SPE-176457-MS

Is Epoxy-Based Polymer Suitable for Water Shut-Off Application?

Farizal Hakiki, OGRINDO Research Consortium, Institut Teknologi Bandung; Damian Dion Salam, OGRINDO
Research Consortium, Institut Teknologi Bandung, Petroleum Engineering Study Program, Institut Teknologi
Bandung; Achmad Akbari, OGRINDO Research Consortium, Institut Teknologi Bandung, Chemistry Study
Program, Institut Teknologi Bandung; Nuraeni Nuraeni, and Wisnu Aditya, OGRINDO Research Consortium,
Institut Teknologi Bandung; Septoratno Siregar, OGRINDO Research Consortium, Institut Teknologi Bandung,
Petroleum Engineering Study Program, Institut Teknologi Bandung

Copyright 2015, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE/IATMI Asia Pacific Oil & Gas Conference and Exhibition held in Nusa Dua, Bali, Indonesia, 20 –22 October 2015.

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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any position of the Society of Petroleum Engineers, its officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written
consent of the Society of Petroleum Engineers is prohibited. Permission to reproduce in print is restricted to an abstract of not more than 300 words; illustrations may
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Abstract
Well known use of epoxy-based polymer is to plug a selective layer in completion process. The similar
behaviour related to its gelation as a completion fluid is a trigger to ask a question: Is epoxy-based
polymer suitable for WSO (water shut-off) application too? Therefore, this paper is aimed to study the
applicability of epoxy-based polymer to ⬙reducing excessive produced water treatment⬙ called WSO
covering synthesising and core-flood experiment. An epoxy-based polymer is synthesised in various
temperature and concentration of reagents those are epoxy and triethylenetetramine which are vary from
6.25% to 50% which diluted in acetone with volume over volume concentration. The polymer is then
characterised using Fann-VG to know the rheology and the gelation behavior with respect to the variables
above mentioned. A polymer consists of 50% (v/v) epoxy and 50% (v/v) triethylenetetramine is chosen
to be applied in core-flood apparatus operating at room temperature, 20 psia injection and 120 psia
confining pressure. Sandstone core with various porosity and permeability are tested to reduce its
poro-perm due to epoxy-based polymer injection. Variation on concentration has shown that higher
concentration gives shorter gelation period. Gelation is defined as a time required to dramatically
changing the viscosity profile. These gelation data can be modelled into a simple mathematical model with
multivariable consist of concentration and temperature. Sandstone cores undergo a reduction on its
porosity over than 54% and permeability upto 100% which means it has potential to resist or even plug
a layer with high water cut.
Keywords: Epoxy resin · Triethylenetetramine · Sandstone coreflood · Water Shut-Off · Gelation time

Introduction
Attempt to reduce excessive produced water has been done by many oil producing companies. This
attempt can be vary from mechanical through chemical method. The chemical method has been more
industrially acceptable and thus has higher application than the mechanical one. The chemical shut-off
methods are most suitable for reservoir-related problems such as: micro matrix cements, polymers, micro
2 SPE-176457-MS

particle blends, foamed systems, resin/particulate chemical blend and gels/gelant (Regina, 2010). Action
to reduce the amount of unwanted produced water can be named water shut-off (WSO) treatment or
conformance control.

Crosslinked Polymer
The success story of water shut-off treatment has been experienced by some fields. Reported by Olsen
(1986), the oil production of the Phosphoria Formation in Hot Springs County, Wyoming increased to 82
barrels per day and the water production decreased to 180 barrels per day. A Through Tubing (TT) water
shut-off successfully carried out in Etelebou Field using a rigid polymer which after placement the system
forms a barrier in both consolidated materials and sand packs, attaining permeability reduction greater
than 99%. It can be design to achieve about 5 ft of penetration into the formation (Augustine, 2004). While
in US, Ashley Valley Oil Field through well AV#2 can reduce 40% water rate and this did result in a
minimal savings on both utilities and water-treatment chemicals (Johnson, 2001). The polymer used in
Ashley Valley was chromium (III) polyacrylamide polymer.
A 12 years’ experience review has been made regarding the application of polymer by Sydansk (1998).
It is telling that quite successful Cr(III)-carboxylate/acrylamide-polymer (CC/AP) gel technology for use
in oilfield conformance-control, sweep-improvement and fluid-shutoff treatments. To create a block at a
particular depth, polymer is initially injected and then cross-linked which is widely done by inorganic
metal cations to form a solid (Azari, 1996). In fractured carbonate core, an experimental conducted by
Simjoo (2009) says that application of a polymer gel consisting of a copolymer of acrylamide-sodium
acrylate crosslinked with chromium acetate can alter fracture conductivity from 279 Darcy ft to 0.017
Darcy ft.
Moreover, the application of metallic-based polymer crosslinkers has been expanded to broaden
applications by combining the metallic-based crosslinking agent with preferred carboxylate anion, such as
acetate (Sydansk, 1990), malonate (Lockhart, 1992), propionate (Moffit, 1993), zirconium lactate (Moffit,
1996) or aluminium citrate (Stavland, 1996). The base chemical of the preferred Cr(III)-carboxylate-
complex crosslinking agent, a form of chromic – carboxylate anion, is a commodity chemical which is
readily available as a concentrated aqueous solution and is relatively inexpensive. As a result, besides
beneficial for specific task for a given reservoir condition, adding carboxylate anion will assist in reducing
the cost of the water shutoff operation. Hence, an existence of crosslinking agent is vital to link water
soluble polymer.

Organically Crosslinked Polymer (OCP)

Ability of various polymer to block the porous medium which is proven by the measurement of reduced
porosity and permeability also performed on some organically cross-linked polymer. Those efforts are
done to answer the environmental issue may come up in conjunction the use of metal cations like chrome
(III) because polyacrylamide is crosslinked using complex bond which is less strong compared to covalent
bond. There will be a possibility that the Cr(III) is produced back to surface. So, the polyacrylamide must
be crosslinked by organic crosslinking agent to obtain the occurrence of covalent bond.
Laboratory study reported by Bryant et al (1997) showed that organically crosslinked polymer (OCP)
system for water shutoff application was emerge as one of the solution to handle the increasing frequency
in high temperature formations. At that time, industry widely used polymer gel-forming compositions
(gelant) deploy a metallic-based polymer crosslinker, then, the study has proven that gelant using organic
crosslinkers, which is phenol-formaldehyde, could be applied and performed well in high temperature
conditions. Base polymer reported by Hardy (1999) the co-polymer of acrylamide and t-butyl acrylate
(PAtBA) are crosslinked by polyethylene imine (PEI). The polymer is even applied for Ekofisk Field,
located in the Norwegian Sector of the North Sea. PEI is found to be more efficient in propagating through
matrix material compared to chromium.
SPE-176457-MS 3

The research conducted by Sandvik (1997) reveals another type of organic material that crosslinked
copolymer, i.e. xanthan gum. This study results a biopolysaccharide (xanthan, scleroglucan) polymer that
has a number of advantages, which are high yield in salt water, shear stable, temperature stable and low
adsorption value. However, many organically cross-linked polymers gels which have been developed still
need improvement due to inefficacy at high temperature and salinity, carcinogenicity or non-eco-
friendliness.
Hence, Sengupta (2011) developed an eco-friendly cross-linked polymer system for water shutoff
application i.e. Hydroquinone (HQ)/Hexamethylenetetramide (HMTA) crosslinked with polyacrylamide
(PAM) and able to reduce up to 99.96% permeability. This eco-friendly cross-linked polymer system has
proven to be able to be applied in oil fields without much damage to environment by having high
mechanical strength, form gels at high temperature and retain stability for longer period. To extend the
application of OCP system, Jayakumar (2013) reported his research about the delayed crosslink polymer
gel system for water shutoff in unconventional oil and gas reservoirs. The hydrolysed polyacrylamide
(HPAM) and PEI are used as crosslinkers, plus acrylamide-2-methylpropane sulfonic acid (AMPS) as
delayed agent, to create the HPAM-PEI-AMPS polymer. Resulting gel is significantly stronger than those
prepared with metallic based crosslinkers, thus, it would be appropriate for water shutoff in unconven-
tional reservoirs.
Epoxy-Based Polymer
Instead of employing polymers above mentioned, the resin has also been used as a polymer to control
water inside wellbore since 1922 (Barnes, 1922). Earlier success story of furfuryl alcohol resins field
applications have been proven in Kern River and San Ardo Fields in 1990 and 1991 respectively
(Littlefield et al, 1992). SPE has summarised through PetroWiki that there are three type of resin which
comonly used in wellbore application: phenolics, epoxies and furan. The most common used among them
is epoxies. Epoxy has good thermal stability up to 400°F and very applicable at 80 to 130°F. It also has
a good stability in acid condition. So, the structure of epoxies do not change in low pH. This compound
has potentialy function to shut off the undesired fluid in wellbore such as water fluid, CO2 and
hydrocarbon gases. Beside the properties of thermal stability, epoxies also have good compressive
strength reach up to 20,000 psi and it is applicable used in sandstone and carbonates wellbore. This epoxy
has been applied in wellbore located in Subterranean Formation (Ng & Thurman, 1996). Following
Kabir’s summary (2001), epoxy is a product of the reaction between epichlorohydrin and bis-phenol A
and a common hardener is diethylenetriamine. Epoxy resin is normally diluted in reactive solvent for
example EGMBE (ethylene glycol mono-butyl ether).
Knowing current facts, this research aims to extend epoxy use in reservoir for fluid isolation in conjunction
to conformance control application and conduct epoxy synthesising which is crosslinked by triethylenetet-
ramine and diluted by acetone. The novelty of crosslinker usage has been initiated by Hakiki et al (2015).

Methodology

The study is conducted for 2 sessions, experimental and propose a basic model of gelation time. The
experimental is to perform ex-situ and in-situ laboratory work. Ex-situ experiment is focusing on the
rheology measurement and gelation observation. While in-situ laboratory work is to conduct the obser-
vation on the gelation of polymer in porous media under high pressure condition through coreflood
experiment. Data derived from ex-situ experiment are then used to construct the predictive model of
gelation time of polymer following the work of Hakiki (2014, 2015) and Yadav (2013).
Experiment
The material for synthesising the polymer system is consisting of epoxy as the main polymer and
triethylenetetramine as the hardener or crosslinker which both diluted in acetone. The structural formula
4 SPE-176457-MS

of each compound is presented through Figure 1 and Figure 2 while the the proposed reaction mechanism
and the polymer system is figured out at Figure 8 and Figure 9 on Appendix, respectively.

Figure 1—Structural formula of epoxy (Hakiki et al, 2015).

Figure 2—Structural formula of hardener (triethylenetetramine) (Hakiki et al, 2015).

Figure 3—Physical appearance of epoxy (transparent/glass colour) and triethylenetetramine (brown).

Synthesising is performed at various epoxy and triethylenetetramine concentration. The variation in

temperature is also conducted. Initial synthesising is being run at ambient temperature (25⫾3 °C) and 1
atm pressure. The previous research reported by Hakiki et al (2015) shows that the predicted reaction
mechanism between epoxy and triethylenetetramine is proposed there (See Figure 8). The visual
observation for the polymer gelation is handled by reversing the bottle position, so it is required to put the
polymer solution in transparent bottle. The quantitative observation is measured by Fann-VG every 6 up
to 24 hours.
The in-situ experiment is executed through coreflood apparatus. Sandstone cores are selected to
represent the porous medium. The polymer for flooding consists of 50% (v/v) epoxy and 50% (v/v)
triethylenetetramine. The polymer is being injected through core within inlet pressure at 120 psia and 20
psia of confining pressure. The porosity and permeability are measured by helium porosimetry (PORG-
200™) and nitrogen permeameter (PERG-200™) respectively. PERG-200TM assumptions are constant
viscosity and Z-factor at upstream and downstream, nitrogen viscosity is at 0.014 cP and flowrate is
determined at average pressure which equals to be (upstream pressure ⫹ downstream pressure)/2.
SPE-176457-MS 5

Mathematical Model
A desired gelation time that reflects the summation of: 1. Substance mixing period in surface, 2.
Pumping period through tubing, 3. Reaching reservoir boundary or particular penetrated area and 4.
Soaking or shut-in period; can be modeled and calculated through multivariable regression method. The
predicted time is to prevent premature gelation while the polymer being experiencing those activities (1
through 4) and also to prevent too long shut-in period. This equation typically has this form for two
compounds and considering temperature effect. The main model derivation can be reviewed from
literature provided by Hakiki (2014, 2015) and Yadav (2013).
(1)

The typical effect of hardener or curing agent or crosslinker is illustrated as follow (See Figure 4).

Figure 4 —Comparison of catalyst effect. Left: Hakiki (2015) equation for CA ⴝ 1.5 wt%, CB ⴝ HMTA & CC ⴝ 1 wt%. Right: Typical catalyst
effect provided by Hess (1980).

Results and Discussion

Physical appearance that reflects epoxy and hardener concentration can be reviewed through Figure 5 and
Figure 6. It shows the higher hardener gives darker solid because the hardener itself is brown (See Figure
3). Viseversa, the higher epoxy concentration will yield brighter solid. The rheology measurement come
up with ambient conditioned experiment yields not really distinctive gelation time for a different
concentration of either epoxy or triethylenetetramine (See Table 1).
6 SPE-176457-MS

Figure 5—Physical appearance of hardener (triethylenetetramine) concentration variation at ambient condition.

Figure 6 —Physical appearance of epoxy concentration variation at ambient condition.

Table 1—Gelation time summary in various epoxy and hardener concentration.

Hardener (% v/v) Epoxy (% v/v) t gel (hours)

50 33 71.25
50 12.5 95.5
50 5 95
25 50 98.23
25 25 146.483
25 12.5 146.483
25 6.25 –
12.5 50 94.25
12.5 25 194.23
12.5 12.5 122.53
12.5 6.25 122.67
6.25 25 194.23
6.25 12.5 122.617
5 50 105.75

The summary of rheology change over time is detail presented on Appendix (Figure 10 to Figure 13).
The notes must be considered that those figures are taken from the laboratory data measurement by
Fann-VG. The maximum dial of Fann-VG is 300. The most important is that polymer can be so viscous
or nearly solid that it is impossible for the solution being measured at this condition. All measurement is
done far below dial 300 because the hard one is in cleansing the rotor and stator of Fann-VG if the
measurement is forced to be conducted at that condition. An attempt to minimise of error reading is that
the measurement is conducted from the leanest to the thickest sample. The sight observation is taken from
its concentration of ingredient. Hence, term ⬙from the leanest to the thickest⬙ is approached by the
concentration used. Cup, rotor and stator cleaning is done in every interval of measurement. A cutter or
other metal like apparatus is used to drag and scratch the polymer film on the surface of cup, rotor and
stator. It also employs acetone to dilute the film.
Figure 10 to Figure 13 depict that getting higher concentration of epoxy or hardener (triethylenetet-
ramine) will cause more rapid viscosity change over the time. Higher concentration means much more
SPE-176457-MS 7

compound exists. Viscosity is increase with increasing polymer concentrations due to the increasing
intermolecular entanglement.
The solvent used, acetone has 133°F (56.1°C) boilling point. Hence, the diluted epoxy and triethyl-
enetetramine should be addressed for a reservoir with a temperature below it. The authors perform the
polymer conditioning at the atmospheric pressure and conditioned temperature in oven at 68⫾3°C. It
yields swelled polymers and faster gelation (See Figure 7) because the acetone is being boiled while the
gelation is yet to reach. The physical solution after kept in oven around 18 hours is bubbled swelling and
being solid in swelled volume. Therefore, they cannot be measured after 18 hours synthesising. Epoxy its
self is able to withstand high temperature condition because the boiling point is ⬎ 400°F (204.4°C) and
triethylenetetramine has 510.8°F (266°C) boiling point. This leads to a further study to select the suitable
solvent instead of acetone.

Figure 7—Epoxy and triethylenetetramine variation for overheated temperature.

8 SPE-176457-MS

Figure 8 —Reaction mechanism of epoxy with hardener (Hakiki et al, 2015).

SPE-176457-MS 9

Figure 9 —Crosslinked molecules of epoxy and hardener (Hakiki et al, 2015).

10 SPE-176457-MS

Figure 10 —Hardener (triethylenetetramine) concentration variation at 50% epoxy.

Figure 11—Hardener (triethylenetetramine) concentration variation at 25% epoxy.

SPE-176457-MS 11

Figure 12—Epoxy concentration variation at 50% hardener (triethylenetetramine).

Figure 13—Epoxy concentration variation at 25% hardener (triethylenetetramine).

12 SPE-176457-MS

Gelation time is needed to prevent some worst case mentioned above and to assist field application
procedure to apply the polymer. The typical well-workover procedure for fluid isolation is detail presented
by Fader et al (1992) which is leading the paramount of predicting the polymer setting time. At this
moment, the current data available is only at room temperature which resulting a good solid of polymer.
Thus, a predictive model is yet to be determined.
Table 2 summerises the porosity and permeability reduction after being injected by polymer. The
results show that the cores have measured porosity although the permeability measurement does not say
so. The permeameter is to measure lateral or horizontal permeability where it is determined through
upstream and downstream pressure gauge. After being injected by polymer, the both edges of core
(upstream and downstream edge) are fully plugged by gelled polymer. The gel is totally being solid.
Hence, it is not possible to allow the nitrogen gas passing through the core. While the helium porosimetry
is working on Boyle’s Law principle where the porosity is not measured by recording the gas rate. It is
measured at static condition. Since they still show observable porosity, they may also be still showing
another direction permeability. This research is, however, only performing lateral or horizontal permea-
bility measurement.

Table 2—In-situ polymer gelation summary for 50% v/v epoxy and 50% v/v triethylenetetramine.
Porosity Permeability Permeability Permeability
Core name Porosity before, % Porosity after, % blocking before (mD) after (mD) reduction

2.3 21.08 0.62 97.06 5864.9 0 100%

P6 27.61 12.61 54.33 1136.0 0 100%
P7 19.27 5.86 69.59 967.4 0 100%
S4 24.92 9.82 60.59 1278.2 0 100%
S5* 25.60 25.60 – 228.3 228.3 –

*No polymer treatment

Thin section treatment is carried out for selected cores among them (See Table 2). Those are Core 2.3,
Core S4 and Core S5 for vertical and lateral slice within 100x and 400x magnificent. Those cores are
selected because it is just to represent the studied cores where Core 2.3 is Berea sandstone while S4 and
S5 are artificial sandstone cores fabricated in authors’ laboratory. The pictures are put on Appendix (See
Table 3). The brown yellowish spots are indicating the pore which have already been filled by
epoxy-based polymer. The red-square-spot aims to indicate the maginification of selected area into 400x
magnificent. Since 100x magnificent result does not cover the whole thin section area, it is possible for
400x magnificent result to spot the area out of the captured 100x magnificent result. Therefore, there is
no red-square-spot in the 100x magnificent result.
SPE-176457-MS 13

Table 3—Thin section of selected cores.

14 SPE-176457-MS

Table 3—Continued
SPE-176457-MS 15

Conclusion
It has been proven that epoxy is able to be crosslinked by triethylenetetramine and it would be well
working below their boiling points. Getting higher concentration of epoxy or hardener (triethylenetet-
ramine) will cause more rapid viscosity change over measurement period and shorter gelation time.
Ex-situ gelation measurement through Fann-VG is not able to be presented significantly and distinguish
although they deploy diferrent concentrations. An in-situ gelation phenomena shows a success application
to block porosity and reduce permeability which the physical appearance through thin sections is shown
acting as supporting evidences. A recommendation is proposed to select another solvent which can
withstand at higher temperature and having higher boiling point than acetone’s.

Nomenclature
ai : Empirical constants where i ⫽ 0,1,2 & 3
CA : Epoxy concentration, % volume
CB : Triethylenetetramine concentration, % volume

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