Carbohydrate Polymers 211 (2019) 204–208

Contents lists available at ScienceDirect

Carbohydrate Polymers
journal homepage: www.elsevier.com/locate/carbpol

Preparation and properties of lignocellulosic fiber/CaCO3/thermoplastic T

starch composites
Wenxi Cheng
School of Materials Science and Engineering, Henan University of Technology, Zhengzhou 450001, China

A R T I C LE I N FO A B S T R A C T

Keywords: Lignocellulosic fiber (LCF)/CaCO3 (CG)/thermoplastic starch (TPS) composites were prepared by blending LCF/
Thermoplastic starch CG hybrid (82/18, g/g) with glycerin and corn starch in different weight ratios (0/35/100, 27/35/100, 54/35/
Lignocellulosic fiber 100 and 81/35/100, g/g/g) at 130℃, which were then characterized by rheology, XRD, SEM and DSC analysis,
CaCO3 tensile test and soil burial test. When the dosage of LCF/CG was not more than 54 g, LCF and CG in LCF/CG/TPS
Torque rheology
composites were well dispersed, and the corresponding composites had better rheological properties. XRD re-
Preparation and properties
sults showed that the crystallinity of TPS in the presence of LCF/CG was significantly reduced after melt blending
process, which caused by the inhibition effect of LCF on the crystallization of TPS. The tensile test results showed
that the tensile strength, modulus and elongation at break of LCF/CG/TPS composite were better than those of
pure TPS. Besides, due to the looser structures, LCF/CG/TPS composites biodegraded faster than pure TPS.

1. Introduction
Entering the twenty-first century, people’s awareness of environ-
mental protection has gradually increased. Sustainable development of
society and its environmental, resource and economic issues are in-
creasingly becoming the concern of the whole society, so the develop-
ment and use of renewable resources instead of oil and other non-re-
newable resources has become a common understanding of the world
(Corre, Bras, & Dufresne, 2010).
Starch is abundant in the roots, stems and leaves of wheat, corn and
potato, and it is a kind of natural macromolecule widely existing in
nature. However, because of the large number of hydrogen bonds be-
tween starch molecules, starch begins to decompose before melting.
Therefore, native starch cannot be used directly as a plastics material.
Plasticizers are incorporated into a starch matrix to enhance the flex-
ibility and processability by increasing the spacing between molecular
chains and increasing the segmental mobility, commonly through re-
ducing the H-bonding between the polymer chains (Juansang et al.,
2017). By adding plasticizer into starch, the starch has thermoplasticity,
which makes it possible to industrialize the processing of starch. Gly-
cerol and water are the most often used starch plasticizers, but other
polyalcohols (e.g. xylitol, sorbitol), amides (e.g. urea, formamide),
amines (e.g. ethanolamine), and polycarboxylic acids (e.g. citric acid)
are also applied (Niazi, Zijlstra, & Broekhuis, 2015). When starches are
treated with a plasticizer under heat and shear conditions, granules of
starch undergoes disruption leading to a homogeneous melt known as
thermoplastic starch (TPS). TPS had be processed via various methods,
such as extrusion (Ghanbari, Tabarsa, Ashori, Alireza, & Mashkour,
2018), blowning (Dang & Yoksan, 2016), casting (Ostafińska et al.,
2017) and so on. However, due to the poor mechanical properties and
water resistance of TPS, the popularization and application of TPS are
affected.
The mechanical properties and water resistance of TPS can be ef-
fectively improved by adding inorganic mineral materials. The com-
monly used inorganic minerals include montmorillonite (Qiao, Jiang, &
Sun, 2005), kaolin (Kaewtatip & Tanrattanakul, 2012) and rectorite
(Chang, Wu, & Anderson, 2012), the produced nanocomposite resulted
an increasing of mechanical and thermal resistance properties respect
to the neat TPS. Campos-Requena, Rivas, Pérez, Figueroa, and
Sanfuentes (2017) prepared TPS/montmorillonite nanocomposite films
by extrusion method, the nanocomposites showed intercalated/ex-
foliated morphology, resulting an increasing of mechanical and thermal
resistance properties respect to the neat TPS.
Adding fibers to TPS is one of the ideal reinforcement methods.
Compared with synthetic fibers, TPS reinforced by natural plant fibers
has the following advantages: from plants, green and natural, com-
pletely degradable and not polluting the environment, low cost, good
compatibility with starch. At present, plant fibers such as cotton
(Prachayawamkora, Ruttanabus, & Boonsom, 2011), hemp (Averous &
Boquillon, 2004), corn peel (Mondragon, Arroyo, & Romero-Garcia,
2008), rice straw (Kaushik, Singh, & Verma, 2010), husk fiber (Lomeli-
Ramirez, Kestur, & Manriquez-Gonzdlez, 2014), luffa fiber (Kaewtatip

E-mail address: wenxi_cheng@haut.edu.cn.

https://doi.org/10.1016/j.carbpol.2019.01.062
Received 12 November 2018; Received in revised form 17 January 2019; Accepted 17 January 2019
Available online 22 January 2019
0144-8617/ © 2019 Published by Elsevier Ltd.
W. Cheng
& Thongmee, 2012), had been used as reinforcers to prepare TPS
composite plastics. The tensile strength and modulus of elasticity of
modified TPS were usually increased, but the elasticity was decreased.
In addition to the original ecology, nano-scale cellulose fibers were
also used to modify TPS (Balakrishnan, Sreekala, Kunaver, Huskić, &
Thomas, 2017; Fazeli, Keley, & Biazar, 2018), and TPS based nano-
biocomposites prepared with nanofibers showed better thermal and
mechanical properties.
Lignocellulose is the most abundant and biodegradable natural
macromolecule material in nature. Lignin, cellulose and hemicellulose
are the main components of lignocellulose (Rabemanolontsoa & Saka,
2016; Rangan, Manchiganti, Thilaividankan, Kestur, & Menon, 2017;
Zhang et al., 2018). They have the advantages of porous, large specific
surface area, renewable cycle, easy degradation, low price and rich
chemical functional groups. They will not bring secondary pollution to
the environment. Under the situation of rapid consumption of resources
and deterioration of environment in the world today, it is of great
strategic significance to pay attention to the development of renewable
lignocellulose resources (Hou, Zhang, & Qiu, 2017). Lignocellulose
fiber (LCF) have received considerable attention as a reinforcing agent
in thermoplastic composites, such as poly-lactic acid, polycaprolactone,
polyamide, PET (Dhakal et al., 2018; Jayamani, Hamdan, Rahman, &
Bakri, 2015; Oliver-Ortega et al., 2018; Santos, Rodrigues, Ramires,
Ruvolo-Filho, & Frollini, 2015). Using cheaper and alternative LCF to-
gether with achieving higher product titres have been identified as
potential strategies (Nieder-Heitmann, Haigh, & Görgens, 2018).
There is a kind of LCF and non-metallic mineral ultrafine powder
hybrid, which is mainly used in concrete mortar, gypsum products,
wood mortar sponge, asphalt road and other fields. The LCF composite
might show different effect on TPS. In this paper, TPS was modified
with LCF/CaCO3 (CG) hybrid and characterized via different methods.
2. Experimental part
2.1. Main raw materials
Corn starch (food grade, 12 ± 1% water, 0.4% protein, 0.2% ash,
and 26 ± 1% amylose, Henan Yongchang Feitian Starch Sugar Co.,
Ltd) and LCF/CG hybrid (LCF: from natural wood, average length < 6
mm; CG: precipitated, content: 18%; PH: 7.0 + 1.0, oil absorption rate:
not less than 5 times of fiber quality, water content: < 5%, heat re-
sistance: 230 (short time up to 280), Foshan Tianze Qingyang Chemical
Technology Co., Ltd.) were dried to remove the moisture at 60 °C for
24 h. Glycerin (food grade, Aladdin biochemical Polytron Technologies
Inc, Shanghai) was used without further treatment.
2.2. Composite preparing and sample obtaining
Corn starch and glycerin (100/35, g/g) were firstly mixed in a high
speed mixer (GH-10, Beijing Zedao Machinery Co., Ltd.) at 500 rpm for
5 min at room temperature, and then different weight of LCF/CG hybrid
(0, 27 g, 54 g or 81 g) was then added and mixed for 5 min. The ob-
tained mixture was subsequently blended at 130 °C and 20 rpm for
500 s with a torque rheometer (RM-200C,Harper Harbin Electrical
Technology Co., Ltd.), thus LCF/CG/TPS composites were obtained,
and coded as TPS, LCF/CG/TPS27, LCF/CG/TPS54 and LCF/CG/TPS81.
Besides, LCF/TPS (44.3/135, g/g) and CG/TPS (9.7/135, g/g) were
prepared according to the ratio of LCF/CG/TPS54 with the same
method.
The specimens for the mechanical characterization (ASTM D638-
2003) were obtained by means of a precision injection molding ma-
chine (TW1580, Ningbo general plastics machinery manufacturing
company, clamping pressure: 40 t).
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Carbohydrate Polymers 211 (2019) 204–208
2.3. Scanning electron microscopy (SEM) analysis
SEM was conducted on a FEI INSPECT F50 (USA) at an acceleration
voltage of 5 kV and a working distance of 14 mm. Samples were cross
sectiond after immersion in liquid nitrogen and subsequently sputtered
with a gold-palladium mixture under vacuum before their morphology
was examined using SEM.
2.4. X-ray diffraction (XRD) analysis
Samples were placed in a sample holder for XRD. The native corn
starch powder was packed tightly in the sample holder, all samples
were placed in an environment with 53% humidity for one day before
testing. XRD patterns were recorded in the reflection mode at an an-
gular range of 5–40° (2θ) at the ambient temperature by a Rigaku D
diffractometer (Japan), using copper radiation Ka (k = 1.5418 Å), vol-
tage of 40 kV and operation currentof 30 mA.
2.5. Differential scanning calorimetry (DSC) analysis
DSC was used to measure the thermal transitions of TPS and LCF/
CGTPS composites. The test was performed with a DSC200F3,
NETZSCH (Germany) differential scanning calorimeter equipment,
fitted with a nitrogen based cooling system. All the measurements were
performed in the temperature range of 25 to + 200 °C at a heating rate
of 10 °C/min in a unsealed pan correspond to first heating.
2.6. Tensile mechanical characterization
All samples were placed in an environment with 53% humidity for
one week before the testing was performed. Tensile testing (ASTM
D638-2003) of samples (type IV) was determined in an Instron 5567
tension machine (Carton, MA, USA) at a crosshead speed of 10 mm/min
at 25 °C. The data was the average of 7 specimens in each treatment.
Tensile strength and strain were directly obtained from this testing.
2.7. Biodegradability test
The biodegradability of samples was investigated with natural soil
burial test (Maran, Sivakumar, Thirugnanasambandham, & Sridhar,
2014). The pH of the soil was 6.7. The soil was kept moist by sprinkling
water at a regular time interval to maintain 20–40% humidity. The
temperature conditions of compost soil at T = 30 ± 2 ℃. the plastic
samples were cut into 10 mm × 20 mm pieces. Every 7 days, five spe-
cimens are removed from the soil, then washed in distilled water and
dried at 60 ± 2 ℃ for 24 h. Finally, the specimens are weighted and
compared with specimens before testing. The percentage weight loss is
calculated using the following equation:
W0-W1
WL(%) = × 100
W0
where W0 is the initial mass, W1 is the mass after degradation. The
weight loss (WL, %) is the average of at least five specimens of each
sample.
3. Results and discuss
3.1. Torque rheological property analysis
Fig.1 listed the torque rheological curves of TPS and LCF/CG/TPS
composites. As shown in Fig. 1, it can be seen that the peak torque and
equilibrium torque of the samples containing LCF/CG hybrid are sig-
nificantly higher than TPS. This indicates that the addition of LCF/CG
hybrid has a significant effect on the rheological properties of the LCF/
CG/TPS composites. The peak torque and the balance torque of TPS are
40 N.m and 16.5 N.m respectively. When 27 g (or 54 g) LCF/CG hybrid
W. Cheng Carbohydrate Polymers 211 (2019) 204–208

Fig. 1. Torque rheological curves of TPS and LCF/CG/TPS composites.

was blended with starch and glycerol (LCF/CG/TPS27), the peak torque Fig. 3. XRD curves of TPS, LCF/CG hybrid, LCF/CG/TPS composites, LCF/TPS
and equilibrium torque of the sample increased to 60 N.m and 23.3 N.m and CG/TPS.
(or 91 N.m and 29.9 N.m). But when the blended LCF/CG hybrid in-
creased to 81 g, the peak torque and equilibrium torque of the sample
As can be seen from Fig. 2b, the cross section section of pure TPS is
(LCF/CG/TPS81) were sharply increased to 121 N.m and 49.3 N.m, and
basically flat, and some unplasticized natural starch granules can be
the tie to reach equilibrium torque of the sample became longer, in-
observed. Fig. 2c shows that the cross section section of LCF/CG/TPS27
dicating that LCF/CG/TPS composites had better rheological properties
was close to that of pure TPS, but a few fibrous processes can be seen on
when the dosage of LCF/CG hybrid was less than 54 g. This may be due
the cross section, which belonged to LCF coated by TPS matrix, in-
to the high degree winding of LCF in LCF/CG/TPS81.
dicating that the compatibility between LCF and TPS matrix was good.
It can be seen from Fig. 2d that LCF was still well dispersed in the TPS
matrix for LCF/CG/TPS54, but on the cross section, there's a lot of fiber-
3.2. Cross section morphology observation
shaped bulges, showing the good reinforcing and toughening effect of
LCF on TPS matrix. As the dosage of LCF/CG hybrid increased to 81 g,
The SEM cross section images of LCF/CG hybrid, TPS and LCF/CG/
there were many clumps on the cross-section of LCF/CG/TPS81
TPS composites are shown in Fig. 2. AS shown in Fig. 2a, LCF/CG hy-
(Fig. 2e), indicating that LCF was agglomerated and poorly dispersed in
brid owned two kinds of structures, i.e., fibrous LCF and granular CG.

Fig. 2. SEM cross section images of LCF/CG hybrid (a), TPS (b), LCF/CG/TPS27 (c), LCF/CG/TPS54 (d) and LCF/CG/TPS (e).

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W. Cheng Carbohydrate Polymers 211 (2019) 204–208

the sample, which further verified that the TPS composites with high Table 1
LCF/CG hybrid dosage were easy to disperse unevenly and had poor Tensile strength, modulus of elasticity and elongation at break data of TPS and
rheological properties LCF/CG//TPSs.
Sample Tensile strength/MPa Modulus/MPa Elongation at break/%
3.3. Crystallinity
TPS 6.52 ± 0.2 41.70 ± 2 2.60 ± 0.2
LCF/CG/TPS27 8.41 ± 0.2 378.3 ± 5 7.21 ± 0.2
Fig. 3 shows XRD curves of TPS, LCF/CG hybrid, LCF/CG/TPS
LCF/CG/TPS54 12.15 ± 0.2 505.6 ± 5 9.43 ± 0.2
composites, LCF/TPS and CG/TPS. As can be seen from Fig. 3, TPS had LCF/CG/TPS81 8.70 ± 0.2 269.1 ± 5 5.67 ± 0.2
a strong 2θ peak at 13.6° and 21.1°, which was the characteristic peak
of V-type crystal formed during thermo-mechanical processing
(Ghanbari et al., 2018). LCF/CG hybrid had a strong 2θ peak at 22.7°, dosage of LCF/CG hybrid increased from 27 g to 81 g, the values of
which was the 002 crystal diffraction peak of lignocellulose, a sharp tensile strength, elastic modulus and elongation at break of LCF/CG/
and strong 2θ peak at 31.2°, which was the typical peak of CaCO3, TPS composites first increased and then decreased, reaching the max-
confirming the composite of LCF/CG hybrid. When LCF/CG hybrid was imum values at 54 g, which were 12.15 MPa, 505.6 MPa and 9.43%,
blended with TPS, the 2θ peaks at 21.1° and 22.7° obviously blunted, respectively, 1.86, 12.11 and 3.63 times as large as those of TPS. It was
indicating that most of the crystal structures of LCF and TPS were de- because that LCF were well dispersed in TPS matrix at low LCF/CG
stroyed by melt blending process, showing the great effect of LCF/CG hybrid dosage for TPS composites, such as LCF/CG/TPS27 and LCF/
hybrid on TPS in crystallinity. CG/TPS54, therefore, LCF played a good toughening and reinforcing
In order to further analyze whether LCF or CG hindered the crys- effect, while for LCF/CG/TPS composite with high LCF/CG hybrid do-
tallization of TPS, LCF/TPS and CG/TPS were prepared and their XRD sage, such as LCF/CG/TPS81, most of LCF winded and resulted in poor
curves were shown in Fig. 3. It can be seen from Fig. 3 that 2θ peaks at reinforcing effect. The effect of LCF/CG hybrid on the strain and tress of
13.6° and 21.1° were still conspicuous in the curve of CG/TPS. While in TPS was different from pure fiber (Fazeli, Florez, & Simão, 2019) or
the curve of LCF/TPS, 2θ peak at 21.1° became weaker and 2θ peak at inorganic particles (Kaewtatip & Tanrattanakul, 2012; Chang et al.,
13.6° almost disappear. This indicated that LCF was the main factor 2012) at high dosage, the later two kinds of materials generally in-
hindering the crystallization of TPS, which might be due to their similar creased strength and decreased toughness.
molecular structures of LCF and starch.
3.6. Biodegradability test
3.4. DSC test
Fig. 5 showed the biodegradation curves of TPS and LCF/CG/TPS
Fig. 4 showed the DSC curves of TPS and LCF/CG/TPS composites.
composites. As shown in Fig. 5, the decomposition rates of LCF/CG/TPS
As shown in Fig.4, pure TPS had a strong and wide melting heat ab-
composites were faster than pure TPS, and the degradation rate in-
sorption peak at 63.4 °C, near to that in the reference (Ghanbari et al.,
creased with the increase of LCF/CG hybrid dosage. For example, after
2018), which was 86.99 °C. When TPS was blended with LCF/CG hy-
28 days, the residual weight of LCF/CG/TPS27, LCF/CG/TPS54 and
brid, the melting heat absorption peaks of TPS composites became
LCF/CG/TPS81 were 50.35%, 45.45% and 41.2%, respectively. This is
weaker and wider, and increasing the LCF/CG hybrid dosage adversely
mainly due to the different water swelling rates of LCF/CG hybrid and
affected Tm of composites. This is because that the crystallinity of LCF/
TPS. When the samples swelled in the soil, the higher the amount of
CG/TPS composite decreased with increasing the added LCF/CG hybrid
LCF/CG hybrid, the looser the sample becomes, which is conducive to
dosage.
the invasion of microorganisms into the sample, thus improving its
degradation rate (Alvarez, Ruseckaite, & Vázquez, 2006).
3.5. Mechanical properties

Table 1 lists the data of tensile strength, elastic modulus and elon-
gation at break of TPS and LCF/CG//TPS composites. As can be seen
from Table 1, the tensile strength, elastic modulus and elongation at
break of pure TPS were the worst, which were 6.52 MPa, 41.70 MPa
and 2.60%. When TPS was blended with LCF/CG hybrid, the produced
samples showed better performance on tensile properties, and as the
4. Conclusion
LCF/CG/TPS composites with wide range and high content of LCF/
CG hybrid (0, 27 g, 54 g, and 81 g per 100 g starch/35 g glycerin) were
successfully prepared with a torque rheometer. LCF and CG were

Fig. 4. DSC curves of TPS and LCF/CG/TPS composites. Fig. 5. Biodegradation of TPS and LCF/CG/TPS composites.

207
W. Cheng
homogeneously dispersed in the TPS matrix until the dosage of LCF/CG
hybrid was above 54 g, at the same time, the responsive LCF/CG/TPS
composites showed good rheological properties. The tensile strength,
Young's modulus and elongation at break of LCF/CG/TPS composites
first increased with the raise dosage of LCF/CG hybrid, reaching the
maximum values at 54 g, which were 1.86, 12.11 and 3.63 times as
large as those of TPS, after that decreased. The crystallinities of TPS
obviously decreased in LCF/CG/TPS composites by the blending pro-
cess due to the hindering effect of LCF on the crystallization of TPS. The
biodegradation rates of composites increased with the increasing of
LCF/CG hybrid dosage.
Acknowledgements
This work was supported by Henan province education department
[grant numbers 15A430020] and Henan University of Technology
[grant numbers 2015XTCX08].
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