International Journal of Application or Innovation in Engineering & Management (IJAIEM)
Web Site: www.ijaiem.org Email: editor@ijaiem.org
Volume 3, Issue 11, November 2014
ISSN 2319 - 4847
Effect of chemical treatments on mpelocissus
Cavicaulis fiber
Ejikeme Patrick C. N.1, Ejikeme Ebere M.1 and Nwosu David C1
Chemical Engineering Department, Enugu State University of Science and Technology, Enugu, Nigeria
ABSTRACT
The tensile strength of Ampelocissus cavicaulis fiber was enhanced by chemical treatment with sodium hydroxide, acetic
anhydride, nitric acid, and zinc chloride. Effects of concentrations of the chemicals and pretreatment time on the tensile
strength of fiber were studied. It was observed that tensile strength of the fiber was increased as the chemical
concentrations and pretreatment time were increased to a point that further increase led to decrease in tensile strength of
the fiber. The SEM analysis confirmed that the chemical treatments succeeded in removing the surface impurities and
lignin components of the fiber which resulted to smooth surfaces of the treated fiber with attendant increase in tensile
strength. Sodium hydroxide had highest effect on the fiber, followed by acetic anhydride, nitric acid, and lastly, zinc
chloride.
Keywords:- Acetic anhydride, ampelocissus cavicaulis, nitric acid, sodium hydroxide, zinc chloride
1.INTRODUCTION
The study of using natural fibers to reinforce composite materials increased dramatically during the last few years due
to the environmental cost of using energy intensive synthetic fiber such as glass, carbon and keular. Composites are
those material made up from two or more distinct materials having different chemical and physical properties provide a
well defined structure [1], [2]. Fiber reinforced composites consists of reinforcing fibers and a polymer matrix which
acts as a binder for the fibers. Many fibers reinforced composite materials offer a combination of strength and modules
that are either comparable to or better than many pure materials [3]. The attractive features of natural fibers as a
reinforcing materials are light weight, high specific modulus, non – toxicity, friendly processing and absorbed CO2
during their growth [4]-[6]. However, these natural fibers are not problem free as reinforcement on composite. The
performance and stability of fiber – reinforced composite materials depends on the development of coherent interfacial
bonding between fiber and matrix. In natural fiber – reinforced composite there is a lack of good interfacial adhesion
between the hydrophilic cellulose fibers and the hydrophobic resins due to their inherent incompatibility [7]. Their
structural compositions such as cellulose, hemicellulose, lignin, pectin and waxy substances allow moisture absorption
from the environment which leads to poor bonding with the matrix materials [8]. Certain chemical treatment on natural
fibers is needed to enhance the performance as reinforcement in polymer composite materials. Natural fibers are
amenable to modification as they bear hydroxyl group from cellulose and lignin. The hydroxyl group may be involved
in the hydrogen bounding within the cellulose molecules thereby reducing the activity towards the matrix. Chemical
modifications may activate these groups or can introduce new moieties that can effectively interlock with the matrix.
In this study, a locally sourced natural fiber; ampelocissus cavicaulis was treated with different chemicals. Effect of
chemical treatments was evaluated based on the tensile strength of the treated fibers.
2.MATERIALS AND METHODS
2.1 Extraction of Fiber
Ampellocissus cavicaulis fibre was obtained from well defined locations in Ebonyi State of Nigeria. This plant fibre was
extracted from the plant stem using water retting extraction process, giving fibre of different lengths and diameters.
Before usage, the fibre was visually selected in order to verify the absence of defects along the length of the fibre.
2.2 Alkali treatment
This procedure was in accordance with work done by nural and Ishak [9] with slight modifications. The Ampelocissus
cavicaulis was treated at 6% NaoH. The fiber was immersed in the alkali solution for 50 minutes, then neutralized with
acetic acid and washed with distilled water repeatedly until all sodium hydroxide was eliminated. Finally, the fiber was
washed with distilled water and dried at room temperature for 48h.
2.3 Acetic anhydride treatment
The acetylation process was in accordance with work done by A.K bledzki, etal [10] with slight modifications. The
Ampelocissus cavicaulis fiber was soaked in distilled water for an hour, filtered and placed in a round bottom flask
containing 10% acetic acid solution for 30 minutes. After which it was placed on flask containing 14% acetic
anhydride solution. The process temperature of acetylation was 300C and duration was 70 minutes. After
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Volume 3, Issue 11, November 2014
ISSN 2319 - 4847
modification, the fiber was washed periodically with distilled water until acid free. Finally, modified fiber was air dried
for certain time before analysis.
2.4. Nitric acid treatment
The nitric acid treatment was according to F. Vautard etal 2013 [11] and W. Z etal 2010 [12] with modifications. The
size reduced ampleocissus cavicaulis fiber was oxidized with 6% nitric acid. The prepared oxidized solution was boiled
to a temperature of 600C and the fiber immersed in the solution at maintained said temperature for 50 minutes. At then
neutralized with NaoH solution and washed with distilled water repeatedly until all the nitric acid was eliminated.
Finally, the fiber was washed again with distilled water and dried to a constant weight temperature.
2.5 Zinc chloride treatment
Zinc chloride treatment was done in accordance with the work done by V. Nadanthangam etal , 2013 with modification
[13]. The fiber was soaked in 3% Zncl solution for 70 minutes after which it was washed with distilled water until the
washing solution became chloride free. The fiber was washed with distilled water and dried at room temperature for 48
hours.
2.6 Tensile strength
Tensile strength is a measurement of the ability of material to withstand forces that tend to pull it apart. It determines
to what extents the material stretches before breaking. The fiber tensile strength tests were performed by a computer
controlled Hounsfield tensometer testing machine (model 5566) with a gauge length of 40mm and a crosshead speed of
5mm/min. The round bars were covered with surgical glove fingers, and the flax was clamped at the top and bottom.
The fiber bundle was wrapped one revolution around each of the two bars and was spread out over the entire gauge
length in a parallel. The machine was wet up to display a force deformation curve at loading and to read the load at
maximum or the break point.
2.7 Determination of lignin content by gravimetric method
This procedure was in accordance with the work done by G. N. Onyeagoro 2012 [14]. 2.0g of the sample were weighed
and placed inside a beaker. 72% H2SO4 was added and allowed to stand for 2 hours. 8% H2SO4 was later added and
the solution refluxed for 3 hours. The residue was filtered with purpling cloth and washed severally with hot water. A
crucible was weighed and the sample was scraped into it. The sample was oven dried at 1100C for 1 hour and then
cooled inside desiccators after which the weight was taken. The sample was ashed in a furnace at 5000C for 3 hours. It
was then cooled inside desiccators and finally weighed. The % lignin was calculated using equation
% Lignin = W2 - W1 x 100
(1)
Ws
Where,
W1 = weight of ash sample + crucible
W2 = weight of oven dried sample + crucible
Ws = initial weight of dried sample
2.8 Determination of cellulose content
This procedure was in accordance with the work done by G. N. Onyeagoro 2012 [14]. 1.5g of fiber sample was weighed
into a beaker followed by addition of 20ml of 80% acetic acid, 1ml of concentrated nitric acid and 3 glass beads. The
content was refluxed for 30 minutes. The sample was cooled and washed into 50ml centrifuge tube containing hot 95%
ethanol, and then centrifuged at 15,000rpm for 5 minutes. Thereafter, the liquid was decanted and 95% ethanol was
added, stirred and filtered by suction. The sample was washed three times with hot benzene, two times with 95%
ethanol and once with ether. The sample was placed inside a weighed crucible and placed in the oven maintained at
1100C for 1 hour. The crucible was then cooled in desiccators and weighed. For ash content determination, the crucible
and its content was placed inside a furnace maintained at 5000C for 3 hours after which it was cooled in desiccators
and weighed. The % cellulose was calculated from equation 2.
% cellulose =
w 2  w1 x100
ws
(2)
Where,
W1 = weight of crucible + sample after ashing
W2 = weight of crucible + sample after drying
Ws = weight of sample
2.9 Surface morphology
Scanning Electron microscropy (SEM) (PHENOM PROX) analysis was carried out on the untreated Ampelocissus
Cavicaulis fiber and on the treated fiber to study its surface texture before and after treatment.
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3. RESULTS AND DISCUSSIONS
3.1. Chemical and mechanical properties of fiber
Chemical and mechanical properties of the natural fibre used was analysed, they are; cellulose, hemicelluloses, lignin,
wax, water content and water soluble substances. These compositions differed with the different species of the plant
and on the grooving conditions. The chemical and mechanical properties of the natural fibre used in thus study are
shown in table 1 and 2 respectively.
Table 1. Chemical properties of fiber
Cellulose
Hemicellulose
Lignin
Ash content
Wax
Moisture
Content
content
content
(%)
(%)
content
(%)
(%)
(%)
(%)
48.967
21.221
31.33
2.43
0.21
0.514
Table 2. Mechanical properties of fiber
Tensile
Elastic
Ultimate
Strength
Modulus
Elongation at break
(Mpa)
(Mpa)
(%)
1.28
238.28
3,971.33
3.00
3.2. Scanning Electron Microscopy of untreated and treated fiber.
The effect of chemical treatment on the surface of Ampelocissus cavicaulis fibers is shown as SEM photomicrographs
in figure 1(a), (b), (c), (d), and (e). The SEM photomicrograph of the surface of untreated fiber in fig 1(a) shows the
presence of wax, oil, and surface impurities. Waxes and oils provide protective layers to the surface of the fibers [2].
The chemical treatments on the fiber were successful in removing the surface contaminants as evidenced in fig 1(b) to
1(e). The differences on the surface morphologies were as a result of the differences on the degrees of effectiveness of
different chemicals used in the pretreatment. The photomicrographs show very clean surfaces.
Density
(g/cm3)
(a)
(b)
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(c)
(d)
(e)
Fig. 1. SEM Images of fiber (a) Untreated fiber, (b) NoaH treated, (c)Acetic anhydride treated, (d) Nitric acid treated,
(e) Zinc Chloride treated.
3.3. Effect of process variables on the tensile strength of the fiber.
Some of the shortcoming and limitations of natural fibers when used as reinforcement for composites are related to the
lower strength properties, lower interfacial adhesion, poor resistance to moisture absorption, lower durability and
dimensional stability (shrinkage and swelling) (CIP-EIP-ECO INNO 2008). To overcome the shortcomings, various
chemical like NaOH, acetic anhydride, Nitric acid and zinc chloride were used to treat the fibers before using as
reinforcement. The chemicals type used are of different efficiencies for improving the mechanical properties of the
fibers with resultant improvement on various properties of the final products. From this study, it has been seen that the
efficiency of the treatment depends not only on the type of the chemicals used, but equally on the concentration of the
chemicals as well as the length of treatment time. Effect of different processing variables like chemical types, chemical
concentration and time of treatment has been seen to induce variations in the physical properties of the fiber.
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3.3.1. Effect of chemical types on the strength of the fiber
The effect of different types of chemical used on the tensile strength of the fiber was studied to understand the
magnitude of variation resulted due to types of chemical used. Fig. 2 shows the tensile strength of the fiber treated with
different chemicals with the untreated sample serving as control.
Figure 2. Effect of types of Chemicals on the tensile strength of the fiber.
It was evidenced from the plots that sodium hydroxide had highest effect on the tensile strength of the fiber. All the
chemical treated fibers had improved tensile strength compared to the untreated fiber. Natural fibers composed of
cellulose, hemicelluloses, lignin and other extractives. Cellulose gives the strength, stiffness and structured stability of
the fiber, and is the major framework components of the fiber. Lignin and hemicelluloses produce the adhesive to hold
the cellulose framework structure of the fiber together, reducing the permeation of substances to the cellulose. The
chemical treatment used resulted in the removal of certain portions of hemicellulose, lignin and other extractives
covering materials. As a result, fiber surface became cleaner as evidenced in the SEM analysis. In other words, finer
surfaces become more uniform due to the elimination of micro voids and thus stress transfer capacity between the
ultimate cells improved. This resulted to higher tensile strength when compared with the untreated fibers.
3.3.1.1. Effect of sodium hydroxide treatment on the natural fibers
Sodium hydroxide (NaOH) is the most commonly used chemical for bleaching and/or cleaning the surface of plant fiber
[15]. It also changes the fine structure of the native cellulose I to cellulose II by a process known as mercerisation.
The standard definition of mercerization proposed by ASTM D1695 is the process of subjecting a vegetable fiber to the
action of a fairly concentrated aqueous solution of a strong base so as to produce greater swelling with resultant
changes in the fine structure, dimension, morphology and mechanical properties [16]. Zeronian 1985 [17] proposed
another definition of mercerization which is suitable for basic research and is more specific. Mercerized cellulose is a
sample of cellulose which has been treated with a solution of an alkali metalhydroxide of sufficient strength to cause
essentially complete conversation of the crystal structure from cellulose I to II. He reported that residual traces of
cellulose I are found even when the strength of the alkali used in the mercerization treatment are considered optimum
for conversation. In that case, no matter the strength of condition of mercerization used there cannot be total
conversion. The resultant increased in the tensile strength of the alkali treated fibre was as a result of the
delignification of the fiber.
Figure 3. Effect of NoaH treatment on the fiber
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Alkali treatment increased the surface roughness resulting in better mechanical interlocking and the amount of
cellulose exposed on fiber surface [18]. Thus increases the number of possible reaction sites and allows better fiber
wetting.
Figure 4. Effect of NoaH pretreatment time on the tensile strength of the fiber.
When the alkali treatment was higher than the optimum conditions, excess delignification of the fibre took place and
resulted in the weakness or damage of the fibre which resulted to reduction on the tensile strength of the treated fiber.
From figure 3, it was evidenced that the tensile strength of the treated fiber increased to a certain level, and decreased
drastically.
3.3.1.2 Effect of acetic anhydride treatment on the fiber.
Acetylation treatment on natural fiber is known as esterification method for plasticizing of cellulose fibers. During
acetylation treatment there is an introduction of acetyl functional group (CH3C00-1) into the fiber. Chemical
modification with acetic anhydride substitutive the polymer hydroxyl groups of the cell wall with acetyl groups,
modifying the properties of these polymers so that they become hydrophobic [19]. This reaction generated acetic acid
as by product which was removed from the fibre before use.
Figure 5. Effect of Acetic anhydride concentration on the tensile strength.
The reaction of acetic anhydride with fiber is as shown below ;
Fiber – OH + CH3 – C (=0) –O – C (= O) CH3  fiber – OCOCH3 + CH3COOH
(3)
The preliminary treatment done confirmed that acetic anhydride alone cannot sufficiently treat fibre, therefore the fiber
was treated with 10% acetic acid for 30mins before treatment with different concentrations of acetic anhydride for
different time intervals. Figure 5, shows the effect of concentration of acetic anhydride on the tensile strength of the
fiber. It can be seen that the tensile strength increased as the concentration of the acetic anhydride increased till a point
were further increased resulted to decrease in the tensile strength. This decrease was as a result of excess
delignification.
Figure 6. Effect of acetic anhydride pretreatment time on the tensile strength
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3.3.1.3. Effect of Nitric Acid treatment on the Fibers
The natural fiber was treated with nitric acid and subsequently analyzed for the tensile strength to develop on
understanding of the property changes and how it will affect the resultant composite. The preliminary work done
showed no appreciable increase in the tensile strength of the fiber when treated at room temperature; therefore the
treatment was done at higher temperature of 600C. Treatment of fiber with nitric acid is called oxidation method and it
introduces an oxidizing group to the surface of the natural cellulose fiber. According to F. Vautard etal 2013 [11], the
oxidation of fiber surface in boiling nitric acid created a rough surface which significantly increased a specific surface
area, and also generated a high density of hydroxyl groups, carboxylic acids and lactones in comparison to the
untreated fibers. These changes resulted to increase in tensile strength of the treated fiber.
Figure 7. Effect of Nitric acid concentration on the tensile strength of the fiber.
From the result on figure 7 and figure 8, there were increase in the tensile strength of the fiber as the concentration and
pretreatment time was increased till the optimum conditions before it started decreasing. This was attributed to the
increase on the quantity of surface functional groups on the surface of the fibers which thus enhanced the ability of the
fibers to establish strong interaction between their molecules.
Figure 8. Effect of nitric acid pretreatment time on the tensile strength of the fiber.
3.3.1.4. Effect of zinc chloride treatment on the fiber
Zinc chloride treatment on natural fibers removes natural and human impurities that are non cellulosic constituents and
other unwanted substances and increase the tensile strength and the affinity of the cellulose for finishes [20]. Zinc
chloride equally act as a swelling agents there by increasing the accessibility of the cellulose to the secondary layer [13].
Figure 9. Effect of Zinc chloride concentration on the tensile strength of the fiber.
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Zinc chloride is known to have destructive effect on fiber especially when used at high concentration and longer
pretreatment time [13]. This is evidenced on the result of the analysis shown on fig. 9 and 10.
Figure 10. Effect of Zinc chloride pretreatment time on the tensile strength of the fiber.
It was noticed that longer treatment time and lower concentration increased the tensile strength of the treated fiber
because of the cleaning and swelling effect of zinc chloride. But deviation from these optimum conditions led to
decrease in tensile strength. This can be attributed to the destructive effect of zinc chloride on the fiber due to high
concentration and long pretreatment time. Equally, excess delignification can reduce the tensile strength of the fibers.
4.CONCLUSION
Chemical treatment of Ampelossisus cavicaulis fiber was successfully carried out using sodium hydroxide, acetic
anhydride, nitric acid and zinc chloride. The mechanical and chemical compositions of the natural fiber were
determined prior to the treatments to ascertain the effectiveness of the treatments on the fiber. SEM analysis revealed
that the chemical treatments were able to remove the surface impurities and the lignin contents of the fiber with
resultant increase in the tensile strength of the fiber. Effect of different concentrations of the chemicals showed that the
tensile strength increased as the concentration of the chemicals were increased to a point that further increased in
chemical concentration resulted to decrease in tensile strength. The same trend was observed for effect of pretreatment
time on the tensile strength. It can be concluded that there exists optimum conditions for the chemical treatment in
which when deviated, will result to decrease in tensile strength. This decrease can be attributed to excess
delignification. It was equally observed that NaoH had highest effect on the fiber followed by acetic anhydride, nitric
acid, and lastly, zinc chloride.
ACKNOWLEDGEMENT
The authors wish to thank PYMOTECH RESEARCH CENTRE AND LABORATORIES ENUGU, ENUGU STATE
NIGERIA for all their facilities used throughout the research work
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AUTHORS
Ejikeme, P. C. N. received his M.Eng in Chemical Engineering from the Enugu State University of
Science and Technology Enugu Nigeria in 1995. He was elected into the Enugu State House of
Assembly in 1992 .He is a member of Nigerian Society of Chemical Engineers. He is also a member of
Nigerian Society of Engineers. He is a Senior Lecturer in the Department of Chemical Engineering of
the Enugu State
University of Science and Technology Enugu
Ejikeme, Ebere .M. received her M.Eng in Chemical Engineering from Nnamdi Azikiwe
University Awka in 2010. S he is a member Society of Petroleum Engineers. She is a member
Nigerian Society of Chemical Engineers. She is also a member of Nigerian Society of Engineers. She
is a Lecturer in the Department of Chemical Engineering of the Enugu State University of Science
and Technology Enugu, Currently, she is doing her PhD.
Nwosu, David C. received his M.Eng in Chemical Engineering from the Enugu State University of
Science and Technology Enugu Nigeria in 1998. He is a member of Nigerian Society of Chemical
Engineers. He is also a member of Nigerian Society of Engineers. He is a Lecturer in the Department
of Chemical Engineering of the Enugu
State University of Science and Technology Enugu and
currently doing his PhD.
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