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Gasification reactivity of char with CO2 at elevated temperatures the effect of heating rate during pyrolysis.

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ASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING
Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
Published online 16 July 2010 in Wiley Online Library
(wileyonlinelibrary.com) DOI:10.1002/apj.483
Research article
Gasification reactivity of char with CO2 at elevated
temperatures: the effect of heating rate during pyrolysis
Hao Liu,1 * He Zhu,1 Liye Yan,1 Yongjun Huang,1 Shigeru Kato2 and Toshinori Kojima2
1
2
Department of Thermal Energy and Power Engineering, Soochow University, Suzhou 215006, China
Department of Materials and Life Science, Seikei University, Tokyo 180-8633, Japan
Received 30 March 2010; Revised 4 June 2010; Accepted 6 June 2010
ABSTRACT: Integrated coal gasification combined cycle (IGCC) technology is being promoted to make better use of
energy resources, and an entrained-flow gasifier is a key item of equipment in the process due to its high gasification
efficiency, smooth discharge of molten ash, etc. The temperature and heating rate under entrained-flow gasification
conditions are very high, and these two parameters can influence the gasification reactivity of a char with CO2 .
Therefore, the clarification of characteristics and mechanisms of char gasification under conditions close to entrainedflow gasification is very important. To obtain a valid kinetics of char gasification, it is necessary to clarify the effect of
heating rate during pyrolysis on char reactivity. The effect of heating rate during pyrolysis on the gasification reactivity
of three types of chars in CO2 was investigated experimentally at elevated temperatures in a novel fluidized bed. It
was shown that even at elevated temperatures, the heating rate has significant influence on the char reactivity during
gasification. A higher heating rate during pyrolysis leads to higher char reactivity of gasification, however it has only
limited effect on the activation energy of char gasification with CO2 . The char reactivity is closely related to its specific
surface area and pore volume. The high reactivity of a char derived from pyrolysis at a high heating rate is most likely
due to its enhanced porous structure as a result of the rapid release of volatile matter at a high heating rate. The effect
of heating rate during pyrolysis on char reactivity is pronounced at low temperatures, and is very different for various
coal types, i.e. very pronounced for a low-rank coal. The gasification reactivity of a char is related to both the char
pore structure and temperature, which suggests that even at elevated temperatures the gasification of a char with CO2
is controlled by both chemical reaction and diffusion inside the particles. Our results demonstrate that it is necessary
to derive the gasification kinetics of a char at a high heating rate to obtain valid kinetic equations for an entrained-flow
gasifier.  2010 Curtin University of Technology and John Wiley & Sons, Ltd.
KEYWORDS: coal; pyrolysis; integrated coal gasification combined cycle; entrained-flow gasifier; char reactivity;
heating rate
INTRODUCTION
Integrated coal gasification combined cycle (IGCC)
technology is proposed as one of the promising technologies to save energy resources and to prevent global
warming. As one of the key components included in this
process, an entrained-flow gasifier is of substantial commercial interest owing to its high gasification efficiency,
smooth discharge of molten ash, etc. The temperature
and heating rate under entrained-flow gasification conditions are very high, whereas these two parameters have
potential effects on the gasification reactivity of a char
with CO2 . To obtain a valid kinetics of char gasification,
*Correspondence to: Hao Liu, Department of Thermal Energy and
Power Engineering, Soochow University, Suzhou 215006, China.
E-mail: liuhao@suda.edu.cn
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
Curtin University is a trademark of Curtin University of Technology
it is necessary to clarify the effect of heating rate during
pyrolysis on char reactivity.
Recent work of Russell et al .[1] has shown that the
intrinsic reactivity of chars treated at temperatures of
typical pulverized coal combustion can be two orders of
magnitude lower than for chars prepared at 1273 K. The
lower char reactivity due to high-temperature treatment
has also been reported by others.[2 – 5]
Char gasification has widely been investigated in
a thermogravimetric analyzer (TGA), a fixed bed, a
drop tube reactor or an entrained-flow reactor, within
a relatively low-temperature range.[1,2,6 – 8] Yang et al .
analyzed various coal gasification data from most gasification systems.[9] A fluidized bed has also been adopted
to study char gasification whereas at comparatively low
temperatures.[10,11]
The previous studies help understanding the gasification kinetics of chars in an entrained-flow gasifier.
906
H. LIU et al.
Asia-Pacific Journal of Chemical Engineering
Meanwhile, considering the high temperature (as high
as 1773 K or even higher[12,13] ) and high heating rate
in an entrained-flow gasifer, research under such conditions is also important. In the past, we have studied
coal gasification at elevated temperatures,[14,15] but we
did not study the effect of heating rate during pyrolysis
on the gasification reactivity of a char.
In this work, we examined the effect of heating rate
during pyrolysis on the gasification reactivity of a char
directly from the change in CO concentration in a
uniquely and delicately made fluidized bed, which can
be operated at temperature up to 1873 K, in different
atmospheres, and at various reaction times.
The main objective of this work was to clarify the
effect of heating rate during pyrolysis on the gasification
reactivity of a char at an elevated temperature, so as to
obtain valid kinetics of char gasification.
Coal sample
Gas
sampling
TC
Insulator
N2
vent.
TRC
to
gas bag
CO2
Siliconit
FBR
Air
compressor
Figure 1. Schematic diagram of the experimental setup
(fluidized bed A) for measurement of gasification rates.
EXPERIMENTAL
Measurement of gasification rates
reaction temperature first, and then the coal particles
were added into the hot fluidized bed so that the particles were heated by the fluidized bed rapidly and
pyrolyzed in an atmosphere of N2 for 10 min. Then
the gas line was suddenly switched to CO2 /N2 mixture (20% CO2 and N2 as balance) so that gasification
began. The heating rate for rapid heating was estimated
by taking convective and radiative heat transfers into
account but ignoring the intraparticle resistance, effects
of evaporation and devolatilization because intraparticle heat transfer is very strong in a fluidized bed, and
the amount of coal sample is so small that evaporation
and devolatilization hardly influence the bulk temperature in the bed. According to calculation, the average heating rate was estimated to be about 1.0–3.0 ×
103 K/s corresponding to a bed temperature ranging
1273–1873 K.
Three types of coals described in Tables 1 and 2
were used in this work. The experimental conditions
for measurements of gasification rates are listed in
Table 3 (fluidized bed Type A). All the velocities
listed in Table 3 are values at bed temperatures. The
production rate of CO was derived from the composition
of exhausted gas at the exit of the reactor. Then the
instantaneous overall reaction rate was derived from
Figure 1 shows the schematic diagram of the experimental setup (fluidized bed Type A, Table 3) for measurement of gasification rates. A fluidized bed, with an
inner diameter of 35 mm, was used as the reactor. The
fluidized bed, together with the distributor, was made of
alumina and heated by siliconit electric heaters so that
it could be operated at high temperatures. Inert alumina
particles with an average diameter of 0.119 mm were
used as the bed particles.
A batch of coal particles were pneumatically fed
into the reactor by nitrogen carrier gas. In this work,
two heating patterns, that is, slow heating and rapid
heating, were adopted to examine the influence of heating rate during pyrolysis on char reactivity. For slow
heating, the coal particles were added into the fluidized bed before heating, and then the fluidized bed,
together with the coal particles, was heated from ambient temperature to the given reaction temperature at a
given temperature-rising rate in the order of several to
tens of Kelvin per minute. When the given reaction
temperature was reached, the gas line was suddenly
switched to CO2 /N2 mixture (20% CO2 and N2 as balance) so that gasification began. On the other hand,
for rapid heating, the fluidized bed was heated to the
Table 1. Properties of parent coals.
Proximate analysis (as received, wt%)
Coal
Taiheiyo
McKinley
Witbank
Ultimate analysis (daf, wt%)
Moisture
Ash
VM
FC
C
H
N
O
S
3.76
10.14
2.40
12.08
12.48
14.43
43.98
34.74
24.10
40.18
42.64
59.07
78.72
76.82
84.37
6.22
5.78
4.67
1.17
1.39
1.95
13.78
15.67
8.55
0.11
0.34
0.46
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering
GASIFICATION REACTIVITY OF CHAR WITH CO2
EXPERIMENTAL RESULTS
Table 2. Ash fusion temperatures.
Oxidation
atmosphere (K)
Reduction
atmosphere (K)
Effect of heating rate during pyrolysis on
initial reaction rate
Coal
Tdef
Them
Tflow
Tdef
Them
Tflow
Taiheiyo
McKinley
Witbank
1543
1603
1583
1593
1693
1643
1743
1738
1658
1503
1543
1583
1573
1598
1643
1743
1638
>1773
The variation of reaction rate with conversion of a char
during gasification is usually expressed in the following
form:
rc = dX /dt = r0 F (X )
(1)
where r0 is the initial reaction rate of gasification and
F (X ) is a function of carbon conversion X . The grain
model and the random pore model are the most popular
models to describe the variation of gasification rates
with conversion (or time). The random pore model
gives:
CO production rate based on chemical stoichiometry.
The experimental details were described in our previous
article.[16]
Char characterization
dX /dt = r0 (1 − X )[1 − f ln(1 − X )]0.5
The coal particles adopted for reaction rate measurement as mentioned earlier, after pyrolysis, were difficult to be collected for nitrogen adsorption analyses,
etc. To facilitate the experiments while minimizing the
influence of the external mass transfer resistance on
the derivation of valid gasification rates, another fluidized bed (Type B, Table 3), with an inner diameter of 42.0 mm, was used as the reactor to prepare
char samples for char characterization. After pyrolysis
at various heating rates in N2 atmosphere, char particles were entrained (discharged) together with alumina
particles. After being completely cooled for 30 min,
the alumina particles were screened out and only the
char particles were picked up for char characterization. The experimental conditions for char characterization are listed in Table 3 (fluidized bed Type B).
Pore structure characterization with nitrogen adsorption and scanning electron microscope (SEM) analyses on the surface morphology of char particles were
conducted.
(2)
where f is a parameter accounting for the effect of
pore structure of char particles. Yang et al . analyzed
various coal gasification data from most gasification
systems.[9] They found that most of the conversion
data for coal gasification reported in the literature,
when plotted against dimensionless time τ , can be
unified into a single curve with reasonable accuracy.
A master curve, which is an approximation for all
the conversion time data for coal gasification, has
been correlated based on the grain model and the
random pore model for gas–solid reactions. In our
case, it was found that a random pore model (f =
2.5) was the best to describe our experimental data.
Accordingly, a random pore model (f = 2.5) was
adopted to derive the initial reaction rate based on our
time variation results of gasification reaction rate from
experiments.
The initial reaction rate of gasification was derived
for chars pyrolyzed at various heating rates. Here, the
Table 3. Experimental conditions.
Fluidized bed
Static bed height (mm)
Alumina particles
Diameter (mm)
Density (g/cm3 )
Diameter of coal particles (mm)
Bed temperature (K)
Minimum fluidization velocity (m/s)
For alumina particles
For coal particles
Terminal velocity (m/s)
For alumina particles
For coal particles
Superficial gas velocity (m/s)
CO2 concentration (%)
N2 concentration (%)
Type A
Type B
100
100
0.119 (0.075–0.149)
3.0
0.194 (0.177–0.210)
1273–1873
0.370 (0.180–0.500)
3.0
0.550 (0.500–0.600)
1273–1873
0.0083–0.0061
0.012–0.0092
0.054–0.039
0.083–0.063
0.429–0.328
0.420–0.333
0.080–0.120
20
As balance
2.43–2.09
1.64–1.82
0.324–0.234
20
As balance
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
DOI: 10.1002/apj
907
H. LIU et al.
Asia-Pacific Journal of Chemical Engineering
Taiheiyo char
McKinley char
0.1
Witbank char
0.1
0.01
0.01
0.001
VM = 43.98
Initial reaction rate (1/s)
0.01
10 K/min
1-3 103 K/min
5 K/min
15 K/min
20 K/min
30 K/min
40 K/min
1-3 103 K/min
0.001
1-3 103 K/min
10 K/min
VM = 34.74
0.0001
VM = 24.10
0.001
5
5.5
6
6.5
7
7.5
8
0.0001
5
5.5
6 6.5 7 7.5
10000/T (1/K)
8
5
5.5
6
6.5
7
7.5
8
Figure 2. Effect of heating rate during pyrolysis on the initial reaction rate. This figure is available in colour
online at www.apjChemEng.com.
Table 4. Activation energy of various coal chars.
Coal char
Activation energy (kJ/mol)
5 K/min
15 K/min
20 K/min
40 K/min
1-3 103 K/min
Taiheiyo McKinley Witbank
65.8
38.4
172.4
1273 K
heating rate for rapid heating was estimated to be in
the order of 1.0–3.0 × 103 K/s corresponding to a bed
temperature ranging 1273–1873 K. Figure 2 shows the
initial reaction rate for Taiheiyo char, McKinley char
and Witbank char, respectively. Obviously, the heating
rate during pyrolysis had significant influence on initial
reaction rate for all the three chars investigated in this
work. A higher heating rate led to higher char reactivity. This was very probably attributed to the different
release behavior of volatile matter during pyrolysis at
different heating rates. On the other hand, the effect
of heating rate on the activation energy of the gasification reaction was limited. Table 4 shows the list of
the activation energy of the three chars, which showed
very different values among different chars. Moreover,
comparison among the three chars revealed that for different chars, the effect of heating rate during pyrolysis
on the reaction rate was different, that is, pronounced
for a char derived from a coal with high volatile matter
content. Furthermore, the effect of heating rate during pyrolysis was pronounced in the low-temperature
range. This result was probably owing to the fact that
at low temperatures, the overall reaction rate was relatively low and the external diffusion resistance was
less important than at high temperatures, and consequently the effect of pore structure on char reactivity
owing to different heating rates was pronounced at low
temperatures.
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
Reaction rate (1/s)
908
1773 K
0.01
0.025
0.008
0.02
0.006
0.015
0.004
0.01
0.002
0.005
0
0
0
0.2 0.4 0.6 0.8 1
0 0.2 0.4 0.6 0.8
Conversion of carbon
1
Effect of heating rate during pyrolysis on the
reaction rate in the whole process of char gasification
(Taiheiyo char). This figure is available in colour online at
www.apjChemEng.com.
Figure 3.
Reaction rate vs carbon conversion
Figure 3 shows the comparison of the gasification
reaction rates in the whole gasification process for chars
derived from pyrolysis at various heating rates (Taiheiyo
char). It can be seen that the heating rates drastically
affected the reaction rate of gasification in the whole
reaction process, not merely in the beginning. A higher
heating rate led to a higher reaction rate. The tendency
at 1273 K was similar to that at 1773 K. Figure 4 shows
Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering
GASIFICATION REACTIVITY OF CHAR WITH CO2
10 K/min
1-3 103 K/min
1373 K
1673 K
0.03
0.02
0.025
Reaction rate (1/s)
0.015
0.02
0.01
0.015
0.01
0.005
0.005
0
0
0
0 0.2 0.4 0.6 0.8
0.2 0.4 0.6 0.8 1
Conversion of carbon
1
(a) Slow heating (1473 K)
(b) Rapid heating (1473 K)
(c) Slow heating (1673 K)
(d) Rapid heating (1673 K)
Figure 4. Effect of heating rate during pyrolysis on the
reaction rate in the whole process of char gasification
(McKinley char). This figure is available in colour online
at www.apjChemEng.com.
the comparison of the gasification reaction rates at rapid
heating rate and 10 K/min heating rate for McKinley
char. Similarly to the case of Taiheiyo char, the reaction
rate at a rapid heating rate was much higher than at a
low heating rate during the whole gasification process.
Microscopic characteristics of chars derived at
different heating rates and temperatures
Figure 5 shows the SEM photographs of Taiheiyo char
pyrolyzed at different heating rates (5 K/min for slow
heating) and different temperatures. It can be seen that
the surface of a char pyrolyzed at a low heating rate
was smooth, whereas that of a char pyrolyzed at a high
heating rate was rough and porous. This tendency was
pronounced as temperature increased.
Figures 6 and 7 show the SEM photographs of
McKinley char and Witbank char pyrolyzed at different
heating rates (5 K/min for slow heating) and different
temperatures. Similar to the case of Taiheiyo char, rapid
heating during pyrolysis led to rough and porous char
surface, which were supposed to be attributed to the
drastic release of volatile matter during pyrolysis at a
high heating rate.
Figure 5. SEM photographs of Taiheiyo char prepared
under slow and rapid heating conditions.
rates at 1473 K for the three coals used in this work,
pyrolyzed at various heating rates, were plotted in
Fig. 8. It can be seen that the initial reaction rate of
chars increased with both specific surface area and pore
volume. Figure 9 shows the correlation between the
initial reaction rate at 1673 K and the specific surface
area as well as the pore volume of chars pyrolyzed at
various heating rates. Similar to the tendency at 1473 K
shown in Fig. 8, the reaction rate at 1673 K was also
closely correlated to the specific surface and the pore
volume of char particles. These results implied that the
external diffusion is not as important as the diffusion
inside particles.
Correlation between microscopic
characteristics and reactivity of chars
DISCUSSION
Figure 8 shows the correlation between the initial
reaction rate and the specific surface area as well as the
pore volume of chars at 1473 K. The initial reaction
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
From the fact that both the microscopic structure of
particle and the gasification temperature influenced the
Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
DOI: 10.1002/apj
909
910
H. LIU et al.
(a) Slow heating (1473 K)
(c) Slow heating (1673 K)
Asia-Pacific Journal of Chemical Engineering
(b) Rapid heating (1473 K)
(d) Rapid heating (1673 K)
Figure 6. SEM photographs of McKinley char prepared
under slow and rapid heating conditions.
reactivity of a char, it was known that even at elevated
temperatures, the gasification of a char with CO2 was
controlled by both chemical reaction and diffusion
inside particles. The initial reaction rate of Witbank char
leveled off at high temperature, which was probably due
to ash fusion behavior. We do not think this was due to
external mass transfer resistance, or else the transition
from a low-temperature range to a high-temperature
range shown in Fig. 2 should be smoother. Besides, the
other two chars had higher initial reaction rates whereas
did not show similar tendency in the high-temperature
range.
The results of this work revealed the strong dependence of char reactivity on the pyrolysis conditions,
which implies that those kinetics of char gasification
with CO2 obtained at a slow heating rate are necessary
to be corrected when applied to a practical entrainedflow gasifier.
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
(a) Slow heating (1473 K)
(c) Slow heating (1673 K)
(b) Rapid heating (1473 K)
(d) Rapid heating (1673 K)
Figure 7. SEM photographs of Witbank char prepared
under slow and rapid heating conditions.
CONCLUSIONS
The effect of heating rate during pyrolysis on the gasification reactivity of three types of chars in CO2 was
investigated through experiments at elevated temperatures, with a uniquely made fluidized bed. The following conclusions were reached:
Even at elevated temperature, heating rate also has
significant influence on char reactivity of gasification.
A higher heating rate during pyrolysis leads to higher
char reactivity of gasification, whereas has only limited
effect on the activation energy of char gasification with
CO2 . The char reactivity is closely related to its specific
surface area and pore volume. Its high reactivity derived
from pyrolysis at a high heating rate is very likely owing
to its more porous structure resulted from the drastic
release of volatile matter at a high heating rate.
Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
DOI: 10.1002/apj
Asia-Pacific Journal of Chemical Engineering
Acknowledgements
1473 K
0.03
0.02
Initial reaction rate (1/s)
GASIFICATION REACTIVITY OF CHAR WITH CO2
This work is supported by the Foundation of State Key
Laboratory of Coal Combustion (China). The authors
also would like to thank NEDO/CCUJ for financial
support of this work under BRAIN-C program (Japan).
0.025
0.015
0.02
0.01
0.015
0.01
NOMENCLATURE
0.005
0.005
0
0
0
5
10
15
Specific surface area
0
20
(m2/g)
0.02 0.04 0.06 0.08
Pore volume
(cm3/g)
Correlation between initial reaction rate and
specific surface area as well as pore volume of char particle
at 1473 K. This figure is available in colour online at
www.apjChemEng.com.
Figure 8.
f
r0
rc
t
T
X
A parameter accounting for the effect of pore
structure of char particles
Initial reaction rate of gasification (1/s)
Reaction rate of gasification (1/s)
Reaction time (s)
Temperature (K)
Carbon conversion (−)
1673 K
Greek letters
0.02
0.03
Initial reaction rate (1/s)
0.025
τ (Reaction time/half life), dimensionless time (−)
0.015
0.02
REFERENCES
0.01
0.015
0.01
0.005
0.005
0
0
0 10 20 30 40 50 60 70 80
Specific surface area (m2/g)
0
0.005
0.01
0.015
Pore volume (cm3/g)
Correlation between initial reaction rate and
specific surface area as well as pore volume of char particle
at 1673 K. This figure is available in colour online at
www.apjChemEng.com.
Figure 9.
The effect of heating rate during pyrolysis on char
reactivity is pronounced at a low temperature, and
very different for various coal types, that is, strong
for low-rank coal but not so significant for high-rank
coal.
The gasification reactivity of a char is related to both
pore structure of chars and temperature, which suggests
that even at elevated temperatures, the gasification of a
char with CO2 was controlled by both chemical reaction
and diffusion inside particles.
These results revealed that it is necessary to derive
the gasification kinetics of a char at a high heating rate
to obtain valid kinetics for an entrained-flow gasifier.
 2010 Curtin University of Technology and John Wiley & Sons, Ltd.
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Asia-Pac. J. Chem. Eng. 2011; 6: 905–911
DOI: 10.1002/apj
911
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