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Energy Sources, Part A, 33:620–630, 2011
Copyright © Taylor & Francis Group, LLC
ISSN: 1556-7036 print/1556-7230 online
DOI: 10.1080/15567030903226256
Non-isothermal Determination of the
Pyrolysis Kinetics of a Mixture of
Olive Residue and Polystyrene
A. ABOULKAS,1;2 K. EL HARFI,1;2 A. EL BOUADILI,2 and
M. NADIFIYINE1
1Laboratoire de Recherche sur la Réactivités des Matériaux et l’Optimisation
des Procédés, Département de chimie, Faculté des Sciences Semlalia,
Université Cadi Ayyad, Marrakech, Morocco2Laboratoire Interdisciplinaire de Recherche en Sciences et Techniques,
Faculté polydisciplinaire de Béni-Mellal, Université Sultan Moulay Slimane,
BP 592, 23000 Béni-Mellal, Morocco
Abstract Pyrolysis of olive residue, polystyrene and their mixture (1:1 weight ra-tio) were investigated by thermogravimetry. Experiments were conducted under N2
atmosphere at four heating rate of 2, 10, 20, and 50 K/min from room temperatureto 900 K. The results showed that the thermal degradation temperature range of
olive residue was 430–660 K, while that of polystyrene was 580–800 K. In general,we can note that the domains of degradation are well differentiated. Discrepan-
cies between the experimental and calculated TG/DTG profiles were considered asa measurement of the extent of interactions occurring on co-pyrolysis. The maxi-
mum degradation temperatures of polystyrene in the mixture were higher than thepolystyrene pure. The calculated residue was found to be higher than experimental.
These experimental results indicate a significant synergistic effect during pyrolysisof mixture of olive residue and polystyrene at the high temperature region. The
kinetic studies were performed using the Friedman kinetic-modeling equation. Theoverall activation energies were: 165 and 219 kJ/mole for hemicellulose and cellu-
lose, respectively; 180 kJ/mole for polystyrene; and 160, 215, and 166 kJ/mole forhemicellulose, cellulose, and polystyrene in the mixture, respectively. Thus, it has
been found that there exists an overall synergy, when two materials were pyrolyzedtogether.
Keywords kinetic, non-isothermal, olive residue, polystyrene, pyrolysis
1. Introduction
As most plastics are not biodegradable, their deposition in landfills is not a desir-
able solution from an environmental standpoint. There is also a lot of controversy
about the incineration of these wastes, due to the release of toxic and greenhouse
gases. Another disadvantage of the traditional incineration of these wastes is that it
Address correspondence to Dr. A. Aboulkas, Laboratoire de Recherche sur la Réactivités desMatériaux et l’Optimisation des Procédés, Département de chimie, Faculté des Sciences Semlalia,Université Cadi Ayyad, BP 2390, Marrakech 40001, Morocco. E-mail: [email protected]
620
Pyrolysis Kinetics of Olive Residue and Polystyrene 621
completely destroys all of its organic matter, which could be otherwise valuable for
different applications. Another type of waste that raises some environmental questions
is biomass waste. Its accumulation and its organic and energetic potential are wasted in
this manner.
Upgrading of these wastes is a necessity both for environmental protection and for
sustainable development. One of the promising ways of taking profit of the energy value
of these wastes is by pyrolysis. Co-pyrolytic techniques have received much attention in
recent years because they provide an attractive way to dispose of and convert polyolefins
and biomass into higher value fuel, and the specific benefits of this method potentially
include: the reduction of the volume of waste; the recovery of chemicals; and the
replacement of fossil fuels (Rutkowski and Kubacki, 2006; Sharypov et al., 2002; Marin
et al., 2002; Bernardo et al., 2009).
Thermogravimetric analysis (TGA) is one of the most common techniques used
to investigate thermal events and kinetics during pyrolysis of solid raw materials such
as biomass, plastic, coal and oil shale (Kok and Pamir, 1999; Kok and Iscan, 2007;
Aboulkas et al., 2007, 2008; Aboulkas and El Harfi, 2009; Caballero et al., 1997; Sorum
et al., 2001; Garcia-Perez et al., 2001). It provides a measurement of weight loss of
the sample as a function of time and temperature. The understanding of kinetics of the
thermal decomposition of fuels or fuel mixtures is crucial to the design and operation
of conversion systems. The thermal decomposition of biomass-derived materials has
been studied (Caballero et al., 1997; Sorum et al., 2001; Garcia-Perez et al., 2001).
Two peaks that appear in thermogravimetric curves are due to hemicellulose (the first
one) and cellulose (the second one), whereas lignin decomposes in a broad range of
temperatures. Numerous studies on the thermal decomposition of polyolefin and, in
particular, polystyrene have been carried out, especially in inert atmosphere (Sorum et al.,
2001; Heikkinen et al., 2004; Encinar and Gonzalez, 2008). Polyolefinic materials, such
as polystyrene, show a different behavior to lignocellulosic materials. Under pyrolysis
conditions, the material decomposition starts at approximately 673 K and progresses
very rapidly up to 723–743 K without producing solid residue that could be used
as combustible for supplying energy to the global process. Consequently, knowledge
of the thermal behavior of mixtures based on cellulose materials and polymers is of
great importance from the processing point of view. In this sense, many reports in
the literature were devoted to the analysis of the effect of co-pyrolysis of cellulose
derivatives and synthetic polymer mixtures (Sharypov et al., 2002; Aboulkas et al.,
2008; Aboulkas and El Harfi, 2009; Zhou et al., 2006; Jakab et al., 2000, 2001).
Zhou et al. (2006) investigated the thermogravimetric characteristics of the pyrolysis
of plastic/biomass mixtures using a thermogravimetric analyzer under heating rate of
20ıC/min from room temperature to 650ıC. The results obtained from this comprehensive
investigation indicated that plastic was decomposed in the temperature range 438–521ıC,
while the thermal degradation temperature of biomass is 292-480ıC. The difference of
weight loss .�W / between experimental and theoretical ones, calculated as algebraic
sums of those from each separated component, is about 6–12% at 530–650ıC. These
experimental results indicate a significant synergistic effect during plastic and biomass co-
pyrolysis at the high temperature region. Sharypov et al. (2002) examined the combination
of biomass with synthetic polymer mixtures and reported that biomass is thermally
degraded at a lower temperature than the polyolefin and independent thermal behaviors
were observed for each component of biomass/plastic mixtures. Jakab et al. (2000, 2001)
analyzed the effect of the presence of cellulose derivatives on thermal decomposition of
vinyl polymers. The presence of lignocellulosic materials slightly affects high-density
622 A. Aboulkas et al.
polyethylene decomposition, as the main degradation processes of cellulose derivatives
have ended before high-density polyethylene begins to degrade. On the other hand,
the effect of the presence of polypropylene on the thermal decomposition of cellulose
derivatives was negligible. When degradation of biomass and polystyrene mixtures was
evaluated, the yield of monomer, dimmer, and trimmer from polystyrene decomposition
was reduced, indicating that the radical chain reactions and intramolecular hydrogen
transfer reactions were hindered by the presence of lignocellulose char (Jakab et al.,
2000).
In the present work, behavior of pyrolysis of olive residue/polystyrene mixture was
investigated under an inert atmosphere using thermogravimetry to obtain an overall
understanding of the interaction of olive residue and polystyrene wastes. The thermal
events taking place during pyrolysis of olive residue/polystyrene were identified and the
kinetic data were obtained to fit thermogravimetric data by an isoconversional Friedman
method.
2. Experimental
2.1. Materials and Samples Preparation
The olive residue were obtained from the Marrakech area, which is located about 300 Km
of Rabat. Olive residue was obtained from the solid product of the traditional olive oil
process (Maâsra in Morocco). Air-dried olive residues were ground to obtain a uniform
material of an average particle size (0.2 mm). The characterizations of the olive residue
are given in Table 1.
The samples of polystyrene were provided by Plador (Marrakech, Morocco); the re-
sults of characterization of this material are given in Table 1. The olive residue/polystyrene
mixture (1:1 weight ratio) was blended by tumbling for 30 min in order to achieve
homogeneity. In all experiments, samples were around 20 mg with particle sizes ranging
approximately from 0.1 and 0.2 mm.
Table 1
Main characteristics of the olive residue and
polystyrene materials studied in wt%
Olive residue Polystyrene
Proximate analysis
Moisture 7.3 —
Volatile matter 74.8 99.6
Ash 5.1 —
Fixed carbon 12.8 0.4
Elemental analysis
C 50.95 91.5
H 5.28 8.5
N — —
O 38.63 —
S — —
Pyrolysis Kinetics of Olive Residue and Polystyrene 623
2.2. Experimental Techniques
Olive residue, polystyrene, and their mixture samples were subjected to TGA in an
inert atmosphere of nitrogen. Rheometrix Scientific STA 1500 TGA analyzer (Rheometic
Scientific, Piscataway, NJ) was used to measure and record the sample mass change with
temperatures over the course of the pyrolysis reaction. Thermogravimetric curves were
obtained at four different heating rates (2, 10, 20, and 50 K min�1) between 300 and
975 K; the precision of reported temperatures was estimated to be ˙2ıC. Nitrogen gas
was used as an inert purge gas to displace air in the pyrolysis zone, thus avoiding
unwanted oxidation of the sample. A flow rate of around 60 ml min�1 was fed to the
system from a point below the sample and a purge time of 60 min (to be sure the air was
eliminated from the system and the atmosphere is inert). The balance can hold a maximum
of 45 mg; therefore, all sample amounts used in this study averaged approximately 20 mg.
The reproducibility of the experiments is acceptable and the experimental data presented
in this article corresponding to the different operating conditions are the mean values of
runs carried out two or three times.
3. Results and Discussion
3.1. Thermal Degradation of Materials and Their Mixture
The weight loss (TG) and its derivative (DTG) for the isolated materials (olive residue
and polystyrene) and their mixture (1:1 mass) at heating rate of 10 K/min are shown in
Figures 1 and 2, respectively. The curves obtained at all heating rates were similar and
the characteristic temperatures are listed in Table 2. It can be seen that the domains of
degradation are well differentiated. The olive residue decomposes at lower temperatures
than polystyrene. It should be added that the major weight lefts of the olive residue and
polystyrene occur at 447–572 and 621–745 K, respectively. The characteristic tempera-
tures for the mixtures change only slightly in comparison with those for each component.
The TG and DTG curves of olive residue showed a slight mass loss occurring
from room temperature to about 420 K due to the loss of water present in the material
and external water bounded by surface tension. The thermal degradation of the olive
residue starts at approximately 430 K, and there follows a major loss of mass where the
Figure 1. Weight loss vs. temperature of pyrolysis of olive residue, polystyrene, and their mixture
(1:1 mass) at 10 K/min.
624 A. Aboulkas et al.
Figure 2. Derivative of weight loss vs. temperature of pyrolysis of olive residue, polystyrene, and
their mixture (1:1 mass) at 10 K/min.
main devolatilization occurs and is essentially complete by approximately 660 K. This
is followed by a slow further loss of mass until 923 K, after which there is essentially
no further loss of mass. The residual weight amounted to around 22%. From Figures 1
and 2, it can be seen that the weight left of polystyrene shows that its degradation occurs
almost totally in a one-step process as can be concluded by the presence of only one peak
in DTG. The polystyrene thermal degradation starts at 620 K and is almost complete at
approximately 745 K with a maximum rate of weight left at 708 K. In the mixture, the
TG and DTG curves show clearly three steps. The first step, obtained in the temperature
range of 453–573 K, is attributed to the decomposition of hemicelluloses. The second
step occurs between 573 and 630 K, which corresponds to the decomposition of cellulose.
The third step occurring between 640 and 754 K was attributed to the decomposition of
polystyrene and lignin in the mixture.
To investigate whether interactions existed between the olive residue and polystyrene,
a theoretical TG/DTG curve was calculated. This curve represented the sum of individual
components behavior in the mixture:
wsum D x1wolive residue C x2wpolystyrene;
where wolive residue, wpolystyrene are weight loss of each material in the same operational
condition and x1, x2 are the mass fractions of olive residue and polystyrene, respectively,
in the mixture. The calculated and experimental curves for olive residue/polystyrene
mixture at 10 K/min are illustrated in Figure 3. We can note that the olive residue
was not affected by the presence of polystyrene. However, the temperature of the DTG
maximum of polystyrene shifted to higher temperatures in the presence of olive residue.
The maximum temperature increased by 10–16ıC. Comparing the TG/DTG curves, some
discrepancies between experimental and calculated curves are observed. The presence of
olive residue resulted in the increase of weight loss of polystyrene pyrolysis. Again, the
residue obtained was found to be lower than the calculated value. Hence, there may be
synergistic interaction between olive residue and polystyrene, when they are co-pyrolyzed.
This synergistic interaction is probably due to the fact that the products formed during
olive residue degradation may influence polystyrene degradation. These results are in
good agreement with those of Jakab et al. (2001). It was shown that the char issued
biomass shifts to a higher temperature of the thermal degradation of polystyrene and the
Ta
ble
2
Ch
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Py
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Py
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Oli
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625
626 A. Aboulkas et al.
Figure 3. Comparison between experimental and calculated TG/DTG values for the olive
residue/polystyrene mixture at 10 K/min.
product distribution changes significantly. This effect is explained by the fact that the
radical chain reactions and intramolecular hydrogen transfer reactions have been hindered
by the presence of lignocellulosic chars. Zhou et al. (2006) found that the reaction of
hydrogen transferring from a polyolefinic chain to biomass-derived radicals will stabilize
the primary products from cellulose thermal degradation. This would result in higher
weight loss and lower yield of char.
3.2. Kinetic Analysis
Non-isothermal kinetic study of weight loss under pyrolysis of carbonaceous materials
is an extremely complex task because of the presence of numerous complex components
and their parallel and consecutive reactions.
The extent of conversion or the fraction of pyrolyzed material, x, is defined by the
expression,
x Dm0 � m
m0 � mf
; (1)
where m is the mass of the sample at a given time t ; m0 and mf refer to values at the
beginning and the end of the mass event of interest.
The rate of the kinetic process can be described by Eq. (2):
dx
dtD K.T /f .x/; (2)
where K.T / is a temperature-dependent reaction rate constant and f .˛/ is a depen-
dent kinetic model function. There is an Arrhenius-type dependency between k.T / and
temperature according to Eq. (3),
K.T / D A exp
�
�E
RT
�
; (3)
where A is the pre-exponential factor (usually assumed to be independent of temperature),
E is the apparent activation energy, T is the absolute temperature, and R is the gas
constant.
Pyrolysis Kinetics of Olive Residue and Polystyrene 627
The isoconversional Friedman method (Friedman, 1964) was adopted in this work
for the kinetic analysis of the thermogravimetric curves of these materials. This method
is directly based on Eq. (2) whose logarithm is
ln
�
dx
dt
�
D lnŒAf .x/� �E
RT: (4)
Plotting ln.dxdt
/ versus 1T
at a given conversion yields a straight line of slope �E=R.
Isoconversional Friedman plots obtained for olive residue are shown in Figure 4,
where two regions can be clearly identified. It is assumed that the first process corresponds
to the hemicellulose degradation, while the second one corresponds to the cellulose
degradation. The average Ea, calculated in such way for the first region, was 165 kJ
mol�1, while Ea for the second region was 219 kJ mol�1. The calculated apparent
activation energies for the pyrolysis of biomass reported in the literature varied over a
wide range. Senneca et al. (2002) found activation energies of 148 and 235 kJ mol�1 for
degradation of hemicellulose and cellulose, respectively. Teng and Wei (1998) found
activation energies of 155 and 199 kJ mol�1 for degradation of hemicellulose and
cellulose, respectively.
A similar study was carried out for the polystyrene. Figure 5 shows the isoconver-
sional Friedman plots for polystyrene. From the slopes, the average Ea for 0:1 < x < 0:9
was 180 kJ mol�1. Ea values do not change significantly with conversion (as can be
concluded from the slopes in Figure 5). The calculated apparent activation energies
reported in the literature for polystyrene varied over a wide range. Similar results were
obtained by Wu et al. (1993) on the pyrolysis of plastic mixtures of MSW and the apparent
activation energy of polystyrene degradation was found to be 172 kJ/mol, whereas Encinar
and Gonzalez (2008) found the polystyrene degradation activation energy to be 137
kJ/mol. Aguado et al. (2003) reported activation energy of polystyrene degradation to
be 123 kJ/mol, while Sorum et al. (2001) found the polystyrene degradation activation
energy to be 312 kJ/mol.
The Friedman method was also applied to the study of thermal degradation of
the olive residue/polystyrene mixture. The isoconversional Friedman plots are shown in
Figure 6. It is possible to take three different regions corresponding to both degradation
Figure 4. Friedman plots for olive residue degradation.
628 A. Aboulkas et al.
Figure 5. Friedman plots for polystyrene degradation.
processes. Activation energies calculated were 160 kJ mol�1 for the hemicellulose degra-
dation, 216 kJ mol�1 for the cellulose degradation, and 166 kJ mol�1 for the polystyrene
degradation in the mixture. When comparing these results with those of the thermal
decomposition of the pure materials, it is noteworthy that the activation energy for the
pyrolysis of polystyrene in the mixture was found to be less than that of pure polystyrene,
and the activation energies of the first two stages of olive residue in the mixture do
not significantly change. This showed that the presence of olive residue resulted in the
reduction of activation energy of the pyrolysis of polystyrene.
The reduction in the activation energy and the increase in the temperature of the
maximum degradation reveal the synergism of the co-pyrolysis of olive residue with
polystyrene. Similar results were obtained by Zhou et al. (2006) and Aboulkas et al.
(2008) on the co-pyrolysis of biomass with plastic. This is probably due to the influence
of products formed during olive residue degradation on polystyrene degradation. This
behavior was also noted for blends of biomass derivatives with other common polymers,
such as polystyrene, with changes in the mechanism of thermal degradation (Jakab et al.,
2000).
Figure 6. Friedman plots for olive residue/polystyrene degradation.
Pyrolysis Kinetics of Olive Residue and Polystyrene 629
4. Conclusions
From the TG and DTG curves, it can be seen that the domains of degradation of olive
residue and polystyrene are well differentiated. The olive residue decomposes at lower
temperatures than polystyrene. The major weight lefts of the olive residue and polystyrene
occur at 447–572 and 621–745 K, respectively.
Comparing the TG/DTG curves, discrepancies between experimental and calculated
curves are observed. It can be seen that the olive residue was not affected by the presence
of polystyrene. However, the temperature of the DTG maximum of polystyrene shifted to
higher temperatures in the presence of olive residue. The presence of olive residue resulted
in the increase of weight loss of polystyrene pyrolysis. Again, the residue obtained was
found to be lower than the calculated value. Hence, there may be synergistic interaction
between olive residue and polystyrene, when they are co-pyrolyzed.
The activation energy for the pyrolysis of polystyrene in the mixture was found to
be less than that of pure polystyrene, and the activation energies of the first two stages of
olive residue in the mixture do not significantly change. This showed that the presence of
olive residue resulted in the reduction of activation energy of the pyrolysis of polystyrene.
The reduction in the activation energy and the increase in the temperature of the
maximum degradation reveal the synergism of the co-pyrolysis of olive residue with
polystyrene. This is probably due to the fact that the radical chain reactions and in-
tramolecular hydrogen transfer reactions have been hindered by the presence of products
formed during olive residue.
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