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(2016) 6:49–59
DOI 10.1007/s13399-015-0174-6
ORIGINAL ARTICLE
Received: 9 January 2015 / Revised: 2 June 2015 / Accepted: 1 July 2015 / Published online: 14 July 2015
# Springer-Verlag Berlin Heidelberg 2015
Influence of reactor length and residence time was studied concentration. As standard feedstock for gasification,
by Zhao et al. [4] and Hernandez et al. [8], respectively. After sawdust was selected, whereas coconut shell was chosen
a critical reactor length, the gas flow and conversion were as non-standard feedstock for comparison. Along with
found to be saturated. In contrast, increase in residence time comparison, another reason behind selecting coconut
showed positive effect on CO and H2 production. However, shell was to assess its gasification potential under
the biomass species were not similar in both cases and cannot entrained flow condition.
be compared directly. But, it is important to evaluate the con-
tradictory findings from these studies. Qin et al. [9]
established that at a very high temperature (1400 °C), the
residence time would have minimal effect if it is over 2 Materials and methods
2.5 s. In the case of temperature, there is no ambiguity
about its influence on the gasification and conversion. 2.1 Sample preparation
Significant increase in gas production was observed for
different biomass from 700 °C to 1400 °C by Zhou Norway spruce (Picea abies) and coconut shell were pyro-
et al. [2], Lapuerta et al. [8], Hernandez et al. [6] and lyzed at 1000 °C to ensure complete devolatilization in an
Zhao et al. [4] in separate studies. entrained flow reactor (1.885 m) with parent particle sizes in
As a whole, the operating parameters did not follow any the range of 150–250 and 500–600 μm. The particle sizes
particular pattern which could generalize the results. However, were chosen in a way that they were distinct enough to exert
these studies provide valuable information about the effect of difference in gasification characteristics yet suitable for
temperature, residence time, particle size and excess air ratio entrained flow condition. The pyrolysis time for different par-
on gasification of raw biomass. Increasing temperature was ticle sizes and samples varied from 0.16 to 0.7 s, whereas the
definitely one of the most popular options to increase the residence time inside the reactor varied from 2 s (for coconut
conversion and gas yield. At the same time, it is essential to shell 500–600 μm) to 9 s ( for spruce 150–250 μm). There-
study the entrained flow gasification with individual gasifying fore, the residence time for pyrolysis was enough for a com-
agents such as CO2 and H2O to produce the right ratio of CO plete devolatilization. It is assumed that the surface area of
and H2 mixture. It is, therefore, also important for modeling different samples was not affected significantly by the higher
purpose which can be later useful for scaling up the process. residence time for the smaller particles in the absence of any
As char gasification is the slowest step of all, it is also neces- activating agent (i.e., CO2 and H2O) [16]. The particle size
sary to study it individually. Disappointingly, char gasification distributions of the raw and pyrolyzed samples are given in
studies under entrained flow condition are scarce in literature. Fig. 1a, b, respectively. The raw samples were well distributed
A few studies in pressurized drop tube furnace were per- in particle size. After pyrolysis, particle size of spruce shrank
formed by Kajitani et al. [13, 14] which addressed the effect to some extent, whereas coconut shell was almost unchanged.
of pressure and temperature on the kinetics of the coal char These samples were used as received from the entrained flow
gasification process under CO2 and air separately. However, pyrolysis process without any further sieving or grinding to
those studies were mainly performed under kinetic control retain the char structure. The chars were denoted as spruce
using very small particles and did not consider the particle char (SC) and coconut shell char (CSC) with average particle
size effect. Another notable work was performed by Tanner size (e.g., 200 for 150–250 μm) in the following figures and
et al. [15] on low temperature gasification of Victorian brown manuscript. The adsorbed moisture on the char surface was
coal char under entrained flow by varying the operating pa- measured by a halogen moisture analyzer (Model HB43-
rameters. They found that the temperature (up to 1000 °C) and S, Mettler-Toledo, USA). Table 1 shows the ultimate
residence time (up to 6 s) were not sufficient to convert the analysis and surface area (CO2 adsorption) of the sam-
coal char completely. Most other char gasification studies con- ples which was determined by ultimate analyzer (Model
cern reactivity and kinetics in thermogravimetric analyzer. 2400, PerkinElmer, USA) and ASAP 2020 (Accelerated
Moreover, depending on the species, the char gasification be- Surface Area and Porosimetry System, Micromeritics,
havior might become very different. That is why biomass USA), respectively. Due to the limitations of using N2
gasification cannot be compared directly with coal char gasi- adsorption at −196 °C for measuring surface area, CO2
fication and therefore, biomass species need to be studied adsorption (0 °C) method was chosen [17]. In the raw
individually under relevant conditions to be considered for sample, sawdust had (0.1 % S) lower sulfur content
large-scale gasification. than coconut shell (0.95 % S). Therefore, all the sulfur
Based on the discussion above, this study aims to was released during pyrolysis for the smaller particle
assess CO2 gasification of chars obtained from entrained size of sawdust, whereas the larger particles retained
flow pyrolysis of two biomass feedstock to evaluate the some. On the other hand, coconut shell char had some
e ff e c t s o f t e m p e r a t u r e , p a r t i c l e s i z e , a n d g a s sulfur left for both the samples.
Biomass Conv. Bioref. (2016) 6:49–59 51
0.8
0.6
0.5
0.4
0.3
0.2
Spruce 150−250 µm
Coconut Shell 150−250 µm
0.1 Spruce 500−600 µm
Coconut Shell 500−600 µm
0
0 100 200 300 400 500 600 700 800 900 1000
Particle size (µm)
0.9
b
0.8
Cumulative mass fraction
0.7
0.6
0.5
0.4
0.3
0.2
Spruce Char from 150−250 µm
Coconut Shell Char from 150−250 µm
0.1 Spruce Char from 500−600 µm
Coconut Shell Char from 500−600 µm
0
0 100 200 300 400 500 600 700 800 900 1000
Particle size (µm)
2.2 Experimental after gasification, whereas the gas line was passed
through two cold traps and particulate filter. After the
2.2.1 Setup particulate filter, a micro gas chromatograph (micro-GC,
Varian CP-4900, Agilent Technologies, USA) was con-
Entrained flow gasification of the char particles was conduct- nected to measure the gas composition. The micro-GC
ed in the same reactor used for pyrolysis. The outer shell of the detects H2, N2, and CO in the first column, and CO2
tube was used for preheating the gas before entering the reac- and CxHy in the second column, respectively. Further
tor. The furnace enclosing the reactor was heated to the desired details about the experimental setup can be found else-
temperature before the experiment. The reactor was 2 m where [18]. It is to be noted that if this process is to be
long with a reaction zone of 1.885 m. A quartz connec- adopted for pilot scale, an autothermal operation would
tor at the bottom was used to collect the residual mass be ensured by burning some biomass or char.
52 Biomass Conv. Bioref. (2016) 6:49–59
2 80
50
1 40
30
0.5 20
SC 200
SC 550
10
CSC 200
CSC 550
0 0
800 850 900 950 1000 1050
o
Temperature ( C)
convert the particles. As char gasification is the slowest step the gas side conversion calculations were fairly close to the
during conversion of biomass into gas, it is of great interest to solid side-based calculations. This means that only gas side
study the effect of operating parameters on the process. The calculation would suffice the need for the char conversion
residence times for the samples were determined to be about 9, calculation for overall mass balance. It would be further sup-
4.5, 7, and 2.5 s for SC200, SC550, CSC200, and CSC550, ported later by the fact that no significant tar production was
respectively. As mentioned in the experimental procedure, observed.
solid conversion was verified from by ash tracing and gas
measurement. All the calculations were in good agreement 3.2 Effect of temperature
considering an experimental error of ±10 %. A representative
graph of the conversion comparison from both solid and gas Temperature is one of the most important factors to convert a
side is shown in Fig. 2 for the experiments performed under char particle completely during gasification. This study was
20 % CO2 for two particle sizes. It shows the uncertainty conducted in the low temperature to evaluate the biomass char
related to the conversion calculation. As seen in the figure, gasification behavior under entrained flow condition.
2 0.08
0.07
CO gas yield (L/g char)
1.5 0.06
0.05
1 0.04
0.03
0.5 0.02
SC 200
SC 550 0.01
CSC 200
CSC 550
0 0
800 850 900 950 1000 1050
Temperature (oC)
54 Biomass Conv. Bioref. (2016) 6:49–59
It was expected that temperature would have positive effect 600-μm particle sizes, respectively, for spruce char. Both con-
on char conversion, but it was also important to quantitatively version and gas release increased for different particle sizes
determine the optimum temperature. Figure 3 shows the effect under consideration with increasing temperature. In this case,
of temperature on the total gas evolution at different temper- the gas evolution could be considered as directly proportional
ature under 20 % CO2. The plot also shows the remaining to the conversion of solids due to negligible or no tar produc-
mass after gasification on the right axis. It is notable that tion during the char gasification process (as seen in Fig. 2).
coconut shell char did not show significant increase in gas However, the conversion efficiency cannot be directly related
release with increasing temperature. In other words, solid con- to the microporous surface area of coconut shell and spruce
version varied from 2 to 8 %. On the other hand, about 25 and char, as the difference in surface area is not significant [23]
50 % conversion were achieved for 150–250 and 500– (Table 1). This might be due to the abundance of micropores
70
Conversion (%)
60
50
40
30
20
10 Spruce
a Cococnut
0
0 5 10 15 20 25
Percentage of CO2
100
70
Conversion (%)
60
50
40
30
20
10
Spruce
b Cococnut
0
0 5 10 15 20 25
Percentage of CO2
Biomass Conv. Bioref. (2016) 6:49–59 55
over mesopores and macropores. According to some previous were observed in the instrument operating range (~50 nm). In
studies [24, 25], mesopores and macropores promote faster comparison, coconut shell char had individual pockets open-
gasification. For biomass, pores are found in the range larger ing up from the surface to release the volatiles. Significantly
than 20 nm [26]. less number of smaller macropores connecting the inner and
To assess this, some of the char particles were gently outer surface was observed which made it difficult for gas
cracked with an agate mortar. The cracked particles were penetration. This, basically, diminished the active surface area
placed on the sample stab under scanning electron microscope for reaction. This was further confirmed by the delayed tran-
(SEM), and thereby, imaging was carried out. The SEM im- sition of coconut shell char gasification process into the intra-
ages in Figs. S1 and S2 (attached as supplementary material) particle diffusion regime (regime II) [19] with respect to
showed that spruce char had the desired morphology of nu- spruce char. The delayed transition to regime II suggests that
merous macropores (in the range of 100–250 nm) on the outer the surface reaction for coconut shell char was slower than the
and inner surface. This indicated the easier penetration of gas mass transfer at a higher temperature with respect to spruce.
into the inner surface of the particle. However, no mesopores The transition temperature to regime II was ~804 °C for
2 0.08
0.07
CO gas yield (L/g char)
0.05
1 0.04
0.03
0.5 0.02
SC 200
SC 550 0.01
CSC 200
CSC 550
0 0
0 5 10 15 20 25
Percentage of CO (%)
2
2.5 0.1
b 0.09
2 0.08
0.07
CO gas yield (L/g char)
1.5 0.06
0.05
1 0.04
0.03
0.5 0.02
SC 200
SC 550 0.01
CSC 200
CSC 550
0 0
0 5 10 15 20 25
Percentage of CO (%)
2
56 Biomass Conv. Bioref. (2016) 6:49–59
spruce char, whereas it was ~904 °C for coconut shell char sawdust at 1000 °C under 20 % CO2. The trend of increase in
[19]. As the activation energy for coconut shell and spruce CO production due to the increase in CO2 concentration was
char was found to be similar, the explanation based on the not linear as Fig. 4 (temperature dependence) shows.
surface area and slow surface reaction was logical in this case. This effect is dependent on the reaction order with re-
Another reason of low conversion of coconut shell char might spect to the partial pressure of CO2. Literature study
be the low residence time for the same reactor length because [19] shows that the order is less than one. So, the max-
of its higher density than wood. imum effect of CO2 concentration on CO production
As for the individual gas yield, CO produced from can be observed at lower concentration of CO2, while
Boudouard reaction was the dominant portion of the total this would not be significant at higher concentrations.
gas production, as this study considers CO2 gasification. Moreover, both particle size and temperature effects are
Figure 4 shows the individual gas release for the gasification observed in Fig. 6a. The production of CO did not
process. However, there was some H2 produced during gasi- increase noticeably for larger particle size at 900 °C,
fication. This H2 was produced due to the moisture (0.03– whereas both particle sizes followed a similar trend of
0.04 g H2O/g char) trapped in the pores of the char particles increase at 1000 °C (Fig. 6b). On the other hand, the
and some residual functional groups in the char [22]. It was yield of H2 dropped when CO2 concentration was in-
assumed that slightly higher H2 production for larger particles creased. However, the yield of H2 fluctuated, as the
was observed for their greater possibility of retaining the func- quantity of trapped moisture in the pores might vary
tional groups. However, H2 production did not follow any with particles.
general trend.
The lower conversion and gas release of the coconut shell
can be attributed to that fact that coconut shell char gasifica-
tion reactivity under CO2 was significantly lower than the
spruce char from entrained flow pyrolysis [19]. This implies
that the residence time (~7 s for CSC200 and ~2.5 s for
CSC550) was not enough for coconut shell char to achieve
significant conversion under the stated conditions. Moreover,
Fig. 1b shows that the particle size did not shrink as the spruce
char which affects the particle motion to some extent. How-
ever, this does not entirely invalidate the gasification possibil-
ity of the coconut shell char as full conversion can be still
possible at a higher temperature and/or using another gasifi-
cation agent. Steam could be a potential option in place of
CO2; however, due to instrument limitation, steam gasifica-
tion was not possible with the described setup for this study.
3.4 Effect of particle size and reactor length some cases 90 %) [21] conversion was achieved during py-
rolysis, the conversion during only char gasification was
Decrease in particle size for spruce char showed significant overlooked as it fell in the error consideration. Therefore, the
increase in the conversion and gas yield. Conversions were importance of the study was in the evaluation of the char
almost doubled at 1000 °C for the smaller particle size com- gasification characteristics under a specific gasifying agent
pared to the larger one at different concentrations of CO2. It is to provide more data for design purpose.
explained in Fig. 7 how conversion changed with particle size. In another study, Zhao et al. [4] found that the gas produc-
As observed from the figure, coconut shell was insensitive to tion and conversion were saturated after a certain reactor
the particle size variation due to its low reactivity. The con- length. This is interesting to note that this conclusion was based
version is directly proportional to the CO production for the on the gasification of raw biomass and the produced gas was
current study. Therefore, it should be noted that if char reac- the combination of pyrolysis and gasification process. With a
tivity is really low [19], there is no benefit in reducing particle higher residence time, it is expected that gasification reaction
size in the range below 1 mm. As the spruce char was collect- will continue as the reaction rate depends on the temperature.
ed after 90 % conversion, 50 % conversion during char gasi- Even at 1000 °C, gasification rate [28] would not be fast
fication would contribute about 5 % to the total conversion of enough to have a complete conversion of char in an entrained
biomass. In this context, char gasification revealed that mini- flow reactor of with even 9 s of residence time. Residence time
mal conversion took place during gasification. Therefore, im- can be increased by increasing reactor length, decreasing gas
portant design considerations should be made for entrained velocity, and particle size. However, lowering the gas velocity
flow gasification of biomass. For highly reactive chars, it would would result in not entraining the particles in the gas. In that
be feasible to grind the particle size down, whereas for less case, the particles would experience a free fall resulting in an
reactive chars, increasing temperature would be the right op- insignificant effect of gas velocity on residence time.
tion. However, particle size reduction would always increase To observe the effect of residence time on char gasification
the energy penalty [27]. From a scientific point of view, it is process, chars of larger particle size (500–600 μm) from both
rather interesting to observe the reaction time by obtaining the samples were fed twice through the entrained flow reactor
fractionally converted chars. With a complete conversion, it (combined reactor length—3.77 m) with 20 % CO2 gas flow
would be difficult to determine the accurate conversion time. at 1000 °C. The result is described in Fig. 8 assuming a con-
In an earlier study [12], it was also reported that there is tinuous reactor. It shows that increasing residence time had
significant variation in gas yield and conversion when particle positive effect on spruce char conversion, and the increase in
size was kept under 1 mm for biomass gasification. However, conversion was almost linear. Being kinetically limited by
those studies were performed on raw biomass and dominated temperature, coconut shell char also showed linear increase
by the conversion caused by pyrolysis. As more than 80 % (in in conversion; nevertheless, the increase was not significant.
70
Conversion (%)
60
50
40
30
20
10
0
0 1 2 3 4 5 6 7 8 9 10
Residence time (s)
58 Biomass Conv. Bioref. (2016) 6:49–59
Figure 8 shows that for the same residence time, the conver- 3. Zhang Y, Kajitani S, Ashizawa M, Oki Y (2010) Tar destruction
and coke formation during rapid pyrolysis and gasification of bio-
sion of coconut shell reached half the conversion of the wood.
mass in a drop-tube furnace. Fuel 89:302–309. doi:10.1016/j.fuel.
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vealed that the coconut shell char would not reach the same 4. Zhao Y, Sun S, Zhou H, Sun R, Tian H, Luan J, Qian J (2010)
conversion as the spruce char even if it were subjected to the Experimental study on sawdust air gasification in an entrained-
same residence time (~9 s). flow reactor. Fuel Process Technol 91:910–914. doi:10.1016/j.
fuproc.2010.01.012
The tar analysis showed that there were a few small 5. Zhao Y, Sun S, Tian H, Qian J, Su F, Ling F (2009) Characteristics
polyaromatic hydrocarbon (PAH) peaks visible in the GC- of rice husk gasification in an entrained flow reactor. Bioresour
MS spectra. Those were identified as naphthalene, biphenyl Technol 100:6040–6044. doi:10.1016/j.biortech.2009.06.030
and isomers of 1-phenyl naphthalene respectively with in- 6. Hernández JJ, Aranda G, Barba J, Mendoza JM (2012) Effect of
steam content in the air–steam flow on biomass entrained flow
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condensed on the char particle during pyrolysis and the re- fuproc.2012.01.030
maining functional groups. However, the intensity of the 7. Hernández JJ, Aranda-Almansa G, Serrano C (2010) Co-
peaks was very low. With increasing temperature (e.g., gasification of biomass wastes and coal–coke blends in an
entrained flow gasifier: an experimental study. Energy Fuel 24:
1000 °C), no visible peak was observed irrespective of particle
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Characterization of residual particulates from biomass entrained
4 Conclusion
flow gasification. Energy Fuel 27:262–270
11. Qin K, Lin W, Jensen PA, Jensen AD (2012) High-temperature
This study addressed the char gasification behavior of biomass entrained flow gasification of biomass. Fuel 93:589–600. doi:10.
using CO2 as gasifying agent. This information would be use- 1016/j.fuel.2011.10.063
ful for reactor design concerning the temperature, particle size, 12. Hernández JJ, Aranda-Almansa G, Bula A (2010) Gasification of
biomass wastes in an entrained flow gasifier: effect of the particle
and gas concentration variation. The effect of these parameters size and the residence time. Fuel Process Technol 91:681–692. doi:
showed positive impact on the gasification efficiency of the 10.1016/j.fuproc.2010.01.018
reactive spruce char. In contrast, coconut shell char showed 13. Kajitani S, Suzuki N, Ashizawa M, Hara S (2006) CO2 gasification
indifference to the operating parameter variation due to its low rate analysis of coal char in entrained flow coal gasifier. Fuel 85:
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with inaccessibility to the inner surface. These findings are ysis of coal char with a pressurized drop tube furnace. Fuel
important from the gasification point of view, as most of the 81:539–546
literature studies considered raw biomass gasification which 15. Tanner J, Kabir KB, Müller M, Bhattacharya S (2015) Low tem-
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brown coal. Fuel 154:107–113. doi:10.1016/j.fuel.2015.03.069
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Acknowledgments The research work was carried out at the Depart- 17. Mahajan OP (1991) CO2 surface area of coals: the 25-year paradox.
ment of Chemical Engineering, Monash University. The authors like to Carbon N Y 29:735–742
acknowledge the financial and technical support for this work from Aus- 18. Chen L, Bhattacharya S (2013) Sulfur emission from Victorian
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Monash Center for Electron Microscopy (MCEM) respectively. conditions. Environ Sci Technol 47:1729–1734
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