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Fuel 169 (2016) 9398

Contents lists available at ScienceDirect

Fuel
journal homepage: www.elsevier.com/locate/fuel

Pyrolysis kinetics of soybean straw using thermogravimetric analysis

Xin Huang, Jing-Pei Cao , Xiao-Yan Zhao, Jing-Xian Wang, Xing Fan, Yun-Peng Zhao, Xian-Yong Wei
Key Laboratory of Coal Processing and Efficient Utilization, Ministry of Education, China University of Mining & Technology, Xuzhou 221116, Jiangsu, China

h i g h l i g h t s

The decomposition zone of soybean straw could be divided into three stages.

The kinetic of soybean straw pyrolysis was studied by three models.

Simulation of pyrolysis showed a good agreement with experimental data.

An insight for future applications of soybean straw was provided.

a r t i c l e

i n f o

Article history:
Received 25 September 2015
Received in revised form 30 November 2015
Accepted 10 December 2015
Available online 17 December 2015
Keywords:
Kinetics
Pyrolysis
Thermogravimetric analysis
Soybean straw
Biomass

a b s t r a c t
Thermochemical conversion of crops straw is receiving renewed attention, due to the energy and material recovery that can be achieved. However, it still lacks the kinetic background which is of great importance for a successful design of thermochemical process. In this work, pyrolysis test for soybean straw
was performed in a non-isothermal thermogravimetric analysis (TGA) in order to determine the thermal
degradation behavior. Pyrolysis experiments were carried out under inert conditions and operated at different heating rates (5, 10, 20, and 30 K/min). Three different kinetic models, iso-conversional Kissinger
AkahiraSunose (KAS), OzawaFlynnWall (OFW) models, and CoatsRedfern method were applied on
TGA data of soybean straw to calculate the kinetic parameters including activation energy, preexponential factor, and reaction order. The activation energy values were 154.15 and 156.22 kJ/mol based
on KAS and OFW models, respectively. Simulation of the soybean straw thermal decomposition using the
obtained kinetic parameters and comparison with experimental data are in good agreement.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
The utilization of biomass wastes including agricultural straw,
municipal solid waste, and livestock manure has attracted more
and more attention owing to their potential energy property. Agricultural application, landfill, and incineration are the most common disposal processes for the wastes, whereas the traditional
disposal routes are becoming increasingly unacceptable due to
land limitations and stringent regulations [1,2]. Alternatively,
using biomass wastes as energy feedstock for bio-fuel production
through thermochemical conversion is regarded as an environmentally friendly disposal route with potential economic benefits.
Several thermochemical conversion technologies, including pyrolysis, gasification, and liquefaction conversion, are currently under
development [3,4]. Among the techniques, pyrolysis is most widely
used in thermal decomposition process and effective for converting
biomass waste into useful products of gas, oil, and solid char in an
Corresponding author. Tel./fax: +86 516 83591059.
E-mail address: caojingpei@cumt.edu.cn (J.-P. Cao).
http://dx.doi.org/10.1016/j.fuel.2015.12.011
0016-2361/ 2015 Elsevier Ltd. All rights reserved.

oxygen-free atmosphere [3,5]. The combustible gas and the oil

products can be used as fuel due to their high calorific values [6].
Moreover, the bio-oil consists of various organic compounds which
can be used as feedstock for value-added chemicals [7,8].
Non-isothermal thermogravimetric analysis (TGA) is one of the
most common methods to investigate the kinetics of pyrolysis.
Accurate pyrolysis kinetic models are essential to the full utilization of particular biomass wastes. It also contributes to design reasonable, efficient, and competent process and scale to establish in
real industrial applications for energy generation. The degradation
of biomass wastes is a tremendously complex process, mainly due
to the large number and diverse nature of thermochemical reactions. Previous studies [9] showed that the pyrolysis of agricultural
biomass consists four individual conversion stages, i.e., moisture
evolution, decomposition of hemicellulose, cellulose, and then lignin. Hemicellulose, which is a branched polymer with a low degree
of polymerization, is normally decomposed at 493588 K, where
cellulose maintains highly ordered and stable crystalline
structures. As a result this, the cellulose undergoes decomposition
at 588673 K [10,11]. Lignin is a three-dimensional polymer

94

X. Huang et al. / Fuel 169 (2016) 9398

consisting of hydroxyl phenylpropane monomers, and bound adjacent to the cellulose fibers to form a lignocellulose. The lignin is
more refractory than the other two components, while having
functional groups with widely distributed thermal stability, and
this results in a board temperature range of decomposition from
433 to 1173 K [11,12].
In the present work, we investigate the kinetics of pyrolysis
process for soybean straw using TGA technique at different heating
rates (5, 10, 20, and 30 K/min) under argon atmosphere and determine the kinetic parameters through iso-conversional Kissinger
AkahiraSunose (KAS) and OzawaFlynnWall (OFW) models
and CoatsRedfern method. The physicochemical properties are
firstly determined by elemental analyzer and FTIR spectrometer.

iso-conversional KAS and OFW models and CoatsRedfern method

were applied on TGA data of soybean straw.
2.4.1. The KAS model
The KAS model [13,14] is one of the most widely used isoconversional methods to calculate pyrolysis kinetics, which is
based on the following expression:





b
AE
E
ln 2 ln

Rg
RT
a

where b is the heating rate (K/min), A is the pre-exponential factor

(min1), a is conversion rate which can be calculated with the lost
weight dividing by the total weight of soybean straw, and g(a) is a
function depending on the decomposition mechanism. In the plot of
lnb=T 2 versus 1=T, slope gives E=R where R numerical valued
8.314 J/(molK) is the gas constant. Doing so for the whole range
of conversion (01) will produce the activation energy for the progressing values of conversion.

2. Materials and methods

2.1. Material
The soybean straw sample was obtained from fields of Xuzhou,
China. It was pulverized to pass through a 40-mesh sieve followed
by drying at 380 K for 24 h and then stored in an airtight container
before use. Ultimate analysis was conducted with an Elementar
vario MACRO cube CHNS elemental determinator. Table 1 summarizes main characteristics of the soybean straw sample.
2.2. TGA
Pyrolysis tests were carried out in a simultaneous differential
thermogravimetric analyzer, which combines a heat flux type
DSC with a TGA (Mettler Toledo TGA/DSC Stare ESI-0910,
Switzerland; with a precision of temperature measurement
0.15 K, DSC sensitivity 0.1 mW and microbalance sensitivity
0.1 lg). Temperature programmed pyrolysis for soybean straw
was conducted under a dry argon atmosphere with a flow rate of
50 mL/min. Sample with mass of 1520 mg was inserted directly
into a ceramic crucible and temperature was ramped from room
temperature to 380 K and holding for 10 min, then heated to
1173 K with different heating rates of 5, 10, 20, and 30 K/min,
respectively. The data of thermogravimetry (TG) and derivative
thermogravimetry (DTG) were obtained using the software of the
analyzer. The experiments were replicated at least twice.
2.3. FTIR analysis
FTIR spectrum of soybean straw was recorded using a Nicolet
Magna 560 spectrometer, by collecting 128 scans at a resolution
of 4 cm1 in reflectance mode with measuring regions of
4000400 cm1.
2.4. Kinetic study
Biomass pyrolysis is a complex process because more than one
reaction is involved. A full kinetic analysis of the complex system is
generally not feasible, but some kinds of effective or average
kinetic description are still needed. In this work, pyrolysis reaction
kinetics was investigated by three different kinetic models, the

2.4.2. The OFW model

Another most common and widely accepted methods in scientific community to compute thermo-kinetic parameter from experimental data is the OFW model [15,16]. The OFW model used a
correlation of the heating rate of the samples, activation energy
and inverse temperature, which was originally used the Doyles
[17] approximation for the temperature integral. The final form
of the OFW equation is expressed as:

logb log


AE
E
 2:315  0:457
Rga
RT

It is evident that a linear plot of logb versus the inverse

temperature is sufficient in order to obtain the activation energy
corresponding to each conversion step.
2.4.3. The CoatsRedfern method
The CoatsRedfern integral method [18] which is derived from
Arrhenius equation was used to analyze the characters of pyrolysis
kinetics. Considering the KAS and OFW models are accurate
enough for the calculation of activation energy, the CoatsRedfern
method can be used to determine the pre-exponential factor as
well as the reaction order. The equations for numerical determination of the kinetic parameters using the CoatsRedferns method
are given below.






ln1  a
AR
2RT
E

ln
1


; n1
ln
bE
E
RT
T2
"
#



1  a1n  1
AR
2RT
E
ln
1

; n1
ln
2
bE
E
RT
n  1T

where n is the reaction order which describes the pyrolysis model.

h
i
a
verAs for first-order reaction (n = 1), the slope of curve ln ln1
T2
sus 1=T produce E=R, then the activation energy is derived. For
multistep reaction (n 1), activation energy can be calculated
through KAS or OFW models. Assuming 2RT  E, the intercept
can be arranged as lnAR=bE where A can be calculated.
3. Results and discussion

Table 1
Characteristics of soybean straw.
a

Proximate analysis (wt.%)

a
b

3.1. FTIR analysis

Ultimate analysis (daf, wt.%)

H/C

Mar

Ad

VMd

FCdb

Ob

1.8

4.7

75.5

19.8

47.8

6.9

1.0

0.1

44.3

A: ash; M: moisture; VM: volatile matter; FC: fixed carbon.

Calculated by difference.

1.73

The assignment of structural feature of the soybean straw is

based on published interpretation for FTIR spectral data and the
standard spectra in FTIR libraries, e.g., Aldrich Condensed Phase
FTIR Library [1922]. As shown in Fig. 1, the spectrum of the soybean straw shows a very strong and board absorption band at

95

1160
1246

1422
1733

2920
2850

Absorbance

1636

1055

3400

X. Huang et al. / Fuel 169 (2016) 9398

4000 3600 3200 2800 2400 2000 1600 1200 800

400

Wavemunber (cm-1)
Fig. 1. FTIR spectrum of soybean straw.

3400 cm1, which is ascribable to H-bonded OAH groups of cellulose [19]. Besides, the band at 2920 cm1 is corresponded to CAH
stretching within the methylene of cellulose. The absorption peaks
at 1733 and 1246 cm1 can be associated with the alkyl ester of
acetyl group in hemicellulose structure and/or the linkage between
hemicellulose and lignin [19]. The C@O groups in alkyl groups of
lignin side chains are suggested to conjugate with the aromatic
structure and result in an adsorption peak at 1636 cm1. The bands
at 2850, 1636, and 1422 cm1 have been attributed to absorption
due to CAH deformation within the methoxyl groups of lignin
[19,20]. The characteristic peaks of lignin were observed at
1320 cm1 (CAO of syringyl ring) and 1510 cm1 (aromatic skeletal vibration) [21]. The vibrations of these bands overlapped the
CAOAC glycosidic bond stretching at 1160 cm1, CAOAC ring
skeletal vibration at 1105 cm1 and CAOAH stretching of primary
and secondary alcohols at 1055 cm1 [19]. The absorption bands in
9301200 cm1 region correspond to the valent CAO, CAC, and
deformation vibrations of ring structures of CH2OH origin [22].

673 and 1173 K was observed, which should be associated with the
decomposition of lignin [24,25].
As shown in Fig. 2, the increase of heating rate contributes to
the deceleration of thermal degradation processes towards high
temperatures, which could be explained that a high heating rate
led the sample to the given temperature in a short time as a result
of increased thermal lag [26,27]. In addition, the yield of volatile
matter decreased slightly with increasing heating rate. At the temperature range from 453 to 773 K, the volatilizing yield is 76.3% at
5 K/min. This yield significantly decreases to 72.1%, 68.7% and
67.5% at 10, 20 and 30 K/min, respectively. On the other hand,
the decrease in heating rates only transferred the peak temperature to lower value without altering thermal profile of decomposition, which could be due to the increase in heat changing efficiency
at lower heating rates compared to higher heating rates. This conclusion is in good agreement with the study by Kim et al. [28], who
proposed that the maximum rate of decomposition increases with
increasing heating rates owing to increasing thermal energy.
3.3. Determination of activation energy
In order to determine the active energy of the pyrolysis of soybean straw, two different model-free, iso-conversion methods (KAS
and OFW models) were carried out. According to KAS and OFW
models, the activation energy can be determined from lnb=T 2
and logb, respectively. Fig. 3a illustrates the liner plot of lnb=T 2
versus 1=T where slopes give E=R at progressing conversion
degrees, while Fig. 3b depicts the linear plot of logb versus 1=T
where slopes give 0:457E=R at progressing conversion degrees.
It should be noticed that using the available experimental data, little or no correlation was observed for values of conversion below
0.1 and above 0.7 [29]. Due to a good correlation was observed
for most sets of experimental data and following the assumption
of the iso-conversional models concerning the constancy of activation energy, we could reliably exclude of some experimental data

3.2. Characteristics of thermal decomposition

80

-0.60

-0.45

-0.30
40
-0.15

0.00
0
373 473 573 673 773 873 973 1073 1173

Temperature (K)
Fig. 2. TG and DTG curves of soybean straw.

0.5

0.4

0.3

0.2

0.1

-10.4

-11.0

-11.6
1.6

1.4

60

20

0.6

1.2

log

5 K/min
10 K/min
20 K/min
30 K/min

= 0.7
-9.2

-9.8

(b)
DTG (% . s-1)

Weight loss (%)

100

(a)

ln( T2

The TG and DTG curves obtained from the pyrolysis of soybean

straw at heating rates of 5, 10, 20, and 30 K/min are shown in Fig. 2.
The decomposition zone of soybean straw could be divided into
three stages. The first one ranging from 383 to 453 K corresponded
to the moisture that the samples contained owing to the hygroscopic nature of soybean straw and very light volatiles [23]. The
main decomposition step took place between 453 and 673 K with
one strong peak around 613 K, which may be caused by the pyrolysis of hemicellulose and cellulose [11], whose existence is proved
by FTIR analysis in Fig. 1. Following the stage, a shoulder between

1.0
0.8

0.6
1.1

1.3

1.5

1.7

1.9

1/T (mK-1)
Fig. 3. Kinetic plot for soybean straw using KAS (a) and OFW models (b).

96

X. Huang et al. / Fuel 169 (2016) 9398

Table 2
Activation energies (E) for different conversion values obtained by KAS and OFW
models.
Conversion (a)

0.1
0.2
0.3
0.4
0.5
0.6
0.7
Average

KAS model

OFW model

Difference (%)

E (kJ/mol)

R2

E (kJ/mol)

R2

154.42
169.56
175.06
176.86
177.54
179.31
46.32
154.15

0.9188
0.9655
0.9827
0.9862
0.9836
0.9839
0.9779

155.20
170.07
175.64
177.63
178.58
179.71
56.69
156.22

0.9270
0.9690
0.9844
0.9876
0.9853
0.9828
0.9871

0.50
0.30
0.33
0.43
0.58
0.22
18.29
1.32

180

E (kJ . mol-1)

150

slopes in the plot of lnb=T 2 or logb versus 1=T may decrease

slightly, resulting in the decrease of activation energy. Damartzis
et al. [29] reported that the values of activation energy brought
the highest value difference close to 100120 kJ/mol for the pyrolysis of stems. Thus, the lower the activation energy is, the faster
the reaction rate is, because the activation energy is the minimum
energy requirement to start a reaction.

120
90
60
KAS model
OFW model

30
0.1

0.2

from 179.31 to 46.32 kJ/mol when the conversion value further

increased from 0.6 to 0.7 for KAS model. Same trend was founded
in activation energy values calculated from OFW model. The conversion from 0.6 to 0.7 corresponded to the temperature range
from 673 to 873 K, during the interactive pyrolysis of main lignin
and low residual cellulose occurred. Vamvuka et al. [27] reported
that cellulose decomposition had the highest activation energies
(145285 kJ/mol), whereas lignin decomposition had the lowest
(3039 kJ/mol) ones, which could be responsible for the obvious
decrease in activation energy with a conversion range of 0.60.7.
In addition, for conversion around 0.7 and temperatures higher
than 723 K, analysis of the activation energy values showed that
the soybean straw may be assigned to direct gasification, where
the kinetic parameters and rate limiting step could be controlled
by oxygen accessibility towards the residual solid [31]. On the
other hand, as the pyrolysis proceeded, a high heating rate led
the sample to the given conversion in high temperature by the reason of thermal lag. As a consequence of this, the absolute value of

0.3

0.4

0.5

0.6

0.7

Conversion ( )

3.4. Determination of pre-exponential factors

Fig. 4. Change in activation energy with progressing conversion for KAS and OFW
models.

because the lack of correlation would not greatly affect the quality
of the computed activation energy [29]. The calculated activation
energies and the respective correlation factor using KAS and
OFW models are listed in Table 2. The mean active energies calculated from KAS and OFW models are 154.15 and 156.22 kJ/mol,
respectively. Satisfactory agreement with a deviation of 1.32% indicated that the activation energy calculated using KAS and OFW
models were believable. Islam et al. [10] investigated the activation
energy with a deviation below 4% using KAS and OFW models in
pyrolysis of fruit hulls. The high agreement validated the reliability
of calculations and confirmed the predictive power of KAS and
OFW models [30].
The results of kinetic analysis show that activation energy is
highly depended on conversion which means that pyrolysis of soybean straw is a complex process involving different reactions. As
shown in Fig. 4, the activation energy values increased smoothly
as the conversion value increased from 0.1 to 0.3, and then kept
at a level within conversion range of 0.30.6, which should be
due to the pyrolysis of hemicellulose and cellulose. As the pyrolysis
proceeded, the activation energy values significantly decreased

The pyrolysis kinetic parameters as a function of conversion

could be determined using CoatsRedfern method. Since KAS and
OFW models are reliable enough, the activation energies calculated
by these models were fitted in order to estimate the
pre-exponential factor and the reaction order. In plot of
h
i
h
i
a
a1n 1
ln ln1
versus 1=T (for n = 1) or ln 1
versus 1=T (for
T2
n1T 2
n 1), slop gives E=R and the intercept is lnAR=bE where A
can be calculated [29]. Calculated pre-exponential factor values
and the reaction order are listed in Table 3. With raising the pyrolysis heating rate, the pre-exponential factor increased significantly
for both KAS and OFW models because of more complex reactions
involved in a shorter time. Reaction order was calculated through
mean value of activation energy and pre-exponential factor
obtained from KAS model [32].
3.5. Validation
After calculating the kinetic parameters of activation energy,
pre-exponential factor and reaction order estimated using KAS
model and CoatsRedfern method, the accuracy of these parameters should be proven in a satisfactory way. The simulation was
carried out for all of the experimental heating rates from 383 to
1173 K and the results are presented in Fig. 5. The simulation

Table 3
Calculated pre-exponential factors (A, min1).
KAS model
E (kJ/mol)
154.15

OFW model
b (K/min)
5
10
20
30

A (min1)

E (kJ/mol)

1
8.19
1
11.26
1
15.46
1
17.04

8.61E+14
5.16E+14
3.85E+14
6.73E+14
4.76E+13
4.08E+15
4.26E+13
5.78E+15

156.22

b (K/min)
5
10
20
30

A (min1)

1
8.30
1
11.43
1
15.72
1
17.31

9.93E+14
8.92E+14
4.42E+14
1.22E+15
5.47E+13
8.05E+15
4.89E+13
1.09E+16

97

X. Huang et al. / Fuel 169 (2016) 9398

1.0

5 K/min

10 K/min

Conversion ( )

0.8

0.6

0.4

0.2

0.0
1.0

n=1
n = 11.3
experiment

n=1
n = 8.2
experiment

20 K/min

30 K/min

Conversion ( )

0.8

0.6

0.4

0.0
373

n=1
n = 17.0
experiment

n=1
n = 15.5
experiment

0.2

473

573

673

773

873

973

1073 1173 373

473

Temperature (K)

573

673

773

873

973

1073 1173

Temperature (K)

Fig. 5. Simulation of soybean straw pyrolysis using the kinetic data calculated from KAS model.

results were in a good agreement with the experimental data for

conversion values. As described in Fig. 5, no obvious effect on the
predictive behavior of the model can be found with the increase
of pyrolysis heating rate in the plots of first-order reaction
(n = 1). In this case, CoatsRedfern method lacks of accuracy for
representing experimental results because the activation energy
and the pre-exponential factor were based solely on both heating
rate and pyrolysis temperature. On the other hand, for multistep
reactions (n 1), the pseudo-order n has no physical meaning
but plays an important role to fit parameter as can be thought as
correlation parameter of pyrolysis model.

4. Conclusions
In this study, the pyrolysis of soybean straw has been investigated under argon atmosphere by means of TGA at different heating rate (5, 10, 20, and 30 K/min). The maximum weight loss of
soybean straw was restricted in the temperature range of 453
673 K owing to the pyrolysis of hemicellulose and cellulose. Simulation of the materials thermal decomposition using obtained
kinetic parameters showed a good agreement with the experimental data. Taking into account of the low moisture and ash content,
the thermochemical system may provide an insight for future
application of soybean straw as a potential candidate for a resource
of energy and chemicals.
Acknowledgements
This work was subsidized by the Fundamental Research Funds
for the Central Universities (China University of Mining & Technology, Grants 2015XKQY05 and 2015QNA18), National Natural
Science Foundation of China (Grant 21206189), Natural Science
Foundation of Jiangsu Province (BK20151141), the Priority
Academic Program Development of Jiangsu Higher Education

Institutions, and the Strategic Chinese-Japanese Joint Research Program (Grant 2013DFG60060).

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