Energy Sources, Part A: Recovery, Utilization, and

Environmental Effects

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Pyrolysis of coconut husk biomass: Analysis of its

biochar properties

Swapan Suman & Shalini Gautam

To cite this article: Swapan Suman & Shalini Gautam (2017) Pyrolysis of coconut husk biomass:
Analysis of its biochar properties, Energy Sources, Part A: Recovery, Utilization, and Environmental
Effects, 39:8, 761-767, DOI: 10.1080/15567036.2016.1263252

To link to this article: https://doi.org/10.1080/15567036.2016.1263252

Published online: 16 Mar 2017.

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ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS
2017, VOL. 39, NO. 8, 761–767
http://dx.doi.org/10.1080/15567036.2016.1263252

Pyrolysis of coconut husk biomass: Analysis of its biochar

properties
Swapan Suman and Shalini Gautam
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad, Jharkhand, India

ABSTRACT KEYWORDS
The effect of pyrolysis at different temperatures on the biochar character- Coconut husk; gross calorific
istics of coconut husk was studied. The biochar obtained was then char- value; functional groups;
acterized by proximate and ultimate analyses, gross calorific value, pH, pyrolysis; surface area
surface area, percentage yield, FTIR, and FE-SEM. The results show that
there was a significant change in the volatile matter, carbon percentage,
surface area, pH, and its functional group as temperature increases. The
moisture content and percentage yield decrease with increasing tempera-
ture. Thus, the results show that the carbonization has a significant influ-
ence on the processing characteristics of coconut husk biochar.

1. Introduction
In recent years, the rising cost of energy is associated with decreasing fossil fuel reserves, and these
are incentives for the development of new green energy technologies using biomass (Brassard et al.,
2014). Recycling of biomass, which is simply to burn to ash for disposal, has seen a sharp increase,
posing a serious social problem for our society and a major challenge in the protection of environ-
ment and natural resources. Globally, biomass is the third largest sources of energy after coal and oil.
India produces approximately 350 million tonnes of agricultural waste per year (Pallavi et al., 2013)
such as straw, bagasse, coconut husk, coffee husks, and rice husks as well as residues from forest-
related activities such as wood chips, sawdust, bark, etc. Pyrolysis of the biomass is the most
promising thermo-chemical process to produce energy from biomass. Of the two processes of energy
conversion from biomass (i.e., thermo-chemical and bio-chemical processes), the thermo-chemical
process has advantage over the bio-chemical process owing to the challenges of rapid and complete
conversion of biomass into energy efficiently (Bhaskar et al., 2011). Pyrolysis is a process in which
thermal degradation of the chemical constituent of biomass is carried out in the inert atmosphere to
produce energy. Biochar, bio-oil, and gas are the three products of the pyrolysis of the biomass,
wherein biochar, a solid carbon-rich by-products of thermal stabilization of biomass (Masek et al.,
2013), has high energy and to some extent is rather comparable to the coal used in the industries as
feed stocks for fuel (Fu et al., 2012; Mohanty et al., 2014).

2. Sample collection and preparation

Coconut husks were obtained from the local market of Dhanbad, Jharkhand, India. The coconut
husks was air-dried and sliced into small sizes. Four samples of 1 kg each were weighed and
pyrolyzed (Demirbas, 2004a) in muffle furnace at different temperatures, viz. 400, 600, 800, and
1000°C at 5–15°C/min heating for 2 hour. The carbonized coconut husks were then grounded to
particle size of below 212 micron (-72 mesh) and further characterized for the biochar properties.

CONTACT Swapan Suman er.ssuman@gmail.com Department of Fuel and Mineral Engineering, Indian School of Mines,
Dhanbad 826004, Jharkhand, India.
© 2017 Taylor & Francis Group, LLC
762 S. SUMAN AND S. GAUTAM

3. Results and discussion

3.1. Proximate analysis and ultimate analysis of coconut husk
Proximate analysis was performed on the prepared sample of coconut husk for determination of
moisture, ash, and volatile matter (VM) contents following the Standard ASTM method (ASTM
E871, E830, and E872, respectively) (Demirbas, 2004b). The results of Proximate and Ultimate
analysis for prepared coconut husk sample are summarized in Table 1 . The VM content of coconut
husk found to be high as 82.94% with heating value as 14.08 MJ/kg and low ash content as 0.92%.
ASTM D5373 Standard test method was followed for Ultimate analysis. The Ultimate analysis of
sample was done using Vario EL-III CHNS analyzer.

3.2. Physicochemical and elemental composition of obtained biochar from coconut husk at
different temperature range
The proximate analysis for coconut husk biochar (CHC) was determined according to ASTM
D1762-84 Standard method. Physicochemical and elemental compositions of obtained biochars at
different temperature are given in Table 1. The VM content gradually diminishes with the increase
in temperature (Lapuerta et al., 2008). The ash content also decreases with increase in temperature. It
is observed that the higher fractions of ash content generally have the lowest values of fixed carbon
and vice versa.
From the Ultimate analysis as presented in Table 1, it can be seen that carbon content (47.92 to
74.08%) in CHC significantly varied with respect to change in temperature from 400° to 1000°C.
Lower H:C ratios likely undergo the greater thermal alteration due to the loss of H and N relative to
C (Table 1). The lowest H:C ratio and highest C:N ratio were observed. Analytical elements and both
H:C and O:C ratios are valuable indicators of the character of CHC (Nguyen and Lehmann, 2009).

3.3. Gross calorific value (GCV), pH, and surface area

The percentage yield, gross calorific value, pH, and surface area measurement of CHC at tempera-
ture range of 400, 600, 800, and 1000°C are given in Table 1. The gross calorific value (GCV) of the
samples was determined by bomb calorific measurement using the (ASTM D4809-00) Standard test
method. The surface area was determined using N2 sorption isotherms using the Brunauer–Emmett–
Teller (BET) Surface Area Analyzer (ASA P2020 BET). 5 g samples are soaked in (1:20, w/v ratio)
slurry in water for the measurement of pH using PCS TestrTm 35 pH meter.

Table 1. Physicochemical and elemental compositions of coconut husk and its obtained biochar at temperature range 400, 600,
800, and 1,000°C.
CH CHC at 400°C CHC at 600°C CHC at 800°C CHC at 1,000°C
VM%* 82.94 30.56 20.82 5.33 4.72
Ash%* 0.92 26.27 21.99 17.32 12.03
FC% 16.14 43.17 57.19 77.35 83.25
C% 47.00 47.92 58.43 67.31 74.08
N% 0.21 1.34 1.02 0.87 0.50
H% 6.07 3.50 3.01 2.67 2.50
S% 0.12 0.17 0.16 0.17 0.17
O% 46.60 47.06 37.38 28.98 22.74
O/C - 0.98 0.64 0.43 0.31
H/C - 0.07 0.05 0.04 0.03
C/N - 35.76 57.28 77.37 148.16
% Yield - 43.33 36.00 34.00 31.00
pH - 8.50 9.64 10.87 11.02
GCV (MJ/kg) - 15.44 19.62 23.28 26.20
BET surface area (m2/g) - 39.57 120.73 256.60 590.41
*Air dry basis.
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 763

The percentage yield of CHC decreases with increase in temperature, which varies from 43.33% to
31.00%. The gross calorific value of CHC increases with increase in temperature, varying between
15.44 MJ/kg and 26.20 MJ/kg as carbon content is increasing with the change in temperature. The
pH of CHC is varying from 8.50 to 11.02. The pH value of CHC increases with temperature; this
may be attributed to the consequence of the relative concentration of non-pyrolyzed inorganic
elements.
The surface area represents the most critical physical properties of biochar (Kalderis et al., 2008).
The surface area of CHC increases with the increase in temperature (39.57–590.41 m2/g), i.e.,
porosity of biochar is increasing with the increase in temperature. The higher the porosity, the
lower will be the strength in biochar.

3.4. Fourier transform-infrared (FT-IR) spectroscopy

The FT-IR spectra of coconut husk and its derived biochars at different temperature ranges are
shown in Figure 1 . FT-IR spectroscopy was analyzed by a Perkin Elmer Spectra 2, USA. These
graphs were plot between wave numbers against transmittance percentage, which shows the
aliphatic loss in their functional group (Lee et al., 2010).
Aliphatic losses obtained at different wave numbers are shown in Table 2, which represents
strong, moderate, and weak striation of coconut husk and its derived biochars at 400, 600, 800, and
1000°C.

3.5. Field emission scanning electron microscope (FE-SEM) image and EDX analysis
Field Emission Scanning Electron Microscope (FE-SEM) images of coconut husk and its
derived biochar are shown in Figures 2 and 3 . Images were captured using a SUPRA’55
MonoCL4 Variable Pressure FE-SEM. Images were taken at several magnifications ranging
from 50× to 20000×. Visual inspection of these images illustrates the differences in micro-
structure among the biomass and derived biochar, with distinct microspores and channels
noticeable (Yargicoglu et al., 2014). There is a large morphological change among the two
phases. Grounded raw CH sample shows fibrous structure with long fibres (Fernandez et al.,
2012) as it can be seen in Figure 2. During thermal change at 800°C, large amounts of volatile

Figure 1. Fourier-transform infrared (FT-IR) spectra of the coconut husk and its derived biochars at temperature range of 400, 600,
800, and 1,000°C.
764 S. SUMAN AND S. GAUTAM

Table 2. Functional losses in coconut husk and its derived biochar at different temperature ranges of 400, 600, 800, and 1,000°C.
Coconut husk
Wave numbers Striations
Functional group (cm−1) Raw 400°C 600°C 800°C 1,000°C
H-bonded O–H 3,400 to 3,800 cm−1 Strong Moderate Weak Weak
stretching vibrations of
hydroxyl groups
C–H stretching of alkyl 2,850 to 2,950 cm−1 Weak Weak Peak not Peak not Peak not
structures observed observed observed
C=O in amide (I), ketone, 1,600 to1,650 cm−1 Strong Moderate Peak not Peak not Peak not
and quinone groups observed observed observed
C–H deformation of CH3 1,400 to 1,460 cm−1 Weak Weak Weak Weak Weak
group
O–H stretching of 1,200–1,270 cm−1 Weak Weak Peak not Peak not Peak not
phenolic compounds observed observed observed
C–O Stretch(alkyl/aryl 1,000–1,150 cm−1 Strong Moderate Weak Peak not Peak not
ethers) observed observed
bending of Si–O 460–990 cm−1 Weak Weak Peak not Peak not Peak not
stretching observed observed observed

Figure 2. FE-SEM image analysis of the coconut husk (CH).

matter flow from the solid material in a short period of time, which varies the particles surface,
shrinking and splitting it as can be seen in Figure 3.
EDX analysis results are shown in Figure 4, where results are presented in mass percentage of the
sample. Coconut husk is basically organic structure with large amounts of carbon and oxygen in its
structure (Figure 4). Some other elements were found too such as Sodium (Na), Aluminium (Al),
Silicon (Si), Chlorine (Cl), and Potassium (K). It can be also seen that some amount of gold is
presents in all the samples, because of gold coating to charge the sample before analysis, due to non-
conducting behavior of sample.
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 765

Figure 3. FE-SEM image analyses of the coconut husk char at 800°C.

Figure 4. EDX analysis of the coconut husk and its derived char at 800°C.

When studying samples at 800°C, it can be noticed that the composition has totally changed
(Figure 4). Every biochar samples showed a huge amount of carbon, and some amounts of Na,
Cl, and K were also found.

4. Thermo-gravimetric analysis (TGA)

A computerized NETZSCH SAT 449F3 thermogravimetry analyzer was employed in a gas flow of 20
ml/minute following the ASTM E1131-03 standard method. The inert gas was nitrogen. The
temperature program used for the TGA starts at room temperature to 105°C. The samples were
then subjected to increased heating to a final temperature of 700°C at an increment rate of 25°C/min.
766 S. SUMAN AND S. GAUTAM

Figure 5. TG and DTG of the CH and its biochars obtained at different temperature ranges at 400, 600, 800, and 1,000°C.

Around 5–20 milligrams of sample were taken and heated up to a final temperature of 700°C, and a
residence time of 1 minute at 700°C was allowed. TGA was performed in both air and nitrogen
atmospheres at a heating rate of 20°C/min.
At 350–550°C, the thermal decomposition of coconut husk is nearly complete as shown in
Figure 5 . The first mass loss (50°C < T < 150°C) is due to presence of moisture and evaporation
of some extractive compounds. The second loss (200°C < T < 400°C) is mainly related to
hemicelluloses and cellulose thermal degradation. The maximum of the DTG curves is attributed
to cellulose complete degradation. Lignin is a more unchanging module presenting a large range
of thermal degradation (from 250 to 600°C or even higher temperatures, depending on biomass
feedstocks), and in this manner, the third degradation step (360 < T < 650°C) is endorsed to
lignin degradation.
The weight loss of CH and its derived biochar occurred at different temperatures ranges at 400, 600, 800,
and 1000°C. According to the TG curves, between 70% and 90% by weight of the samples were decomposed
at temperature below 700°C. Most of the weight loss occurred at the temperature between 150°C and 450°C.
This is a good indication that these waste residues are easily decomposed via thermal processing and would
be excellent feedstocks for pyrolysis reactions (Jindo et al., 2014). The weight loss of CH was 70–90% of the
total weight. This behavior reflects the higher mineral content in this material (Jindo et al., 2014). Thermal
analysis of all the derived biochars at different temperatures showed a similar thermal degradation profile,
where weight loss decreases with the increase in pyrolysis temperature (Kim et al., 2014). The weight loss of
prepared biochars at different temperature ranges 400, 600, 800, and 1000°C varies from 15% to 30%.

5. Conclusion
The work is an attempt at exploring the effect of pyrolysis on the processing characteristics of
coconut husk biochar. With the increase in pyrolysis temperature, yield, VM, H, and H/C ratio of all
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 767

the biochars decrease; but ash, FC, C, aromaticity, degree of carbonisation, HHV, pH, and surface
area increase. Higher pyrolysis temperatures (600–800°C) promote condensation reactions and
aromaticity, through decomposition of functional groups.
The conversion of coconut husk by pyrolysis to biochar can be a potential option to utilize these
wastes for various sustainable purposes like as a substitute of renewable energy sources for fossil-
derived fuel inputs; as a soil ameliorant, enhancer of soil fertility, and C-sequestration; and in waste
water treatment. In particular, biochar derived particularly from coconut husk waste (600 to 800°C)
has better potential to be used for steel making, and biochar derived at temperatures (400 to 1000°C)
has more enhanced relevance for soil amelioration, C-sequestration, and waste water treatment.
Thus, the results obtained have a potential application of thermal and metallurgical purposes.

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