Polymer-Plastics Technology and Engineering

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Preparation and Properties of Biodegradable

Polymer Film Based on Polyvinyl Alcohol and
Tropical Fruit Waste Flour

Ooi Xian Zhong , Hanafi Ismail , Nor Aziah Abdul Aziz & Azhar Abu Bakar

To cite this article: Ooi Xian Zhong , Hanafi Ismail , Nor Aziah Abdul Aziz & Azhar Abu Bakar
(2011) Preparation and Properties of Biodegradable Polymer Film Based on Polyvinyl Alcohol and
Tropical Fruit Waste Flour, Polymer-Plastics Technology and Engineering, 50:7, 705-711, DOI:
10.1080/03602559.2010.551391

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Polymer-Plastics Technology and Engineering, 50: 705–711, 2011
Copyright # Taylor & Francis Group, LLC
ISSN: 0360-2559 print=1525-6111 online
DOI: 10.1080/03602559.2010.551391

Preparation and Properties of Biodegradable Polymer Film

Based on Polyvinyl Alcohol and Tropical Fruit Waste Flour
Ooi Xian Zhong1, Hanafi Ismail1, Nor Aziah Abdul Aziz2, and Azhar Abu Bakar1
1
School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia,
Penang, Malaysia
2
School of Industrial Technology, Universiti Sains Malaysia, Penang, Malaysia

production by solution casting. The excellent chemical

In this study, two different types of tropical fruit waste flour, resistance, good thermal barrier, good mechanical proper-
rambutan waste flour (RWF) and banana waste flour (BWF), were ties and physical properties of PVOH have been employed
blended with polyvinyl alcohol (PVOH) by solution casting method. in various applications, including dip coating, adhesives
The structure of the blend film was characterised by Fourier Trans- and solution casting film[2,5–7].
form Infrared Spectroscopy. The tensile strength and elongation at
break of tropical fruit waste flour-filled polyvinyl alcohol were The limiting factor of PVOH is the cost, which must be
lower, but the tensile modulus was higher, than that of PVOH film. competitive with non-degradable synthetic polymers such
At a similar blend ratio, the tensile properties of the PVOH/RWF as polyethylene and polypropylene in packaging applica-
film were higher than the PVOH/BWF film, but the PVOH/BWF tions[8]. Therefore, the combination of economical and
film showed higher water uptake than PVOH/RWF film. ecological demands has led to the incorporation of waste
into biodegradable polymers. Sedlarik et al.[2] described a
Keywords Polyvinyl alcohol; Solution casting; Tensile proper- number of studies that utilise the waste from leather indus-
ties; Tropical fruit waste flour
try, dairy industry, and mineralogy. For example, Ozaki
et al.[9] investigated a green composite by utilising waste
INTRODUCTION wood and a totally biodegradable polymer. The wastes
Plastic materials made from petroleum have been widely produced by the agricultural sector also cause serious
used in several applications, such as packaging, agricul- waste disposal problems. It is believed that there will be
tural, catering, construction materials. Today, in spite of wide development prospects and commercial application
the obvious benefits of synthetic plastic, the downfall of for tropical fruit waste flour as a potential filler in polymer
these plastics is that the high degree of chemical stability films to sustain the ecological and economical demands.
of petroleum polymers have resulted in a low degradation The aim of this study was to develop a biodegradable
rate in the environment[1]. With the increasing amount of polymer film based on tropical fruit waste flour and
plastic waste, biodegradable polymers have been increas- poly(vinyl alcohol) using different contents of rambutan
ingly used in the plastics industry to offer an alternative waste flour (RWF) and banana waste flour (BWF). Their
solution to waste disposal. effects on the tensile properties and biodegradability of
Generally, the biodegradable polymers can be divided PVOH=tropical fruit waste flour blends were studied.
into three groups[2]. The first group includes biopolymers,
or polymers of natural origins, whereas the second group EXPERIMENTAL
consists of synthetic biodegradable polymers (oil based
Materials
polymers with a hydrolysable backbone chain). The last
Polyvinyl alcohol (PVOH), with a fully hydrolysed,
group is the synthetic polymers that undergo physical or
molecular weight average of 89,000–98,000 g=mol and a
chemical modification to achieve biodegradability. Poly-
density 1.269 g=cm3, was supplied by Sigma-Aldrich (M)
vinyl alcohol (PVOH) is a synthetic biodegradable
Sdn. Bhd. The tropical fruit waste flours used in this study
polymer[3] with the technological potential as a
were rambutan skin and banana skin, which were supplied
water-processible polymer[4], thus allowing for film
by Zarm Scientific & Supplies (M) Sdn. Bhd. The rambu-
tan skin and banana skin were analysed for carbohydrates,
Address correspondence to Hanafi Ismail, School of Materials
and Mineral Resources Engineering, Universitya Sains Malaysia, protein, fat, crude fibre, ash, and moisture, as shown in
Engineering Campus, 14300 Nibong Tebal, Penang, Malaysia. Table 1. Glycerol (85% purity) and tween-80 (non-ionic
E-mail: hanafi@eng.usm.my surfactant) were supplied by Merck (M) Sdn. Bhd., whereas

705
706 O. X. ZHONG ET AL.

TABLE 1 Morphology Studies

The proximate composition for rambutan skin and The surface of the specimens was scanned using a scan-
banana skin ning electron microscope (SEM) (model Zeiss Supra
35VP). The test specimens were taken with maximum care
Composition Rambutan skin Banana skin
to avoid surface damage and contamination that could
Moisture (%) 5.78  0.14 8.71  0.06 affect the results. The surfaces of the test specimens were
Protein (%) 5.97  0.04 6.77  0.06 coated with a thin gold layer to prevent electrical discharge
Fat (%) 0.42  0.01 0.94  0.04 during examination.
Crude Fiber (%) 14.17  0.22 2.93  0.09
Ash (%) 3.33  0.36 2.46  0.17 Fourier Transform Infrared Spectroscopy (FT-IR)
Carbohydrate (%) 70.33  0.16 81.12  0.02 FTIR spectra were obtained and recorded using Fourier
transform infrared spectroscopy (model Perkin-Elmer).
FTIR was used to obtain some qualitative information
hexamethylenetetramine (HMTA) (cross-linking agent) about the functional groups and chemical characteristics
was purchased from Sigma-Aldrich (M) Sdn. Bhd. All of the PVOH=TFWF blends. The selected scanning range
chemicals were analytical grade reagents. was 550 cm1 to 4000 cm1 at 4 cm1 of resolution. For
each spectrum, 4 scans were co-added.
Film Preparation
Calculated amounts of PVOH, tropical fruit waste flour Water Absorption
(TFWF) (i.e., rambutan waste flour (RWF) and banana Dried PVOH=TFWF blend films were immersed in dis-
waste flour (BWF)), glycerol, HMTA, and Tween-80, as tilled water at room temperature (25
C). Once equilibrium
shown in Table 2, were mixed homogeneously with stirring was reached (24 h), moisture on the surface of the films was
in 200 ml of de-ionised water in a reaction flask and heated removed, and the weight of the films was measured[10]. The
in a water bath for 2 h at 95
C. At the end of this incu- percentage of water absorption (Wa) of the film was calcu-
bation, the mixture was cooled to room temperature, and lated with the following Equation (1):
films were cast onto clean glass plates.
Wa ¼ ½ðWe  Wi Þ=Wi   100 ð1Þ
Tensile Properties
where We is the weight of the film at the adsorbing equilib-
The tensile test was carried out with an Instron testing rium, and Wi is the initial weight of the dried film.
machine (model Instron 3366). The cross-head speed was
set at 20 mm=min. The average thickness of the specimens Water Vapour Transmission (WVT)
was about 0.10 mm. Other parameters of the tensile The WVT was determined according to ASTM E96. An
machine and conditioning of the tensile specimens followed impermeable cup with desiccant silica gel was closed with a
ASTM D882. All these tests were conducted at room tem- sample of PVOH=TFWF blend film firmly fixed on top.
perature, and the average value of five repeated tests was The cups then were weighed with their contents and were
recorded for each composition. placed in a desiccator containing distilled water at ambient
temperature. The films were weighed every 24 hours until a
TABLE 2 steady increase in weight was achieved. The water vapour
Formulation for preparation of PVOH=RWF and transferred through the films and absorbed by the silica
PVOH=BWF blends gel was determined from the weight gain of the cup. The
water vapour transmission rate, WVTR (g=h.m2) was
PVOH RWF BWF Glycerol HMTA Tween-80 calculated according to Equation (2):
Blends (g) (g) (g) (g) (g) (g)
WVTR ¼ DW=ðDt  AÞ ð2Þ
A 10 0 0 1.5 0.1 0.6
B 9 1 0 1.5 0.1 0.6
where A was the area exposed to water transfer (m2), and
C 8 2 0 1.5 0.1 0.6
DW=Dt was calculated by the linear regression from the
D 7 3 0 1.5 0.1 0.6
points of weight gain and time of transfer[11].
E 6 4 0 1.5 0.1 0.6
F 9 0 1 1.5 0.1 0.6
Natural Weathering
G 8 0 2 1.5 0.1 0.6
The weathering test was conducted according to ASTM
H 7 0 3 1.5 0.1 0.6
D1435. All specimens were attached to a rack with a speci-
I 6 0 4 1.5 0.1 0.6
men holder. The rack was adjusted to face the equator at
 PVA AND FRUIT WASTE FLOUR IN BIODEGRADABLE POLYMER FILMS 707

an angle of 45
and situated in an open area free from over- effect of TFWF[13] and the low effective cross-sectional
shadowing by other objects; thus, the specimens were area of the PVOH matrix towards TFWF as reported by
exposed to all environment effects, such as rain fall, sun- Rahman et al.[14].
light, dew, and wind. This test was performed for 1 month However, at the same blend ratio, the tensile strength
to determine the degree of degradation. Moisture at the and elongation at break of the PVOH=RWF blend film
surface of specimens was removed with a clean towel, were higher than those of the corresponding PVOH=
and they were left in air for 24 h at room temperature BWF blend, indicating that the compatibility of the PVOH
before mechanical testing and observation of the sample and RWF is better than that of PVOH and BWF.
surface under SEM. The tensile modulus of the PVOH=TFWF film as a
function of TFWF loading for both RWF and BWF is
RESULTS AND DISCUSSION presented in Table 3. The experimental results show that
Tensile Properties the tensile modulus increases with the TFWF loading. This
Table 1 illustrates the tensile properties of PVOH= trend was attributed to the stiffening effect of the TFWF.
TFWF blends as a function of the TFWF content for ram- At the same blend ratio, the tensile modulus of the
butan waste flour (RWF) and banana waste flour (BWF). PVOH=RWF blends was higher than that of the PVOH=
The tensile strength of PVOH=RWF and PVOH=BWF BWF blends. Interestingly, the RWF was significantly
blends decreased with the increase of both RWF and more rigid than the BWF.
BWF loading. As a starch filler, the same behavior was also
observed for the tropical fruit waste flour and probably Water Absorption
reflects the poor interfacial adhesion between the TFWF A decrease in water sensitivity for blend films is required
and PVOH. for most applications of films[12]. However, due to the
This result indicates that the TFWF could not improve hydrophilic nature of the PVOH and water sensitivity of
the tensile properties of the blends because of the excellent the TFWF, the percentage of water uptake was consider-
mechanical properties of PVOH itself and the poor com- ably increased for films blended with both RWF and
patibility of PVOH and TFWF in nature[12]. As reported BWF, as shown in Table 4. The water uptake of the blend
by most researchers[5,11], the values of the tensile strength films increased with increasing TFWF. At the same weight
and elongation at break of the PVOH=starch films were ratio, water uptake of PVOH=BWF blends was higher than
lower than those of the pure PVOH films and decreased those of the PVOH=RWF blends. This difference was
with increasing starch loading. Also, similar observation attributed to the better compatibility between PVOH and
as reported by Ramaraj[8] on PVOH and coconut shell RWF compared to BWF; thus, the free volume of the
powder composite films. PVOH=RWF was lower, and the tendency to absorb water
The percentage of elongation at break decreased from was decreased. According to Elizondo et al.[15], the
238% (pure PVOH film) to only 52% and 27% at the load- capacity of the polymer film to absorb water was reduced
ing of 10 wt% RWF and BWF, respectively. The dramatic because of the strong interaction between the two polymers
drop in the elongation at break was related to the stiffening and homogenisation of the blends.

TABLE 3
Tensile properties of PVOH=TFWF films in initial state and after subjected to natural weathering
Initial state After 1 month weathering
Tensile Elongation Tensile Tensile Elongation Tensile
strength at break modulus strength at break modulus
Blends (MPa) (%) (MPa) (MPa) (%) (MPa)
A 26.3  0.91 238.2  2.25 136.4  1.46 13.2  0.55 51.0  1.91 154.7  1.35
B 8.9  0.53 52.2  1.36 156.5  1.28 6.0  0.09 14.2  1.73 162.1  1.08
C 6.4  0.85 27.2  1.18 167.9  1.83 4.9  0.32 10.8  0.02 174.0  0.06
D 5.1  0.68 23.5  1.73 197.3  1.68 3.4  0.03 6.7  0.08 209.7  0.10
E 3.7  0.60 10.8  1.17 226.6  2.34 1.5  0.09 2.7  0.02 244.3  0.61
F 2.8  0.29 26.7  1.29 152.4  1.46 1.7  0.07 4.1  0.86 163.9  1.35
G 2.0  0.14 11.0  1.85 166.5  1.16 0.6  0.15 3.3  0.03 179.1  0.40
H 1.7  0.20 8.0  0.74 175.8  1.29 0.5  0.08 1.5  0.32 194.9  0.05
I 0.8  0.25 3.5  0.04 212.5  1.94 Fragmented Fragmented Fragmented
708 O. X. ZHONG ET AL.

TABLE 4
Water absorption and water vapor transmission rate (WVTR) according to the quantities of PVOH, RWF and BWF
used in the elaboration of the blends of PVOH=TFWF blends film
Blends PVOH (g) RWF (g) BWF (g) Water Absorption (%) WVTR (g h1 m2)
A 10 0 0 131.4  0.16 4.9  0.05
B 9 1 0 137.1  0.02 5.6  0.03
C 8 2 0 138.6  0.01 6.0  0.11
D 7 3 0 139.8  0.04 6.4  0.01
E 6 4 0 140.5  0.17 6.5  0.07
F 9 0 1 141.2  0.20 8.1  0.19
G 8 0 2 144.1  0.03 9.3  0.22
H 7 0 3 148.6  0.18 9.8  0.06
I 6 0 4 154.1  0.22 11.7  0.15

Furthermore, the water absorption capability acts as an the WVTR of a hydrophilic film depends on both the
important property, especially for biodegradable materials. diffusivity and solubility of water molecules in the film
As reported by earlier studies, microorganisms require a matrix. Thus, the hydrophilic nature of PVOH and the
moist environment to survive[16] and be able to export water sensitivity of TFWF lead to the absorption of water
hydrolytic enzymes that break down the biopolymers[17]. molecules and result in an increase of the WVTR of
Therefore, surface of the materials were degraded by PVOH=RWF blends and PVOH=BWF blends. The
microorganisms such as fungi and bacteria due to the WVTR of PVOH=RWF blends was lower than that of
absorbed water. the corresponding of the PVOH=BWF blends. Again, this
difference may result from the poor compatibility between
PVOH and BWF, which leads to an increase in the
Water Vapor Transmission Rate (WVTR)
interchain spacing, thus allowing more water molecules
of the PVOH/TFWF Films
to diffuse through the films.
WVTR is a measurement used to determine the ability
of moisture to penetrate and pass through a material[10].
The WVTR was calculated and is shown in Table 4. In gen- Fourier Transform Infrared (FT-IR) Characterisation
eral, with an increase of RWF or BWF, the WVTR of the The spectra of PVOH (Fig. 1a), rambutan waste flour
blend films increased. According to Gontard & Guilbert[18], (Fig. 1b) and banana waste flour (Fig. 1d) were studied

FIG. 1. FT-IR spectra of (a) PVOH, (b) rambutan waste flour, (c) PVOH=RWF (6:4 weight ratio) blends, (d) banana waste flour, and (e) PVOH=BWF
(6:4 weight ratio) blends.
 PVA AND FRUIT WASTE FLOUR IN BIODEGRADABLE POLYMER FILMS 709

and compared with the PVOH=RWF (6:4 weight ratio) The tensile strength and elongation at break of the
blend (Fig. 1c) and the PVOH=BWF (6:4 weight ratio) PVOH=RWF blend film decreased to 67% and 26%
blend (Fig. 1e), as presented in Figure 1. For each of the of its initial value, respectively, which was similar for
films, the spectra of the blends were similar to that of spec- PVOH=BWF blends.
tra of pure PVOH. The strong and wide absorption band at Interestingly, the 6:4 (weight ratio) of the PVOH=BWF
3245 cm1 of the PVOH (Fig. 1a) film indicated that there blend films were fragmented after being subjected to natu-
were plenty of water hydroxyl groups in the films which ral weathering for 1 month. Therefore, no value is shown
correspond to the PVOH component as reported by for the tensile strength, elongation at break and tensile
El-Sawy et al.[19]. Peaks at 2908 cm1 and 1084 cm1 were modulus. This failure might be attributed to the environ-
attributed to the C-H stretching and CO stretching, mental effects such as rain fall and winds that act as
respectively, whereas the peaks at 1324 cm1 and 829 cm1 external forces to break the weak PVOH=BWF blend films.
were due to the C-H bending. Additionally, the reduction of tensile properties could be
The spectra of rambutan waste flour (Fig. 1b) were
similar to the spectra of banana waste flour (Fig. 1d), but
rambutan waste flour has a peak at 1717 cm1 that was
assumed to arise due to carbonyl group C=O stretching
(Fig. 1). In the spectra of rambutan waste flour (Fig. 1b)
and banana waste flour (Fig. 1d), the broad and wide
absorption band around 3421 cm1 arose from OH group
stretching vibrations. The peaks at 1052 cm1 are attribu-
ted to the stretching vibration of CO in COH groups.
In the IR spectra of the blends (Fig. 1c and Fig. 1d), the
entire characteristic spectrum of the blends seems to
overlap compared to a single polymer component. The
major OH group appearing in PVOH (Fig. 1a) film at
3245 cm1 and in rambutan waste flour (Fig. 1b) and
banana waste flour (Fig. 1d) at 3421 cm1 was prominent
in both PVOH=rambutan waste flour and PVOH=BWF
blends (peak at 3261 cm1 for PVOH=RWF and
3273 cm1 for PVOH=BWF), confirming the interaction
of different -OH groups in the TFWF and PVOH in the
blends. A similar shift was reported in for gellan and
PVA blends[20].

Natural Weathering
There is a limited number of studies on the bio-
degradability of materials based natural weathering. In
this study, the natural weathering was done to determine
the durability of the material in a natural condition. The
common environmental effects are sunlight, rain fall,
dew, and winds. Schiers[21] reported that the ultraviolet
(UV) ray from the sunlight is the most common cause
of the deterioration of polymer mechanical properties,
leading to cracking or catastrophic failure of the
product when polymer particles are exposed to natural
weathering.
Table 1 shows the tensile properties of PVOH=TFWF
blends after being subjected to natural weathering for 1
month. The tensile strength and elongation at break of
the PVOH=RWF blend film and the PVOH=BWF blend
film decreased significantly after being subjected to natural
weathering. In contrast, the tensile modulus of the PVOH=
RWF blend film and PVOH=BWF blend film increased FIG. 2. Micrographs of PVOH (a) before, (b) after 1 month of natural
after being subjected to natural weathering for 1 month. weathering, and (c) detailed micrograph at 200  magnification.
710 O. X. ZHONG ET AL.

attributed to the breaking down of long molecular chains Further evidence of the degradation of PVOH=RWF
in PVOH. blends and PVOH=BWF blends was provided by the
The tensile modulus of the PVOH=TFWF blends SEM micrographs. Figures 2–4 show the SEM micrograph
increased after being subjected to natural weathering for of PVOH, PVOH=RWF, and PVOH=BWF films after 1
1 month, indicating that the PVOH=TFWF blends become month of natural weathering. Severe deterioration
stiff due to the stiffening effect of the TFWF. According to occurred on the surface of all weathered PVOH=TFWF
Andrady et al.[22], the cross-linking of polyethylene tends to blends. In addition, there were many pores (Fig. 4b) and
make the material brittle when undergoing the oxidative cracks (Fig. 3b) widely spread throughout the surface
scission process. This reaction could explain the dramatic of the weathered PVOH=TFWF blends. This structure
drop of the elongation at break and the increment of tensile correlates with the dramatic reduction of tensile properties
modulus for both PVOH=RWF blends and PVOH=BWF of the PVOH=TFWF blends. Danjaji et al.[23] also
blends after exposure to natural weathering. reported that cracks appeared on the surface of the

FIG. 3. Micrographs of PVOH=RWF at 6:4 weight ratio (a) before, (b) FIG. 4. Micrographs of PVOH=BWF at 6:4 weight ratio (a) before, (b)
after 1 month of natural weathering, and (c) detailed micrograph at after 1 month of natural weathering, and (c) detailed micrograph at
200  magnification. 100  magnification.
 PVA AND FRUIT WASTE FLOUR IN BIODEGRADABLE POLYMER FILMS 711

LLDPE=sago starch blends upon exposure to natural 8. Ramaraj, B. Modified poly(vinyl alcohol) and coconut shell powder
weathering. composite films: Physico-mechanical, thermal properties, and swelling
studies. Polym. Plast. Technol. Eng. 2006, 45, 1227–1231.
9. Ozaki, S.K.; Monteiro, M.B.B.; Yano, H.; Imamura, Y.; Souza, M.F.
CONCLUSIONS Biodegradable composites from waste wood and poly(vinyl alcohol).
Polym. Degrad. Stab. 2005, 87, 293–299.
Two series of blend films were prepared from rambutan
10. Tang, S.; Zou, P.; Xiong, H.; Tang, H. Effect of nano-SiO2 on the per-
waste flour (RWF) and banana waste flour (BWF) with formance of starch=polyvinyl alcohol blend films. Carb. Polym. 2008,
PVOH by a solution casting method. These blends showed 72, 521–526.
that the tensile strength and elongation at break decreased, 11. Parra, D.F.; Tadini, C.C.; Donce, P.; Lugao, A.B. Mechanical proper-
but the tensile modulus and water uptake increased with ties and water vapor transmission in some blends of cassava starch
edible films. Carb. Polym. 2004, 58, 475–481.
increasing tropical fruit waste flour (TFWF) content. More
12. Chen, Y.; Cao, X.; Chang, P.R.; Huneault, M.A. Comparative study
interestingly, the PVOH=rambutan waste flour film exhib- on the films of (polyvinyl alcohol)=pea starch nanocrystals and
ited higher tensile strength, elongation at break, and tensile poly(vinyl alcohol)=native pea starch. Carb. Polym. 2008, 73, 8–17.
modulus, but it showed lower water uptake than the 13. Morreale, M.; Scaffaro, R.; Maio, A.; Mantia, F.P.L. Effect of adding
PVOH=banana waste flour film. This difference was due wood flour to the physical properties of a biodegradable polymer.
Compos. Pt. A 2008, 39, 503–513.
to the rambutan waste flour having better compatibility
14. Rahman, W.A.W.A.; Ali, R.R.; Zakaria, N. Studies on Biodegrad-
and stronger interactions with the PVOH than the banana ability, Morphology and Mechanical Properties of Low Density
waste flour. Polyethylene=Sago Based Blends, 1st International Conference on
Natural Resources Engineering & Technology, Putrajaya, Malaysia,
July 24–25, 2006.
ACKNOWLEDGMENT
15. Elizondo, N.J.; Sobral, P.J.A.; Menegalli, F.C. Development of films
The authors gratefully acknowledge the financial sup- based on blends of cruentus flour and poly(vinyl alcohol). Carb.
port from a USM fellowship and Research University Polym. 2009, 75, 592–598.
Grant (account no.: 1001=PBAHAN=814065). 16. Zabel, R.A., Morrell, J.J. Wood Microbiology: Decay and its Preven-
tion, Academic Press: San Diego, 1992.
17. Khachatourians, G.G.; Qazi, S.S. Entomopathogenic Fungi: Bio-
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