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P-ISSN: 2303-1832 Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi 07 (1) (2018) 33-39

e-ISSN: 2503-023X DOI: 10.24042/jipfalbiruni.v7i1.2459


April 2018

CHARACTERIZATION OF ACTIVE CARBON PREPARED FROM


COCONUTS SHELLS USING FTIR, XRD AND SEM TECHNIQUES

Andi IkhtiarBakti*1, Paulus Lobo Gareso2


1, 2
Departement of Physics, Faculty of Mathematics and Natural Sciences, Universitas Hasanuddin,
Makassar-South Sulawesi, Indonesia
*Correspondence address: andiikhtiar@yahoo

Accepted: October 25th, 2017. Approved: February 2th, 2018. Published: April 24th, 2018

Abstract: Activated carbon is produced from coconut shells through physical and chemical activation. With
pyrolysis method, the optimum activation temperature for physics activation is 600 oC, and for chemical,
activation is to soak it in activator ZnCl2 10% and Na2Ca3 10%. Activated carbon was analyzed by Fourier
Transformation Infrared (FTIR) and X-ray Diffraction (XRD) methods. The FTIR result showed that the
coconut shells succeeds in becoming carbon. The XRD results confirm the existence of several phases of
crystals like graphite around the peaks of 36o and 44o, there are two wide diffraction peaks and can be
interconnected with carbon and graphite content. The SEM result showed that the carbonization of pyrolysis
and activation processes created porosity and a large surface area for absorption.

© 2018 Physics Education, UIN Raden Intan, Lampung, Indonesia.

Keywords: activated carbon, coconut shell, FTIR, SEM, XRD

INTRODUCTION The development of methods of reusing


Coconut shell as a raw material is often waste materials as activated carbon was
converted into activated carbon (Arami- expected to be a solution in waste
Niya, Daud, Mjalli, Abnisa, & Shafeeyan, utilization, such as jatropha seed,
2012). Based on data obtained, Southeast corncobs, coconut shell, palm fiber and
Asia was a region with a considerable sawdust, which proves very good to be
amount of coconut production with four converted into activated carbon because of
countries as its main producers; India, its hard texture and strength due to the high
Indonesia, Philippines, and Sri Lanka lignin and carbon content and low ash
contributing 78% of coconut production in levels of these materials (Lehmann &
the world (Rao, A.H.L.Swaroop, Rao, & Joseph, 2009; Promdee et al., 2017; Rao et
Bharath, 2015). In regard to the production al., 2015).
of the activated carbon, Indonesia is The process of producing activated
currently one of the main exporter carbon from coconut shell consists of
countries of activated carbon pyrolysis method, turning coconut shell
(Cocommunity, 2016). into charcoal, then activation process. The
Activated carbon has been known as activation process was divided into two,
the most effective and useful adsorbent for namely physical activation and chemical
removing pollutants from contaminated activation. The process of physical
gas and liquid flow. This is due to the fact activation is obtained by carbonization
that the activated carbon has a large active with an oxidizing gas or carbon dioxide in
surface area which can provide a well- high temperatures (400-1000oC), while
developed porous structure of absorption chemical activation was immersed it in the
capacity and good mechanical properties chemical solutions of a certain
(Hidayu, 2016). The fundamental for concentration such as ZnCl2, Na2CO3,
producing activated carbon was carbon- KOH, and KCl (Hung, 2012). Activated
rich organic material (A.R Hidayu, 2016). carbon produces better carbon crystal
34 Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi, 07 (1) (2018) 33-39

structures and amorphous structures that shell sample was then dried in the oven at
are stacked irregularly by carbon rings that 110oC for 24 hours to remove surface
are useful for producing an adsorbed gap, moisture and then milled to the desired
with 97% pure carbon (Pradhan, 2011; size. Then an analysis was performed to
Rani, Mohammad, Matali, & Kadir, find out the volatile and carbon content as
2014). well as to measure the composition of each
The activation process is carried out by element. This method is similar to the
mixing the initial material with the previous research method (Hidayu,
activation reagent and afterward heating it Muhammad, Matali, & Sharifah, 2013).
under the inert atmospheric pressure (A.R
Hidayu, 2016). This process was usually Activated Carbon
performed at lower temperatures and times The coconut shell was activated using
compared to the process of physical physical activation by being fed into a
activation. The surface area and the pyrolysis reactor which was heated to a
resulting porosity are better than the temperature of 600oC and it was stored for
activation. Therefore, this research used an hour. The activated carbon was
the coconut shell as the main ingredient in immersed in ZnCl2 10% and Na2CO3 10%
making activated carbon considering its then stored for 24 hours at room
abundant material in Indonesia and very temperature. After the activation process
affordable market value. was complete, activated carbon was then
cleaned with aquades and dried using an
METHODS oven at 100° C for thirty minutes. After
Raw Material that, the activated carbon was sieved using
Coconut shell (CS) was selected for ASTM Standard. The Test Sieving has a
the manufacture of activated carbon. The size of 70-200 Mesh. The sieve model
material was cleaned with aquades several used consists of three sieve arrangements.
times to remove dust and dirt. The coconut

RESULT AND DISCUSSION


FTIR Analysis
Table 1. The major wavenumber in regards to the chemical bonding compound value of FTIR
spectra of ZnCl2 and Na2CO3 (Fan, Dai, & Huang, 2012).

Wave number (cm-1) Assignments ZnCl2 Na2CO3


3500-3300 O-H Stretching (intermolecular hydrogen bonded)
2930-2900 C-H Asym. Stretching * *
2720 C-H (aldehydes)
1740 C=O stretching in esters
1625-1610 C=C Aromatic skeletal stretching
1580-1570 C=C stretching band * *
1450-1420 C-H Asymmetric. Bending
1375-1317 C-H Asymmetric. And symmetric. bending
C-O Asymmetric. stretching of aromatic ethers,
1284-1240 esters, and phenols
1260-1000 C-O in carboxylic acids, alcohols, phenols and * *
esters or the P=O bond in phosphate esters
700-400 C-C stretching * *
Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi, 07 (1) (2018) 33-39 35

Figure 1. FTIR of activated carbon of ZnCl2 and Na2CO3

FTIR spectra of the activated carbon cm-1 (Si-O) as the result of silica
of the ZnCl2 AND Na2CO3 samples, containing minerals (Hidayu,
respectively. FTIR spectra contained vast Muhammad, Matali, & Sharifah, 2013;
and strong bands at 3200-3500 cm-1 for Rani, Mohammad, Matali, & Kadir,
hydroxyl (O-H) stretching vibration 2014). The FTIR spectra have confirmed
groups. The structure contains many that activated carbon has been
carbons bonds which also act as a remover successfully converted into carbon (NB,
of hydrogen, and the oxygen atoms of that N, & Y, 2016). For activated carbon, clear
frequency may contain stretching of during the hardening and activation
amines (NH2) and alcohol (OH) groups process, most of the functional group
lost during the activation to 600°C. This adsorption peak is lost. Because the
indicates the dehydration of cellulose and functional groups of the spectrum
lignin components (Shilpi, 2012). feedstock are evaporated as volatile
Meanwhile, the absorption peak at 2900- materials when heat is supplied to the
2850 cm-1 for the stretching vibration sample. This proves that the activation
(CH) of the (-CH) 3 group is completely process has been successfully performed
removed from the activated carbon and the carbon retains some functional
sample. The carbonyl group (C = O) was group of sensitive IR, functional group
observed in samples ZnCl2 and Na2CO3 in (C-O) (Hesas, Arami-Niya, Daud, &
1740- 1700 cm-1 is expected to come from Sahu, 2013).
the lignin network. However, this peak is
virtually non-existent after pyrolysis and Analisis XRD
the immersion activation process with Spectrum X-ray diffraction pattern of
ZnCl2and Na2CO3 because it is volatile. the activated carbon of ZnCl2 and Na2CO3
Peaks ranging from 1200-1000 cm-1 show samples. The diffraction peaks are
the presence of stretching (C-O) and 830 observed at the diffraction angle of 2θ =
36 Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi, 07 (1) (2018) 33-39

29,5o, 34,6o and 39,4o respectively which and 40o-50o which revealed an amorphous
corresponds to silicate minerals, iron ore, structure that was irregularly stacked by
and quartz. While the rest of the other carbon rings and useful for generating an
peaks that are observed at the diffraction adsorbed gap.
angle of 44.5o corresponding to sodalite, For uncarry Carbon, a sharp peak
analcime and sodium silicate, observed at 44,5° may be due to the
respectively (Pradhan, 2011). The two presence of Zn and Na used during the
active carbon samples showed two broad carbon activation process (A.R Hidayu,
diffraction peaks located at 2θ = 30o-40o 2016).

Figure 2. XRD activated carbon of ZnCl2 and Na2CO3

The findings are in accordance with microstructure of the raw ZnCl2 and
previous studies by Kushwaha et al., and Na2CO3. Images of the show that the
Rani et al. (Kushwaha, Padmaja, & activation stage produced an extensive
Sreelatha, 2012). Samples contain two external surface with quite and pores.
broad diffraction peaks and can be The surface topology differed
attributed to the presence of carbon and strongly between raw coconut shell and
graphite (Matali, Khairuddin, Sharifah, & active carbon physical and chemical
Hidayu, 2013). (Roozbeh, 2013). Very high porosity was
observed on the external surface of the
SEM Analysis ZnCl2 and Na2CO3. SEM morphology
Scanning electron microscopy (SEM) shows that visible pores were seen in
was used to observe the surface physical samples of ZnCl2 and Na2CO3, apparent
morphology of the samples. Figure 3 pores indicating activated carbon
shows the SEM images of the processes were successful.
Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi, 07 (1) (2018) 33-39 37

(a)

(b)

Figure 3. Morphology on the surface of activated carbon magnification of 3000x (a) Na2CO3 (b)
ZnCl2
38 Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi, 07 (1) (2018) 33-39

CONCLUSION Procedia Engineering 148, 106–


Activated carbon was produced from 113.
coconut shell through physics activation
of 600oC and chemical activation by Arami-Niya, A., Daud, W. M. A. W.,
immersing it in 10% ZnCl2 activating Mjalli, F. S., Abnisa, F., &
agent. Activated carbon was analyzed by Shafeeyan, M. S. (2012). Production
Fourier TransformationSpectroscopy of microporous palm shell based
Infrared (FTIR)and Xray Diffraction activated carbon for methane
(XRD) methods. adsorption: modeling and
FTIR results show that functional optimization using response surface
groups of spectrum raw materials were methodology. Chemical
evaporated as volatile materials when the Engineering Research and Design,
heat was supplied to samples and 776–784.
immersion activation processes with
Cocommunity, T. (2016). Initiatives
ZnCl2. This proves that the activation
Towards Product Diversification
process has been successfully performed
Seek Out Viable Opportunities in the
and the carbon retains some functional IR
Coconut Industry. Monthly
functional groups, functional groups (C-
Newsletter of the Asian and Pacific
O) until the coconut shell was
Coconut Community, XLVI(8), 1–32.
successfully converted to carbon. The
XRD results confirm the presence of Fan, M., Dai, D., & Huang, B. (2012).
several phases of crystals (graphite) Fourier Transform Infrared
around peaks of 36o and 44o, with two Spectroscopy for Natural Fibers.
broad diffraction peaks and can be Retrieved from
attributed to the presence of carbon and www.intechopen.com
graphite. For non-transported carbon, a
sharp peak observed was at 44.5°. It might Hesas, R. H., Arami-Niya, A., Daud, W.
be due to the presence of Zn and Na used M. A. W., & Sahu, J. N. (2013).
during the carbon activation. In Preparation and Characterization of
conclusion, coconut shell can be utilized Activated Carbon from Apple Waste
as cheap and efficient raw material for the by Microwave-Assisted Phosphoric
production of activated carbon with very Acid Activation: Application in
promising commercial value.The SEM- Methylene Blue Adsorption. Bio
EDS results showed that the Resources, 8(2), 2950–2966.
carbonization of pyrolysis and activation
processes creates porosity and large Hidayu, A. ., Muhammad, N. F., Matali,
surface area for absorption, where the S., & Sharifah, A. S. . (2013).
pores of the coconut shells and the husk Characterization of activated carbon
are still visible, in contrast to CA8 and prepared from oil palm empty fruit
CAZ activated carbon that showed the bunch using BET and FTIR
pores that indicate activated carbon techniques. Procedia Engineering
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Hung, J. J. (2012). The Production of
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