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Insights into Pyrolysis of Banana Pseudo Stem Waste through

Thermogravimetric Analysis: Physicochemical Characterization, Kinetics, and
Reaction Mechanism

Conference Paper · August 2024

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 International Journal of Applied Engineering Research ISSN 0973-4562 Volume 19, Number 3 (2024) pp. 202-207
© Research India Publications.

Insights into Pyrolysis of Banana Pseudo Stem Waste through

Thermogravimetric Analysis: Physicochemical Characterization, Kinetics,
and Reaction Mechanism

Manisha Jagadale*, Rakesh Kumar Ghosh, Deb Prasad Ray and Sanjoy Debnath
ICAR-National Institute of Natural Fibre and Engineering Technology, 12 Regent Park,
Kolkata-700040, W.B. (India)

Abstract generated during banana cultivation, including

In world, for every tone of banana produced, about 4 leaves, pseudo stems, rachis, and peels. It's worth
tons of biomass waste is generated. In present study, noting that for every ton of banana production,
to determine thermal degradation banana pseudo approximately 100 kg of waste fruit and four tons of
stem waste (BPS) thermogravimetric analysis was lignocellulosic waste are generated (Fernandes et al.,
conducted from room temperature to 900°C at three 2013). This waste comprises 74% pseudo stem, 12%
different heating rates 10, 20, and 30 °C/min to leaves, 11% peels, and 4% peduncle (Souza et al.,
determine pyrolysis behavior, kinetic parameters and 2010).
thermodynamic parameters. Model-free method i.e. Unfortunately, a large portion of banana
Flynn-Wall-Ozawa, were used to determine lignocellulosic waste is often left in the field for
activation energy. The average activation energy decomposition without any recovery efforts. Farmers
values for BPS 187.35 kJ mol-1 when OFW were commonly dispose of this waste by dumping it into
used for analysis. Thermodynamic parameters pre- rivers and lakes or burning it. However, improper
exponential factor (A, s-1), changes of enthalpy (ΔH), handling of these wastes can lead to environmental
entropy (ΔS), and Gibbs free energy (ΔG) of BPS issues, as they may emit hazardous greenhouse gases
were also evaluated and discussed in the current that harm the environment (Padam et al., 2014).
context. Thermodynamic parameters revealed Therefore, it is crucial to explore various approaches
endothermic, non-spontaneous, and high degree of to recover energy and produce value-added products
randomness for BPS pyrolysis. from banana wastes.
Keywords: Pyrolysis, Banana pseudo stem waste, Various conversion processes can be used to extract
Kinetic Triplets, Master Plot. energy from banana biomass. Various research
groups have investigated thermal, thermochemical,
1. Introduction and biochemical methods of conversion. The
Globally, Banana (Musa paradisiaca) is a prominent utilization of these waste materials can be harnessed
fruit and fibre crop native to Southeast Asia's to produce bioenergy and bioproducts through the
Malaysian-Indonesian region (Bhushan et al., 2019). implementation of a biorefinery approach. Hence,
According to statistics, India holds the position of to further advance technology and science in this
being the largest grower of bananas globally, area, there is a significant desire to develop a
contributing 29 million tons, which accounts for capable, sensible, and eco-friendly approach to
approximately 25.43% of the total global banana assess banana pseudo stem waste (BPS). Pyrolysis is
production (Singh et al., 2020). Other major banana a promising technique for transforming BPS wastes
producing countries are China, Brazil and into useful fuels and products. The thermal
Philippines. In India, bananas are predominantly characteristics of biomass are influenced by its bio
cultivated in Karnataka. However, other states such components, including cellulose, hemicellulose,
as Andhra Pradesh, Assam, Gujarat, Kerala, lignin, pectin, tannin, other polyphenols, and
Maharashtra, and Tamil Nadu also engage in banana inorganic compounds, as well as the environmental
cultivation. A substantial amount of waste is conditions within the reactors. Therefore, in order to

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© Research India Publications.

construct and operate a commercial biomass thermal 2.3 Determination of pyrolysis kinetic triplets
processing unit, it is necessary to have a thorough It is stated that when biomass is heated in inert
understanding of the kinetics and pyrolytic atmosphere, as per the one-step global model it
behaviour of the biomass in question. The present converted into solid (char), liquid (tar) and gaseous
work provides a detailed explanation of the pyrolysis compound (Liborio et al., 2024). During the
of banana pseudo stem material by pyrolysis of biomass, multiple complicated chemical
thermogravimetric analysis. reactions and transitions between phases happen
together. Therefore, the determination of kinetic and
2. Material and methods thermodynamic parameters associated with the
2.1 Biomass Characterization converting mechanism was complicated and
The raw banana pseudo stem (BPS) was obtained challenging (Nawaz and Kumar, 2023; Singh and
from farmers field of West Bengal (India). The BPS Sarkar, 2023). A general equation which can be used
was washed thoroughly and dried in hot air oven at to describe the pyrolysis of biomass in one step is as
105°C for 24 hr. The complete dried BPS was follows:
grounded to smaller particle size and same was used 𝒌(𝑻)
Solid biomass → Volatile (gases and tar) + char
for all experiment. The proximate and ultimate
(solid residue) (1)
analysis was conducted as per the procedure Where, volatiles refer to gas and tar, for
described in (Jagadale et al., 2023; Jagadale et al., instance, whereas the rate constant of the process is
2024). The H/C and O/C atomic ratios in raw BPS denoted as k and is expressed using the Arrhenius
were established based on prior research. The equation;
investigation of the higher heating value (HHV) was
𝒌(𝑻) = 𝑨𝒆(−𝑬𝒂⁄𝑹𝑻) (2)
conducted using a bomb calorimeter. The chemical
Where, Ea (kJ/mol), T (K), R (8.314 J/K. mol) and A
constituents of the banana pseudo stem were
(1/s) represents the activation energy, absolute
determined by estimating cellulose, hemicellulose
reaction temperature, gas constant and pre-
(as per to TAPPI-17 standards), lignin (as per to
exponential factor, respectively.
TAPPI-222 standards), and fat and wax (as per to
The rate of reaction to transform solid to volatile
TAPPI-204 standards).
state as given below:
𝒅𝛂
2.2 TGA experiments = 𝐤(𝐓) 𝒇(𝛂) (3)
𝒅𝒕
Thermogravimetric is an established method for where α, t, k(T), 𝑓(α) represent the degree of
studying the thermal behavior of biomass. It involves conversion of pyrolysis process, fraction of time, the
determining the rate at which the biomass decreases rate constant and the reaction model, respectively.
weight as a result of temperature or time. This where, Conversion, α, can be calculated using Eq. (4)
𝒎 −𝒎
approach has been described by Jagadale et al., 2024; 𝛂 = 𝒎𝒊 −𝒎𝒂 (4)
Chen and Felix, 2024; Sahu and Gangil, 2023; Durga 𝒊 𝒇

et al., 2022). The researchers used the concepts of where mi, ma, and mf are the initial, instantaneous
reducing weight loss, the temperature, and time to and final mass of the jute stick during pyrolysis.
investigate thermal degradation, kinetics, Combination of the equation (2) and (3) gives the
thermodynamics, and reaction mechanisms fundamental equation to calculate kinetic parameters
(Chandrasekaran, Ramachandran and Subbiah, (5), on the basis of TGA results.
𝒅𝛂
2017; Abreu-Naranjo et al., 2024). A 10±5 mg = 𝐀 𝒇(𝛂). 𝒆(−𝑬𝒂⁄𝑹𝑻) (5)
𝒅𝒕
amount of powdered raw JS was deposited in an The heating rate (β) can be expressed as;
alumina pan of TGA-55. The sample was subjected 𝐝𝐓 𝐝𝐓 𝐝𝛂
𝜷 = 𝐝𝐭 = 𝐝𝛂 х 𝐝𝐭 (6)
to pyrolysis at three different heating rates: 10, 20,
and 30 °C/min. The related data were recorded from Plugging Eq. (5) and Eq. (6), the equation rewritten
ambient temperature to 900°C in the presence of as;
𝒂 𝐝𝛂 𝑨𝑹𝑻𝟐 𝟐𝑹𝑻
inert N2 gas, with a flow rate of 60 ml/min. The TGA 𝐠(𝛂) = ∫𝟎 =( ) [𝟏 − ] 𝒆(−𝑬𝒂⁄𝑹𝑻) 7)
𝐟(𝛂) 𝜷𝑬 𝑬
experiment was done three times to verify result
repeatability.
As per (Coats and Redfern, 1964), the term 2RT/E
in Eq. (7), is almost equivalent to unity that was

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 International Journal of Applied Engineering Research ISSN 0973-4562 Volume 19, Number 3 (2024) pp. 202-207
© Research India Publications.

ignored and Eq. (8) became as; 78.89%, and 12.11%, respectively. The percentages
𝑨𝑹𝑻𝟐 of carbon, nitrogen, oxygen, and hydrogen were
𝐠(𝛂) = ( ) 𝒆(−𝑬𝒂⁄𝑹𝑻) (8)
𝜷𝑬 determined to be 35.8%, 21.7%, 37.9%, and 7.9%,
In this study, ICTAC recommended Flynn-Wall- respectively. The biochemical compositions were
Ozawa (OFW) (Ozawa, 1965; Flynn, 1997), used to cellulose (32.5%), hemi-cellulose (28.12%), lignin
determined kinetic and thermodynamic parameters. (32.2%), and extractives (9.8%) respectively. The
Table 1 represents OFW model with their equation, physiochemical characteristics of BPS reported by
plotting parameters, and slopes to calculate Kumar et al., 2020 falls in same range. The higher
activation energy) test was run to definite specific heating value determined by bomb calorimeter
kinetic model delivering different output from group (HHV) is 15.99 MJ/kg. The majority of these
means. parameters are within the range reported by other
researchers for different lignocellulosic biomasses
Table 1 Iso conversional Kinetic model assigned for derived from agriculture.
activation of kinetic energy
Iso- 3.2 Thermogravimetric analysis
Kinetic Plotting Slope
conversiona
l method
equations parameters value Thermal behavior of BPS was determined using
𝐼𝑛𝛽 1 𝐸𝛼 thermogravimetric analyzer in the range of 29-900°C
𝐴𝐸𝛼 𝐼𝑛(𝛽) 𝑉𝑠 ( ) −1.052 at three different heating rates (10, 20 and 30°C/min).
𝑇 𝑅
= 𝐼𝑛 ( )
𝑅𝑔(𝛼 Figure 1 shows TGA graph plotted by % Wt. loss Vs
FWO
− 5.331 temperature and Figure 2 shows DTG plotted %Wt.
𝐸𝛼 loss/°C vs temperature. From Figure 1 it can be seen
− 1.052 ( )
𝑅𝑇 that for lower two heating rates i.e. 10 and 20°C/min
the nature of curve is slightly different than higher
2.4 Thermodynamic parameters estimation heating rate i.e. 30°C/min. TGA graph shows
In this study, the method of Flynn-Wall-Ozawa different temperature zone due different bio
(OFW) was used to calculate the pre-exponential constituents of BPS, i.e. cellulose, hemicellulose and
factor (A, s-1) using the equation developed by lignin (Sahu et al.,2023). First temperature zone
Arrhenius. Furthermore, the enthalpy changes (ΔH, exists from ambient temperature to 180°C in which
kJ mol−1), Gibbs free energy (ΔG, kJ mol−1), and maximum moisture content is removed, second
entropy (ΔS, J/mol⋅K) were determined using the temperature zone belongs in the temperature range of
specified equations given by(Balsora et al., 180-365°C, in which maximum weight loss is
2023;Chen et al., 2023) by using activation energy of observed and maximum volatile matter is removed
the OFW Method; from raw biomass. The third temperature zone varies
𝑬𝜶
( )
𝜷𝑬𝜶 𝒆 𝑹𝑻𝒎 from 366 to 900°C in which char formation take
𝑨= (9)
𝑹𝑻𝟐𝒎 place. Similar report has been presented by
∆𝑯 = 𝑬𝜶 − 𝑹𝑻𝒎 (10) researchers for different biomasses.
𝑲 𝑻
∆𝑮 = 𝑹𝑻𝒎 𝒍 𝒏 ( 𝑩𝒉𝑨𝒎 ) + 𝑬𝜶 (11)
∆𝑺 = (∆𝑯 − ∆𝑮)/𝑻𝒎 (12)
100 TGA Graph
-23 10oC/min
Where, KB= Boltzmann constant (1.381 × 10 J/K); 20oC/min
80
h= Planck constant (6.626 × 10-34 J⋅s); 30oC/min

Tm= DTG peak temperature, K

Weight (%)

60

40
3. Result and Discussion
3.1 Biomass characterization 20

The physiochemical components of BPS play a 0

crucial role in determining the characteristics and
100 200 300 400 500 600 700 800 900
possible applications of biomaterials and bioenergy. Temperature (oC)
The levels of moisture content, fixed carbon, volatile
matter, and ash were determined to be 12.11%, 8.7%, Figure.1 Basic thermogravimetric analysis

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 International Journal of Applied Engineering Research ISSN 0973-4562 Volume 19, Number 3 (2024) pp. 202-207
© Research India Publications.

From Figure 2 the shift of peak temperature was BPS-Activation energy

Activation Energy, kJ/mol

observed without changing the degradation pattern 600
with increase in heating rates. The peaks were 500
noticed in first stage at 40℃-60°C showed removal
400
of moisture present in BPS. Followed by this, peaks
were noticed at 200-300°C and 320-365°C, showed 300
rapid degradation of hemicellulose and cellulose 200
respectively of BPS. 100
0
0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
-30 Conversion
DTG Graph
-25
Figure 3 Activation energy of BPS by OFW
10oC/min
20oC/min method
-20
30oC/min
DTG (% /min )

-15
3.8 0.
1
-10 3.6 0.
2
-5 3.4 0.
3.2 3
0
0.
ln β

100 200 300 400 500 600 700 800 900 3 4

Temperature ( C)o 0.
2.8 5
Figure2 Basic derivative thermogravimetric 2.6 0.
6
analysis 2.4 0.
7
2.2
3.3 Determination of Activation energy 0.
2 8
The activation energy is the minimal energy needed 0 0.0005 0.001 0.0015 0.002 0.0025 0.
to start a chemical reaction in biomass. Figure 3 9
illustrates the activation energy of BPS using the 1
1/T
OFW technique throughout the range of 0.1-0.9. The
graph illustrating the relationship between OFW and Figure 4 Activation energy of BPS by OFW
time is displayed in Figure 4. The range of activation method
energy values for BPS was 33.72-486.95, with a
mean value of 187.35 kJ mol−1. The average 3.3.1 Thermodynamic parameters
activation energy (Eα) for BPS falls within the same The parameters associated with the thermodynamic
range as cotton stalk (202.5 kJ mol−1) (Silva et al., of the BPS were computed based on the activation
2019) and paddy straw (203.72 kJ mol−1) (Gao et energy of the OFW technique. These parameters
al., 2021). However, it is higher than potato stalk include the pre-exponential factor (A, S-1), changes
(125.99 kJ mol−1) (Nawaz and Kumar, 2023) and in enthalpy (ΔH, kJ/mol), Gibbs free energy (ΔG,
finger millet straw (172.18 kJ mol−1) (Karuppasamy kJ/mol), and entropy (ΔS, J/mol⋅K). The calculations
Vikraman et al., 2021). were performed at a heating rate of 10°C/min and the
results are presented in Table 2. For the design and
expansion of the pyrolysis reactor, it is necessary to
take into account the needed process parameters of
the BPS pyrolysis. The thermodynamic
characteristics of the BPS pyrolysis process are
crucial for the design and scaling up of the pyrolysis
reactor. The pre-exponential factor for BPS varies
from 101 to 1060.The mean value of the pre-
exponential component for the BPS was 1059.

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 International Journal of Applied Engineering Research ISSN 0973-4562 Volume 19, Number 3 (2024) pp. 202-207
© Research India Publications.

The Gibbs free energy (ΔG) is the minimum amount Acknowledgements

of energy or heat needed to produce usable goods Authors are thankful to the Director, ICAR-NINFET,
from biomass. The mean value of Gibbs free energy for providing facilities and materials.
(ΔG) for BPS was 116.12 kJ mol−1. The enthalpy
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