PREPARATION AND CHARACTERIZATION OF

ACTIVATED CARBON FROM WASTE SAWDUST

FROM SAW MILL

D. Shrestha, G. Gyawali and A. Rajbhandari (Nyachhyon)

Journal of Institute of Science and Technology

Volume 22, Issue 2, January 2018
ISSN: 2469-9062 (print), 2467-9240 (e)

Editors:
Prof. Dr. Kumar Sapkota
Prof. Dr. Armila Rajbhandari
Assoc. Prof. Dr. Gopi Chandra Kaphle
Mrs. Reshma Tuladhar

JIST, 22 (2): 103-108 (2018)

Published by:
Institute of Science and Technology
Tribhuvan University
Kirtipur, Kathmandu, Nepal
 JIST 2018, 22 (2): 103-108 © IOST, Tribhuvan University
ISSN: 2469-9062 (p), 2467-9240 (e) Research Article

PREPARATION AND CHARACTERIZATION OF ACTIVATED

CARBON FROM WASTE SAWDUST FROM SAW MILL
Dibyashree Shrestha1, Gobinda Gyawali2, Armila Rajbhandari (Nyachhyon)*3
1
Patan Multiple Campus, Tribhuvan University, Lalitpur, Nepal
2
Research Centre for Eco Multi-Functional Nano Materials,
Global Research Laboratory, Sun Moon University, Korea
3
Central Department of Chemistry, Tribhuvan University, Kathmandu, Nepal
*Corresponding E-mail: [email protected]

Received: 1 November, 2017; Revised: 25 November, 2017; Accepted: 27 November, 2017

ABSTRACT
Activated carbon was prepared in laboratory using waste sawdust powder of Shorea robusta (Sal) from saw
mill by chemically activated Na2CO3 followed by carbonization technique. Thus prepared activated carbon
was characterized by Iodine Number (IN) and Methylene Blue Number (MBN). Iodine number was found to
be 534.6 mg/g whereas MBN was found to be 196.08 mg/g which indicated the presence of micropores as
well as mesopores in the prepared material. This was also exposed by SEM image. Specific surface area was
measured by BET method and was found to be 10.01 m2/g. Then phase state of samples was determined by
X-ray diffraction (XRD), which indicated the amorphous nature of the prepared material. The development
of surface functionality due to activation was examined by Fourier Transform Infrared Spectroscopy (FTIR)
which showed the presence of oxygenated functional groups such as ether, diketone, lactone, phenol on the
material. These functional groups are considered to be electrochemically active and contribute to the
capacitance of electrical double layer capacitance (EDLC). Further, electrochemical characterization of
prepared material was carried out by conductivity test and cyclic voltammetry. The cyclic voltametric curve
showed symmetric rectangular shape indicating electrical double layer capacitive behavior.

Keywords: Wood derived activated carbon, Chemical activation, Conductance, Specific capacitance, EDLC.

INTRODUCTION (Nahil et al., 2012). The choice of carbon as the

The preparation of activated carbon from wood- material is due to its unique properties of electrical
based industrial residue like sawdust from sawmill conductivity as well as structural diversity.
is one of the most environmental friendly solutions Different literatures showed that the activated
of transforming negative-valued wastes to valuable carbon could be used as electrode materials for
materials. Wood is a natural fiber raw material with electric double layer capacitors (EDLCs), Li-ion
varying properties in morphology and chemical batteries and fuel cells (Beguin et al., 2010;
composition. The major chemical constituents of Frackowick et al., 2007; Frackowick et al., 2001;
wood are cellulose, hemicelluloses and lignin Becker et al., 1957, Endo et al., 2001). Preparation
(Chowdhury et al., 2012). Such lingo-cellulosic of highly porous carbons may be a challenging art
carbonaceous material can be used for the and attention has been given for activation
preparation of activated carbon (Beguin et al., (physical and chemical), carbonization and
2010). Activated carbons are unique and versatile templeting methods using zeolite and mesoporous
in their performance. They have major industrial silica (Pandolfo et al., 2006; Sharma et al., 2010;
significance. Activated carbon materials Wang et al., 2012; Simon et al., 2008; Zhang et al.,
characterized by high specific surface area and 2009). Each approach has its own advantages for
tunable porosity find utility in many vital the formation of carbons with controlled pore
technologies namely energy storage, energy texture and /or improved surface area, which are of
conversion, sensors, environmental protection, great importance and considered to be the key
production of fine and bulk chemicals, and catalysis factors in optimizing the performance in their

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Preparation and Characterization of Activated Carbon ...

applications. For energy storage system having high through 150 µm sized sieve. Thus obtained sawdust
energy density and excellent rate performance is powder was used as a precursor for the preparation
desirable. This study presents preparation of of activated carbon.
activated carbon from locally available material. Preparation of activated carbon by
Sawdust from Shorea robusta (Sal), a solid residue carbonization method
generated in the timber industry has been selected The fine powdered precursor was preheated for two
to prepare activated carbon. The prepared material hours and was impregnated with Na2CO3. The ratio
was subjected for electrochemical characterization. of precursor to activating agent was 1:1 (wt:wt).
They were left for 24 hours for proper soaking.
MATERIALS AND METHODS After soaking, the precursors were dried in an oven
Materials at 1100C. The dried precursors were carbonized in
All the chemicals and reagents used were of tube furnace at 4000C for 3 hours in an inert
analytical grade and procured from Merck atmosphere of nitrogen. Continuous flow of pure
Company. All the experiments were carried out in nitrogen was used to create an inert atmosphere.
distilled water. The sawdust of Shorea robusta The carbonized samples were cooled to room
species has been collected from local saw mill. temperature maintaining inert atmosphere of
nitrogen. The cooled samples were washed with
Methods
distilled water for several times till they became
Preparation of sawdust powder neutral. Finally the washed sample was dried in an
The collected waste wood from saw mill was sun- oven at 1100C and stored in air tight bottles. Table
dried for few days and followed by preliminary 1 show the sample name and preparation condition.
stages such as crushing, grinding and sieving

Table1: Sample name and preparation condition

S.N. Sample name Activating Preheating Preheating Carbonization Carbonization Atmosphere
agent time (hour) temperature temperature holding time
(oC) (oC) (hour)
1 WAC-Na2CO3 Na2CO3 2 110 400 3 N2

Sample characterization Conversion factor is calculated by following

The Proximate analysis equation 2.
The proximate analysis of the precursor was Conversion factor (f) = (Molecular weight ×
conducted according to ASTM D121 (ASTM 2009) Normality of Iodine × 10) / (Weight of WAC ×
and the results are expressed in terms of moisture, Blank reading) .....……………………..………. (2)
volatile matter, fixed carbon, and ash contents. C = (Blank reading – Volume of hypo consumed
Determination of Iodine Number (IN) after adsorption on activated carbon)
Iodine number (IN) is a relative indicator of porosity Determination of Methylene Blue Number
in an activated carbon. It is the measure of micro (MBN)
pores up to 2 nm size found in activated carbon. It Methylene blue number (MBN) was considered as a
is determined according to the ASTM D4607-94 measure of mesoporosity of 2-50 nm sized pore
method (ASTM 1999). 0.1 g of WAC-Na2CO3 was sand was determined by adsorption of dye per gram
separately taken in different conical flasks and of adsorbent. In this study, 0.05 gm of WAC-
added 5 mL of 5% HCl, boiled and cooled. To this Na2CO3 was placed in contact with 50 mL of a
solution, 10 mL of 0.1N Iodine solution was added. methylene blue solutions at different concentration
The contents were vigorously shaken for about 4 (50, 100, 150, 200, 250 and 300 mg/L) for 24 hours
minutes and filtered. Then 10 mL filtrate was at room temperature. The suspension was filtered
titrated against standard (0.1N) hypo solution using and the remaining concentration of methylene blue
starch as an indicator. The concentration of iodine was analyzed using UV/vis spectrophotometer. The
adsorbed by WAC-Na2CO3 was calculated by using methylene blue number of WAC-Na2CO3
following equation. (maximum adsorption capacity) was calculated by
Iodine number = C × Conversion factor (f) ...... (1) using Langmuir Isotherm.

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 D. Shrestha, G. Gyawali and A. Rajbhandari (Nyachhyon)

Qe(mg/g) = (Co-Ce)V / M ………......………….. (4) of 100 mV/S for 100 cycles. Capacitance values
Where, were estimated from CV.
Qe = Amount of methylene blue adsorption
Co(mg/L)= Initial concentration of methylene blue RESULTS AND DISCUSSION
Ce (mg/L)= Equilibrium concentration of methylene Proximate Analysis of Precursor
blue The results obtained from proximate analysis of
V (L) = Volume of methylene blue precursor are given in Table 2. It revealed that the
M(g) = Mass of WAC-Na2CO3 moisture and ash content of the precursor was
8.56% and 1.07% respectively. This result also
showed that the precursor has 31% of volatile
Scanning Electron Microscopy (SEM): The matter, low ash and moisture content. The low ash
SEMU-8000, Hitachi Co. Ltd., Japan was used to content in the sample indicates that the precursor
study surface morphology of theWAC-Na2CO3. contains low inorganic matter.
X-ray Diffraction (XRD): Bruker D-8 Advance X-
ray Diffractometer using monochromatized Cu-Kα
Table 2: Proximate analysis of sawdust of
radiation was used to record XRD.
Shorea robusta (Sal)
Fourier Transform Infrared Spectroscopy (FTIR):
Surface functional groups present in WAC-Na2CO3 S.N. Parameter Observed value (%)
were estimated by Fourier Transform Infrared (FTIR) 1 Moisture 8.56
Spectroscopy analysis with Thermo Electron
Corporation Nicolet 4700. The % transmission of 2 Total Ash 1.07
samples was recorded over 4000-500 cm-1. 3 Volatile Matter 31.98
Surface area determination by BET: The specific 4 Total Carbon 48.0
surface area was measured from nitrogen
adsorption- desorption isotherms at 77 K data using
Brunauer, Emmett and Teller (BET). Iodine Number and Methylene Blue Number
Electrochemical performance: Iodine number of prepared WAC-Na2CO3 was
Preparation of electrode found to be 534.6 indicating the presence of
In order to prepare electrode, 0.3 g of graphite micropores in the sample. Similarly, methylene
powder, 0.3 g of paraffin wax, 0.4 g of WAC- blue number was found to be 196.08 mg/g
Na2CO3 was mixed homogenously and heated for indicating presence of mesopores.
few minutes. Then the electrode material was Scanning Electron Microscopy (SEM)
formed which was poured and packed tightly to Scanning Electron Microscopic (SEM) image of
about 2 cm at the bottom of 3 mL plastic syringe. sample WAC-Na2CO3 is presented in figure 1.
Then the electrical contact was made by keeping a
copper wire. This electrode has been used as
working electrode.
Preparation of Electrochemical cells
Three electrode cell system has been applied. Here,
as prepared electrode was used as the working
electrode, saturated calomel electrode has been
used as reference electrode, whereas platinum
electrode was used as counter electrode. The
electrolyte used here was 0.5 M H2SO4.
Cyclic Voltammetry (CV)
Electrochemical performance of WAC-Na2CO3 was
evaluated by Cyclic Voltammetry (CV). The CV
measurements were obtained in
Potentiostat/Galvanostat by using Polarization
Monitor Software interfaced with IBM computer in
the potential range of -0.5 to 1 volt. The cyclic
stability of prepared ACs was obtained at scan rate Fig. 1. SEM image of WAC-Na2CO3

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Preparation and Characterization of Activated Carbon ...

In SEM image of WAC-Na2CO3, one can observe

mesopores along with micropores. Similarly, the
cylindrical micro and mesoporous channel could
also be seen. Besides this, bigger sized macropores
are also obvious on the surface which is anticipated
to be responsible for low surface area of this
sample. The breakdown of wall of micro and
mesopores may have been occurred due to
continuous reaction of excess activating agent.

X-ray Diffraction (XRD)

X-ray diffraction analysis of the sample was carried
out in order to determine the degree of crystallinity
or amorphous nature of the activated carbons. The
X-ray diffraction spectra WAC-Na2CO3is presented
in figure 2.

Fig. 3. FTIR Spectra of WAC-Na2CO3

The small peak at around 2353cm-1in FTIR spectra

is recognized for the presence of C-N group. The
band at 1680 cm-1 was likely to be a combination of
the carboxyl C=O stretching of non aromatic
carboxylic acid and lactone structure. Similarly, the
next band is observed at the region around 1576
cm-1 which may be assigned to a combination of
C=C stretching vibration of the aromatic ring
structures and conjugated systems such as diketone,
ketoester and quinine (1550-1680 cm-1). The band
at 1300-1000 cm-1may be probably due to the C-O-
C lactone structure, the stretching C-O vibrations of
Fig. 2. XRD pattern of WAC-Na2CO3 phenol structures and ethers, and the bending O-H
modes of phenol structures. Similarly, the band at
As can be seen in figure 2, the XRD pattern of the 1700 cm-1is attributed due to the presence of C=O
sample exhibit diffraction peaks at around 2θ = 25 stretching (Joshi et al., 2014).
degree. In the same way, WAC-Na2CO3 exhibited BET Surface Area
another weak peak at around 2θ = 43 degree. The BET surface area WAC-Na2CO3 was found to be
diffraction peaks at around 2θ = 25 degree having 10.45m2/g, which is considered to be small. It may
002 planes and 2θ = 43 degree having [101] plane be due to break down of walls of micro as well as
assigned for hexagonal graphitic carbon (Liu et al., mesopores and certainly due to the formation of
2009). The XRD pattern indicates that the macropores.
laboratory prepared activated carbons are Cyclic Voltammetry
amorphous, similar to commercial activated carbon
Figure 4 shows the cyclic voltamogram of WAC-
and poorly graphitized.
Na2CO3 at the scan rate of 100 mVs-1 for 100 cycles
Fourier Transform Infrared Spectroscopy measured in 0.5 M H2SO4 aqueous electrolyte
(FTIR) solution within a potential range of -0.5 to 1 volt
In figure 3, the spectra clearly indicate the creation against saturated calomel as reference electrode. In
of surface functional groups on the surface of figure 4, one can see the current density of 1st cycle
sample. It may be due to an effect of activating was 0.21 A/g. But there was slight decrease in
agent used during carbonization. current density after 10 cycles.

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 D. Shrestha, G. Gyawali and A. Rajbhandari (Nyachhyon)

graphitic carbon, however broad peak showed

amorphous nature.
The electrodes prepared from activated carbon
showed a small current response during cyclic
voltammetry measurement. Similarly, the specific
capacitance was found to be low. It might be due to
high resistance because specific conductivity value
was also found to be low. These values are quite
reasonable as the specific surface area was found to
be small. The abundance of macropores may be
another reason for low capacitance. However,
rectangular shape of CV curve showed electrical
double layer capacitive behavior. Conversely, it
needs further enhancement of surface area for
significant improvement in capacitive behavior.

ACKNOWLEDGEMENT
Fig. 4. Cyclic Voltamogram of WAC-Na2CO3 DS is thankful to Institute of Science and
Technology, Tribhuvan University to conduct Ph.
However, the shape of CV was found to be D. research in Central Department of Chemistry,
rectangular indicating electrical double layer Kirtipur. Global Research Laboratory, Sun Moon
capacitance (EDLC) behavior. In the same way, CV University is highly acknowledged for recording
shape is mirror symmetric even at high scan rate SEM, XRD and FTIR.
indicating the high reversibility of the sample.
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