Copolymer SJ-1 as a Fluid Loss Additive for Drilling Fluid with high

content of salt and calcium

Hongping Quan,1,2 Huan Li,1,2 Zhiyu Huang,1,2 Tailiang Zhang 1,2 Shanshan Dai *,1,2

1
School of Chemistry and Chemical Engineering, Southwest Petroleum University,

Chengdu, P. R. China

2
Engineering Research Center of Oilfield Chemistry, Department of Education,

Chengdu, P. R. China

Address correspondence to Shanshan Dai, School of Chemistry and Chemical Engineering,

Southwest Petroleum University, Chengdu 610500, P. R. China. *E-mail:

wuyang1228@gmail.com Tel.: +86-28-83037305. Fax: +86-28-83037305.

1
Copolymer SJ-1 as a Fluid Loss Additive for Drilling Fluid with high

content of salt and calcium

Abstract: A ternary copolymer of 2-acrylamide-2-methyl propane sulfonic acid

(AMPS), acrylamide (AM) and allyl alcohol polyoxyethylene ether (APEG) with a

side chain polyoxyethylene ether (C2H4O)n SJ-1 were designed and synthesized in

this work. Good temperature resistance and salt tolerance of “-SO3-”of AMPS,

strong absorption ability of “amino-group” of AM, and good hydrability of side

chain polyoxyethylene ether (C2H4O)n of APEG provides SJ-1 excellent properties

as a fluid loss additive. The chemical structure of ternary copolymer was

characterized by Fourier transform infrared (FTIR) spectroscopy. The molecular

weight and its distribution was determinated by gel permeation chromatography

(GPC). The API fluid loss of drilling fluid decreased gradually with the increasing

concentration of NaCl and CaCl2 in the mud system. SJ-1 was applied well in the

drilling fluid even at a high temperature of 220oC. Results of Zeta potential of

modified drilling fluid showed the dispersion stability of drilling fluid system.

Scanning electron microscopy (SEM) analysis showed the microstructure of the

surface of the filter cake obtained from the drilling fluid modified by SJ-1.

Keywords: drilling fluid; fluid loss addictive; filter cake; temperature resistance;

salt tolerance

1. INTRODUCTION

Water-based drilling muds including bentonite were well known and widely used

[1-4]
in the petroleum industry recently . The main component of water-based drilling

fluid are water, salt, insert solids and clays such as montmorillonite. One of the

important functions of water-based drilling fluid was to form filter cake on the wall of

2
the well bore, prevent water leakage and maintain the stability of the well wall [5]. The

properties of the water-based drilling fluid, such as the rheology and filtration loss,

are effected by the fluid loss additive. Polymers, which are non-toxic, degradable and

[6-8]
environment friendly , are the best choice to be used as drilling fluids additives.

However, the traditional polymers as fluid loss additive are not stable at the work

condition of drilling fluid, especially at high salt condition and high temperatures. The

resulting drilling fluids often presents poor properties such as high filtration. If the

drilling fluid was applied in the high salt or calcium environment, the flocculated

structure of clay particles will appear and the value of API fluid loss will increase

obviously. Furthermore downhole accident such as borehole collapse will happen in

severe case. To solve the problems mentioned above, a novel fluid loss additive SJ-1

was developed in this work [9-12].

To make sure the fluid loss additive has an excellent ability of absorption, the

monomer with strong absorption groups, such as amino-group, are introduced [13-14].

To make sure the additive has an excellent ability of salt tolerance, the monomer with

stable group which is not sensitive to the cation, such as -SO3-, are introduced [15-17].

To make the fluid loss additive has an excellent ability of temperature resistance, the

monomer with inflexibility groups such as big side group, are introduced. At the

same time, the monomer that are hard to hydrolyze are introduced to get rid of the

side effect hydrolysis, such as polyoxyethylene ether (C2H4O)n [18]. In this work, a

good property of filtrate loss control even at high temperatures and salt condition of

SJ-1 synthesized by polymerization of AMPS, AM and APEG.

3
2. EXPERIMENTAL

2.1 Materials

AMPS, AM from Chengdu Kelong Chemical Reagent Factory (China).

APEG-1000 were industrial grade from Jiangsu Haian petrochemical factory (China).

Potassium persulfate, sodium hydroxide, sodium bisulfite, were analytical grade from

Chengdu Kelong Chemical Reagent Factory (China).

2.2 Synthesis

APEG (0.006 mol) was added in a three-necked flask, using moderate amount of

water to dissolve in a heated water bath. And then added AMPS (0.029 mol) and AM

(0.084 mol) to the mixed solution. The pH was adjusted to 7-8 with NaOH; Adding

0.2 wt% potassium persulfate and sodium bisulfite, stirred and mixed uniformly

reacted at 60oC. After completion of the reaction, the product was extracted with

ethanol, shear granulation, vacuum drying and grinding to obtain a white powdery

polymer fluid loss additive. Chemical structure of SJ-1 was shown in the Scheme 1.

In laboratory studies, the best parameters of copolymer SJ-1 were obtained:

monomer concentration was 15 wt%; molar ratio of n(AM):n(AMPS):n(APEG) was

14:5:1; the reaction temperature was 60oC; the concentration of monomer initiator

was 0.2 wt%.

2.3 Characterization

The pellet samples were prepared by pressing the mixture of the SJ-1 and KBr,

4
and then measured with FTIR (WQF-520, China) spectrophotometer at range between

4000 and 500 cm−1.

The molecular weight distribution of SJ-1 was measured by GPC (Waters e2695,

USA). The polymer was dissolved into distilled water forming the solution with

concentration of 2 mg/mL. The measurement was performed at the room temperature

(23°C) for 90 min.

2.4 Sample Preparation

Freshwater base mud containing 4 wt% of sodium bentonite and 0.2 wt% of

Na2CO3 was prepared by mixing the raw bentonite, Na2CO3 and freshwater at a

certain ratio, stirring for 20 min at a high speed of 10000 rpm and aging for 24 h at

room temperature. Salt-water base mud was prepared by adding different

concentration of NaCl into the above freshwater base mud, and then submitted to a

pre-hydration period of 24 h. Calcium-water base mud was prepared by adding

different concentration of CaC12 into the above freshwater base mud, and then

submitted to a pre-hydration period of 24 h. Polymer based mud was prepared by

adding different concentration of SJ-1 into the freshwater base mud, Salt-water base

mud and Calcium-water base mud respectively, and then submitted to a pre-hydration

period of 24 h.

2.4 Fluid Filtration Property Test

Drilling fluid filtration were measured according to American Petroleum Institute

5
(API) specifications and Chinese SY/T5621-93. The API filtrate volume (FLAPI) of

the mud was determined with a medium-pressure filtration apparatus (ZNS-2 type

China).

Apparent viscosity (AV), plastic viscosity (PV), yield point (YP) were measured

by rotational viscometer (ZNN-D6, China) at different temperatures.

Aging experiments of bentonite-polymer fluids were carried out in a frequency

conversion rolling oven (BRGL-7 type, China) at a series of temperatures for 16 h.

The filter cake of sample was tested by SEM (JSM-7500F, Japan) analysis and

the filtrate of sample was tested by Zeta electric potential (Zeta PALS/90plus,

Brookhaven, America) at different conditions.

3. RESULTS AND DISCUSSION

3.1 Chemical structure and molecular weight

The chemical structure of SJ-1 was analyzed by FTIR after purified, the results

were shown in Fig. 1.

A strong absorption peak of 3330.64 cm-1 was assigned to the stretching

vibration of N-H. The absorption peak observed at 2933.20 cm-1 and 2863.77 cm-1

were due to the stretching vibration of –CH3 and –CH2 respectively. The absorption

peak of 1673.91 cm-1 was attributed to the stretching peak of C=O. The absorption

peak of 1544.70 cm-1 was due to the stretching vibration of C-N, while 1201.43 cm-1

was attributed to C-O-C. Moreover, absorption peaks of 1112.72 cm-1 and 1041.37

cm-1 were according to the bending vibration of -SO3-. Results mentioned above were

6
consistent with the chemical structure of SJ-1 shown in scheme 1.

The molecular weight and its distribution of SJ-1 was synthesized under the best

optimum synthesis condition mentioned in 2.2. The result showed that the weight

average molecular weight was 8.1×105, and the number average molecular was 6.2×

105. Thus, the molecular weight distribution coefficient is 1.29. These all meet the

technical requirements for oilfield application [19].

3.2 Effect of concentration of SJ-1 on the properties of drilling fluid

Different concentration of SJ-1 was added to the freshwater base mud. The

rheological and API fluid loss properties have been measured by rotational viscometer

and medium-pressure filtration apparatus respectively. The results were shown in

Table 1.

According to Table 1, with the increase of loading of SJ-1, the API fluid loss of

drilling fluid decreased obviously. When the concentration of SJ-1 was or ever than

1.2 wt%, the values of fluid loss became stable. At the same time, the rheological

property of drilling fluid changed as the increase of polymer concentration. SJ-1

contributes to build up the network structure, which results in a viscosity-building

ability. If the rheological property of drilling fluid was bad, thinner might be required

for the drilling fluid, so the optimum concentration of fluid loss addictive SJ-1 in the

freshwater base mud was 1.2 wt%.

7
3.3 Evaluation of temperature resistance

1.2 wt% SJ-1 was added to the freshwater base mud, then, rolling 16h by

frequency conversion rolling oven at different aging temperatures. The rheological

and API fluid loss have been measured by rotational viscometer and medium-pressure

filtration apparatus respectively. The results were shown in Table 2.

The value of API fluid loss of drilling fluid raised with the increase of

temperature, when the concentration of SJ-1 was equal to 1.2 wt%. The API fluid loss

of drilling fluid was still below 13 mL even at 220oC showing its property of

temperature resistant. Three reasons account for this phenomenon: firstly, the main

chain of the polymeric molecule is connected by C-C, which is stable at high

temperatures. Secondly, the -SO3- of the AMPS has a strong temperature resistance

performance, introducing the -SO3- into the polymer molecule can significantly

improve the property of temperature resistance. Lastly, APEG molecule contains a

polyoxyethylene group, which can improve the hydrophilic property and the

adsorption capacity of the SJ-1 at high temperatures.

With the increase of temperature, the rheological property of drilling fluid which

reflected on apparent viscosity, plastic viscosity and yield value decreased. Some of

the SJ-1 was degraded at high temperature, which can lead to breaking up the network

structure to a certain extent. But these negative influence held within limits and

control. The little change on the performance of the drilling fluid was less affected.

8
3.4 Evaluation of salt tolerance

3.4.1 The effect of NaCl at 120 oC

1.2 wt% SJ-1 and different concentration of NaCl were added to the freshwater

base mud, then, aged 16 h at 120oC. The rheological and API fluid loss have been

measured by rotational viscometer and medium-pressure filtration apparatus

respectively. The results were shown in Table 3.

Table 3 illustrated that the API fluid loss of drilling fluid decreased gradually by

the growing concentration of NaCl in the mud system. When the salt concentration

was 30 wt%, the fluid loss achieved the lowest, namely 7.5mL, which indicated the

good salt tolerance of SJ-1.

Five reasons account for this phenomenon: Firstly, when the NaCl was added to

the freshwater base mud, the value of the Zeta electric potential of the clay particles

would decrease and the hydration shell would be reduced, which would lead to

generate the flocculated structure in the freshwater base mud. So, the API filter loss

increases. Secondly, when the NaCl was added to the freshwater base mud, the

adsorption of the fluid loss additive on the surface of the clay particles would increase,

which would lead to the Zeta electric potential of the clay particles increase and the

hydration shell thicken. So, the API filter loss would decrease. When the

concentration of the NaCl was 2 wt%, the effect of the NaCl on the clay particles

played a leading role, and the API filter loss was increase. Meanwhile, with the

increase of the concentration of the NaCl, the effect of the NaCl on the fluid loss

9
additive was increased and the API filter loss was decrease. When the concentration

of the NaCl was 25 wt%, the effect of the NaCl on the fluid loss additive played a

leading role, so the API filter loss was lower than that without the NaCl. Thirdly, the

SJ-1 with good temperature resistant remains at a comparatively high level. And it is

benefit for adsorbing clay particles and free water to form aggregate, which form a

thin and dense mud cake on the wall. The appearance of mud cake effectively

reducing the filtrate loss. Lastly, because of the adding of fluid loss additive SJ-1, the

hydrophilic radical of this treating chemical mainly include sulfonic acid and

polyoxyethylene side chain which enjoy a favorable hydrophilicity and good

solubility in a saline environment. It can bring enough hydrated film to clay and

ensure the drilling fluid system has good salt tolerance.

3.4.2 The effect of CaCl2 at 120oC

1.2 wt% SJ-1 and different concentration of CaCl2 were added to the freshwater

base mud, then, aged 16 h at 120oC. The rheological and filtration properties have

been measured by rotational viscometer and medium-pressure filtration apparatus

respectively. The results have shown in Table 4.

Table 4 illustrated that the fluid loss of drilling fluid decreased gradually by the

growing number of CaCl2 in the mud system. When the CaCl2 was 8%, the fluid loss

comparatively lower 12.6 ml; however, the API fluid loss remain unchanged by the

raising of CaCl2. When the CaCl2 was 10%, the API fluid loss was 12.0ml.

Two reasons account for this phenomenon: Firstly, the -SO3- of the SJ-1

10
molecular chain has strong hydration capacity, and the hydration of the clay particles

can be thickened. Meanwhile, the -SO3- and the calcium do not occur the precipitation

reaction in the drilling fluid containing calcium ions. So the SJ-1 can form a thick

hydration shell on surface of clay, which can ensure the SJ-1 has good fluid loss

performance in the drilling fluid containing calcium ions. Secondly, because of

the-SO3-, the SJ-1 can resist a temperature of 120oC in which polymer rarely degrade

or degrade in a small quantity, the original nature of many polymer molecules can be

maintained, and they can adsorb clay particles and free water, forming an aggregate

that acts as a thin and dense mud cake on the borehole wall, which effectively reduces

the leakage of filtrate into formation.

3.5 Zeta Electric Potential Test

1.2 wt% SJ-1 was added to the freshwater base mud at 120oC. The Zeta electric

potential and API filter loss have been measured by Zeta potential analyzer and

medium-pressure filtration apparatus respectively. The results were shown in the

following Fig. 2.

Fig. 2 shows that in different temperatures, both drilling fluid system and Zeta

electric potential have a big change. The absolute value of the Zeta electric potential

of the mud system gradually decreased with the increase of aging temperature, and the

filter loss is gradually increase with the increase of experimental temperatures. It

means that with the increase of aging temperatures, the character of mud system

changes a lot, in which the absorption capacity of polymers on the surface of clay

11
particles is reducing, leading to the increase of filter loss of mud. However, because

the SJ-1 contains many -SO3- and side chain polyoxyethylene ether (C2H4O)n, which

exhibits unique and hydration and dispersion capacities at high temperature, the

negative influence held within limits. The Zeta electric potential test shows that this

mud system still has a good dispersion stability in high temperature.

1.2 wt% SJ-1 and different concentration of NaCl were added to the freshwater

base mud at 25oC. The Zeta electric potential and API filter loss have been measured

by Zeta potential analyzer and medium-pressure filtration apparatus respectively. The

results were shown in the following Fig. 3.

Fig. 3 shows that with an increase of NaC1, filter loss is decreasing, along with

the absolute value of Zeta electric potential rising up, which is compatible with the

data of Zeta electric potential test. With the increase of electrolyte, the coalescence of

electrolyte is gradually gentle, and the aggregation of clay particles in drilling fluid is

impeded, resulting in the increase of the small particles in the mud with the expansion

of the degree of mineralization. At the same time, SJ-1 particles is adsorbed on the

surface of clay particles; sulfonic acid group can chemically react to Na+ and Ca2+ in

salt; the steric of polyoxyethylene side chain in particles is large. Thus, it is more

difficult to aggregate clay particles, and the compression of salt on the electric double

layer is reduced, with the improvement of the resistance of fluid loss additive to salt.

In addition, with the increase of polymer, both apparent and plastic viscosities are

increasing to a small extent.

12
3.6 SEM analysis of filter cake

In order to explore the microstrcuture of the filter cake formation and the

filtration mechanism research, the formation of the filter cake was observed by type

JSM7500F SEM.

Fresh water base mud and polymers of 1.2 wt% density are added into drilling

fluid to test the API filter loss in normal temperature. After drying, the appearance of

filter cake can be seen through SEM in following Fig. 4:

Fig. 4 (a) shows that the surface of the base mud is uneven and friable, with

some ravines and small poles. Some big particles can be seen, so the mud is bad in

dispersion and the cake formed is of a poor quality, causing a terrible dehydration.

Fig. 4 (b) shows that after an aging process, the cakes are uniform and dense on

their surfaces, with no big pores and coarse particles. Polymers adsorb into clay

particles, forming a reticulated polymer, which effectively blocks the pore of borehole

wall and prevents the filtrate in the drilling fluid leaking to formation. Thus, the

drilling fluid is presented to be in good character, and the filtrate loss is less than base

mud. Then, hydration swelling and dispersion of shale is decreasing, which can better

avoid borehole wall collapsing to protect reservoir.

Fresh water base mud polymers of 1.2% density are added into fresh water base

mud, which is then stirred up speedily for 10 minutes. Next, NaC1 is mixed into it and

then stirred up for 10 minutes. API filtrate loss is tested and the Fig. 5 shows the SEM

images of the filter cake:

Fig. 5 (a) shows that the filter cakes, with NaCl of 30% density added into the

13
mud system mixed with the fluid loss additive, are dense on their surfaces, and

distributed regularly in tight connection, narrowing the pores for less filtration loss. It

means that filtration loss of drilling fluid can be effectively reduced by adding a large

quantity of NaCl into drilling fluid system. The polyoxyethylene side chain in the

fluid loss additive raise the resistance of polymers to salt, and its plastic-protection

function impede the coalescence of NaCl to clay particles, contributing to the regular

distribution of clay particles in the drilling fluid system. Thus, the cake formed is

dense.

Fig. 5 (b) shows that the cakes, with NaCl of 30% density added into the mud

system mixed with the fluid loss additive aging 30 min at 120oC, are dense and

smooth on their surfaces, and distributed regularly in tight connection, narrowing the

pores of filtrate loss.

4. CONCLUSIONS

With FTIR analysis, the composition of the synthetic polymer SJ-1 was

consistent to the designed structure. The weight average molecular weight of SJ-1 was

8.1×105, and its number average molecular was 6.2×105. The molecular weight

distribution coefficient was 1.29. The character evaluation proves that the best amount

of SJ-1 in the mud is 1.2%, and the API filtrate loss is 9.2 mL. Salt-resistance of SJ-1

is effective and keep its effectiveness in the drilling fluid system in which the aging

temperature is 220oC, the mass density of NaCl is 30 wt%, and CaCl2 10 wt%. The

Zeta electric potential test on clay particles proves that with an increase of SJ-1, the

14
API filtrate loss in drilling fluid is decreasing and the absolute value of Zeta electric

potential is increase. Hydrated membrane is thickened by the increase of the density

of negative charge of clay particles, contributing to the reduction of filtrate loss of

drilling fluid. In addition, the SEM analysis proves that cakes with SJ-1 added in is

even and dense on their surfaces with no big pores or coarse particles, and the filtrate

loss is less than base mud. Besides, those cakes can effectively resist to the pollution

of electrolytes. And in the mud system with NaCl of 30% density, the cakes formed

are distributed regularly in tight connection, narrowing the filtrate loss pores and

reducing the amount of filtrate loss.

ACKNOWLEDGE

The authors thank the Engineering Research Center of Oilfield Chemistry,

Ministry of Education Key for experiment condition support.

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Indication of figures and tables

Scheme 1. Chemical structure of SJ-1.

Table 1. Relationship between SJ-1 concentration and fluid loss.

Table 2. Fluid loss of drilling fluid changed with aging temperature and polymer
concentration.

Table 3. Performance evaluation of salt resistance of drilling fluid at high

temperature.

Table 4. Performance evaluation of calcium resistance of drilling fluid under high

temperature.

Fig. 1. FTIR spectrum of polymerization product.

Fig. 2. The impact of Zeta Electric Potential and API filter loss on mud system in
different temperatures.

Fig. 3. The impact of Zeta Electric Potential and API filter loss on mud system in
different salt contents.

Fig. 4. SEM photos of (a) API filter cake formed by base mud. (b) API filter cake
modified with SJ-1 (both of aging temperature 120oC).

Fig. 5. SEM photos of (a) API filter cake formed by base mud + SJ-1 + 30 wt% NaCl.
(b) API filter cake formed by base mud + SJ-1 + 30 wt% NaCl after the aging process
of 30 min.

18
Table 1. Relationship between SJ-1 concentration and fluid loss.

SJ-1
AV PV YP API filter loss
concentration
/mPa·s /mPa·s /Pa /mL
/wt%
0.0 12.5 7.0 5.62 23.0
0.1 16.0 10.0 6.13 11.8
0.3 19.5 13.0 6.64 11.2
0.6 23.5 16.0 7.67 10.4
0.9 30.0 21.0 9.20 9.4
1.2 37.0 26.0 11.24 9.2
1.5 44.0 31.0 13.29 9.2
1.8 52.5 36.0 16.86 9.1

Table 2. Fluid loss of drilling fluid changed with aging temperature

Experimental AV PV YP API filter loss

conditions /mPa·s /mPa·s /Pa /mL
120oC，16h 43.5 34.5 9.20 10.6
140oC，16h 38.5 32.0 6.64 10.6
160oC，16h 20.8 17.0 3.83 11.5
180oC，16h 13.0 9.5 3.58 12.1
200oC，16h 13.0 11.0 2.04 12.5
220oC，16h 12.5 11.0 1.53 13.0

19
Table 3. Performance evaluation of salt resistance of drilling fluid at high

temperature.

NaCl
Experimental AV/mPa· API filter loss
concentration PV/mPa·s YP/Pa
conditions s /mL
/wt%
0.0 32.0 27.5 4.60 10.6
2.0 20.0 17.5 2.56 16.0
5.0 17.5 15.0 2.56 13.0
Aging
temperature 10.0 18.0 16.0 2.04 12.6
120oC, aging 15.0 17.0 15.0 2.04 12.6
time 16h
20.0 17.0 15.0 2.04 12.6
25.0 17.5 15.0 2.56 10.4
30.0 19.5 18.0 1.53 7.5

Table 4. Performance evaluation of calcium resistance of drilling fluid under high

temperature.

CaCl2
Experimental AV PV YP API filter loss
concentration
conditions /mPa·s /mPa·s /Pa /mL
/wt%
0.0 32.0 27.5 4.60 10.6
2.0 9.5 9.0 0.51 26.0
Aging
temperature 4.0 10.0 9.0 1.02 19.0
120oC, aging 6.0 9.0 8.0 1.02 17.0
time 16h
8.0 8.5 8.0 0.51 12.6
10.0 8.5 8.0 0.51 12.0

20
 Scheme 1. Chemical structure of SJ-1.

Fig. 1. FT-IR spectrum of polymerization product.

21
Fig. 2. The impact of Zeta Electric Potential and API filter loss on mud system in

different temperatures.

Fig. 3. The impact of Zeta Electric Potential and API filter loss on mud system in
different salt contents.

22
 (a) (b)

Fig. 4. SEM photos of (a) API filter cake formed by base mud. (b) API filter cake
modified with SJ-1 (both at the aging temperature 120oC).

(a) (b)

Fig. 5. SEM photos of (a) API filter cake formed by base mud + SJ-1 + 30 wt% NaCl.
(b) API filter cake formed by base mud + SJ-1 + 30 wt% NaCl after the aging process
of 30 min.

23