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Effect of Carbonization Temperature on Combustion

Reactivity of Bagasse Char
a
Surinder Katyal
a
Department of Chemical Engineering, The University of Sydney, Sydney, Australia

Available online: 23 Oct 2007

To cite this article: Surinder Katyal (2007): Effect of Carbonization Temperature on Combustion Reactivity of Bagasse Char,
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 Energy Sources, Part A, 29:1477–1485, 2007
Copyright © Taylor & Francis Group, LLC
ISSN: 1556-7036 print/1556-7230 online
DOI: 10.1080/00908310600710715

Effect of Carbonization Temperature on

Combustion Reactivity of Bagasse Char

SURINDER KATYAL
Department of Chemical Engineering
The University of Sydney
Sydney, Australia
Downloaded by [Oklahoma State University] at 11:12 30 October 2011

Abstract The combustion reactivity of bagasse chars was investigated under isother-
mal conditions at 400ıC in air. The bagasse char samples were prepared by carboniz-
ing bagasse in a fixed bed reactor at temperatures between 500ıC and 800ıC. It was
observed that raising the carbonization temperature resulted in a significant decrease
in reactivity of bagasse char. This was manifested by the decrease in the values of the
maximum reaction rate, average rate based on 50% burnout and conversion achieved
in 30 minutes with the increase in carbonization temperature. The decrease in reac-
tivity of bagasse char with carbonization temperature was attributed to changes in
the reactive components of bagasse.

Keywords bagasse, burnout, char, combustion, pyrolysis, reactivity

Introduction
The reactivity of a char is an important property that moderates its behavior during
combustion or gasification. The conditions under which a char is produced affects the
chemical, physical and structural properties of char and consequently the kinetics and
reactivity of char combustion or gasification (Smith et al., 1994). The reactivity of a char
is considered to depend on parameters used in its preparation such as heat treatment
temperature, heating rate, holding time, pressure, nature of gaseous atmosphere and type
of reactor. Among these factors, the effect of temperature is considered as the most
prominent. The reactivity of the char decreases with the increase in temperature at which
a char is produced during heat treatment. This effect has been observed for chars obtained
from coal (Smith and Polly, 1956; Jenkins et al., 1973; Radovic et al., 1983; Khan, 1987;
Kasaoka et al., 1987; Zhang et al., 1996) and from lignocellulosic materials (DeGroot
and Richards, 1988; Kannan and Richards, 1990; Kumar et al., 1992; Janse et al., 1998;
Devi and Kannan, 2000). Various reasons presented in the literature for decrease in
reactivity with carbonization temperature are the thermal annealing of active sites; reduced
accessibility of surface area and pores; decrease in volatile matter and repolymerization
of volatile matter; crystalline realignment; decrease in the catalytic activity of mineral
matter due to sintering if they have any activity; decrease in H and O contents or in
H/C and O/C ratios; decrease in the ratio of active surface area to total surface area

Address correspondence to Surinder Katyal, Department of Chemical Engineering and Tech-

nology, Panjab University, Chandigarh, India–160014. E-mail: skatyal@pu.ac.in

1477
 1478 S. Katyal

(Blake et al., 1967; Jenkins et al., 1973; Mahajan and Walker, 1973a; Ashu et al., 1978;
Laurendeau, 1978; Sahu et al., 1988; Devi and Kannan, 1990; Van Heek and Muhlen,
1991; Kashiwaya and Ishii, 1991; Cozzani, 2000).
The present study focuses on studying the effect of heat treatment temperature dur-
ing carbonization on the combustion reactivity in air of chars obtained from sugar cane
bagasse. Bagasse is a by-product of sugar cane processing and is traditionally combusted
in sugar mill boilers to meet internal energy needs. The bagasse char samples were
produced in a fixed bed pyrolysis reactor under flowing nitrogen gas at different temper-
atures. The reactivity of chars was obtained by means of isothermal thermogravimetry,
which is a widely used method to investigate the reactivity of carbonaceous/char materi-
als. There have been a few attempts to understand the combustion/gasification kinetics of
bagasse char under nitrogen-oxygen mixtures in the past (Luo and Stanmore, 1992a, b;
Villegas et al., 1998; Aguilar et al., 2001a, 2001b). However, the effect of heat treatment
Downloaded by [Oklahoma State University] at 11:12 30 October 2011

temperature on the combustion reactivity and burnout behavior has remained unexplored
for bagasse char and the present work is an attempt in this direction.

Experimental Work
The sugar cane bagasse used in this work was obtained from CSR Victoria Mill, Queens-
land, Australia. It was dried at 105ıC, ground and sieved to obtain the particles of
0.25–0.50 mm size fraction. The char samples were prepared by pyrolyzing the bagasse
in a fixed bed reactor at different heat treatment temperatures under inert nitrogen. The
details of the experimental set up and procedure has been reported elsewhere (Katyal
et al., 2003). In short, the bagasse samples were heated from ambient temperature to
the different temperatures of 500, 600, 700, and 800ı C at 20ıC/min and kept at that
temperature for 45 minutes. The char samples were then cooled to ambient temperature
under nitrogen. The char samples were ground and sieved to get particles of size less
than 150 m which were used for reactivity measurement.
The characterization of raw bagasse and char samples was carried out by conducting
proximate and ultimate analyses. The char reactivity was measured thermogravimetrically
using a TA Instrument Thermograviametric Analyser (TGA 2950). Approximately 3–
4 grams of the fine char samples were placed in the sample pan in the form of a single
layer and were heated from room temperature to 400ı C under nitrogen and kept at that
temperature to ensure thermally stable isothermal conditions. Air was then admitted to the
system by switching off nitrogen and maintained until the desired burnout was achieved
or no weight loss was observed. The flow rate of the gas (nitrogen or air) was maintained
at 40cc/min. The continuous records of weight loss, rate of weight loss with respect to
time were obtained for different chars and were further analyzed using TA Instruments
Universal Analysis software program.
The burnout was determined from the ratio of weight loss relative to initial weight
of char on a dry ash free basis as follows:

.Wo W /
XD (1)
.Wo Wash /

where Wo , W , and Wash represents the initial weight, the instantaneous weight of char
at any time and weight of ash. The reactive portion of char .Wo Wash / is the total
carbon available for combustion and .Wo W / is the amount combusted at any time.
The reaction rate R was determined from rate of weight loss (DTG) data at any time
 Carbonization Temperature on Reactivity of Char 1479

was related to the conversion as follows:

1 dW dX
RD D (2)
.Wo Wash / dt dt

The maximum reaction rate .Rm / corresponded to the maximum value of rate of weight
loss .dw=dt/max . It was considered as a measure of char reactivity and was termed as
maximum reactivity, as adopted by past workers (Jenkins et al., 1973; Devi and Kannan,
2000). The reaction rate at 25% conversion was also determined in addition to maximum
rate. Further, two more parameters, x30 and t0:5 were used to describe the char reactivity.
They were the fraction of char combusted on daf basis in 30 minutes and the time
consumed for first 50% burnout, respectively. The time, t0:5 was also used to determine
average combustion rate .R0:5 / using the following equation, as adopted by past workers
(Muira et al., 1989; Senneca et al., 1998):
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0:5
R0:5 D (3)
t0:5

Results and Discussion

Char Properties
The bagasse char samples produced at temperatures of 500ı C, 600ı C, 700ı C, and 800ıC
were designated as 500CTB, 600CTB, 700CTB, and 800CTB chars, respectively. Table 1
shows the yield of char samples as well as the proximate and ultimate analyses of raw

Table 1
Proximate and ultimate analysis of raw bagasse and bagasse char samples

Sample

Bagasse char

Raw
Analysis bagasse 500CTB 600CTB 700CTB 800CTB

Yield (%, dry bagasse basis) — 22.10 20.50 18.95 17.80

Proximate analysis
(%, dry basis)
Volatile matter 84.70 27.00 19.10 12.05 9.00
Ash content 2.20 9.00 10.50 12.10 15.10
Fixed carbon 13.10 64.00 66.90 74.95 75.90
Ultimate analysis
(%, dry ash free basis)
C 47.11 79.37 82.19 87.40 90.23
H 6.85 3.57 1.06 0.93 0.44
N 0.21 0.47 0.32 0.43 0.36
S 0.18 0.00 0.00 0.00 0.01
O 45.65 16.59 16.43 11.24 8.95
 1480 S. Katyal

bagasse and char samples. The yield of char samples decreased as the carbonization
temperature was increased due to the pyrolytic degradation of bagasse samples. The
yield of char decreased from 22.10% for 500CTB char to 17.80% for 800CTB char.
Previous studies on production of char from pyrolysis of bagasse in laboratory/pilot
scale equipments have also shown similar trends (Mobarek and Fahmy, 1982; Rodriguez
et al., 1987; Zanderson et al., 1999; Katyal et al., 2003). The major degradation of
bagasse is considered to occur between 350ıC–500ıC yielding volatiles (combustible
gases and condensable liquid tar) and devolatilized char. The degradation of bagasse
beyond 500ıC was much lower and slower and lead to very little decrease in char
yield (Katyal et al., 2003). Previous studies based on thermogravimetric analysis of
bagasse under inert conditions also suggest that the degradation start at 200ıC–225ıC and
continues mainly up to 400ıC–425ıC (Nassar, 1985; Roque-Diaz et al., 1985; Varhegyi
and Antal, 1988; Aimen and Stubington, 1993; Nassar et al., 1996). For this reason,
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the lowest heat treatment temperature chosen during carbonization in the present work
was 500ıC.
Table 1 demonstrates that the volatile matter of the char samples decreased and
corresponding fixed carbon and ash content increased continuously with increase in car-
bonization temperature. Similarly, the carbon content of the char samples increased at
the expense of all other elements. The 800CTB char produced at 800ıC had very high
carbon content of 90% and very low volatile matter of 9%.

Combustion Reactivity of Bagasse Char

Figure 1 shows the burnout level versus time curves under air at 400ı C of the four
char samples 500CTB, 600CTB, 700CTB and 800CTB. Figure 2 shows combustion rate
versus burnout levels curves for the char samples. Table 2 compares various combus-
tion reactivity parameters of the char samples. Figures 1 and 2 and Table 2 show that
the combustion reactivity of bagasse char decreased with increase in char carboniza-
tion temperature. The 500CTB and 600CTB chars were much more reactive than the
700CTB and 800CTB chars. The decrease in reactivity was more pronounced between
500CTB and 700CTB char, while smaller difference was manifested between 700CTB
and 800CTB char.

Figure 1. Comparison of conversion versus time curves for isothermal combustion at 400ıC of
bagasse char samples.
 Carbonization Temperature on Reactivity of Char 1481
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Figure 2. Comparison of rate versus conversion curves for isothermal combustion at 400ıC of
bagasse char samples.

The burnout versus time curves obtained for chars carbonized at higher temperatures
(700CTB and 800CTB) were linear, while the curves for chars carbonized at lower
temperatures (5000CTB and 600CTB) were linear to most of the conversion levels and
turned asymptotic thereafter as the reaction slowed down. The burnout of bagasse char
samples in a particular time decreased with the increase in char carbonization temperature.
The 800CTB char required more than three times longer to achieve complete burnout
as compared to that taken by 500CTB char. Similarly, the time required to achieve 50%
burnout was 55.61 minutes for 800CTB char as compared to 8.39 minutes for 500CTB
char, demonstrating an increase of more 6.5 times.
The burnout versus conversion curves obtained for 700CTB and 800CTB chars were
flat to most of the conversion levels, further indicating that the combustion rates for
these chars were weak and low. On the other hand, the combustion rates for 500CTB
and 600CTB chars manifested an increase with conversion leading up to maxima and ul-
timately declining towards zero. The increase in reactivity up to intermediate conversion
values has been attributed in literature to an increase in surface area as the combustion
reaction proceeds. At higher conversion levels, pores become more open and too wide
and become accessible to the transport of gas phase reaction participants as combus-
tion reaction proceeds, leading to a decrease in rate (Jenkins et al., 1973; Mahajan and
Walker, 1978a, 1978b). Figure 2 shows that the combustion rate of chars decreased at

Table 2
Reactivity parameters for isothermal combustion at 400ıC
of bagasse char samples

Bagasse Rm  102 , xm , t0:5 , R0:5  102 , x30,

char sample %/min % min %/min %

500CTB 10.80 10.50 8.39 5.96 97.15

600CTB 8.09 13.08 10.49 4.77 93.25
700CTB 1.90 28.71 32.04 1.56 47.04
800CTB 1.43 36.43 55.61 0.90 21.85
 1482 S. Katyal

all conversion levels with the increase in carbonization temperature. The maximum rate
decreased from 10.80%/min for 500CTB char to 1.43%/min for 800CTB char. The max-
imum rate of 500CTB char was 1.33, 5.62, and 7.55 times that of 600CTB, 700CTB,
and 800CTB chars, respectively. The converison corresponding to the maximum rate
.xm / also increased with increase in carbonization temperature, as shown in Table 2.
Similar behavioral trend about decrease in reactivity is observed for average reaction
rate based on 50% burnout and burnout achieved in 30 minutes. The time, t0:5 increased
from 8.39 minutes for 500CTB char to 55.61 minutes for 800CTB char and the corre-
sponding rate R0:5 decreased from 5:96  10 2 %/min for 500CTB char to 8:99  10 2
%/min for 800CTB char. Similarly, x30 , decreased from 97% for 500CTB char to 22%
for 800CTB char, indicating decrease in reactivity. Figure 3 shows the relationship be-
tween the maximum reaction rate, average rate based on 50% burnout, and reaction rate
at 25% burnout value and corroborate decreasing trend of reactivity with carbonization
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temperature.
The decrease in the reactivity of bagasse char samples in the present study could
be attributed to significant changes in the chemical composition of the present char
samples observed with the increase in the carbonization temperature. There was a con-
tinuous decrease in O and H content, H/C and O/C ratios, and volatile content with
an increase in the carbonization temperature. The O, H, H/C, and VM decreased from
16.59%, 3.57%, 4:50  10 2 , and 27%, respectively, for 500CTB char to 8.95%, 0.44%,
4:88  10 3, and 9%, respectively, for 800CTB char. An unpublished study conducted on
the bagasse char samples prepared from precursor bagasse and under conditions similar
to the present work, suggested that the surface area decreased and the pore structure
underwent changes as the char preparation temperature was increased from 600ıC to
800ıC (Syna, 2006). The results obtained in the present work are consistent with the
past research studies conducted on studying reactivity during combustion/gasification
of carbonacous materials (Jenkins et al., 1973; Radovic et al., 1983; Senneca et al.,
1997, 1998; Janse et al., 1998; Cozzani, 2000; Devi and Kannan, 2000; Miguel et al.,
2003). Therefore, the decrease in the reactivity of char at higher carbonization temper-
atures could be attributed to a combination of the degradation of reactive components

Figure 3. Relationship between carbonization temperature and combustion rates for isothermal
combustion at 400ıC of bagasse char samples.
 Carbonization Temperature on Reactivity of Char 1483

of char; and possible changes in surface area, pore size and structure and other physical
characteristics.

Conclusions
From the results obtained in the present work, it can be concluded that the reactivity
of bagasse char samples decreased with increase in char carbonization temperature. The
various combustion reactivity indicators such as maximum rate, time required to achieve
50% burnout, average rate based on 50% burnout, fraction of char combusted in 30
minutes showed a decline with increase in char carbonization temperature. The decrease in
reactivity was much higher as char carbonization temperature was increased from 500ıC
to 700ıC, while smaller difference in reactivity was manifested as the char carbonization
temperature was raised from 700ıC to 800ıC.
Downloaded by [Oklahoma State University] at 11:12 30 October 2011

Acknowledgments
The author would like to thank Dr. Marjorie Valix and Prof. Brian S. Haynes, Department
of Chemical Engineering, The University of Sydney, Australia, for their contribution to
this work. The author would also like to thank Key Center for Polymer Colloids, The
University of Sydney, Australia for providing TGA facility for experimental work.

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Nomenclature
R reaction rate (%/minute)
Rm maximum reaction rate (%/minute)
t time (minutes)
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t0:5 time consumed for first 50% burnout of char (minutes)

T temperature (ıC or K)
W weight of the bagasse char sample at any time t (mg, %)
Wo weight of the bagasse char sample initially (mg, %)
Wash weight of the ash obtained at the end of reaction (mg, %)
x fractional conversion or burnout (dimensionless)
x30 fractional conversion or burnout achieved on daf basis in 30 minutes
(dimensionless)
xm fractional converison or burnout corresponding to the maximum reaction rate
(dimensionless)