Fuel 350 (2023) 128824

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Full Length Article

Oxidative pyrolysis of pellets from lignocellulosic anaerobic digestion

residues and wood chips for biochar and syngas production
F. El abdellaoui a, b, *, R.P. Roethlisberger a, H. Ez-Zahraouy b
a
Institute of Thermal Engineering, School of Engineering and Management Vaud, HES-SO University of Applied Sciences and Arts Western Switzerland, Switzerland
b
Laboratory of Condensed Matter and Interdisciplinary Sciences, URL-CNRST, Faculty of Sciences, Mohammed V University in Rabat, Morocco

A R T I C L E I N F O A B S T R A C T

Keywords: Compared to pyrolysis in an inert atmosphere, oxidative pyrolysis for biomass conversion is autothermal and
Wood chips decreases the concentration of tars in the produced gases. The aim of this work is to study a fixed bed reactor for
Lignocellulosic anaerobic digestion residues oxidative pyrolysis on a laboratory scale with a capacity of 1.5 kg/h of lignocellulosic anaerobic digestion res­
Oxidative pyrolysis
idues (Pellets-DR) at a temperature range of 600 ◦ C and under a low specific airflow of 0.012 kg/m2.s. Wood
Tars
chips (WC-P16F05) were used as a reference to evaluate the potential of Pellets-DR conversion to biochar and
Biochar
Syngas syngas using oxidative pyrolysis. Oxidative pyrolysis produced only 10% and 6% of tars on a fuel dry and ash-
free basis for Pellets-DR and wood chips, respectively, which is equivalent to a concentration of 25 g/Nm3 and
38.6 g/Nm3 in gases. Ultimate and proximate analysis of biochar produced from both types of biomasses showed
that the main element present was carbon in the case of wood chips (87.8%). However, carbon is present in only
48.33% of the biochar from Pellets-DR. The main difference between Pellets-DR and wood chips was also found
in biochar’s low heating value (LHV), which is estimated to be 31.9 MJ/kg for wood chips and 13.01 MJ/kg for
Pellets-DR. The propagation of the oxidation zone was inversely proportional to biomass density, and it plays a
key role during biomass oxidative pyrolysis; it was about 0.14 cm/min and 0.5 cm/min for Pellets-DR and wood
chips, respectively. Air flux was the most important factor affecting the oxidation zone propagation velocity, but
in this study, low values of air flux meant that changes in air flux did not have a significant effect on the yield and
the composition of the products. Regardless of its high ash content, Pellets-DR may have the potential to be
converted into biochar and syngas by oxidative pyrolysis.

1. Introduction after gasification and upgrading, the gas from pyrolysis can be used as an
engine or turbine fuel to produce electricity or be upgraded to liquid
Biomass, which originates from forests, agriculture, and various in­ fuels and chemicals through biological fermentation or catalytic
dustrial processes that use forestry, agricultural materials, and food upgrading via the Fischer-Tropsch process [8,9].
waste, is a potential energy feedstock and source of bioproducts [1–3]. Biomass nature (source, particle size, ash content, and moisture) and
Biomass pyrolysis occurs in the absence of oxygen to produce per­ thermochemical conversion parameters (temperature, heating rate, and
manent gases, condensates (water and tars), and solid biochar. As a solid residence time) affect the quality and quantity of gases and biochar from
byproduct from biomass pyrolysis, biochar can be a viable alternative to pyrolysis. Recent works on biomass pyrolysis focus on optimizing pro­
the complete combustion of agricultural and forest residues, which re­ cess parameters and the use of low-quality feedstocks to enhance the
leases carbon into the atmosphere. Recently, many researchers have technical and economic challenges linked to biomass pyrolysis. The ef­
become interested in studying carbon sequestration, the potential of fect of biomass types, pyrolysis temperature, and residence time on
biochar, and its function of keeping carbon in soil in a stable state [4]. biochar was investigated by [10–12]. However, the effect of feedstock,
Besides its potential for carbon sequestration, biochar can be upgraded pyrolysis temperature, and residence time on tars was investigated by
into activated biochar, which is commonly used as a catalyst or as an [11,13].
adsorbent for gas and wastewater treatment [5–7]. On the other hand, Pyrolysis in an inert atmosphere needs an external heat supply to

* Corresponding author at: School of Engineering and Management Vaud, HES-SO University of Applied Sciences and Arts Western Switzerland, Switzerland and
Faculty of Sciences, Mohammed V University in Rabat, Morocco.
E-mail address: [email protected] (F. El abdellaoui).

https://doi.org/10.1016/j.fuel.2023.128824
Received 27 March 2023; Received in revised form 8 May 2023; Accepted 28 May 2023
Available online 6 June 2023
0016-2361/© 2023 Elsevier Ltd. All rights reserved.
F. El abdellaoui et al. Fuel 350 (2023) 128824

occur, and the process is limited by thermal transfers from the reactor porosity and density [14,16,18]. Previous studies mentioned that not all
wall to the biomass. The external heat source for biomass decomposition these parameters are independent variables and most are interrelated;
reactions is one of the biggest problems with scaling up and using thus, drawing conclusions about the dependency of each separate
biomass pyrolysis technologies. Moreover, as the first step of gasifica­ parameter on the behavior of the oxidation zone is difficult [19]. Also,
tion, pyrolysis produces biochar, water, permanent gases (CO, CO2, studies that looked at how air mass flow affects other aspects of the
CH4, H2, and N2), and tars, which is one of the biggest challenges for oxidation zone, like temperature, yields, and compositions of products,
gasification scaling up and commercialization. Besides the optimization found that this parameter had a big effect on both the temperature and
of the parameters affecting the pyrolysis process, to improve the quality the quality of the products from biomass oxidative pyrolysis [13,14,16].
of the produced gas in terms of the yield of tars, pyrolysis can be As mentioned before, the use of marginal and residual biomass
controlled by air injection in small quantities. Compared to pyrolysis in sources improves the sustainability of the system by avoiding the use of
an inert atmosphere, oxidative pyrolysis allows the process to be auto- high-quality resources such as wood. But the effect of the biomass or bed
thermal and decreases the yield of tars in the produced gases [14–16]. properties has been rarely investigated, and the previous few studies
The presence of oxygen was also found to enhance the surface of the showed that the front propagation velocity was higher when particle
pores compared to pyrolysis in an inert atmosphere [12]. Thus, oxida­ size, water content, or ash content was low or when the heating rate
tive pyrolysis may be a promising technology to enhance pyrolysis ef­ value was high. Moreover, ignition front propagation velocity was
ficiency in terms of energy and quality of the products. inversely proportional to bed bulk density [9,16,18,20]. Few studies
On the other hand, biomass is a low-energy-density fuel, unlike other were interested in the effects of biomass on product yields and compo­
energy sources, it is a dispersed source. In addition to the optimization of sitions. Woody biomass, such as wood chips and pellets, and residues
plant design, the exploitation of marginal and low-quality biomass such from agriculture were investigated in a fixed bed, and the effects of ash
as residue from agriculture and industry (lignocellulosic anaerobic content and density on propagation velocity and the product yields and
digestion residue, paper industry, and so on) may be an attractive so­ compositions were studied. The results confirmed that propagation ve­
lution to improve the economic reliability and sustainability of the locity is inversely proportional to density. Moreover, the ash content
system while avoiding the exploitation of high-quality resources such as affects both the propagation velocity and the product yields and com­
wood. However, the utilization of new biomass presents a big technical positions [14,16]. However, the residues from lignocellulosic anaerobic
challenge. Due to the high ash content, the low density, the size distri­ digestion, characterized by their high ash content compared to residues
bution, which is known to be very heterogeneous, and, in some cases, from agriculture and by their heterogeneity, were not investigated
the high moisture compared to woody biomass, these parameters play previously using oxidative pyrolysis.
an important role during biomass oxidative pyrolysis [14,16]. But few The present paper focuses on the oxidative pyrolysis of lignocellu­
studies were interested in the effect of these parameters on biomass losic anaerobic digestion residues characterized by a high ash concen­
oxidative pyrolysis, which means front propagation velocity, reaction tration in a batch fixed bed reactor and in a downward reverse
kinetics, temperatures, product yields, and compositions. Moreover, smoldering configuration with a very low air flux. The study’s aim was
mineral elements, which represent 0.1% of ash in the case of woody to investigate the potential of using the residues from a biological pro­
biomass and more than 10% in the case of biomass from residues, are cess to produce syngas and biochar via thermochemical conversion. The
found in oxidized form in the ash after complete combustion of organic study focuses on observing and measuring the following distinct char­
biomass. K, Na, Ca, Mg, P, and Si are the most common inorganic acteristics: temperatures; average oxidation zone velocity; yields and
components. They appear as ions or are related to the organic structure. compositions of biochar; permanent gas and tars; and the effect of air
During biomass thermochemical conversion, ash is a key parameter to flux on biomass oxidative pyrolysis. The results were compared to the
evaluate the potential for slagging and fouling. Ash can partially melt at oxidative pyrolysis of wood chips. This study could provide new insights
high temperatures, leading to fouling within the reactor or hard chunks into the combination of biological processes and a thermochemical
of material in the combustion chamber (slagging or clinkering) [17]. process, which is oxidative pyrolysis at very low air flow.
Nevertheless, even at lower temperatures, certain mineral elements in
ash, such as silica, potassium, and chlorine, may cause severe issues. 2. Material and methods
However, since they operate as catalysts, certain alkaline metals may
have a positive impact on biomass thermochemical conversion. In this 2.1. Biomass characterization
case, oxidative pyrolysis at a lower temperature range (550–750 ◦ C)
compared to gasification (800–1100 ◦ C) may be a promising process for Wood chips from forests and Pellets-DR were used for the oxidative
high ash biomass thermochemical conversion. pyrolysis experiments. The samples were characterized using proximate
In the case of a fixed bed configuration, oxidative pyrolysis consists and ultimate analyses. The moisture and ash content in biomass samples
of the formation of an oxidation zone, which propagates toward the raw were determined according to the International Organization for Stan­
biomass, where drying, pyrolysis, and partial oxidation of biomass and dardization ISO 18134–2 and ISO 1171, respectively. The Higher
volatiles occur to produce biochar, condensates (tars and water), and Heating Value (HHV) of biomass samples was determined using Differ­
permanent gases (CO, H2, CH4, and CO2) [14]. The process is controlled ential Scanning Calorimetry (DSC) according to ISO 18125. Carbon,
by the oxidation zone and its propagation through the fixed bed, which hydrogen, and nitrogen content were measured on a dry basis, and the
is a porous medium. The phenomenon is called “smoldering,” which is a oxygen yield was determined by difference. The biochar samples ob­
slow, low temperature (550–750 ◦ C), flameless, and oxygen-limited tained as a product from oxidative pyrolysis experiments were also
combustion driven by the energy released by the oxidation reactions characterized using the same methods for biomass ultimate and proxi­
of a solid phase fuel [16]. mate analyses.
During biomass oxidative pyrolysis, the oxidation zone is defined by
distinctive characteristics such as propagation velocity, temperature, 2.2. Fixed bed oxidative pyrolysis reactor
geometry (thickness and shape), yields, the composition of the produced
biochar, condensates (tars and water), and permanent gases. Earlier The stainless-steel cylindrical tube used for the fixed bed reactor for
studies on biomass oxidative pyrolysis investigated the oxidation zone biomass oxidative pyrolysis tests has an internal diameter of 180 mm, a
propagation velocity. The propagation rate, which is controlled by thickness of 3 mm, and a height of 800 mm. To decrease wall heat losses
combustion, heat, and mass transfers, depends on: air flow rate; fuel and preserve adiabatic conditions, 200 mm of Nappe Super-wool HT
properties (ash, size, bulk density, thermal conductivity, moisture, vol­ thermal insulation was used. Fig. 1 illustrates the oxidative pyrolysis
atile matter, and elemental composition); and air bed properties such as reactor for the batch counter-current system. The process consists of

2
F. El abdellaoui et al. Fuel 350 (2023) 128824

Fig. 1. Batch oxidative pyrolysis reactor with gas sampling line (left) and with different zones and thermocouples (right).

multiple steps, including biomass and air feeding, ignition, and oxida­ thermocouple was continuously recorded by an Agilent Data Acquisition
tion zone propagation in a fixed bed of biomass. Initially, the reactor was System 34970A and visualized by LabVIEW. The biomass was fed in
fed with biomass to create a 600 mm heigh bed. With the aim of elab­ batch mode at the top of the reactor and formed a fixed bed, supported
orating mass balances and evaluating biochar quality, the biochar was by a grate installed at the bottom of the reactor. The grate was connected
extracted by the end of the experiment for weighing and analysis to the biochar’s extraction device, which enabled the biochar manual
(Fig. 1). extraction. Produced gas was sent to a post-combustion chamber via a
As the reactor was equipped with pipes containing K-type thermo­ heated line. A gas sampling line was installed at the outlet of the reactor
couples along the reactor, temperature measurement was performed for post-analysis. The reactor’s air supply was controlled by a Mass
every 5 cm. Fig. 1 shows the implementation of the integrated temper­ StreamTM mass flowmeter and controller from Bronkhorst. During the
ature thermocouples. During experiments, the temperature from each tests, two pressure probes were placed at the inlet and outlet of the

Fig. 2. Sampling line with a heated line and a cold bath at 20 ◦ C and − 10 ◦ C with bubbling bottles (left) samples of condensates of water and tars (middle), and tars
after water evaporation (right).

3
F. El abdellaoui et al. Fuel 350 (2023) 128824

reactor to detect plugging or bridging. pyrolysis are biochar, permanent gases, and condensates (tars and
water). Thus, the mass balances can be written as follows:
2.3. Gas sampling line ṁin = ṁb,in + ṁAsh,in + ṁH2O,b,in + ṁO2,in + ṁN2,in (1)

Fig. 2 shows the condensates (tars and water) and permanent gases where ṁin [kg/h] is the total mass flow in the inlet of the reactor, and
sampling line, it consists of a heated pipe connecting the reactor with the ṁb,in , ṁAsh,in , ṁH2O,b,in , ṁO2,in , ṁN2,in, are respectively the biomass in dry
condenser, a series of bubbling bottles for tars condensation, and and ash free basis , ash, water from biomass , permanent gas, oxygen,
equipment for pressure and flow rate adjustment and measurement. The and nitrogen mass flow in the inlet of the oxidative pyrolysis reactor.
temperature for heating the pipe was carefully selected to prevent both ṁout = ṁbiochar,out + ṁAsh,out + ṁpg,out + ṁH2O,py,out + ṁH2O,b,out + ṁtars,out (2)
tars condensation and thermal decomposition. The temperature of the
condenser and bubbling bottles was selected to ensure qualitative tars Where ṁout [kg/h] is the total mass flow at the outlet of the reactor,
separation from permanent gases. To absorb the remaining traces of and ṁbiochar,out , ṁAsh,out , ṁpg,out , ṁH2O,py,out , ṁH2O,b,out , ṁtars,out are respectively
water and to protect the upstream gas analyzer, the last bottle was filled biochar in a dry and ash free basis, ash, permanent gases, water from
with silica gel. The gas was then sent through a pump, a gas flow meter, pyrolysis, water from biomass, and tars mass flow at the outlet of the
and a gas analyzer for the identification of permanent gases (N2, CO, oxidative pyrolysis reactor.
CO2, H2, CH4, and O2). Collected condensates from the sampling line Permanent gases analysis gives the mass flow of CO2, CO, CH4, N2,
were evaporated using a rotary evaporator RC900 (KNF, Switzerland) and O2 at the outlet of the reactor.
for gravimetric tar and water concentration determination. ṁpg,out = ṁCO2,out + ṁCO,out + ṁH2,out + ṁCH4,out + ṁN2,out + ṁO2,out (3)

Eqs. (4) to (15) were used to calculate the overall mass balance,
2.4. Operating mode
starting with determining consumed biomass and produced biochar at
the end of each experiment.
2.4.1. Starting up stage
During this stage, the oxidation zone was generated, and a biomass
• Biomass mass flow
bed of about 600 mm in height was supplied into the reactor. The heated
air was injected at a flow rate of 40 l/min for biomass drying, pyrolysis,
By knowing biomass fed to the reactor during a test, average wood
and partial oxidation. After 20 min, the temperature increases to around
consumption was calculated ṁb .
250 ◦ C; the excess heat of the bed’s surface starts, leading to the tem­
perature increasing at TV1 (Fig. 3). After the preheating and the gen­ mb
ṁb = (4)
eration of the oxidation zone, air was introduced at ambient ttest
temperature from the top of the reactor. Thus, a fixed bed was obtained Where mb [kg] is the mass of biomass consumed during the test, and
with low-temperature wood at the top (<100 ◦ C) and a high- the ttest [h] is the test duration.
temperature biochar bed at the bottom (about 600 ◦ C). The low and
high temperature zones were separated by a thin zone called the • Air
oxidation zone.
The inlet air volume flow rate in the reactor was obtained using a
2.4.2. Stationary stage flow meter. Thus, the mass flow rate was calculated using the formula:
After the oxidation zone generation, it propagates upward in the
fixed bed, which is a counter-current smoldering configuration, and a ṁa = V̇ a × ρa (5)
rapid temperature increase occurs when the oxidation zone passes 3
Where ṁa [kg/h] is the average air inlet flow, V̇ a [m /h] is the air
across a thermocouple to reach a value of 600 ◦ C (Fig. 3). At this stage,
volume flow, and ρa [kg/m3] is the air density.
the sampling line is connected to the reactor for condensate and per­
manent gas sampling.
• Biochar

2.5. Mass balances At the end of each test, the biochar collected in the tank was
weighted and kept for analysis. The mass flow rate of biochar was
The reactive are air and biomass, and the products from oxidative determined by weighing the biochar after each extraction. Thus, the
average flow rate of biochar ṁbiochar was calculated from the total bio­
char mass and the test duration.
mbiochar
ṁbiochar = (6)
ttest
where ṁbiochar [kg/h] is the average biochar mass flow, mbiochar [kg] is
the total mass of produced biochar.

• Permanent gases

The mass flow rate and composition of the produced permanent

gases were determined.
Fig. 2 shows the system for permanent and condensable gas sam­
pling. Permanent gases were characterized using Vario Luxx gas
analyzer from MRU Instruments. The average flow rate of permanent
gases was determined using the mass conservation of nitrogen as an inert
gas.
Fig. 3. Temperature evolution during a starting up stage of a test with ṁN2,in = ṁN2,out (7)
wood chips.

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F. El abdellaoui et al. Fuel 350 (2023) 128824

Where ṁN2,in [kg/h] is nitrogen flow in the inlet of the reactor, and 2.6. Equivalence ratio for autothermal operation
ṁN2,out [kg/h] is the nitrogen mass flow at the outlet of the reactor.
Nitrogen from the air at the inlet was used as a tracer to calculate the Equivalence ratio (ER) is a parameter commonly used to quantify
total mass flow rate of permanent gases at the outlet of the reactor. whether the mixture of fuel and the oxidizer is rich, lean, or stochio­
Knowing the mass fraction of nitrogen in the air at the inlet and the mass metric. The air/fuel equivalence ratio is defined as the ratio of the actual
fraction of nitrogen in the sampled gases at the outlet can be written as flow rate of air to the flow rate of air that would be needed to achieve
follows: stoichiometric combustion of the biomass fed to the reactor and is
calculated as follows [21]:
ṁN2,in
ṁpg = (8) ( A)
YN2,out
ER = F( AStioc
) (16)
Where ṁpg [kg/h] is permanent gas (non-condensable gas) mass flow F

rate, ṁN2,in [kg/h] is nitrogen mass flow in the inlet of the reactor, and Depending on the value of ER, the distinction is between the fuel-rich
YN2,out [% mass] is N2 mass fraction in the produced permanent gases, mixture (ER >1), fuel-lean (ER <1), and stoichiometric mixture (ER =
calculated from its volume concentration as follows: 1).
MN2 × [N2 ]
YN2,out = (9) 3. Results and discussion
Mpg

The other compounds mass fraction in the produced permanent gases 3.1. Biomass analysis
were calculated by the same equation:
Mi × [Xi,out ] Table 1 presents the proximate and ultimate analyses of wood chips
Yi,out = ∑ (10) and Pellets-DR. The results show that the main differences between
Xi,out × Mpg
wood chips and the Pellets-DR are ash content and volatile matter. The
where i = N2, CO, CO2, H2, CH4, Yi,out [%mass] is compound mass ash content of Pellets-DR is 21.7%, but only 0.5% of minerals are present
fraction in the produced gas, Mi [g/mol] is compound molar mass, [Xi,out ] in wood chips. Moreover, volatile matter in wood chips (82.9%) is
[%vol] is compound volume fraction in the produced gas, Mpg [g/mol] is higher compared to Pellets-DR (57.1%).
permanent gases molar mass. Feedstock bulk density was also the main difference between wood
Finally, mass flow rate of each gas in the permanent gases was chips (244 kg/m3) and Pellets-DR (700 kg/m3). The bulk density of the
calculated using the equation: two feedstocks was calculated based on their mass and volume. The
results are given in Table 2.
ṁi = Yi .ṁpg (11)

where ṁi [kg/h] is mass flow of compound i, Yi [% mass] is mass

fraction rate of compound i in the produced gases, and ṁpg [kg/h] is 3.2. Air/biomass ratio and equivalence ratio
mass flow rate of permanent gases.
The biomass consumption rate, air biomass ratio, and equivalence
• Condensates ratio were calculated from the biomass consumption rate. The equiva­
lence ratio indicates the consumption of biomass to sustain oxidation
Condensates were calculated by weighing over the sampling time the zone propagation under the same air flux. The results are given in
average flow rate of the sampled condensable gases (tars and water). Table 3 on a dry basis. The average biomass consumption was 0.020 kg/
Unless the ratio between the flow rates of condensable gases and per­ m2. s for wood chips and 0.017 kg/m2. s for Pellets-DR, for a specific air
manent gases at the outlet of the reactor is constant, thus: flux of 0.012 kg/m2. s. Thus, the air/biomass ratio was 0.615 and 0.734
⎛ ⎞ for wood chips and Pellets-DR, respectively, and the equivalence ratio
ṁcg ⎝ṁcg ⎠ was 0.102 and 0.153, which means that the oxidation zone consumed 10
= (12) to 15% of the stoichiometric air to provide energy to the process through
ṁpg ṁpg
sample partial combustion.
where ṁcg [kg/h] is the mass flow rate of condensable gases. Con­ The oxidative pyrolysis of three types of biomass —pine, miscanthus,
densable gases include tars, water from oxidative pyrolysis, and water and wheat straw — was previously investigated. The main difference
from biomass in the inlet of the reactor. By assuming that biomass water between the three types of biomass was ash content. It was 0.3, 3, and
content was totally collected in the condensable gases, thus: 8.2% on a dry basis for pine, miscanthus, and wheat straw, respectively
[16]. The ER reported in the previous study was between 11% and 14%,
%W
ṁH2O,b = ṁb × (13)
100 Table 1
where ṁH2O,b [kg/h] is water mass flow rate from biomass in the inlet Proximate and ultimate analyses of wood chips and Pellets-DR.
of the reactor, ṁb [kg/h] is wet biomass mass flow rate in the reactor WC-P16F05 Pellets-DR
inlet, and %W [% mass] is biomass moisture. wt.% 8,16 7,80
Thus, water and tars mass flow rate from biomass oxidative pyrolysis
were calculated using the equations:
Proximate analysis (% dry mass)
ṁH2O,OP = ṁcg YH2O,cg − ṁH2O.b (14) Ash at (815 ◦ C) 0,50 21,70
VM 82,90 57,10
FC 16,60 21,20
ṁtars = ṁcg − ṁH2O,OP − ṁH2O,b (15)

where ṁH2O,b , ṁH2O,OP , ṁcg YH2O,cg , ṁtars , and ṁcg [kg/h] are respectively Ultimate analysis (% dry mass)
water mass flow rate from biomass in the reactor inlet, water mass flow C 50,50 41,20
H 5,80 4,40
rate from oxidative pyrolysis, water from sampled condensable gases N 0,20 1,30
mass flow rate, tars mass flow rate, and total sampled condensable gases O (the difference) 41,90 34.30
mass flow rate. LHV (MJ/kg dry mass) 20,32 15,15

5
F. El abdellaoui et al. Fuel 350 (2023) 128824

Table 2
Bulk density of wood chips and Pellets-DR.
Biomass WC-P16F05 Pellets-DR

Bulk density, ρwood, (kg/m3) 244 700

Table 3
Air biomass and equivalence ratio during oxidative pyrolysis of wood chips and
Pellets-DR.
WC-P16F05 Pellets-DR
2
Air mass flow rate (kg/m . s) 0,012 0,012
Average biomass consumption (kg/m2. s) (dry basis) 0,020 0,017
Air/biomass ratio (dry basis) 0,615 0,734
Air/biomass stoichiometry (dry basis) 6.016 4.789
Equivalence ratio (dry basis) 0.102 0.153

which is comparable to our results for Pellets-DR with an ash concen­ Fig. 4. Fixed bed temperature for a batch test with wood chips with 0.012 kg/
tration (21.7% of ash concentration) higher than residues from agri­ m2.s air flux.
culture and wood chips reported in previous work.

3.3. Oxidation zone propagation

The average propagation velocity was 0.50 cm/min for wood chips
and 0.14 cm/min for Pellets-DR (Table 4). The difference between the
two feedstocks may be explained by the density, which is 244 kg/m3 for
wood chips and 700 kg/m3 for Pellets-DR. The same results were found
by investigating wood chips and wood pellets. It was concluded that the
oxidation zone propagation velocity was inversely proportional to the
biomass bulk density, and an average propagation velocity of 0.4 cm/
min was reported [14]. However, 0.28 cm/min, 0.37 cm/min, and 0.39
cm/min were reported for pine, miscanthus, and wheat straw pellets,
respectively. The differences between the three types of biomasses were
the ash content and density [16]. According to the same author, how­
ever, ash concentration had a significant impact on the propagation
velocity of the oxidation zone. Furthermore, earlier research has also
shown that biomass with a low ash content has a high propagation rate
[18]. Other factors, like density, moisture, and size distribution, also
affect the rate of propagation, which makes it difficult to understand and Fig. 5. Fixed bed temperature for a batch test with Pellets-DR with 0.012 kg/
m2.s air flux.
explain their influences [14,16,18].

significant difference in terms of water content. Therefore, there is only

3.4. Temperatures
a slight difference in the final temperature. As illustrated in Fig. 4 and
Fig. 5, the temperature in the fixed bed at the thermocouple TV1 is stable
During a test in batch mode, the oxidation zone propagates upward
at around 50 ◦ C before it increases rapidly to 600 ◦ C when the oxidation
in the fixed bed. Fig. 4 and Fig. 5 show the temperature of the fixed bed
zone reaches the thermocouple TV1. This difference in temperature may
on the thermocouples TV1, TV2, and TV3 (Fig. 1) during a test with
be explained by the presence of wood at an ambient temperature above
wood chips and Pellets-DR, respectively, with an airflow of 0.012 kg/
the oxidation zone. As a result, a fixed bed with low-temperature wood
m2. s. The oxidation zone was supposed to reach a given thermocouple
on top (<100 ◦ C) and high-temperature biochar on the bottom (around
when its temperature increased rapidly to reach a temperature of
600 ◦ C) were obtained. The low and high temperature zones are sepa­
500 ◦ C- 600 ◦ C.
rated by a thin zone called the oxidation zone.
For both wood chips and Pellets-DR, the temperature has the same
Moreover, comparing the thermal behavior of wood chips and
behavior. Moisture content has been strongly linked to overall biomass
Pellets-DR, the time needed for the thermocouple TV1 to reach a tem­
thermochemical conversion performance [22,23]. Also, a high moisture
perature of 600 ◦ C is relatively long (50 min) in comparison to wood
content presents a challenge from a thermal point of view; it increases
chips (20 min). This difference may be explained by the oxidation zone
drying and devolatilization time and reduces the global energy of the
propagation velocity, which is faster in the case of wood chips (0.5 cm/
reactor because of the endothermic reactions during water evaporation.
min) instead of 0.14 cm/min for Pellets-DR and is inversely proportional
However, in the case of dried Pellets-DR and wood chips, there is not a
to feedstock bulk density (700 kg/m2 for Pellets-DR and 244 kg/m3 for
wood chips). According to earlier studies, the structure of the oxidation
Table 4 zone, which depends on the density and size distribution of the wood,
The average propagation velocity for wood chips and Pellets-DR with 0.012 kg/
explains why the temperature in wood chips was higher than in wood
m2.s air flux.
pellets [14]. Moreover, this difference in temperature directly affects the
WC-P16F05 Pellets-DR kinetics of reactions involved during pyrolysis, biochar gasification,
Wood bulk density (kg/m3) 244 700 homogeneous and heterogeneous oxidation reactions, and water shift.
Wood mass flow rate (kg/m2. s) 0,020 0,017 Thus, further investigations into how temperature affects the reaction
Average propagation velocity (cm/min) 0,500 0,140
mechanisms could explain this relationship.

6
F. El abdellaoui et al. Fuel 350 (2023) 128824

Fig. 6 shows temperature variation along the reactor walls and the Table 5
fixed bed at the thermocouple TV1 through time during a batch test with Inlets and outlets flow rates (kg/h) of the oxidative pyrolysis of the two types of
wood chips and a 15 l/min airflow. TV1, installed inside the fixed bed biomass for 0.012 kg/m2.s air flux.
reactor, is in the same position as the thermocouple T19, fixed to the Flow rate (kg/h) Chemical WC- Pellets-
reactor’s internal walls (Fig. 1). At the beginning of the test, T19 was formula P16F05 DR
around 50 ◦ C. This temperature rises to 200 ◦ C when the oxidation zone Inlets
reaches the thermocouple TV1. The zone of fixed bed wood above the Biomass (dry ash free) CxHyOz 1.865 1.267
oxidation zone is subject to low temperatures (<200 ◦ C). Then, when the Water (from biomass) H2O 0.166 0.108
Oxygen (from air) O2 0.242 0,242
oxidation zone reached TV1, T19 increased rapidly to reach a maximum
Nitrogen (from air) N2 0.91 0,91
value of 480 ◦ C after 40 min. This increase is due to the heat exchanges Ash (from biomass) 0.010 0,302
between the oxidation zone and the reactor walls.
Outlets
3.5. Oxidative pyrolysis product yields Biochar (dry ash free) 0.527 0,329
Tars 0.102 0,131
Results from wood chips and Pellets-DR with an airflow of 0.012 kg/ Condensate (tars and water from 0.300 0,220
oxidative pyrolysis)
m2.s are presented in this section. The products entering and leaving the Total condensate 0.467 0,330
oxidation zone beds for the two types of biomass were taken into ac­ Drying water H2O 0.170 0,109
count when calculating the mass balances based on the experimental Permanent gases CO2 0.984 1.102
findings. The method used in the calculation was described in Section CO 0.487 0,259
H2 0.016 0,018
2.5, and Table 5 gives the inlets and outlets of the oxidative pyrolysis
CH4 0.071 0,045
reactor. Nitrogen N2 0.910 0,910
Because of the significant difference in ash content between wood Ash (from biochar) 0.013 0,389
chips and Pellets-DR, the yields of products from oxidative pyrolysis
were calculated based on a mass dry ash-free basis. The results are
presented in Fig. 7. Because oxygen from the air reacts entirely within 121% for Pellets-DR. As the study was conducted under the same con­
the bed and is recovered as a product of biomass oxidative pyrolysis, the ditions of ER and temperatures, the difference may be explained by
total mass of the measured yields exceeded 100% [13,14]. biomass properties such as ash content and bulk density.
As Fig. 7 shows, the yield of biochar was 28% for wood chips and In the case of biomass oxidative pyrolysis, with an extremely low air
25% for Pellets-DR. The yield of condensates was about 26% for wood flux, the heating rate and the obtained temperature are low compared to
chips and 25% in the case of Pellets-DR. However, the mass fraction of the rapid pyrolysis process, where the heating conditions are particu­
tars on a dry ash-free basis was 10.36% for Pellets-DR and 5.47% for larly important, whereas the heating rate plays a significant role in
wood chips. The yield of permanent gases was 83.6% for wood chips and product yield distribution [24]. The produced biochar yields are

Fig. 6. Fixed bed and wall temperatures for a batch test with wood chips with 0.012 kg/m2.s air flux.

7
F. El abdellaoui et al. Fuel 350 (2023) 128824

3.6. Products composition from oxidative pyrolysis

3.6.1. Gases

3.6.1.1. Permanent gases. Fig. 8 shows the composition of the perma­

nent gases during a test in batch mode with wood chips and Pellets-DR
with an airflow of 0.012 kg/m2. s, CO2 is the dominant gas for both
biomasses, varying from 75% for Pellets-DR to 55% for wood chips.
Thus, the Low Heating Value (LHV) of produced permanent gases is
12.33 MJ/kg and 11.38 MJ/kg for Pellets-DR and wood chips, respec­
tively (Fig. 9). The amount of CO from Pellets-DR was 19%; it was lower
than the amount from wood chips, which was 25%. The differences can
be explained by the catalytic effect, which is higher in the case of Pellets-
DR because of the high ash content compared to wood chips. However,
the results from the literature observed higher yields of CO2 and CO with
Fig. 7. Mass yield on a dry ash free basis of oxidative pyrolysis of wood chips higher ash content in biomass during pyrolysis [25,26,28]. Also, it was
and Pellets-DR with 0.012 kg/m2.s air flux.
claimed that the decarboxylation of uranic acids alone could explain the
increase in the total yield of the catalytic formation of carbon dioxide
relatively high compared to rapid pyrolysis, where 60–70% of the dry [16].
biomass input was recovered as organic compounds, and this difference In a previous study, the pyrolysis of wood chips was investigated in
can be explained by the heat transfer conditions in the fixed bed and inert and oxidative atmospheres [13]. In the case of inert pyrolysis,
within the particle size [13,25,26]. The thermal behavior and the effect increasing the temperature yields a higher production of carbon mon­
of the heating rate of biomass during biomass pyrolysis in an inert and oxide and hydrogen. The results were attributed to the secondary tar
oxidative atmosphere were largely investigated both on a particle scale cracking reactions. Whereas, in the case of an oxidative atmosphere,
[24] and in a wire mesh [27], and it was confirmed that higher heating even at elevated temperatures, compared to inert pyrolysis, the presence
conditions resulted in higher condensate products and lower yields of of air increased the carbon dioxide, but there was no significant differ­
biochar. ence between the yields of biochar in the inert or oxidative atmosphere
Temperature plays a key role in product distribution during biomass for low air flux. The results were attributed to the oxidation reactions of
pyrolysis; previous studies reported that increasing temperatures from organic elements, which resulted in a drastic decrease in tar cracking
375 ◦ C to 575 ◦ C resulted in biochar and condensate yields decreasing reactions inside the biochar bed and the partial oxidation of biochar in
from 30 to 23 wt% and 43 to 32 wt%, respectively, while permanent gas the presence of oxygen. During oxidative pyrolysis, more CO, CO2, and
yields increased from 11 to 30 wt% [13]. The same results were reported H2 were produced than during inert pyrolysis [13,27].
for a fixed-bed reactor [24]. Therefore, in the case of oxidative pyrolysis
of wood chips, when comparing our results with the previous results, the 3.6.1.2. Condensates. The condensates from biomass oxidative pyroly­
difference in terms of temperatures must be taken into consideration. In sis are composed of water from biomass, water from pyrolysis reactions,
this study, a maximum temperature of 600 ◦ C was reached using a very and tars (organic matter). Produced tars represented about 10% and 6%
low air flow, whereas the temperature obtained from previous studies of of the initial biomass on a dry and ash-free basis for Pellets-DR and wood
fixed bed oxidative pyrolysis was 750 ◦ C [14,16]. To the best of our chips, respectively, which is the equivalence of a concentration of 25 g/
knowledge, there are no experimental studies on oxidative pyrolysis of Nm3 and 38.67 g/Nm3 in the produced gases (Fig. 10). According to the
residues from lignocellulosic anaerobic digestion. However, few studies current study and previous works on biomass pyrolysis in inert and
have investigated the oxidative pyrolysis of biomass from agriculture, oxidative atmospheres, oxidative pyrolysis produces less tars than inert
which is also characterized by a high ash content compared to woody pyrolysis [13,14]. The difference is explained by the presence of oxygen,
biomass but lower than Pellets-DR in the present study. The results which results in the partial oxidation reactions of volatiles from biomass
showed that ash content plays a significant role in product distribution pyrolysis during homogeneous and heterogeneous secondary reactions.
during biomass oxidative pyrolysis [16,18].Section 3.6 goes into more Analyzing the tars composition would explain in detail the mechanisms
detail about how ash content affects product yields and compositions. involved in tars reforming during biomass oxidative pyrolysis. However,
the present study was limited to the determination of tars gravimetry.
Previous studies on wood chip pyrolysis in an oxidative atmosphere
found that the presence of oxygen had no effect on the distribution of

Fig. 8. Composition of permanent gases from oxidative pyrolysis of wood chips Fig. 9. Low Heating Values of permanent gases from oxidative pyrolysis of
and Pellets-DR with 0.012 kg/m2.s air flux. wood chips and Pellets-DR with 0.012 kg/m2.s.

8
F. El abdellaoui et al. Fuel 350 (2023) 128824

3.6.2. Biochar
Table 6 presents a proximate and ultimate analysis of biochar from
wood chips and Pellets-DR. The ultimate and proximate analysis of
biochar produced from both types of biomasses revealed that carbon was
the most abundant element in wood chips (87.8%), but only 48.3% in
Pellets-DR. This difference could be explained by the high ash content in
the case of Pellets-DR (54.2%), which represents only 2.5% for biochar
from wood chips. Thus, the main difference between Pellets-DR and
wood chips was also found in biochar’s Low Heating Value (LHV), which
is 31.9 MJ/kg for wood chips and 13.01 MJ/kg for Pellets-DR.
The results from the present analysis on produced biochar are
compared with the results on wood chips and wood pellets [14] and with
the results from biomass from agriculture such as wheat straw and
miscanthus [16], which reported the catalytic effects of ash on sec­
Fig. 10. Tars and water concentrations in the produced gas from a test with ondary biochar formation by condensation or polymerization of the
wood chips and Pellets-DR with 0.012 kg/m2.s.
primary tars and the interaction between the resulting volatiles and
biochar [30].
organic compounds, and it was reported that the decrease in the pro­
duction of lumped compounds was due to oxidation or cracking re­
3.7. Effect of air flux
actions caused by higher temperatures inside the fixed bed reactor, but
the mechanism was difficult to explain [13]. Therefore, considering the
3.7.1. Equivalence ratio
tar compounds individually confirmed that the production of carboxylic
As mentioned before, the equivalence ratio is the most important
acids, levoglucosan, or guaiacols preferentially decreased while that of
parameter that affects the front propagation velocity during biomass
light aldehydes did not appear to be influenced by the presence of ox­
oxidative pyrolysis. Porteiro et al.[18] investigated in detail the effect of
ygen, which means that selectivity is involved in the oxidation of
air flux on different types of biomass oxidative pyrolysis. Based on the
organic compounds [13]. Moreover, they observed that cracking re­
amount of air, three regimes were determined. The results of this study
actions were enhanced during oxidative pyrolysis. In addition to the
are presented together with the fuel stochiometric limit in Fig. 11. The
work on the comparative study between inert and oxidative pyrolysis of
stochiometric limit is used to identify the combustion regime of each
wood chips, oxidative pyrolysis of wood chips and wood pellets was
point (sub-stochiometric or combustion with excess air). Depending on
investigated. The results confirmed that about 40% of the organic con­
the specific mass flux of air and biomass, the distinction was between
densates were quantified in the collected samples because it is difficult
three stages: the first phase with a positive slope corresponds to the
to identify and quantify all the organic compounds using Gas
oxygen-limited phase, and the second stage, the reaction-limited phase,
Chromatography-Mass Spectrometry (GC–MS) [14]. This can be because
takes place where the curve reaches its maximum value. The final stage
of the presence of low concentrations to be separated in the chroma­
represented by a negative slope is known as quenching by convection; it
tography, and it may also be explained by the pyrolytic lignin, which can
begins when the air exceeds the stoichiometric limit.
be present in the sample of tars but is not quantified by chromatography
To investigate the effects of air flux on the front propagation velocity,
[29]. Therefore, by identifying and quantifying 40% of tar organic
the yield, and the composition of the products, three air fluxes at 10 l/
compounds, it was reported that 57% of them are classified as primary
min, 15 l/min, and 20 l/min for wood chips were used. Table 7 repre­
tars and the rest, 43%, as secondary tars and tertiary groups [14]. Most
sents the results of the equivalence ratio for each test. The air flux was in
of the organic compounds detected during biomass pyrolysis in an inert
the range of 0.008 and 0.017 kg/m2. s, which is lower than 0.1 kg/m2.s.
atmosphere are primary tars produced directly from biomass decom­
Thus, the present study is about low air flux and is limited to the first
position [27,28]. Therefore, the occurrence of tar cracking and oxida­
regime, known as the oxygen-limited zone.
tion reactions during biomass oxidative pyrolysis results in more
In the case of wood chips and for the three specific air fluxes of 0.008,
secondary tars and fewer primary tars compared to inert pyrolysis.
0.012, and 0.017 kg/m2. s, the equivalence ratio was 0.079, 0.102, and
Regarding the water concentration in the products, previous studies
0.131, respectively (Table 7). Thus, it increases with increasing specific
on the pyrolysis of wood chips in inert and oxidative pyrolysis showed
air flux, which means that at low air flux, less air is consumed to
that pyrolysis water yields were 15 to 27% higher in oxidative pyrolysis
maintain the oxidation zone and its propagation along the fixed bed. The
than in inert pyrolysis because of oxidation reactions [13].
limited airflow may explain the lower temperature obtained in the fixed
Moreover, the concentration of water produced during the oxidative
bed during the test in Section 3.4, which also influenced the reaction
pyrolysis of wood chips was higher in the case of wood chips compared
to Pellets-DR. This difference may be explained by the high value of ash
Table 6
content in the case of Pellets-DR (21.7%) compared to wood chips
Biochar from oxidative pyrolysis of wood chips and Pellets-DR.
(0.5%). Indeed, Williams et al. [26] claimed that the ash content acts as
a catalyst to convert the oxygen in the pyrolysis oil to CO2 and CO at WC-P16F05 Pellets -DR
higher temperatures and to H2O at lower temperatures. The same results wt. % 3.2 2.5
were observed later in the case of oxidative pyrolysis of woody biomass
and agricultural residues with high ash content, where CO and CO2 were Proximate analysis (% dry mass)
higher while oxygen content in the condensates was lower in the case of Ash at (815 ◦ C) 2.5 54.2
miscanthus and wheat straw than those of pine wood [16]. VM 13.2 8.1
FC 84.3 37.7
The complexity of the composition of tars makes it difficult to
characterize it in detail. Hence, enhancing the methods of sampling and
analysis of the tars may help to understand the mechanisms linked to the Ultimate analysis (% dry mass)
C 87.8 48.3
formation and reforming of tars. Moreover, changing the parameters,
H 1.8 0.4
such as temperature and ER, may explain the effect of these parameters N 0.3 0.9
on the composition of the products from biomass oxidative pyrolysis. O (by difference) 6.3 8.2
LHV (MJ/kg dry mass) 31.93 13.01

9
F. El abdellaoui et al. Fuel 350 (2023) 128824

Fig. 11. Air flow rate versus fuel mass flux with the three combustion phases (with permission from Elsevier)) [18].

Table 7
Air biomass ratio and equivalence ratio for different values of air flux during
oxidative pyrolysis of wood chips.
10 l/ 15 l/ 20 l/
min min min

Air mass flow rate (kg/m2. s) 0,008 0,012 0,017

Average biomass consumption (kg/m2. s) (dry 0.017 0,020 0,021
basis)
Air/biomass ratio (dry basis) 0,481 0,615 0,786
Air/biomass stoichiometry (dry basis) 6,016 6,016 6,016
Equivalence ratio (dry basis) 0,079 0,102 0,131

kinetics and oxidation zone propagation during biomass oxidative py­

rolysis. However, the air is not the only parameter affecting the reaction
kinetics and oxidation zone propagation; other factors include chemical Fig. 12. Repartition of products from oxidative pyrolysis of wood chips at
reactions, bed compaction, mass, and heat transfers. This study limited different air mass fluxes.
to the effect of air flux is not enough to explain the effect, and only an
approach that separates the impact of the chemical, thermal, and
physical phenomena that control the process would explain this impact.
Furthermore, a modeling approach may be a powerful tool for more
investigations and could provide more answers. For the present study,
the air/biomass mass ratio changes between 0.48 and 0.78. In the case of
stoichiometric conditions, this ratio is about 6.016 kg/kg of biomass.
Thus, the oxidation zone consumes between 8% and 13% of the stoi­
chiometric air to convert biomass into biochar and gases (Table 7).

3.7.2. Products yield

As Fig. 12 shows, increasing the specific air flux from 0.008 to 0.017
kg/m2.s increased the amount of condensates and permanent gases.
However, changing the values of air flux did not significantly influence
the yields of the produced biochar. This means that the increase in
Fig. 13. Composition of permanent gases from oxidative pyrolysis of wood
permanent gas is due to gas reforming or volatile oxidation rather than
chips at different values of air mass fluxes.
biochar oxidation. Previous studies concluded that there is no significant
biochar oxidation under extremely low air fluxes and that the only
significantly with an increase in air flux. At extremely low airflow and
source of energy for the process is the oxidation of volatile matter
under oxygen-limited conditions, increasing air flow did not signifi­
[13,18].
cantly affect the permanent gas composition.
Fig. 13 shows the composition of permanent gases at different air
fluxes; the results show that increasing air flux reduces CO2 concentra­
3.7.3. Propagation velocity
tion. However, the concentrations of CH4, H2, and CO did not change
Regarding the average propagation of the oxidation zone in the case

10
F. El abdellaoui et al. Fuel 350 (2023) 128824

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