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Mechanical and thermal characterization of bagasse fiber/coconut

shell particle hybrid biocomposites reinforced with cardanol resin

A. Balaji, R. Udhayasankar, B. Karthikeyan, J. Swaminathan, R.

Purushothaman

PII: S2211-7156(20)30034-5
DOI: https://doi.org/10.1016/j.rechem.2020.100056
Reference: RECHEM 100056

To appear in: Results in Chemistry

Received date: 17 April 2020

Accepted date: 6 June 2020

Please cite this article as: A. Balaji, R. Udhayasankar, B. Karthikeyan, et al., Mechanical
and thermal characterization of bagasse fiber/coconut shell particle hybrid biocomposites
reinforced with cardanol resin, Results in Chemistry (2020), https://doi.org/10.1016/
j.rechem.2020.100056

This is a PDF file of an article that has undergone enhancements after acceptance, such
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© 2020 Published by Elsevier.

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MECHANICAL AND THERMAL CHARACTERIZATION OF BAGASSE FIBRE /

COCONUT SHELL PARTICLE HYBRID BIOCOMPOSITES REINFORCED WITH
CARDANOL RESIN

A. Balajia*, R. Udhayasankarb, B. Karthikeyanb, J. Swaminathanc and

R. Purushothamana
a* Department of Mechanical Engineering, A.V.C. College of Engineering,
Mayiladuthurai, TamilNadu, India - 609 305.
b Department of Mechanical Engineering, Faculty of Engineering and
Technology, Annamalai University, Tamil Nadu, India - 608 002.
c Department of Chemistry, A.V.C. College of Engineering, Mayiladuthurai,
Tamil Nadu India - 609 305.

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Corresponding Author Email ID : [email protected]

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Abstract -p
The primary aim of this study is to develop a biocomposite by using biopolymer and natural
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fibers/particles from renewable resources. With the aid of poly-condensation process, the
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cardanol thermoset biopolymer resin from cashew nut shell liquid (CNSL) was synthesized.

The abundantly available, bagasse fiber (20mm of length) and coconut shell particle (50 μm)
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were applied as reinforcement material to produce a new ecological hybrid biocomposite. The
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prepared fiber and particles are treated chemically. Hybrid composites of Cardanol (C)

reinforced with bagasse fiber (BF), Coconut shell powder (CP) and Bagasse fiber / Coconut
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shell powder (BC) were manufactured using a compression moulding process. This four

different kinds of composites, though the sequences are done to have C, C / BF, C / CP, and C /

BC. The mechanical properties of the prepared biocomposites were evaluated through tensile,

flexural and impact test. These evaluation predicts that C/BF possess comparatively more

strength with other hybrid composites. The presence of fiber and particle are attributed in all

the biocomposites using FT-IR spectroscopy analysis. Similarly during thermal analysis, C/BF

corroborate with higher thermal stability than other biocomposites by thermal gravimetric

analysis.
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Keywords : Fiber and Particle-reinforced composites, Hybrid biocomposites, Bagasse fiber,

Coconut shell particle, biocomposites.

Introduction

In the early 1900s, practice of natural fiber /particle as reinforcement in plastics is considered

as uncomplicated one. But it is helpful to get better mechanical and thermal properties of the

bio composites. This material has been recognized across the globe [1]. Nowadays, the need for

natural fibers is considered to be the greatest option for synthetic fibers in the form of growing

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environmental concerns and government policy. [2, 3]. Joshi et al, [4] explored the

explanations why natural fiber / particle composites are eco-friendly compared with glass fiber

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reinforced composites. Possible explanations are that natural fiber composites have a higher
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fiber content for comparable output, minimizing the more populating base polymer content;
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natural fiber manufacturing has a smaller environmental impact relative to glass fiber
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production.

CNSL, a sustainable agricultural fuel and a consequence of the cashew industry, is very
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positive in this path. It is used as a source of unsaturated hydrocarbon phenol, an outstanding

monomer for the manufacture of thermosetting polymers [5]. Cardanol & its variants have been
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tested and used in vast of applications. Cardanol can also be used for polyurethane synthesis in
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conjunction with lignin- compounds with higher mechanical and thermal properties[6].

India is gifted with plenty of natural fiber such as Ramie, Jute, Bagasse, Pineapple, Bamboo,

Coir, Sisal, Banana, etc. Such natural fibers are both reusable and biodegradable by nature and

acquire strong technical merits such as specific strength, low cost, good modulus of elasticity,

low density, increased thermal properties and decreased respirational irritation. It is important

to remember that different varieties of natural fibers are readily accessible in order to show that

the thermoplastic and thermoplastic matrices are efficient and well stabilized [7, 8]. To the
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creation of new biocomposites with enhanced environmental efficiency and mechanical

properties, natural fibers should be changed with appropriate binding agents or by outside layer

with suitable resins to impart hydrophobicity.

Chemical modifications are very much required to customize the fiber interface. Behzad and

Sain [9], proposed a variety of mechanisms for the coupling of materials, namely: (i) the

removal of poor boundary layers; (ii) the construction of a difficult and flexible layer; (iii) the

forming valence bonds between each materials; (iv) the enhancement of wetting among

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substrate and polymer; (v) Construction of an exceptionally cross-linked interphase zone with a

modulus intermediate between the substrate and the polymer; (vi) Surface substratum acidity

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transition. A number of researchers have studied Chemical alteration of natural fibers to
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maximize conformity to the polymer matrix [10]. The various chemical treatments were carried
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out like alkali, acetylation, benzoylation, acrylation, silane etc. Besides that, alkaline treatment
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may be found to be an inexpensive option among all methods[11].

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Throughout recent history, the expansion of composites with reinforcements of two and more

form and shape (fiber / particle) was introduced to account for their shortcomings, ensuing in
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an ambitious hybrid impact [12-14]. Hybrid composites, consisting of more than one
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reinforcement forms with different aspect ratios were designed to improve the mechanical and

thermal properties of the reinforced composite model. This is because of properties of hybrid

composites may be stronger than that of single reinforced composites [15, 16]. Still, minimum

numbers of work have been developed with hybrid composites composed of a biopolymer and

different forms of natural fiber reinforcement.

The aim of our work is to synthesis biocomposite qualitatively and economically using locally

available materials like bagasse fiber and coconut shell particles. It is proposed to achieve by
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preparation of various composite materials viz., C, C/BF, C/CP, and C/BC using cardanol resin

by reinforcing bagasse fiber and coconut shell particles in different combinations. Finally, it is

proposed to analyse the various properties like mechanical, morphological, thermal stability

and chemical configuration of all the prepared biocomposite materials to envisage the

economically and best biocomposite out of all the combinations.

Methods

Materials

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CNSL from Ganesh Chemicals (Pondicherry, India) was used as the basic compound for this

analysis. The Indian Scientific Solution, Mayiladuthurai, Tamil Nadu India, supplied Epoxy

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Polymer (Commercial Name: Bisphenol-A [LY 556]), HY 951 (as a hardener; Commercial
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Name: Araldite) and NaOH (alkaline) Sugar cane bagasse has been chopped down in
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Chidambaram, Cuddalor District, Tamil Nadu, India from a sugar cane juice shop on the
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roadside. Coconut shells are gathered from our own home.

Preparation of Cardanol resin

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Cardanol resin was made from cardanol derived from bio-organic CNSL and formaldehyde in

the existence of sodium hydroxide, a basic catalyst. . Thus the resin was prepared using a
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specific ratio of the CNSL: HCHO: NaOH reactants to the ratio of 1: 1.6 : 0.136 which is
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equivalent to 227 : 48 : 5.43 by weight (grams),[17 ]. CNSL of 227 g was taken in a bottle and

NaOH of 5.43 g were dissolved slower for a period of 30 minutes, using a magnetic stirrer at

300 rpm for the basic catalyst. In a separating funnel, the additional mixture was taken and

stored for one day at room temperature.

Throughout due course of time, a poly-condensation reaction happens, in which a mud-colored

reacting resin was settled down and an unreacted dark brown liquid was present at the top of

the resin. The reactive resin was isolated and stored in a double neck circular bottom flask

with a magnetic stirrer. The resin- flask was held in an oil bath tub and heated to a temperature
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of 100 to 120 ⁰Celsius. This heating process was carried out for three hours in order to improve

its viscosity. Then the resin was collected and cooled down at room temperature. The cardanol

Resin Preparation Set-up for Poly Condensation Process and cardanol resin was shown in Fig.

1 & 2.

Insert Figure 1 & 2

Preparation of fibers and particles

Commercially unusable bagasse fibers and coconut particles were used in this study. Bagasse

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fiber washed with high pressure water for around one to two hours. It helps to remove loose

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bagasse pieces, organic materials and sugar contaminants from the samples. They were dry for
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2 to 3 days in a sun and hot air furnace at 100 ° C for 24 hours to extract moisture from it [18].

Subsequently, the fibers were transversely sliced to 20 mm in length. The coconut shell has
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been dried and grounded into coconut shell powder and then sieved in keeping with the
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standard ASTM NO.170 to 625 mesh sieves. 100 g of the coconut shell particles have been put
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in a series of sieves organized in descending order of fineness and shaken for 15 min, which is

the prescribed period for the full sorting of the particles, which is to be held below the sieves
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[19]. For this analysis, 50 μm particle size was used.

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Alkaline treatment in bagasse fibers and coconut particles

Chemical treatment in the presence of NaOH is essential for the pre-treatment of bagasse fiber

and coconut particles. The bagasse fiber and coconut particles are added to 100 ml of NaOH

solution where the mixture is mixed persistently for 12 hours to partly extract hemicelluloses,

pectin, lignin and wax together with the outer layer of the cell wall [20]. The fibers and the

particles were soaked in purified water and then the fibers and the particles dried in the hot air

furnace at 100 ° C for 24 hours [21]. Figure 3 shows NaOH treated bagasse fiber and coconut

particles.
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Insert Figure 3

Composites Preparation

The biocomposite materials for this study were fabricated by compression moulding process.

In the beginning desired quantity of bagasse fiber (10 wt%), coconut particles (10 wt%) and the

cardanol polymer were taken, the suitable hardener like epoxy (bisphenol-A [LY 556]) and

araldite [HY951] also taken to fabricate the polymer composites. The mixing ratio is 10:1 for

the polymer with the hardener in terms of weight [24]. The size of the mould used in this work

was 300 X 300 X 3 mm. It has been coated with a release agent to keep the composites from

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sticking onto the mould. Thereafter only the mixture can be placed. To confirm the uniform

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distribution of the resin all over the laminate, a pressure of 100 kgf/cm2 has been applied
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gradually on it. It‟s also helps to eliminate the entrapped air [25]. For attaining absolute curing,

the laminate remained kept under same pressure for nearly 2 hours. Table 1 presents various
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compositions.
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Insert Table 1
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Composite Characterizations

Unitek – 94100 (2003) testing machine helps to carried out the tensile and flexural tests of the
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composites with 0 to 100 kN of load range and 5 to 250 mm/min of cross head speed. Those
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two tests were measured according to ASTM D 638 and ASTM D 790 standards respectively.

Five samples from each composite were tested and through that the average results were

reported.

Izod impact test on notched specimen was conducted by following ASTM D-256 standard

using an EMIC pendulum machine. Pendulum weight of 0.6 kg, falling height of 0.125 and

impact speed 3.46 m/s. The standard specimen size is 65 mm× 13 mm × 3 mm with the depth

of „V‟-notch as 2 mm and an angle at 45o. The dial indicator available on the machine shows

the impact energy of various specimens. The impact strength was estimated from the mean
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values recorded for five different specimens. Figure 4 shows the schematic diagram for ASTM

D standards for tensile, flexural and impact specimen.

Insert Figure 4

FT-IR helps to examine the changes in the chemical composition of C, C/BF, C/CP, and C/BC

composites. It displays as the transmittance mode of resolution 4 cm-1 varying from wavelength

500 to 4000 cm-1 with 50 scans and represented by the band intensities by Fourier transform

technique.

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Fracture surface has been captured through SEM. In order to increase the conductivity of thee

sample, a layer of gold coating has been done over the samples before undergone to the SEM

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examination. This gold coat also helps to stops the electrostatic charging during examination.
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In order to compare thermal stability with thermal degradation of prepared bio composites, the
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thermal analysis has been recorded by NETZSCH STA 449F3 facilitated at Department of
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physics, Annamalai University, Annamalai Nagar, Tamil nadu, India. Platinum pan which

holds 10 gm of each sample has been heated with a heating rate of 5 °C/min from 28.5 to 800
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°C at in a nitrogen atmosphere.

Results and Discussion

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FT-IR NaOH treated bagasse fiber and coconut particles

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The FT-IR (Fourier Transform Infrared spectrometer) analyses were carried out for NaOH

treated bagasse fiber and coconut particles and shown in Figure 5. A wide peak about 3430

cm-1 invoke the occurrence of O-H stretching indicates the hydrogen intermolecular bonding of

cellulose and lignin, cross linked phenolic polymers present in fiber and particles [22]. A

medium peak observed at 2920 cm-1 shows the existence of C-H stretching vibration.

Similarly, lignin occurrence is indicated by the existence of carbonyl, C=O group which is

endorsed by a medium peak attained at 1650 cm-1 [23]. Due to C-C stretching, the Weak band

has been seen around 1590 and 1450 cm-1. The presence of C-H bending is indicated by peak
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at 1050 cm-1. The aromatic C-C stretching is presence through the medium band appears

around 850 cm-1, which strengthens the presence of lignin in both fiber as well as particles.

Insert Figure 5

Measurements of bagasse fiber and coconut particles

Bagsse fiber length and coconut particles diameter were measured through Scanning Electron

Microscope (SEM) -JEOL JSM 6610 LV. A total of 8 bagasse fiber numbers were chosen

randomly. Similarly small amount of coconut particles take. Each fiber and particles was put

in a 50X magnification scanning electron microscope. Length and diameter were measured at

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different locations of each and every fiber and particles. To measure the fiber and particles

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dimensions, the image shown in figure 6 is used.

Insert Figure 6
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Tensile Strength
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Effect of tensile strength for the biocomposites as a role of BF, CP and BC reinforcement is
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plotted on Figure 7. Compared with neat polymer composite, the trend shows clearly an
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improvement in tensile strength for fiber and particle reinforcement. The tensile strength

obtained for C, C/BF, C/CP and C/BC composites were 24, 36, 28 and 32 MPa respectively.
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Higher tensile strength was shown to C / BF polymers composites than to C, C / CP and C /

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BC. In general, fiber-reinforced composites have greater tensile strengths compared to particle-

reinforced composites [26]. The tensile strength of C / CP composites decreased somewhat

with the addition of particle loading, thus increasing the interfacial area, and the poor

interfacial bonding between the particle and matrix polymers decreased the strength. Tensile

strength improved slightly with the loading of fiber and particles. Due to fiber's capacity to

withstand stresses transferred from the polymer materials, the strength of the composites is

improved [27].

Insert Figure 7
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Flexural Strength

Figure 8 illustrates the influence of bagasse and coconut reinforcing particles on the

flexural strengths of composites. This result was also comparable with the tensile strength

trend; it had a maximum bending strength of 75 MPa for C / BF composite. Thus, cardanol can

bind well to the bagasse fiber, which will have high flexural strength [28]. The flexural strength

of C / BC composite is 74 MPa, a small decrease owing to incompatibility of the material with

stresses from the polymer matrix.

Insert Figure 8

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Impact Strength

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The impact strength of C / CP (1,75 J) was found to be higher than all other composites,
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contradictory to the above-mentioned mechanical properties. This is due to the impact of

particle absorption compared to fiber. Micro-space between fiber or particle and matrix is
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created due to weak interfacial bonding, contributing to a several micro-cracks where impact
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exists, which easily facilitate crack spread and reduces the impact strength [29]. The
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impact effect is shown in Figure 9.

Insert Figure 9
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Morphological study
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Figure 10 represents the tensile fractured surface on CE, C/BF, C/CP & C/BC composite.

Figure 10a (CE - Composites) shows evidence of absence of fibers, particles and also confirms

there is no voids of fibers. The C / BF sample reveals (Figure 10b) an erratically broken

pattern, which suggests the interfacial zone between fiber and polymer. This material is shown

by trapped fiber, lack of fiber cohesion, lack of voids, and strong adhesion to the fiber-matrix

interface. It contributes to better tensile strength for C/BF (36 MPa) composites [33]. Figure

10c exemplifies the tensile fractured surface of C/CP composite that contains particles revealed

by number of small holes. Consequently, creation of elongate the crack propagation [31, 32].
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Figure 10d shows C/BC composite SEM image, which evidently reveals the particles and fiber

and weak interfacial bonding between particles/fiber and polymer.

Insert Figure 10

FT-IR of Composites

Figure 11 shows the comparative FT-IR spectral analysis of CE, C/BF, C/CP & C/BC

composites. The experimental assignments of FT-IR for important vibrational frequencies are

tabulated in Table 2. A broad peak in the range 3600 - 3400 cm-1 indicates the existence of O-H

stretching representing intermolecular hydrogen bonding of cellulose and lignin, cross linked

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phenolic polymers present in fiber and particles [22] Similarly, C-H stretching vibration has

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been indicated by the observed frequency range 3000 - 2800 cm-1. A powerful band around
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1700 cm-1 strengthens the presence of C = O groups which clearly invoke the acidic functional

cellulose group present in bagasee fiber and coconut shell particles 1 [23, 33]. The medium
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band seen around 1450-1400 cm-1 indicates the existence of C-C stretching vibration. The
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medium band observed at 1250 cm-1 shows the presence of C-H bending vibration in all

composites. A strong band around 800 cm-1 point out the existence of aromatic C-C stretching
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which strengthens the presence of lignin in both fiber as well as particles. A slight deviation
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was found in the region around 3000-2750 cm-1 in C/BF composite compared to other
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composites. Comparing Figure 4 and 11 a band shift around 3600-3400 cm-1 occurs between

coconut shell particles and all the other biocomposites. A broad band occurs in coconut shell

particles whereas sharp peak occurs in all the other biocomposites.

Insert Figure 11 & Table 2

Thermal Analysis

Figure 12 show the weight loss curves for C, C/BF, and C/CP and C/BC polymer composites.

Figure 12 indicates that C / BF composites had a significantly higher thermal stability than the

other three composites. There was no major difference in thermal stability between C&C / BC
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composites. Each and every composites exhibited higher thermal stability up to 65 °C (only 1.5

to 2.5 % weight loss). It was noticed that all laminates showed 20 % weight loss from 300 to

358 °C, due to the initial decomposition of hemicellulose & cellulose the heat of evaporation of

moisture in the sample. The cruel weight loss from 358 to 460 0C is due to the most important

components of cellulose, hemicelluloses and lignin [34]. It was noticed in all the samples in

480 °C temperature region could be viewed as the complete decomposition of all flammable

materials and the formation of char. Decompositions gave the total weight losses of 88, 81,

84.2 and 86.5 wt % of C, C/BF, and C/CP and C/BC composites respectively. C/BF has the

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least weight loss (81%) compared with other composites. The experimental thermal stability is

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pretty higher in bagasse fiber than that of other natural fiber and particles reinforced polymer
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composites described in literature [35]. This suggests that composite C/BF was a well

enhanced level of fiber incorporation.

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Insert Figure 12
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Conclusion
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To achieve the synthesis of economically and eco friendly biocomposite, locally available

materials like bagasse fiber and coconut shell particles were used as binding materials with
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cardanol resin in various combinations. The resultant was the preparation four different
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composites viz, C, C/BF, C/CP and C/BC. Significant studies like mechanical strength

including tensile, flexural, impact strength and tensile fracture analysis of the biocomposite

materials were carried out. The results obtained results from the various analyses were

compared with fiber, particle and fiber/particle composites. The following conclusions were

made through this study.

Among the four composites, the C/BF composite has greater mechanical strength, such as

higher tensile strength and flexural strength than the other three composites. Similarly, C/BC

composite was found to acquire intermediate mechanical properties between C/CP and C/BF.
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With absence of voids, well trapped fiber and good adhesion between fiber matrix

interfaces, C/BF composite has better microscopic view through SEM.

FT-IR analyses reveal the presence of cellulose and lignin, cross linked phenolic polymers

in fiber and particles which strengthens the bonding between fiber and particles with epoxy

resin.

Finally, it was concluded that the C/BF composite holds the superior properties among all

the other different composites prepared.

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Kannan, R. Udhayasankar and A. Haja Madieen. 2019. Study on mechanical and
morphological properties of sisal/banana/coir fiber-reinforced hybrid polymer composites. J
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34. Szcześniak, L., A. Rachocki, and J. Tritt-Goc. 2008. Glass transition temperature and
thermal decomposition of cellulose powder. Cellulose. 15(3):445-451.

35. Barreto, A. C. H., D. S. Rosa, P. B. A. Fechine, and S. E. Mazzetto. 2011. Properties of

sisal fibers treated by alkali solution and their application into cardanol-based biocomposites.
Compos PartA: Appl S. 42(5): 492-500.
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Fig. 1 Cardanol Resin Preparation Set-up for Poly Condensation Process

Fig. 2 Cardanol Resin

Fig. 3 NaOH treated (a) bagasse fiber and (b) coconut particles

Fig. 4 Schematic Diagram for ASTM D standards specimens (a) Tensile, (b) Flexural and
(c) Impact.

Fig. 5 FT-IR of NaoH treated bagasse fiber and coconut particles

Fig. 6 (a) Length measurement of single bagasse fiber (b) Diameter of coconut particles
with scanning electron microscope (SEM).

Fig. 7 Effect of Bagasse fiber and Coconut particles on tensile strength

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Fig. 8 Effect of Bagasse fiber and Coconut particles on flexural strength

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Fig. 9 Effect of Bagasse fiber and Coconut particles on impact strength

Fig. 10 Photomicrographs of composite fracture surfaces of a sample subjected to tensile

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strength, for (a) Cardanol polymer (C), (b) Cardanol bagasse fiber (C/BF), (c) Cardanol
coconut particles (C/CP) and (d) Cardanol bagasse fiber and coconut particles (C/BC).
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Fig. 11 Comparative FT-IR spectral analyses of all the four biocomposites
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Fig. 12 TGA curves for C, C/BF, and C/CP and C/BC biocomposites
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Table 1 Composition of composites

S.No Composites Composition
1. Cardanol (C) Neat Polymer (100 wt%)
2. Bagasse Fiber (C/BF) Cardanol (90 wt%) + Bagasse Fiber (10 wt%)
3. Coconut shell particle (C/CP) Cardanol (90 wt%) + Coconut shell particle (10 wt%)
Cardanol (90 wt%) + Bagasse Fiber (5 wt%) + Coconut
4. Hybrid (C/BC)
shell particle(5 wt%)

Table 2 FT-IR Vibrational frequency assignment for Composites

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S. No. WAVE ASSIGNMENT INDICATIONS

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NUMBER -p
1 3600 -3400 cm-1 O-H group vibration Presence of inter-molecular
hydrogen bonding.
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2 3000 - 2800 cm-1 CH2 stretching vibration In the all the composites
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3 1700 cm-1 C=O stretching vibration Acidic functional group of the

cellulose present in the bagasse
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fiber and coconut shell particles.

4 1450 -1400 cm-1 C-C stretching vibration Both fiber/particles and resin.
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5 1250 cm-1 C-O stretching vibration In all the composites

6 800 cm-1 Aromatic C-C stretching In fiber and particles

vibration
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Highlights
 Effect of natural fiber and particles hybridization on randomly oriented cardanol is
studied by synthesis of biocomposites.
 Four different kinds of biocomposites are prepared by differenct combinations of
locally available materials like bagasse fiber and coconut shell particles.
 Mechanical properties and surface analysis are carried out for all the composites.
 FT-IR analysis and thermal gravimetric analysis were carried out to study the
chemical structure and thermal stability of all composites.
 The resultant of all the analyses predicts cardanol reinforced with bagasse fiber
C/BF is superior among all the other biocomposites.

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