Xiaodong Chen1, Xin Gao2, Junyu Chen3, Yunfeng Liu4, Chunyu Song5, Wenlei Liu6, Yuan Wan6, Xiangzheng Kong6, Ying Guan6, Zhengsong Qiu6, Hanyi Zhong6, Jinghua Yang7, Lifeng Cui1. 1. College of Smart Energy, Shanghai Jiao Tong University, Shanghai 200240, PR China. 2. Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430000, PR China. 3. Faculty of Geology, Lomonosov Moscow State University, Moscow 119991, Russia Federation. 4. Research Institute of Natural Gas Technology, Southwest Oil and Gas Field Company of PetroChina, Chengdu 610213, PR China. 5. School of Materials Science and Engineering, Dongguan University of Technology, Dongguan 523808, PR China. 6. School of Petroleum Engineering, China University of Petroleum (East China), Qingdao 266580, Shandong, PR China. 7. Faculty of Earth Resources, China University of Geosciences, Wuhan 430000, PR China.
Abstract
Aiming at the challenge that environmental protection and high-temperature fluid loss reduction performance of the traditional water-based drilling fluid treatment agent are difficult to balance, our studies added psyllium husk as a high-temperature-resistant and environmentally friendly filtrate reducer to a water-based drilling fluid. The composition, physical and chemical properties, and microstructure of psyllium husk are characterized. Then, the effects of psyllium husk after hot rolling at different temperatures on the rheological properties and fluid loss properties of bentonite-based slurry are evaluated. The results show that the psyllium husk added to the bentonite-based slurry can effectively improve the rheological properties and fluid loss properties of the bentonite-based slurry, and the temperature resistance can reach 160 °C. After hot rolling at 160 °C, adding 1 w/v % psyllium husk can reduce the API fluid loss and high-temperature and high-pressure fluid loss of the bentonite-based slurry by 76.04 and 56.91%, respectively, showing excellent fluid loss reduction performance at high temperatures. The branched structure and uronic acid of psyllium husk can inhibit the degradation of its own molecular structure to a certain extent, which is the fundamental reason why psyllium husk still has excellent fluid loss reduction performance at high temperatures. Psyllium husk is expected to replace some traditional synthetic polymers and be used in environmentally friendly high-temperature-resistant water-based drilling fluids.
Aiming at the challenge that environmental protection and high-temperature fluid loss reduction performance of the traditional water-based drilling fluid treatment agent are difficult to balance, our studies added psyllium husk as a high-temperature-resistant and environmentally friendly filtrate reducer to a water-based drilling fluid. The composition, physical and chemical properties, and microstructure of psyllium husk are characterized. Then, the effects of psyllium husk after hot rolling at different temperatures on the rheological properties and fluid loss properties of bentonite-based slurry are evaluated. The results show that the psyllium husk added to the bentonite-based slurry can effectively improve the rheological properties and fluid loss properties of the bentonite-based slurry, and the temperature resistance can reach 160 °C. After hot rolling at 160 °C, adding 1 w/v % psyllium husk can reduce the API fluid loss and high-temperature and high-pressure fluid loss of the bentonite-based slurry by 76.04 and 56.91%, respectively, showing excellent fluid loss reduction performance at high temperatures. The branched structure and uronic acid of psyllium husk can inhibit the degradation of its own molecular structure to a certain extent, which is the fundamental reason why psyllium husk still has excellent fluid loss reduction performance at high temperatures. Psyllium husk is expected to replace some traditional synthetic polymers and be used in environmentally friendly high-temperature-resistant water-based drilling fluids.
With the development of drilling engineering technology, the depth
of drilling is gradually increasing and the formation is becoming
more and more complex, which puts forward higher requirements on the
performance of the drilling fluid.[1−3] During the circulation
of the drilling fluid, the liquid phase will invade the formation
under the action of the pressure difference. At the same time, the
solid phase will form a thinner mud cake in the formation.[4−6] Multiple research studies have demonstrated that when the fluid
loss of the drilling fluid occurs, it will cause the shale formation
to hydrate and swell, which will induce the instability of the borehole
wall. When the fluid loss is large, a thicker mud cake will be produced,
which is prone to drilling accidents such as wear of drilling tools
and stuck drills.[6−8] When drilling into deep formations, the components
of the drilling fluid are prone to high-temperature degradation and
failure,[9] thus deteriorating the performance
of the drilling fluid[2,10] and triggering a series of downhole
complex accidents.[6] Therefore, the development
of high-temperature-resistant drilling fluid treatment agents, effective
control of the high-temperature filtration, and wall-building performance
of the drilling fluid has always been the research focus of deep well
and ultradeep well drilling engineering.Researchers synthesized
copolymers with acrylamide and heat-stable
monomers (such as 2-acrylamido-2-methylpropanesulfonate, N-vinylpyrrolidone, etc.).[11−14] The temperature resistance has exceeded 160 °C,
but it is also affected by the disapproval merits of the high expenditure,
harder manufacturing process, environmental protection issues, and
many other constraints.[15,16] Therefore, it remains
a big challenge to execute the research of anti-high-temperature filtration
reducers.With the increasingly stringent environmental regulations,
the
exploitation of green and environmentally friendly drilling fluid
treatment agents is of great significance for protecting the environment.
In recent years, researchers have carried out a lot of research and
developed a richer variety of environmentally friendly treatment agents.[17−19] Among them, because polysaccharide polymers have the advantages
of wide sources, low price, easy modification, and biodegradability,
they are extensively applied in drilling fluids to improve rheological
properties and fluid loss properties,[18,20] such as xanthan
gum, starch derivatives, cellulose derivatives, and so on. When the
hot rolling temperature is greater than 140 °C, it is susceptible
to oxidative decomposition or thermal degradation at high temperature,
leading to breakage of the molecular chain and losing the control
effect on the performance of the drilling fluid.[9−11,21]Psyllium is a plant in the genus Plantago, mainly from Iran and India,[22,23] which is typically
used in the medical field in some countries and has the ability to
lower cholesterol and promote intestinal peristalsis.[22,24,25] Meanwhile, benefiting from its
unique ability to absorb water, thicken, and form gels, it has also
been utilized in food production and drug transportation.[25,26] The main component of psyllium is highly branched arabinoxylan,
where the main chain structure is (1→4)-β-d-xylose
and the side chain is located at the position of C-3 and C-2,[26−28] which contains a small amount of uronic acid.[29] The presence of branched structures in polymer molecules
can effectively increase the steric hindrance of the molecular chain
and the rigidity of the main chain[30,31] and improve
the thermal stability of the polymer to a certain extent. It has been
reported that uronic acid has the function of the antioxidant properties,
which can availably inhibit the oxidative decomposition of polymers.[32,33] As the temperature increases, the molecular movement intensifies
and the oxidative decomposition rate of the polymer will increase.
The presence of uronic acid can preserve the polymer from the oxidative
decomposition at high temperatures, thereby enhancing the polymer’s
thermal stability performance.As psyllium husk is an easily
biodegradable treatment agent, this
article investigates the feasibility of applying it in drilling fluids.
First, the composition and structure of psyllium husk are characterized,
and then, the influence of psyllium husk on the rheology and fluid
loss of water-based drilling fluids is systematically evaluated, and
the mechanism of action through relevant analysis and testing methods
is carried out. At present, there is no report of the application
of natural polysaccharides in drilling fluids at 160 °C. This
study will provide a new perspective for the future selection of environmentally
friendly treatment agents. This is the highlight of this study.
Materials and Methods
Materials
Psyllium
husk is provided
by Xianchangyue Biotechnology Co., Ltd. Sodium-based bentonite for
the drilling fluid is provided by Shandong Huawei Bentonite Co., Ltd.,
which meets API standards. Na2CO3, NaCl, CaCl2, and absolute ethanol are all analytical reagents, provided
by Sinopharm Chemical Reagent Co., Ltd. All experimental reagents
have not been purified.
Composition Determination
of Psyllium Husk
The monosaccharide content of psyllium husk
was analyzed by GCMS,
which refers to Petal’s method.[33] The content of uronic acid was determined according to the method
of Blumenkrantz and Asboe-Hansen using d-glucuronic acid
as the standard.[34]
Water
Absorption Measurement
A total
of 1.00 g of psyllium husk was accurately weighed and placed in a
nonwoven bag. The nonwoven bag was soaked in deionized water to start
timing. Once the psyllium husk came in contact with deionized water,
the variation in bag weight was weighed and recorded after specific
time intervals. Before weighing, the bag was carefully taken out from
water and the excessive water was drained for 3 min. The relationship
between the water absorption quality of psyllium husk was tested at
20 °C with time.
Rheological Property Measurement
Psyllium husk of different qualities was added into 350 mL of deionized
water, stirred at 8000 rpm for 20 min, and tested for rheology using
an Anton Paar MCR72 at a temperature of 25 °C and a shear rate
of 0.1–1000 s–1.The power-law model
is used to fit the rheological data. The power-law model mainly describes
the exponential relationship between shear stress and shear rate.
The important parameters are the flow pattern index (n) and consistency coefficient (K). The fitting formula
is as followsA total of 14.0 g of sodium bentonite
and 0.7 g of Na2CO3 are added to 350 mL of deionized
water, stirred at
a high speed, and let it stand for 24 h in an airtight manner to obtain
bentonite-based slurry. Psyllium husk of different qualities was added
to the sodium bentonite-based slurry and placed in an aging tank to
hot rolling for a period of time to simulate the effect of high temperature
on the drilling fluid to evaluate the stability of the drilling fluid.
The rheological properties of the drilling fluid before and after
hot rolling were tested using a six-speed rotary viscometer.The ZNN-D6 six-speed rotational viscometer (Qingdao Haitongda)
was used to test the apparent viscosity (AV), plastic viscosity (PV),
and yield point (YP) of the drilling fluid. The calculation formula
is as follows
Filtration Property Measurement
Psyllium
husk of different qualities was added to the sodium bentonite-based
slurry, hot rolling was performed at different temperatures, and then
tested for API fluid loss using a ZNZ-D6 medium pressure filter loss
instrument. The API filter paper is used as the fluid loss medium,
and the fluid loss is 30 min under the condition of a pressure difference
of 0.7 MPa. High-temperature and high-pressure static fluid loss can
simulate the fluid loss of the drilling fluid downhole to a certain
extent. After hot rolling, the high-temperature and high-pressure
(HTHP) static filtration experiment is carried out. A GGS71-B (Qingdao
Haitongda) HTHP loss tester is used for the HTHP static filter loss
test. The test temperature is the corresponding hot rolling temperature,
the test pressure difference is 3.5 MPa, and the test time is 30 min.
The filtrate is collected by a graduated cylinder.
Biodegradability Evaluation
In terms
of toxicity, the concentration for 50% of maximal effect (EC50) was measured as the toxicity level based on the luminescent bacteria
method recommended by the National Standards of the People’s
Republic of China GB/T 15441-1995 (Water quality determination of
the acute toxicity-luminescent bacteria test).
Results and Discussion
Composition and Structure
of Psyllium Husk
The chemical composition of the psyllium
husk studied in this paper
is exhibited in Table . It can be concluded that xylose and arabinose have the highest
content and are the main components of psyllium husk. Noticeably,
psyllium husk also contains a certain concentration of uronic acid,
which can scavenge free radicals and exhibit excellent antioxidant
properties.[26,33]
Table 1
Composition
of Psyllium Husk
composition
relative content/(w/v %)
arabinose
21.4
xylose
75.4
galactose
1.6
glucose
0.6
rhamnose
0.3
uronic acid
0.7
The molecular structure of the psyllium husk is shown
in Figure . It is
a highly
branched arabinoxylan with the main chain structure of (1 →
4)-β-d-xylose, the side chain is located at C-3 and
C-2.[26−28] It has been demonstrated that the existence of the
branched chain structure is more beneficial to improve the rigidity
of the molecular main chain and the steric effect between branched
chains so as to improve the temperature resistance of polymers.[30,31] Meantime, its effective component of uronic acid can effectively
remove oxidation groups in polymers and inhibit the oxidative decomposition
of polymers. Accordingly, with the increase in temperature, the intensification
of molecular thermal motion and acceleration of the oxidative decomposition
rate of the polymer will be effectively inhibited due to the existence
of uronic acid.[26,33] At the same time, the degree
of the branched chain structure of the polymer will be further deepened
due to the breakage of its molecular chain by increasing temperature,
by inference, the rigidity of the molecular main chain continues to
improve, and the steric effect between branched chains also improves
the ability of the molecular chain to resist thermal decomposition.
Figure 1
Molecular
structure of the psyllium husk.
Molecular
structure of the psyllium husk.
Water Absorption
The change in water
absorption quality of psyllium husk with time is depicted in Figure . It can be seen
that with the prolonged water absorption time, the water absorption
quality of psyllium husk increases. When the water absorption time
is 1440 min, 1.0 g of plantain seed shell powder can adsorb 62.34
g of water molecules. At the same time, the water absorption rate
of the psyllium husk decreases with time, indicating that the psyllium
husk can adsorb a large number of water molecules in a short time.
When the water absorption time is 30 min, the psyllium husk can adsorb
33.16 g of water molecules. This is because the seed shell powder
of plantain is a branched polysaccharide, and its molecular branched
chain structure has a large number of hydrophilic groups, which can
adsorb a large number of water molecules. Meanwhile, the psyllium
husk after water absorption will form a hydration membrane to increase
the elasticity of the molecular chain, which is conducive to the formation
of compressible mud cake to reduce filtration.[35,36]
Figure 2
Relationship
between psyllium husk water absorption quality and
time at 20 °C.
Relationship
between psyllium husk water absorption quality and
time at 20 °C.
Microstructure
Characterization
The
1 w/v % psyllium husk deionized water suspension was freeze-dried
and observed with a scanning electron microscope, as shown in Figure . It can be concluded
that the molecular chains of psyllium husk are intertwined and connected
to form a sheet structure. Figure b shows a partially enlarged picture, it can be seen
that a large number of nanofibers are intertwined and connected to
construct a three-dimensional network structure.[37] These reticular structures come together to form a sheet
structure with gaps. Moreover, the pores in the three-dimensional
network structure are more conducive to the entry of water molecules
and form hydrogen bonds with the hydroxyl groups of psyllium husk,
showing good hydrophilic ability.
Figure 3
Scanning electron microscopy (SEM) images
of psyllium husk (a)
1000× and (b) 10,000×.
Scanning electron microscopy (SEM) images
of psyllium husk (a)
1000× and (b) 10,000×.Psyllium
husk of different qualities is added to the bentonite-based
slurry, and the rheological curve is shown in Figure . It can be concluded that the psyllium husk
suspension exhibits shear thinning. As the shear rate increases, the
viscosity of the psyllium husk suspension decreases with increase
in the shear stress. When the shear rate is low, the psyllium husk
will adsorb a large number of water molecules, increase the viscosity
of the drilling fluid, and help carry cuttings during the circulation
of the drilling fluid. As the shear rate increases, polymer molecules
move in the direction of flow, the aggregation of polymer chains decreases,
and the viscosity of the drilling fluid decreases which is more beneficial
to the drilling process.
Figure 4
Effect of concentration on rheological properties
of psyllium husk
solution.
Effect of concentration on rheological properties
of psyllium husk
solution.The power-law model is used to
fit the rheological curve. As shown
in Table , the suspension
of psyllium husk under different concentrations well-conforms to the
power-law model and R2 is more than 0.97.
The consistency coefficient tends to 1 with the increase in the concentration
of psyllium husk, indicating the corresponding increase in the viscosity
of the suspension.
Table 2
Rheological Parameters of the Power-Law
Model for a Psyllium Husk Suspension at Various Concentrations
concentration
of psyllium husk/(w/v %)
k/Pa sn
N
R2
0.1
0.000932
1.1632
0.991
0.5
0.004893
0.9197
0.9749
1.0
1.535028
0.4653
0.9897
1.5
7.162599
0.4437
0.9876
2.0
21.98374
0.4064
0.9893
The different qualities of psyllium husk are added
into the bentonite-based
slurry, hot rolling was performed at 160 °C for 16 h, and the
rheological parameters are shown in Figure . Before and after 160 °C hot rolling,
the viscosity of the base slurry increases with the amount of psyllium
husk increasing, and the apparent viscosity of the experimental slurry
changed little. After hot rolling at 160 °C, the apparent viscosity
of the base slurry is maintained at about 22 mPa s when the amount
of psyllium husk is 1.0 w/v %; when the dosage is further increased,
the apparent viscosity of the base slurry increases sharply to 80
mPa s, which is not conducive to the flow and pumping of the drilling
fluid. Therefore, the optimum dosage of psyllium husk is 1.0 w/v %
in a water-based drilling fluid.
Figure 5
Effect of psyllium husk on the viscosity
of bentonite-based slurry
before and after 160 °C hot rolling. (a) Apparent viscosity and
(b) yield point.
Effect of psyllium husk on the viscosity
of bentonite-based slurry
before and after 160 °C hot rolling. (a) Apparent viscosity and
(b) yield point.The high-temperature
stability of the drilling fluid is judged
by the rheological parameters after hot rolling at different temperatures,
as shown in Figure . It can be seen that with the increase in the hot rolling temperature,
the viscosity of the bentonite-based slurry decreases. Nevertheless,
after the addition of 1.0 w/v % psyllium husk, the apparent viscosity
first remains basically unchanged and then significantly decreases.
When the hot rolling temperature is lower than 160 °C, the viscosity
is basically maintained at about 25 mPa s. When the hot rolling temperature
is further increased to 180 °C, the viscosity rapidly decreases
to 8 mPa s, indicating that the molecular chain of the psyllium husk
is affected,[38] basically losing the ability
to adjust the viscosity of the bentonite-based slurry. Therefore,
psyllium husk can be used in a high-temperature environment of 160
°C.
Figure 6
Effect of hot rolling temperature on the rheological property of
the drilling fluid.
Effect of hot rolling temperature on the rheological property of
the drilling fluid.
Filtration
Property Measurement
The
different qualities of psyllium husk are added into bentonite-based
slurry, and its API filtration after hot rolling at different temperatures
is tested, as shown in Figure . With the increase in hot rolling temperature, the API filtration
of bentonite-based slurry increases. After adding 1w/v % psyllium
husk, the API filtration decreases slightly with the increase in temperature.
After hot rolling at 160 °C for 16 h, the API filtration is 11.6
mL, and the reduction rate of API filtration is 69.87%; when the temperature
increases to 180 °C, the API filtration begins to increase which
is due to the destruction of the molecular structure of the psyllium
husk, hence resulting in poor filtration reduction performance.
Figure 7
Effect of hot
rolling temperature on psyllium husk precursor experimental
slurry. (a) Bentonite-based slurry and (b) bentonite-based slurry
+ 1 w/v % psyllium husk.
Effect of hot
rolling temperature on psyllium husk precursor experimental
slurry. (a) Bentonite-based slurry and (b) bentonite-based slurry
+ 1 w/v % psyllium husk.With the increase in
the amount of psyllium husk before and after
160 °C hot rolling, the API filtration decreases (Figure ). When the amount of psyllium
husk is greater than 1 w/v %, the reduction rate slows down gradually,
and the experimental slurry filtration is always less than that before
hot rolling. When the dosage of psyllium husk is 1 w/v %, the API
filtration before hot rolling is 14 mL, and the filtration reduction
rate is 61.11%; after hot rolling at 160 °C, the API filtration
is 9.2 mL and the filtration reduction rate is 76.04%, illustrating
that the psyllium husk has excellent filtration reduction performance.
This is mainly due to the following pieces of evidence: on the one
hand, the psyllium husk is mainly adsorbed on the surface of clay
particles through hydrogen-bonding, increasing the thickness of the
hydration layer and improving the coalescence stability of clay particles
so as to produce mud cake with relatively dense structure, reduce
the permeability of mud cake, and effectively reduce the fluid loss.
On the other hand, with the increase in the amount of psyllium husk,
the viscosity of the experimental slurry increases. According to the
Darcy formula, the increase in viscosity is also conducive to reduce
the fluid loss.
Figure 8
Effect of the addition of different qualities of psyllium
husk
on the filtration of bentonite-based slurry before and after 160 °C.
Effect of the addition of different qualities of psyllium
husk
on the filtration of bentonite-based slurry before and after 160 °C.Generally, fluid loss control can be achieved by
forming tight
mud cakes to effectively plug the pores of the formation or increasing
the viscosity of the drilling fluid.[39] After
the API fluid loss cake is freeze-dried, it is observed using a scanning
electron microscope, as shown in Figures and 10. Before hot
rolling, the clay particles are connected by edge-to-surface, but
due to the aggregation of some clay particles, a large number of irregular
pores are formed in the clay. After adding 1 w/v % psyllium husk,
filamentous and flaky structures are observed in the mud cake, indicating
that it forms a bridge structure, which is beneficial to adsorb water
molecules and retard the migration of water molecules. At the same
time, it can be used in the mud cake. Spherical insoluble particles
are detected on the surface to block pores and participate in the
formation of mud cakes, thereby effectively reducing fluid loss. After
hot rolling at 160 °C, the clay particles are transformed into
a surface-to-surface connection due to dehydration, which causes the
pores of the mud cake to increase and enlarge. After adding 1 w/v
% psyllium husk, the mud cake has an obvious honeycomb structure,
and the bridging effect of the psyllium husk can still be observed,
indicating that the psyllium husk can still reduce filtration by adsorbing
water molecules at this time.
Figure 9
Mud cake SEM image of bentonite-based slurry
before and after 160
°C hot rolling. (a) Before hot rolling and (b) after hot rolling.
Figure 10
Mud cake SEM image of 1 w/v % psyllium husk experimental
slurry
before and after 160 °C hot rolling. (a) Before hot rolling and
(b) after hot rolling.
Mud cake SEM image of bentonite-based slurry
before and after 160
°C hot rolling. (a) Before hot rolling and (b) after hot rolling.Mud cake SEM image of 1 w/v % psyllium husk experimental
slurry
before and after 160 °C hot rolling. (a) Before hot rolling and
(b) after hot rolling.The fluid loss performance
evaluation of HTHP at 160 °C and
3.5 MPa is shown in Figure . After 160 °C hot rolling, with the increase in psyllium
husk addition, the HTHP fluid loss of the experimental slurry first
decreases and then changes little. When the added amount of psyllium
husk is 1 w/v %, the fluid loss of HTHP is the lowest, which is 81.0
mL, and the reduction rate of fluid loss of HTHP is 56.91%. When the
amount of psyllium husk increased further, the HTHP filtration did
not change much.
Figure 11
Effect of different psyllium husk concentrations on the
HTHP fluid
loss of bentonite-based slurry.
Effect of different psyllium husk concentrations on the
HTHP fluid
loss of bentonite-based slurry.
Anti-pollution Performance Evaluation
Anti-salt Pollution Performance Evaluation
1 w/v %
psyllium husk and different concentrations of NaCl are
added to the bentonite-based slurry, and the fluid loss performance
changes after hot rolling at 160 °C are investigated, as shown
in Figure . When
30 w/v % NaCl is added to the bentonite-based slurry, the fluid loss
increased from 40.4 to 276.8 mL, indicating that the fluid loss could
no longer be controlled at this time. After adding 1 w/v % psyllium
husk, the API fluid loss decreased to 44.2 mL, and the fluid loss
reduction rate is 84.03%.
Figure 12
Effect of NaCl concentration on filtration
performance of the drilling
fluid. (a) Bentonite-based slurry and (b) bentonite-based slurry +
1 w/v % psyllium husk.
Effect of NaCl concentration on filtration
performance of the drilling
fluid. (a) Bentonite-based slurry and (b) bentonite-based slurry +
1 w/v % psyllium husk.Studies have shown that
under high salinity conditions, the adsorption
between the polymer and the clay particles can effectively reduce
fluid loss. The electrolyte reduces the solvation ability of water
molecules to a certain extent, the electrostatic repulsion between
the polymer and the clay particles, and increases the adsorption of
anionic polymers on the surface of the clay particles.[40] The polymer molecules in water form a stretched
structure due to the charge repulsion between the molecules. When
the anionic polymer is adsorbed on the surface of the clay particles,
it will have a good colloidal stabilization effect on the clay particles
and prevent the clay particles from flocculating in a high-salt solution.[41] As the concentration of NaCl increases, the
flocculation between the clay particles becomes more serious. When
the concentration of NaCl increases to 30 w/v %, the fluid loss reduction
performance of the psyllium husk on the clay weakens, but compared
with the base slurry, it can still effectively inhibit the flocculation
of clay particles.At the same time, the branched structure
can be adsorbed on the
surface of the clay particles through the hydrogen-bonding of the
polyhydroxyl group, which improves the coalescence stability of the
clay particles.
Anti-calcium Pollution
Performance Evaluation
1 w/v % psyllium husk and different
concentrations of CaCl2 are added to the bentonite-based
slurry, and the fluid loss
performance changes after hot rolling at 160 °C are investigated,
as shown in Figure . When 0.3 w/v % CaCl2 is added to the bentonite-based
slurry, the fluid loss increases from 40.4 to 85.2 mL, indicating
that the fluid loss can no longer be controlled at this time. After
adding 1 w/v % psyllium husk, the API fluid loss decreases to 66.2
mL, and the fluid loss reduction rate is 22.30%.
Figure 13
Effect of CaCl2 concentration on filtration performance
of the drilling fluid. (a) Bentonite-based slurry and (b) bentonite-based
slurry + 1 w/v % psyllium husk.
Effect of CaCl2 concentration on filtration performance
of the drilling fluid. (a) Bentonite-based slurry and (b) bentonite-based
slurry + 1 w/v % psyllium husk.This is because after hot rolling, Ca2+ will cause edge-to-edge
bonding and edge-to-surface bonding between the clays, resulting in
a three-dimensional structure, resulting in an increase in filter
loss. With the further increase in Ca2+ concentration,
the clay particles are transformed into surface-to-surface connection,
which makes the clay flocculate and settle and increase the fluid
loss.[35] After adding 1 w/v % psyllium husk,
the low concentration of Ca2+ will promote the adsorption
of anionic polymers on the clay surface and prevent the flocculation
of clay particles, so the fluid loss will not change much. As the
concentration of Ca2+ increases, the flocculation of clay
particles leads to an increase in the fluid loss of the drilling fluid.
Comparison with Conventional Filtration Reducers
The fluid loss reduction performance of different fluid loss additives
on bentonite-based slurry is shown in Figure . Before hot rolling, several environmentally
friendly fluid loss additives can effectively reduce the API fluid
loss of bentonite-based slurry. After hot rolling at 160 °C,
the molecular structure of the commonly used modified natural polymer
fluid loss agent is destroyed, and the fluid loss performance becomes
worse, and the fluid loss increases to more than 20 mL. Only the experimental
slurry with psyllium husk has excellent fluid loss performance, with
a fluid loss of only 9.2 mL, indicating that the temperature resistance
of psyllium husk is better than other commonly used environmentally
friendly fluid loss reducer and can be applied to 160 °C in the
drilling fluid.
Figure 14
Effect of different environmentally friendly filtrate
reducers
on the filtration properties of bentonite-based slurry before and
after 160 °C hot rolling.
Effect of different environmentally friendly filtrate
reducers
on the filtration properties of bentonite-based slurry before and
after 160 °C hot rolling.This is because the psyllium husk has a natural branched structure
and has better temperature resistance than linear polymers.[42] At the same time, the uronic acid contained
in the molecular chain of the psyllium shell powder has strong reducing
properties, which can inhibit the oxidative decomposition of the polysaccharide
polymer, further improve the temperature resistance, and ensure that
the molecular structure of the polysaccharide polymer is not damaged
to a certain extent.
Evaluation of Biological
Toxicity
Table shows that
the EC50 value of the psyllium husk, which meets the national
standard GB/T 15441-91 of the People’s Republic of China. It
belongs to an environmentally friendly filtration reducer.
Table 3
EC50 Mesurement of Psyllium
Husk
test number
EC50 value/(mg L–1)
standard/(mg L–1)
result
1
1.2 × 105
30,000
environmentally friendly
and non-toxic
2
0.94 × 105
environmentally friendly
and non-toxic
3
1.12 × 105
environmentally friendly
and non-toxic
Mechanism Analysis
The fluid loss
reduction mechanism of psyllium husk is similar to that of other high
molecular polymers, mainly including adsorption, thickening, trapping,
and physical blocking. At the same time, psyllium husk has excellent
water absorption properties which can effectively reduce the content
of free water in drilling fluids, form a hydration film, increase
the elasticity of molecular chains, and help form compressible mud
cakes, thereby reducing fluid loss. However, psyllium husk still exhibits
good filtration reduction performance at high temperatures above 140
°C which is unmatched by the existing natural polymer polymers.
The branched structure of psyllium husk is one of the reasons for
improving its own temperature resistance. The branched structure can
improve the polymer’s thermal stability because of the structural
rigidity between the molecular main chains and the steric hindrance
effect between the branches. At the same time, as the hot rolling
temperature increases, the molecular thermal movement intensifies
and the natural polymer is easily affected by the dissolved oxygen
contained in the drilling fluid, which leads to degradation. Uronic
acid can effectively remove free oxidizing groups and substances and
inhibit the oxidative degradation of polymers.[26,33] Therefore, psyllium husk has a certain concentration of uronic acid
which effectively prevents the oxidative degradation of the molecular
structure at high temperatures. This provides a reference for the
future optimization of other natural polymer materials and provides
the possibility to improve the temperature resistance of the drilling
fluid treatment agent from another perspective.
Conclusions
This article explores the feasibility of using
psyllium husk as
an environmentally friendly filtration reducer for high-temperature-resistant
water-based drilling fluids. Psyllium husk has excellent temperature
resistance. After hot rolling at 160 °C, when the concentration
of psyllium husk is 1 w/v %, the reduction rates of API fluid loss
and HTHP fluid loss are 76.04 and 56.91%, respectively, and much lower
than other commonly used natural polymer fluid loss additives. Simultaneously,
the psyllium husk shows excellent anti-pollution performance. The
fluid loss reduction mechanism of psyllium husk is similar to that
of other high molecular polymers, mainly including adsorption, thickening,
trapping, and physical blocking. The three-dimensional network structure
contained in psyllium husk exhibits excellent water absorption and
viscosity-increasing properties. In addition, the adsorption group
contained in the molecular chain can be adsorbed on the surface of
the clay, effectively improving the agglomeration stability of the
clay. Thickening of the hydration layer is beneficial to reduce fluid
loss and inhibit shale hydration. Meanwhile, the branched side chains
and uronic acid of the psyllium husk improve the thermal stability
of the molecule and retard high-temperature decomposition. In addition,
psyllium husk is environmentally friendly, renewable, and low in cost
and can replace some natural polymers or synthetic polymer filtrate
reducers.