Sand Control Using Organic Acid Catalysed Resin

by

Mohd Fizdrul Haqeem Bin Mohd Letfinuddin

14371

Dissertation submitted in partial fulfilment of the requirement for the

Bachelor of Engineering (Hons)

(Petroleum Engineering)

FYP II September 2014

Universiti Teknologi PETRONAS

Bandar Seri Iskandar
31750 Tronoh,
Perak Darul Ridzuan
 CERTIFICATION OF APPROVAL

Sand Control Using Organic Acid Catalysed Resin

by

Mohd Fizdrul Haqeem Bin Mohd Letfinuddin

14371

A project dissertation submitted to the Petroleum Engineering Programme

Universiti Teknologi PETRONAS

in partial fulfilment of the requirement for the

BACHELOR OF ENGINEERING (Hons)

(PETROLEUM)

Approved by,

_________________

(Noor Ilyana Bt. Ismail)

UNIVERSITI TEKNOLOGI PETRONAS

TRONOH, PERAK

September 2014

i
 CERTIFICATION OF ORIGINALITY

This is to certify that I am responsible for the work submitted in this project, that the
original work is my own except as specified in the references and
acknowledgements, and that the original work contained herein have not been
undertaken or done by unspecified sources or persons.

_________________________________

MOHD FIZDRUL HAQEEM BIN MOHD LETFINUDDIN

ii
 ABSTRACT

Recent resin injection for sand consolidation in the oil wells can give up to 600-700
psia of the compressive strength (Wasnik, Mete, & Ghosh, 2005). This would be
enough to withstand high pressure from the formations and drilling activities in short
period of time. However, resin injection alone is not effective to produce long lasting
permanent result. Catalyst need to be added together with the resin injection to
enhance the consolidation treatment. Resin injection alone also takes longer period to
cure and hardened. Hence, addition of catalyst into the treatment is crucial to reduced
curing time. Previous resin treatment on multi layered formation in Peninsular
Malaysia has used Hydrochloric acid (HCl) as the catalyst (Keith et al., 2013).
Unfortunately, strong acid like Hydrochloric acid cause serious corrosion problems
to the equipment. Acetic acid which is an organic acid is chose as the main catalyst
for the resin injection treatment. An experiment was conducted to determine the
effectiveness of Acetic acid as main catalyst for epoxy resin in formation sand
consolidation treatment. Parameters tested were curing time, permeability and
compressive strength. The experiment considers whether Acetic acid catalysed resin
could give high curing rate, high compressive strength and also better permeability to
the consolidated sand. Results obtained for curing test is economical viable as the
resin cured in less than 24 hour. Permeability test for organic acid catalysed resin
produced good results as 4 of the samples permeability values are in the range of
normal formation permeability which is 0-500 md. While, the rest 5 samples
recorded values greater than 500 md. For compression test, all samples indicates
results of greater than 700 psi which is better than previous uncatalysed resin
treatment.

iii
 ACKNOWLEDGEMENT

First and foremost, I would like to express my appreciation and praise to God for His
guidance and blessings throughout my final year tenant. Special gratitude and
upmost appreciation to my FYP's supervisor, Mrs. Noor Ilyana Bt. Ismail for
guiding, monitoring and teaching me throughout the whole 14 weeks of final project
period. I also would like to thank to lab technicians from Geosciences department for
their times, supports and guidance upon completing my project.

Last but not least, my appreciation goes to my family and friends for their
encouragement and guidance without which the completion of this project would not
be possible

iv
 TABLE OF CONTENTS

CERTIFICATION i

ABSTRACT iii

ACKNOWLEDGEMENT iv

CHAPTER 1 : INTRODUCTION 1

1.1 Background of study 1

1.2 Problem Statement 2

1.3 Objectives 3

1.4 Scope of study 3

1.5 Relevancy and Feasibility 4

CHAPTER 2 : LITERATURE REVIEW 5

2.1 Sand production 5

2.2 Causes of sanding 5

2.3 Sand production categories 7

2.4 Effect of sand production 8

2.5 Methods of sand control 8

2.5.1 Mechanical methods 9

2.5.2 Chemical methods 9

2.5.2.1 Resin injection 10

2.5.2.2 Resin categories 10

2.5.2.2.1 Thermosetting resins 10

2.5.2.2.2 Thermoplastic resins 11

2.5.2.3 Resin treatment advantages 11

2.5.2.4 Epoxy resin 12

2.5.2.5 Catalyst 12

2.5.2.6 Organic acid 13

v
 2.5.2.7 Acetic acid 14

2.5.2.8 Resin curing 15

CHAPTER 3 : METHODOLOGY 16

3.1 Preliminary studies 16

3.2 Pre experimental studies 16

3.3 Experimental flow process 17

3.4 Experimental designs 17

3.4.1 Test cores preparation 17

3.4.2 Experiment procedures 18

3.4.3 Calculations 19

3.4.3.1 Resin,hardener & acid concentration 19

3.4.3.2 Permeability 20

3.5 Research Methodology and Project Activities 21

3.6 Experiment flow chart 22

3.7 Tools Required 27

CHAPTER 4 : RESULTS AND DISCUSSIONS 28

4.1 Curing time 28

4.2 Permeability 29

4.3 Compressive strength 31

4.4 Permeability vs. Compressive strength 32

CHAPTER 5 : CONCLUSIONS AND RECOMMENDATIONS 35

REFERENCES 36

BIBILIOGRAPHY 37

vi
LIST OF FIGURES :

Figure 1 : Sand production 5

Figure 2 : Sand arches 6

Figure 3 : debris and damage in the perforation tunnel 6

Figure 4 : principle of sand control polymer treatment 9

Figure 5 : Sand sample taken from Pantai Teluk Batik, Lumut 17

Figure 6 : Permeability calculation 20

Figure 7 : Project gantt chart and key milestones for FYP I 23

Figure 8 : Project gantt chart and key milestones for FYP II 24

Figure 9 : Important dates for FYP 1 25

Figure 10 : Important dates for FYP II 26

Figure 11 : Custom made sand mould 27

Figure 12 : Uniaxial compression machine 27

Figure 13 : Rock permeability machine 27

Figure 14 : Sand screening machine 27

Figure 15 : Resin coated sand 28

Figure 16 : Curing time results 29

Figure 17 : Permeability results 30

Figure 18 : Compressive strength results 32

Figure 19 : Permeability vs. Compressive strength for Uncatalysed resin 33

Figure 20 : Permeability vs. Compressive strength for Acetic acid

catalysed resin 33

Figure 21 : Permeability vs. Compressive strength for Hydrochloric

acid catalysed resin 34

vii
LIST OF TABLES :

Table 1: Curing time vs. resin concentration 28

Table 2: Permeability vs. resin concentration 29

Table 3: Unconfined compressive strength vs. resin concentration 31

viii
 CHAPTER 1

INTRODUCTION

1.1 Background of Study

Sand production is one of the main problems facing by oil and gas industry recently.
Usually most of the sand production comes from sandstone formation wells which
are unconsolidated. The real challenges of the sand production is it can cause erosion
and failure to the flowlines, pumps, separators and many other equipment. High
maintenance cost of these equipment could cause to the closure for some oil
producing wells. Reduced in oil production also could be happen because of this
sand production. The produced sand that enter through perforated production tubing
will settle down in the bottom hole of the wellbore which eventually lead to the
production reduction. Apart from that, well integrity is also affected due to the sand
production. Sand that produced can affect formation stability.

There are several factors of leading to sand production in oil wells. Carlson et al.
(1992) stated that, in better cemented rocks, sanding may be induced throughout
incidents in the well's production life. For instance, excessively reduced in
production rates, fluctuation of reservoir pressure, alteration of gas and liquid ratio,
and water influx has becomes the major elements in introducing sanding during oil
and gas production. As reaction to this, many solutions had been introduced to
eventually reduced the sand production in most oil wells globally. The most popular
present methods of controlling sand are based on two principles; bridging of sand
grain and consolidation of the sand in-situ (Dewprashad, Abass, Meadows, Weaver,
& Bennett, 1993). 'Bridging' of the sand grains could be achieved by using gravel
packs, slotted liners, and sand screens techniques. For in-situ sand consolidation,
proper plastics (polymers) or other cement based materials were used to attach the
sand grains together without great impact in permeability reduction.

1
However, following the current trend, chemical based formation consolidation are
preferable rather than mechanical based consolidations. This is due to economical
consideration as mechanical based sand control technique are more expensive
compared to polymer injection application. According to Wasnik et al. (2005), one of
the advantages of resin consolidation is; it is cheaper as compare to gravel packing
and frac packing technique.

Therefore, it is crucial to determine which techniques should be applied and the

decision largely depend on the reservoir properties and financial status of the
operators. In this research, details of the polymers injection technique used in sand
control is studied to come out with better post-treatment result.

1.2 Problem Statement

Currently, the available resins injection for sand consolidation in the oil wells can
give up to 600-700 psia of the compressive strength (Wasnik et al., 2005). This
probably would be enough to withstand high pressure from the formations and the
drilling activities in shorter period. However, to ensure formations sand remained
consolidated for longer period of time, the compressive strength of the consolidated
sand should be increased. This can prevent from repeating the same treatment as it
require huge budgets to run each treatment. Long well shut-in period for sand
consolidation treatment also could cause economical loss as production stops.
Previous resin treatment usually takes up to 24 hours for the resin to cure.

To overcome those problems, some operators used resin catalysed by Hydrochloric

acid for sand consolidation treatment (Keith et al., 2013), but, there are problems
related to this method. Externally catalysed Hydrochloric acid could cause corrosion
especially to the production tubing. The most straight forward way by bull heading
the treatment fluid from surface to formation cannot be done due to stated problem. It
need proper ways of fluid conveyance in determining the success of the treatment.
Hence, in this project, organic acid is introduced to replace Hydrochloric acid as the
catalyst for resin injection. This is due to its less reactive to the metal and more
convenient to use.

2
1.3 Objectives

 To determine the compressive strength of sand consolidation when treated

with resin catalysed by Organic Acid
 To determine the curing time of the sand consolidation when treated with
resin catalysed by Organic Acid.
 To determine the permeability of the organic acid catalysed resin for sand
consolidation treatment
 To compare the treatment results between resin catalysed by organic acid,
inorganic acid (Hydrochloric acid), and uncatalysed resin.

1.4 Scope of study

This study focuses on the use of polymer (resins) for sand consolidation in the gas
and oil wells. The resins will be treated and catalysed with Organic acid in order to
increase compressive strength and also it is expected to reduce hardening time after
the placement. The principle is; the resins will be injected into the formations in
order to coagulate and bound the sand particles together. The compressive strength
and hardening time of the consolidated sand that is injected with catalysed resins
and without catalyse will be recorded. The results will be analysed to determine
whether the catalyst (Organic Acid) is effective to enhance the parameters stated.
The results between catalysed resin by organic acid and catalysed resin by inorganic
acid(Hydrochloric acid) also will be compared.

3
1.5 Relevancy and Feasibility

This project is related the author’s field of study since sand control is one of the
major subject in Petroleum Engineering field. In project perspective, the author are
trying to find an alternative solution to the current available resin injection
techniques. The organic acid catalyst was introduced to accommodate the problems
related to curing rate and uniaxial compressive strength of the resin consolidated
sand. Apart from that, this project also aimed to solve the problem of previous resin
catalysed by hydrochloric acid which cause serious corrosion issue after the
treatment. Hence, as a Petroleum engineer, the author carried out some experimental
work to determine the effectiveness of Acetic acid as a catalyst for sand
consolidation treatment.
In addition, this project is feasible by taking into account the time constraint
and the capability of final year student with the assistance from the supervisor and
coordinator. It is a big hope that the project is accomplished.

4
 CHAPTER 2

LITERATURE REVIEW

2.1 Sand Production

Sand grains in undisturbed reservoirs is held together by friction and cohesion forces
between the grains (Saether, 2010). Sand production occurs when the pressure and
stresses around the well bore is higher than the formation strength. Then the sand
grains will lose the contact and transformed from solid rock to sand. Once the sand is
detached, it follows the fluid stream through the perforations and into the well.
During its transport along with the fluid stream, the sand grains- and fragments are
subjected to effects from gravity and hydrodynamic forces.

Figure 1: Sand production (Saether, 2010)

2.2 Causes of Sanding

In unconsolidated formations, sand production may be triggered during the first flow
of formation fluid due to drag from the fluid or gas turbulence (Carlson et al., 1992).
This has caused the sand grains to be detached from the sand rock and being carried
to the perforations and thus produced together with the oil and gas in the production
flowlines.

Another reason that lead to the sanding is; fluctuations or excessively reduced in
production rates. The reduction of the production rates will affect the perforation
cavity stability. The inconsistent in production rates will affect the stability of the
sand arches. An arch is in curvy shaped and function to interlock the sand grains.
This arch is stable at constant flow rate and production rate. Any changes in the
production rates will results in collapse of the arch and thus leading to sanding until
the new arches formed.

5
 Figure 2: Sand arches (Carlson et al., 1992)

Furthermore, water influx also plays important role in causing the sand production.
Water that break through from the surrounding aquifers will reduce capillary
pressure between the sand grains (Mcleod, 1997). The sand grains will detached by
the effect of flow friction as the results of water contact.

Other than that, perforating activities also could lead to the sand production of the oil
and gas formations. Perforation process will alter the permeability of the surrounding
perforation cavity's surface. This has weaken the formation especially near to well
bore. As a result, this weakened formations may be collapsed and produced sand
when the production rates fluctuated.

Figure 3: Debris and damage in the perforation tunnel (Carlson et al., 1992)

6
2.3 Sand Production Categories

2.3.1 Transients

Sand production usually happen during clean up after perforation and

acidizing process. At this conditions, sand production will decreases with
time at a constant production flow rates.

2.3.2 Continuous

Sand that produced in unconsolidated reservoirs which is not equipped with

sand control equipment.

2.3.3 Catastrophic

This is the worst case scenario of the sand production in unconsolidated

sandstone formations. Usually, at this sand production category, the large
amount of sand produced due to excessive production of reservoir fluids. The
differences in hydraulic pressure leading to fluid transport into the well and
changes of pressure near the well bore of the formations has caused the
instability of the shale, clays, and sandstones. As the shales is exposed to the
drilling mud, the cations and anions in the mud filtrate are repelled while the
uncharged water is freely contacted to the structure of shale. Thus, it caused
the clay to swells and leading to stress build up in the shale. As the result,
shale caving and fragmentation formed.

7
2.4 Effect of Sand production

Production of sand causes many problems. Sand that produced from sandstone
formation introduced a number of potentially and costly problems (Waltman, 2010).
Most of them are due to economics related. Below are listed several problems related
to sand production:

1. Affect functionality of regularity for many equipment such as production

flowlines, valves, and separators.
2. Sand that fills and settled down in the separators, storage tanks, and
transportation vessel could lead to process problems and this may cause shut
downs and operations removal for some oil and gas rig.
3. Loss of production due to too much of sand production would result in shut in
wells in order to run the cleaning process in the flowlines.
4. Casing collapse. The sand produced from the sandstones formations will
leave an empty space behind the casing (caving). The extra pressure from the
drilling process would result in casing collapsing.

2.5 Method of Sand Control

Recently, there are various available methods that being used to control sand
production from the formations. Some of these techniques include mechanical,
cement packing and gravel packing (Karian, 2000). Most researchers used polymers
and plastics like furan resins for sand consolidation treatments (Friedman,
1991a,1999b,1989). Basically, the current techniques of sand consolidations and
sand control can be classified into two categories, which are mechanical methods and
chemical methods.

8
 2.5.1 Mechanical methods

This type of sand control method require mechanical components and

equipment to reduce and prevent the sand from being produced together with
formation fluids. The available mechanical methods composed of :

 Gravel packing
 Pre-slotted liners
 Pre-packed screens
 Frac-packing

2.5.2 Chemical methods

Sand control by chemical consolidation involves the process of injecting

chemical into the semi consolidated or unconsolidated formation
(Wasnik et al., 2005). The chemical used usually comes from resins or
polymer liquid resin. Polymers or plastic consolidation is one of the invented
technique to control sand production. Generally, as the polymer solution is
injected into the formation, it gets either adsorbed or becomes attached to the
walls (lahalih & Ghloum, 2010). However, sand consolidation using
polymers treatments should consider some requirements to ensure its
effectiveness. First is, polymers injection should give and provide sufficient
compressive strength to the unconsolidated sand. The other one is, the
operators should ensure that the polymers injected into the well does not
affect too much on the formation permeability. This is because alteration in
permeability will result in loss of reservoir fluid formation.

Figure 4: Principle of sand control polymer treatment (Zaitoun & Pichery, 2009)

9
2.5.2.1 Resin injection

The use of resins for artificial sand consolidation was first mentioned
in 1947 and from the 1960's onwards, sand consolidation gained in
popularity as an alternative to gravel packing (Fader, Surles, Shotts,
& Littlefield, 1992). Resin injection are broadly used as the sand
consolidation technique in order to mitigate and reduced sand
production from an unconsolidated sand stones formations. The resins
functioned by coating the sand grains which is then followed by an
over flushed to enhance permeability. Few hours after the treatments,
resins injected will harden and thus forming permeable consolidated
sandstones. Basically, the main objectives of resins injection is to
enhance compressive strength of the formation especially in well bore
surrounding area. As consequence, sand grains will not be detached
although in fluctuations production rates condition.

2.5.2.2 Resins can be divided into two categories:

2.5.2.2.1 Thermosetting resins

Generally, thermosetting resins are a type of resin which can
transform irreversibly under heat influences from a fusible and
soluble material into infusible and insoluble through
formation of a covalently cross-linked thermally stable
network. Relatively, thermosetting usually contains low
molecular weight which is about less than 10000 daltons.
Curing process has chemically transform the chains into a
molecule by cross-links. Effect of heating, chemical reaction
and under severe conditions can intently break the chemical
bonds between the chains. The most popular thermosetting
resins available recently are formaldehyde condensation
products with phenol (phenolic resin) or with urea or
melamine (amino resins). Besides, polyester resins are epoxy
resins are broadly used for surface coating and many other
functions. Thermosetting resins are chemically stable for

10
 indefinite time over a wide range of temperature, inert to
wellbore fluids, rocks and greens to the environment.

2.5.2.2.2 Thermoplastic resins

Thermoplastic resins are a type of resins which can soften and
flow as it is introduced to heat and pressure, the changes is
reversible. It consists of monomers building blocks which
linked up chains with high molecular weight, approximately
more than 10000 daltons. Cohesion force of the polymer
matrix is provided through physical bonds between the chains.
However, by heating and dissolving the chains, the physical
bonds can easily broken. Polyethylene, polypropylene and
polystyrene are several examples of available thermoplastic
resins.

2.5.2.3 Resin Treatment Advantages

o Unneeded the use of sand gravel which could limit the reservoir fluid
production.
o Unneeded of internal screen when comes to resin consolidation, thus
eliminate mechanical risks associated to screen placement.
o Treatment can be done only through existing tubing or coiled tubing.
o Treatment is cheaper as compared to gravel packing and frac packing
techniques.
o Treatment is effective in fine sand, which are complicated to control
using gravel packing.
o Increase compressive strength of the formation while retaining 60-
90% of the original permeability.
o Yield approximately 90% or even more than the original productivity.

11
2.5.2.4 Epoxy resin

Epoxy resins, which is also known as polyepoxides are a class of

reactive prepolymers and polymers which contain epoxide functional
group. It is a common name for a type of strong adhesive used for
sticking things together and covering surfaces. Epoxy resins reacted
by cross-linked either with themselves through catalytic
homopolymerisation, or with a wide range of co-reactants including
polyfunctional amines, acids, phenols, alcohol, and thiols. Reaction of
polyepoxides with themselves or with polyfunctional hardeners forms
a thermosetting polymer, often with strong mechanical properties as
well as high temperature and chemical resistance. Curing of epoxy
resins referred reaction of the linear epoxy resin with suitable
curatives to form 3D cross-linked thermoset structures. Curing may be
achieved by reacting an epoxy itself (homopolymerisation) or by
forming a copolymer with functional curatives or hardeners (Pascault
et al., 2002). Basically, any molecule containing reactive hydrogen
may react with epoxide groups of the epoxy resin. Epoxy curing
reaction may be accelerated by addition of small quantities of
accelerators. tertiary amine, carboxylic acids and alcohols are
effective accelerators.

2.5.2.5 Catalyst

The word catalyst can be described as the substance used to increase

in the rate of chemical reaction of one or more reactants due to
participation of an additional substance under the process called
'Catalysis'. In this project perspective, the action of catalyst is needed
to enhance the performance of the resin injection for sand
consolidation purpose. Suitable catalyst are needed to increase the
mechanical strength of the consolidated formation and control the
curing or solidification time depending on the various downhole
temperature. For low temperature application, a strong organic acid is
used, while for high temperature applications, a weak organic acid is
12
used (Fader et al., 1992). By this injection of catalyst together with
resin, the rate of polymerization of the chemical reaction system can
be adjusted ranging from few minutes up to few hours depends on
amount of catalyst injected. The injected catalysed resin are also
expected to produce great result as compared to non catalysed resin
injection. Therefore, experimental procedures must be conducted to
determine whether catalyst added up together with resin injection can
boost up the compressive strength or not.

2.5.2.6 Organic acid

Organic acid defined as organic compounds with acidic properties.

Generally, organic acid is a weak acid and do not dissolve completely
in water as compared to strong mineral acids(inorganic acids). In oil
and gas industry, simple organic acids such as acetic or formic acids
are widely used for oil and gas well stimulation treatments. This is due
to its less reaction to metal as compared to strong inorganic acids likes
sulphuric and hydrochloric acid. Keith et al. (2013) in their research
has used Hydrochloric acid (inorganic) as the catalyst in resin
injection for well consolidation treatment. Although the treatment was
successful, the placement or conveying method became their main
problem in this treatment. Externally catalyzed resin would cause
corrosion especially to the production tubing. Based on this,
organic acids are used at high temperature conditions or when it need
longer contact time between the pipes and acids. This usually happen
when acids need to be injected into greater depth of reservoirs. In this
project, organic acid is going to be used as reaction catalyst to furan
resin for formation consolidation treatment. The function is to enhance
the curing period of the resin's treatment and also provides extra
compressive strength to the consolidated formations. As described
earlier, in some cases organic acid is used as external catalyst to
regulate the curing temperature of the resin's consolidation treatment.

13
2.5.2.7 Acetic acid

Among the available organic acids, Acetic acid was chosen as the
catalyst in the resin injection for formation consolidation treatment.
Acetic acid, containing the group CH3COOH. This type of acid can be
thought of as ethanoic acid and it gives vinegar with sour taste and
pungent smell. It is relatively considered as weak acid and partially
dissociated acid in an aqueous solution. Acetic acid is one of the
simplest carboxylic acid. They are usually colourless and non
oxidizing which means more convenient to use. In industry, Acetic
acid broadly used in many applications and one of them as for catalyst
reaction. In easiest way, general acid catalysis means all species
capable of donating protons contribute to reaction rate acceleration.
With carbonyl compounds such as esters, synthesis and hydrolysis go
through a tetrahedral transition state, where central carbon has an
oxygen, an alcohol group, and the original alkyl group. Acids can
generally protonate the carbonyl, which makes the oxygen positively
charged (Röper et al., 2000). This has make it easy in receiving double
bond electron when the alcohol attacks the carbonyl carbon. This
enables ester synthesis and hydrolysis. The reaction is an equilibrium
between the ester and its cleavage to carboxylic acid and alcohol; acid
+ alcohol ester + water. Generally, the main objective of acid
catalyst in resin system is to accelerate the condensation reaction of
resin treatment and thus increase the cure rate. Organic acid such as
Acetic acid could act as cross-linkers for polymeric material including
resin. Besides, Acetic acid can also act as cross-linker on the
compressive strength of actual solid cores (lahalih & Ghloum, 2010).
Since the proppant samples is from bank sand, it may contains fine
particles of sea shells which is carbonate material. The heated and
oxidized carbonate materials during thermal reclamation will convert
carbonates to water soluble and very alkaline lime, or calcium oxide
(CaO). The presence of lime in the sand must be neutralized by the
acid catalyst before it can start to cure the resin. Acetic acid was

14
chosen due to its catalytic strength, reliability, availability and cost
effective compared to other organic acids.

2.5.2.8 Resin Curing

"Cross-linking" or "curing" is the process that changes liquid formed

resins into 3D solid network. Building blocks that consists of small
monomer or oligomer molecules aggregating into clusters are called
'cross-linking' process. The clusters will then continue to aggregate
and becoming larger until a network is formed that spans the reacting
mass. Viscosity can be seen increasing during clusters build-up due to
extension of Stoke's law for velocity which when clusters size
increase, clusters movement slowly becomes restricted (Wasnik et al.,
2005). The cluster network will span the reacting mass and any
movement in large quantity is restricted at the so-called gel point. At
the gel time, viscosity of the fields will drops asymptotically to
infinity. Before this to be happens, the system need to be in target well
bore as fluid cannot be squeezed after this stage. Until the gel time,
the viscosity will remain constant. Resin curing rate or solidification
time plays important role in determining the success of formation
consolidation treatment. Basically, temperature and catalyst are the
two parameters which dominantly determine the curing rate of the
treatment. Presence of catalyst could reduce eventually half of the
actual curing time. In some cases, it would take up to 7 days to fully
cure the injected resins at 70o F reservoir temperature. Villesca et al.
(2010) recommended that addition of catalyst only for wells with
bottom hole temperature 1600F of below. This to prevent from any
premature curing occur during resin consolidation treatment. Other
than that, integrity of the consolidated formation could be affected due
to presence of catalyst for resins injection at higher reservoir
temperature. Alz((SO4)3, AlCl3, and NH4Cl are examples of lewis acid
catalysts that enhance ionic polymerization.

15
 CHAPTER 3

METHODOLOGY

For FYP I, the method and the project flow process consists of preliminary study and
pre experimental work.

3.1 Preliminary Studies

In this section, it focuses on understanding the project fundamental and theories.

Preliminary studies have been highlighted in project planning and literature review.
It includes study on the type of resin and possible catalyst that can be used in the
experiment. Journals and articles related to the study subject would be really helpful
to get clear view about the project. The main objectives of this research project are to
determine the compressive strength and the curing time of the formation when
treated with catalysed resin. The result will be compared with the resin catalysed by
Hydrochloric acid treatment.

3.2 Pre experimental studies

In this part, catalysed resin experiment is prepared. Below are the list of parameters
required for the experiment.

 Sand sizes : ranges from 212 - 600 microns

 Source of sand : Pantai Teluk Batik, Lumut, Perak
 Resin : Epo Thin Epoxy Resin
 Hardener : Epo Thin Epoxy Hardener
 Amount of resin : 10%, 20%, 30%
 Brine water (3% KCl) : 420 ml
 Type of catalyst: 2 Mole of Acetic acid and Hydrochloric acid
 Amount of acid catalyst : (1/5) of the resin concentration
 Amount of sand : 420.4 gram per pack
 Equipment required : Rock permeability machine, Uniaxial compression
machine, sand mould, Sand screening machine
 Curing period (H)

16
  Curing temperature (oC)
 Permeability (md)

3.3 Experimental flow process:

1. Proppant consolidation treatment

2. Permeability test
3. Compressive strength test : Uniaxial compressive strength Triaxial
Compression test
4. Curing period test : Oven (temperature constant @70o C)

3.4 Experimental Designs ( for FYP II )

3.4.1 Test cores preparation

To conduct the experiment, sand sample is first being collected from coastal
beaches near Lumut. The reason of sand collected around that area is
because the beach sand properties are similar with sandstone reservoirs in
offshore fields. This sand samples is going to be used as man-made
proppant to prepare the proppant pack. A flow cell is a type of equipment
that widely used in preparing the proppant pack.

Figure 5: Sand samples taken from Pantai Teluk Batik, Lumut

17
3.4.2 Experiment Procedures

Sand samples near Teluk Batik beach was first collected and screened. Sand
size of 212-600 microns being weighted at 420.4 g for each samples. The
sand is saturated with 420 ml completion brine (3% KCl) as pre-flush
treatment to enhance sand consolidation. Then, sand was mixed with resin
and 2 Mole acid for 10%, 20%, and 30% resin concentration ratio to sand
weight. For instance, at 10% resin concentration, 1/10 of the total sand weight
is the amount of resin used. Acid catalyst amount will be 1/5 of the resin
amount, and hardener is 2/5 of the resin amount. The procedures were
repeated for 20% and 30% resin concentration. A custom made mould with
inside diameter of 55 mm and length of 110 mm was used in preparing sand
core samples. Prior to this, the grease was first put on the interior wall of
mould to prevent the cured samples stuck inside the mould. As the mould was
vertically positioned, the mixture of sand, resin, and acid was slowly poured
into the mould while the mould was slightly tamped to enhance packing of
the sand grains. The packed sand cores was then placed in an oven for curing
at 70oc. The curing duration for each samples was recorded. Cured sand cores
were then undergoes permeability and compression strength test.

18
 3.4.3 Calculations

3.4.3.1 Resin, Hardener and acid concentration

Sand amount : 420.4 gram

1. - For 10% resin concentration:

0.1 × 420.4 g = 42.04 g (resin amount)
- Hardener : 2/5 of the resin amount
2/5 × 42.04 g = 16.816 g (hardener amount)
- Acid (Hydrochloric / Acetic) : 1/5 of the resin amount
1/5 × 42.04 = 8.408 g (Acid amount)

2. -For 20% resin concentration:

0.2 × 420.4 g = 84.04 g (resin amount)
-Hardener : 2/5 of the resin amount
2/5 × 84.04 g = 33.63 g (hardener amount)
-Acid (Hydrocholric / Acetic) : 1/5 of the resin amount
1/5 × 84.04 g = 16.82 g (Acid amount)

3. -For 30% resin concentration:

0.3 × 420.4 g = 126.12 g (resin amount)
-Hardener : 2/5 of the resin amount
2/5 × 126.12 g = 50.45 g (hardener amount)
-Acid (Hydrocholric / Acetic) : 1/5 of the resin amount
1/5 × 126.12 g = 25.224 g (Acid amount)

19
3.4.3.2 Permeability

For the permeability test, the data obtained from Rock Permeability
machine will be put inside the Darcy equation in order to determine
the permeability of the sand core samples. The machine provides the
pressure to run the test (∆𝑃). For the permeability test, the initial
pressure recorded at 1000 kPa. The flow rate (m3/s) of the water
flowing inside the core can be obtained from the volume of water
collected divided by test time. For the other parameters, the values are
as follows:

Core Area : 0.00238 m2

(∆𝑃) : 1000 kPa

µ (water) : 8.9× 10-4 Pa.s

Core Length : 0.11 m

Test time : 5 min

After running the test, the permeability can be calculated through

following Darcy's equation:

Darcy Equation:

𝑘 𝐴∆𝑃
Q (m3/s) = 𝜇𝐿

From the Darcy's equation, the value of permeability (k) obtained is in

(m2 ). Then, it needed to be converted into Darcy using conversion
factor of 1 Darcy = 9.86923 × 10-13 m2 .

Figure 6 : Permeability calculation

20
3.5 Research Methodology and Project Activities

Define Problem
statement and Objectives

Perform literature study

and preliminary research

Experimental Design

Data Analysis

Discussion and
Recommendation

Reporting and
Documentation

21
 3.6 Experiment Flow Chart

Start

Sand core
preparation

Curing process OVEN : @ 70OC

NO

Curing check
YES

Permeability test

Compression test

22
Activities in FYP 1 week
1 2 3 4 5 6 7 8 9 10 11 12 13 14
Project title selection and meeting with FYP 
supervisor
Study the factors of sand production
Analyse the available methods of sand control
Study resin consolidation treatment for sand
control application
Draft the methodology of the project
Extended proposal submission 
Proposal defence 
Write abstract and expected results
Submission of interim draft report 
Submission of final interim report 

Legend
Project section timeline
 Project milestones (important weeks)

Figure 7: Project Gantt Chart and key milestones for FYP I

23
Activities in FYP II week
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
Project work commences
Briefing and update on FYP II progress
Chemicals Preparation
Lab booking and registration
Equipment Preparation : custom made
the Sand Pack
Submission of Progress Report 
Result Analysis
Pre-SEDEX/ Poster Exhibition 
Submission of Final draft/ Technical 
paper
SEDEX 33 
Final oral presentation/ Viva 
Submission of hardbound copies 
Figure 8: Project Gantt chart and key milestones for FYP II

Legend
Project section timeline
 Project milestones (important weeks)

24
 10th July 2014
Week 13 (2014)
(Week 8)
• Project title • Proposal • Submission
selection • Submission defence • Submission of interim
of extended of interim report
proposal draft report
9 th June 2014
Week 9 (2014) Week 14 (2014)
(Week 3)

Figure 9: Important dates for FYP I

25
 10 th Dec 2014 22-23 rd Dec
(Week 9) (Week 14) 2014
• Progress • SEDEX 33 • Hardbound
report • Pre-SEDEX • Technical • Final oral copies
submission poster paper presentation submission
exhibition submission
5 th Nov 2014 10-11 th Dec 5 th Jan(Week
(Week 7) (Week 12) 2014 16) 2015

Figure 10: Important Dates for FYP II

26
3.7 Tools Required

1. Mould: Sand pack preparation

2. Uniaxial compression machine
3. Rock permeability machine
4. Sand screening machine

Figure 11: Custom made Sand mould Figure 12: Uniaxial compression
(size: 55mm×110mm) machine

Figure 13: Rock permeability machine Figure 14: Sand screening machine

*Noted that all of the equipment are taken from UTP Geosciences lab at block 14
and 15.

27
 CHAPTER 4

RESULTS & DISCUSSIONS

4.1 Curing Time

Table 1: Curing time vs. Resin concentration

Type of resin Resin concentration (%) Curing time (Hour)

Uncatalyzed Resin 10 9
20 15
30 20
Resin + Acetic acid 10 7
20 13.5
30 16
Resin + HCL 10 5
20 11
30 14

Based on the table(1) and figure(16) , it is clear that amount of injected resin is
proportional to the curing and hardening period. As the resin concentrations increase,
the longer it takes for the resin coated sand to
cure. For each resin concentration, addition of
acids catalyst had reduced the curing period of
the sand samples. However, Hydrochloric acid
catalysed resin gives quite shorter period for the
samples to cure as compared to Acetic acid
catalysed resin. This is due to Hydrochloric acid
is stronger acid as compared to Acetic acid.
Catalytic reaction is much effective in stronger
acid. (Van Rhijn, De Vos, Sels, & Bossaert,
Figure 15: Resin coated sand
1998)

28
 Figure 16: Curing time results

4.2 Permeability

Table 2: Permeability vs. Resin concentration

Type of resin Resin concentration (%) Permeability (md)

Uncatalyzed Resin 10 434
20 255
30 237
Resin + Acetic acid 10 542
20 510
30 474
Resin + HCL 10 866
20 818
30 773

29
Table (2) and figure (17) shows the summary of permeability of resin coated sand
with different types of catalyst and resin concentration. It can be seen that the resin
concentration is inversely proportional to the permeability values of the resin-coated
sand. As the resin concentration increase, the permeability values decrease. This is
because the cross-linked formed between the grains increased as the resin
concentration increase and this will thus reduced the permeability of the fluid to
flow. It was observed that both Hydrochloric acid and Acetic were good enough to
permit the fluid flows. Hydrochloric acid shows better permeability with 10% resin
results in 434 md, 20% resin concentration for 818 md, and 30% resin concentration
for 773 md. While, Acetic acid gives 542, 510, and 474 md for 10%, 20%, and 30%
resin concentrations. Since normal range of acceptable permeability is 0-500 md,
and the difference was not too much from Hydrochloric acid catalysed resin, Acetic
acid is considerable to replace Hcl for resin catalyst in real well scenario.

Figure 17 : Permeability results

30
4.3 Compressive Strength

Table 3: Compressive strength vs. Resin concentration

Type of resin Resin concentration (%) Compressive Strength

(Psi)
Uncatalyzed Resin 10 1358.11
20 1406.90
30 1493.90
Resin + Acetic acid 10 1482.28
20 1662.13
30 1972.51
Resin + HCL 10 1914.49
20 2432.28
30 2494.65

Table (3) shows relationship between resin concentration for each type of resin with
the compressive strength of the sand core samples. Compressive strength test on the
sand core samples found that HCl catalysed resin gives higher strength than Acetic
acid catalysed resin with 1914.50 psi, 2432.28 psi, 2494.65 psi for each 10%, 20%,
and 30% of resin concentration. While, for Acetic acid acid catalysed resin, it shows
1482.28 psi, 1662.13 psi, 1972.51 psi for 10%, 20%, and 30% resin concentrations.
Dewprashad et al. (1998) stated that from SEM micrograph, it was observed that as
the resin concentration increase, it will thus increase in areas and numbers of contact
points between grains. Hence, the higher of resin concentration, the stronger grain-
to-grain bond of the sand will be. Although, HCl catalyst is much better in strength,
but Acetic acid catalysed resin could also produce long lasting result and bear with
high formation pressure since Wasnik et.al (2005) stated that previous resin injection
treatment results in 600-700 psi compressive strength.

31
 Figure 18: Compressive strength results

4.4 Permeability vs. Compressive strength

Figure (19),(20,(21) summarized the relationship between permeability and

compressive strength of the core samples. It can be seen that for different type of
catalyst and resin concentrations, permeability value is inversely proportional to the
compressive strength of the sand core samples. As the resin concentration increase,
the permeability of the resin core samples decrease. This is because, the increase in
grain-to-grain bonds as results of increasing in resin concentrations caused reduced
in permeability to fluid flow. For Acetic acid catalysed resin, 10% resin
concentration does not give much difference between permeability and core samples
compressive strength. However, for increasing in resin concentrations, there is major
drop in permeability as the compressive strength increased. The same situation
occurs for the Hydrochloric acid catalysed resin. At initial resin concentration,
permeability and compressive strength still in tolerance mode, but, as the resin
concentration increase, it is obviously be seen that increase in compressive strength
results in major drop in permeability values of the sand core samples.

32
Figure 19: Permeability vs. Compressive strength for Uncatalysed resin

Figure 20: Permeability vs. Compressive strength for Acetic acid catalysed resin

33
Figure 21: Permeability vs. Compressive strength for Hydrochloric acid catalysed
resin

34
 CHAPTER 5

CONCLUSIONS & RECOMMENDATIONS

The study of resin coated sand using acid catalyst has been successfully conducted
for range of samples in different resin concentration from 10% to 30% by weight of
sand. Based on the obtained results for each parameters tested, the objectives of the
study are fully achieved. For the curing and hardening time, results gained for Acetic
acid catalysed resin in each resin concentrations is within 24 hours. Shorter period of
curing process is better due to economical reason. Permeability values for each
samples of Acetic acid catalysed resin is good and acceptable as it in between 400-
600 md which is in ranges of normal formation permeability. Besides, results from
compressive strength test indicates that Acetic acid catalysed resin for sand
consolidation treatment is more than enough to withstand high formation pressure in
longer period of time as the values are greater than previous resin treatment strength
(600-700 psi). Apart from its promising results, the reliability, availability and cost
effectiveness has become the major factors of why Acetic was chosen.

Since the sand mould was custom made, the core samples produced does not
perfectly formed cylindrical shape. This defect is less much effect the permeability
and compressive strength results. It is recommended that UTP management could
provide special mould for sand cores production. Besides, only 3 samples per
different type of catalyst can be produced in this study due to time constrains. For the
future, the number of samples should be added in order to obtain precise results data.

35
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