Polymer-Plastics Technology and Materials

ISSN: 2574-0881 (Print) 2574-089X (Online) Journal homepage: https://www.tandfonline.com/loi/lpte21

Effect of microcrystalline cellulose on

characteristics of cassava starch-based bioplastic

Akbar Hanif Dawam Abdullah, Oceu Dwi Putri, Anti Khoerul Fikriyyah, Rossy
Choerun Nissa & Sinda Intadiana

To cite this article: Akbar Hanif Dawam Abdullah, Oceu Dwi Putri, Anti Khoerul Fikriyyah,
Rossy Choerun Nissa & Sinda Intadiana (2020): Effect of microcrystalline cellulose on
characteristics of cassava starch-based bioplastic, Polymer-Plastics Technology and Materials,
DOI: 10.1080/25740881.2020.1738465

To link to this article: https://doi.org/10.1080/25740881.2020.1738465

Published online: 11 Mar 2020.

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POLYMER-PLASTICS TECHNOLOGY AND MATERIALS
https://doi.org/10.1080/25740881.2020.1738465

Effect of microcrystalline cellulose on characteristics of cassava starch-based

bioplastic
Akbar Hanif Dawam Abdullaha, Oceu Dwi Putria, Anti Khoerul Fikriyyaha, Rossy Choerun Nissaa,
and Sinda Intadianab
a
Research Unit for Clean Technology, Indonesian Institute of Sciences, Bandung, Indonesia; bDepartment of Physic Education, Sultan Ageng
Tirtayasa University, Banten, Indonesia

ABSTRACT ARTICLE HISTORY

The vast consumption of conventional plastics has a significant effect on the environment Received 20 October 2019
that encourages the utilization of natural resources as the raw materials to substitute the Revised 13 January 2020
petroleum-based plastics. Poor mechanical and moisture barrier properties of starch-based Accepted 17 January 2020
bioplastics causing the development of modified starch-based bioplastics by incorporating KEYWORDS
reinforcing material. Microcrystalline cellulose (MCC) as a filler of thermoplastic starch shows Bioplastic; starch;
strong reinforcing ability and high surface area besides its renewability, biodegradability, microcrystalline cellulose;
and affordability compared to nanocellulose. This study aimed to investigate the effect of mechanical properties;
MCC on the physical, mechanical, and biodegradability properties of starch-based bioplastic. physical properties;
Bioplastic was prepared by melt-mixing starch and glycerol (3:1, w/w) with MCC (5%, 10%, biodegradability
15%, and 20%, w/w). Density and water contact angle of bioplastic increased with the
increase of MCC concentration. Conversely, the moisture content decreased with the
increase of MCC concentration. Mechanical properties evaluation showed that bioplastic
with the addition of MCC had higher tensile strength than that without MCC where 20%
MCC exhibited the highest tensile strength of 16.7 MPa with elongation of 1.31% and
Young’s modulus of 1.5 GPa. In addition, the decomposition temperature of bioplastic
with MCC slightly increased which indicated the higher stability. Cross-section micrograph
after tensile test showed that the visible inhomogeneous starch granules decreased with the
increase of MCC concentration. FTIR spectra exhibited that the intermolecular interaction in
bioplastics occurred through C-H, C = O, C-O-C, C-O-H, and O-H groups. In addition,
biodegradability tests of bioplastic showed that the growth of microbes increased in the
presence of MCC and microbes covered the bioplastic more than 60% in 21 days. The results
showed that MCC performed an important role to enhance the physical, mechanical, and
biodegradability properties of starch-based bioplastic.

CONTACT Akbar Hanif Dawam Abdullah akba001@lipi.go.id Research Unit for Clean Technology, Indonesian Institute of Sciences, Bandung,
Indonesia
© 2020 Taylor & Francis
2 A. H. D. ABDULLAH ET AL.
1. Introduction
Nowadays, plastic which initially only acts as a packaging
has become a daily necessity. The raw material used by
plastics is synthetic polymers from petroleum that cannot
be renewed and is a non-biodegradable material.[1] This can
cause environmental damage if plastic continues to be used
in everyday life because non-biodegradable plastics need
hundreds of years to fully decompose by microorganisms.
Meanwhile, burning plastic is also not a solution to destroy
it.[2] Indonesia is reported as the second-largest contributor
in the world after China which dumps plastic waste into the
ocean.[3] If this continues, it will threaten the entire marine
ecosystem. One effort that could be a solution to this
problem is to change conventional plastic packaging into
bioplastics based on natural resources that can be renewed
and can be degraded naturally.[4]
Bioplastics are designed to facilitate degradation
through enzymatic reactions of microorganisms such as
bacteria and fungi.[5] This is because bioplastics are made
from various types of natural polymers, one of which is
starch. Starch is a natural polymer that is close to the
properties of an ideal polymer that can be used to make
bioplastics.[6] However, bioplastics made from starch also
have disadvantages where high hydrophilicity and poor
mechanical properties. To overcome this weakness, the
addition of a reinforcing agent to the starch matrix which
can improve the mechanical properties of bioplastics is
necessary.[7] The employment of reinforcement agents
such as nanoclay,[8] lignocellulose,[9] passion fruit peel
flour,[10] and polylactid acid[11] has been investigated to
obtain bioplastics with enhanced mechanical properties.
In this matter, cellulose is reported as a noteworthy alter-
native material to reinforce bioplastics due to its abun-
dance in nature, biodegradability, mechanical properties,
and cost-effectiveness.[9]
Microcrystalline cellulose (MCC) has the potential to
be used as a reinforcing material for biopolymer. The
derivation of high-quality wood pulp that produces
crystalline cellulose can be fragmented into cellulose
fractions as a hydrolysis product. Native cellulose has
a theoretical modulus of 167.5 GPa which makes it one
of the strongest and stiffest existing natural fibers. The
diameter of MCC can be around 5–10 nm with a length
of 100 nm to several micrometers. Therefore, MCC has
a higher specific surface area than other cellulose fibers
which is good for improving the mechanical properties
of starch bioplastics.[12] However, the use of microcrys-
talline cellulose (MCC) as the reinforcement agent for
bioplastics was scarcely reported.
Thus, this study aimed to investigate the effect of MCC
as a reinforcement agent on the characteristics of cassava
starch-based bioplastics. The bioplastics were characterized
for their physical, mechanical, and biodegradability
properties.
2. Materials and methods
2.1. Materials
Cassava starch was supplied by PT. Surya Pati Kencana
(Pati, Indonesia). Glycerol, microcrystalline cellulose,
Potato Dextrose Agar (PDA), and Salt Agar (SA) were
purchased from Merck (Darmstadt, Germany).
2.2. Methods
2.2.1. Preparation of bioplastics
Bioplastics were prepared by mixing cassava starch
and glycerol with MCC. Concisely, cassava starch
and glycerol were pre-mixed with the ratio of 3:1
(w/w) in a Phillips Blender HR2118/01 for ± 3 min.
MCC was added to the pre-mixtures at 5%, 10%, 15%,
and 20% (w/w). The mixtures were melt-mixed sub-
sequently in a Labo Plastomil 30R150 Toyoseiki mixer
at 130°C for 8 min. Bioplastic sheets were compres-
sion molded from the mixtures (± 5 g) under a load of
40 kgf/cm2 at 135°C for 10 min.
2.2.2. Characterization of bioplastics
2.2.2.1. Density, moisture content, and contact angle
of bioplastics. The density of the bioplastics was deter-
mined according to ASTM D792-08 (2008). A 25 mL
pycnometer and a water bath were used at a constant
temperature of 25°C. The moisture content was evalu-
ated by drying the samples at 105°C for 24 h and cooling
in a desiccator for 1 h at room temperature. The weight
of the samples before and after drying was measured to
determine the moisture content. The samples were
introduced to a controlled condition at 25°C and 55%
RH for 96 h before the drying process. Surface hydro-
phobicity was assessed by means of contact angle mea-
surement. The bioplastics (1 cm x 1 cm) were prepared
to measure the water contact angle in ambient condition.
To determine the average static contact angle, droplets of
water (±5 µL) were dropped onto the surface of bioplas-
tics at three different spots on the sample surface.
2.2.2.2. Microstructure of bioplastics. Cross-section
morphology of bioplastics were examined by a Jeol JSM-
IT300 Scanning Electron Microscope (Tokyo, Japan).
Prior to analysis, the thin layers of gold (~10 nm) were
sputtered on the surface of the samples. The analyses were
performed under an accelerating voltage of 20 kV.

2.2.2.3. FTIR analysis of bioplastics. FTIR spectra of
bioplastics were recorded at 4 cm−1 scanning resolution
by using a Thermo Scientific Nicolet iS5 ATR-FTIR
spectrometer (Madison, WI, USA) at the range of
wavenumber from 4000 cm−1 to 400 cm−1 with an
average of 16 scans for spectrum integration.
2.2.2.4. Mechanical properties of bioplastics. The ten-
sile strength, elongation, and Young’s modulus of bio-
plastics were measured according to ASTM D882-12
(2012) using a universal testing machine (UCT-5T,
Orientec Co. Ltd, Japan) with initial gauge separation
of 100 mm and the crosshead speed of 50 mm/min with
mean ± SD (n = 3). Prior to testing, bioplastic samples
were stored in a condition of 25°C and 55% relative
humidity for 24 h.
2.2.2.5. Thermal properties of bioplastics. To deter-
mine the effect of MCC on the thermal stability of
bioplastics, thermogravimetric analysis was carried out
by a Netzsch TG 209 F1 Libra (Selb, Germany) appa-
ratus from 40°C to 500°C with a heating rate of 10 K/
min under inert atmosphere (N2 flow 20 ml/min).
2.2.2.6. Biodegradability of bioplastics. Bioplastics
degradation was evaluated by using Aspergillus Niger
in a potato dextrose agar (PDA) medium. A 3.9 g of
potato dextrose agar (PDA) and salt agar (SA) dissolved
in 100 mL distilled water and poured into petri dishes.
Aspergillus Niger were dropped and spread on each
sample surface (3 x 3 cm) placed on the medium by
Figure 1. Density of bioplastics with different MCC content.
POLYMER-PLASTICS TECHNOLOGY AND MATERIALS 3
using a disposable sterile spreader followed by incuba-
tion at 37°C and 90% RH for 21 days. The growth of
microbes on the samples was observed to determine the
microbial biodegradability at an interval time of 3 days.
3. Results and discussions
Bioplastics density is shown in Figure 1. The density
increased with the increase in MCC concentration. It
might be attributed to the increase of thickness of
bioplastics which corresponded to the higher content
of MCC as a filler in the starch matrix. Furthermore,
hydrophobicity of bioplastics also increased which
shown by the increase of water contact angle that
increased along with the higher concentration of
MCC. Since the contact angle reflects the surface char-
acteristic of bioplastics,[10] hence, hydrophobicity of
bioplastics also increased which shown by the increase
of water contact angle that increased along with the
higher concentration of MCC (Table 1).
Since bioplastics were expected to be an alternative
for conventional plastics, it should be waterproof in
nature to prevent any leakage of liquid or solids packed
by these bioplastics. Therefore, lower moisture content
of bioplastics after the addition of MCC than its native
bioplastics is necessary. In general, reinforcement of the
bioplastics structure by adding some reinforcement
agents would decrease the uptake of water or moisture
in the environment due to the low flexibility of the
reinforcement agents.[9] As shown in Figure 2, the
moisture content of bioplastics clearly depended on
4 A. H. D. ABDULLAH ET AL.

Table 1. Contact angle of bioplastics with different MCC the MCC content in the bioplastics. With the increase
content. in MCC concentration, the moisture content of bio-
MCC content (%) Contact angle (°) ± SD plastics decreased. Bioplastic without MCC had
0 50.2 2.28 a moisture content of 20.33%, whereas the addition of
5 53.5 1.61
10 55.7 2.79 20% MCC decreased the moisture content to 9.16%.
15 63.5 2.29
20 65.9 3.02
The addition of MCC into bioplastic matrices was
responsible for the decrease of the moisture content

Figure 2. Moisture content of bioplastics with different MCC content.

Figure 3. Tensile strength (a), elongation (b), and Young’s modulus (c) of bioplastics with different MCC content.

Figure 4. TGA (a) and DTG (b) curves of bioplastics with different MCC content.
due to the ‘hydrophobic’ character of highly crystalline
of cellulose fibers in contrast with starch-glycerol
hydrophilic nature.[13] Thus, the moisture in the envir-
onment around the bioplastic difficult to pass through
the bioplastic matrices.
The influence of MCC on the mechanical properties
of bioplastics is depended on its moisture content
where the higher content of moisture would increase
the flexibility because water can act as a plasticizer.[14]
As depicted in Figure 3, with lower moisture content,
POLYMER-PLASTICS TECHNOLOGY AND MATERIALS 5
the tensile strength of bioplastics increased. On the
other hand, the addition of MCC reduced the elonga-
tion and increased the Young’s modulus. The increase
in tensile strength was attributed to the inherent adhe-
sion of the MCC-starch interface due to the chemical
similarity of starch and MCC.[13] Oppositely, the elon-
gation was decreased with the increase in MCC con-
tent. The reduction of elongation in the presence of
fibers in polymer matrices is a general tendency
observed in thermoplastic composites.[12] The volume
6 A. H. D. ABDULLAH ET AL.
fraction and the distribution of reinforcement agent in
the matrix affected the elongation at break in common
composites. The addition of a rigid reinforcement agent
could reduce the elongation due to the occurring of
stress concentrations.[15] Hence, the addition of MCC
could reduce the elongation of starch matrices. In case
of modulus, the higher concentration of MCC
increased the modulus. It suggested that the addition
of MCC to the starch matrices could increase its crys-
tallinity and increase the modulus significantly.[12]
Moreover, it also suggested that MCC was well dis-
persed in starch matrices due to its small size and
large specific surface area which resulted in a higher
length-to-diameter ratio of the reinforcing phase and
the formation of hydrogen bonds between starch and
MCC that caused the increase in modulus.[16,17]
Figure 4 illustrates the weight loss of bioplastics and
its derivation. All samples showed a relatively same
degradation stage. The first stage which is lower than
100°C indicated the mass loss due to the evaporation of
water and volatiles contained in the bioplastics.
Figure 5. SEM micrographs of bioplastics with (a) 0%, (b) 5%, (c) 10%, (d) 15%, and (d) 20% MCC content.
The second stage with the highest rate of degradation
at 250–400°C was attributed to the decarboxylation,
depolymerization, and decomposition of glycosyl
groups of starch matrix and MCC. At this stage, it
can be seen that there were two peaks in the DTG
curves of bioplastics after the addition of MCC.
According to Xian et al.[17], MCC exhibited the decom-
position temperature of 335°C. This explained that
the second lower peak at around 355–361°C was clearly
ascribed to the decomposition of MCC. Further degra-
dation stage from 400°C to 550°C was associated with
the residual weight of the polymer and the higher
amount of crystalline cellulose.[17] Moreover, the TGA
curves indicated that the decomposition of bioplastics
with MCC addition occurred at a relatively same tem-
perature around 312–317ºC which corresponded to the
temperature of thermal depolymerization of
polysaccharide[18], whereas the addition of 5% MCC
showed the highest decomposition temperature at
317.4ºC, owing to the high decomposition temperature
of MCC. These results indicated that the thermal

stability of bioplastics was slightly improved with the
addition of MCC due to the higher content of higher
thermal stability component in the bioplastics.
SEM micrographs of the bioplastic cross-section
after the tensile test are shown in Figure 5. Starch
granules were still visible indicated the incomplete gela-
tinization in the manufacturing process of
bioplastics.[19] Meanwhile, in Figure 5(b–e), MCC can
be differentiated from the darker color and it showed
a uniform dispersion of MCC in the starch matrix. The
alteration after MCC addition signified by the typical
plastic deformation where, throughout the tensile test,
MCC imposed the samples to experience shear
deformation.[17]
Figure 6 shows the FTIR spectra of bioplastics with
different MCC concentrations which exhibit similar
manners. The peaks at 996 cm−1 and 1015 cm−1
assigned for C–O–C bond stretching at β-(1-4)-
glycosidic of MCC and C–O–H bending of starch.
The absorption bands at 1151 cm−1 and 1079 cm−1
were ascribed to C–O–C pyranose ring. The broad
peak around 3000 to 3600 cm−1 was attributed to O–
H stretching from hydrogen bonding of starch and
glycerol, whereas a peak at 2929 cm−1 was attributed
to C–H stretching in the methyl and methylene
groups.[17,20] The similar manners exhibited by all
FTIR spectra indicated the similar chemical composi-
tions of bioplastics before and after addition of MCC.
Degradation of bioplastics is presented in Figure 7. It
can be seen that after 21 days of degradability test, all
samples showed changes in the appearance. An increase
in the biodegradation rate of bioplastics with MCC was
Figure 6. FTIR spectra of bioplastics with different MCC content.
POLYMER-PLASTICS TECHNOLOGY AND MATERIALS 7
expected. The samples were covered by microbes more
than 60% in 21 days which indicated the heavy growth
level of microbes. More clear degradation was obvious at
the high content of MCC shown the effective enzymatic
degradation that occurred in the samples with a high con-
centration of MCC. This occurrence might be attributed to
the increase of carbon sources in the samples when the
MCC was added and eventually resulted in the increase in
the biodegradation rate. It was due to the increase in the
hydrolysis of random chain scission which triggered the
reduction of rapid molecular weight. This molecular
weight reduction produced the smaller resulting molecules
which more sensitive to enzymatic attack and resulting in
faster degradation. Hence, bioplastics with high MCC
concentration exhibited faster degradation.[20]
4. Conclusions
MCC content influenced the physical, mechanical, and
biodegradability properties of starch-based bioplastics.
MCC was homogeneously dispersed in the starch
matrix with typical plastic deformation, where the
interaction between starch and MCC occurred through
physical interaction. MCC addition increased the ten-
sile strength and Young’s modulus and decreased the
elongation. The density and hydrophobicity also
increased with the increase of MCC content. The
higher content of MCC with higher thermal stability
properties in the bioplastics caused the improvement of
the thermal stability of starch-based bioplastics.
Moreover, MCC addition triggered the enzymatic
degradation more efficiently. These results indicated
8 A. H. D. ABDULLAH ET AL.
Figure 7. Degradation of bioplastics (a,f) 0%, (b,g) 5%, (c,h) 10%, (d,i) 15%, and (e,j) 20% of MCC addition exposed for (a–e) 0 day
and (f-j) 21 days.
MCC performed an important role to enhance the
physical, mechanical, and biodegradability properties
of starch-based bioplastic.
Acknowledgments
This study was supported by the Ministry of Research,
Technology and Higher Education of the Republic of
Indonesia, INSINAS Project fiscal year 2019 with grant num-
ber 010/P/RPL-LIPI/INSINAS-1/II/IV/2019.
Disclosure Statement
No potential conflict of interest was reported by the authors.
Funding
This work was supported by the Kementerian Riset
Teknologi Dan Pendidikan Tinggi Republik Indonesia [010/
P/RPL-LIPI/INSINAS-1/II/IV/2019].
Notes on contributors
Akbar Hanif Dawam Abdullah received his Ph. D. Degree in
materials engineering from Bandung Institute of Technology
in 2015. He is currently a professional researcher in Research
Unit for Clean Technology, Indonesian Institute of Sciences
(LIPI). His current research interests are bioplastic compo-
sites based on functional natural polymer.
Oceu Dwi Putri received her bachelor degree in chemistry
from Indonesia University of Education. She works for
Research Unit for Clean Technology, Indonesian Institute
of Sciences (LIPI) and her research interest focus on the
modification of functional properties of the starch-based
bioplastics. She is currently a master’s student majoring in
materials engineering at Sirindhorn International Institute of
Technology, Thammasat University, Thailand.
Anti Khoerul Fikriyyah received her bachelor degree in phy-
sics from State Islamic University of Sunan Gunung Djati.
She works for Research Unit for Clean Technology,
Indonesian Institute of Sciences (LIPI) and her research
interest focus on the processing technology of starch-based
bioplastics. She is currently a master’s student majoring in
energy security at Universitas Pertahanan Indonesia.
Rossy Choerun Nissa received her bachelor degree in food
technology from Pasundan University. She works for
Research Unit for Clean Technology, Indonesian Institute
of Sciences (LIPI) and her research interest focus on the
processing technology and antimicrobial properties of bio-
plastic composites based on functional natural polymer. She
is currently a master's student majoring in biotechnology at
Padjajaran University, Indonesia.
Sinda Intadiana received her bachelor degree in physics
education from Sultan Ageng Tirtayasa University. Her
research interest focus on the the improvement of mechanical
properties of starch-based bioplastics.
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