IJSTE - International Journal of Science Technology & Engineering | Volume 6 | Issue 1 | July 2019

ISSN (online): 2349-784X

Isolation and Characterization of Cellulose Oil

Palm Fronds Biomass Residue
Khairunnisah Marpongahtun
PG Student Lecturer
Department of Mathematics and Natural Science Department of Mathematics and Natural Science
Universitas Sumatera Utara Universitas Sumatera Utara

Emma Zaidar
Lecturer
Department of Mathematics and Natural Science
Universitas Sumatera Utara

Abstract
The objective of this work was to isolate cellulose from oil palm fronds (Elaeis guineensis) and its characterization. Isolation using
method combining physical treatment and repeated chemical treatments. Alkali treatments were performed using hydrolyzed with
45% H2SO4, respectively. High levels of cellulose were successfully extracted, with 5 grams of cellulose for every 10 grams of
raw oil palm fronds. The morphology of the cellulose was investigated using scanning electron microscope (SEM). Fourier
transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD) The extracted cellulose was found to have smaller diameter
(59 – 60 nm) and smoother surface compared to the untreated fibers. The results from FTIR, and XRD indicate that the
hemicelluloses and lignin were extensively removed from the isolated cellulose. Alkali treatment helped in removal of
hemicelluloses, while bleaching assisted in delignification. The extracted cellulose showed high crystalline index of 68.75%
resulted from removal of lignin and hemicelluloses via alkali and bleaching treatments. This isolated cellulose fiber has great
properties and can be used in many applications such as reinforcement agent in biocomposite.
Keywords: Cellulose, Oil palm fronds, Chemo-mechanical
________________________________________________________________________________________________________

I. INTRODUCTION

Cellulose is defined as a macromolecule, a nonbranched chain of variable length of 1–4-linked -d-anhydroglucopyranose units. In
contrast, cellulose pulp represents purified cellulosic materials, and still contains other carbohydrates. Cellulose is a naturally
occurring hydrophilic polymer and is the main substance that makes up plant cell walls and contributes to the physical stability of
the cells [1]. Thus, cellulose is probably the most abundantly available organic compound on Earth. Cellulose does not dissolve in
water, and has high crystallinity and high molecular weight and can degraded naturally [2].
Cellulose can be obtained from various sources of natural fiber, one of which is from the palm oil industry. Oil palm plantation
has generated a huge quantity of lignocellulosic resources consistently throughout the year in the form of oil palm trunk (OPT),
empty fruit bunches (EFB), oil palm fronds (OPF) and leaves. The palm fronds was reported to be the largest biomass which makes
up to 70% of the total residues generated from palm oil industry[3]. That contributes to huge amount of agricultural wastes
(lignocellulosic and cellulosic hemibiomass) every year from thinning, replanting and pruning processes[4]. The huge amounts of
waste generated has not been utilized optimally, its usage is only as a boiler fuel, hardening the surface of the road body in the
garden and can usually be burned in the incinerator while the ashes are used as potassium fertilizer, yet the combustion produces
smoke that becomes air pollution and the most common disposal methods for such agricultural waste leaving it to decompose
naturally in the plantation, these case harmful to the environment for a long time [5]. Its necessary to pretend an alternative
environmental friendly way of managing the largely produced agricultural wastes.
Oil palm fronds rich in cellulose could be exploited for many uses and purposes as raw material for the production of cellulose
nanofiber, paper, film, textiles, building material and food additives production and composite. Cellulose found in oil palm fronds
and lignin are 40-50% and 20-21% respectively. Oil palm empty bunches are 43-65%, and 13-37% and oil palm trunk are 29-37%
and 18-23%. [5,6]. The economic potential of these residues are often overlooked. Global production of OPF is approximated to
be 250 MMT (wet weight), to world oil palm cultivation land (13.46 million hectares) reported by Sime Darby Plantation. Recent
studies have shown strong interest in this organic polymer due to its superior characteristics, such as high water absorption capacity
and large surface areas[7].There are several techniques isolation of cellulose nanofiber by mechanically (high pressure,
ultrasonication, ultrafine grinding), chemistry (acid hydrolysis, oxidation, solvents) organic) and enzymatic[8]. Cellulose can be
hydrolyzed,
Recently researchers reported the isolation of cellulose fibers from rice husk by alkali and bleaching treatments, which were
subsequently converted to nanocrystals using a sulfuric acid (H2SO4) hydrolysis treatment[9]. Isolation of microcrystalline
cellulose has been carried out from jute cellulose by using the same acid hydrolysis (H 2SO4) approach[10]. Previous researchers

All rights reserved by www.ijste.org 47

 Isolation and Characterization of Cellulose Oil Palm Fronds Biomass Residue
(IJSTE/ Volume 6 / Issue 1 / 010)

the production of cellulose nanofibre from oil palm empty fruit bunches (EFB) showed that the optimum condition was obtained
by combining chemical and mechanical treatment[11].
The purpose of this study was to isolate the cellulose from oil palm fronds using chemo mechanical treatment combines to
successfully remove lignin and hemicellulose. The physical method used was the ultrafine grinder, while the chemical methods
were alkali and bleaching treatments. Then, the isolated cellulose was characterized using a scanning electron microscope (SEM),
Fourier transmission infrared (FTIR), and X-ray diffraction (XRD).

II. MATERIALS AND METHODS

Materials and Solution Preparation

The material used in this research was Fresh Oil Palm Frond (OPF) were collected from the Indonesian Palm Oil Board North
Sumatera. Chemical reagents used were purchased from Merck with pure analysis (pa), sodium hydroxide (NaOH) and sodium
chlorite (NaClO2). To assist in physical treatment, an ultrafine grinder was used.

Alkaline Treatment
A total of 50 g of refined oil palm fronds powders were inserted into a beaker glass, added with distilled water until it was
submerged and then was stirred at a temperature of 50 oC for 2 hours, then filtered and repeated with the same treatment. The
resulting residue was added with 500 mL of 2% NaOH and stirred at 80 °C for 2 hours. Then, it was filtered and washed until the
filtrate was neutral and repeated with the same treatment resulting an empty palm oil bunch pulp. The resulting pulp was dried in
an oven with a temperature of 50 °C [12].

Bleaching Process
The dried pulp from the alkaline treatment was added with 250 ml of 5% NaOCl and 8-10 drops of glacialCH3COOH while stirred
at 60-70 °C for 1 hour. After that, it was cooled, filtered and washed with distilled water. The resulting residue was added with
250 mL of 0.05N HNO3 while stirred at 70 °C for 1 hour then filtered and washed until the filtrate was neutral. Then, it was heated
with 17.5% NaOH for 1 hour, filtered and washed until the filtrate was neutral. Then, it was bleached with 5% NaOCl to produce
wet alpha-cellulose and finally was dried in an ovento form cellulose fiber gel[11].

Hydrolysis with H2SO4

As many as 2 g of alpha-cellulose was hydrolyzed with 30 mL of 45% H 2SO4 while stirred for 45 min at 45oC. Then, it was
neutralized with distilled water and homogenized for 30 min. After that, it was centrifuged for 2hours at 8000 rpm to separate the
solution with the precipitate. The ultrasonic process was conducted for 2 hours[8].

III. RESULT AND DISCUSSION

The Resulting Cellulose was Analyzed by FTIR Shown in the Figure Below

Fig. 1: The FTIR Spectrum of the isolated cellulose from oil palm fronds:(a) raw oil palm frond, (b) alkali treatment and (c) bleaching
treatment

All rights reserved by www.ijste.org 48

 Isolation and Characterization of Cellulose Oil Palm Fronds Biomass Residue
(IJSTE/ Volume 6 / Issue 1 / 010)

The observed spectrum was dominated by strong peaks that appeared in the area between 3289,233 to 3486.43 cm -1. which showed
stretching of the hydroxyl group (OH) according to the study [10,12]. OH peaks show hydrophilic properties of the main ingredients
of natural fibers such as cellulose, hemicellulose and lignin. Stretching of the saturated C-H aliphatic group is indicated by a
decrease between 2904.83 to 2855,203 cm-1. which marks the methylene groups in cellulose[10]. The sharp peak between
1632,1797 to 1592,646 cm-1 is the characteristic of the ester of the group C = C aromatic carboxylic group.
This peak gradually decreases due to bleaching and hydrolysis has been reduced after hydrolysis and will eventually disappear
after acid hydrolysis. The peak is from 1375 to 1365.51 cm-1 stretching CH3 group from the aromatic hydroxy lignin ring. The
peaks from 1373.26 to 1325.22 cm-1 change shape to asymmetrical C-H from each raw fiber. The raw C-C sample shows the same
peak at 1317 cm-1. The absorption peaks on wave numbers 903 cm-1 and 898 cm-1 found in the samples of oil palm frond and
cellulose samples indicate the presence of C-H groups (close to 900 cm-1 referring to the C-H group). From the FTIR results, it can
be concluded that the cellulose was successfully isolated from oil palm frond.

Morphological Analysis of Celulose

The image from SEM in Figure 2 showed the structure of individual fibre.

Fig. 2: Image SEM of cellulosefibre

Based on the dimensions of the width and length of the fibermorphology diameter that has been done using imageJ application,
it is obtained to range from 60 nm, it can be categorized as cellulose nanofibre. [8] Through the process of acid hydrolysis a large
number of amorphous structures have been successfully removed. [11] It can be observed that the fiber is in the form of individual
fibers and not in bundles. This is caused by mechanical chemo treatment that occurs in OPF during isolation which is successfully
removed by lignin and hemicellulose.

X-Ray Diffraction (XRD)

XRD analysis was carried out to see the changes in the crystallinity of cellulose and nanocerate cellulose. X-ray diffraction can
provide information about the structure of the polymer, including about the amorphous and crystalline state of the polymer. The
curve changes the intensity to 2Ɵ (deg) show in figurer 3.

Fig. 3: XRD from (A) Cellulose fibre, (B) alkali treatmentand (C) bleaching treatment

All rights reserved by www.ijste.org 49

 Isolation and Characterization of Cellulose Oil Palm Fronds Biomass Residue
(IJSTE/ Volume 6 / Issue 1 / 010)

Based on Figure 3, it can be observed that the peak of cellulose fiber is sharper than raw OPF. This indicates that the cellulose
fiber possesses higher crystallinity index in comparison with raw OPF. Broader peaks correspond to more amorphous region as
raw OPF has high amount of lignin and hemicellulose, meanwhile cellulose fiber has sharper peak due to elimination of
hemicellulose and lignin after acid hydrolysis treatment.[12]. The diffractogram was presumed to represent typical cellulose
because it showed a single peak at 2θ = 22° and a shoulder in the region 2θ =19°. The crystallinity index were 68.75% and 24.31%
for cellulose fiber and raw OPF respectively. Which progressively increased. The acid hydrolysis treatment managed to improve
the crystallinity index of the cellulose fiber by 44.44%. This finding complements a previous study on recovery of nanocellulose
from OPF which obtained crystallinity index of 57.7%.[10] Crystallinity index obtained in this study was higher than theirs and
this could be attributed to the time of acid hydrolysis. According to Sheltami et al. [14], the crystallinity level of cellulose is
influenced by removal of amorphous polymers

IV. CONCLUSION

Cellulose was successfully isolated from oil palm fronds using combining method, The images from SEM showed good dispersion
of individual fibers and the cellulose size from the chemo-mechanical treatment and was supported by the results from The XRD
analysis showed increment of crystallinity index of cellulose Improvement were attributed to the removal of hemicellulose and
lignin the OPF samples. The FTIR spectra confirmed the removal of noncellulosic polysaccharides by some shifting and change
in intensities of the peaks. Based on the results obtained, cellulose is suitable to be used for various applications. The isolation of
cellulose from the oil palm fronds could be exploited on a larger scale and serve as a proper practice for agricultural waste
management.

REFERENCES
[1] Abdul Khalil, H. P. S., Hanida, S., Kang, S. C. W. & Nik Fuaad, N. A. (2007). Agro-hybrid composite: The effects on mechanical and physical properties of
oil palm fiber (EFB)/glass hybrid reinforced polyester composites. Journal of Reinforced Plastics and Composites, 26, 203–218.
[2] Abdul Khalil, H. P. S., Ismail, H., Ahmad, M. N., Ariffin, A. & Hassan, K. (2001). Conventional agro-composites from chemically modified fibres. Polymer
International,50, 1
[3] Awalludin MF, Sulaiman O, Hashim R, Nadhari WNAW (2015) An overview of the oil palm industry in Malaysia and its waste utilization through
thermochemical conversion, specifically via liquefaction. Renew Sust Energ Rev 50:1469–1484
[4] Sime Darby Plantation. Palm oil facts and figures. Available online at: http://www.simedarby.com/upload/Palm_Oil_Facts_and_Figures.pdf [accessed
08.12.14] Environmental and physiological factors affecting the succinate product ratio during carbohydrate
[5] Syamani, F. A., Subyakto, S. and Suryani, A. (2015). Changes in oil palm frond fibre morphology, cellulose crystallinity and chemical functional groups
during cellulose extraction phases. Chemistry and Materials Research, 7: 105 –104
[6] Mangonsoekarjo, Manajemen Agribisnis Kelapa Sawit (GadjahMada University Press, Yogyakarta, 2003)
[7] Sabrina, S. M. S., Roshanida, A. R. and Norzita, N. (2013). Pretreatment of oil palm fronds for improving hemicelluloses content for higher recovery of
xylose. Jurnal Teknologi (Sciences & Engineering), 62(2): 39 –42
[8] Owolabi AWT, Ghazali A, Wanrosli WD, Abbas FMA (2016). Effect of alkaline peroxide pre-treatment on microfibrillated cellulose from oil palm fronds
rachis amenable for pulp and paper and bio-composite production. BioResources 11(2):3013–3026
[9] Khalil HPSA, Mohamed SA, Ridzuan R, Kamarudin H, Khairul. A (2008) Chemical composition, morphological characteristics,and cell wall structure of
Malaysian oil palm fibers. Polym Plast Technol Eng 47(3):273–280D
[10] Johar, N., Ahmad, I., & Dufresne, A. (2012). Extraction, preparation and characterization of cellulose fibres and nanocrystals from rice husk. Industrial Crops
and Products, 37, 93–99
[11] Fahma, F. et al. (2010). Isolation, preparation and characterization of cellulose nanofibers from oil palm empty fruit bunch (OPEFB). Cellulose, 17, 977–985,
https://doi.org/10.1007/s10570-010-9436-4.
[12] Jonoobi, M., Khazaeian, A., Md Tahir, P., Azry, S. S., & Oksman, K. (2011). Characteristics of cellulose nanofibers isolated from rubberwood and empty
fruit bunches of oil palm using chemo-mechanical process. Cellulose, 18, 1085–1095
[13] Siro, I. & Plackett, D. (2010). Microfibrillated cellulose and new nanocomposite materials: A review. Cellul., 17(3), 459–494, https://doi.org/10.1007/s10570-
010-9405-y.
[14] Sheltami, R. M., Abdullah, I., Ahmad, I., Dufresne, A. and Kargarzadeh, H. (2012). Extraction of cellulose nanocrystals from mengkuang leaves (Pandanus
tectorius). Carbohydrate Polymers, 88: 772 –779.

All rights reserved by www.ijste.org 50