PETROLEUM EXPLORATION AND DEVELOPMENT

Volume 45, Issue 2, April 2018

Online English edition of the Chinese language journal

Cite this article as: PETROL. EXPLOR. DEVELOP., 2018, 45(2): 336–342. RESEARCH PAPER

Adsorption damage and control measures of slick-water

fracturing fluid in shale reservoirs
GUO Jianchun*, LI Yang*, WANG Shibin
State Key Laboratory of Oil & Gas Reservoir Geology and Exploitation in Southwest Petroleum University, Chengdu 610500, China

Abstract: The slick-water polymer adsorption damage and control measures in shale were examined using a shale pack model of the
Ordovician Wufeng Formation–Silurian Longmaxi Formation in the Changning block of the Sichuan Basin. The adsorption law of slick
water under different displacement time, concentrations, pH values and temperatures of polymer were tested by traditional displacement
experiment and UV-Vis spectrophotometer. The adsorption equilibrium time was 150 min, the amount of adsorption was proportional to
the concentration of the polymer, and the maximum adsorption concentration was 1 800 mg/L. With the increase of pH value, the adsorp-
tion capacity decreased gradually, the adsorption capacity increased first and then decreased with the increase of temperature, and the ad-
sorption capacity was the largest at 45 C. The adsorption patterns of polymers on shale were described by scanning electron microscopy
and magnetic resonance imaging. It is proved that the adsorption of polymer on shale led to the destruction of the network structure of
anionic polyacrylamide molecules, and the shale adsorption conformation was characterized qualitatively. Finally, according to the ad-
sorption law and adsorption mechanism, it is proposed to reduce the adsorption quantity of polymer on shale surface by using hydrogen
bond destruction agent. The effects of hydrogen bond destruction on four kinds of strong electronegative small molecules were compared,
the hydrogen bond destroyer c was the best, which lowered the adsorption capacity by 5.49 mg/g and recovered permeability to 73.2%.
The research results provide a reference for the optimization of construction parameters and the improvement of slickwater liquid system.

Key words: shale; hydraulic fracturing; slick-water; polymer; shale adsorption; desorption

Introduction conventional reservoir fracturing are to reduce the concentra-

Shale reservoirs are typical low porosity and low perme-
ability reservoirs[13], and hydraulic fracturing is the key tech-
nology for developing this kind of resource[45]. The usage rate
of slick-water fracturing fluid system exceeds 80% in shale
fracturing[67]. However, slick-water has low viscosity and
poor proppant carrying capacity. In order to enhance the
proppant delivering capacity, the pumping rate of slick water
fracturing is much higher than that of conventional fracturing,
which results in sharp increase of operation friction[811].
Therefore, the resistance reducing agent in slick-water (usu-
ally anionic polyacrylamide) is one of the important guaran-
tees for shale fracturing[1214]. However, the hydrophilic
groups in the anionic polyacrylamide form a chemical bond
with the oxygen-containing groups in the shale, the adsorption
and retention occur in the wall of the rock and the pore of the
matrix. And the oil and gas flow channels are reduced or even
blocked by fracturing. It restricts the effect of fracturing seri-
ously[1517].
At present, the main reservoir protection techniques in
tion of fracturing fluid, shorten the operation time and reduce
the relative molecular mass of the polymer, etc[1822]. However,
the pore throat radius of the shale reservoir and the polymer
molecules are both nano-scale, which would cause larger
damage to the fracture and matrix permeability[2324].
Taking the shales of the Ordovician Wufeng – Silurian
Longmaxi formations as examples in the Changning block of
the Sichuan Basin, this study examines the adsorption law and
influencing factors of polymer in slick-water. Combined with
the microscopic analysis of adsorption morphology, the
measures for reducing the adsorption damage to shale reser-
voir are put forward.
1. Experiments of shale adsorption damage
The main component of resistance reducing agent in the
slick-water system is usually anionic polyacrylamide. To ver-
ify whether shale would adsorb anionic polyacrylamide, shale
samples were pulverized into 0.21 to 0.30 mm (7050 mesh)
particles and put into a sand pack tube first. The shale had a

Received date: 14 Oct. 2017; Revised date: 10 Jan. 2018.

* Corresponding author. E-mail: guojianchun@vip.163.com; 1106521119@qq.com
Foundation item: Supported by the China National Science and Technology Major Project (2016ZX05021, 2016ZX05023).
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/).
 GUO Jianchun et al. / Petroleum Exploration and Development, 2018, 45(2): 336–342

Fig. 1. Experimental integrating shale displacement unit and

ultraviolet spectrophotometer.
quartz content of 60.2%, calcite content of 14.7%, and clay
mineral content of 13.9% (mostly illite and chlorite). The dis-
placement with anionic polyacrylamide solution of 1000 mg/L
last 5 h, and then nitrogen gas was used for reverse displace-
ment for 1 h (to prevent mechanical retention). The experi-
mental device is shown in Fig. 1.
The infrared spectra of the shale sample before and after
displacement were tested, combined with the absorption peak
characteristics of anionic polyacrylamide infrared spectrum
and the absorption peak characteristics of shale infrared spec-
trum[2526], it can be seen that the shale adsorbed anionic pol-
yacrylamide during slick-water flooding process.
2. Rules of shale adsorbing polymer
In this study, the concentrations of anionic polyacrylamide
before and after adsorption were measured by chromogenic
method of starch and chromium iodide[27], and the adsorption
capacity was calculated by the concentration change.
Based on the test results of adsorption capacity, the adsorp-
tion rules of polymer in shale at different time, concentrations,
relative molecular mass, pH values and temperatures were
figured out.
2.1. Adsorption rules at different time
The slick water samples with anionic polyacrylamide con-
centrations of 500, 1 000, 2 000 mg/L were prepared (with
relative molecular mass of 1 800104). Adsorption capacity
test was carried out according to the above experimental pro-
cess, the concentration of the sample was tested every 10 min,
through a total test time of 240 min, and the adsorption equi-
librium curves are shown in Fig. 2.
As shown in Fig. 2, adsorption capacity increases with time,
and the adsorption equilibrium time is independent of the
concentration. The three kinds of slick water samples all have
adsorption equilibrium time of 150 min, which is the time
reaching the saturated adsorption. The adsorption of slick
water on shale surface accords with the Langmuir adsorption
law[28]. The adsorption sites of the rock surface are completely
occupied by anionic polyacrylamide, and the adsorption
reaches the state of dynamic equilibrium.
2.2. Adsorption rules at different concentrations
Three kinds of slick water samples with different relative
 337 
Fig. 2. The adsorption equilibrium curves of slick-water
samples in shale (at 25 C and pH of 7.0).
Fig. 3. The limiting concentration curves of slick-water samples
in shale (at 25 C and pH of 7.0).
molecular mass of anionic polyacrylamide were prepared,
respectively, diluted to 2003 000 mg/L (every 200 mg/L for a
concentration point). After displacement for 150 min, the ab-
sorbance was measured and the adsorption capacity was cal-
culated. The results are shown in Fig. 3.
It can be seen from Fig. 3 that the amount of adsorption in-
creases with the relative molecular mass of anionic poly-
acrylamide. When the molecular mass is 1 800104, the ad-
sorption capacity is up to 8.6 mg/g. At the same time, with the
increase of polymer concentration, the adsorption capacity
increases rapidly. Increase of adsorption capacity slows down
when the concentration exceeds 800 mg/L, and the limiting
concentration is reached at 1 800 mg/L. The main reason for
the increase of adsorption capacity is that the interaction be-
tween anionic polyacrylamide chains enhances with the in-
crease of concentration, leading to the decrease of permeabil-
ity of shale pack model[2930]. When the polymer concentration
in slick water is more than 1 800 mg/L, the adsorption sites on
the surface of the shale are completely occupied by the poly-
mers, and the adsorption capacity will not increase with the
rise of polymer concentration anymore.
2.3. Adsorption rules at different pH values
The pH value of the polymer solution would change the
distribution of the molecular chains of the polymer, but the
molecular structure of the polymer will be destroyed if the
acidity or alkalinity of the solution is too strong (slick-water
system in field hydraulic fracturing is generally weakly alka-
 GUO Jianchun et al. / Petroleum Exploration and Development, 2018, 45(2): 336–342
Fig. 4. Adsorption laws of slick water samples with different pH
values in shale (at the temperature of 25 C and polymer
concentration of 1 800 mg/L).
line). Considering the systematicity of the study on adsorption
mechanism, the scope of the acidity and alkalinity range was
expanded in this research. The adsorption laws of polymer
solution with pH values of 3-11 were tested. The experimental
results are shown in Fig. 4.
With the increase of pH value, the amount of adsorption
decreases on the whole, and the process can be divided into 5
stages. A (pH < 4.0), C (pH = 6.0-7.5) and E (pH > 10.0) are
intervals where the adsorption quantity doesn’t correlate with
the pH value, because under the strong acidity and alkalinity,
the molecular structure has been destroyed, and the molecular
structure of the polymer will not change much under the neu-
tral condition, so the adsorption quantity is unaffected. B (pH
= 4.0-6.0) and D (pH = 7.5-10.0) are intervals where the ad-
sorption capacity is negatively correlated with the pH value.
Because the anionic polyacrylamide is in linear state under the
acidic condition, and the molecular chains curl with the in-
crease of pH value, which is not conducive to the combination
of polymer and shale adsorption sites, and leads to rapid re-
duction of the adsorption capacity[3132].
2.4. Adsorption rules at different temperatures
Reservoir temperature is a key factor affecting fracturing,
and also an important variable affecting the law of adsorption.
The variation curve of adsorption capacity and equilibrium
time of shale with reservoir temperature of 20100 C is
shown in Fig. 5.
Fig. 5. Relationship between temperature, adsorption capacity
and adsorption equilibrium time (at pH of 7.0 and polymer
concentration of 1 800 mg/L).
 338 
It can be seen from Fig. 5 that with the increase of tem-
perature, the adsorption amount increases first and then de-
creases. X section (T < 45 C) is the section where the adsorp-
tion capacity is in positive correlation with temperature, as the
temperature rises, the diffusion speed of polymer molecules
accelerates, and more polymer molecules get away from the
binding of water molecules, the collisions between polymer
molecules and shale surfaces increase, thus leading to the
rapid increase of adsorption capacity. Y section (T = 4570 C)
is the section where the adsorption is in negative correlation
with temperature, as the temperature continues to rise, the
desorption rate of polymer molecules will accelerate at the
same time, which will cause the polymer molecules to sepa-
rate from the shale surface and melt into the slick water again,
so the adsorption capacity decreases rapidly. Z section (T >
70 C) is a section where adsorption is not correlated with
temperature. When the temperature is above 70 C, the
amount of adsorption no longer changes with the temperature.
The adsorption capacity is stabilized at about 2.7 mg/g and the
adsorption and desorption of the polymer on shale surface
reach dynamic equilibrium at this time[33].
With the increase of temperature, the adsorption equilib-
rium time decreases continuously. The adsorption equilibrium
time decreases sharply at 2045 C, and the adsorption equi-
librium time is in exponential negative correlation with the
temperature. At 4570 C, the adsorption equilibrium time
decreases continuously, and is in linear negative correlation
with the temperature. The equilibrium time will not change at
70100 C. The adsorption of polymer on shale surface ac-
celerates because of the acceleration of the molecular irregular
movement with the increase of temperature[34]. However,
when the temperature is higher than the critical temperature,
the irregular motion of polymer molecules is restricted, and
the adsorption equilibrium time shortens slightly even stops
shortening.
3. Visualization of polymer adsorption morphology
on shale surface
3.1. SEM analysis before and after adsorption
Scanning electron microscope images of polymer solution
before and after adsorption are compared (Fig. 6). Firstly, the
original morphology of the polymer solution with a concen-
tration of 1000 mg/L was observed under different magnifica-
tion (Fig. 6a, 6c, 6e, and 6g). It is obvious that the original
polymer solution before adsorption has a good three-dimen-
sional network structure, and the molecular chains are in very
regular linear unidirectional arrangement, this is the very
structure needed for resistance reducing agent of slick-water.
However, the residual polymer solution after adsorption has
obvious structure variation (Fig. 6b, 6d, 6f, and 6h). The
three-dimensional network structure of the polymer is de-
stroyed and the molecules are entangled. Nano-scale molecu-
lar clusters are formed, reaching the scale of the shale pore
throat radius. The pore throat radius of the shale is reduced or
 GUO Jianchun et al. / Petroleum Exploration and Development, 2018, 45(2): 336–342

Fig. 6. SEM images of polymer solution before and after adsorption.

Table 1. NMR images during displacement.

Sequence number Time Sagittal plane 1 Sagittal plane 2 Sagittal plane 3

1 20 min

2 60 min

3 150 min

Note: the red represents pores, the blue represents polymer; the sample is 2.5 cm in diameter and 7.5 cm long.

even blocked by polymer adsorption, which is finally mani-
fested as permeability damage.
3.2. NMR imaging during shale displacement
The adsorption process of polymer during shale displace-
ment was imaged by NMR, and sagittal planes at different
displacement stages were selected to analyze (Table 1). After
displacement of 20 min, a large number of polymer signals
appeared in the dominant channels of shale, and similar ef-
fects were shown on different sagittal planes. At this point, the
polymer just broke through the end of the shale. After 60 min
of displacement, all pore channels had polymer signals, the
displacement pressure difference increased obviously, and the
shale permeability reduced greatly. NMR images at 150 min
show that the polymer in slick-water has made most pore
throats radius decrease or even blocked.
4. Measures to control adsorption damage
According to the classical force analysis of polymer flood-
ing, the main forces acting in adsorption and retention of
polymer in reservoir include the Van der Wals force, electro-
static force and hydrogen bonding[35]. Because the Van der
Wals force and electrostatic force are irreversible physical and
chemical phenomena, there are no effective solutions in the-
ory and engineering. In order to reduce the adsorption capac-
ity of polymer on the shale surface, hydrogen bond destroyer
is used to destroy the hydrogen bonding between the polymer
and the shale. Hydrogen bonding is a reversible force acting
on the shale surface by anionic polyacrylamide, and hydrogen
bonds can be easily destroyed by small molecules with strong
electronegativity to reduce the adsorption capacity of polymer
on shale. The effects of hydrogen bonding destruction of four
kinds of small molecules with strong electronegativity were
compared, and the experimental results are shown in Table 2.
The “c” agent has the best effect of hydrogen bonding de-
struction, and it can reduce the adsorption capacity by 63.7%
at the concentration of 1 000 mg/L. The “a” agent takes the
second place, and can reduce the adsorption by 55.7% at the
same condition. The “b” agent has the worst effect, and only
reduces the adsorption capacity by 36%. But the reduction of
adsorption capacity is not completely equivalent to the recov-
ery degree of permeability damage. Therefore, dynamic dis-

 339 
 GUO Jianchun et al. / Petroleum Exploration and Development, 2018, 45(2): 336–342

Table 2. Comparison of adsorption capacity reduction of dif-

ferent hydrogen bonding destroyers.
Type of hydro- Concen- Adsorption Reduction of Percentage
gen bonding tration/ capacity/ adsorption ca- reduction in
destroyer (mg·L1) (mg·g1) pacity/(mg·g1) adsorption/%
500 5.46 3.16 36.7
a 1 000 3.82 4.80 55.7
2 000 3.65 4.97 57.7
500 7.23 1.39 16.1
b 1 000 5.52 3.10 36.0
2 000 4.16 4.46 51.7
500 4.77 3.85 44.7
c 1 000 3.13 5.49 63.7
2 000 3.02 5.60 65.0
500 6.09 2.53 29.4
d 1 000 4.61 4.01 46.5
2 000 3.91 4.71 54.6
Note: the polymer concentration was 1 800 mg/L, the temperature
was 25 C, the pH value was 7, and the test time was 150 min.
placement experiments were conducted with the four kinds of hydro-
gen bonding destroyers to test the permeability damage.

Four shale pack models with the same porosity and perme-
ability were displaced with water for 120 min, and their per-
meabilities were all reduced by 18.6%. Then they were dis-
placed with slick-water with concentration of 1 000 mg/L, it is
obvious that their permeabilities were reduced by 40.2% fur-
ther. Finally, they were displaced with slick-waters of 1 000
mg/L concentration containing the four different types of hy-
drogen bonding destroyers, and the results show their perme-
abilities recovered to various degrees (Fig. 7). Because the
adsorption force of the polymer acting on the shale surface
was destroyed, the polymer was desorbed from the rock
quickly, pore throat channels of rock were cleared, realizing
the recovery of residual permeability. The residual perme-
abilities of the shale pack models can be recovered to 73.2%,
68.3%, 57.8% and 49.4% by hydrogen bonding destroyers c, a,
d and b respectively.
Although there is no method and theory in China and
abroad about recovering the fracturing fluid damage by de-
stroying the adsorption force, the results of the study show
that the adsorption of polymer in slick-water on shale surface
can cause permeability damage, and the hydrogen bonding
destroyer can reduce adsorption capacity of the polymer sig-
nificantly, thus recovering the permeability damage caused by
polymer in slick-water. Therefore, considering the adsorption
of polymer in shale reservoirs has engineering significance in
predicting and removing the slick-water fracturing fluid per-
meability damage, and determining the reasonable liquid pa-
rameters and operation parameters.
5. Conclusions
The adsorption of anionic polyacrylamide in shale con-
 340 
Fig. 7. Dynamic verification of shale adsorption damage.
forms to the Langmuir isothermal adsorption process. The
adsorption equilibrium time is 150 min, the adsorption capac-
ity is positively correlated with the concentration of polymer,
and the limiting concentration is 1 800 mg/L. The amount of
adsorption decreases gradually with the increase of pH value.
With the increase of temperature, the adsorption amount in-
creases first and then decreases, the maximum adsorption
capacity is at 45 C.
Adsorption of the polymer will lead to the destruction of
the molecular network structure of the anionic polyacrylamide,
and the aggregated polymer molecules on shale surface leads
to blocking of micro cracks and the reduction of pore throat
radius.
Hydrogen bonding is a reversible force of adsorption be-
tween the shale surface and anionic polyacrylamide, and hy-
drogen bonds can be easily destroyed by small molecules with
strong electronegativity to reduce the adsorption capacity of
polymer on shale.
Permeability of shale pack models reduced by 18.6% by
clear water flooding, and the polymer flooding reduced the
permeability further by 40.2%. The “c” hydrogen bonding
destroyer agent has the best effect. It can reduce the adsorp-
 GUO Jianchun et al. / Petroleum Exploration and Development, 2018, 45(2): 336–342
tion capacity by 5.49 mg/g and recover the permeability to
73.2%.
In actual fracturing, shortening the operation time, reducing
the concentration of fracturing fluid and the relative molecular
mass of the polymer are still the keys in designing low dam-
age fracturing fluid system for shale. Hydrogen bonding de-
stroyer can remove the adsorption effect of the polymer, break
the limit of the conventional low damage fracturing fluid sys-
tem and improve the development effect of shale reservoirs.
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