International Journal of Sustainable Energy

ISSN: 1478-6451 (Print) 1478-646X (Online) Journal homepage: http://www.tandfonline.com/loi/gsol20

Experimental investigation of the pyrolysis of

biomass to produce green fuels

Leena Kapoor

To cite this article: Leena Kapoor (2019): Experimental investigation of the pyrolysis
of biomass to produce green fuels, International Journal of Sustainable Energy, DOI:
10.1080/14786451.2019.1566235

To link to this article: https://doi.org/10.1080/14786451.2019.1566235

Published online: 16 Jan 2019.

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INTERNATIONAL JOURNAL OF SUSTAINABLE ENERGY
https://doi.org/10.1080/14786451.2019.1566235

Experimental investigation of the pyrolysis of biomass to produce

green fuels
Leena Kapoor
Department of Chemical Engineering, University of Petroleum & Energy Studies, Dehradun, India

ABSTRACT ARTICLE HISTORY

This work aims to utilise the experimental approach to perform the Received 3 August 2018
analysis of three-biomass feed stocks – bamboo, mustard and camellia Accepted 21 December 2018
and to provide insight into the operation and design of pyrolysis
KEYWORDS
processes. Experiments on biomass fast pyrolysis were performed in a Pyrolysis; bio oil; hydrous
fixed bed (tubular) reactor at a temperature of 500°C and a residence pyrolysis; tubular reactor
time of 2 min under the constant flow of nitrogen. The analysis of
pyrolysis gases and bio oil produced by pyrolysis was done using GC-MS
and GC-TCD. Hydrous pyrolysis of biomasses was performed in a high-
pressure autoclave for the temperature range 250–400°C and at a
pressure of 20 bar with 30 min of residence time. Experiments were
conducted both with and without the use of a catalyst. The pyrolysis
vapour is made to pass through the catalyst bed of ZSM-5 (Si/Al = 35).
The results for all the biomass samples are then compared.

1. Introduction
Due to potential climate changes and high crude prices, bio fuels have attracted considerable atten-
tion of many researchers. The use of biomass provides a clean source of energy that will improve our
environment from pollution (Badea et al. 2008). The energetic and industrial usage of biomass is
becoming more and more technologically and economically attractive. Biomass can be transformed
through both thermal and biological processes into various forms of energy. The thermal process for
biomass conversion uses heat and catalysts to convert biomass into chemicals, fuels and electric
power. Mainly three thermal processes are being used for converting biomass into various useful
forms of biofuels, i.e. pyrolysis, direct combustion and gasification (Kassaye, Pant, and Jain 2017).
In recent times, a high temperature conversion process known as fast pyrolysis has increasingly
being studied to convert biomass into char and bio oil (Orfao, Antunes, and Figueiredo 1999).
Fast pyrolysis is considered one of the emerging technologies which produces more amount of liquid
product, i.e. large yield of bio oil. Though it offers high conversion efficiency, it suffers from the dis-
advantage of large energy necessities, making it energetically and economically limited. However, at
low to moderate temperature conditions processes such as hydrous pyrolysis and anaerobic digestion
transform wet biomass into bio crude and biogas, respectively. Thus in comparison to conventional
pyrolysis, hydrous pyrolysis can operate at moderate temperature conditions. With hydrous pyrol-
ysis the whole biomass can be converted to bio fuel with a relatively high solid residue, high heating
value and gaseous mixture (N2, H2, CH4, CO2, CO) along with aqueous product rich in organics
(Choudhary, Malik, and Pant 2017). The reactor temperature is considered to be one of the main
parameters that affects the yield and composition in hydrous pyrolysis (Choudhary, Malik, and
Pant 2017).

CONTACT Leena Kapoor lkapoor@ddn.upes.ac.in

© 2019 Informa UK Limited, trading as Taylor & Francis Group
2 L. KAPOOR

Bio oil formed from biomass suffers from the disadvantage of instability, incomplete volatility,
low heating value, incompatibility and acidity when compared with petroleum. It has been found
that the bio oil consists of oxygenated organic compounds, which hinder its use as a fuel (Dermibas
and Arin 2010). Elimination of these oxygenated compounds from bio oil is must to make it more
economical to be used as a fuel. Zeolite can be used as a catalyst for removing oxygen from organic
compounds formed in pyrolysis vapour and thus converting them to hydrocarbons (Ranzi et al.
2008).
The zeolite catalyst is frequently being used for biomass catalytic pyrolysis and also for upgrading
bio oil. The selection of zeolite as a catalyst by many researchers (Ates, Pütün, and Pütün 2006) for
biomass pyrolysis is mainly due to its porous structure, less deactivation due to coke and more stable
thermally. Zeolite also gives good settlement between activity and shape selectivity basically to C12
hydrocarbons. It has been found by researchers (Carrero et al. 2011) that with the ZSM-5 zeolite cat-
alyst, the quantity of gaseous products is increased while the concentration of liquid product
decreases. This may be expected as the use of catalyst leads to cracking which decreases the product
molecules’ molecular weight.
When comparing the catalytic pyrolysis and non-catalytic pyrolysis process in the fluidised bed
reactor for pine chips it has been found that the organic fraction in bio oil produced is decreased
comparatively with catalytic pyrolysis (French and Czernik 2010). When compared to other catalyst,
the ZSM zeolite gave the highest yield of the organic fraction (French and Czernik 2010).
Several researches (Ellis et al. 2015) have been done for biomass pyrolysis using different biomass
sources. Many different types of biomass feedstock were screened: forestry residues, agricultural resi-
dues, grasses, bark, nuts and seeds, wood, algae, cellulose and lignin and are tested to different con-
ditions of pyrolysis in different reactors. Rice husk, wheat straw and olive bagasse represent a
significant portion of these researches (Masnadi et al. 2014); however, much of the work is done
on wood because of its comparability and consistency between tests (Bridgwater 1999). As reported
in the literature (Tinwala et al. 2015), oil yields of 65% at 550°C were reported by intermediate pyrol-
ysis of rapeseed in a fixed bed reactor at a nitrogen flow of about 100 cm3/min and with a particle size
ranging from 0.6 to 0.85 mm at a heating rate of 300°C/min. A thermal pyrolysis study for neem seed
as a biomass feedstock has been done in a semi batch reactor at a heating rate of 20°C/min and with a
temperature range of 400–500°C which resulted in a bio oil yield of about 38 weight percentage (Sai-
kia et al. 2015). About 63.48 weight percentage bio oil yield on the dry weight basis was obtained by
intermediate pyrolysis of groundnut shell carried out at a temperature of 475°C in a fluidised bed
reactor (Tinwala et al. 2015). For groundnut shell, biomass basic parameters such as viscosity, low
heating value, density and pH value were identified as 24.56 cSt, 31.07 MJ/kg, 1.2 kg/m3 and 4.20
(Tinwala et al. 2015). Limited work has been done in the field of fast pyrolysis by utilising the
fixed bed reactor using mustard, camellia and bamboo as biomasses (Multiphase Reactor Engineering
for Clean and Low-Carbon Energy Applications 2017).
Limited literature is available on the physiochemical characterisation of different biomasses such
as pinewood, jatropha seeds, bagasse and their co products such as bio oil/ pyro oil, bio char from the
pyrolysis process. Further investigations are required to understand its throughput. The bio oil pro-
duction process via pyrolysis is still not feasible commercially. To compete with fossils fuel technol-
ogy, bio oil needs to overcome many social, economic and technical barriers. Fast char removal
methods have to be established to decrease solid contamination in bio oil (Badea et al. 2008). To
maximise production of pyrolysis products, a good understanding of the pyrolysis process has to
be done. As municipal solid waste, agricultural residue and wood waste can be easily processed to
a much useful and clean form of energy through the biomass pyrolysis process, so more focus in
improving this technology is being done by many researchers (Saikia et al. 2015).
The major objective of the present investigation is to produce an environmentally safe bio fuel
(bio oil) from a few representative renewable sources using a laboratory scale fixed bed tubular
and hydrous pyrolysis reactor. This study focusses on the pyrolysis of few biomass species such as
bamboo, mustard (Khari) and camellia for potential bio fuel production by fast and hydrous
 INTERNATIONAL JOURNAL OF SUSTAINABLE ENERGY 3

pyrolysis. The complete physiochemical characteristics, suitability and availability of the three bio-
mass selected was done via ultimate and proximate analysis. Further study on heating schedule
employed, i.e. high heating rate (HHR) and slow heating rate (SHR) pyrolysis, was done.

2. Materials and methodology

2.1. Feedstock
The biomass material selected for this study is bamboo, mustard (khari) and camellia. All these biomasses
are used in their natural form. Camellia was obtained from Dehradun (Camellia) and others from Delhi.
Before each run, the feed stocks were pretreated to enhance the product formations. All feedstock was first
dried to a moisture content of less than 10−12 wt. % and crushed to a sieve size of about 2 mm to enhance
heat transfer. The experiments were conducted at a temperature range of 500 ± 10°C.

2.2. Biomass characterization

To determine carbon, nitrogen, hydrogen, and sulphur contents in biomass and bio chars sample, a
CHNS analyzer (Perkin Elmer, 2400 series II) was used while the oxygen percentage was calculated
by means of difference as shown in Table 1. The heating value for the three-different biomass
samples used was found by a bomb calorimeter and theoretically determined by the modified
Dulong’s formula.
Proximate analysis of all biomasses was done according to standard ASTM methods as shown in
Table 2. The moisture content one of the main characteristics has to be taken into account as it affects
the final conversion while fixed carbon and volatiles content in biomass represent the burning rate of
biomass. The flow meter (Wet type, Nova Instruments, India) had been used for measuring the total
amount of gas produced by biomass pyrolysis. By making use of an online gas analyzer model no.
ACE 9000X CGA (Ace gas analyzers, India) the composition of the gas and its value were measured
simultaneously. The PH meter with model no. EW-99855-16 (Eutech bench top meter) was used for
measuring the PH value of bio oil at room temperature. Density for bio oil was determined by using a
density bottle at room temperature. A redwood viscometer was used for measuring the kinematic
viscosity of bio oils at 40°C. The calorific value of all three biomasses was determined theoretically
by using the modified Dulong’s equation and experimentally with a bomb calorimeter (model:
Advance isoperibol I.P-3, Advance Instruments Ltd).
The TGA study of the three-biomass samples was carried out in a TGA-Q600 instrument with a
continuous flow of nitrogen at 40 ml/min and at a heating rate of 10°/min. The three samples (bam-
boo, mustard and camellia) weighing about 10–12 mg were heated from room temperature to 900°C.
The results of TGA analysis for the three-biomass samples are shown in Figures 1–3.
The bio oils of the three-biomass samples (bamboo, mustard and camellia) were studied by GC-
MS with a TCD detector (Perkin Elmer Claurus 600 equipment) and a DB-5 ms column with a col-
umn temperature of 70°C. The biomass samples were kept for at least 2 min in the detector and were

Table 1. Carbon, hydrogen, nitrogen and sulphur content of biomass.

C N H S O HHV (MJ/kg)
Samples Ultimate analysis (wt %) C/N ratio C/H ratio Theoretical Experimental
Biomass
Bamboo 44.90 0.72 6.038 0.018 48.342 62.68 7.435 17.235 15.15
Mustard (Khari) 46.31 4.45 7.055 0.036 42.149 10.3985 6.5641 15.94 16.12
Camellia 38.90 0.71 5.875 0.165 54.35 54.57 6.621 18.401 20.24
Bio char
Bamboo 68.04 1.17 1.5 0.14 15.95 58.1 45.36 22.5 24.22
Mustard (Khari) 68.83 1.77 2.53 0.11 13.29 38.88 27.20 24.6 25.84
Camellia 64.22 0.53 1.03 0.31 24.12 121 62.34 19.3 20.01
4 L. KAPOOR

Table 2. Proximate analysis of different feedstock (biomass).

Biomass name Moisture content (%) Ash content (%) Volatile matter (%) Fixed carbon (%)
Bamboo 9.37 2.57 70.31 17.75
Mustard (Khari) 6.86 14.98 70.78 7.38
Camellia 0.49 4.78 80.20 14.53

heated to about 290°C where the rate of increase was found to be 10°C/min. Helium is used as a
carrier gas at 1 ml/min.

2.3. Experimental work

2.3.1. Fast pyrolysis
Pyrolysis experiments were done under an inert atmosphere of nitrogen at a temperature of 500 ±
10°C in duplicates in a tubular (fixed) reactor. The reactor is a vertical tube with the material of con-
struction Inconel 800. The internal diameter of the tube is 25 mm with a tube length of about 3 ft.
The heat for the reaction is provided by an electrical resistance coiled (power 3 kW, single phase,
220 V). The maximum temperature attained by the fixed bed reactor is around 1100°C. The heating
zone is around 1.5 ft long. The PID-based programmable controller with 16 steps (including ramp)
has been used. Three thermocouples are being positioned one with the controller and the other two
with the digital temperature indicator. Two glass condensers follow the reactor, where cold water was
used for quenching vapour to get bio oil. The liquid product after condensation collected in a con-
tainer was bio oil. The by-product (solid) known as char was cooled and then weighed. The differ-
ence between the solid biomass from liquid and bio char gives the gas yield.

2.3.2. Hydrous pyrolysis

Hydrous pyrolysis experiments were done in duplicates in a 1 L capacity stirred reactor (made of SS-
316) at 5.9 MPa pressure and at a temperature of 500 ± 10°C. For controlling the temperature of the

Figure 1. DSC-TGA analysis for bamboo.

 INTERNATIONAL JOURNAL OF SUSTAINABLE ENERGY 5

Figure 2. DSC-TGA analysis for camellia.

Figure 3. DSC-TGA analysis for mustard.

reactor, a coiled tube and a jacketed furnace were used. At the outlet of the reactor, a condenser along
with a chiller is attached to condense the vapour coming from the reactor. A glass pipette is used for
collecting the non-condensable from which samples of gas were taken for analysis. For controlling
6 L. KAPOOR

the pressure, temperature and string speed, a PID controller assembly is connected with the whole
reactor (Choudhary, Malik, and Pant 2017).
The reactor was first charged with a biomass to water (W/B) ratio of about 1:6 and was sealed.
Nitrogen was then made to pass through the reactor so as to create the inert atmosphere in the reac-
tor till the desired pressure of 25 bar is reached. A backpressure regulator controls the pressure of the
vessel. Without including the heat up time for the reactor, a run time of about 20 min was then
recorded till the reactor reaches the final test temperature. For all the run, 120 rpm stirring speed
was maintained. A shell and tube condenser kept at a temperature of 2°C were used to condense
the vapour formed during the run. A separating funnel was used to separate condensable vapours
into gas and liquid phases.

3. Result and discussion

3.1. Product yield
3.1.1. Fast pyrolysis
Bio oil, gas (non-condensable) and char are the main products formed from biomass fast pyrolysis.
The total amount of product formed in terms of calorific values and mass balance is reported in
Tables 3 and 4. It is found that different biomasses have produced dissimilar gas, bio oil and bio
char composition. The yield of liquid generally depends on vapour residence time, temperature, bio-
mass type and ash content that have a wide effect on vapour cracking. Compounds identification was
made by computer matching with a mass spectral library. The product fractions are grouped as
organic acids, heterocyclic compounds, branched amides, cyclic oxygenates and hydrocarbons as
shown in Figures 4 and 5.
From Tables 3 and 4 it can be inferred that the amount of volatiles plus gases produced is more
without using the catalyst as compared to with the use of a catalyst. The production of bio oil is less
with the catalyst because the catalyst has stopped the unwanted reaction in the volatiles and gases
released, thus the quality of bio oil produced will be good.

3.1.2. Hydrous pyrolysis

The gaseous products’ composition was examined by GC (Nucon series-5700) having a cryosphere
column with TCD (thermal conductivity detector). Argon was used as the inert gas. Detector and
injector temperatures were 150°C and 120°C, respectively. WinAcds 6.2 software was used for cal-
culating the peak areas and also for recording the chromatograms. CO2, CO, H2 and CH4 gases were
detected based on their retention time in accordance to calibration mixture of a gas chromatograph.
The GC-MS with an Elite 5-MS column (30 m length, 0.25 mm i.d., and 0.5 m film thickness) using
helium as the carrier gas was used for determining the chemical composition of hydrous pyrolysis
products. The compounds identified are grouped as organic acids, hydrocarbons, branched amides,
heterocyclic compounds and cyclic oxygenates. The amounts of compounds detected in various bio-
masses through hydrous pyrolysis are shown in Figure 6. The overall product yield through hydrous
pyrolysis at a temperature of 500°C is shown in Table 5. Table 5 also depicts the water content,
specific gravity, viscosity, pH and heating value of bio oil formed at 500°C by hydrous pyrolysis
of selected biomass samples. The pH measured for bio oil ranges from 1 to 1.3 and this may be
due to carboxylic acids and phenolic present in bio oil as shown in Table 5.

Table 3. Overall product yield obtained from fast pyrolysis without using catalyst with 2 g sample.
Product yield (wt. %) Calorific value (MJ/kg)
Sample name Bio char Bio oil Gases Biomass Bio char Bio oil Pyrolysis gases
Bamboo 21 ± 0.5 59 ± 0.5 19 ± 0.5 17.235 ± 0.143 24.21 24.45 6.91
Mustard 22 ± 0.5 55 ± 0.5 16 ± 0.5 15.94 ± 0.5 20.09 20.87 8.49
Camellia 30 ± 1 50 ± 1 13 ± 1 18.401 ± 1 23.28 22.64 8.40
 INTERNATIONAL JOURNAL OF SUSTAINABLE ENERGY 7

Table 4. Overall product yield obtained from fast pyrolysis using catalyst with 2 g sample.
Product yield (wt. %) Calorific value (MJ/kg)
Sample name Bio char Bio oil Pyrolysis gases Bio oil Pyrolysis gases Bio char
Bamboo 31.93 51.07 17 29 6.91 24.21
Mustard 26.65 55.01 18.33 25 8.49 20.09
Camellia 38.83 45.87 15.29 27 8.40 23.28

Figure 4. Fast pyrolysis product fractions.

3.2. TGA-DSC analysis for biomass samples

Thermo-gravimetric analysis for different biomass samples was done to know the rate of mass con-
verted at a specified heating rate in respect with temperature and also to find the feasibility of differ-
ent biomasses towards the pyrolytic process. TGA process is essential in analysing any feedstock
before using. TGA analysis was done on a TGA/DSC TA instrument with model number SDT

Figure 5. Fast pyrolysis with catalyst product fractions.

8 L. KAPOOR

Figure 6. Hydro pyrolysis product fractions.

Table 5. Overall product yield and properties of bio oil obtained from hydro pyrolysis.
Product Yield (wt. %) Bio oil
Biomass samples Bio char Bio oil Gases Water content Sp. gravity Viscosity PH Heating value MJ/Kg (HHV)
Bamboo 34.41 49.2 16.39 15–35 wt.% 1.1–1.3 40–100 Cp 2–3.7 16–19
Mustard 49.17 38.12 12.70 10–30 wt.% 1–1.2 30–100 Cp 2–3.5 18–20
Camellia 18.02 61.45 20.48 8–20 wt.% 1.2–1.3 35–100 Cp 2–3 15–20

Q600 at a constant nitrogen flow of 100 ml/min with a constant heating rate 10°C/min. The biomass
sample was heated from room temperature to 900°C in a TGA/DSC instrument. It is found that the
breakdown rate for bamboo is observed to be the maximum in comparison with other biomass feeds
(T = 250°C–500°C), i.e. bamboo break down to gaseous and liquid products more rapidly in com-
parison to other feedstock’s. For camellia, the loss in weight percentage after 225°C is detected
where the active pyrolysis zone started and cellulose and hemicellulose get disintegrated. Mustard
starts to break down at 150 °C with a severe weight percentage loss until 450°C due to decomposition
of hemicellulose bonds. Mustard has a low lignin content. Camellia decomposes slowly after 400°C.
Thus, the selected feedstock’s can be used as a potential source for pyrolysis.

3.3. Pyrolytic gases composition

The gas obtained from biomass pyrolysis consisted mainly CO2, O2, CO, H2, CH4, and with lower
CnHn gaseous streams (where, n < 4) obtained by the fast pyrolysis of various biomass at 500°C. Lar-
ger CO2 signifies the breakdown of hemi cellulosic and cellulosic contents, whereas the presence of
CH4 and CO is due to the release of volatiles by secondary cracking. For gases, the bamboo sample
has shown the highest calorific value.

4. Conclusion
For the current study, three types of biomass were selected and analysed, i.e. bamboo, mustard, and
camellia. In this study, pyrolysis and hydrous pyrolysis experiments for bamboo, mustard and camel-
lia biomass samples were performed. For carrying fast pyrolysis experiments, a tubular (fixed) bed
reactor was used while hydrous pyrolysis experiments were carried out in a high-pressure auto
 INTERNATIONAL JOURNAL OF SUSTAINABLE ENERGY 9

clave under nitrogen atmosphere. Out of the three biomasses selected for fast pyrolysis conditions,
bamboo produced the highest liquid yield 59%, while through hydro pyrolysis the highest liquid
yield 61% was produced with camellia. Bamboo has produced bio oil with a highest heating value
of 29 MJ/kg.

Acknowledgments
The author gratefully acknowledges the support and guidance provided by Prof. S.K Gupta (UPES, Dehradun), Dr K.K
Pant (Professor, Department of Chemical Engineering, IIT Delhi) and Dr Parichay Kumar Das (Professor, UPES
(Dehradun)).

Disclosure statement
No potential conflict of interest was reported by the author.

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