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Effect of Composition of HPAM/Chromium(Ⅲ) Acetate Gels on Delayed

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DOI: 10.1080/01932691.2015.1041034

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 Journal of Dispersion Science and Technology

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Effect of Composition of HPAM/Chromium(III)

Acetate Gels on Delayed Gelation Time

Feifei Sun, Meiqin Lin, Zhaoxia Dong, Daoyi Zhu, Shuang Long Wang & Jie
Yang

To cite this article: Feifei Sun, Meiqin Lin, Zhaoxia Dong, Daoyi Zhu, Shuang Long
Wang & Jie Yang (2016) Effect of Composition of HPAM/Chromium(III) Acetate Gels on
Delayed Gelation Time, Journal of Dispersion Science and Technology, 37:6, 753-759, DOI:
10.1080/01932691.2015.1041034

To link to this article: http://dx.doi.org/10.1080/01932691.2015.1041034

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Aug 2015.

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 Journal of Dispersion Science and Technology, 37:753–759, 2016
Copyright # Taylor & Francis Group, LLC
ISSN: 0193-2691 print=1532-2351 online
DOI: 10.1080/01932691.2015.1041034

Effect of Composition of HPAM/Chromium(III) Acetate

Gels on Delayed Gelation Time
Feifei Sun, Meiqin Lin, Zhaoxia Dong, Daoyi Zhu, Shuang Long Wang, and
Jie Yang
Institute of Enhanced Oil Recovery, China University of Petroleum, Beijing, China

GRAPHICAL ABSTRACT
Downloaded by [Zhejiang University] at 22:06 26 February 2016

A delayed crosslinking system employed with hydrolyzed polyacrylamide (HPAM) and

chromium acetate was developed for high profile control in low-temperature reservoirs. The cross-
linking system formed strong gel at polymer concentration range of 3000–5000 mg/L, and the
gelation time was delayed to 8–30 days, which offered the crosslinking system enough time to flow
into deep water-producing zones and plug large pore paths, forcing follow-up fluids to enter
low-permeability layer and reduce disproportionate permeability. The effect of polymer hydroly-
sis degree, polymer concentration, pH, and crosslinker concentration on delaying gelation time
was evaluated using bottle testing. Meanwhile, sand-packed tube displacement experiments
revealed the plugging performance of delayed crosslinking system. According to Fourier trans-
form infrared spectroscopy (FTIR) analysis, as well as crosslinking mechanism between polymer
and chromium acetate, the delayed mechanism of crosslinked system demonstrated that due to
stronger affinity of acetate complexes as a ligand, its substitution in situ by carboxylate group
of polyacrylamide slowed down the initial rate-determining step of crosslinking reaction.
Keywords Delayed crosslink, FTIR, gel, ligand-change, polymer

INTRODUCTION an effective method to control water to flow into faulted

Water production in conventional reservoirs is a serious
issue in the development cycle of reservoirs, especially
when oilfields have developed into the middle-late period.
As the follow-up displacement water almost flows into high
permeability layer, quite a part of low permeability zones
has not been reached yet. Hydraulic fractures, natural frac-
tures, and faults are the mainly pathways that connect the
water source to wells.[1] Polymer gel plugging technology is
Received 18 March 2015; accepted 11 April 2015.
Address correspondence to Feifei Sun, Institute of Enhanced
Oil Recovery, China University of Petroleum, 18 Fuxue Road,
Changping District, Beijing, China. E-mail: sff_happy@126.com
Color versions of one or more of the figures in the article can
be found online at www.tandfonline.com/ldis.
and fractured reservoirs.[2] Further, delayed polymer
crosslinked system for high profile control has become an
key technology that ensures the polymer crosslinked sys-
tem in low viscosity to enter deep problem zones and form
strong gel under reservoir conditions.
A delayed copolymer of polyacrylamide and 2-acrylamide-
2-methylpro panesulfonic acid (AMPS) with chromium (III)
acetate crosslinker has been previously used for
high-temperature water shut-off applications,[3] while under
the reservoir temperature of 65 C, this crosslinked system
kept no gelation within a long time. Organic crosslinkers,
such as phenolic resin, urotropine, and salicylic acid, were
also introduced to react with polyacrylamide as the delayed
system, which provides a longer time than the metallic cross-
linker at elevated temperatures.[4] However, only when the

753
 754 F. SUN ET AL.
temperature is higher than 90 C, the system of polyacryla-
mide, urotropine, and salicylic acid can gelatinize. Mean-
while, restrict conditions are required for the synthesis of
polyacrylamide and phenolic resin. In addition, a delayed
gel system developed with hydrolyzed polyacrylamide poly-
mer, polyethyleneimine (PEI), and dextran sulfate (DS) has
been reported.[5] In the case of this system, controlled release
of active PEI crosslinker from the PEI:DS complex caused
further delay in gelation. DS was primarily used as a con-
trolled release agent, especially in the pharmaceutical indus-
try. But it is too expensive to be widely used in oilfield
applications. Thereby, at low and medium temperature, the
most common delayed gel system is hydrolyzed polyacryla-
mide (HPAM) and chromium acetate. Albonica et al.[6–8]
demonstrated that polyacrylamide=chromium gels can be
delayed by adding a stronger ligand than carboxyl group
on partially hydrolyzed polyacrylamide such as oxalate or
malonate. Thereby, oxalate was added to polymer=chromium
Downloaded by [Zhejiang University] at 22:06 26 February 2016
acetate system to delay the gelation time. As a result, oxalate
increased the gelation time by several days but resulted in
weak polymer gel, which limited its in situ application.
Herein, the crosslinking system was prepared by polya-
crylamide with a hydrolysis degree of 0% and chromium
acetate, which has a low initial viscosity, high stability,
and long gelation time in low-temperature reservoir. Chro-
mium (III) acetate forms a complex ion in solution, and by
a ligand-exchange chromium is able to react with the car-
boxylate groups of polymer molecules to create crosslinks
among polymer chains, which eventually results in a
network-structured gel. The difficulty in ligand-exchange
causes a controlled release of chromium leading to delayed
crosslinking reaction.
EXPERIMENTAL
Materials
Polyacrylamide (PAM) used with an average molecular
weight of 1.2  107 and a hydrolysis degree of 0% was
obtained from SNF company (Beijing, China) in the form
of white powder. Thiourea used as stabilizer was obtained
from a supplier in the form of white powder. Chromium
acetate used as crosslinker was obtained from a supplier
in the form of dark green solution. Sodium hydroxide, used
to control the pH of crosslinking solution, was obtained
from a supplier in the form of solution. An hydrous sodium
carbonate obtained from a supplier was used to control the
hydrolysis degree of polymer.
Preparation of Polyacrylamide Crosslinking System
Thiourea and polyacrylamide powder was successively
added to the aqueous solution under the rotating speed
of 400 r=min with stirring rod for 4 hours, and the prepared
homogeneous polymer solution needed to be aged for 24
hours. With polyacrylamide concentration varying from
0.3% to 0.5% (mass fraction), chromium acetate and thio-
urea were sequentially added into polymer suspension with
additional 20 minutes stirring to obtain crosslinking sol-
ution, crosslinker concentration varied from 0.036% to
0.083% (ratio of HPAM and chromium acetate changed
from 14:1 to 6:1), while thiourea was constant at a concen-
tration of 0.01%. Finally, polymer crosslinking solution
was placed under the temperature of 65 C for gelatinizing,
and the gelling states were observed periodically.
Bottle Testing
Gelling characterization of the polymer crosslinking sys-
tem was carried out using Sydansk’s code.[9] Sample with
same amount of 18 ml was placed into uniform testing glass
bottle with rubber plug sealing, and plastic film was used to
cover the sealing position (as an additional way to prevent
evaporation). The bottle containing sample was then
placed into an oven of 65 C. Samples were monitored
periodically by inverting the bottle, and according to the
observation a gel code was assigned to the sample.
Sand-Packed Tube Displacement Experiment
The installation of the sand-packed tube displacement
experiment is referred to reference.[10] The tube used in
the experiment was 50 cm long. The velocity of fluid was
always 0.40 mL=min when water-flooding and polymer
gel-flooding occurred.
Fourier Transform Infrared Spectra Analysis
Fourier transform infrared (FTIR) spectra were
obtained from the conventional pressed KBr pellet method
containing about 1.5% of dried gel using an FTIR-80 V
spectrophotometer.
RESULTS AND DISCUSSION
Effect of Polymer Hydrolysis Degree on Gelation Time
The reactivity of HPAM is dependent on the fraction of
carboxylate groups that is described as the degree of
hydrolysis. The hydrolysis degree of polyacrylamide was
controlled to corresponding 0.001%, 0.005%, and 0.01%
by sodium carbonate in this experiment. Polymer crosslink-
ing system with 5000 mg=L polyacrylamide and 500 mg=L
chromium acetate was placed under the temperature of
65 C, and its gelation time and strength were determined
by inverting the bottle periodically. Figure 1 presented that
at the same pH value, the gelation time of the system was
delayed greatly as the polymer hydrolysis degree decreased.
When the degree of hydrolysis was 0.01%, the crosslinking
solution gelatinized within only 2 days, by changing the pH
the gelation time can be delayed to 7 days. Whereas the
hydrolysis degree of crosslinking solution decreased to
 A DELAYED CROSSLINKING SYSTEM
FIG. 1. Effect of polymer hydrolysis degree on gelation time.
Downloaded by [Zhejiang University] at 22:06 26 February 2016
0.001%, the gelation time was delayed dramatically to 30
days, which provides the crosslinking system enough
time to flow into the deep layer of reservoir that needed
to be profile controlled. It is noteworthy that pH value
played an important role in controlling the gelation
time while the hydrolysis degree was constant. When the
degree of hydrolysis was increased from 0.001% to 0.01%,
more amide groups were hydrolyzed into carboxylate
because of the alkalinity in solution, as the content of
carboxylate in polymer solution was increased. More car-
boxylic groups crosslinked with the same content of chro-
mium acetate, resulting in fast reaction rate. Therefore,
the hydrolysis degree of polymer have to be adjusted to
control the release rate of carboxylic group to delay the
gelation time.
Effect of Polymer Concentration on Gelation Time
A typical gel formulation contains 7000–10,000 mg=L
polymer, 500–2000 mg=L crosslinker, and water.[11]
According to Seright,[12] a low initial viscosity gelant would
have lower extrusion pressure in the narrow aperture frac-
tures than a partially gelled higher viscosity system. This
feature was also useful in large pore paths which especially
needed to be deep profile controlled. In this study, we
employed polymer concentration of 3000–5000 mg=L, and
a constant crosslinker concentration of 500 mg=L to pre-
pare low viscous gelant. The polymer concentration had
a great influence on the delay of gelation time, as shown
in Figure 2. The crosslinking system gelatinized fast within
3 days when the polymer concentration was 5000 mg=L at
the pH value of 6 or 5. The gelation time of crosslinking
system increased as the polymer content and pH value
decreased, respectively. When the polymer content
decreased to 4000 mg=L, the gelation time was prolonged
over 20 days, even delayed to 60 days after the polymer
concentration was reduced to 3000 mg=L at a low pH value
755
FIG. 2. Effect of polymer concentration on gelation time.
of 3. Apparently, the polymer concentration contributed
more to the delay of gelation time than that of hydrolysis
degree. For the polymer concentration of 5000 mg=L, when
the pH value decreased to 4 or 3, the crosslinking system
gelled delayed within 8–10 days, consequently, flowing gels
were still obtained with a low initial viscosity of 30 mPa  s
at 65 C. The final gelation time of the crosslinking system
was suitably low for solving the disproportionate per-
meability problem.
Effect of Crosslinker Concentration on Gelation Time
Cao xu-hong et al.[13] found that for polyacrylamide-based
systems, there is a critical crosslinker concentration below
which the systems do not form continuous three-dimensional
network structure. As the concentration of crosslinker
increased, both gel strength and gelling rate increased corre-
spondingly.[14] Based on the bottle testing observation with
a targeted gelation time ranging from several days to 30 days
at 65 C, formulas with a hydrolysis degree of 0.01%,
5000 mg=L polymer, pH value of 3, and a range of varying
content of crosslinker were prepared. The curve of gelation
time as the function of crosslinker concentration with
HPAM-to-crosslinker ratio from 6:1 to 14:1 is presented in
Figure 3. The gelation time decreased slightly from 8 days
to 6 days as the crosslinker content increased from 360 to
620 mg=L, while the crosslinker content increased to
830 mg=L, the gelation time was shortened to 3 days. Thus,
as the concentration of chromium acetate increased (the ratio
of HPAM-to-crosslinker decreased), the gelation time
decreased sharply because of the formation of continuous
network structure. However, compared with the polymer
concentration, crosslinker concentration had less effect on
delaying of gelation time, although the concentration of
crosslinker may determine whether the polymer chains can
be crosslinked to form a continuous network.
 756 F. SUN ET AL.
FIG. 3. Effect of crosslinker concentration on gelation time.
Downloaded by [Zhejiang University] at 22:06 26 February 2016
Effect of Temperature on Gelation Time
The gelation time of crosslinking system can be con-
trolled by the reservoir temperature. The effect of this fac-
tor on gelation time was studied by placing the same
crosslinking formula under different temperatures of
65 C and 80 C for gelatinizing. The gelation states were
monitored periodically when the formulas with hydrolysis
degree of 0.01%, polymer of 5000 mg=L, and HPAM-to-
crosslinker ratio of 10:1 were gelling under the temperature
of 65 C and 80 C, respectively. As a result, the system
under high temperature of 80 C gelatinized within 2 days
even at different pH values (Figure 4), while under low
temperature the system crosslinked delayed to 9–10 days
at pH values of 4 or 3. The reason may be that at high tem-
perature of 80 C, carboxylate side groups of polyacryla-
mide and chromium complex dispersed faster than that at
low temperature, which resulted in shorter contact
time for the reaction between polymer and crosslinker.
FIG. 4. Effect of temperature on gelation time.
According to the study from Willhite et al,[15] the
first-order reaction between polymer and chromium com-
plex is called uptake reaction, with the rate constant
referred to k1. Lockhart et al.[16] found that k1 >>kn, where
kn refers to all of the reaction steps leading up to cross-link
formation, subsequent to the first-order determining step.
High temperature caused carboxylate side groups colliding
with chromium complex at a high rate, leading to the first
reaction rate k1 larger than that under low temperature,
following that the whole crosslinking formation reaction
rate increased, thus the resulting gelation time was
decreased greatly. For the temperature of 65 C, the gel-
ation time of testing formula at pH values of 4 or 3 was
prolonged to 9–10 days, which is long enough for delayed
system to carry out in-depth profile control, while under
high temperature, gelation time of the system has to be
further delayed by altering other determining factors.
Effect of pH Value on Gelation Time
The gelation time highly depends on pH value of the
crosslinking solution, which has been revealed during ana-
lyzing the test results of other determining factors above.
The time taken for the gelant to attain the resulting gel
strength changed with pH values. The effect of pH values
on gelation time was investigated by observing the gelation
state of crosslinking system with a hydrolysis degree of
0.001%, polymer content of 5000 mg=L, and HPAM-to-
crosslinker ratio of 10:1 under different pH values from 3
to 7. As shown in Table 1, when the pH value varied from
3 to 6, the gelling of crosslinking system was accelerated so
that the gelation time was decreased sharply from 30 days
down to 5 days, until at a high pH of 7, the crosslinking
system did not gelatinize even within 30 days. The influence
of pH value on gelation time attributed to its effect on the
charge density of the crosslinking solution. At the pH
higher than 5, a linear chromium trimer was the dominant
intermediates in crosslinking solution, meanwhile, partial
hydrolyzed polyacrylamide has a high density of negative
charge, more carboxyl groups of polymer became reactive
activated carboxylate side groups which easily bind with
linear chromium complex. While the pH value in solution
decreased, the linear chromium trimer converted into a cyc-
lic trimer structure, and hydrolysis degree of polymer
decreased because of strong acidity of solution, which led
to more nonionizing carboxyl groups existing in the
TABLE 1
The influence of pH value on gelation time
pH 3 4 5 6 7
Gelation time=day 30 27 10 5 No gelation
Sydansk code F F E F No gelation
 A DELAYED CROSSLINKING SYSTEM
crosslinking solution; as a result, the rate of crosslinking
reaction between cyclic trimer and carboxyl groups slowed,
making crosslinking system to maintain its flowing state
during the process of injection.
Plugging of Gel on Single Sand-Packed Tube
Crosslinking system, with a hydrolysis degree of 0.001%,
polymer concentration of 5000 mg=L, chromium acetate of
500 mg=L, and a pH value of 5, was injected into a single
sand-packed tube with length of 50 cm and permeability
of 1800 mm2 at a flow velocity of 0.4 mL=min; after gelling
in the sand-packed tube for 12 days at the temperature of
65 C, the follow-up water flooding was carried out on this
sand-packed tube at the same flow velocity. Throughout
the entire experiments, water flooding of 0.5 Vp was first
performed to stabilize pressure (Figure 5a), followed by
injection of polymer crosslinking solution of 1.0 Vp, then
followed by water flooding sequently (Figure 5b). As
Downloaded by [Zhejiang University] at 22:06 26 February 2016
shown in Figure 5, before the injection of crosslinking sol-
ution, the pressure of water flooding began to rise and
finally stabilized at 4.7 KPa; after crosslinking system
flooding in sand-packed tube, along with the follow-up
injecting of water, the pressure continued to increase and
eventually kept constant at 2500 KPa. The permeability
of sand-packed tube decreased from 1890 to 3.6 mm2, which
meant that the crosslinking system flowed into the deep
section of sand-packed tube and gelled to shut off the large
pore paths of the sand tube. As a result, the follow-up
water was forced to flow into the low permeability zone
that never involved in before. In this way, the residual oil
in the low permeability layer was finally extracted as a
result of disproportionate permeability reduction.
FIG. 5. The pressure of water flooding before and after gelling.
757
FIG. 6. FTIR spectra of (1) HPAM and (2) crosslinked gel.
Delayed Gelation Mechanism
The gelation time can be controlled by altering factors
such as hydrolysis degree, polymer concentration, crosslin-
ker concentration, temperature, and pH value, while the
gelation mechanism is almost the same. The reactivity of
chromium acetate depends on its structure and types of
ligands appeared in solution. Chromium (III) acetate
changes into a complex ion while kept in solution, and both
amide and carboxylic groups are hydrolyzed into carboxy-
late ions through the hydrolysis, the rate of which increases
especially when the temperature is superior to 60 C. The
carboxylate side ions of polymer reacts with the chromium
trimer by a ligand replace of acetate groups, as has been
mentioned above, the rate constant of the ligand substi-
tution reaction is referred to k1, which is the determining
step of the entire crosslinking reaction (Scheme 1), and
compared with inorganic ligands, acetate shows a more
delayed replaced reaction by carboxylate side group of
polyacrylamide due to its stronger affinity with chromium
as a ligand. After finishing the first-order ligand-exchange
reaction, the carboxylate group of a second polymer mol-
ecule continues to react with the same chromium trimer
at the follow-up reaction step. In this way, a crosslink is
created among polymer chains via chromium crosslinker.
The difficulty in the determining step leads to the delay
of the reaction to crosslinking formation. The crosslinking
reaction takes place among polymers and chromium acet-
ate building a continuous network structure which denoted
as gel. Chromium=polyacrylamide chains crosslink into
3-D network structure through chromium–oxygen coordi-
nate bonds. The FTIR spectra of polymer and crosslinked
gel were present in Figure 6. The medium C ¼ O stretching
vibration of HPAM occurred at 1661 cm1, the corre-
sponding band in polymer gel is a weak band at
1670 cm1, and as shown in Scheme 1, steric hindrance
formed from the link of carboxyl group with chromium,
 758 F. SUN ET AL.
SCH. 1. Reaction mechanism of HPAM and chromium acetate.
Downloaded by [Zhejiang University] at 22:06 26 February 2016
making the stretching vibration of C ¼ O move to a higher
frequency. Compared with the O–H deformation vibration
of HPAM at 1453 cm1 and 1413 cm1, a strong intensity
band of 1421 cm1 corresponds to O–H deformation
vibration of crosslinked gel, because several oxygen atoms
that can form hydrogen bonds simultaneously existing in
each structural unit. The strong intensity band observed
at 735 cm1 has been assigned to Cr–O stretching
vibration,[17] which demonstrates the presence of ring struc-
ture linked up with Cr–O covalent bonds.
CONCLUSION
Gel times for the runs decreased with the increase of
HPAM hydrolysis degree, HPAM concentration, chro-
mium acetate concentration, temperature, and pH values,
and among these altering factors, hydrolysis degree, poly-
mer concentration, and pH are preferred factors to delay
the gelation time. HPAM–chromium acetate system can
be controlled to delay gelation over the range of 8–30
days, even 60 days, which means that the system is pro-
vided enough flowing time into deep water-producing
zones of reservoir to shut off the large water paths.
Besides, the pressure after treatment is ten times larger
than that before injecting the crosslinking system, demon-
strating that the following fluid has entered the narrow
fracture instead of large pore paths. Compared to inor-
ganic ligands, acetate shows relative inertness to reservoir,
and stronger affinity as a ligand, so it is a preferred cross-
linker to realize delay gelation while reacting with partial
hydrolyzed polyacrylamide. As a result, with polymer gel
plugging high permeability zones, the follow-up fluids
have opportunity to enter low-permeability layer to
improve its sweep efficiency and recover more residual
oil in a heterogeneous reservoir.
FUNDING
This work is part of a research project sponsored by a
National Natural Science Foundation of China (Grant
51374219).
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