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Energy Sources, Part A: Recovery,

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A Study on Gel Fracturing Fluid for

Coalbed Methane at Low Temperatures
a b a c c a
C. Dai , Q. You , H. Zhao , B. Guan , X. Wang & F. Zhao
a
State Key Laboratory of Heavy Oil Processing, China University of
Petroleum, Qingdao, China
b
School of Earth and Space Sciences, Peking University, Beijing,
China
c
Fracturing & Acidizing Service Center of Langfang Branch, Oil
Exploration & Development Institute, Langfang, China

To cite this article: C. Dai , Q. You , H. Zhao , B. Guan , X. Wang & F. Zhao (2011) A Study on Gel
Fracturing Fluid for Coalbed Methane at Low Temperatures, Energy Sources, Part A: Recovery,
Utilization, and Environmental Effects, 34:1, 82-89, DOI: 10.1080/15567036.2010.545806

To link to this article: http://dx.doi.org/10.1080/15567036.2010.545806

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 Energy Sources, Part A, 34:82–89, 2012
Copyright © Taylor & Francis Group, LLC
ISSN: 1556-7036 print/1556-7230 online
DOI: 10.1080/15567036.2010.545806

A Study on Gel Fracturing Fluid for Coalbed

Methane at Low Temperatures

C. DAI,1 Q. YOU,2 H. ZHAO,1 B. GUAN,3 X. WANG,3 and

F. ZHAO1
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1
State Key Laboratory of Heavy Oil Processing, China University of
Petroleum, Qingdao, China
2
School of Earth and Space Sciences, Peking University, Beijing, China
3
Fracturing & Acidizing Service Center of Langfang Branch, Oil Exploration
& Development Institute, Langfang, China

Abstract Active water and plant gum fracturing fluids are widely used for coalbed
methane in China, however, the limitations of poor rheological property, high con-
tent of water insoluble substances, and high residual content need to be resolved.
Considering the low temperature (20–40ıC) and low permeability of the coalbed
methane reservoir, gel fracturing fluid, which can solve the problems above, was
studied in this article. The gel fracturing fluid is composed of nonionic polyacrylamide,
cross-linker (ZrOCl2 ), pH modifier, gel breaker containing (NH4 )2 S2 O8 , and activator.
The optimized formula and performance evaluation of gel fracturing fluid were also
investigated. The experimental results show that this gel fracturing fluid has the
advantages of easy preparation, low cost, strong shearing resistance capacity, low
filtration coefficient, rapid break, lack of residual after gel breaking, and ease of flow
back. The performance of the gel fracturing fluid is superior to that of active water
and vegetable gum, and it is very suitable for use as a fracturing treatment in coalbed
methane at low temperatures.

Keywords coalbed methane, fracturing fluid, low temperature, performance evalua-

tion, zirconium gel

Introduction
Coalbed methane is, unconventionally, natural gas where mainly methane exists in the
form of adsorption on the surface of the coal matrix, and a small portion is distributed in
pore medium and dissolved in the coalbed water (Fu et al., 2007). A coalbed is usually
a naturally fractured reservoir, and the buried depth is within 1,000 m. The original
permeability is low and the porosity is less than 5% (Luo and Liang, 1997). In China,
the coalbed with low permeability is mainly developed by hydraulic fracturing, which
effectively connects coalbed cracks with the wellbore and enhances production capacity
of coalbed methane.
During fracturing operations, the performance of fracturing fluid is a very important
factor that is related to the success of fracturing. Fracturing fluid should not only have

Address correspondence to Dr. Qing You, School of Earth and Space Sciences, Peking
University, No. 5 Yiheyuan Road, Haiden Districk, Beijing 100871, China. E-mail: youqing_
dandong@yahoo.com.cn

82
 Gel Fracturing Fluid for Coalbed Methane 83

certain viscosity to carry sand into the coalbed cracks, but also should be easy to
break to avoid coalbed damage. Active water fracturing fluid is widely used because
of easy preparation and little damage to the coalbed, however, considering its rheological
property, its application is limited to fracturing scale. Vegetable gum is another widely
used fracturing fluid for coalbeds in China, which has advantages of low cost and
high temperature resistance. But high content of the water insoluble substance and high
residual content after gel breaking for fracturing fluid causes great damage to coalbeds
(Lu, 1995; Cong et al., 2004). In view of the characteristics of coalbed methane, a gel
fracturing fluid is proposed and investigated in this article.
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Experimental Materials and Instruments

Materials and instruments used in this study are as follows:
Polymer: Nonionic polyacrylamide, its viscosity-average molecular weight is 965  104 ,
degree of hydrolysis is 3.31%, and solid content is 94.48%
Cross-linker: ZrOCl2 (AR)
Chemical reagents: .NH4 /2 S2 O8 (AR), pH modifier (to adjust cross-linking time), acti-
vator for low temperature
Brine: Formation simulation water of Hancheng #5 block (the salinity is 499.66 mg/l).
Instruments: REOLOGICA rheometer, GGS42 high temperature and high pressure filtra-
tion instrument, pH meter, capillary viscometer, TDL-5-A centrifuge, etc.

The Screening of Gel Fracturing Fluid

In view of its adjustable cross-linking time and gel strength, easy preparation, and low
cost, gel is widely applied in profile control, water shutoff, acidizing, fracturing, and sand
control, etc. Considering the characteristics of coalbed methane (low temperature, 20–
40ı C), cross-linking rate of gel, gel strength, gel cost, source of raw material, and toxicity,
zirconium gel is optimized as a fracturing fluid for coalbed methane. Zirconium gel is
made of polyacrylamide (PAM) and ZrOCl2 , its cross-linking mechanism is as follows:
(1) the Zr(IV)-ligand of a multi-core hydroxyl bridge is generated through hydrolysis
and hydroxyl bridge action; (2) then the Zr(IV)-ligand cross links with the carboxyl of
PAM to form the bulk gel (Zhao, 1998).

ZrOCl2 ! ZrO2C C 2Cl

ZrO2C C 7H2 O ! Œ.H2 O/7 ZrO2C

Œ.H2 O/7 ZrO2C C HC ! Œ.H2 O/7 Zr.OH/3C

 84 C. Dai et al.
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Optimized formula of fracturing fluid

The viscosity of different formulas, which is composed of PAM and ZrOCl2 , were
measured by a REOLOGICA rheometer after shearing for 2 h in the condition of 170
s 1 and 30ıC. The experimental results were shown in Figure 1.

Figure 1. The viscosity equivalent diagram of fracturing fluid (30ı C).

 Gel Fracturing Fluid for Coalbed Methane 85

The screening criteria are as follows: (1) the viscosity of formula is over 50 mPa
s
after shearing for 2 h; (2) low cost—according the criteria and Figure 1, the formula of
0.4% PAM C 0.035% ZrOCl2 was screened as gel fracturing fluid for coalbed methane.

Performance Evaluation of Gel Fracturing Fluid

Cross-linking Time
It takes a very short time to inject fracturing fluid into the coalbed from a surface facility
during fracturing operations. At the same time, in order to make fractures and carry
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sands, it is necessary for gel fracturing fluid to form gel quickly with high viscosity.
At the present, there are many methods to determine cross-linking time; among them,
the pick and hang method is easy and convenient to apply. The experimental results of
the cross-linking time of gel fracturing fluid after adding a pH modifier were shown in
Table 1.
As shown in Table 1, for coalbed methane at low temperature, the cross-linking time
of 0.4% PAM C 0.035% ZrOCl2 C 0.10% pH modifier is only 20 sec, which is suitable
for fracturing in coalbed methane at low temperatures.

Shear Resistance
The shear resistance of zirconium gel fracturing fluid was investigated by rheological
curve. Viscosity variation of zirconium gel fracturing fluid (formula: 0.4% PAM C
0.035% ZrOCl2 C 0.10% pH modifier) was determined in the condition of 170 s 1
shearing rate and 30ıC by a REOLOGICA rheometer. The experimental results were
shown in Figure 2.
From Figure 2, it can be seen that the viscosity of fracturing fluid was over 100
mPa
s after shearing for 2 h at 170 s 1 . The flow behavior index and consistency
index of the fracturing fluid were, respectively, 0.6816 and 2.1349 Pa
s n , which
were in accordance with indicators of general technical conditions for fracturing fluid.
Therefore, zirconium gel fracturing fluid can satisfy requirements of shear resistance for
the fracturing operation.

Filtration Performance
When the fracturing fluid is squeezed into the coalbed, the more the filtration volume
is, the lower the efficiency of the fracturing fluid, and the more damage is done to the

Table 1
The cross-linking time of different formulas at 30ıC

Cross-linking
No. Formula time/sec

1 0.4% PAM C 0.035% ZrOCl2 C 0.10% pH modifier 20

2 0.4% PAM C 0.035% ZrOCl2 C 0.08% pH modifier 40
3 0.4% PAM C 0.035% ZrOCl2 C 0.06% pH modifier 60
 86 C. Dai et al.
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Figure 2. The viscosity of fracturing fluid versus sheering time (30ı C).

coalbed. It is necessary and important to control the filtration of the fracturing fluid
during the fracturing operation.
Static filtration of the fracturing fluid was determined by a GGS42 high temperature
and high pressure filtration instrument (the temperature was 30ı C, filter medium was
circular filter paper, and the filter pressure is 3.5 MPa). The experimental results were
shown in Figure 3.
The filtration coefficient is used to evaluate the filtration performance of the fracturing
fluid. The lower the filtration coefficient is, the higher the efficiency of the fracturing fluid

Figure 3. The static filtration curve of fracturing fluid at 30ıC. (color figure available online)
 Gel Fracturing Fluid for Coalbed Methane 87

Table 2
Effect of gel breaker concentration on fracturing fluid (30ıC)

Ammonium persulfate concentration, % 0.02 0.04 0.08 0.12 0.16

Breaking gel time, h 43.05 38.85 30.40 24.30 18.02

and the less damage it has to the coalbed. It can be seen from Figure 3, by calculating,
that the static filtration coefficient was 6:635  10 4 m/min1=2 and filter loss rate was
1:11  10 4 m/min, which could meet the indicators of general technical conditions for
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fracturing fluid. Therefore, the zirconium gel fracturing fluid can satisfy the requirement
of filtration performance for fracturing treatments.

Gel Breaking Performance

Gel breaking performance is a very important factor used to evaluate fracturing fluid. The
fracturing fluid for coalbed methane should not only have high viscosity to make fractures
and carry sands, but also should be broken quickly at low temperatures (20–40ıC), which
makes it easy to flow back and reduces damage to the coalbed.
Ammonium persulfate is often used for gel breaking below 54ı C (Chen et al., 1999),
however, it could not break gel quickly and absolutely. The results were shown in Table 2.

As shown in Table 2, it is hard to break gel for fracturing fluid only with ammonium
persulfate. As a result, a low temperature activator was added into the gel breaking, and
the experimental results were shown in Table 3.
As shown in Table 3, after adding the activator at low temperature, the gel breaking
time was shorter, and the formula of 0.065% .NH4 /2 S2 O8 C0:035% activator could break
gel fracturing fluid within 2 h, which made the gel breaking fluid flow back easily and
in a timely manner.

The Damage of Gel Breaking Fluid to Coalbed Core

The coal cores of Hancheng #5 block were used to investigate the damage of gel breaking
fluid to the coalbed. The experimental steps were as follows: (1) Dry the cores in the

Table 3
Effect of combined gel breaker and activator on
fracture fluid (30ı C)

The formula of breaking gel

Breaking Ammonium persulfate Activator

gel time, h concentration, % concentration, %

2 0.065 0.035
3 0.073 0.027
4 0.084 0.016
5 0.09 0.01
 88 C. Dai et al.

Table 4
The harm of gel breaking fluids on the permeability of coal cores (30ıC)
3
Gel breaking fluids k1 =10 m2 k2 =10 3
m2 Harm rate, %

3% KCl 4.6116 2.9152 36.8

Gel fracturing fluid 4.5306 2.8111 38.0
Vegetable gum fracturing fluid 4.8693 1.7659 63.8
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oven and weigh the core. (2) Saturate it with formation water and measure the wet weight
and then calculate the pore volume. (3) Put the coal core into the core holder and exert
2.0 MPa confining pressure. (4) Water flood for over 10 pore volumes and measure the
stable permeability k1 . (5) Inject 2 pore volumes of gel breaking fluid and close the core
holder for 2 h. (6) Oppositely water flood again and measure the stable permeability k2 .
(7) Calculate the damage rate for the coalbed according to Eq. (1):

k1 k2
D  100%; (1)
k1

where  is the harm rate for the coalbed, %; k1 is the permeability of the coal core,
10 3 m2 ; and k2 is the permeability of coal core after injecting gel breaking fluid,
10 3 m2 .
The experimental results of three kinds of fracturing fluids were shown in Table 4.
From Table 4, it can be seen that 3% KCl had the lowest damage to the coal core, the
vegetable gum had the highest damage, and the damage of the gel fracturing fluid was
medium. The damage rate of the gel fracturing fluid was slightly higher than that of 3%
KCl and was obviously less than that of the vegetable gum.

Residual Content
The residual of fracturing fluid after gel breaking has serious effects on the coalbed,
such as blocking pore medium and constraining the mobility of methane. As a result,
high residual content of the fracturing fluid after gel breaking is adverse to improve the
fracturing effect. The residual content of both zirconium gel and vegetable gum fracturing
fluids were measured. The experimental results show that there was no residual content
for zirconium gel fracturing fluid, which was favorable to the fracturing operation, but
the residual content of the vegetable gum fracturing fluid was 1,305 mg/l, which would
seriously affect the fracturing effect.

Conclusions
1. Zirconium gel fracturing fluid formed by PAM and ZrOCl2 was prepared for
coalbed methane at low temperatures.
2. Zirconium gel fracturing fluid has the advantages of easy preparation, low cost,
strong shear resistance capacity, low filtration, no residual content, and little
damage to the coalbed.
 Gel Fracturing Fluid for Coalbed Methane 89

Acknowledgments
This study was sponsored by the National S&T Major Project (No. 2008ZX05037-3),
Science Funds for Distinguished Young Scholar of Shandong Province (No. JQ201013),
China Postdoctoral Science Foundation (No. 20090460481), and Taishan Scholars Con-
struction Engineering (No. ts20070704).

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