International Journal of Polymer Analysis and

Characterization

ISSN: 1023-666X (Print) 1563-5341 (Online) Journal homepage: http://www.tandfonline.com/loi/gpac20

Extraction and characterization of alkali-treated

red coconut empty fruit bunch fiber

K. J. Nagarajan & A. N. Balaji

To cite this article: K. J. Nagarajan & A. N. Balaji (2016) Extraction and characterization of
alkali-treated red coconut empty fruit bunch fiber, International Journal of Polymer Analysis and
Characterization, 21:5, 387-395, DOI: 10.1080/1023666X.2016.1160814

To link to this article: https://doi.org/10.1080/1023666X.2016.1160814

Accepted author version posted online: 03

Mar 2016.
Published online: 02 Apr 2016.

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INTERNATIONAL JOURNAL OF POLYMER ANALYSIS AND CHARACTERIZATION
2016, VOL. 21, NO. 5, 387–395
http://dx.doi.org/10.1080/1023666X.2016.1160814

Extraction and characterization of alkali-treated red coconut

empty fruit bunch fiber
K. J. Nagarajan and A. N. Balaji
Department of Mechanical Engineering, K.L.N. College of Engineering, Pottapalayam, Tamil Nadu, India

ABSTRACT ARTICLE HISTORY

This article discusses the extraction and characterization of new natural fiber Submitted 18 February 2016
extracted from red coconut empty fruit bunch. The physicochemical, Accepted 1 March 2016
mechanical, and thermal properties of alkali-treated red coconut empty fruit KEYWORDS
bunch fibers (ARCEFBFs) were reported and compared with other natural FTIR; mechanical properties;
fibers for the first time. Cellulose content (65.02 wt%), wax (0.32 wt%), density physicochemical properties;
(1.421 g/cc), and tensile strength (1299.49 MPa) were identified in ARCEFBFs. red coconut empty fruit
Fourier transform infrared spectroscopy and X-ray diffraction analysis bunch fibers; TGA analysis;
confirmed that ARCEFBFs are rich in cellulose content with crystallinity index XRD
of 53.6%. Thermogravimetric analysis revealed that these fibers are thermally
stable until 270.48°C.

Introduction
Nowadays, eco-friendly natural-fiber composite materials are used in many static and dynamic
applications like aerospace, construction, sports equipment, food packaging, and automotive
industries because fiber is biodegradable, little energy is needed for production of fibers, its low
density, it has properties that lower the level of hazards in manufacturing processes, and low cost
compared to synthetic fiber.[1] However, natural fibers have some drawbacks such as low mechanical
properties and low thermal properties compared with synthetic fiber and its incompatibility with
polymer matrix.[2–5] These kinds of problems are resolved using fiber surface treatment.[6] Natural
fibers are extracted from various parts of plants such as stem (bamboo and elephant grass), leaves (sisal
and sansevieria), seeds (cotton), fruits (coir), fruit bunch (palm and banana), and so on.[7] Natural
fibers contain cellulose fibrils inbuilt in lignin matrix. These cellulose fibrils offer better mechanical
properties.[8] The strength of reinforcement of natural fiber depends on its cellulose character and
crystallinity.[9] Fibers extracted from palm tree empty fruit bunch proved as excellent reinforcements
in polymer matrices.[10] The newly identified red coconut empty fruit bunch fiber, which is the waste
product of the red coconut tree, has not been investigated until now despite its presence worldwide and
abundance in South Asian countries. The coconut tree is a member of the family arecaceae (palm
family). It is grown in more than 90 countries of the world, with a total production of 62 million tons
per year.[11] It is the only accepted species in the genus Cocos. The coconut tree produces edible,
pod-like fruits, and oil that are extensively used in various cuisines around the world. The tree can
produce an annual fruit yield in the range of 300–500 per tree and the fruit production is estimated
to exceed 300,000 tons annually in India.
Concerning the above, this investigation involves the study of extraction of fibers from red coconut
empty fruit bunch and provides comprehensive information about the physicochemical properties,
mechanical properties, crystalline index, crystallite size, and thermal stability of ARCEFBFs using
techniques such as chemical analysis, mechanical analysis, Fourier transform infrared spectroscopy

CONTACT A. N. Balaji balajime@yahoo.com Department of Mechanical Engineering, K.L.N. College of Engineering,

Pottapalayam 630612, Tamil Nadu, India.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/gpac.
© 2016 Taylor & Francis
388 K. J. NAGARAJAN AND A. N. BALAJI

(FTIR) spectroscopy analysis, X-ray diffraction (XRD) analysis, and Thermogravimetric analysis
(TGA) in comparison with other natural fibers.

Materials and methods

Materials
Red coconut empty fruit bunch was collected from the red coconut tree garden in Coimbatore
District, Tamil Nadu, India.

Fiber extraction
The fibers were extracted from the red coconut empty fruit bunch by retting method. The collected
empty fruit bunch remained in distilled water for 1 wk. The fibers were extracted by removing the
outer layer of red coconut empty fruit bunch after the degradation process. The extracted fibers were
washed in distilled water thoroughly more than five times to remove any pulp adhering them. They
were then dried in sunlight for about 6–7 h to remove the moisture. Figure 1 shows the extraction
process of red coconut empty fruit bunch fibers.

Alkali treatment
Alkali treatment of natural fibers promotes the ionization of the hydroxyl group to the alkoxide and
improves mechanical properties. The red coconut empty fruit bunch fibers were treated with 5%
sodium hydroxide (NaOH) solution over a period of 60 min at 30°C to distribute hydrogen bonding
in network structure and remove certain amount of debonding content such as wax and oils from the
fiber surface.[12,13] Then the fibers were washed several times with distilled water to remove all traces
of NaOH from the fiber surface. The washed fibers were dried at room temperature for 72 h.

Physicochemical properties
The chemical composition of the ARCEFBFs in terms of the cellulose, lignin, and wax content was
determined using standard test methods. The percentage of wax content of ARCEFBFs was quantified

Figure 1. Extraction process of red coconut empty fruit bunch fibers (a) red coconut tree (b) red coconut empty fruit bunch, and
(c) red coconut empty fruit bunch fibers.
 INTERNATIONAL JOURNAL OF POLYMER ANALYSIS AND CHARACTERIZATION 389

by the Conrad method.[14] The moisture content of the ARCEFBFs was evaluated with an electronic
moisture analyzer (Sartorius, Model MA45). The density of ARCEFBFs was determined using the
Mettler Toledo xsz05 balances method, and the diameter of about 20 fibers was determined using
an air-wedge micrometer.[15]

Mechanical properties
The mechanical properties of the single ARCEFBFs were measured at room temperature according
to the ASTM D 3822 standards, using an Instron 5500 R universal testing machine. The load was
measured with 1 kN at a loading rate of 5 mm/min for 70-mm gauge length.[16,17] Twenty single
ARCEFBFs were tested and the average value was reported.

XRD analysis
X-ray powder diffraction (XRD) is a rapid analytical technique majorly used for phase identification of
a crystalline material and can provide information on unit cell dimensions. The powdered samples of
ARCEFBFs were subjected to XRD analysis in X’Pert-Pro diffractometer system with monochromatic
Cu Kα radiation wavelength of 0.154 nm to determine the crystallinity index (CI) and crystallite size of
the ARCEFBF. The XRD analysis was carried out in (2h) range of 10°–81°. The crystallinity index (CI)
of the ARCEFBF was calculated using the Equation (1):[18]
Ic Iam
CI ¼ � 100 ð1Þ
Ic

where Ic represents maximum intensity of the peak (2,0,0) that contributes to crystalline fraction and
Iam represents minimum intensity of the peak (1,1,0) that contributes to amorphous fraction.
The crystallite size (L) of the ARCEFBFs was calculated for the crystallographic plane (2,0,0), using
Scherrer’s formula [Equation (2)]:[19]
Kk
L¼ ð2Þ
b cos h

where k is the Scherrer constant (0.84), k is the X-ray wavelength (0.154 nm), b is the peak’s full-width
at half-maximum, and h is the Bragg angle.

FTIR analysis
Shimadzu spectrometer (FTIR-8400S, Japan) was used to derive the FTIR spectra of the powdered
samples of ARCEFBFs in potassium bromide (KBr) matrix with a scan rate of 32 scans per
minute at a resolution of 2 cm 1 in the wave number region 4000–400 cm 1 at atmosphere room
condition.[20] FTIR spectra are used to find out the free functional groups present in ARCEFBF.

Thermogravimetric analysis
Thermal stability behavior of the ARCEFBFs was analyzed by TGA using Jupiter thermal analyzer
(Model STA 449 F3, NETZSCH, Germany). The TGA analysis was carried out to measure the
degradation characteristics of ARCEFBFs in nitrogen atmosphere for preventing oxidation
effects at a flow rate of 20 ml/min. The measurement were examined with alumina crucible in the
temperature range of 30–500°C at a heating rate 10°C/min.[21]
390
Table 1. Comparison of physicochemical and mechanical properties of ARCEFBFs with other natural fibers.
Chemical properties Physical properties Mechanical properties
Crystal Young’s Tensile Elongation
Cellulose Hemicellulose Lignin Wax Moisture Density Diameter CI size modules strength at brake
Natural fiber (wt%) (wt%) (wt%) (wt%) (wt%) (g/cc) (µm) (%) (nm) (GPa) (MPa) (%) Reference
ARCEFBFs 65.02 — 15.82 0.34 14.14 1.421 90–109 53.6 6.46 4.887 1299.49 4.45 Present work
Coir 43 0.3 45 — — 1.2 — — — 4–6 175 30 [22–24]
Bamboo 26–43 30 21–31 — — 0.60–1.10 — — — 11–17 140–230 — [22]
Ramie 76 15 1 — — 1.5 — — — 24.5 560 2.5 [22]
Sisal 78 19 8 2 11 1.5 50–300 55 16.99 9.4–22 511–635 2.0–2.5 [23,24]
Cotton 85–90 1–3 0.7–1.6 — 1.0 1.6 — 68 5–7 5.5–12.6 287–597 — [24]
Flax 85 9 4 1.7 10 1.5 — 70 5.4 61.4–128 400–938 3.6–3.8 [23,24]
Ferula 53.3 8.5 1.4 — — — — 48 1.6 52.7 475.6 4.2 [23]
Hemp 58.7 14.2 6 0.8 9 1.47 — 80 4.5 70 690 2.0–4.0 [23,24]
Jute 58–63 20–24 12–15 0.5 12.6 1.3 40–350 65.8 29.25 10–30 400–773 1.5–1.8 [23,24]
Althea 44.6 13.5 2.7 — — — — 68 2.4 65.4 415.2 3.9 [23]
Borassus 53.4 29.6 17.0 — — — — 38.4 — 10.8 34.8 34.8 [26]
Century 71.65 22.24 6.09 — — — — 53.2 — 8.6 275 3.4 [29]
Mendong grass 72.14 20.2 3.44 — — — — 58.6 14.3 17.4 452 — [24]
Rice straw 64 — 8 — — — — 57 3.75 26 450 — [24]
Thespesia 60.63 26.64 12.70 — — — — 48 — 61.2 573 0.79 [27]
Napier grass fiber 47.12 31.27 21.63 — — — — 62.4 2.83 13.15 88.40 0.99 [25]
strands
 INTERNATIONAL JOURNAL OF POLYMER ANALYSIS AND CHARACTERIZATION 391

Results and discussion

Physicochemical and mechanical properties
The physicochemical and mechanical properties of ARCEFBFs compared with other natural fibers are
provided in Table 1.[22–28] The cellulose content of ARCEFBFs was found to be 65.025 wt%, which is
higher than other natural fibers like coir, bamboo, ferula, hemp, jute, althea, Borassus, rice straw,
Thespesia, and Napier grass fiber strands. In general, tensile strength and Young’s modules of fibers
increase with an increase in the cellulose content.[29] Higher lignin content (15.82 wt%) of ARCEFBFs
keeps water in the fiber and acts as protection against biological attack and potentially contributes to
the fiber structure, properties, and morphology.[29] The wax content of ARCEFBFs was only 0.32 wt%,
which is lower compared to the wax content found in other natural fibers like sisal, flax, hemp, and
jute, and may provide better interfacial bond between fiber and polymer matrix. The density of the
ARCEFBFs was 1.427 g/cc, which is significantly low in comparison with ramie, sisal, cotton, flax, and
hemp fibers. The diameters of the ARCEFBFs changes from 90 to 109 µm, with an average value of
99 µm, which is almost the same as other natural fibers. The tensile strength of ARCEFBFs was found
to be 1299.49 MPa with 4.45% of strain rate and Young’s modulus of ARCEFBFs exhibited 4.887 GPa,
respectively. From the Table 1, it can be seen that the tensile strength of ARCEFBFs was higher than
that of other natural fibers.

XRD analysis
The X-ray diffractogram of the ARCEFBFs is shown in Figure 2. It can be observed that minimum
intensity of the peak (1,1,0), that corresponds to the amorphous fraction (Iam) occurred at 2h ¼ 19.2°
and maximum intensity of the peak (2,0,0) that corresponds to crystalline fraction (Ic) occurred at
2h ¼ 21.9°. The peak at 2h ¼ 19.2° indicated the presence of non-cellulosic materials like hemicellulose,
amorphous cellulose, and lignin in the fiber, whereas the peak at 2h ¼ 21.9° indicates the content of
cellulose in fiber.[30] The estimated crystallinity index (CI) for the ARCEFBF was 53.6%, which is higher
than for the ferula, Borassus, century, and Thespesia, and lower than for jute and hemp.[22–28] The
peak’s full-width at half-maximum (b) and Bragg angle (h) of the ARCEFBF is 0.020 rad and
0.1911 rad. Using Scherrer’s equation [Equation (2)], the crystallite size (L) of ARCEFBF was found

Figure 2. X-ray diffractogram of ARCEFBFs.

392 K. J. NAGARAJAN AND A. N. BALAJI

to be 6.46 nm, which is higher than for cotton, flax, ferula, hemp, althea, rice straw, and Napier grass
fiber strands.[22–28]

FTIR analysis
Fourier transform infrared spectra with the classical peaks of ARCEFBFs are presented in Figure 3.
The unique features of the ARCEFBFs spectrum are due to its contents such as lignin, cellulose,
and hemicelluloses. The spectra exhibit peaks at 3436, 2925, 1747, 1645, 1502, 1456, 1257, and
1076 cm 1. The strong and broad peaks at 3436 cm 1 are associated with the hydrogen-bonded
O–H (alcohol group) stretching vibration of the hydroxyl groups in cellulose molecules. The peak
at 2925 cm 1 represents the C–H stretching vibration of alkyl groups in aliphatic bonds of cellulose
and hemicellulose.[31] The absorption peak at 1747 cm 1 refers to C=O stretching vibration of alpha
keto carboxylic acid in lignin or ester group in hemicellulose-saturated aliphatic functional group.
The medium peak at 1645 cm 1 refers to the presence of absorbed water confirming the hydrophilic
nature of the fiber.[32] The C–C band of ARCEFBFs fiber represents aromatic vibration at 1502 cm 1
from methoxyl groups of lignin. The peak signal at 1456 cm 1 indicates the C–H bend of alkenes.[33]
The intensity peak at 1257 cm 1 represents C–O stretching of acetyl group in lignin and hemicellu-
loses. The medium peak signal at 1076 cm 1was due to C–N stretching of aliphatic amines.[34]

Thermogravametric analysis
Thermal stability of the ARCEFBFs was investigated by thermogravimetric method. Figure 4 shows the
TGA thermogram of ARCEFBFs. The initial degradation was observed between room temperature
and 120°C due to evaporation of moisture content from ARCEFBFs, at which stage a minor mass
loss (5.2%) occurred. The second stage of degradation progressed from the temperature region of
225–372°C, in which a peak quite close to 270°C related to thermal depolymerization of hemicelluloses
with mass loss of 7.3%. A very predominant peak at 372°C showed a major mass loss of about 54% due
to degradation of cellulose. From the TGA curve it can be clearly observed that the ARCEFBFs are
thermally stable up to 270°C, which is higher than for other natural fibers like ferula, bamboo, okra,
althea, piassava, and artichoke.[22] The final region from 372 to 500°C indicated the consequence of
oxidative degradation of charred residue.

Figure 3. FTIR spectrum of ARCEFBFs.

 INTERNATIONAL JOURNAL OF POLYMER ANALYSIS AND CHARACTERIZATION 393

Figure 4. TGA thermogram of ARCEFBFs.

Conclusion
In this investigation, the physicochemical properties, mechanical properties, crystalline characteristics,
and thermal analysis of ARCEFBFs were studied. From the investigation, the following conclusions
were drawn: The tensile properties of the ARCEFBFs appear superior to those of other natural fibers
due to higher cellulose content and study results confirmed that ARCEFBF is one of the best alterna-
tives for synthetic fibers in composite structures. The wax content and density of the ARCEFBFs are
low compared to other natural fibers; due to this ARCEFBFs make an alternative material in manufac-
turing lightweight polymer composite products. The ARCEFBFs exhibited better crystallinity index
and crystalline size compared to other natural fibers and therefore provide good mechanical properties
and reduced moisture absorption and chemical reactivity. The thermal analysis of the ARCEFBFs
showed that they are thermally stable up to 270°C and, hence, suitable as reinforcement in thermoset
polymers. In addition, the results of the investigation proved that ARCEFBFs are versatile and have
engineering potential as effective reinforcement in polymers to produce lightweight and low-cost
products with high strength for industrial applications, automobile applications, building construc-
tion, consumer articles, and sports utensils.

Acknowledgment
The authors are grateful for the support rendered by the Management of K.L.N. College of Engineering.

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