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Procedia Chemistry 19 (2016) 558 565

5th International Conference on Recent Advances in Materials, Minerals and Environment

(RAMM) & 2nd International Postgraduate Conference on Materials, Mineral and Polymer
(MAMIP), 4-6 August 2015

Synthesis and characterization of activated carbon produced from

kenaf core fiber using H3PO4 activation
M.S. Shamsuddina, N.R.N. Yusoffa,* , and M.A.Sulaimana
a
Faculty of Earth Science, University Malaysia Kelantan, 17600 Jeli, Kelantan, Malaysia

Abstract

Kenaf core fiber (KF) which is an agricultural biomass was used to produce low-cost activated carbon using acidic chemical
activating agent. The aim of this study is to find out the changes occuring in kenaf core fiber during activation with phosphoric
acid (H3PO4). The surface area of the formed phosphoric acid treated kenaf core fiber activated carbon (KFAC) was determined
by physical adsorption of N2 gas. Brunauer, Emmett and Teller (BET) surface area, and micropore volume values were 299.02
m2/g and 0.12 cm3/g, respectively. Fourier transform infrared (FT-IR) spectroscope analysis identified the present of carbonyls,
alkenes and hydroxyls. Field Emission Scanning Electron Microscope (FESEM) image showed gradual formation of pores due to
elimination of volatiles and contaminants. Powder X-ray diffraction (XRD) analysis indicated the appearance of broad diffraction
background revealed predominantly amorphous structure. The proximate and ultimate analysis showed high percentage of carbon
and low percentage of ash which is an indication of a good material for production of porous carbon.
2016
2016TheTheAuthors.
Authors. Published
Published by Elsevier
by Elsevier B.V. B.V.
This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia.
Peer-review under responsibility of School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia
Keywords: Kenaf core fiber; activated carbon; chemical activation; phosphoric acid

1. Introduction

Activated carbons (AC) are made from materials rich in carbon through carbonization and an activation
process. A porous structure and its adsorption properties can be obtained in carbonaceous materials via either
chemical or physical 1 activation. Physical activation involves pyrolysis of the source material at 800C -1000C
to produce charcoal. This is then followed by activation using steam, carbon dioxide (CO 2) or oxygen (O 2).

* Corresponding author. Tel.: +609 947 7000; Ext: 3941; fax: +609 - 947 7012.
E-mail address: nraihan@umk.edu.my

1876-6196 2016 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia
doi:10.1016/j.proche.2016.03.053
 M.S. Shamsuddin et al. / Procedia Chemistry 19 (2016) 558 565 559

Chemical activation involves the impregnation of the precursor material with a chemical activating agent
followed by activation at temperatures of 400C-700C under nitrogen atmosphere 2. Zinc chloride (ZnCl2),
potassium hydroxide (KOH) and phosphoric acid (H 3PO4) are widely used as chemical activating agents. The
activating chemical agents influence the pyrolytic decomposition and inhibiting formation of tar and volatile
matter, thus enhancing the yield of AC3. The dehydration and oxidation characteristics of chemical activation
agent require much lower activation temperature compare to physical activation 4. A comparative study of
chemical (H3PO4) and physical activation using biomass fiber as AC has been reported 5. The research found
that the surface area recorded by physical activation was slightly higher than chemical activat ion but lower in
term of yield production. The carbonization of biomass at high temperature would trigger the emission of
higher greenhouse gaseous (GHG) such as carbon monoxide (CO) and methane (CH 4)6 which is an unfriendly
approach.
There has been remarkable interest in the production of AC due to its adsorptive, environmental, thermal,
electrical and mechanical characteristics7,8. It is proof from previous study that AC is one of the leading industrial
materials due to its well developed pore structure and adsorption properties9,10,11. Recent developments in modern
technologies have resulted in various novel applications of AC. Coal-based AC is the most common adsorbent used,
however, it is costly and not sustainable. Abundant low cost agriculture biomass, which contain high amounts of
natural polymers such as cellulose, hemicellulose, and lignin, are suitable alternative materials to produce low-cost
and green adsorbents with necessary modification to enhance its efficiency 12. Various studies on the production of
AC have been done by applying different agricultural biomass including rice husk 13, grape seed14, rambutan peel15,
kenaf fiber16, maize cob17 and date pit18.
Kenaf (Hibiscus cannabinus, L) is herbaceous annual plant that belongs to the family of Malvaceae. Kenaf
possess two kind of fibers that may be explored to produce AC. The long fiber contain approximately 30% of the
total volume of the plant whereas the short fiber represents the remaining of 70% 19. The stem of kenaf plants
consists of the outer bark (bast) and inner core, both contain fibrous components. Recent studies have demonstrated
the capability of kenaf core and bast fibres to enhance bioremediation 20 and adsorption21 process. There were earlier
studies have been made to produce ACs from the inner cores of kenaf where the first study utilized KOH and CO2
through physicochemical activation22, whereas the other study utilized potassium oxalate (K2C2O4) under different
impregnation ratios23. Both studies have significantly increased the evolution porosity in the carbon matrix. Hence,
the objectives of the present study were to synthesis the AC from kenaf core fiber using H3PO4 as activating agent
and conducted the characterization of elemental analysis, surface area, surface chemistry and morphological
properties.

2. Experimental methodology

2.1. Raw materials

The raw kenaf core fiber (KF) sample was obtained from Lembaga Kenaf dan Tembakau Negara. Phosphoric
acid (H3PO4) (85% acid) and Sodium Hydroxide (NaOH) were obtained from Merck (M) Sdn, Bhd, Malaysia. All
chemicals used in the investigation were of analytical grade.

2.2. Sample preparation

Preliminary washing of the raw materials with hot distilled water were conducted and dried in an oven at 105C
for 24 h to remove all moisture. The dried samples were cut into small pieces, sieved to the size of 500-600 m and
stored in air-tight containers to prevent moisture build up and fungi infections. Chemical activation was carried out
by initially carbonizing the precursor in muffle furnace under inert atmosphere from room temperature to
carbonization temperature of 400C for 1 hour under a closed system. The resulting char was labelled as KFC. The
KFC was subsequently impregnated with 30% ortho-phosphoric acid (H3PO4) with impregnation ratios of 1:4 (w/w)
for 24 h of soaking duration. Next, the sample was filtered using a vacuum pump and dehydrated overnight in an
oven at 105C. The dried sample was then pyrolysed for activation at temperatures of 500C. After the activation
560 M.S. Shamsuddin et al. / Procedia Chemistry 19 (2016) 558 565

period of 1 hour the sample was allowed to cool down to the room temperature. The resultant activated carbon was
labelled as KFAC. KFAC then washed with 1.0 M NaOH and successively rinsed with hot distilled water followed
by cold distilled water until the filtrate reached a stable pH of 6 - 7. The samples were then dried in an oven at 110C
for 24 h. The produced ACs were further crushed and sieved to get the particles size of 200-300 m and were kept
in an airtight container prior to analysis.

2.3. Physical and chemical characterization

2.3.1 Proximate and ultimate analysis

Proximate analysis to determine the moisture content, volatile matters, fixed carbon, and ash residues of the
precursor (KF) was carried out using Thermogravimetric Analyzer (Perkin Elmer TGA7, US). Approximately 30
mg activated carbon were placed in a platinum crucible on the pan of a microbalance and then heated between 22C
and 900C at a heating rate of 10C/min, with constantly weighed. Ultimate analysis was done using the Elemental
Analyzer (Perkin Elmer, Series II 2400) to evaluate the percentage of carbon, hydrogen, and oxygen value was
determined by difference24.

2.3.2 Fesem analysis

Morphological study of raw KF, KFC and KFAC was done using a Zeiss Supra 35VP Field Emission Scanning
Electron Microscope. The samples were mounted onto a FESEM holder with double-sided electrically conducting
carbon-adhesive tabs to prevent the surface of the specimens when exposed to the electron beam. The samples were
then coated with a 20 nm thick layer of gold using a Polaron Equipment Limited model E500, set at a voltage of 1.2
kV (10 mA) and a vacuum 20 Pa for 10 min.

2.3.3 Powder X-ray diffraction study

X-ray diffraction analysis (XRD) was performed on KFAC in order to determine the crystallinity or amorphous
nature. The analysis was performed by Brukers D2 Phaser X-ray diffractometer using Cu-K (=0.15406 ) radiation
source operating under a voltage of 40 kV and a current of 25 mA. The diffraction angle (2) was varied from 10 to
90. The X-ray diffraction patterns were collected with a scan rate of 4.2C/min.

2.3.4 FTIR spectrum study

The surface chemistry of the samples were analysed by identifying the surface functional groups of the samples
using Fourier transform infrared spectroscope (FTIR-2000, Perkin Elmer). The spectra were recorded from 4000 to
500 cm-1 resolution in the mid-infrared region.

2.3.5 Surface area analysis

Nitrogen adsorption at 77 K (liquid nitrogen) was conducted using a Micromeritics ASAP 2020 V3.04H
(Micromeritics) instrument to obtain the adsorption isotherm of the sample. The Brunauer-Emmett Teller (BET)
method was used to calculate specific surface area of the activated carbon from the isotherms. All samples were
degassed at 350C for 6 h prior analysis.
 M.S. Shamsuddin et al. / Procedia Chemistry 19 (2016) 558 565 561

3. Results and discussion

3.1. Raw material characterization

The proximate analysis involves the determination of moisture content, volatile matter, fixed carbon and ash
content of the raw KF. The results of the proximate and ultimate analyses values are shown in Table 1. In view of
the data of proximate analysis, KF shows low moisture content (5.6%), high percentage of volatile matter (77.3%),
average content of fixed carbon (11.0%) and low ash content (6.9%). High volatile matter content usually reduces
the solid yield in the carbonization stage while a low inorganic content is vital due to their abilities to produce a low
ash and high fixed carbon content25. Ultimate analysis showed that raw KF has 50.5% of carbon and 8.47% of
oxygen. Experimental conditions of the carbonization and activation steps are not the only major contribution
towards porous structure of AC but also being influenced by the original nature and structure of the starting
material. High phenolic content in lignin compound of biomass make it important in AC preparation as it leading to
higher carbon yields than those obtained from the two other main macromolecular compounds of biomass: cellulose
and hemicellulose26,27.

Table 1. Proximate and ultimate analysis values of raw KF.

Proximate analysis (%) Ultimate analysis (%)

Fixed carbon 11.00 C 44.02

Moisture content 5.60 H 7.82
Ash content 6.90 N 0.46
Volatile matter 77.30 O 47.42

3.2. Surface morphology

FESEM micrographs of raw KF, KFC and KFAC produced are depicted in Fig. 1(a), 1(b) and 1(c) respectively.
The surface of raw KF as shown in Fig. 1(a) was curly form, highly packed, porousless, and having no cavities. An
early work has been conducted on various concentration of H3PO4 activation using frond waste of Saudi Arabian
date trees (R-PDF)28. The finding found that the surface of R-PDF was curly form resulted from the presence of
cellulose, hemicelluloses and lignin in the raw material without any cracks. However, the surface of KFC as shown
in Fig. 1(b) became rough and some irregular pores started to form due to removal of volatile matter after
carbonization at 400C29. Some anonymous fragments with small pores at early stage of formation were observed as
well on the surface of KFC, which might indicate the residues of tarry substances formed during the carbonization
stage. This was agreed by previous study where the surface porosity of the char products were increased after
carbonization process, resulting in large surface area with small voids on the surface 30. Furthermore, these voids
formation assisted on the decomposition of volatile matter from biomass. Activation at 500C with H3PO4 resulted
in the creation of more pores and a substantial removal of volatiles matter. This has been approved by the well-
developed pores which clearly observed on the surface of the KFAC as shown in Fig. 1 (c). Pore development in the
KFC during pyrolysis was also important as this would enhance the surface area and pore volume of the KFAC by
promoting the diffusion of H 3PO4 molecule into the pores and thereby increasing the H3PO4carbon reaction via
acid hydrolysis processes which would then create more pores31. The glycosidic linkage in hemicellulose and
cellulose will be hydrolyzed by H3PO4 along with the cleavage of aryl bond in lignin32.
562 M.S. Shamsuddin et al. / Procedia Chemistry 19 (2016) 558 565

(a) (b) (c)

Fig 1. Micrograph of (a) KF raw, (b) KFC (Carbonization at 400C) and (c) KFAC (Activation at 500C with H 3PO4)

3.3. Phase analysis

Fig. 2 illustrates the X-ray diffraction (XRD) pattern of the KFAC. Appearance of broad diffraction background
and the absence of a sharp peak reveals a predominantly amorphous structure 33. There are two broad diffraction
background corresponding to 2 = 25 and 2 = 43 in the spectrum. The crystallinity recorded by KFAC is 8.5%
with 91.5% amorphous. This value recorded was closed to previous study which used different lignocellulosic raw
materials34. The study applied oil palm empty fruit brunch (EFBAC), bamboo stem (BSAC) and coconut shell
(CSAC) as activated carbon and their XRD analyses revealed all the synthesized AC in the form of amorphous state
with low crytallinity. Table 2 showed the crystallinity and amorphous percentage in the KFAC with comparing with
AC derived from other lignocellulosic raw materials.

700
600
500
400
Intensity (a.u)

300
200
100
0
10 30 50 70 90
2 Theta

Fig. 2. X-ray diffraction of the KFAC.

Table 2. Crystallinity and amorphous percentage of KFAC and other AC derived from lignocellulosic raw material
Samples Crytallinity % Amorphous % References
KFAC 8.50 91.50 Recent study
34
CSAC 8.19 91.81
34
EFBAC 1.68 98.32
34
BSAC 13.25 86.75
 M.S. Shamsuddin et al. / Procedia Chemistry 19 (2016) 558 565 563

3.4. Fourier transform infrared analysis

The FT-IR spectra of raw KF and KFAC are depicted in Fig. 3. The raw KF and KFAC all displayed bands at
3350-3200 cm-1 representing stretching vibration of O-H in hydroxyl groups. The present of this group in raw and
AC was reported in the previous literature1,35. The raw KF characteristic band at 2907 cm-1 assigned to C-H
stretching indicate the methyl and methylene groups2 and band at 1737 cm-1 correspond to the C=O stretching of the
acetyl group in hemicellulose35. In addition, bands at 1595 cm-1 and 1423 cm-1 of raw KF are indicative of aromatic
compounds (C-C) stretching in the aromatic ring. Bands at 1325 cm-1 and 1235 cm-1 attributed to N-O and C-O
stretching vibration respectively. Other important absorption bands at 1036cm -1 represent C-O stretching36 and 1235
cm-1 associated to the C-O stretching of the aryl group in lignin35. It can be suggested from the spectrum that the
main oxygen groups present in the raw KF are carbonyl, ethers and alcohols group which are normally present in
plant cellulose37. The spectra of the KFAC are different from that of the raw material where many bands disappeared
during the AC preparation including the carbonization and the activation. The band intensities were found to be
dependent on the activation temperature. Elimination of peaks at 2907 cm-1, 1737 cm-1, 1423 cm-1 and 1325 cm-1
indicates decomposition of functional groups present in oxygenated hydrocarbons, reflecting the carbohydrate
structure of cellulose and hemicellulose38,39. The reduction of intensity of band 1235 cm-1 in raw KF to 1218 cm-1 in
KFAC was believed to be due to the alteration of lignin structure containing the ester and ether linkage after the
chemical treatment40. The band at 1737 cm-1 which correspond to C=O stretch in aldehydes, saturated aliphatic
which present only in raw KF is due to thermal instability of aldehyde and ketone groups at high temperature41.
However, introduction of peaks at 766 cm-1 shows formation bending vibration from C (triple bond), C-H from
alkynes which corresponds to COC stretching (ester, ether and phenol) and out-of- plane bending in benzene
derivatives.

Raw KF
100
95
90
T ransmittance %

85
80
KFAC
75
70
65
60
4000 cm-12000
Fig.3500
3. FT-IR 3000 2500(KF)
spectra of raw 1500
and activated (KFAC) 1000 500
kenaf core fiber.

Fig. 3. FT-IR spectra of raw (KF) and activated (KFAC) kenaf core fiber.
564 M.S. Shamsuddin et al. / Procedia Chemistry 19 (2016) 558 565

3.5. Surface area and porosity study

Surface area analysis by BET showed that the carbon synthesized after activation with H 3PO4 (KFAC) had
better surface properties in term of surface area and micropore area compare to carbonized sample (KFC). An early
research has been done on the efficiency of H3PO4 as activating agent in producing activated carbon with surface
area up to 1720 m2/g with impregnation ratio as its significant influence2. It is clearly shown that the dehydration
process by chemical activating agent increase the surface area and porosity42. This could be a good indication of the
H3PO4 impregnation as a catalyst of porosity development. It is supported by previous study that pore structure was
started to be organized on the surface area after H3PO4 activation of precursor due to the release of tars from cross-
linked framework43. Table 3 showed the surface properties values of KFC and KFAC. It demonstrated that KFAC
provide better properties of carbon with BET surface area (299.02 m2/g), micropore area (229.20 m2/g) and
micropore volume (0.12 cm3/g). KFC recorded lower surface properties with BET surface area (13.68 m 2/g),
micropore area (7.16 m2/g) and micropore volume (0.004 cm3/g).

Table 3. Surface properties of KFC and KFAC

Physical properties KFC KFAC
Surface area cm2/g 13.68 299.02
Micropore area m2/g 7.16 229.20
Micropore volume cm /g3 0.004 0.12

4. Conclusion

This study discussed the preparation of activated carbon using H 3PO4 as activating agent. Pore structure and
surface chemistry of the raw KF are altered after being carbonized and activated with dehydration agent. Clear
FESEM image on the changes of surface morphology from raw KF to KFAC indicate the increase of surface area
and pore development after carbonize and acid treatment. The FTIR spectroscopy showed presence of significantly
different peak frequencies of functional group before and after activation. The XRD results confirmed that KFAC
showed less crystallinity with broadness peak due to amorphous nature. BET surface area and porosity increase
from after carbonization and activation.

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