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https://doi.org/10.1007/s12633-017-9691-1

ORIGINAL PAPER

Preparation and Characterization of Nanoclay-Based (Na-MMT

and Bentonite) Polyacrylamide Hydrogels as Water Shut-Off Agent
for Enhanced Oil Recovery
Sahar Amiri1

Received: 27 March 2017 / Accepted: 15 November 2017

© Springer Science+Business Media B.V., part of Springer Nature 2018

Abstract
A novel poly(acrylamide)/ clay mineral composite was synthesized by controlled radical polymerization of acrylamide,
clay minerals using potassium persulfate (KPS) and N, N -methylenebisacrylamide (MBA) as redox initiator and cobalt
acetylacetonate (Co(acac)2 ) as a catalyst in an aqueous solution. Synthesized nanocomposite copolymer was characterized
by FTIR, XRD and DSC. XRD indicated intercalation formation by an inter-planar spacing increase between the clay layers.
DSC showed an increase in the thermal stability of the mentioned hydrogels. Hydrogels with acceptable gel strengths,
gelation time and gel stability were prepared by crosslinking of aqueous solutions of synthesized nanocomposite copolymer
with Chromium (III) acetate for using in water shut-off operations in oil reservoirs. The effects of pH, salinity, Co(acac)2 ,
temperature, and clay minerals on the gelation time were investigated, and the activation energy was measured. By increasing
temperature, gelation occurred more rapidly. The addition of Co(acac)2 increased loss and storage modulus because of
reversible activation-deactivation radical polymerization and decreased the gel swelling. Polymer chains can be diffused
between the clay layers so the elastic modulus (G ) of the prepared hydrogels increased than hydrogels without nanoclays,
and the reversible interaction between clay and acrylamide chains led to increased loss modulus (G ).

Keywords Montmorillonite · Bentonite · Cobalt acetylacetonate · Loss modulus and elastic modulus · Reversible
interaction

1 Introduction can be diffused into the wall to provide a deeper barrier

against the excess water and can be removed.
Unwanted water production in oil reservoirs is one of the Polymer hydrogels were injected to near wellbore
serious problems which negatively impact the economy of for providing higher permeability zones or fractures and
hydrocarbon production and additional operations such as preferential seal, which divert water to low permeability
separation, handling and disposal increase exploration costs. un-swept hydrocarbon-rich areas and increase oil recovery
Several methods are available for water shutoff treatments [2, 3].
in the hydrocarbon wells, which are divided into mechanical Hydrogels are three-dimensional hydrophilic cross-
and chemical methods [1, 2]. Mechanical methods are linked networks of water-soluble polymers including a
expensive and time-consuming, so chemical methods are wide range of chemical compositions and bulk physical
more attractive for water shut-off applications such as cross- properties. In contact with water, hydrogels swell, absorb
linked gel polymer networks containing acrylamide. Oil a significant amount of water or biological fluids but
reservoirs have porous media and wall so polymer hydrogels do not dissolve because of chemical crosslinks (tie-
points, junctions), or physical crosslinks (entanglements
or crystallites) [2–4]. Hydrogels undergo a volume phase
 Sahar Amiri
[email protected]
change when surrounding conditions such as temperature,
salinity or pH change. The main drawback of these systems
1 Department of Polymer Engineering, Science and Research is a low mechanical strength during the pump injection
Branch, Islamic Azad University, Tehran, Iran or increasing temperature and entrance into the formation
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pores. Temperature, salinity or pH led to the breaking used as a crosslinker agent on the formation of hydrogels.
of polymer chains and a considerable decrease in their Viscoelastic properties of PAM/Cr(III) hydrogels were
molecular weight. For overcoming this problem and form determined through MCR300 Rheometer. Since the tem-
a gelant solution of hydrogels with appropriate mechanical perature of most Southern oil reservoirs is around 90 ◦ C, it
properties, some additives can be used such as cross-linker was taken as a base temperature in our tests.
agents or clays [2–4].
The most common polymers which are used for the
gel treatment of oil reservoirs are polyacrylamides (PAM) 2 Experimental Work
based copolymers. PAM hydrogels show good versatility
with various additives to achieve acceptable gelation time, 2.1 Materials and Methods
gel strength and gel stability. Recently, various crosslinking
agents are used in the synthesis of acrylamide copolymers Acrylamide (AAM), sodium sulfite, 1-Chloro-3-methylpan-
such as N,N/ -methylene-bis-acrylamide (MBA) [5, 6]. tene, sodium montmorillonite (Na-MMT), bentonite, potas-
Cr(III) Acetate is a good candidate as a cross-linker agent sium persulphate (KPS), chromium (III) acetate (Cr (III))
which can improve the mechanical strength of hydrogel and and N, N -methylenebisacrylamide (MBA) obtained from
prevent reduction of strength properties. The addition of Sigma-Aldrich (Co., Ltd., USA) by >98% purity. Sodium
inorganic clays improves strength and thermal properties of chloride (NaCl) salt, methanol and Co(acac)2 were procured
PAM/Cr(III) hydrogels because of increased junction sites from the Merck by >98% purity.
between AM chains and exfoliated clay layers, and elastic
modulus increased compared to pure hydrogels [5–7]. 2.2 Synthesis of the PAAM and PAAM/Clay
In these systems chain breakages lead to hydro- Nanocomposite Copolymers
gel decomposition so reversible activation-deactivation of
chains is attractive for the preparation of hydrogels with The nanocomposite copolymers were synthesized by free
desired properties. Cobalt complexes are good candidates radical polymerization and controlled radical polymeriza-
for controlled radical polymerization because of unstable tion of acrylamide (AAM) using KPS and MBA as initiator,
and reversible cobalt–carbon bond under thermal and pho- Na-MMT and bentonite as clays, sulfonated based salt
tolytic treatment and this makes cobalt complexes suitable as comonomer, and Co(acac)2 as catalyst while the chain
candidates for persistent-radical effect (PRE). The PRE- growth was controlled in an inert atmosphere of nitrogen
state is the origin of the high propensity of the radicals gas (Table 1). The sulfonated monomer was synthesized via
to undergo reversible deactivation rather than self-coupling reaction of sodium sulfite and 3-Chloro-3-methylpropene
reactions [8–10]. (Scheme 1). An AAM solution of desired concentration was
In this research, we have synthesized partially poured into a three-necked, round bottom flask in an oil bath
hydrolyzed polyacrylamide-clay copolymers in the pres- at 65 ◦ C, then sulfonated monomer aqueous solution was
ence of Co(acac)2 as a catalyst in a controlled radical added into the flask and allowed to mix until the mixture was
polymerization system which initiated via redox system homogenized (30 min). The homogeneous suspension was
of potassium persulfate and sodium metabisulfite and purged with nitrogen gas, and KPS and MBA aqueous solu-
montmorillonite (MMT) and bentonite as clay. Copolymer tion was added to the flask. After that Co(acac)2 was added
structure was characterized by X-ray diffraction (XRD), to the suspension and mixed at 500 rpm for 24 h at 65 ◦ C.
Fourier transform infrared spectroscopy (FTIR) and Dif- Later on, it was washed with methanol and water solution
ferential scanning calorimetry (DSC). Cr(III) Acetate was (75:25) several times to remove the homopolymer, and the

Table 1 Content of additive in hydrogels synthesis

PAAM PAAM/Co(acac)2 PAAM/MMT/Co(acac)2 PAAM/ Bentonite /Co(acac)2

KPS (50 ppm)    

sulfonated monomer (500 ppm)    
MBA (50 ppm)    
AM (10000 ppm)    
Co(acac)2 (50 ppm) –   
MMT (1000 ppm) – –  –
Bentonite (500 ppm) – – – 
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Scheme 1 Structure of O
sulfonated polyacrylamide in the O H H
N N
presence of MBA CH2
+ NaO CH2
+ H2C CH2
H 2N S
MBA
O O
AAM O
Sulfonated based salt

O O

n N N n m
m H H
C O CH2 CH2 C O

NH2 O S O O S O NH2

ONa ONa

resulting precipitate was collected and dried overnight at 2.4 Characterization of Nanocomposite Copolymer
60 ◦ C [8–10]. Hydrogel
For synthesis of sulfonated polyacrylamide/clay, first the
clay suspension was separately prepared in a beaker by The PAAM, and nanocomposite copolymer hydrogels were
gradual addition of different concentrations (1000 ppm) individually characterized by X-ray diffraction (XRD),
of nanoclay powder in 500 ml of double distilled water. Fourier transform infrared spectroscopy (FTIR) and Differ-
Then, and the clay was left with stirring for 72 h at ential scanning calorimetry (DSC). XRD was carried out on
500 rpm until full dispersion of the clay was obtained obtained copolymers to evaluate the degree of clay exfo-
[10, 11]. An AAM solution of desired concentration was liation and polymer intercalation between the clay layers,
poured into a three-necked, round bottom flask in an oil using a Xpert Philips diffractmeter (USA) with nickel fil-
bath at 65 ◦ C, then sulfonated monomer aqueous solution tered Cu Kγ radiation was used in this work. Data were
and dispersed clay were added to the flask and allowed collected at a rate of 2◦ θ min over the 2θ = 5–30◦ range.
to mix until the mixture was homogenized (30 min). The Fourier transform infrared spectroscopy (FTIR) spectra of
homogeneous suspension was purged with nitrogen gas, and various samples were recorded on a Bruker IFS 48 FTIR
5 ml of KPS and MBA aqueous solution was added to flask. spectrometer in the range of from 400 to 4000 cm−1 using
After that Co(acac)2 added to the suspension and mixed conventionally pressed KBr pellets. Differential scanning
at 500 rpm for 24 h at 65 ◦ C. Later on, it was washed calorimetry (DSC) measurements were performed by a Net-
with methanol and water solution (75:25) several times zsch DSC 200 apparatus from 0 ◦ C to 400 ◦ C temperature
to remove the homopolymer, and the resulting precipitate variation rates of 10 ◦ C/min−1 for the heating and cooling
was collected and dried overnight at 60 ◦ C (Scheme 2) runsn [8–10].
[10–12].
2.5 Rheological Characterization of Hydrogels
2.3 Preparation of the PAAM /Cr (III) Hydrogel
Bottle testing was the method used to investigate gelation
The synthesized nanocomposite copolymer and distilled time, gel strength, and gel deformability, also called
water were stirring for 2 h, then aged for 48 h at room rheological properties, of hydrogels. To test long-term gel
temperature to obtain a homogeneous solution. The PAAM stability, the bottle test method is fast to assess the gelation
solution had to be diluted to the required concentrations kinetics over a wide-ranging chemical formulation. To
as a main preparation step shortly before the experiment. achieve the goal, 50% of bottles with a 50-ml capacity
Similarly, Cr(III) (as the cross-linker) was added into were filled with the gelant of nanocomposite copolymer
distilled water at room temperature while a magnetic stirrer which was a mixture of cross-linker solution and copolymer
was used for 10 min to mix the diluted Cr(III) with PAAM suspension diluted in distilled water solution. The gelation
solutions to obtain a gelant solution. Thiourea (5000 ppm) process, as soon as the filled bottles filled were put into the
was finally added to all samples to stabilize against oxygen- oven, was monitored as a function of time. The process was
induced polymer degradation [7, 8]. then investigated frequently by tilting the bottles to assess
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Scheme 2 Structure of O H H
sulfonated polyacrylamide/clay O N N
CH2 + NaO CH2 + H2C CH2
in the presence of MBA
H2N S
O O
AAM O
MBA
sulfonated monomer

H H
N N
n k k n
CH2 CH2 C O
O C O O
O S O O S O NH2
NH2
ONa Hydrophilic ONa
MMT or Bentonite

H H
N N
n k k n
CH2 CH2 C O
O C O O
O S O O S O NH2
NH2
ONa OH OH HO ONa
OH
MMT or OH
OH Bentonite
OH
OH2 OH

N N
n k k n
CH2 CH2 C O
O C O O
O S O O S O NH2
NH2
ONa ONa

the flow behavior of gel under the influence of gravity. The water. The appropriate solution of partially hydrolyzed
gel strengths were expressed alphabetically in Syndansk’s polyacrylamide and cross-linkers were thoroughly mixed at
strength code from A to J, as shown in Table 2 [11–13]. room temperature using a magnetic stirrer. The elements
of both elastic and viscous characteristics are presented
2.6 Measurement of the Gelation Time for viscoelastic materials whatever. In order to evaluate the
viscoelastic properties of the synthesized polymer gels, a
Gelation time is defined as the required time to either reach a Bohlin Gemini II Rheometer (Malvern Instruments, UK)
certain viscosity or the inflection point on the viscosity-time was used to study the gels. Moreover, the synthesized
curve. The formation time for gel strength of code C has polymeric gel samples were prepared and aged for 90 h
usually been considered as the gelation time of water-shut at 85 ◦ C and then to carry out the rheological tests the
off gels. First, a stock solution of polyacrylamide which was rheological measurements were conducted by oscillatory
partially hydrolyzed in distilled water was made and then measurements. Also, to achieve a more quantitative way to
kept for aging at ambient temperature for 24 h and further present the bottle test results, the viscosity analyzes were
fresh solution of crosslinkers was also prepared in distilled carried out using a Physica Rheolab MC 1 (Anton-Paar

Table 2 Bottle test gel strength

rating Syndansk’s code and gel Code Gel description Code Gel description
description
A No detectable gel formed F High deformable non-flowing gel
B Highly flowing gel G Moderately deformable non-flowing gel
C Flowing gel H Slightly deformable non-flowing gel
D Moderately flowing gel I Rigid gel
E Barely flowing gel J Ringing rigid gel
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GmbH., Germany). In our experiment, 10 ml of each gel to the symmetrical and asymmetrical C(=O)2 stretching,
sample was taken, and the viscosity was measured in the respectively. The bands at 1660 cm−1 and 1460 cm−1 are
range of shear rates from 10 to 500 s−1 at 85 ◦ C [11–13]. attributed to stretching of the C = O group of amides
and CH2 scissoring, respectively. Peaks at 1641 cm−1, 10340
cm−1 , 918 cm−1 , 523 cm−1 , 52530 cm−1 and 475 cm−1
3 Result and Discussion are related to OH groups of Na-MMT, Si-O-Al bending
vibrations of octahedral Al, Al-Al-OH, Si-O-Si, Al–O and
The FTIR spectra of sulfonated polyacrylamide (PAAM), Mg–O bending vibrations, respectively [8–10, 14, 15].
PAAM /Na-MMT and PAAM /Bentonite nanocomposite are The peak at 3650 cm−1 is associated with the stretching
shown in Fig. 1. PAAM and synthesized nanocomposite vibrations of structural O−H groups in the chemical
copolymers were confirmed by FTIR spectroscopy. The structure of the Na-MMT. By the formation of PAAM/Na-
characteristic absorbance broad bands at 3000–3500 cm−1 MMT copolymer, the stretching band of Si-O-Si is slightly
related to N-H and O-H stretching, 2900–3050 cm−1 related shifted to 1040 cm−1 , and the peak for the stretching band
to the N-H stretching of the NH2 group and C-H bond of the OH groups is weakened. Also, the band at 780 cm−1
stretching vibrations, and peak at 1663 cm−1 related to is ascribed to the Si-O symmetrical stretching vibrations.
C=O stretching of amide I, strong peak at 1664 cm−1 and The absence of the IR absorption peak for the Na-MMT on
1550 cm−1 related to N-H bending of amide II and peak the nanocomposite sample showed the exfoliation of MMT
at 1120 cm−1 related to stretching of CN. The relative plates in PAAM polymer. This spectrum is in agreement
weak peaks at 1450 cm−1 and 1663 cm−1 are related with the XRD results [14, 15].

Fig. 1 FTIR of a PAAM, b PAAM/ Co(acac)2 , c PAAM/ Bentonite/ Co(acac)2 and PAAM/ MMT/Co(acac)2
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3.1 XRD Analysis and increases as the chain mobility is hindered. Tg of

neat linear PAAM is seen at about 180 ◦ C, but Tg of
XRD patterns of PAAM and PAAM/clay copolymers are sulfonated monomer and PAAM is seen as a single peak
shown in Fig. 2. PAM has an amorphous nature with a at 87 ◦ C which indicated the formation of sulfonated
characteristic broad diffraction peak ranging from 2θ = 5 PAAM copolymer with higher chain mobility than PAAM
to 60◦ , and the peak lies at about 27◦ . The characteristic (Fig. 3). The high amount of sulfonated PAAM copolymer
crystalline peak of Na-MMT is seen at 2θ = 4.5 and decomposition done at 227 ◦ C. In the presence of Co(acac)2 ,
8.6◦ . Sulfonated PAAM is amorphous and showed a weak reversible formation-decomposition of interaction between
peak at 2θ = 22–27. Formation of intercalated and acrylamide chains and sulfonated monomer led to shifted Tg
partially exfoliated nanocomposites of PAAM/clay with of sulfonated PAAM to lower temperature (76 ◦ C).
higher interlayer spacing was indicated by diminishing of Co(acac)2 led to formation of reversible hydrogen bond-
PAAM characteristic peak. The peak 2θ = 4.5 completely ing, crosslinking sites increased and sub-chain mobility of
disappeared after nanocomposite formation, and a peak at PAAM and increased flexibility of polymer network, so
2θ = 22–25 was originated from anhydrous Na-MMT and Tg shifted to a lower temperature. Also, reversible hydro-
seen after losing interlayer water of hydrous Na-MMT and gen bonding led to formation of new polymer chain and
indicated complete exfoliation of clay and dispersion in the semi-crystalline structures which reduced decomposition
polymer matrix. This water was absorbed by the hydrophilic of copolymer at 243 and 264 compared to absence of
AAM [8–10, 14–16]. Co(acac)2 [8–10]. By the addition of MMT and bentonite,
formation of strong polymer–clay reversible interaction for-
3.2 DSC Analysis mation shifted Tg to 56 ◦ C and 58 ◦ C, respectively, which
indicated interaction of polymer chains with clay surfaces
The glass transition temperature (Tg) of polyacrylamide probably due to insertion of the polymer chains within
and effect on nanocomposite formation was studied by the clay layers. Clay layers exfoliated between acrylamide
DSC. Tg is an indicator of the polymer segment mobility chains, junction sites increased, Td shifted to a higher

Fig. 2 XRD of a PAAM, b PAAM/Co(acac)2 , c PAAM/Bentonite/Co(acac)2 and PAAM/ MMT/Co(acac)2

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Fig. 3 DSC of sulfonated PAAM in the presence of Co(acac)2 , MMT and bentonite

temperature and enhanced the thermal stability of hydrogels to hydrogel, the viscosity increased and is greater than
[8–10, 16–18]. those of polymer solution. The addition of nano-clay
led to increase in active crosslinking points so can
reinforce the hydrogel network and increased viscosity.
4 Characterization of Rheological Properties The addition of crosslink agent and Co(acac)2 , increased
molecular mobility and formed new cross-linking sites.
4.1 Effect of Cross-Linker (Cr(III)) Exfoliation of nanoclays may result in a sharp increase in
viscosity at very low shear rates, even at moderately low
Even small amounts of Cr(III) play a prominent role in concentrations [18–20]. The important parameter is nano-
modifying the properties of hydrogels. In general, di- and clay concentration because nano-clay can act as catalyst
tri-functional cross-linkers are employed. The nature of and accelerate polymer degradation. For this reason and
the cross-linkers and the concentration of cross-linkers not controlled nano-clay activity, Co(acac)2 and cross-link were
only modify the swelling and mechanical properties of used which controlled and increased the molecular mobility
hydrogels but also influence the amount of soluble polymer and cross-linking points, respectively, and hence increased
formed during the polymerization reaction. The solubility, the reaction rate and decreased the gelation time. The
reactivity, and steric hindrance of a given cross-linker presence of the cross-linker increased the dense domain,
determines its efficiency. Controlling of swelling behavior which in turn resulted in the reduction of the gelation time
of the hydrogel in the presence of the cross-linker agent and subsequently in the increase of the elastic modulus
is an important parameter and literature results indicate [16–18].
that increasing cross-linkers concentration led to increased
swelling. By increasing cross-linkers to copolymerization, 4.3 Effect of Temperature on the Gelation Time
networks formed between cross-linker agent and copolymer
chains, the density of crosslink increased, space between The effect of temperature on gelation time of gelling
the polymer chains decreased, and swelling ratio of the solutions which were prepared with different concentrations
hydrogel increased [15–17]. of polymer and crosslinking agent at pH 8.5 and kept for
gelation at different temperatures is shown in Fig. 5. By
4.2 Effect of Clay on the Gelation Time of Hydrogel increasing temperature, the reaction rate of amide group
and methylol group was accelerated and consequently the
The viscosity of AM hydrogels as a function of time is gelation time decreased. In fact, increasing the gelation
shown in Fig. 4. In the case of PAAM hydrogels, by temperature results in a decrease in gelation time mainly
increasing the time the viscosity increased slowly without becuase at higher temperature, gels are formed faster
any significant difference versus time. By adding nano-clay because of rapid crosslinking which is depicted in Fig. 5.
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Fig. 4 Effect of clay on gelation time

As temperature was increased, the molecular mobility The gelation time can be correlated to the temperature
increased, new cross-linking sites formed, so cross-linking according to Arrhenius’s equation:
formation accelerated, reaction rate increased and the
gelation time decreased. Also, the degree of hydrolysis GT = M expEa /RT (3)
of the polymer increases at elevated temperatures which
decreased the gelation time. By the addition of bentonite where GT , Ea , R, T, and M are gelation time (min),
and MMT, nanoclay layers exfoliated between AM chains, activation energy (KJ/mol/K), universal gas constant,
crosslinking sites increased and led to faster reaction and gelation temperature (K) and frequency factor in hr,
reach to gelation state [17–19]. respectively.

Fig. 5 Effect of temperature on gelation time of hydrogels

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Fig. 6 Effect of temperature on

gelation time of hydrogels

4.4 Effect of Clay on the Viscoelastic Properties and G for the nanocomposite gels containing 2000 ppm
of Hydrogel of clay with 10,000 ppm of polymer concentration. By
adding clay to acrylamide hydrogels, effective junction
The effect of clay on the viscoelastic properties of the points are available, and strong interactions are formed
nanocomposite hydrogels, including the elastic modulus between polyacrylamide chains and the clay, so G is
(G ) and viscous modulus (G ) determined using a Bohlin increased by adding nanoparticle. In the presence of cross-
Gemini II Rheometer (Malvern Instruments, UK) are shown linker and Co(acac)2 also more interactions are formed
in Fig. 6. Comparison of the gelation behavior of the so G significantly increased. G shows viscous energy
nanocomposite hydrogels showed that at the initial state which is related to dissipating properties of nanocomposite
G is larger than G which is related to a liquid state hydrogels. Through the addition of clay, this parameter
where viscous properties dominate, and therefore most of increased, but a peak is seen. This peak is due to the
the energy is lost as viscous heat. After gel formation, a friction at the nanoclay-polymer joint that results from
cross-linked network is formed so both G and G increased sliding of the adsorbed chains along the nano-clay surfaces.
which the rate of increase of G is much higher than that By adding cross-linker and Co(acac)2 , the friction between
of G and the elastic properties of the gelling hydrogel networks increased, and the viscous energy dissipating
begin to dominate and G becomes larger than G . This properties of the nanocomposite hydrogels, G , and peak
increase is continued until a plateau value with time is height increased but the peak decreased with increasing
reached, at which point the gelation process is completed reaction time after the peak value and reached a steady state
[18–20]. Figure 6 shows the time sweep profiles of G value [17–20].
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The increase of G by adding cross-linker is due to the the energy barrier of this process decreases, and the gelation
presence of Co(acac)2 in the system which distinguished happens sooner [13, 15, 17].
itself by the high level of control. The difference of
this method with free radical polymerization is reversible
deactivation of radicals (or intermittent activation of 5 Conclusion
dormant species) which provides a similar probability of
growth for all chains and forms polymers with narrow Acrylamide-based nanocomposite hydrogel was synthe-
molecular weight distribution. Notably, the cobalt–carbon sized via free radical and controlled radical polymerization
bond formation by the dual contribution of degenerative in the presence of Co(acac)2 . Effects of Co(acac)2 , Na-
chain transfer and reversible termination is explained, in MMT and bentonite on hydrogel properties were examined
addition to the impact of additives which are able to by XRD, FTIR, and DSC. XRD revealed the formation
coordinate the metal. Viscoelastic nature of hydrogels of a hydrogel with remarkable mechanical toughness with
is remaining, and the viscous modulus (G ) plot never intercalated and exfoliated nanoclay structures. DSC results
decreased to zero. The addition of cross-linker decreases indicated that formation of reversible crosslinks between
gelation time and the gelation point appears sooner clay and acrylamide chains improved the thermal stabil-
[18, 19]. ity of hydrogels which was confirmed that it is related to
the intercalation of intercalant into MMT layers of clay via
4.5 Effect of Salinity on the Gelation Time the ion-exchange reaction and also exfoliation in PAAM
of Hydrogels matrix. Also, by rheology measurements, further confirma-
tion was corroborated. Formation of new joins caused a
The gelling solutions were prepared with 10,000 ppm reduction in the gelation time and also increased G/ and G//
of salt (NaCl) added, so that the final polymer, Na- which is due to strong and reversible interactions between
MMT, and cross-linker were 10000, 2000 and 500 ppm, polyacrylamide chains and the clay.
respectively. Solution salinity affected hydrogel gelation
rate and reaction. In Fig. 7, the impact of salinity of
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