SPE-191317-MS

Temperature-Switchable Polymers for Improved Oil Recovery

Roland Reichenbach-Klinke and Tobias Zimmermann, BASF Construction Solutions GmbH; Arne Stavland and
Daniel Strand, International Research Institute of Stavanger

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Norway One Day Seminar held in Bergen, Norway, 18 April 2018.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
A new copolymer based on hydrophobically modified polyacrylamide was characterized by its rheological
behavior. Viscosities were measured at various temperatures and salinities in comparison to a regular
acrylamide/sodium acrylate copolymer (HPAM). It is proven that the viscosity of these new associative
polymers increases with temperature, while the viscosity of HPAM is decreasing.
This effect was further explored in oscillatory rheology and porous media studies. Polymer solution was
injected into a Bentheimer sandstone with a permeability of around 2 Darcy at 20°C and the pressure drop
was measured along the core. From the pressure drop the resistance factor, RF, was derived, which is a
measure of the in-situ viscosity in the porous medium.
Next, the temperature was increased to 45°C. This resulted in an increase of the RF from 15 to 94. At
60°C a RF of even 152 was observed. By reducing the flow rate from 0.5 ml/min to 0.1 ml/min the RF could
be further increased to 562. Finally, the flow rate and the temperature were set to the initial values and a RF
of 21 was measured, which shows that the thermothickening behavior of the novel polymer is reversible.
Monitoring the effluent viscosity indicated that the increase of the RF / in-situ viscosity is due to polymer
being retained in the porous media. This retained polymer lowers the permeability of the rock pores and
thereby increases RF. By lowering the temperature, the properties are switched back to the original state
and the polymer is released from the rock matrix.
The thermothickening behavior of the discussed copolymers can be quite beneficial for applications like
polymer flooding or in-depth conformance control. During injection at surface temperature the viscosity of
the fluid is low and therefore it can be injected at high rates. Once the polymer solution migrates deeper
into the reservoir formation, the temperature of the fluid will rise gradually; in-situ viscosity will increase
and simultaneously the flow rate will decrease. Both effects will help to improve sweep efficiency.

Introduction
Hydrophobically modified or associative, water-soluble copolymers do not simply rely on the thickening
effect by molecular weight, but additionally on intermolecular hydrophobic interactions of the polymer
chains. In aqueous solution, the hydrophobic groups on the along the polymer backbone interact with each
other, which leads to the formation of an intermolecular polymer network based on weak and reversible non-
2 SPE-191317-MS

covalent bonds. Since the viscosity of this polymer network is significantly larger than that of independent,
individual polymer chains, associative polymers generally show superior viscosifying capabilities than non-
associating polymers when polymers of a similar molecular weight are compared.
So-called thermo-associative polymers are a special class of this type of materials. These polymers
contain certain chemical entities, e polyalkylene oxide or N-isopropylacrylamide, which increase their
hydrophobicity with temperature. They have a so-called lower critical solution temperature (LCST) above
which they are no longer water-soluble. The functional principle of such a thermo-associative polymer is
outlined in figure 1. The polymer consists of a water-soluble backbone, along which thermo-sensitive side-
chains are distributed. By increasing the temperature, the hydrophobicity of the thermo-sensitive groups is
enhanced and the interaction between these entities is strengthened, resulting in an intermolecular polymer
network. A more detailed discussion about thermo-associative polymers can be found in the review by
L'Alloret et al. (1997).

Figure 1—Structure and working mechanism of thermo-associative polymers.

While water-soluble polymers usually exhibit a decrease of viscosity with increasing temperature, an
enhancement of viscosity can be observed with thermo-associative polymers. It is evident that this socalled
thermo-thickening behaviour is of advantage for applications in enhanced oil recovery (EOR) and improved
oil recovery (IOR), as downhole temperatures in the hydrocarbon bearing formations are in general higher
than surface temperature.
However, despite the obvious benefits of thermo-associative polymers for IOR/EOR applications, like
conformance control or polymer flooding, there is surprisingly little work published in this area with this
class of polymers. Gel systems based on ethylene oxide – propylene oxide block copolymers had been
suggested for sweep improvement and water shut-off (Frampton et al. 2009). Moreover, acrylamide based
copolymers bearing thermo-associative groups were proposed as oil-displacing agent (Zhu et al. 2013).
More recently, thermo-responsive, acrylamide based copolymers were evaluated for polymer flooding
application (Leblanc et al. 2015). According to this publication, beneficial performance at high temperature
and high salinity conditions was observed with these polymers.
In the following, the performance of a thermo-associative copolymer will be evaluated in regard of
rheology and porous media behaviour. Its potential for EOR/IOR applications will be discussed based on
these findings.

Shear Rheology
The thermo-associative polymer (TAP) is a terpolymer of acrylamide, sodium acrylate and a small amount of
a thermo-sensitive co-monomer. The TAP has a molecular weight of around 19 million Da. As a reference a
standard, anionic polyacrylamide (APAM) with a similar molecular weight was used. Both polymers exhibit
the same anionic content of around 25%.
SPE-191317-MS 3

First, the properties of the two polymers were compared at 25°C and two different salinities. In 1% NaCl
brine (see figure 2) both polymers achieve the same viscosity level at the lower concentrations from 500
to 1500 ppm. Only at the highest measured polymer dosage of 2000 ppm TAP shows a higher viscosity
compared to APAM. This can be explained by the associative behavior of this copolymer. Above a certain
threshold concentration – the so-called critical association concentration – the intermolecular interactions
between the associative side-chains on the polymer backbone are dominating the rheological behavior
(McCormick et al. 1986, Sheng 2011). This then materializes in a steeper increase in viscosity of the
associative polymer if compared to the APAM without associative groups.

Figure 2—Viscosity of TAP and APAM at 25°C in 1% aqueous NaCl

solution. Measured with Anton Paar MCR-502 and double gap geometry.

Figure 3—Viscosity of TAP and APAM at 25°C in synthetic sea water.

Measured with Anton Paar MCR-502 and double gap geometry.

When moving to higher salt concentrations the critical association concentration occurs already at lower
polymer concentration, see figure 3 for the viscosity data in synthetic sea water (SSW). This is due to
4 SPE-191317-MS

the hydrophobic interactions between the associative side-chains, which become stronger in a more polar
environment. These data also exemplify the superior salt tolerance of associative polymers.

Figure 4—Viscosity of TAP and APAM at increasing temperature in 1% aqueous

NaCl solution. Measured with Brookfield LV with UL adapter at 6 rpm (= 7.34 s-1).

Figure 5—Viscosity of TAP and APAM at increasing temperature in synthetic

sea water. Measured with Brookfield LV with UL adapter at 6 rpm (= 7.34 s-1).

The rheology at elevated temperatures was investigated at two different salinities (1% NaCl and SSW)
and polymer concentrations of 1000 and 2000 ppm. Figure 4 shows the data in 1% NaCl brine. At the
lower polymer concentration of 1000 ppm both polymers exhibit similar viscosity levels over the whole
temperature range, while at the higher concentration of 2000 ppm there are pronounced differences in the
viscosity behavior. Both polymer reveal the same viscosity at 20°C. But then the APAM viscosity declines
at elevated temperature, while the viscosity of the TAP does not change much over the whole temperature
range.
SPE-191317-MS 5

When moving to the higher salinity (see figure 5), the trends are similar at 1000 ppm polymer
concentration. At the higher concentration, the TAP now reveals an increase of viscosity with temperature.
Its thermo-associative character can rationalize this behavior of the TAP. As outlined in the introduction,
the thermo-sensitive groups, incorporated into this copolymer enhance their hydrophobic strength with
increasing temperature. This then leads to the formation of an intermolecular, associative polymer network,
which in turn results in a higher viscosity. As had been shown, higher polymer concentration and higher
salinity of the solvent further facilitates intermolecular interactions materializing in improved viscosity at
elevated temperature.

Oscillatory Rheology
In general, polymers possess viscous and elastic properties, they behave as viscoelastic fluids. While
the determination of the viscous properties is straightforward and performed by shear rates scans, the
measurement of the elastic part is more demanding. Mostly, this is done by oscillatory rheology.
In the polymer flooding application, the contribution of viscoelastic properties of the polymer to the
oil recovery is currently debated controversial. Hence, quite some effort was done to characterize the
viscoelasticity of standard HPAM polymers (Heemskerk 1984). More recent work even recommended to
include the determination of the elastic contribution in the screening process of polymer selection for a
reservoir (Wilton 2013). In this paper, the viscoelastic properties of a regular HPAM and an associative
polymer were compared. It was concluded that the associative polymer showed an earlier onset of the elastic
contribution if compared to the standard HPAM.
The TAP was characterized by frequency scans within the linear viscoelastic region at 20 and 50°C. The
polymer was dissolved in a brine containing 1.5% NaCl and 0.1% CaCl2. Anton Paar MCR-502 equipped
with a double-gap geometry was used for all measurements.

Figure 6—Frequency scan of TAP at 20°C and 3000 ppm polymer concentration.

The frequency scan at 20°C is shown in figure 6. Due to sensitivity limitations of the measurement device,
a polymer concentration of 3000 ppm was the minimum dosage which enabled confident and reproducible
results. As can be realized from figure 6 the loss modulus G’’ is higher than the storage modulus G’ over the
whole freuquency range, indicating a viscous dominated flow behavior. In contrast, G’ is higher than G’’
at 50°C over a wide range of frequencies (see figure 7). Only at the higher frequencies the storage modulus
is dropping to lower values than the loss modulus.
6 SPE-191317-MS

It is also interesting to compare the two different moduli at the two temperatures individually (see
figures 8 and 9). While G’’ is identical at low frequencies for both temperatures and higher at 20°C at high
frequencies, the storage modulus behaves quite differently. G’ is larger at 50°C over a large frequency range.
Only at high frequencies G’ becomes higher at 20°C.
From these data, it is evident that the elastic properties of TAP, which are described by the storage
modulus, are more pronounced at the elevated temperature of 50°C if compared to 20°C over a wide
frequency range. Obviously, the polymer network induced by the thermo-associative behavior contributes
to a more elastic flow behavior. It is also indicated that this polymer network is at least partially destroyed
at higher frequencies resulting in a viscous dominated flow.

Figure 7—Frequency scan of TAP at 50°C and 3000 ppm polymer concentration.

Figure 8—Loss moduli of TAP at 50°C and 20°C (3000 ppm polymer concentration).
SPE-191317-MS 7

Figure 9—Storage moduli of TAP at 50°C and 20°C (3000 ppm polymer concentration).

Next, the elastic properties were quantified by the cross-over analysis of the storage and loss moduli at a
polymer concentration of 5000 ppm. From the intersection of the two moduli the crossover frequency ωx can
be determined. Further, the relaxation time τ can be calculated from the inverse of ωx (τ = 1/ωx). Changes
in the relaxation time τ indicate changes in the lifetime of the crosslinks between the individual polymer
chains. In other words, the relaxation time is a measure of the time required for the polymer molecules to
react to a change of the flow conditions.

Figure 10—Frequency scan of TAP at 20°C and 5000 ppm polymer concentration.
8 SPE-191317-MS

Figure 11—Frequency scan of TAP at 50°C and 5000 ppm polymer concentration

From the data displayed in figure 10 a crossover frequency ωx of 0.11 1/s and a respective relaxation
time of τ = 9.1 s can be derived. At 50°C ωx = 0.016 1/s and τ = 62.5 s (see figure 11). Hence, TAP
exhibits a significant higher relaxation time at 50°C if compared to 20°C, indicating more pronounced elastic
properties at the elevated temperature.
If compared to the regular APAM the storage and loss moduli are very similar at 20°C (see figures 12
and 13). G’ being only slightly higher for the TAP. However, at 50°C the picture changes. While the loss
moduli are still in the same range (see figure 14), G’ of the TAP is now significantly higher than the one of
the APAM over the whole frequency range (see figure 15 for details). Obviously, the elastic properties of
the TAP are superior to the APAM at elevated temperature.

Figure 12—Storage modulus of TAP and APAM at 3000 ppm and 20°C.
SPE-191317-MS 9

Figure 13—Loss modulus of TAP and APAM at 3000 ppm and 20°C

Figure 14—Loss modulus of TAP and APAM at 3000 ppm and 50°C
10 SPE-191317-MS

Figure 15—Storage modulus of TAP and APAM at 50°C.

Porous Media Studies

In terms of sweep efficiency and IOR potential by polymers, mobility ratio is the critical parameter. In
porous media, the flow behavior of regular APAM polymers is well known; at low to moderate flow rate the
mobility reduction is nearly stable and controlled by the relative polymer viscosity. This implies that polymer
concentration and brine salinity are the two design parameters. The use of thermo-associative polymers
introduces even more flexibility. Formation of intermolecular network will increase the mobility reduction.
The thermo-associative behavior of TAP had been further investigated in coreflood experiments at 100%
water saturation. The experimental set-up consisted of two serially mounted Bentheimer sandstone cores
with a permeability of around 2D for each core; core length = 7 cm and diameter = 3.8 cm. The polymer
concentration was 1000 ppm. The different brine compositions are shown in table 1.

Table 1—Brine compositions.

Salt, SSW g/L LSFB g/L MSFB g/L NaCl g/L

NaCl 23.500 1.400 14.359 10.00

KCl 0.746 0.111 - -
CaCl2 × 2H2O 1.911 2.270 0.730 -
MgCl2 × 6H2O 9.149 2.170 0.400 -
Na2SO4 3.408 1.070 2.240 -
NaHCO3 0.168 0.470 0.080 -
TDS, g/L 33.55 5.86 17.50 10.0
Ionic Strength, mol/L 0.636 0.123 0.294 0.171

In the first experiment, the polymer, 1000 ppm TAP in SSW was injected through the two serially mounted
Bentheimer cores. Initially, the flow rate was fixed, q = 0.5 ml/min. The first 6 pore volumes (1 pv = 1 single
core pore volume = 17.8 ml) were injected at 20°C (see green curve in figure 16 for temperature level). The
delayed pressure response in the second core corresponds to breakthrough of polymer from front core after
1.3 pore volumes. This is a value which is typically also observed for regular APAM, indicating that at low
SPE-191317-MS 11

temperature the associative polymer exhibits a flow behavior similar to APAM. The differential pressures
increased to a stable level of 38 mbar which corresponds to RF = 14.9.
Then, the temperature in the oven was increased to 45°C. A rapid pressure increase lasting for
approximately 10 pvs was observed in the front core, while the second core differential pressure was nearly
stable. At equilibrium, differential pressure in both cores were 4 times higher than that found at 20°C, even
though figure 8 reports constant viscosity from 20 to 60°C. By increasing the temperature to 60°C, the
differential pressures increased further, as seen in figure 16.

Figure 16—Differential pressure across the two serially mounted Bentheimer cores
during injection of 1000 ppm TAP in SSW at constant injection rate of 0.5 ml/min.

The flow behaviour observed in figure 16 can be explained by the thermo-associative behavior of the TAP.
At low temperature, the intermolecular associative network is still relatively weak and does not impact the
polymer propagation significantly. At elevated temperature, the intermolecular interactions become stronger
due to the thermo-associative effect and the flow behavior within the porous medium is changed. This
correlates nicely with the higher elasticity observed in the oscillatory rheology measurements discussed
previously.
After injection of 50 pvs the flow rate was lowered to 0.2 and 0.1 ml/min. Thereafter, the temperature was
reduced to 20°C and the differential pressure, relatively rapidly approached the same level as before heating
the cores. The mobility reduction vs. flow rate and temperature is shown in figure 17. This type of experiment
demonstrates that at low temperature the TAP polymer has flood properties like a regular APAM polymer.
The onset of intermolecular network observed as viscosity increase in bulk samples did indeed alter the flow
properties in the porous media. Mobility reduction at low rate increased from 15.9 at 20°C to 562 at 60°C.
Upscaled to field conditions figure 17 can be read as follows: The lower right corner represents injection of
TAP at high velocity and low temperature with mobility reduction similar to regular APAM, while in-depth
properties (represented by upper left corner) deviates strongly from the regular APAM polymer, indicating
an improved flow diversion effect deep in the reservoir with the associative polymer.
12 SPE-191317-MS

Figure 17—Mobility reduction for 1000 ppm TAP in SSW – Injection rate / Temperature sweep

In order to study the effect of salinity a second experiment was performed, which is a rerun of the previous
experiment in low salinity brine (LSFB). Initially, the polymer was injected at 20°C and flow rates of 1.0
and 0.5 ml/min. Thereafter at pv = 21, the temperature was increased to 62°C. Figure 18 shows that the
temperature step induces a significant increase in differential pressure. The flow rate was then reduced to q
= 0.2 and q = 0.1 ml/min. Finally, the temperature was lowered to 20°C.

Figure 18—Differential pressure across the two serially mounted Bentheimer cores during injection of 1000 ppm TAP in LSFB.

The LSFB pressure profiles in figure 18 are similar to figure 16; a significant temperature-induced
pressure increase when increasing the temperature from 20 to 62°C. Figure 19 shows a similar trend when
injecting 1000 ppm TAP in MSFB brine. In this experiment, the temperature was increased from 20 to 50°C
only.
SPE-191317-MS 13

Figure 19—Differential pressure across the two serially mounted Bentheimer cores during injection of 1000 ppm TAP in MSFB.

For thermo-associative polymers in porous media, the mobility reduction depends on the applied shear
rate. The shear rate γ̇ can be derived from the following equation:

Here, q is the flow rate, A is the core inlet surface area, k is the permeability, φ is the porosity and α is the
tortuosity factor, which is set equal to 2.5 in this case. Mobility reduction, RF, is simply the ratio between
the differential polymer pressure and the differential pressure during brine injection.

Figure 20—Mobility reduction for 1000 ppm TAP in Bentheimer

sandstone cores, three different brine types and variation of temperature.

Figure 20 summarizes the results from the core flood experiments. At 20°C, TAP in the three different
brine yielded approximately the same RF, in the range of 101. At elevated temperatures, RF increases and
becomes strongly shear thinning. This agrees with previous results from Reichenbach-Klinke et al. (2015
and 2016). The polymer viscosity is sensitive to brine salinity, and one method to exclude the viscosity term
14 SPE-191317-MS

in RF is to define RF* == RF/η. Here η is the polymer bulk viscosity. Figure 21 shows RF∗ for the different
flood experiments. At 20°C and flow rate of q = 0.5 ml/min (corresponding to shear rate γ̇ = 38 s-1) TAP
yielded RF* = 1.9 in SSW, 1.5 in MSFB and 1.2 in LSFB. Reichenbach-Klinke et al. (2015) reported, for
the same polymer and brine (SSW) RF* = 2.9 at flow rate of q = 1.0 ml/min, and RF* = 2.3 at q = 0.5 ml/
min. For comparison, regular APAM polymers will at same condition yield RF* close to unity.
This indicates some effect of the intermolecular interactions for the associative polymer TAP even at low
temperature, resulting in improved mobility reduction if compared to a regular APAM.

Figure 21—Viscosity adjusted mobility reduction, RF*, for 1000 ppm TAP in Bentheimer
sandstone cores, at two different temperatures and in three different brine types.

The results in figure 21 indicate that temperature has a larger impact on the thermo-associative induced
mobility reduction than brine salinity. RF*(LSFB at 62°C) is like RF*(SSW at 60°C) and higher than
RF*(MSFB at 50°C), even though the effective MSFB brine salinity is higher than LSFB.

Figure 22—Differential pressure response when switching from 50 to 20°C

during continues injection of 1000 ppm TAP in Bentheimer sandstone cores.
SPE-191317-MS 15

In all the experiments, the differential pressure declined rapidly when switching from high to low
temperature. Figure 22 shows that at pv = 0, the temperature was lowered from 50 to 20°C. After less than
1 pv, the front core differential pressure started to decline and reached an equilibrium within 4 pv. At the
flow rate of 0.1 ml/min, 1 pv is equal to 3 hours, while the effective cooling time is in the range of 1 hour.
The second core differential pressure is somewhat delayed, but less than during pressure build-up, as seen
in figure 18.

Figure 23—Effluent polymer viscosity during injection of 1000 ppm

TAP in MSFB - effect of lowering the temperature from 50 to 20°C

Figure 24—Normalized effluent polymer concentration during injection of

1000 ppm TAP in MSFB - effect of lowering the temperature from 50 to 20°C
16 SPE-191317-MS

It is likely to explain the pressure decline by weakening of the intermolecular network, inducing flow
of polymer, which was retained within the core at elevated temperature. It may also be observed from the
differential pressure profiles, as in figure 22 where the second core pressure increased at injection of 2 pv.
Analyzes of the effluent polymer samples supports this explanation. The effluent viscosity at 50°C was
stable at 4.4 mPas (the low effluent viscosity is due to mechanical degradation when flowing through the
back-pressure regulator), as indicated by the dotted line in figure 23. After reducing the temperature, the
effluent viscosity increased during the first pore volumes of produced polymer and reached a maximum
at 7.5 mPas. By assuming that the effluent polymer has the same rheological properties as the injected
polymer it is possible to quantify the released polymer. A similar effect as shown in figure 23 was observed
during the LSFB flood experiment. By integrating of the normalized polymer concentration in figure 24,
the released polymer corresponds to an amount of approximately 1 pv at 1200 ppm which is in addition
to the injected 1000 ppm.
Figure 25 shows the results from core flood experiments with low molecular weight TAP. Compared with
the results in figure 20, the thermo-thickening effect of low molecular weight TAP, in LSFB and MSFB, is
low. Mobility reduction increased from 4.5 at 20°C to approximately 6.0 at elevated temperatures. However,
if increasing the associative content in the low molecular weight TAP, we reproduced the results shown
in figure 20. From this we can conclude that both molecular weight and associative content are important
factors that contribute to the thermo-thickening behaviour.

Figure 25—Mobility reduction for 1000 ppm low molecular weight TAP in
Bentheimer sandstone cores, two different brine types and variation of temperature.

Summary and Discussion

From the rheology and porous media data discussed above, it is evident that the TAP reveals a pronounced
temperature-dependent behavior. At elevated temperature higher viscosity, elasticity, RF and polymer
retention was measured. The change of the polymer properties with temperature must relate to the different
strength of intermolecular interaction between the individual polymer strands depending on temperature. As
outlined by L'Alloret et al. (1997), by increasing the temperature the hydrophobicity of the thermosensitive
groups within the thermo-associative polymer is enhanced and the interaction between these entities is
strengthened.
In porous media flow, one could imagine a mechanism as depicted in figure 25: Initially, within the
pore body, the individual polymer strands (black coils in figure 26) are connected by the hydrophobic
SPE-191317-MS 17

interactions between the thermo-associative groups (purple in figure 26). As these polymer aggregates are
too large to move through the pore throats, the interactions between the polymer molecules need to be
broken before flow through the pore throat is enabled. If these interactions are too strong a breakage is
not happening and the polymer is retained by mechanical entrapment within the pore. This assumption is
supported by the strongly shear-thinning behavior and the reversibility of the polymer retention. Once the
temperature is decreased the intermolecular interactions become weaker, polymer flow through the pore
throat is possible and the polymer, which was retained at elevated temperature, is moving through the porous
medium. Similarly, at higher flow rate these interactions are broken, and flow is enabled.
What needs to be considered in this regard is the fact that a polymer is not a single, uniform component,
but has a wide range of molecular weights. Because the thermo-associative groups are distributed along
the polymer backbone statistically, this will lead to different numbers of thermo-associative groups per
polymer strand. Meaning that polymer coils with higher molecular weight will bear more thermoassociative
groups than others with lower molecular weight. This will then lead to a significant variation in the strength
and mode of intermolecular interactions between the polymer molecules. Hence, one can imagine that at a
specific condition some fractions of the TAP are flowing through the pore throats, while others are retained.

Figure 26—Sketch of associative polymer flow through pore throats.

Conclusions and Outlook

A thermo-associative polymer with interesting features for enhanced and improved oil recovery applications
was introduced. At low temperature, this polymer exhibits a behaviour similar to a regular APAM and a
moderate mobility reduction, which facilitates a good injectivity, is observed. When the thermo-associative
polymer moves deeper into the reservoir and the temperature increases, the intermolecular polymer network
becomes stronger, resulting in an enhancement of the mobility reduction effect. This will lead to improved
in-depth sweep efficiency and flow diversion deep in the reservoir. Moreover, it was shown that the thermo-
thickening effect is completely reversible.
One possibility to exploit these features of the TAP in enhanced oil recovery could be to make use of
the high retention at elevated temperature. E.g. Hoteit et al. (2016) showed that high retention of polymer
can induce additional oil recovery during post-polymer chase water injection. The discussed TAP could be
a very suitable polymer for such an application.

Acknowledgements
Martin Matzinger is acknowledged for performing the rheology studies.

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