Waste Management 30 (2010) 12201224

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Waste Management
journal homepage: www.elsevier.com/locate/wasman

Valorisation of waste tyre by pyrolysis in a moving bed reactor

E. Ayln, A. Fernndez-Colino, R. Murillo *, M.V. Navarro, T. Garca, A.M. Mastral
Instituto de Carboqumica, CSIC, M Luesma Castan 4, 50018-Zaragoza, Spain

a r t i c l e i n f o a b s t r a c t

Article history: The aim of this work is to assess the behaviour of a moving bed reactor, based on a screw transporter
Received 14 July 2009 design, in waste tyre pyrolysis under several experimental conditions. Waste tyre represents a signicant
Accepted 2 October 2009 problem in developed countries and it is necessary to develop new technology that could easily process
Available online 6 November 2009
big amounts of this potentially raw material. In this work, the inuence of the main pyrolysis process
variables (temperature, solid residence time, mass ow rate and inert gas ow) has been studied by a
thorough analysis of product yields and properties. It has been found that regardless the process opera-
tional parameters, a total waste tyre devolatilisation is achieved, producing a pyrolytic carbon black with
a volatile matter content under 5 wt.%. In addition, it has been proven that, in the range studied, the most
inuencing process variables are temperature and solid mass ow rate, mainly because both variables
modify the gas residence time inside the reactor. In addition, it has been found that the modication
of these variables affects to the chemical properties of the products. This fact is mainly associated to
the different cracking reaction of the primary pyrolysis products.
2009 Elsevier Ltd. All rights reserved.

1. Introduction
In the developed countries, approximately one used tyre per ca-
pita and per year is produced. Scrap tyres suppose a special chal-
lenge for their disposal or reuse because of their size, shape and
physicochemical properties. In order to deal with residues disposal,
the European Commission in the Landll of Waste Directive (Euro-
pean Commission, 1999) proposes the following routine: to reduce,
to reuse, to recycle and, nally, to perform an energy valorisation
process. Although it would be desirable to implement only the
three rst strategies, waste tyre generation is so high that it is
unavoidable to make use of the energy valorisation processes.
Scrap tyres have high-volatile, moderate sulfur content and low-
ash contents with a caloric value greater than that of coal or bio-
mass. These properties make it an ideal material for thermochem-
ical treatments (combustion, pyrolysis and gasication). Among
these processes, pyrolysis would be very interesting because not
only valuable products can be obtained but low emissions are also
generated, since approximately only 20% of the raw material is -
nally burnt (Murillo et al., 2006) to provide the internal energy
demand.
In the pyrolysis process, the organic volatile matter of tyres
(mainly the rubber polymer/s) is decomposed to low molecular
weight products, liquids or gases. The inorganic components and
the non-volatile carbon black remain as a solid residue which is
relatively unaltered, and therefore can be recycled in worthwhile
applications. The derived oils can be used as fuels or as a source
* Corresponding author. Tel.: +34 976 733977; fax: +34 976 733318.
E-mail address: ramonm@icb.csic.es (R. Murillo).
of rened chemicals (Laresgoiti et al., 2004). Gases are also useful
as fuels and the solid char may be used either as smokeless fuel,
carbon black or activated carbon precursor (Laresgoiti et al.,
2000; Berrueco et al., 2005).
There are a number of studies in the literature related to tyre
pyrolysis carrying out very different experimental procedures,
ranging from laboratory to commercial scale plants. Such studies
have been focused on different items of the pyrolysis process, such
as kinetics, reactor design, products characterisation, economics,
etc. Results obtained are related not only to the feedstock and
operating conditions used for the experiments, but also to the spe-
cic characteristics of the system used, such as type of reactor, ef-
ciency of heat transfer, etc.
Beyond laboratory scale, some bench scale experimental studies
on the disposal of scrap tyres have already been reported by vari-
ous researchers but many problems are still far from solution.
Within this context, Roqul et al. (2008) have developed a batch
system where the solid is fed from a chamber placed on top of a
xed-bed re-tube heating reactor with a power system. Cunliffe
and Williams (1998) have studied the pyrolysis of tyres including
the steel core in a static-bed batch reactor. Roy et al. (1990) and
Pakdel et al. (2001) worked in two different vacuum systems able
to process up to 32 kg/h. The main part of this system is a 3 m long
reactor composed by two horizontal heating plates, one on top of
the other, heated by commercial eutectic molten salts circulating
counter-currently with the feedstock. The feedstock is conveyed
over both heating plates while being agitated. Dai et al. (2001) used
an experimental unit which consists of ve components: a com-
bustion chamber, a variable-speed screw feeder that can be placed
at two different levels along a Circulating Fluidized Bed, a reactor

0956-053X/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.wasman.2009.10.001
 E. Ayln et al. / Waste Management 30 (2010) 12201224 1221

assembly with two cyclone separators, a cooling system and a gas- Table 1
circulating pump and preheating system. This system is used to Experimental pyrolysis conditions.

process 5 kg/h of tyre powder. Diez et al. (2005) compared results Experiment T (K) Solid residence Mass ow rate Inert gas ow
obtained at two different working scales, laboratory batch experi- time (min) (kg/h) (l N/h)
ments with 50 g of ground tyre shreds and bench scale experi- T 873 873 3.7 3.5 11.4
ments of batches of 20 kg. The bench plant consists of a T 973 973 3.7 3.5 11.4
discontinuous feeding system and an electrically heated chamber T 1073 1073 3.7 3.5 11.4
SRT 1 873 5.3 3.5 11.4
containing a wormscrew that pushes the shredded tyre material SRT 2 873 3.7 3.5 11.4
through the reactor. Galvagno et al. (2002) utilised a pilot scale SRT 3 873 2.5 3.5 11.4
experimental pyrolysis plant to treat scrap tyres which consists SRT 4 873 1.9 3.5 11.4
on a rotary kiln reactor externally heated working with a maxi- SRT 5 873 1.5 3.5 11.4
MFR 1 873 3.7 3.5 11.4
mum feeding rate of around 50 kg/h of tyre.
MFR 2 873 3.7 6 11.4
The present study used a pyrolysis system for rubber tyre load- MFR 3 873 3.7 8 11.4
ing up to 15 kg/h in a moving bed reactor. The main objective of INERT 1 873 3.7 3.5 11.4
the research work in progress is to evaluate both, process perfor- INERT 2 873 3.7 3.5 68.4
mance and chemical characteristics of the products obtained, while INERT 3 873 3.7 3.5 144.0

varying the main operational parameters. Scrap tyre samples used

for the treatment, solid and liquid by-products and the produced
gas were analysed and the results are discussed in the present same gas chromatograph was used since it is equipped with a
paper. split/splitless injector, FID detector and a wide bore capillary Supe-
lco KCl/Al2O3 column.
The ultimate tyre oil composition was determined using a Carlo
2. Experimental Erba analyser model EA1108. In addition, thin layer chromatogra-
phy with FID detector (IATROSCANTM MK-5) was performed to
The raw material used for the pyrolysis experiments was a sam- determine the saturated, aromatic and polar compounds in the
ple of tyre rubber shreds (without steel core) supplied by Negrell sample. Finally, the tyre oil was also analysed by GC-FID in a Varian
Residus SL, a Spanish waste tyre recycling company. These tyre Star 3400 model in order to nd the boiling point range according
shreds were a mixture of tyres from trucks, tractors and cars. The to the simulated distillation method described in ASTM D2887-04.
average particle size was 5 mm approximately and had the follow-
ing ultimate and proximate analyses: C (ar) 81.72%; H (ar) 6.54%; S
3. Results and discussion
(ar) 1.87%; N (ar) 0.55%; moisture (ar) 0.71%; ash content 6.64% and
volatile matter (ar) 62.58% where ar means as received. The ulti-
The inuence of the main process variables (reaction tempera-
mate analysis was determined with a Carlo Erba EA1108 instru-
ture, mass ow rate, solid residence time and inert gas ow) on
ment. The moisture was determined by ISO-589-1981, the ash
the product yields and their properties have been studied and
content by ISO-1171-1976 and the volatile matter by ISO-5623-
the results are reported below. For all the runs performed, it has
1974.
been found that the tyre devolatilisation is complete and the ob-
The experimental system has been described in detail else-
tained pyrolytic carbon black has a volatile matter content under
where (Ayln et al., 2008) and consists of four main parts: the feed-
5%. Therefore, it has been demonstrated that the performance of
ing system, the reactor, the solid collecting system and the
the experimental system is suitable for waste tyre processing, at
condensing system. The feeding system presents a total capacity
least in the range of variables studied.
of 10 kg approximately and allows carrying out the process contin-
uously under inert atmosphere by using nitrogen as carrier gas. The
reactor is a continuously operated moving bed reactor and de- 3.1. Temperature inuence on the reaction product yields and
signed to process up to 15 kg/h of waste tyre. The tyre shreds move properties
through the reactor and, at the same time, they decompose into a
gaseous product and a solid residue. The solid residue leaves the It is well-known that pyrolysis is a chemical process where ef-
reactor by gravity falling into a solid collecting system and the gas ciency depends mainly on the temperature and the heating rate. In
reaches the condensing system by natural convection helped by many studies, this variable do not only inuence the degree of con-
the carrier gas. Eventually, the non-condensed pyrolysis gas is version achieved, but also the product distribution, mainly through
pipelined to a burner before it reaches the atmosphere. Several cracking reactions.
experiments were carried out under the same conditions to deter- The inuence of the process temperature was evaluated at three
mine the plant reproducibility. It was observed an excellent pro- different values, 873, 973 and 1073 K. Table 2 shows the volatile
cess reproducibility and stability. In the present work, four series
of experiments have been carried out in order to study the main Table 2
operation variables: reaction temperature, solid residence time, Product yields, proximate analysis of the solid and gas residence time at different
mass ow rate and inert gas ow. The pyrolysis conditions for reaction temperatures (3.5 kg/h, solid residence time = 3.7 min, N2 = 11.4 l N/h).
these experiments are collected in Table 1. Reaction temperature (K) 873 973 1073
Yields to solid and liquid products were directly obtained by
Product yields
weight. The gas fraction percentage was calculated through a mass Solid (wt.%) 40.6 39.0 41.0
balance. The pyrolysis products obtained in all the experiments Liquid (wt.%) 41.5 31.3 27.5
have been characterized as follows: permanent gases were ana- Gas (wt.%) 17.9 29.7 31.5
lysed in a Varian 3800 CP gas chromatograph equipped with a Char proximate analysis
thermal conductivity detector (TCD) and HAYESEP Q and Mole Moisture (wt.%) 1.26 0.86 0.45
Sieve HP-Al/KCl columns. Hydrogen was analysed in a Hewlett Volatile (wt.%) 4.41 2.15 1.33
Volatile conversion (%) 97.3 98.8 99.2
Packard 5890 series II model, equipped with a TCD detector, a Mole
Gas residence time (s) 16.7 14.9 13.5
Sieve column and argon as carrier gas. For C1C4 compounds the
1222 E. Ayln et al. / Waste Management 30 (2010) 12201224

matter conversion and the product yields at the different process Table 3
conditions. It is also observed that almost total conversion has Ultimate analysis, thin layer chromatography and simulated distillation of the
pyrolysis oil obtained at different reaction temperature (3.5 kg/h, N2 = 11.4 l N/h,
been reached for all the temperatures tested, leaving the volatile solid residence time = 3.7 min).
matter <5% in the char. Although the solid yield obtained after
the reaction remains constant, the gas fraction increases and there- Reaction temperature (K) 873 973 1073

fore the liquid fraction decreases when the temperature reaction is Ultimate analysis
increased. This could be mainly due to the more severe cracking of Carbon (wt.%) 88.58 91.00 90.56
Hydrogen (wt.%) 10.40 8.17 7.66
the primary pyrolysis products occurring at higher temperatures. Nitrogen (wt.%) 1.43 1.39 1.28
The mechanism of leading to the changes between gas fraction Sulfur (wt.%) 1.05 1.12 0.93
and liquid fraction has been thoroughly reported elsewhere (Mas- Thin layer chromatography
tral et al., 2000). Saturate (wt.%) 4.8 2.2 0.0
There are several works published about the inuence of tem- Aromatic (wt.%) 67.8 68.5 72.8
perature on tyre pyrolysis. In these works, it can be observed that Polar (wt.%) 27.5 29.4 27.2
there is a signicant dispersion on the yields reported in terms of Boiling point distribution
working temperature (Chang, 1996; Laresgoiti et al., 2004; Leung <473 K 46.5 55.5 59.3
473623 K 36.5 33.7 33.4
et al., 2002; Williams et al., 1990). The most signicant variations
>623 K 17 10.8 7.3
are reported on the gas and liquid yields, in such a way that in
these works the gas yield varies in a range from 4% to 53% for a
reaction temperature of 873 K. These variations indicate that the
product yields are not only inuenced by the reaction temperature, hand, the cracking effect, explained according to the gas analysis,
but also by the specic characteristics of the system, mainly heat- (see Fig. 1) is also observed in the liquid simulated distillation re-
ing rate and reactor type. Hence, different reactor designs can lead sults (see Table 3). A more severe cracking of the liquid pyrolysis
to different gas residence times, varying the cracking of the pri- products is obtained at increasing temperature and the yield of
mary pyrolysis products. the lowest boiling point fraction increases notably (from 46% to
It has been also observed a great inuence of this variable on 59%) in the temperature range studied.
the characteristics of the conversion products, except in the case
of the solid product where no inuence was found in terms of both 3.2. Solid residence time inuence on the reaction product yields and
solid yield and volatile matter content. Fig. 1 shows gas composi- properties
tion for the reaction temperatures studied. The composition has
been expressed in terms of yield to the different gas compounds Other important variable in the pyrolysis process is the solid
since the gas yield varies noticeably for each temperature. As it residence time. The optimization of the solid residence time inside
was expected, higher reaction temperature produces a higher the reactor is a key factor in order to scale up an industrial system.
cracking in the gas phase, increasing both the total gas yield and Lower residence times involve lower reactor volumes to process a
the fraction of light gases in the mixture, such as hydrogen and certain load of tyre and, therefore, lower cost of the systems. In or-
methane. With respect to the temperature inuence on COx pro- der to carry out this study, ve experiments were performed at dif-
duction, there is a slight increase in COx with reaction temperature ferent solid residence times by varying the speed of the screw in
probably due to the decomposition of inorganic compounds like the moving bed reactor. The solid residence time inside a screw
calcium carbonate present in the tyre composition. These com- reactor can be calculated according to Eq. (1), where tr is the solid
pounds decompose at higher temperatures than organic residence time, L is the reactor length, rpm is the rotational speed
compounds. and P is the screw pitch
In addition, Table 3 shows the results of ultimate analysis, thin L
layer chromatography and simulated distillation of the pyrolysis tr 1
rpm  P
oil. It is observed a decrease in the hydrogen percentage and an in-
crease of aromatic compounds when the temperature is increased. The range of solid residence time studied varies from 1.5 to
This could be attributed to the promotion of aromatisation reac- 5 min. Due to experimental limitations, it was not possible to per-
tions at higher reaction temperatures as it has been previously re- form experiments above or below these residence time values. In
ported by this research group (Bartle et al., 2000). On the other this range, neither in the product yields nor in the reaction conver-
sion were variations observed, obtaining similar values in all the
runs performed. However, according to previous simulations, the
variation of the solid residence time involves the variation of the
16.0
gas residence time (from 15 to 21 s in the range studied). This var-
14.0 600 C iation is due to the increment of the free volume inside the reactor.
700 C
800 C According to Eq. (2), the higher the screw speed, the lower the solid
12.0 residence time and the higher the free volume. Eq. (2) calculates
(g /g tyre)*100

10.0 the solid mass ow rate in terms of screw geometry, rotational

screw speed and bed density
8.0
C p  DT 2  DE2 =4  P  rpm  q  1  U  a  60 2
6.0
where C is the mass ow rate (kg/h), DT is the screw diameter (m),
4.0 DE is the core diameter (m), q is the particle density (kg/m3), U is
2.0 the free volume percentage inside the screw, a is the section reduc-
tion due to screw inclination (horizontal screw, a = 1).
0.0 The increase of the gas residence time would favour the crack-
H2 COx H2S CH4 C2 C3 C4
ing of the primary pyrolysis products and would promote a change
Fig. 1. Composition of the gas fraction obtained at different reaction temperatures in the gas/liquid ratio. However, experimentally, these variations
(3.5 kg/h, N2 = 11.4 l N/h, solid residence time = 3.7 min). seem not to be important enough to change the yields to the three
 E. Ayln et al. / Waste Management 30 (2010) 12201224 1223

fractions obtained and similar values were obtained in the ve 6.0

experiments. The average solid product yielded 38.9%, the liquid 3.5 kg/h
yielded 42.6% and nally the gas yielded 18.5% being the variations 5.0 6 kg/h
8 kg/h
between the different values (2.7 wt.% for char, 2.1 wt.% for oil and
4.4 wt.% for gas) always under the experimental error evaluated in 4.0

(g /g tyre)*100
a previous work (Ayln et al., 2008). In addition, the volatile matter
content was always under 5 wt.% even at the shortest residence 3.0
time. These results indicate that the reaction has been completed
in all the experiments including the one performed at such a low 2.0
residence time as 1.5 min.
Regarding to the product characterisation, no relevant differ- 1.0
ences were observed and similar values to those reported in Table 3
for the experiment performed at 873 K were obtained.
0.0
H2 COx H2S CH4 C2 C3 C4

3.3. Mass ow rate inuence on the reaction product yields and Fig. 2. Composition of the gas fraction obtained at different mass ow rate
properties (T = 873 K, N2 = 11.4 l N/h, solid residence time = 3.7 min).

Results of a set of three experiments (3.5, 6 and 8 kg/h) have

Table 5
been analysed in order to study the inuence of this variable.
Ultimate analysis, thin layer chromatography and simulated distillation of the
The product yields obtained are shown in Table 4, where it is ob- pyrolysis oil obtained at different mass ow rate (T = 873 K, solid residence
served that this variable affects considerably to the gas/liquid ratio time = 3.7 min, N2 = 11.4 l N/h).
obtained, while the solid yield remains constant. According to Eq.
Mass ow rate (kg/h) 3.5 6.0 8.0
(2), the higher the tyre ow rate, the lower the free volume inside
Ultimate analysis
the reactor and, on the other hand, as a consequence of a higher
Carbon (wt.%) 88.58 85.81 83.52
tyre ow rate, there is an important increment in the volatile mat- Hydrogen (wt.%) 10.40 10.78 10.66
ter released. Both effects make that the gas residence time inside Nitrogen (wt.%) 1.43 4.61 0.90
the reactor decreases considerably (from 17 to 3 s). This remark- Sulfur (wt.%) 1.05 0.98 0.91
able decrease of the gas residence time when the tyre ow rate Thin layer chromatography
is increased, limits the cracking of the gas fraction. Therefore, a big- Saturate (wt.%) 4.8 5.5 5.8
ger amount of liquid is obtained in the process. It must also be Aromatic (wt.%) 67.8 65.2 64.7
Polar (wt.%) 27.5 29.3 29.5
pointed out that the proximate analysis of the solid product indi-
cates a volatile content lower than 5 wt.% in all the experiments. Boiling point distribution
<473 K 46.5 38.9 25.9
Thus, it can be concluded that the material devolatilisation has 473623 K 36.5 32.7 33.3
been achieved even for the highest tyre ow rate studied. >623 K 17 28.4 40.8
The effect of a lower cracking when the tyre ow rate is in-
creased can be also observed in the product characteristics. Fig. 2
shows the composition of the gas fraction expressed in terms of 3.4. Inert gas ow rate inuence on the reaction product yields and
gas compound yields. When the mass ow rate is increased, the properties
gas fraction obtained presents a higher percentage of the heaviest
compounds. It is worth to highlight that the increase of the yield in The last variable that has been assessed is the inert gas (nitro-
light compounds is doubled in the case of the lowest tyre ow rate gen) ow rate. Three experiments have been carried out to check
(3.5 kg/h). the inuence of this variable on product yields and properties:
Regarding to the liquid fraction characteristics the variations 5 vol.% N2, 20 vol.% N2 and 35 vol.% N2 in the gas fraction inside
are not so noticeable. It has not been found any difference in the the reactor (these percentages correspond to an inert gas ow of
ultimate analysis data and only a very slight decrease of the aro- 11.4, 68.4 and 144 l N/h, respectively). It could be expected that
matic hydrocarbons percentage has been observed when the tyre the residence time of the gas phase produced by pyrolysis would
ow rate is increased. However, some differences have been found decrease at increasing inert gas ows. High nitrogen ow rates re-
in the simulated distillation curves. In Table 5 it can be observed moved the products quickly from the reaction zone and hence min-
that when the tyre ow rate is increased, the gasoline percentage imised secondary reactions such as cracking. However, according
in the liquid yield decreases, varying between 25% and 47% in to the experiments performed, no inuence of the nitrogen ow
the studied range. rate has been detected. Both, the product yields and product prop-
erties are similar to those reported in Table 2 for the experiment
performed at 873 K. Probably, no change has been found because
Table 4 the variation of the gas residence time as a consequence of the in-
Product yields, proximate analysis of the solid and gas residence time at different
mass ow rate (T = 873 K, solid residence time = 3.7 min, N2 = 11.4 l N/h).
ert gas increment is almost negligible (the gas residence time only
changes from 17 to 15 s although the inert ow rate has been nota-
Mass ow rate (kg/h) 3.5 6.0 8.0
bly increased). Nevertheless, it has been considered that higher
Product yields percentages of nitrogen in the nal gas would suppose an excessive
Solid (wt.%) 40.6 39.9 39.9 dilution of the gas fraction and therefore these gases may not have
Liquid (wt.%) 41.5 46.4 48.4
Gas (wt.%) 17.9 13.6 11.7
enough caloric value to satisfy the process energy requirement.

Char proximate analysis

Moisture (wt.%) 1.26 1.58 1.54 4. Conclusions
Volatile (wt.%) 4.41 3.87 4.41
Volatile conversion (%) 97.3 97.8 97.4
According to the results shown in this paper, the total conver-
Gas residence time (s) 16.71 6.74 3.23
sion of waste tyre has been achieved under all tested experimental
1224 E. Ayln et al. / Waste Management 30 (2010) 12201224
conditions. It has been found that the volatile matter yield in the
produced char is lower than 5 wt.% in all the runs. Therefore, it
would be possible to select the most appropriate operational
parameters in terms of desired product distribution. The maximum
oil yield is obtained working at low temperatures (around 873 K)
and high mass ow rates (8 kg/h). Moreover, it has been proven
that the solid residence time needed to achieve the total conver-
sion is <1.5 min. This residence time is clearly lower than other re-
ported in literature for different reactor geometries. That would be
a remarkable asset of this experimental system compared to other
bench-scale reactors and the scaling up of the technology could be
performed taking into account the obtained experimental results.
Acknowledgements
Authors would like to thank to Negrell Residus SL the tyre sam-
ple supply and to the Spanish Science and Education Ministry the
FPU Pre-Doc grant (E. Ayln).
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