer with small microgel was 30.5%, followed by the polymer
with large microgel of 27.2% and polymer of 25.5%.
The injection pressure curves of three systems in Fig. 7 may
help to explain the reason. All of them firstly increased to the peak
and then decreased to the flat because of the reduction of flow
resistance of oil and water during the water flooding stage. The dif-
ference appeared as the chemical solution injection. For the poly-
Fig. 7. Injection pressure of polymer with and without microgel during the whole mer flooding, the injection pressure sharply increased to the
flooding process. plateau due to the high viscosity of displacing phase and then
gently decreased because the oil bank was pushed out. For the
formance control. The intensive particle size distribution and reg- solution combined by polymer and microgel injection, their pres-
ular microscopic morphologies of DPGs demonstrated they were sures did not reduce after reaching the peak . The pressure of the
feathered with the good acid-resistance ability. small microgel nearly kept constant during the injection process,
which indicated the small microgel could migrate and remedy
3.3. Oil displacement efficiency of two microgel sizes in the one- the pressure dropping caused by the oil saturation reduction. How-
dimensional core flooding experiments ever, the pressure of the large microgel continuously increased
during its injection. And the pressure descent rate of large microgel
Oil displacement efficiency of polymer with and without micro- was much less than those of other two experiments during the
gel were compared to optimize microgel size selection strategy in post-water flooding. Both meant the sever blockage was occurred.
the relative homogeneous reservoir. The ratio of microgel size to Compare to the small microgel with the size ratio of 0.45, the large
pore throats sizes of 0.45 and 1.03 were respectively corresponded microgel with the size ratio of 1.03 may be unable to enter into
the unobstructed migration and slight blockage. The oil recovery small pores of the core, which failed to achieve a more incremental
curves of polymer flooding and polymer with two size microgel recovery factor.
combination flooding in Fig. 6 presented the system of polymer The effluents in Fig. 8 vividly show the oil production processes
with small size microgel featured with the best performance in of three experiments. Compare to the polymer flooding, the com-
Fig. 8. Images of three effluent during tertiary oil recovery process with different displacing solutions. (a) Polymer with large size microgel flooding; (b) Polymer with small
size microgel flooding; (c) Polymer flooding.
330 Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334
Total
25.2
17.1
55.6
10.1
30.4
water cut. The minimum water cut of microgel with size ratio of
3.2
0.45 was lower than others and featured a longer duration. It could
be concluded the migration of microgel was more important than
its blockage in the homogeneous condition. The small microgel
would be recommended for the oil displacement.
360 mD 3.4. Microgel size selection strategy through three parallel core
14.9 flooding experiments
21.1
22.4
37.3
1.1
0.2
Three different permeability cores were paralleled for core
flooding experiments to investigate microgel size selection strat-
egy in the multi-layered heterogeneous reservoir. From the Sec-
tion 3.2, it can be known the large microgel will plug the high
permeability core and the small microgel can easily migrate in it.
780 mD
The two microgels with the size ratio of 0.97 and 2.22 to the mid-
17.5
22.8
15.8
44.4
61.9
12.0
9.1
3.5
11.5
23.8
51.6
7.4
4.9
Fig. 9 shows the oil recovery of the core flooding experiment using
small microgel was firstly higher than that using large microgel.
The oil recovery incremental rate of small microgel obviously
increased with the microgel injection, which lead a higher recovery
factor at the later stage of microgel injection. With the polymer
injection, the oil recovery factor of two experiments firstly became
360 mD
similar and then the large microgel featured a higher recovery fac-
13.9
24.7
10.8
3.1
1.7
6.0
tor at the later stage of polymer flooding and the whole post-water
flooding stage.
The injection pressure of the large microgel in Fig. 10 was obvi-
ously higher than that of the small microgel during the microgel
and polymer injection stage, which was similar with the core
flooding experiments in the homogeneous condition. They both
Summary of three parallel core flooding results of small and large microgels
780 mD
21.3
37.6
58.8
10.1
fluid went along the high permeability core, which caused the low
46.2
22.3
68.5
15.0
6.2
1.1
flowing into the other cores. The inversion point appeared as the
Microgel injection
Polymer flooding
Fig. 9. Oil recovery curves and incremental oil recovery factor of two sizes microgels followed by polymer flooding.
Fig. 10. Injection pressure curves of two sizes microgels followed by polymer flooding.
rence of the fractional flow inversion was a little later in the middle were respectively conducted and compared after CO2 flooding.
permeability core, which was the reason for the largest ultimate Fig. 12 presented the oil recovery curves and incremental oil recov-
incremental recovery factor achieved by the large microgel in the ery of the each cycle injection. It showed MAC injection had the
middle permeability core. ultimate oil recovery of 76.7%, which was higher than that of
From the above results, it could be known the blockage of high WAC of 64.3%. Since the oil recovery after CO2 flooding was similar
permeability zone was the first step to realize conformance control in two experiments, the difference of the ultimate oil recovery fac-
in the heterogeneous reservoir. The large microgel was preferred tors between WAC and MAC could reflect the role of microgel in
though it may cause the serious plugging in the middle and low conformance control. The incremental oil production was both
permeability zones. In this work, the unexpected fractional flow from the first round of aqueous and CO2 alternated injection for
changing during the polymer flooding process after large microgel WAC and MAC. The higher recovery factor of MAC was also attrib-
injection may be caused by the too high flow resistance of microgel uted to the first round cycle injection because the microgel could
in the middle and low permeability zones. However, it was control- occupy the gas channel and forced the aqueous phase into the
lable via manipulating the injection amount of microgel. unwept volume. There was not much remaining oil in the areas
which aqueous and gas could reach for the followed cycle injection.
3.5. Comparison of conformance control by water alternate CO2 (WAC) The injection pressure of MAC and WAC in Fig. 13 reflected the
injection and microgel alternate CO2 (MAC) injection in dual core plugging efficiency of two methods. Due to the impact of gas com-
flooding experiments pressibility, the pressure curves increased during the aqueous
phase injection stage and decreased once CO2 was injected. Com-
The acid-resistance microgel with the median size of 3.5 lm pare to the increment of flow resistance during WAC injection
was used for the conformance control in the dual core flooding caused by the Jamin effect and three phases flowing effect, the flow
experiments. The high permeability core of 15 mD featured with resistance increased by the microgel blockage was much larger
the median pore size of 4.2 lm, which indicated it can be blocked during MAC injection. The increased pressure of MAC injection
by the selected microgel based on the above study. Water alternate was 1.5–3 times higher than that of WAC injection, which was ben-
CO2 (WAC) injection and microgel alternate CO2 (MAC) injection eficial for the swept volume enlargement. The high injection pres-
332 Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334
Fig. 11. Fractional flow curves of three cores during the whole displacement process (a) small microgel; (b) large microgel.
Fig. 12. Oil recovery curves and incremental oil recovery factor of WAC and MAC in each injection stage.
Z. Liu et al. / Chinese Journal of Chemical Engineering 43 (2022) 324–334 333
Fig. 13. Comparison of injection pressure curves of MAC and WAC with the back pressure of 22 MPa.
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