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Extraction and Characterization of Cellulose from Durian Rind

Article · December 2014

DOI: 10.1016/j.aaspro.2014.11.034

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Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243

“ST26943”, 2nd International Conference on Agricultural and Food Engineering, CAFEi2014”

Extraction and Characterization of Cellulose from Durian Rind

Patpen Penjumrasa,e,*, Russly B. Abdul Rahmana,b,c, Rosnita A. Taliba, Khalina Abdand
a
Department of Process and Food Engineering, Faculty of Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
b
Department of Food Technology, Faculty of Food Science and Technology, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor,
Malaysia
c
Halal Products Research Institute, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
d
Department of Biological and Agricultural Engineering, Faculty of Engineering,Universiti Putra Malaysia, 43400 UPM Serdang, Selangor,
Malaysia
e
Department of Food Science and Technology, Maejo University-Phrae Campus, 54140 Phrae, Thailand

Abstract

Cellulose was extracted from durian rind using delignification with acidic sodium chlorite then followed by mercerization
with 17.5% (w/v) sodium hydroxide. Gas pycnometer indicated that density of extracted cellulose was 1.59 g/cm3. Fourier
transform infrared (FTIR) confirmed the removal of non-cellulosic components. The micrograph by scanning electron
microscopy (SEM) displayed non-fibrous components scattered over the surface of durian rind were removed. Most of cellulose
presented a diameter and aspect ratio in the range of 100 - 150 μm and 20 - 25, respectively. In the future, cellulose from durian
rind has a potential to be used as a reinforcement elements in composite materials.

©
© 2014
2014 The
The Authors. Published by
Authors. Published by Elsevier
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/3.0/).
Peer-review under responsibility of the Scientific Committee of CAFEi2014.
Peer-review under responsibility of the Scientific Committee of CAFEi2014
Keywords: Durian rind; cellulose; delignification; mercerization; FTIR; SEM

1. Introduction

Cellulose, the major constituent of all plant materials, forms about half to one-third of all plant tissues and it is
constantly replenished by photosynthesis (Sun et al., 2004; Mandal and Chakrabarty, 2011). It is the main structural
component that confers strength and stability to the plant cell walls (Dufresne, 2006) which is organized into

* Corresponding author.
E-mail address: patpen@phrae.mju.ac.th, p_atp@hotmail.com

2210-7843 © 2014 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/3.0/).
Peer-review under responsibility of the Scientific Committee of CAFEi2014
doi:10.1016/j.aaspro.2014.11.034
238 Patpen Penjumras et al. / Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243

microfibril in the cell wall, interrupted by hemicellulose and surrounded by a lignin matrix. Depending on the type of
plant, most of plant materials consist of approximately 40 - 55% of cellulose, 15 - 35% of lignin and 25 - 40% of
hemicellulose. In the natural plant cell wall, crystalline cellulose is embedded with these substances, which make it
difficult to obtain pure cellulose (Rachtanapun et al., 2012). Chemically, cellulose is a linear natural polymer of
anhydroglucose units linked at the one and four carbon atom by β-glycosidic bond. This is confirmed by presence of
three hydroxyl groups (OH) with different acidity/reactivity, where the secondary OH located at the C-2, and C-3
position, and primary OH located at the C-6 position. It is also verified, by the formation of strong various
intermolecular and intramolecular hydrogen bond (Sun et al., 2004; Mandal and Chakrabarty, 2011). In recent years,
the interest in cellulose based-materials has been increasing due to the demand for renewable resources and growing
on environmental awareness (Mohanty et al., 2005).
Natural cellulose fibers are increasingly being used as reinforcement materials in thermoset and thermoplastic
polymeric matrices instead of glass fiber because of their unique characteristics, such as renewability, low density
and high specific strength (Ochi, 2008). There are several plants such as cotton, wood, bamboo, flax, hemp, sisal,
and jute that are rich in cellulose (Li et al., 2014). However, in the last decade research focusing on the use of
cellulosic waste as filler has growing rapidly. Agro-wastes materials such as coconut husk fibers, banana rachis,
mulberry bark, soy bean, wheat, straw, and soy hulls (Johar et al., 2012) have been studied as a resource in the
production of cellulose fiber. Although a variety of natural fibers were investigated in detail, the use of durian rind
as a natural source for the production of cellulose has not been explored yet.
Durian rind is a plant waste of durian fruit consumption. Durian (Durio zibethinus Murray) is the most popular
fruit in Southeast Asia, particularly in Thailand, Malaysia, Indonesia, and Philippines (Booncherm and Siriphanich,
1991). It is well known as the “king of fruit”. It has been vigorously widened and entrenched into a multidisciplinary
of food processing industries (Foo and Hameed, 2011), but only one-third of durian is edible, whereas the seeds and
the shell become waste (Amid and Mirhosseini, 2012). In the common practice, durian residues are burned or sent to
the landfills, without taking care of the surrounding environment. Meanwhile durian rind was found to provide a
good source of cellulose (Rachtanapun et al., 2012). The aim of this work was to extract cellulose from durian rind
using chlorination and mercerization process and to characterize its cellulose contents.

2. Materials and methods

2.1. Materials

Durian rind was collected from Phatthalung province, Thailand. Reagent-grade Sodium hydroxide (NaOH) and
acetic acid (CH3COOH), and technical-grade sodium chlorite (NaClO2) of 80% purity were purchased from Fisher
Chemicals Sdn. Bhd. (Malaysia).

2.2. Extraction of cellulose from durian rind

Durian rind cellulose was prepared using two steps process according to Tawakkal et al. (2012). The first step is
the production of holocellulose using chlorination method or bleaching process. The durian rind was ground using
grinder. Then 20 g of samples were rinsed with tap water to remove dust and were subsequently soaked with
640 mL in 1,000 mL beaker. Next, 4 mL of CH3COOH, and 8 g of NaClO2 were added to the beaker for every hour
for duration of 5 h where lignin was completely separated from fiber. After that, the sample was left in the water
bath overnight. It was then washed and rinsed with tap water until the yellow color (the color of holocellulose is
white) and the odor of chlorine dioxide was removed. The second step of this process is to convert the holocellulose
to cellulose using mercerization at room temperature. The holocellulose obtained from previous step was added with
80 mL of 17.5% NaOH and the mixture was thoroughly stirred with glass rod. After that, for every 5 min intervals,
another 40 mL of NaOH solution was added into the mixture for 3 times. The mixture was allowed to stand for
30 min, making the total time for NaOH treatment was 45 min and then 240 mL of distilled water was added to the
mixture and allowed to standing for 1 h before filtering. Next, 800 mL of 8.3% NaOH solution was added into
cellulose for 5 min and rinsed with water. Then alkaline cellulose was neutralized by adding 120 mL of 10% acetic
acid. Subject the cellulose in acid treatment for 5 min. Finally, the cellulose was filtered, washed, and rinsed with
 Patpen Penjumras et al. / Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243 239

distilled water until the cellulose residue was free from acid and then dried overnight in vacuum oven at 80 °C. The
weight of cellulose obtained was recorded. Then the percentage of cellulose was calculated as shown in Eq. (1).
Cellulose was kept in air tight container at room temperature and ready for analysis.

‡ŽŽ—Ž‘•‡ሺΨሻ  ൌ ሺʹȀͳሻ ൈ ͳͲͲ (1)

where, W1 = weight of durian rind (g) and W2 = weight of cellulose (g)

2.3. Measurement of density

The density of the untreated durian rind, holocellulose and cellulose were measured using Helium Pycnometer
Micromeritics (AcuuPyc II1340, USA) at equilibrium rate 1.00 psig/min. All samples were tested with 5 purges at
purge fill pressure of 19.5 psig.

2.4. Fourier Transform Infrared Spectroscopy (FTIR)

The change in chemical compositions of untreated durian rind, holocellulose and cellulose were examined by
FTIR (Perkin Elmer, Spectrum One FT-IR Spectrometer, USA) with the attenuated total reflectance (ATR)
technique. All the spectra were recorded in the transmittance mode with a resolution of 4 cm-1 in the range of 4000
to 500 cm-1. Ten scans were averaged for each sample.

2.5. Characterization of morphological feature

The morphologies of the untreated durian rind, holocellulose and cellulose were characterized using scanning
electron microscope (SEM). The samples were sputter-coated with gold. Images were taken at an accelerated
voltage of 5 kV. The dimension of the cellulose after ground with grinder and sieved with test sieve (Retsch, AS 200
digit, Germany) in between 250 μm and 125 μm was calculated using stereo microscope (Olympus, Olympus
SZX12-CCD, USA). The length and diameter of 70 cellulose fibers were selected randomly and measured.

3. Results and discussion

3.1. Yield of cellulose

Delignification with acidic sodium chlorite and mercerization with 17.5% (w/v) sodium hydroxide (NaOH) were
performed to extract cellulose from durian rind. After mercerization process, 33.12 ± 0.108% of cellulose was
obtained. The result shows the similar yield with stalk fiber such as rice, wheat and barley that consist of cellulose
approximately 28 - 48, 29 - 51 and 31 - 45%, respectively and 26 - 43% in bamboo cane fiber (Han and Rowell,
1996).

3.2. Density of materials

The density of untreated durian rind, holocellulose and cellulose were measured without grinding the samples.
Table 1 shows the density of samples and found that the density of sample was increased after each stage due to
chemical process. Alkali treatment or mercerization is a chemical process of exposing natural fibers in an interaction
with high concentration of basic aqueous solution to stimulate sufficient swelling by removing non-cellulosic
components such as lignin, hemicellulose, pectin, waxes and impurities (Goda et al., 2006). These indicated that
amorphous regions were removed leaving behind the crystalline regions and providing crystalline cellulose to
improve its density. The increasing of crystalline regions was also expected to increase their stiffness and rigidity
and also strength due to the regulated and dense molecular structure. In addition, the higher amount of cellulose
increases the Young’s modulus in the crystalline region along the longitudinal direction (Sakurada et al., 1962; Johar
et al., 2012). It was assumed that the mechanical properties of fibers and reinforcing efficiency will be improved
240 Patpen Penjumras et al. / Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243

after treatment (Rong et al., 2001). Sun et al. (2005) reported that density of cellulose crystal are 1.582 and 1.599
g/cm3 for alpha and beta polymorphs respectively because native cellulose of high plants is a mixture of alpha and
beta cellulose, thus the true density of 100% crystalline natural cellulose is between 1.582 and 1.599 g/cm 3.

Table 1. Density of untreated durian rind, holocellulose and cellulose.

Samples Density (g/cm3)
Untreated durian rind 1.46 ± 0.002
Holocellulose 1.48 ± 0.002
Cellulose 1.59 ± 0.005

3.3. Spectroscopy analysis

FTIR spectroscopy is an appropriate technique to establish the variations introduced by different treatments on
the chemical structure of extracted sample (Zuluaga et al., 2009). Fig. 1 shows the FTIR spectra for (a) untreated
durian rind; (b) holocellulose and (c) cellulose.

Fig.1. FTIR spectra for (a) untreated durian rind, (b) holocellulose and (c) cellulose.

The peak near 3400-3200 cm-1 was observed in all spectra, which corresponds to O-H stretching vibration of –
OH group in cellulose molecules as well as intramolecular and intermolecular hydrogen bonds (Sun et al., 2004;
Yan et al., 2009; Tawakkal et al., 2010; Mandal and Chakrabarty, 2011). It was suggested that the peak was
narrower or high intensity for cellulose, which demonstrated that extracted cellulose contained more –OH group
than untreated durian rind and holocellulose. The absorbance at 1602 cm-1 was shown in untreated durian rind and
holocellulose. These results indicated that chlorination could not remove lignin completely. However, this peak
disappeared from cellulose after mercerization due to extraction process that has removed most lignin from
structure. Generally, the band at 1466-1421 cm-1 is attributed to lignin and xylan due to CH3 deformation
(asymmetric) in lignin as well as CH2 bending (Mahato et al., 2013) and this peak was found in extracted cellulose
as shown in Fig. 1. However, Mahato et al. (2013) also reported that the band at around 1430 cm-1 to the scissoring
motion of cellulose I and band at around 1420 cm-1 to the cellulose II. The band around 1313 cm-1 in spectra of
cellulose can be attributed to CH2 wagging vibration in cellulose and the band around 1155 cm-1 was representative
of anti-symmetric bridge stretching of C-O-C groups (Spiridon et al., 2010). Moreover, the FTIR spectrum shows a
peak of 1237 cm-1 for untreated durian rind which indicated C-O stretching vibration of acetyl group of lignin and
similar peak was also illustrated at 1239 cm-1 in holocellulose. However, this peak absented after mercerization
 Patpen Penjumras et al. / Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243 241

indicated that lignin was removed completely (Tawakkal et al., 2010). Holocellulose and cellulose gave spectrum
around 1425 cm-1 which was attributed to the CH2 bending. The band at 892 cm-1 was referred to the glycosidic C-H
rock vibration which was characteristic of cellulose structure (Li et al., 2014). These results indicated that cellulose
molecule was not removed during extraction using chemical treatments both of delignification and mercerization
stages. The main peaks for each sample are concluded in Table 2.

Table 2. Peak absorption of samples at different stages of treatment.

Band position (cm–1)
Untreated Delignification Mercerization Involved group References
durian rind (holocellulose) (cellulose)
3281 3319 3338 Strain O-H Mandal and Chakrabarty (2011);
Tawakkal et al. (2010
1367 1361 1364 Strain C-H cellulose, hemicellulose Sun et al. (2005)
1315 1313 1313 CH2, cellulose, hemicellulos Xu et al. (2013)
1016 1015 1027 C-O Stretching in cellulose Spiridon et al. (2010)

3.4. Morphology analysis

The visual macroscopic evaluation of durian rind after each stage of treatment is shown in Fig. 2. The
effectiveness of process was observed through its color changes where the brown color of untreated durian rind was
changed to white color after neutralization with acidic solution in mercerization stage as shown in Fig. 2(c). The
white color of final product was a clear indication that almost pure cellulosic material has been recovered and agreed
with FTIR spectra results.

Fig. 2. Photographs of (a) untreated durian rind; (b) holocellulose and (c) cellulose.

Fig. 3 shows the micrographs of untreated durian rind, holocellulose and cellulose. The difference between the
untreated durian rind, holocellulose and cellulose was observed based on the reduction in diameter for each stage.
The size reduction was mainly attributed to the separation of the fiber’s primary cell wall due to the removal of
lignin after bleaching and hemicellulose after mercerization. The micrograph of untreated durian rind also
demonstrates the amount of non-cellulosic components scattered over the surface (Mandal and Chakrabarty, 2011).
An important consequence of diameter reduction was the increasing of aspect ratio (L/d, L is the length and d is
diameter), which should provide higher reinforcing ability of the cellulose for composite application (Johar et al.,
2012). The diameter distribution and aspect ratio of 70 samples of cellulose extracted from durian rind are shown in
Fig. 4. Most particles displayed a diameter and aspect ratio in the range of 100 - 150 μm and 20 - 25, respectively.
Generally, aspect ratio has to be superior to 10, which is considered as the minimum aspect ratio for good strength
transmission for any reinforcement (Bourmaud and Pimbert, 2008). In this study, all of cellulose fibers obtained had
an aspect ratio superior to this value.
242 Patpen Penjumras et al. / Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243

Fig. 3. Scanning electron micrograph of (a) untreated durian rind; (b) holocellulose and (c) cellulose.

Fig. 4. Distribution of (a) diameter and (b) aspect ratio for cellulose collected between 250 μm and 125 μm test sieves.

4. Conclusions

Extraction of cellulose from durian rind using two steps of chlorination and mercerization process was done
successfully. Non-cellulosic components were removed. Extracted cellulose presented a density of 1.59 g/cm3. The
spectrum of cellulose confirmed the removal of non-cellulosic components by loss of peak at 1237 cm-1 which
indicated C-O stretching vibration of acetyl group of lignin. The color was changed from brown to white and the
micrograph of cellulose showed the removal of non-cellulosic component scattered over the surface. The diameter
presented in range of 100 - 150 μm and aspect ratio in range of 20 - 25 which is higher than minimum aspect ratio
value for good strength transmission for any reinforcement materials. Therefore, cellulose from durian rind can be
used as reinforcement elements in composite materials such as the adding of cellulose as fillers to polylactic acid
(PLA) to enhance its mechanical property.

Acknowledgements

The authors would like to thank to The German Academic Exchange Service (DAAD) and Southeast Asian
Regional Center for Graduate Study and Research in Agriculture (SEARCA) for providing financial supporting for
this research.
 Patpen Penjumras et al. / Agriculture and Agricultural Science Procedia 2 (2014) 237 – 243 243

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Accepted for oral presentation in CAFEi2014 (December 1-3, 2014 – Kuala Lumpur, Malaysia) as paper 98.

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