PETROLEUM EXPLORATION AND DEVELOPMENT

Volume 45, Issue 4, August 2018

Online English edition of the Chinese language journal

Cite this article as: PETROL. EXPLOR. DEVELOP., 2018, 45(4): 764–769. RESEARCH PAPER

Development of key additives for organoclay-free oil-based

drilling mud and system performance evaluation
SUN Jinsheng1, 2, *, HUANG Xianbin2, JIANG Guancheng3, LYU Kaihe2, LIU Jingping2, DAI Zhiwen2
1. CNPC Engineering Technology R & D Company Limited, Beijing 102206, China;
2. School of Petroleum Engineering, China University of Petroleum, Qingdao 266580, China;
3. School of Petroleum Engineering, China University of Petroleum (Beijing), Beijing 102249, China

Abstract: Traditional oil-based drilling muds (OBMs) have a relatively high solid content, which is detrimental to penetration rate in-
crease and reservoir protection. Aimed at solving this problem, an organoclay-free OBM system was studied, the synthesis methods and
functioning mechanism of key additives were introduced, and performance evaluation of the system was performed. The rheology modi-
fier was prepared by reacting a dimer fatty acid with diethanolamine, the primary emulsifier was made by oxidation and addition reaction
of fatty acids, the secondary emulsifier was made by amidation of a fatty acid, and finally the fluid loss additive of water-soluble acrylic
resin was synthesized by introducing acrylic acid into styrene/butyl acrylate polymerization. The rheology modifier could enhance the at-
traction between droplets, particles in the emulsion via intermolecular hydrogen bonding and improve the shear stress by forming a
three-dimensional network structure in the emulsion. Lab experimental results show that the organoclay-free OBM could tolerate tem-
peratures up to 220 C and HTHP filtration is less than 5 mL. Compared with the traditional OBMs, the organoclay-free OBM has low
plastic viscosity, high shear stress, high ratio of dynamic shear force to plastic viscosity and high permeability recovery, which are bene-
ficial to penetration rate increase, hole cleaning and reservoir protection.

Key words: organoclay-free; oil-based drilling mud; rheology modifier; emulsifier; fluid loss reducer; weak gel; reservoir protection

Introduction bling a high rate of penetration and a good reservoirs protec-

[1]
Traditional oil-based drilling muds (OBMs) use organoclay
as thickening agents and blown asphalt or organic lignite to
reduce fluid loss, which have played an important role in the
development of drilling engineering and are still widely used
today in drilling complex, deep and ultra-deep formations and
complex structural wells. However, traditional OBMs have
some limitations. For example, colloidal particles of organo-
clay and blown asphalt have negative influence on the rate of
penetration[23]. After aging, organoclay and blown asphalt are
likely to cause the drilling fluids to thicken. Colloidal particles
can become pollutants in reservoirs. The drilling fluid is dif-
ficult to increase to high density at high colloidal content.
Thus, OBMs with low colloidal content are widely used[4].
However, low colloidal content reduces the shear stress of
OBMs, resulting in a poor cleaning effect[57].
Organoclay-free OBM has the following advantages com-
pared to traditional OBMs: excellent rheological properties,
unique shear stress structure, strong thixotropy[6, 8] and good
shear shinning properties; Organoclay-free OBM does not use
colloidal components such as organoclay and asphalts, ena-
tion performance. Therefore, organoclay-free OBM is benefi-
cial for efficient exploitation of oil and gas resources and has
become an important direction of drilling fluid development
in the future.
The study of organoclay-free OBM systems and additives
have been undertaken for some time worldwide, but only re-
cently in China. The organoclay-free OBMs, developed by
Halliburton and other companies, have superior rheology and
reservoir protection performance and good field application
effects[9]. However, the functional mechanism of organo-
clay-free OBM is not well understood, and there are only a
few studies reporting the additives, rheology modification
mechanism of the organoclay-free OBM and the drilling fluid
system. An organoclay-free OBM is described in this study,
the synthesis of key additives, functional mechanism and sys-
tem performance are also presented.
1. Key additives of organoclay-free OBM
Key additives of organoclay-free OBM include: rheological
modifier (RM), primary and secondary emulsifiers, and fil-

Received date: 28 Apr. 2018; Revised date: 31 May 2018.

* Corresponding author. E-mail: sunjsdri@cnpc.com.cn
Foundation item: Supported by the Basic Research Funds Reserved to State-run Universities (18CX02171A, 18CX02033A).
Copyright © 2018, Research Institute of Petroleum Exploration & Development, PetroChina. Publishing Services provided by Elsevier B.V. on behalf of KeAi Com-
munications Co., Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
 SUN Jinsheng et al. / Petroleum Exploration and Development, 2018, 45(4): 764–769

trate reducer. Among them, RM is the main additive.
1.1. Rheological modifier (RM)
1.1.1. Synthesis of RM
The RM is high in viscosity due to the intermolecular hy-
drogen bonding between fatty acid dimers and suitable to be
used as the rheological modifier for OBMs. However, RM has
poor hydrophilicity. In this study, diethanolamine was used
for the amidation of RM to increase its hydrophilicity. The
reaction is shown in equation (1). The hydrophilicity of the
fatty acid dimer is expected to increase with the addition of
amide groups according to hydrophile-lipophile balance (HLB)
theory. Theoretically, hydrophilicity of the fatty acid dimer
can be also enhanced using saponification of the fatty acid
with a strong base. However, the internal phase of the OBM
generally is high concentration brine, which reduces the hy-
drophilic effect of the fatty acid salt. The HLB was estimated
by Davies base method in this study. HLB base values of the
hydrophilic functional groups—COOK+, —COONa+, R3N(ter-
tiary amine), —COOH, —OH and —O— are 21.1, 19.1,
9.4, 2.1, 1.9 and 1.3, respectively[10].
Detailed synthesis process of RM is: fatty acid dimer and
diethanolamine were mixed at the ratio of 1:2.05 (molecular
fraction) and placed into a four-necked flask. An electric
mixer, condenser and reflux apparatus and dean stark trap
were attached to the flask and nitrogen was injected into the
mixture for 10 min before the reaction was started. The mix-
ture was heated by oil bath quickly to the reaction temperature
of 175 C to react for 4 hours. During the reaction process,
water in the dean stark trap was removed in time. At the
end of the reaction, the brown thick fluid produced was the
RM.

1.1.2. Effects of RM dosage on emulsion modulus is shown in Fig. 2. Stable emulsion can be formed in the OBM,
# thanks to the synergetic effect of the primary and secondary
An emulsion with an oil-water ratio of 85:15 (5 white oil:
emulsifiers. With an amphiphilic structure, RM can adsorb
water) and 3% (wt/V) of emulsifier SPAN-80 was prepared
onto the oil-water interface. Due to the solubilization of the
using a shearing mixer. Dynamic frequency of the emulsion
emulsifier on the oil-water interface, the concentration of RM
was scanned using a Haake MARS III rheometer in cone plate
mode to test the storage modulus (G') and loss modulus (G'')
of the emulsion. The frequency scanning range was 0.1 to 10
s1 and test temperature was held at 25 C and shear stress was
maintained at a constant 0.1 Pa.
Experimental results are shown in Fig. 1. It can be seen
pure emulsion has a higher G'' compared to G' within the fre-
quency range used in this study. This means the emulsion
mainly has viscous deformation and is in liquid state. After
RM is added, G' is higher than G'', indicating that the emul-
sion would change from a liquid state into a “gel state”. When
the RM concentration is lower than 3 g/L, G' increases with
the increase of RM concentration, but reduces when the con-
centration of RM is greater than 3 g/L. This could be because
the interaction force between the emulsion droplets is overly
large, leading to unstable flocculation of the emulsion and
reduction of G'.
It is reported in the literature [11] that, with the increase of
structural force in an emulsion, the influence of frequency on
G' decreases over time, i.e., the slope of a G' curve decreases.
It can be seen in Fig. 1(a) that the slope of the G' curve de-
creases gradually with the increase of RM content. This indi-
cates that the interaction force in the emulsion increases with
the increase of RM concentration.

1.1.3. Functional mechanism of RM

Fig. 1. Effect of rheological modifier (RM) concentration on
The functional mechanism of RM in organoclay-free OBM storage modulus (a) and loss modulus (b) of the emulsion.
 765 
 SUN Jinsheng et al. / Petroleum Exploration and Development, 2018, 45(4): 764–769
Fig. 2. Functional mechanism of rheological modifier (RM).
increases at the oil-water interface. Due to hydrogen bonding
between the RM molecules, RM would form a “film” at the
oil-water interface. On one hand, RM accumulation on the
interface strengthens the interface film, which is conducive to
the stability of the emulsion. On the other hand, the hydrogen
bonding between RM adsorbed on different water droplets
enhances the droplet-droplet interaction force in the emulsion.
There are hydroxy groups on particle surfaces, e.g. water-
borne acrylic resin filtrate reducer, calcium carbonate super-
fine powder and barite. In drilling fluid, RM can not only
adhere to the oil-water interface, but also the solid-liquid in-
terface due to the hydrogen bonding effect. This can streng-
then droplet-droplet, droplet-particle and particle-particle in-
teractions, thus forming a 3D network structure connected by
weak interactions in the emulsion (weak gel structure)[8], en-
hancing the structural force of the emulsion to serve as shear
stress.
Within the appropriate concentration (03 g/L), RM can
increase emulsion structural force and stability. However,
flocculation occurs when the RM concentration is too high,
which reduces emulsion stability and emulsion structural
force.
1.2. High temperature resistant emulsifier
1.2.1. Design principle of emulsifier resistant to high
temperatures
Appropriate HLB value: Emulsifiers are the base to main-
tain emulsion stability and improve other properties of OBM.
To form stable oil-in-water emulsion, the emulsifier must be
hydrophilic and lipophilic, and be hydrophilic and lipophilic
balance under certain conditions. For nonionic emulsifiers, the
HLB value generally ranges between 3.0 and 6.0. The perfor-
mance of an ionic emulsifier is highly sensitive to water salin-
ity. For ionic emulsifiers with specific HLB values, the hy-
drophilic interaction of the emulsifier decreases gradually
with the increase of water salinity. In OBM, two different
emulsifiers (primary and secondary emulsifiers) are generally
used to form the dense composite membrane[12] to achieve the
best emulsification effect. The primary emulsifier is generally
a fatty acid or modified fatty acid with a lower HLB value.
The secondary emulsifier has a higher HLB value, which can
stabilize the emulsion and also wet the solid phase.
Strong interaction forces at the lipophilic and hydrophilic
 766 
ends: the molecular structure of the emulsifier must tolerate
high temperatures. In addition, the emulsifier should have
strong interactions with both oil and water phases at the inter-
face. Therefore, high-temperature stability requires strong
hydrophilic and lipophilic groups (generally hydrophobic
groups of similar carbon chain length as the oil phase) in
emulsifiers.
1.2.2. Primary emulsifier
In this study, the primary emulsifier was obtained from the
reaction of fatty acid and maleic anhydride. The synthesis
method is reported in reference [13]. The hydrophilic groups
are carboxylic acids and the hydrophobic groups are long
chain fatty acids. The bivalent soap salt generated by the reac-
tion between the carboxylic acid groups and CaO in the OBM
not only has strong hydrophilic property but also increases
emulsion stability based on the directional wedge theory [14].
1.2.3. Secondary emulsifier
The secondary emulsifier in this drilling fluid is a fatty acid
amide. The hydrophilic group is the amide group and the hy-
drophobic group is the long chain fatty acid. Its synthesis
principles are: Step 1: partial amidation products are gener-
ated through the amidation of fatty acid polyamines and fatty
acids. Step 2: the partial amidation products react with diacid
to amidate the primary amine groups completely and generate
the secondary emulsifier of fatty acid amides.
1.2.4. Evaluation of high temperature emulsion
performance
The following OBM was prepared: base fluid of 5# white
oil and 30% CaCl2 aqueous solution at the ratio of 85:15 + 1%
organoclay + 1% primary emulsifier + 3% secondary emulsi-
fier + 3% CaO. The OBM was stirred at a rate of 5 000 r/min
for 30 min. The prepared OBM was placed into a roller fur-
nace for high-temperature aging. The roller furnace tempera-
tures were set at 150 C, 180 C and 220 C respectively. At
the end of the aging process, the mixture was stirred for 2 min
at a rate of 5 000 r/min. An electrical stability tester was used
to test the electrical stability (ES) of the drilling fluid. Fig. 3
shows the emulsion formed using the primary and secondary
emulsifiers has a high ES after high-temperature aging. It is
superior to SPAN-80 and ONEMUL in high-temperature
emulsification performance.
1.3. Waterborne acrylic resin filtrate reducer
1.3.1. Synthesis of filtrate reducer
Under high temperature conditions, without filtrate reduc-
ers like organoclay, asphalt or lignite, it would be difficult to
reduce fluid loss. But modified asphalt and organoclay are
lipophilic colloids, which would increase the viscosity of the
drilling fluid, and thus reduce rate of penetration. A water-
borne acrylic resin with strong hydrophilic property has been
developed by introducing hydrophilic monomer acrylic acid
 SUN Jinsheng et al. / Petroleum Exploration and Development, 2018, 45(4): 764–769
Fig. 3. Comparison of high-temperature emulsification per-
formance of different emulsifiers.
into the emulsion polymerization of styrene and butyl acrylate.
The chemical structure is shown in Fig. 4a. The water-phase
contact angle of the pure styrene acrylic resin is relatively
large. However, the contact angle of distilled water on the
developed waterborne acrylic resin pressed pill decreases to
121° (Fig. 4b). The lipophilicity of waterborne acrylic resin is
stronger than the hydrophilic property and the majority of the
resin particles in the emulsion is in the oil phase, resulting in
the bending of the oil-water interface. This increases emulsion
stability[15]. The glass transition temperature of the developed
waterborne acrylic resin is 103 C. When the ambient tem-
perature is higher the glass transition temperature, the water-
borne acrylic resin is in the rubber state, which is beneficial to
plugging of the formation pores. In addition, the waterborne
acrylic resin type materials generally have a film-forming
property, which is conducive to the formation of compact
filter cake to reduce fluid loss.
Fig. 4. Structure of waterborne acrylic resin (a) and its contact
angle with distilled water (b).
 767 
1.3.2. High-temperature performance of the fluid loss
reducer
The following drilling fluid was prepared to evaluate the
performance of the filtrate reducer: base fluid of 5# white oil
and 30% CaCl2 aqueous solution at the ratio of 85:15+ 1%
organoclay + 1% primary emulsifier + 3% secondary emulsi-
fier + 3% CaO + barite (ρ = 1.5 g/cm3).
API filter loss (FLAPI) and high-temperature high-pressure
(HTHP) filter loss (FLHTHP) of the drilling fluid after aging at
the high temperature of 220 C for 16h are shown in Table 1.
The HTHP filter loss was measured at 180 C and 3.5 MPa.
Apparently, the commonly used fluid loss reducers like oxi-
dized asphalt and organic lignite aren’t suitable for the or-
ganoclay-free environment with high filtration loss, failing to
meet the requirements of drilling engineering. The synthe-
sized polymer fluid loss reducer presented in this paper has
excellent filtration reduction performance, with a HTHP fil-
tration loss of less than 5 mL.
2. Development and performance evaluation of
organoclay-free OBMs
2.1. Selection of base oil, additives and system formula
The 5# white oil wa taken as the base oil. Firstly, the 5#
white oil has high flash and ignition points, which can ensure
the safety of the drilling process. Secondly, the aniline point
of the base oil should be higher than 60 C under general con-
ditions, and the 5# white oil has a high aniline point which can
cause little damage to the rubber parts of the drilling machin-
ery. Thirdly, the 5# white oil has appropriate viscosity, which
is beneficial for rheology control. Fourthly, the 5# white oil
has low toxicity, making it environmentally friendly.
The wetting agent is used to reverse the wettability of barite
surface, to change the hydrophilic surface into a lipophilic
surface, and thus enhance dispersion of barite in the OBM.
The wetting agent can influence the filter loss of OBM con-
siderably. With poor wettability, barite can easily precipitate,
and the weighted drilling fluid has high filter loss. Lecithin is
a natural surfactant, with HLB ranging between 7.5 and 8.0[16].
It has excellent emulsification, scattering and wetting proper-
ties. Therefore, lecithin was chosen as the wetting agent.
To block the formation pores of different sizes, two kinds of
superfine calcium carbonate powders with different sizes (25
μm (500-mesh) and 6.5 μm (2 000-mesh)) were used as plug-
ging materials.
Table 1. Comparison of performance of different filtrate re-
ducers for OBM.
High-temperat
API filter ure
Type of filtrate reducers
loss/mL high-pressure
filter loss/mL
3% organic lignite 7.2 40.8
3% blown asphalt 7.0 26.4
3% organic lignite + 3% blown asphalt 6.4 16.8
2% waterborne acrylic resin 3.4 4.4
 SUN Jinsheng et al. / Petroleum Exploration and Development, 2018, 45(4): 764–769

Table 2. Comparison of organoclay-free OBMs and traditional OBMs.

Plastic Yield High-temperature
Apparent Gel Electrical
viscos- point YP/PV/ high-pressure
Type Condition viscosity/ strength stability/
(Pa·(mPa·s) 1)
-
ity (PV)/ (YP)/ filter loss/
(mPa·s) /Pa V
(mPa·s) Pa·(mPa·s) mL
Before aging 78.5 72 6.64 0.092 2.0/3.5 - 891
Traditional OBM
After aging 91.0 85 6.13 0.072 2.5/3.5 8.6 482
Before aging 62.0 50 12.26 0.245 5.5/7.0 - 1426
Organoclay-free OBM
After aging 55.0 45 10.22 0.227 5.0/6.5 4.2 706

Table 3. Comparison of permeability recovery of cores polluted the same density, organoclay-free OBM containing no colloi-
by the organoclay-free OBM and the traditional OBM. dal solid phase has lower viscosity, which is good for increas-
Initial Permeability Permeability ing the rate of penetration. The traditional OBM has high vis-
Drilling
permeability/ after pollution/ recovery/ cosity before and after aging, which has negative effect on
fluid type
103 µm2 103 µm2 % increasing rate of penetration. Besides, the organoclay-free
72.3 68.2 94.3 OBM has higher yield point, gel strength and higher ratio of
Organoclay-
96.2 92.5 96.2 yield point to plastic viscosity before and after aging than
free OBM
65.1 62.7 96.3 traditional OBMs, which is conducive to cutting-carrying.
86.8 79.8 91.9
Traditional 2.2.2. Reservoir protection performance
87.2 81.2 93.1
OBM
76.2 68.2 89.5 Artificial cores 25 mm in diameter and 50 mm long with
the gas permeability of approximately 50  100 × 103 µm2
Under the same density, high-purity barite has a small im-
were used to test changes of gas permeability of the cores
pact on the viscosity of the drilling fluid, so in this study,
before and after polluted by the organoclay-free OBM and the
high-purity barite with a density of 4.3 g/cm3 was used as the
weighting agent. traditional OBM and compare their performance in reservoir
The following organoclay-free OBM formula was formed protection. Firstly, the initial gas permeability (K0) of the
through lab tests: base fluid (the volume ratio of 5# white oil cores was tested. Secondly, one surface of the man-made core
to 30% CaCl2 aqueous solution is 85:15) + 0.3% RM + 2 % was polluted for 2 h at 60 C and 3.5 MPa using a HTHP
primary emulsifier + 3% secondary emulsifier + 1.5% wetting drilling fluid dynamic damage device (JHMD-II type, Jinzhou
agent + 2% waterborne acrylic resin + 4% calcium carbonate Modern Petroleum Scientific Technology Company). Thirdly,
superfine powder (25 μm) + 4% calcium carbonate superfine the polluted surface was cut and the reverse gas permeability
powder (6.5 μm) + 4% CaO + barite (ρ = 2.2 g/cm3). of the polluted core (K1) was tested. Finally, the permeability
recovery was calculated using the experimental results. Three
2.2. Organoclay-free OBM performance parallel tests were carried out and the mean permeability re-
The rheological property, filtration property and reservoir covery was calculated.
protection property of the organoclay-free OBM were tested, As shown in Table 3, the mean permeability recovery of
and compared with those of traditional OBM with organoclay. cores polluted by the organoclay-free OBM system is greater
The traditional OBM formula used was: base fluid (with the than 95%, while permeability recovery of the traditional OBM
volume ratio of 5# white oil to 30% CaCl2 aqueous solution of is lower than 92%. Therefore, although the traditional OBM
85:15) + 1.0% VGPLUS (organoclay) + 5% ONEMUL has fairly good reservoir protection performance, the organo-
(emulsifier) +1.5% VERSACOAT (wetting agent) + 4% clay-free OBM without organoclay and asphalt colloids can
VERSATROL (fluid loss reducer) + 0.5% SACKBLACK further reduce damage to the formation and has a better res-
(fluid loss reducer) + 4% CaO + barite (ρ = 2.2 g/cm3). ervoir protection performance.
2.2.1. Evaluation of general properties 3. Conclusions
Table 2 shows the general properties of the organoclay-free In this study, a kind of organoclay-free OBM system has
OBM and the traditional OBM before and after aging. The been developed, which contains four key additives (RM, pri-
aging was conducted at 220 C for 16 h. HTHP filter loss was mary emulsifier, secondary emulsifier and filtrate reducer).
tested under 180 C and 3.5 MPa. Rheological performance RM is a modified fatty acid that could replace organoclay in
was tested under 50 C. It can be seen that both OBMs can OBMs, which is prepared by the reaction between dimer acid
tolerate high temperatures up to 220 C, have ES of greater and diethanolamine. After RM is added, the storage modulus
than 400 V after aging and HTHP filter losses within the ac- of the emulsion increases significantly and the emulsion is in
ceptable range. However, compared with the traditional OBM, a “gel state”. The primary emulsifier is a modified fatty acid
the organoclay-free OBM has the following advantages: under and the secondary emulsifier is a fatty acid amide. Both pri-
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 SUN Jinsheng et al. / Petroleum Exploration and Development, 2018, 45(4): 764–769
mary and secondary emulsifiers have strong hydrophilic and
lipophilic groups, and excellent emulsion performance after
high-temperature aging, superior to similar commercial prod-
ucts made by foreign companies. The filtrate reducer is a kind
of waterborne acrylic resin with good emulsion stabilizing and
fluid loss reducing performance. It can control the HTHP fil-
ter loss in organoclay-free OBMs at less than 5 mL.
RM is the main additive. The functional mechanism of RM:
In organoclay-free OBMs, RM is adsorbed on the oil-water
interface and solid-liquid surface, strengthening the drop-
let-droplet, droplet-particle and particle-particle interactions in
the emulsion through hydrogen bonding, forming a 3D net-
work structure connected by weak interactions, thus strength-
ening the gel structure of the emulsion, improving the rheol-
ogy and stabilizing the performance of the emulsion.
Performance evaluation experiments show that compared
with the traditional OBMs, the organoclay-free OBM has low
plastic viscosity, high shear stress, high ratio of yield point to
plastic viscosity and high permeability recovery, which are
beneficial to penetration rate increase, hole cleaning and res-
ervoir protection.
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