Applied Energy 99 (2012) 386–392

Contents lists available at SciVerse ScienceDirect

Applied Energy
journal homepage: www.elsevier.com/locate/apenergy

Biomass temperature profile development and its implications under

the microwave-assisted pyrolysis condition
Xiaoquan Wang a, William Morrison b, Zhenyi Du a, Yiqin Wan a,c, Xiangyang Lin a,d, Paul Chen a,
Roger Ruan a,c,⇑
a
Center for Biorefining and Department of Bioproducts and Biosystems Engineering, University of Minnesota, 1390 Eckles Avenue, St. Paul, MN 55108, USA
b
Department of Chemical and Biological Engineering, University of Wisconsin – Madison, 1415 Engineering Drive, Madison, WI 53706, USA
c
MOE Biomass Engineering Center, Nanchang University, No. 235 East Nangjing Road, Nanchang, Jiangxi 330047, PR China
d
College of Bioscience and Biotechnology, Fuzhou University, No. 2, Xueyuan Road, Fuzhou University District, Fuzhou, Fujian 350108, PR China

h i g h l i g h t s

" Microwave-assisted pyrolysis of corn stover was studied in a bench-top system.

" Exothermic reactions were observed during microwave-assisted pyrolysis.
" Exothermic reactions can sustain the pyrolysis reactions without external heat.
" Liquids were collected at different times to extract desirable products.

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

Article history: Microwave-Assisted Pyrolysis (MAP) is a highly scalable process that has the potential to realize the Dis-
Received 2 January 2012 tributed Biomass Energy Production System (DBEPS) concept. This study was to illustrate the heating
Received in revised form 25 May 2012 properties of MAP when applied to biomass, and to demonstrate the feasibility of manipulating the heat-
Accepted 25 May 2012
ing operation to fully utilize exothermic reactions as a means to save energy. Alternate microwave heat-
Available online 28 June 2012
ing of corn stover revealed exothermic reactions occurring in temperature ranges of 188.4–224.0 °C and
367.0–387.0 °C. These exothermic reactions can potentially sustain the pyrolysis reactions in the absence
Keywords:
of external heat sources, indicating that alternative dielectric heating is a practical energy-saving opera-
Microwave-assisted pyrolysis
Temperature profile
tion mode for MAP. Analysis of the liquid products obtained from different heating intervals suggests that
Exothermic it is possible to selectively extract the primary pyrolysis products by collecting the condensables at spe-
Differential yield cific heating times. The solid chars produced during MAP have desirable microwave absorbent properties
Bio-oil and could be recycled in the MAP process.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction chemicals, a variety of biomass conversion routes are possible. In

The use of biomass as a renewable source of energy has been
stimulated strongly by governments and international donor agen-
cies in the past decades. The major motivations include the desired
reduction of green house gas (GHG) emissions, the threat of deple-
tion of traditional fossil fuels, the national policies to secure the en-
ergy supply by diversification of resources, and the creation of job
opportunities in the new economic society. To replace fossil fuels
in the production of heat, electricity, transportation fuels and
⇑ Corresponding author. Addresses: Center for Biorefining and Department of
Bioproducts and Biosystems Engineering, University of Minnesota, 1390 Eckles
Avenue, St. Paul, MN 55108, USA; MOE Biomass Engineering Center, Nanchang
University, No. 235 East Nangjing Road, Nanchang, Jiangxi 330047, PR China.
Tel.: +1 612 625 1710.
E-mail address: ruanx001@umn.edu (R. Ruan).
recent years, there has been increased interest in the utilization
of lignocellulosic agricultural crops and forest residues as feed-
stocks for biofuels and bioproducts because of their abundant
availability and non-food nature [1,2].
The US federal government has invested heavily in the develop-
ment of technologies for converting cellulosic biomass into ethanol.
However, cellulosic bioethanol faces difficult economic barriers. The
process is highly dependent on costly enzymes and there are addi-
tional economic problems associated with feedstock. Although cel-
lulosic residues in the field are rather inexpensive, collection and
transport of these residues to the processing plants is a large contrib-
utor to the overall cost. Based on a study funded by the DOE, delivery
costs for corn stover range from $43.1 per dry ton for a 500 dry ton/
day facility (22 miles average collection diameter) to $51.6 per dry
ton for a 4000 dry ton/day facility (62 miles average collection diam-
eter). The difference in delivered costs between facility sizes reflects

0306-2619/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.apenergy.2012.05.031
 X. Wang et al. / Applied Energy 99 (2012) 386–392
transport costs, which account for 33% of total delivered costs for a
500 dry ton/day facility and 40% for a 4000 dry ton/day facility [3].
Research has found that the financial advantage provided by large
processing capacity may be offset by high delivered costs of feed-
stock, suggesting that biomass processing development should in-
clude smaller-scale facilities to be economically viable.
Ruan and his colleagues proposed the Distributed Biomass En-
ergy Production System (DBEPS) concept based on the emerging
Microwave-Assisted Pyrolysis (MAP) technology [4]. DBEPS relies
on easy operation and scalable technologies that can be imple-
mented on medium-sized farms where crop residues are converted
to bio-oils with minimal transportation. The bio-oils produced can
be simply used as home heating oil or transported to a central bior-
efinery where upgrading and further refining of advanced products
can be carried out. A promising DBEPS can be judged on the follow-
ing criteria: (1) affordable financial investment, (2) low transport
costs, (3) foolproof technology (easy operation and maintenance),
and (4) economic, environmental and social benefits for the rural
community. They estimated that a 40–50 million gallon cellulosic
ethanol plant costs about $300 million to build while the cost for
building an on-farm DBEPS facility would be lower than
$200,000 [4]. Feedstock may be collected from one farm or neigh-
boring farms with minimal transport costs. Operating a DBEPS
facility should not require special experience or expertise. The
products can be used locally or sold in the markets to earn money.
The MAP process embraces the principles of DBEPS. There are
three key advantages of the MAP process. Due to the nature of fast,
volumetric and selective heating by microwave energy, thermo-
chemical reactions can take place rapidly in large-sized biomass
materials such as woody biomass or cornstalks. Therefore, very fine
feedstock grinding required by conventional pyrolysis is not neces-
sary for MAP, resulting in substantial energy savings [5–8]. In con-
trast to popular fluidized bed pyrolysis [9,10], there is no rigorous
agitation and fluidization during the MAP process. Therefore, the
presence of particles in the vapor stream is minimal and the col-
lected bio-oils and gas are very clean [11]. Furthermore, micro-
wave is a mature technology, easy to control and relatively
inexpensive and highly scalable. It is an ideal on-farm processing
unit without worries of long start-up and shut-down time or
immobility [7,12].
Although some progress in the MAP technology development
has been made mainly in the United States, Europe and Asia, the
efforts to understand the process mechanism, control strategies,
and energy-saving abilities are still needed for market penetration.
The feedstock temperature measurement and its interpretation
during the microwave heating are of the utmost interest [13,14].
One of the most important parameters to be measured in the
thermo-chemical conversion of biomass units is the temperature
[5,6,13–15]. While only knowing the furnace temperature is suffi-
cient for control of the conventional process, in dielectric heating
the product temperature is usually much higher than the furnace
temperature [6,12,16–19]. Therefore, it is necessary to measure
the product temperature for control of the dielectric heating units.
Either contact or non-contact measurement techniques may be
used to measure the feedstock or product temperature. The most
common contact temperature measurement method is the ther-
mocouple. A contact temperature measurement method that was
specially developed for dielectric heating and similar applications
is the so-called optical fiber thermometer (OFT). This technology
is based on a special sensor material that emits or reflects light
depending on its temperature. The sensor material is placed on
the tip of a glass fiber that transmits the emitted or reflected light
to a control unit which calculates the temperature of the sensor.
Due to the optical measuring principle, the measurement is not af-
fected by the electromagnetic field of dielectric heating. The main
problem with the OFT is the high cost, making it very unlikely to be
387
used in a commercial MAP system. A common non-contact tem-
perature measurement method is the pyrometer [20]. These units
detect the infrared light that is emitted by any material and calcu-
late the surface temperature based on the adjusted emission factor.
Unlike the contact measurement technique, pyrometers can only
measure the surface temperature.
To date, the thermodynamics of pyrolysis of biomass, coal and
municipal solid wastes is not well understood. This may be due
to composition heterogeneity; the large number of components in-
volved in the intermediates and end products; the dependency of
the process over numerous parameters including the temperature,
space and time dependent physical, thermodynamic and transport
properties, the particle shape, size, shrinkage factors and moisture
content [21]. Other literatures have concluded the thermal degra-
dation of cellulose is endothermic, while the char formation is exo-
thermic [22]. The heat of pyrolysis is a key parameter for the
reactor design and control; unfortunately, it has been an arbitrary
and experience dependent value.
This study was focused on the direct temperature measurement
of the biomass particles during MAP of corn stover pellets. The
influence of the innovative operation mode (alternate microwave
heating) on the pyrolysis performances was also investigated.
2. Materials and methods
2.1. Microwave oven and pyrolysis set-up
A series of experimental runs were performed in a modified Pan-
asonic microwave oven (model NNSD787S, USA), the batch wise
bench-scale operational set-up is shown in Fig. 1. The designated
amount of biomass sample, depending on bulk density, was placed
into a 500 ml round quartz flask. For the safety and stabilization of
the quartz reactor temperature, a brick of asbestos was placed
underneath the flask to insulate it from the metal oven bottom.
The time for microwave treatment was in the range of 10–30 min.
A constant power input of 1250 W at the microwave frequency
2450 MHz was used for each run. To avoid the potential condensa-
tion of produced vapor along the exit pipeline of the microwave
reactor, a heated and insulated line was connected between the exit
of the reactor and the first stage of condensation train.
The volatiles were condensed with a five-stage condensation
train. The temperature of the cooling water was kept in the range
of 0–5 °C and the condensed liquids (i.e. bio-oil) from the flasks
were collected. Most vapors could be condensed in the first two
collection flasks with very small amount lost as aerosols. The
bio-oils obtained at different time were transferred to different
beakers for further analysis. The solid char residue was cooled to
room temperature before it was weighed. To avoid tedious disman-
tling of fragile glassware, the condensates adhering to the inside
walls of the condensation train and collection flasks were collected
using in situ microwave heated ethanol. The residual oil was fur-
ther concentrated at 40 °C using a vacuum rotovap (Buchi R-141,
Flawil, Switzerland) to a near constant weight. This weight plus
the previously collected bio-oil weight was recorded as the total
produced bio-oil. The gas product was sampled with a gas-bag or
flared under the lab hood. The weight of the gas product was cal-
culated by difference.
2.2. Materials
Air-dried corn stover pellets were provided by Lone Tree Man-
ufacturing (Bagley, MN). The pyrolysis charcoal was prepared from
MAP as described in Section 2.1. The related physical and chemical
properties of corn stover pellets and pyrolysis charcoal are summa-
rized in Table 1.
388 X. Wang et al. / Applied Energy 99 (2012) 386–392

Fig. 1. Schematic diagram of the MAP set-up (1) microwave control panel; (2) insulation plate; (3) quartz reactor with thermocouple probe; (4) grounded wire; (5)
thermometer; (6) condensation train; (7) cooling system; (8) gas sampling/flare; (9) lab ventilation hood.

Table 1 2.4. Bio-oil analysis

Properties of corn stover pellets and pyrolysis char.

Properties Corn stover pellets Pyrolysis charcoal Chemical compositions of the liquid products were analyzed
Diameter (mm) 6 3–5 using an Agilent 7890–5975 °C gas chromatography/mass
Length (mm) 10–20 9–15 spectrometer (GC–MS, Santa Clara, CA) with a DB-5-MS capillary
Bulk density (kg/m3) 340 100 column. The GC was programmed at 45 °C for 0.5 min and then in-
Moisture content (wt.%) 7.66 n.a.
creased at 15 °C/min to 290 °C where it was held constant for
High heating value (MJ/kg) 18.30 23.01
5 min. The injector temperature was 250 °C, and the injection size
Ultimate analysis, wt.%
was 1 ll. The flow rate of the carrier gas (helium) was 1.2 ml/min.
Carbon 40.40 76.53
Hydrogen 5.30 1.19 The ion source temperature was 230 °C for the mass selective
Nitrogen 1.10 0.21 detector. The compounds were identified by comparison with the
Sulfur 0.10 n.d. NIST Mass Spectral Database.
Chemical composition, wt.%
Cellulose 37 n.a.
Hemicelluloses 27 n.a.
3. Results and discussion
Lignin 18 n.a.
Extractives 18 n.a. 3.1. Microwave power calibration
Note: n.d. not determined, n.a. not available.
To ensure that the proposed method of direct temperature mea-
2.3. Temperature measurement device surement worked under the microwave heating condition, a series
of calibration runs were performed. 1000 g of distilled water was
It is well known that multiple temperature sensors could pro- heated by the corresponding power of 1250, 1000, 750 and
vide more accurate results. However, due to the small amount 500 W. Four calibration curves are given in Fig. 2, one for each
(100 g) of biomass and microwave leaking concerns, only one Ome- power level, 100%, 80%, 60% and 40% respectively. There was a lin-
ga (Stamford, Connecticut) model KHIN-IM60 type K thermocouple, ear relationship between the measured water temperature and
300 mm long with sheath diameter of 6.0 mm, was used for the microwave heating time. Furthermore, in each case the water
measurement of the particle sample temperature during the dielec- starts to boil between 100 °C and 102 °C. The microwave heating
tric heating. The thermocouple has a response time of 0.75–1 s and efficiency (converting electricity to heat) can be calculated based
an error within ±1.1 °C. Due to the non-uniform heating nature of a on the thermal-work equivalent formula:
microwave’s electromagnetic field, the thermocouple tip was al- Q Q kg water 4184
ways positioned in the center of the spherical quartz flask. The ther- W¼ ¼ ¼ ð1Þ
t t slope of the calibration line
mocouple was grounded with wire to avoid generating sparks in
the electromagnetic field. The temperature data were collected at where W is the power level, in Watts, Q is the heat of water, in J;
intervals of 10, 60 or 120 s by the SPER Scientific model 800,023 and t is the heating time, in s.
four-channel thermometer (Taiwan, ROC). The measurements were The calibration results are presented in Table 2, which shows
all done in duplicates and data reported are the average values that the microwave energy conversion efficiency decreases with
(average standard deviation for the mean was less than 5%. decreasing power level. The calibration results suggest that the
 X. Wang et al. / Applied Energy 99 (2012) 386–392 389

Fig. 2. Microwave power calibration using 1000 g distilled water.

densibles. The rate of emission of pyrolysis vapors increased at

Table 2 first, reached a peak, and then declined. The temperature of the
Microwave power level and electricity to heat conversion efficiency. pellets increased rather steadily for 360 s. At 240 s, 419.0 °C, the
Power Absolute Slope of Absorbed Microwave pellets began to glow. A similar phenomenon was observed in
level (%) power (W) calibration power (W) conversion Menéndez’s work [17].
curve efficiency (%) The observed time–temperature relationship curve reveals cer-
100 1250 4.16 1005.77 80.46 tain information. The slope of the corn stover curve and the fact
80 1000 5.74 728.92 72.89 that it is continually changing, provides information about micro-
60 750 7.82 535.04 71.34
wave absorption properties. The initial small slope, correlating to
40 500 17.30 241.85 48.37
a slow rate of temperature increase, is because that the raw corn
stover is a poor microwave absorber. This period is short because
a series of rapid reactions take place during pyrolysis, which
change the feed’s physico-chemical properties. After the primary
microwave should be operated at the full load of the unit as de- volatiles are emitted, charcoal is formed. At that time, the slope be-
signed by the manufacturer. If operated otherwise, more energy comes increasingly steeper because char and other similar carbo-
will be lost during the electricity to heat transformation with each naceous materials are excellent microwave absorbers. As the
step down in power level. control, charcoal can reach as high as 5 °C/s (300 °C/min) while
biomass feedstock, such as corn stover, averages a heating rate be-
3.2. Pyrolysis time–temperature profiles tween 2 and 3 °C/s (120–180 °C/min). This rate depends on the
power level, the moisture content and the microwave absorbance.
Pyrolysis time–temperature profiles are useful for any thermal
conversion process of biomass because they show the temperature
history and help to understand the reaction mechanism. There are 3.3. Alternate microwave heating
few publications regarding the direct measurement method of the
particle temperatures under microwave heating conditions, but In addition to the nature of the material (dielectric properties)
without a detailed description. Here, in Fig. 3, the development being treated, the temperature attained in microwave irradiation
profiles of corn stover temperature versus microwave heating time depends on the microwave power applied to the sample. The
are illustrated. Pyrolysis charcoal derived from corn stover was se- majority of the absorbed microwave power is converted to heat
lected as the control sample. within the material as
In the course of microwave heating, several significant observa-
2
tions were made. First, at about 60 s, 116.6 °C steam started to emit DT 2pf  e0  e00eff  jEj
¼ ð2Þ
from the heated corn stover particles. The steam was immediately Dt q  Cp
condensed in the entrance of the condensation train. At 90 s,
152.2 °C, the particles began to emit white pyrolysis smoke, i.e. where E is the magnitude of the internal electric field, e00eff is the rel-
pyrolysis vapors, including condensables (bio-oil) and non-con- ative effective dielectric factor, e0 is the permittivity of free space, f
390 X. Wang et al. / Applied Energy 99 (2012) 386–392

Fig. 3. Feedstock temperature profiles during the microwave heating.

Fig. 4. Feedstock temperature versus alternate microwave heating (on–off–on mode).

is the microwave frequency, T is the temperature, t is the time, q is
the density, and Cp is the heat capacity [23].
To understand the thermal effects on the biomass MAP process,
a novel experimental design was proposed. An alternate micro-
wave on–off–on operation mode was used instead of the more
common continuous microwave heating mode. Although the
alternate mode has a rectangular wave rather than a sine or cosine
wave, it is very similar to the common alternate current concept.
The time interval between the switch on and off is arbitrary, but
for the convenience of data logging and manual operation, 1 or
2 min intervals were used in the experiments. Alternate heating
is a potential energy-saving heating mode for the MAP design
and operations. The measurements of temperature vs. alternate
microwave heating time are presented in Fig. 4.
According to Eq. (2), if the microwave was switched off, i.e.
internal electric field E = 0, the particle temperature should be
constant. However, as seen in Fig. 4, this was only observed
during time interval 120–240 s. The temperature did increase
significantly during the microwave-off mode intervals of intervals
360–480 s and 600–720 s. These intervals see a temperature in-
crease of 188.4–224.0 °C and 367.0–387.0 °C respectively. Particle
size is an important parameter because microwave heat up the
biomass materials from inside out. For example, 60 – 300 mm
diameter wood blocks had higher temperature in the center than
the outer region during microwave heating [6]. However, pellets
of 6 mm diameter, which is much smaller than the microwave
penetration depth, were used in this study and the temperature
distribution inside each pellet should be relatively uniform.
 X. Wang et al. / Applied Energy 99 (2012) 386–392 391

Table 3 temperature drop intervals can be explained by the black body

Temperature changes vs. time intervals during alternate microwave heating. radiation mechanism. The time interval versus temperature
Time interval (on Temperature Time interval (off Temperature
change data are reported in Table 3.
mode) (S) changes (°C) mode) (Sec) changes (°C)
3.4. Differential pyrolysis bio-oil yields during the alternate microwave
0–120 26.8– 79.6 120–240 106.4– 0.8
heating
106.4 105.6
240–360 105.6– 82.9 360–480 188.5– 35.5
188.5 224.0 The concept of alternate microwave heating lead to the differ-
480–600 224.0– 143.0 600–720 367.0– 20.0 ential pyrolysis bio-oil yield or the bio-oils produced at different
367.0 387.0 time intervals. For convenience and normalization purposes, the
720–840 387.0– 156.0 840–960 543.0– 17.0
defined equation of differential yield was presented as:
543.0 526.0
960–1080 526.0– 413.0 1080–1200 939.0– 305.0 y mi
939.0 634 Y ¼ Pi ¼ P ð3Þ
1200–1320 634.0– 231.0 1320–1440 865.0– 210.0
yi mi
865.0 655.0
1440–1560 806.0– 151.0 where Y is the normalized differential yield (%), yi is conventional
655.0 product yield, m is the produced bio-oil mass, and i is the time
interval.
The differential pyrolysis bio-oil yields during the alternate
Therefore, the temperature increase during microwave-off period microwave heating versus pyrolysis time are shown in Fig. 5. The
can be possibly explained by the exothermic nature of the bio- cumulative yield of bio-oil during the intervals from the 120–
mass pyrolysis reaction. In fact, such self-sustaining reaction re- 600 s dominated the entire process. During the off-mode interval
gions were also observed in coal, peat, and wood pyrolysis, between 120 s and 180 s, the bio-oil yield still increased. In every
though the frequent tools were DSC, DTG or other microgram other off-mode operation interval, the differential yields decreased.
sampling instruments [24–26]. Heat generation during biomass A possible explanation to the exceptional case is that the exother-
pyrolysis is largely due to secondary decomposition of the vola- mic reaction increased the particle temperature and hence the
tiles, possibly catalyzed by the remaining solid [27]. Exothermic reaction rate.
reactions can take place at any temperatures; however, at low
temperatures, the heat generated is lost to the surroundings. 3.5. GC–MS analysis of bio-oils produced at different time intervals
The rate of exothermic reactions increases with external heating
temperature accompanied by increasing heat generation rate. The liquids produced at different time intervals were analyzed
Above a certain temperature, the rate of heat generation matches with GC–MS, and the chromatograms are provided as Supplemen-
or exceeds the rate of heat loss, resulting in a net increase in heat tary materials. Small amount and simple molecular components
which helps sustain the pyrolysis process [28]. Therefore it is pos- dominated the product distribution near the beginning of the pro-
sible to design on-and-off heating schemes to use the exothermic cess. In fact, there were no condensates obtained in the first min-
reactions for substantial energy savings, which will be quantified ute. While in the second minute, the main components collected
in future study. in the condensers were water and formic acid. Between the third
As for 120–240 s interval, the minute temperature change of and sixth minute, uniform bio-oil with complicated compositions
106.4–105.6 °C is due to water vaporization (drying region). The was obtained.
temperature drops remarkably during the 1080–1200 s and After the sixth minute, due to the secondary cracking occur-
1320–1440 s microwave-off intervals. It is important to note that rence, heavier tar and more water were produced. The heavy com-
at these intervals the temperature was greater than 600 °C. These ponents with high boiling point cannot be detected with the

Fig. 5. Differential pyrolysis bio-oil yields during the alternate microwave heating.
392 X. Wang et al. / Applied Energy 99 (2012) 386–392
conventional GC–MS analyzer, and thus the plain and sparse peaks
appear in the graph. The variation of pyrolysis products at different
intervals reveals the potential of this process to selectively collect
bio-oil products with desired oil quality and quantities during MAP
of biomass.
4. Conclusions
In this study, we used shielded thermocouples directly to
measure the temperatures of solid biomass during MAP. With an
on-and-off alternating heating scheme, we observed multiple
exothermic reaction temperature regions. This suggests that it is
possible to design on-and-off heating schemes to fully utilize the
exothermic reactions for substantial energy saving. The chemical
profiles of condensables collected at different times of the pyroly-
sis suggests the possibility of selectively extracting desirable prod-
ucts at given times. It was found that the solid biochar was a good
microwave absorbent which can improve heating efficiency and
possibly promote in situ catalytic cracking of primary pyrolytic
products.
Acknowledgements
The authors would like to express their gratitude to DOE, DOT,
USDA and Initiative for Renewable Energy and Environment (IREE)
at the University of Minnesota for their financial supports to the
research.
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.apenergy.2012.
05.031.
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