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To cite this article: Banchamlak Bemerw, Bewuket Teshome, Magdi Gibril & Fangong Kong
(2021): Development of Papyrus Fiber Reinforced Natural Rubber Composite for Shoe Sole,
Journal of Natural Fibers, DOI: 10.1080/15440478.2021.1875375
Article views: 44
Introduction
An outsole is the foundation of a shoe, it provides comfort and protection for the foot against the
ground roughness. Normally, it could be made out of wood, leather, and rubber. Recently petroleum
resins such as PU, PVC, EVA, and synthetic rubbers are used. The production of these materials affects
the environment as well as increase landfill (Hasan, Rashid, and Arefin 2015).
CONTACT Magdi Gibril magdi.gibril@gmail.com State Key Laboratory of Biobased Material and Green Papermaking, Qilu
University of Technology, No. 3501 Daxue Rd., Changqing District – Jinan, Shandong, China.
© 2021 Taylor & Francis
2 B. BEMERW ET AL.
Natural rubber (NR) is called the supreme agricultural colonist of all time. Originally it is
indigenous from the amazon valley forest but also cultivated principally in southeast Asia,
(Abraham et al. 2013; Rippel et al. 2005). Natural rubber is a high molecular weight polymer of
isoprene which is found in rubber latex in the form of an aqueous dispersion. Latex particle size is
varying approximately from 0.05 to 3 µm (Jiménez Saelices, Save, and Capron 2019). The latex
constitutes rubber 30–40%, proteins 1–1.5%, resin 1.5–3.0%, minerals 0.-0.9%, carbohydrate
0.8–1.0% and water 55–70% (Riyapan, Riyajan, and Kowalczyk 2015). Specific density of fresh NR
latex is 0.96– 0.98 g/cm−3. Its pH varies from 6.5 to 7.0 (Nakamura et al. 1990; Phomrak et al. 2020).
NR hardens below 0 °C and softens and weakens above 800°C, losing its strength and becoming tacky.
In between these temperatures, it can flow under stress and permanent deformation occurs under
prolonged strain (Huneau 2011; Toki et al. 2009). These undesirable properties are reduced by
vulcanization (Anand, Varghese, and Kurian 2015; Long 2005). The cross-linking increases the useful
temperature range of rubber and hardens it. The rubber becomes much stronger and does not creep
while returns to its original shape upon release of stress (Adili et al. 2012; Tang et al. 2019). Besides,
surface properties will be improved and its solubility will decrease. Sulfur is the most important
vulcanizing compound for natural rubber (Moonlek and Saenboonruang 2019; Parra et al. 2005).
Vulcanized rubber is used for several applications from tires to shoe soles. However, natural rubber
showed limited mechanical properties, to overcome this challenge particulate fillers are used. The
presence of fillers leads to an increase in modulus, strength, abrasion, and tear resistance (Moonlek
and Saenboonruang 2019; Stelescu et al. 2014). However, NR is often reinforced by fillers such as
carbon black, silica, and synthetic fibers. Those fillers are unsustainable and major pollutant to the
environment. Consequently, the application of natural fibers to reinforce rubber is the subject of many
reports due to their economic and environmental benefits. For example, sisal and oil palm fibers
reinforced NR composite resulted in a material having good mechanical properties (Datta, Parcheta,
and Surówka 2017). Kenaf fiber was also used as a reinforcement for NR resulting in better mechanical
properties (Long 2005; Moonlek and Saenboonruang 2019). Also, short fiber reinforced rubber
composites can be used where large deformation is not desirable (Stelescu et al. 2014).
Papyrus fiber was also reported as reinforcement in natural rubber composite in a limited number
in literature. Cyprus papyrus is one of the 600 families of Cyperaceae species, found in African
wetlands especially around the Nile river and Victorian lake (Egypt, Ethiopia, Sudan, and Uganda)
(Viji, Sivadas, and Pandurangan, 2014). It is a cellulosic fiber used for making ancient paper, boats,
mats, baskets, and the root for fuel and food (Opio et al. 2014). Papyrus plant needs 6 to 12 months for
harvesting. It grows to about four meters high and has a tall, green triangular shaped stem, which is
wide at the base and tapers to the top as shown in Figure 1a. Its stem is approximately five to eight
centimeters thick (Borojevic and Mountain 2013). Papyrus fiber was reported as reinforcement in NR
for particleboard. A thermal insulation value was found close to the commercial thermal insulation
board. It is also used as a reinforcement for polylactic acid (Morrison et al. 2014; Nishino, Hirao, and
Kotera 2007). Papyrus plants as a sustainable cheap source of natural fibers, that have a better stiffness
per weight than glass, which results in lighter components, this form alternative for the most widely
applied synthetic fibers in the field of composite technology. However, the properties of papyrus fiber
were not intensively studied and its potential as a reinforcement of natural rubber for an outsole
application is not reported until this day.
In the current work, PNR composites were prepared to investigate the influence of papyrus fiber
loading and length on various properties of natural rubber for a shoe sole. The main aim was to reach
the optimal properties of PNR composites; with the hypothesis, papyrus fiber will improve the
mechanical properties of unreinforced natural rubber. Therefore, papyrus fiber was extracted and
characterized by selected properties. Three levels of fiber length and loading were prepared and mixed
with natural rubber after mastication and rubber compounding. Samples were tested for various
properties, based on the result, optimum parameters were identified.
JOURNAL OF NATURAL FIBERS 3
Fiber’s preparation
The Papyrus plant shown in Figure 1a was collected from Lake Tana, Bahir Dar, Ethiopia. The stem
cover was removed and chopped (Figure 1b,c) for ease of retting. Then it is left 2 days in daylight for
drying before retting (Figure 1d). Biological Retting was performed for 14 days (Figure 1e) and dried
for 2 days (Figure 1f) where most of the lignin will be removed easily as illustrated in Figure 1. Water
retting is a biological phenomenon where pectin in the soft cells are dissolved using microorganism
which frees the fiber bundles and makes it possible to separate fibers from the woody core (Pandey
2016). The fibers were manually extracted as shown in Figure 1g. Fibers were chopped for easy and
effective transfer of load (Roy et al. 2018). Three fiber length levels were chosen i.e. 10 mm, 15 mm,
and 20 mm.
Figure 1. Fiber extraction process flow from the papyrus plant; (a) papyrus plant from lake Tana (b) sample plant stem (c) plant stem
cover removed (d) dried stem for two days prepared for retting (e) stem soaked in water for 14 days (f) stem dried for 2 days, and (h)
the microscopic view of papyrus fiber diameter.
4 B. BEMERW ET AL.
Characterization
The fiber was characterized using FTIR, TGA, light microscope, and FAVIMAT + fiber tester by
applying ASTM standards. Samples (soles) were characterized for sole abrasion, sole hardness, tensile
strength, density, and flexing using ISO standards. Besides, FTIR, TGA, SEM, and water absorption
tests were conducted.
Morphological analysis
The compatibility of the fiber with the matrix was analyzed using a scanning electron microscope
(Philips XL-30 SEM, the Netherlands). Samples were scanned using electron beams to produce
a magnified image for analysis.
Figure 2. The FTIR spectra (a) and TGA value diagram (b) of papyrus fiber.
Getachew Alemayehu, and Gorade 2020). FTIR result shows that there is a high amount of OH group
stretch throughout the fiber structure. The absorption peaks were observed in two regions 3660–
2860 cm−1 and 1630– 400 cm−1. Identification of the intensity bands in the range from 3660–
2860 cm−1 is an indication for stretching vibration of O-H and C-H bonds in polysaccharides. The
broad peak at 3332 cm−1 is characteristic for stretching vibration of the hydroxyl group in polysac
charides which are present in cellulose-I (Kale, Alemayehu, and Gorade 2020; Vinod et al. 2019). It
also shows the intra and intermolecular hydrogen bond vibration in cellulose fiber. The broad peak at
2914 cm−1 is an indication for CH stretching vibration of all hydrocarbons constituent(Khan et al.
2019). Typical bands for cellulose around 1616 cm−1 are an indication for C = O stretch. Hydrocarbons
show the existence of lignin and hemicelluloses. The intensity bands at 1428 cm−1, 1367 cm−1,
1334 cm−1, 1039 cm −1 and 456 cm−1 belong to stretching and bending vibration of – CH2 and –
CH, -OH and C-O bonds in cellulose (Kommula et al. 2016; Mayandi et al. 2016; Vignesh, Balaji, and
Karthikeyan 2016) as shown in the Figure 2a.
Natural fibers contain cellulose, hemicelluloses, and lignin, which contribute to the thermal stability
of natural fibers. Accordingly, degradation temperatures of these contents might play a significant role
in the strength of the thermal stability of papyrus fiber strands. Also, the thermal stability of the
papyrus fiber strands was studied to evaluate the possibility of their use as reinforcement. Thermal
analysis of papyrus fiber was performed using TGA, which makes it possible to obtain information on
the change in physicochemical properties when determining their quantitative content by burning
micro samples in the range of 25°C – 1000°C as shown in the Figure 2b. The fiber shows a minor
weight loss in the range 25°C – 100°C, corresponding to the loss of absorbed moisture in the fiber
strands. The initial degradation stage occurred in the ranges of 250 °C – 400°C. This thermal
degradation is related to the de-polymerization of hemicelluloses and some fractions of cellulose
and lignin (Mayandi et al. 2016). Another degradation stage occurs in the ranges of 400°C – 600°C.
This thermal degradation correlates with the cleavage of glycoside bonds of cellulose and α and β aryl-
alkyl-ether linkages of lignin (Mayandi et al. 2016).
Thermogravimetric analysis shows that the papyrus fiber is thermally stable up to 250°C similar to
initial decomposition temperatures of other natural fibers (Kommula et al. 2016). Therefore, the fibers
could be successfully used as reinforcement when the molding temperature was reset under 250°C.
FAVIMAT+ FIBER test was used to understand the mechanical properties of papyrus fiber i.e.
specific tensile strength, elongation, and modulus. The results are shown in Table 1. Tensile strength
was 650.48 cN/tex and the elongation at break is 2.99% which indicates the fiber has much more
strength than the ideal strong jute fiber which is 30.1 cN/tex and elongation at break is 1.55%. Other
long-staple fibers like Sisal fiber have tenacity 40– 49 cN/tex, strain 2–3%, and Hemp has a tenacity of
22.6– 44.0 cN/tex (Arpitha 2017; Kicińska-Jakubowska 2012).
Linear density and geometrical properties such as length and diameter were analyzed using a light
microscope, weighting balance, and measuring scale, a summary of the result is shown in Table 2. The
nominal linear density of papyrus fiber was found to be 1.82 dtex.
The average length of papyrus fiber was found to be 1.2 m and the average weight was 0.02182 gm.
Furthermore, the diameter was found to be 3975.32 µm, 4004.56 µm, and 3837.41 µm from three
different areas microscopic views as observed in Figure 1h.
Table 3. Effect of fiber concentration and length on flex resistance, abrasion resistance, shore hardness, density and tensile strength.
Response
Factor 1 Factor 2 Response 1 2 Response 3 Response 4 Response 5
Shore Hardness Density Tensile strength
Run A:Fiber amount B:Fiber length Flex resistance Sole Abrasion resistance (Shore A) (g/cm3) (N/mm2)
B10 20 10 0.8 418.1 66 1.1 4.914
A15 10 15 0.7 377.9 62.3 1.1 7.16
C10 30 10 1.1 474.3 69 1.1 4.142
C15 30 15 1.1 474.3 69 1.1 3.542
B20 20 20 0.8 418.1 66 1.1 3.714
A10 10 10 0.7 377.9 62.3 1.1 7.77
A20 10 20 0.7 377.9 62.3 1.1 6.56
B15 20 15 0.8 418.1 66 1.1 4.314
C20 30 20 1.1 474.3 69 1.1 2.942
JOURNAL OF NATURAL FIBERS 7
Figure 3. Basic sole test results; (a) flex resistance, (b) sole abrasion resistance, (c) shore hardness, (d) density and (e) tensile strength.
of 60– 68 as shown in Figure 3c. When the amount of fiber increases, the hardness of the sample sole
increases, but it is still within the standard. In another case unlike expectation density of sample sole
were found to be constant in number 1.1 gm/cm3 but still they are below the maximum permitted
value of ISO 2781: 2014 which is 1.5 gm/cm3. Papyrus fiber reinforced natural rubber composite
exhibited optimum hardness which increased by 18.70% than that of virgin rubber. Flexural resistance
improved by 20%.
Both fiber length and concentration has shown a significant effect on the tensile strength of sample
sole, as illustrated in the main effect plot Figure 3e, which shows decreases in tensile strength when
fiber amount increase until it reaches 30%. There is a slight increment in strength after 30% fiber
loading. The best performance was recorded when fiber concentration is 10% and 10 mm in length.
According to ISO 20871: 2012, the tensile strength of rubber materials should have a minimum of 8 N/
mm2. Based on the above test results optimization was done using design expert software, which is
found to be 16.7% fiber concentration and 10 mm fiber length. The results obtained are described in
Table 3 and Figure 3 with a comparison to ISO standard values and 100% pure natural rubber.
Thermal properties
The thermal properties of purely natural rubber and optimized sample soles were investigated with the
use of thermogravimetric analysis. The measurements obtained are presented in Figure 4. As it can be
observed thermal degradation of natural rubber sole started at 300 oC and it shows a direct shift of
state. Whereas for optimized sole the decomposition started at 200 oC but the process is slow until it
reaches 400°C which implied enhanced thermal resistance compared to the pure natural rubber sole.
FTIR analysis
FTIR has been successfully used in the analysis and characterization of papyrus fiber reinforced natural
rubber composite. The spectra, Figure 4c, obtained were almost identical, showing that the polymeric
units in both elastomers are the same except for small differences. From the spectra of a pure natural
rubber sole, two transmission peaks occurred in the region between 2900 cm−1 and 3000 cm−1 and were
8 B. BEMERW ET AL.
Figure 4. TGA and FTIR of the 100% natural rubber and optimized PNRc sole.
assigned to the symmetrical and asymmetrical stretching mode of C-H bonds in a methyl group (Mizi
Fan1). Both papyrus fiber-reinforced and pure natural rubber sole showed a transmission peak at
10776 cm−1 and it was assigned to carbon- sulfur-carbon group stretching vibrations introduced by
carbon-sulfur bonds during Sulfur (Mizi Fan1) vulcanization. This transmission was observed to be
higher for the papyrus fiber reinforced sole compared with pure natural rubber.
It can be concluded, the rate of transmission was lower for papyrus fiber reinforced sole compared
to the pure natural rubber sole. The decrease in the transmission is related to the clustering and
entanglement of filler particles into long (Liu and Weidong 2006) chain.
Water absorption
The initial weight of the unreinforced natural rubber sole shows lower water absorption compared to
the optimized reinforced sole. The initial weight of pure natural rubber sole was 67.55 gm and the final
weight was found to be 67.56 gm and the water absorption is 0.014%. On the other hand, the optimized
sample sole initial weight was 61.59 gm after immersion and drying for 24 hr. While final weight is
found to be 61.64 gm. Therefore, the percentage of water absorption was 0.081%. It can be observed
that water absorption increased in the presence of fiber. The hydrophilic behavior of natural cellulosic
fibers exhibits weak resistance to moisture when they come in contact with water (Debeli et al. 2019).
Even if the water absorbency increased the result is acceptable according to ISO 20344 for rubber sole
which is 6.6%.
Figure 5. SEM Micrographs of the composite prepared with 10% papyrus fiber (a,b) and with 30% papyrus fiber (c,d).
Conclusion
The Cyprus papyrus plant, from Tanna lake (Ethiopia), was beneficiated as a source of cellulosic fibers
using enzymatic degradation. For purpose of preparation green composites, the extracted fibers were
used to reinforce the rubber.
The physical and mechanical properties of the extracted fibers were investigated. The natural rubber
was reinforced with extracted fibers to prepared green composite (soles) by compression molding at three
levels of fiber loading and fiber length. The prepared composites were characterized for their flex
resistance, tensile strength, abrasion resistance, density, and hardness using ISO standards. Results
revealed that papyrus fiber reinforced natural rubber composite exhibited optimum hardness which
increased by 18.70% than that of pure rubber. The Flexural resistance and hardness of the composites
materials were improved significantly. Also, the TGA analysis showed that the thermal stability of the sole
has been enhanced due to the presence of papyrus fiber. Flexing resistance shows an excellent improve
ment at all levels. While the tensile strength, abrasion resistance, and density don’t show much improve
ment but they are within the tolerable range with ISO standards and better than the unreinforced sole.
Therefore, the application of papyrus fiber for shoe sole making is shown possible to have an
alternative in the sector and to minimize the environmental impact of disposal of the papyrus plant. In
the future, researchers may focus on the surface modification of papyrus fiber for better interfacial
adhesion with resins.
ORCID
Magdi Gibril http://orcid.org/0000-0003-0282-3310
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