A PRELIMINARY STUDY OF FIXED BED PYROLYSIS OF ESPARTO (STIPA TENACISSIMA)

Javier Ábrego (1); Ahmed el-Amarti (2); Abderrahmane Debdoubi (2); Jesús Arauzo (1); Alberto Gonzalo (1)
(1)
Thermochemical Processes Group (GPT), Aragón Institute of Engineering Research (I3A), University of Zaragoza, María
de Luna 3, 50018 Zaragoza, Spain. E-mail: [javabr; jarauzo; agonca]@unizar.es
(2)
Unité Calorimétrie et Matériaux, Université Abdelmalek Essaadi, Facultés des Sciences, P.O. Box 2121, Tétouan 93002,
Morocco. E-mail: [ahmed-elamarti; debdoubi]@hotmail.com

ABSTRACT: Esparto grass (Stipa Tenacissima) has been pyrolysed in a fixed bed reactor. An experimental design
methodology has been applied in order to determine the influence of two parameters: final pyrolysis temperature and
heating rate. These values ranged, respectively, from 350 to 650 ºC and from 5 to 15 ºC min-1. Solid, liquid and
gaseous fractions have been determined for each experiment. Gas composition has been determined by means of
chromatographic analysis. Product distribution showed a major liquid fraction as main pyrolysis product. This liquid
fraction depends on temperature and heating rate and shows a maximum yield of 49.8% at 595 ºC and 5 ºC min-1. The
solid fraction decreases dramatically until 500 ºC and shows little variation at higher temperatures, with almost
negligible influence of heating rate. Gas fraction seems to depend only on heating rate, with higher yields at 15 ºC
min-1. BET surface area of chars obtained at the maximum temperature of 650 ºC show significant porous
development.
Keywords: Fixed bed, pyrolysis, grass.

1 INTRODUCTION
3 EXPERIMENTAL SECTION
Esparto grass is a very abundant herbaceous plant in
arid regions of Morocco and Spain. In Morocco, esparto 3.1 Materials
is the most available biomass, with an estimated Esparto grass came from oriental Morocco and was
production of 560.000 tons of dry matter annually [1]. In characterized by means of proximate/ultimate analyses
the past, several local industries such as paper mill, sugar and lower heating value determination, as showed in
or cement industries used this material and thus provided Table 1. Moisture content was determined heating a
an important economical sustain, together with a source sample at 105 ºC accordingly to ASTM D2016-25. Ash
of fuel for domestic heating and cooking. Nowadays, content was determined with the standard procedure
local industries for its exploitation no longer exist, and ASTM D-542, burning 2g of sample at 800 ºC during 5h.
this potential valuable resource is thus underutilized. The volatile matter was analysed according to ISO
Nevertheless, esparto is easily available in large areas 562/1974. Fixed carbon was determined by difference.
of these two countries, and its surface coverage is as large Lower heating value was obtained using a Parr bomb
as 3.6 Mha in Morocco, specially in the oriental region of calorimeter with 1g of sample.
the country [2]. In Northern Africa, the overall surface
coverage is estimated as 7 MHa [3]. Thus, one should Table 1: Analysis of esparto grass sample.
think of esparto grass as an immense biomass natural
Proximate % by weight
reservoir in these areas, capable of being processed as a
renewable energy source. As a result, some kind of
thermochemical valorisation should be considered apart Moisture 5.20
Ash 2.20
from its domestic use for cooking and heating. Volatiles 80.5
Scarce references have been found regarding a Fixed Carbon 16.8
thermochemical use of esparto. Debdoubi et al. [1]
assessed the possibility of briquetting partially pyrolysed
Ultimate (organic fraction) % by weight (daf)
esparto at temperatures between 160 and 400 ºC, and
obtained good mechanical properties and combustion Carbon 46.94
behaviour of these briquettes. Díaz-Terán et al. [4,5] Hydrogen 6.44
prepared activated carbons from esparto using different Nitrogen 0.86
pyrolysis temperatures and KOH and K2CO3 as activation Oxygen 43.56
agents. No studies regarding product distribution on
pyrolysis or gasification have been found. Gasification Lower Heating Value (MJ/kg) 19.1
and pyrolysis processes for esparto could lead to valuable
gaseous or liquid fuels, respectively. 3.2 Fixed bed pyrolysis plant
For pyrolysis experiments, the experimental system
depicted in Figure 1 was used. The fixed bed reactor is
2 AIM OF THIS STUDY cylindrical and made of stainless steel, and lies inside an
electrical furnace. The furnace is connected to a PID
The main purpose of this work is to make a temperature controller and is capable of reaching
preliminary study of esparto fixed bed pyrolysis in maximum temperatures of 950 ºC with heating rates
nitrogen atmosphere, in order to study its product between 1 and 50 ºC min-1. Esparto grass samples were
distribution depending on two selected factors: final placed in a steel basket th at hangs from the upper part of
pyrolysis temperature and heating rate, and consequently, the reactor and heated at the selected heating rates and
assess its feasibility for energy generation via final temperatures. A flow of nitrogen (100 Nml/min)
thermochemical processes. Also, valuable solid products created an inert atmosphere for pyrolysis. This gas was
such as charcoal or activated carbon could be obtained. introduced at the upper part of the reactor.
Figure 1: Laboratory scale fixed bed pyrolysis plant.

In each experiment, 2.5 g of raw material were used. 650 ºC. Regarding the influence of heating rate, the effect
The composition of the generated gas fraction was of this parameter on char yield is minimal, as seen in
determined by means of an Agilent 3000A portable Figure 2.
chromatograph connected to the products outlet. Before
this equipment, the liquid fraction was determined
gravimetrically in a refrigerated condenser, followed by a 40
cotton filter placed afterwards that retained the rest of 5 ºC/min
condensable compounds. The remaining solid fraction 15 ºC/min
Char Yield (wt. %)

was cooled after the experiment under nitrogen 35

atmosphere in the upper part of the reactor (cooled by a
water jacket) and weighted.
30
3.3 Experimental Procedure
Pyrolysis of esparto grass was carried out in the
temperature range between 350 and 650ºC, and with 25
heating rates varying between 5 and 15 ºC/min. No hold
time was maintained after reaching the final temperature.
20
Experimental design methodology was used as a tool 350 400 450 500 550 600 650
for investigating the influence of these selected parameters
in the solid, liquid and gaseous product yields. Results Temperature (ºC)
were analyzed by applying analysis of variance Figure 2: Char yield (wt. %) as a function of temperature
(ANOVA) methodology, in order to study the influence and heating rate.
of the variables and their possible interactions on
observed responses. 4.2 Liquid yield
After pyrolysis, BET surface area of one selected
char was determined by means of a Micromeritics ASAP 55
2020 analyzer.
50
Liquid Yield (wt. %)

45
4 RESULTS
40
4.1 Char yield
35
The evolution of char yield with temperature and
heating rate is shown in Figure 2. As can be seen, at 350 30 5 ºC/min
ºC around 65% of the initial weight has gone to liquid
25 15 ºC/min
and gaseous products. Debdoubi et al. [1] found a similar
weight loss (61%) when esparto was partially pyrolysed 20
at 350 ºC for briquetting. As temperature increases up to 350 400 450 500 550 600 650
500 ºC, an additional weight loss of about 10% of the Temperature (ºC)
initial esparto is observed. From this intermediate
Figure 3: Liquid yield (wt. %) as a function of
temperature, only a slight weight loss is detected up to
temperature and heating rate.
 Unlike solid fraction, liquid yield (also referred to as
bio-oil) is significantly affected by changes in heating
rate. Figure 3 shows the evolution of liquid yield with
temperature for heating rates of 5 and 15 ºC min-1. Higher
yields of bio-oil are obtained when applying the highest
heating rate of the considered interval.
The influence of temperature is greater in the first
half of the considered interval (up to 500 ºC a significant
increment is observed). Above 550 ºC, bio-oil generation
seems to stop for both heating rates, as seen in Figure 3.
In these temperature conditions and for lower heating
rates, liquid yield can reach up to 50% of the initial
weight of esparto grass.
The high yields of liquid fraction at 350 ºC could be
partly related to the release of water from biomass at low
temperatures. Horne and Williams [6] reported high
water contents (near to 30% by weight) in bio-oils from
flash pyrolysis of wood, at temperatures ranging from
400 to 600 ºC. Similar values were also reported by
Boateng et al. for pyrolysis of switchgrass [7]. Apart
from the moisture content, a significant percentage of this
water probably comes from the cellulosic fraction of the
initial esparto grass. It is known that cellulose
decomposes yielding a maximum rate of water formation
about 300 ºC [8].
Apart from water content, further analyses of bio-oil
composition would be required to evaluate its suitability
as an alternative fuel.
4.3 Gas yield
In the chosen intervals of temperature and heating
rate, gas yield has shown to depend only on the latter. As
shows Figure 4, an increase in heating rate from 5 to 15
ºC min-1 produces increments of gas yield up to 10% by
weight. Surprisingly, temperature does not seem to have
a measurable effect in gas fraction. This can be caused by
the fact that in this work, gas yields have been calculated
by difference from solid and liquid fractions. Anyway,
this could also indicate that a majority of the gas fraction
is generated below 350 ºC, and further increases of
temperature (in the considered interval) have little effect
on this yield.
4,5
4
3,5
3 CO2
%Volume
2,5
2 C2H6
1,5
1
0,5
0
50 150 250 350
Temperature, ºC
Figure 5: Evolution of gas composition with temperature.
T= 650 ºC, heating rate 10 ºC min-1.
Besides (and similarly to liquid yields), gas fraction
at the lowest temperature considered is relatively high,
suggesting maximum rates of gases generation below 350
ºC.
40
Gas yield (wt. %)
35
30
25
5 10 15
-1
Heating Rate (ºC min )
Figure 4: Gas yield (wt. %) as a function of heating rate.
4.4 Gas composition
Figure 5 shows the evolution of gas composition (in
volume %, and excluding nitrogen used as inertizing
agent for pyrolysis) in a selected experiment. This
particular experiment (650 ºC and 10 ºC min-1) was
chosen because it covers the entire temperature range
studied and was made at an intermediate heating rate. As
a result, it can illustrate the gas release of any of the
experiments done in this work.
The region below 250 ºC shows the generation of
important quantities of carbon oxides (CO and CO2),
probably due to decomposition of the carboxyl groups
from cellulosic and hemicellulosic fractions [7] contained
in esparto grass. Thus, carbon oxides and water are
released almost simultaneously as a result of the
decomposition of these fractions. As can be seen in
Figure 5, the evolved gases at temperatures lower than
350 ºC (including CO2) represent a much higher volume
than the gases evolved beyond this temperature. Besides,
CO2 is the heaviest gas and accounts for most of the
weight percentage of the gases.
H2
CH4
CO
C2H4
450 550 650
 Thus, the observations made regarding gas yields in cellulose, European Polymer Journal, 2001, 37(5), p.
the previous section are confirmed. This large evolution 933.
of CO2 has also been observed in previous works [4].
Finally, beyond 550 ºC, a second stage of gas release
is observed. Hydrogen, methane, CO2 and CO begin to 7 ACKNOWLEDGEMENTS
increase from this temperature. These could be related to
decomposition of lignin that occurs at higher The Authors wish to thank AECI (Agencia Española
temperatures than cellulose and hemicellulose, and over a de Cooperación Internacional –Spanish Agency for
broader interval [4,7]. International Cooperation) for providing financial support
to this investigation. This work was done within the
As a guide to evaluate its possible use for adsorbent project AECI A/012707/07, entitled Valorisation de
production, BET surface area was measured for a char biomasse végétale, de sous-produits et des résidus
obtained at 650 ºC and 10 ºC min-1. The carbonaceous industriels dans la production de l´énergie.
solid gave a surface area of 413 m2/g, in accordance to
values reported elsewhere [4]. This implies a significant
development of porous structure of chars with pyrolysis, 8 LOGO SPACE
and suggests that further treatments such as chemical or
physical activation could lead to an activated carbon
suitable for the removal of pollutants from water or
gases.

5 CONCLUSIONS

Product distribution (solid, liquid and gaseous

fractions), gas composition and surface area of high
temperature pyrolysis chars have been determined from
fixed bed pyrolysis experiments at low heating rates and
temperatures below 650 ºC. The three fractions obtained
are suitable for its use as fuels and, in the case of chars,
for activated carbon production. This preliminary study
Thermochemical Processes Group (Aragón Institute for
shows encouraging results regarding the use of esparto as
Engineering Research)
a renewable energy source in Southern Spain and the
North of Africa.

6 REFERENCES

[1] A. Debdoubi, A. El Amarti and E. Colacio,

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[2] H. Kerrouani, Annals of the forest research in
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[3] H. Nadjia, P.N. Dioufa, A. Benabourab, Y. Bedarda, University of Zaragoza – Spain
B. Riedla and T. Stevanovic, Comparative study of
lignins isolated from Alfa grass (Stipa tenacissima
L.), Bioresource Technology, 2009, 100(14), p. 3585.
[4] J. Díaz-Terán, D.M. Nevskaia, A.J. López-Peinado
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Mesoporous Materials 2003, 60, p. 173.
[6] P.A. Horne, P.T. Williams, Influence of temperature
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[7] A.A. Boateng, K.B. Hicks and K.P. Vogel, Pyrolysis
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