Fabrication and characterisation of

thermoplastic starch/poly(butylene succinate)

blends with maleated poly
(butylene succinate) as compatibiliser
Q. Yin*1,2, F. Chen1,2, H. Zhang1,2 and C. Liu1,2
Thermoplastic starch/poly(butylene succinate) (TPS/PBS), an entirely biodegradable polymer
blend, was prepared by a two-step extrusion method. Maleic anhydride grafted PBS (rPBS) was
successfully synthesised as an interfacial compatibiliser. The miscibility, morphology, thermal
behaviour and mechanical properties of the TPS/PBS blends were investigated. The results
demonstrated that the strength and elongation at break of TPS/PBS blends were greatly
increased with the addition of rPBS in PBS blends due to improved interfacial miscibility. Better
distribution and smaller phase domain were observed in the blends with higher content of
compatibilisers. The water resistance was also enhanced by incorporation of rPBS. It was
indicated that compatibilised TPS/PBS blends possessed a combination of good biodegrad-
ability, improved strength and high water resistance. TPS/PBS blend was expected to serve as a
promising packing material.
Keywords: Biodegradable, PBS, TPS, Compatibilisation, Water resistance

Introduction It is well known that mechanical properties decreased

In recent years, environmental concerns and shortage of
petroleum resources have driven efforts on the devel-
opment of biodegradable and renewable materials,
which are known as ‘green materials’. Starch based
bioplastics are attractive candidates due to its renew-
ability, low price and abundant availability. However,
thermoplastic starch (TPS) is sensitive to humidity and
has inferior mechanical properties in comparison with
the petroleum based polymers, limiting its applications.1
To improve the mechanical properties and water resist-
ance of TPS, many methods have been tried, such as
modifying the starch structure,2 blending with biode-
gradable polymers of PLA,3–6 PCL7–9 or PVA,10,11
reinforcing by fibres or nanoclays, and adding
compatibilisers.
Poly(butylene succinate) (PBS), an available aliphatic
polyester, exhibits excellent biodegradability, flexibility
and high heat distortion temperature.12 Great
progress has recently been made in renewable based PBS
with a breakthrough biotechnology in commercial
production.13 Hence, it is expected to be a promising
eco-friendly alternative to blend with starch.
1
The State Key Laboratory of Bioreactor Engineering, East China
University of Science and Technology, Shanghai 200237, China
2
Key Laboratory for Ultrafine Materials of Ministry of Education, School of
Materials Science and Engineering, East China University of Science and
Technology, Shanghai 200237, China
*Corresponding author, email yinqunjie0911@163.com
obviously by directly blending biopolymers with TPS.
The major problem of this blend system is the poor
interfacial interaction between hydrophobic biopoly-
mers and hydrophilic TPS. To enhance the interfacial
interactions of TPS/PBS blends, reactive compatibilisers
are added by forming blocking or grafting copolymer at
the surface of the incompatible blends.14
Maleic anhydride (MAH) is the most commonly used
compatibiliser to be grafted onto the polymer backbone.
These grafted reactive functional groups can react with
the hydroxyl groups of starch to form covalent bonds
and thus achieve stronger interfacial adhesion. The
grafting of MAH onto PLA was first reported by Carl-
son et al.15,16 Michel et al.17 reported that starch blends
composed of MAH-g-PLA exhibited finer dispersed
phase in size of 1–3 mm and a dramatic improvement in
ductility. Ren et al.18 showed that the interfacial affinity
between TPS and synthetic polyesters was improved by
the compatibiliser. Wang et al.19 concluded that the
addition of starch and glycerol led to higher crystallinity
and lower crystallisation rate, while the crystal types and
crystallite sizes of PBS did not change. Reactive PBS
with terminal NCO groups was synthesised and blended
with PBS to enhance the miscibility between the two
phases.20 The mechanical properties and water resist-
ance were obviously improved after compatibilisation.
Kanitporn et al.21 demonstrated that starch-g-PBS was a
good compatibiliser for PBS and starch by promoting
strong interfacial adhesion. Recently, the MAH grafted
compatibilising technology had developed maturely.

Ñ Institute of Materials, Minerals and Mining 2015

Published by Maney on behalf of the Institute
Received 19 April 2015; accepted 07 July 2015
362 DOI 10.1179/1743289815Y.0000000031 Plastics, Rubber and Composites 2015 VOL 44 NO 9

However, few studies focused on the effect of the
interfacial compatibiliser MAH-g-PBS on starch/PBS
blend properties in detail.
The objectives of the present work were first to syn-
thesise MAH grafted PBS (MAH-g-PBS, rPBS) and
then with rPBS as an interfacial compatibiliser to pre-
pare the biodegradable TPS/PBS blends. In addition, the
effects of rPBS on the mechanical properties, thermal
behaviours, morphology and water absorption of TPS/
PBS blends were evaluated.
Experimental
Materials
PBS was purchased from Xinfu Company (Hangzhou,
China). Cassava starch was provided by Shengda Co.
Ltd (Gansu, China) with 12 wt-% moisture. Glycerol
was from Sino Chemical Reagent Co. Ltd. MAH was
purchased from Shanghai Ling Feng Chemical Reagent
Co. Ltd. Dicumyl peroxide as an initiator was obtained
from Aladdin Industrial Corporation (analytical re-
agent). Chloroform and methanol were supplied by
Shanghai Chemical Reagent Co. Ltd.
Fabrication of TPS/PBS blends
Cassava starch and glycerol were mixed in a high speed
mixer for 5 min. TPS and TPS/PBS blends were extruded
through a co-rotating twin screw extruder (SHJ-20,
China) with an L/D ratio of 46. The temperature profiles
from feed throat to die were 90–125?. Extruded strips
were cut into small cylinders and dried at 80? for 12 h.
TPS/PBS blends with different rPBS contents were
extruded through the twin screw extruder. Extrusion
process parameters were set as described above. Finally,
the blends were compression moulded at 135? for 2–5
min at 10 MPa for further experiment.
Fourier transform infrared spectroscopy
Fourier transform infrared spectroscopy (FTIR) of
purified PBS and maleated PBS was obtained with a
spectrometer Nicolet 6700 (USA).
Nuclear magnetic resonance spectroscopy
Chemical structure of MAH-g-PBS was confirmed by
1
H-NMR (nuclear magnetic resonance) at ambient
temperature on a 400 MHz Bruker spectrometer.
Mechanical properties
Blends were pressed with a flat sulphuration machine
into a sheet, and the mechanical property measurements
were performed at room temperature. Tensile strength,
modulus and elongation at break were measured on a
mechanical tensile tester (CMT6104-SANS, China)
according to GB/T 1040-2006 with the crosshead speed
of 10 mm min21. Each sample was tested five times, and
the average values were given.
Differential scanning calorimetry
The melting and crystallisation behaviour of TPS/PBS
blends were carried out on a differential scanning calori-
meter (DSC, Pyris Diamond, USA). The cold crystal-
lisation temperature (Tc), melting temperature (Tm),
crystallisation enthalpy (DHc) and melting enthalpy
(DHm) were determined from the second heating scan. An
empty high volume pan was used as a reference.
Yin et al. Fabrication and characterisation of TPS/PBS
Dynamic mechanical analysis
Dynamic mechanical analysis (DMA E4000, Rheology,
Japan) was used to investigate the glass transition tem-
perature (Tg) and compatibility of TPS/PBS. Glass
transition temperature was recorded as a function of
temperature.
Water absorption
Specimens (15 mm|15 mm|0.5 mm) in a rectangular
shape were first dried in a vacuum oven at 60? for 48 h
and weighed. The masses of specimens before and after
immersion for time i were designated as m0 and mi re-
spectively. Water absorption (W) was calculated as
equation (2):
Wi 2 W0
W ð%Þ ¼ £ 100% ð2Þ
W0
Scanning electron microscope
To obtain the natural fracture surface, samples were
kept in the liquid nitrogen to break. The dispersion of
the blends was observed with scanning electronic mi-
croscopy (SEM, Hitachi H-800, Japan) at an accelera-
tion voltage of 15 kV.
Results and discussion
Characterisation of rPBS
The FTIR spectra of PBS and rPBS are shown in
Fig. 1.Three representative absorption peaks at 2950,
1721 and 1162 cm21 were observed, which were assigned
to the -CH2- stretching, the -C ¼ O stretching vibration
and the asymmetric stretching of -CO respectively.24
Compared with the FTIR spectrum of PBS, a weak
absorption peak at 1633 cm21 was found in the spec-
trum of rPBS, which was ascribed to the symmetric
stretching of the anhydride groups of MAH. Although
the grafting ratio of MAH exhibited infinitesimally due
to the low content of MAH, the result was consistent
with the neutralisation titration result of Yogaraj et al.25
This further verified that anhydride groups of MAH had
been successfully grafted to the PBS.
Figure 2 represents the 1H-NMR spectra of the rPBS
and PBS. The signals at 4.12, 1.74 and 2.64 ppm were
characteristic protons of PBS molecules.26 In addition,
new peaks at 3.52 and 2.74 ppm were found in rPBS,
1 FTIR spectra of MAH-g-PBS (rPBS) and PBS
Plastics, Rubber and Composites 2015 VOL 44 NO 9 363
Yin et al. Fabrication and characterisation of TPS/PBS
1
2 H-NMR spectra for rPBS and PBS in CDCl3
which can be attributed to the signals from methine and
methylene protons of MAH ring. It was indicated
that chemical interactions occurred between the MAH
and PBS.
Mechanical properties
Figure 3 illustrates the mechanical properties of TPS/
PBS blends with different contents of rPBS. Without the
addition of rPBS, the tensile strength and elongation at
break of TPS/PBS (60/40) blend were only 6.4 MPa and
4% respectively. The inferior mechanical properties of
TPS/PBS were mainly due to its poor affinity between
the hydrophilic TPS and hydrophobic PBS.27 For starch
based TPS/PBS blends, even blended with a certain
3 Stress–strain curves of TPS/PBS blend with different contents of rPBS
364 Plastics, Rubber and Composites 2015 VOL 44
content of rPBS, the mechanical properties of the TPS/
PBS blends were slightly increased. The result suggested
that rPBS had little influence on improving the mech-
anical properties of TPS/PBS blends (rich TPS), which
was agreed with the report of Ren et al.18 It was con-
sidered that the amount of compatibilisers was too little
to form effective chemical bonds between starch and
PBS phase. On the contrary, TPS/PBS (40/60) blends
(rich PBS) exhibited a good flexibility with elongation
*20%, higher than the average value with the same TPS
content.28 More importantly, the tensile strength of
TPS/PBS (40/60) blends increased over twofold at the
same rPBS content. Interestingly, the mechanical prop-
erties of TPS/PBS blends (rich PBS) were improved
obviously with the introduction of rPBS. However, the
mechanical properties of the TPS/PBS blends (rich PBS)
were not altered obviously when rPBS content was fur-
ther increased from 5% to 10%. The result suggests that
rPBS has a good compatibilising effect. Additionally,
rPBS and PBS were thermodynamic miscible. Both of
them transferred stress effectively and enhanced the
interfacial adhesion between PBS and TPS.
Thermal properties and crystallisation
behaviour
PBS was reported to be a typical semicrystalline poly-
mer. It was said that the physical, mechanical and
thermal resistance properties of the polymer were
strongly dependent on the solid state morphology and its
crystallinity.12 In fact, the crystallisation of TPS is quite
complicated. It also varies with the category of starch,
the amount of plasticisers, storage time, temperature
and humidity. Figure 4 and Table 1 describe the crys-
tallisation behaviour of PBS, TPS and TPS/PBS blends.
NO 9
 Yin et al. Fabrication and characterisation of TPS/PBS

isothermally at the given cooling rate. Many authors

have explained double melting behaviour by the melt
recrystallisation model.30 The exothermic dip between
the double melting peaks was attributed to the recrys-
tallisation. L represented the lower melting temperature
of original crystals, H represented the higher melting
temperature of recrystallised crystals, and DT was the
difference between them (Table 1). The shoulder peaks
became more and more evident with the addition of
TPS. Meanwhile, both L and H temperatures shifted to
lower temperature. It was mainly due to the crystal-
lisation of PBS. However, the melting temperature of the
blends with rPBS decreased gradually with the increase
of compatibiliser contents,31 which was verified in Fig. 5.
The result suggested that the rPBS actually improved the
compatibility and the mutual interaction between starch
and PBS molecules.

4 Cooling DSC thermograms at cooling rate 58c min21 for
neat polymer and blends after melting at 158C for 3 min: a
TPS/PBS (40/60); b TPS/PBS/rPBS (40/58/2); c TPS/PBS/
rPBS (40/55/5); d TPS/PBS/rPBS (40/50/10); e pure PBS; f
TPS (25% glycerol)
No obvious crystallisation behaviour occurred in TPS.
This could be attributed to the fact that crystalline
particles of starch had been destroyed during the plas-
ticising and shearing process. Hence, the crystals in the
blends essentially resulted from PBS phase. Table 1
figures up the crystallinity (Xc %) of PBS, TPS and PBS
blends according to equation (3)29:
DH m
X c% ¼ ð3Þ
w £ DH m
*
*
where DHm and DH m represent the melting enthalpy of
PBS and 100% crystalline PBS respectively, w is the
*
weight fraction of PBS in the blends, and DH m
21
(PBS) ¼ 110.5 J g .
Figure 4 shows that the crystallisation temperature of
PBS (Tc) shifted to lower temperature. The result
suggests that the crystallisation of PBS was restricted by
TPS and rPBS. A major reason for this was that the TPS
suppressed the nucleation of PBS in the blends for its
high melt viscosity.19 Distinctly, both crystallisation
temperature and crystallinity of PBS decreased with the
increase of compatibiliser’s content. It can be indicated
that rPBS promoted the migration of pure PBS mol-
ecular chain segments.
As illustrated in Fig. 5, PBS and its blends show
obvious double melting peaks upon crystallised non-
Compatibility and phase morphology
Table 2 shows the data for tan d of the blends.
A single tan d peak of PBS occurred at 223.4?, corre-
sponding to its glass transition. Apart from the TPS/
PBS/rPBS (40/58/2), a slight shift in the tan d peak of
PBS phase to higher temperature was observed in
binary blends. Two distinct tan d peaks emerged in the
DMA data of TPS. As described by Lourdin et al., one a
relaxation peak was found at low temperature and
closed to the glass transition of glycerol, which was
from the glycerol rich phase.32 The other transition,
b relaxation at room temperature, was related to the
glass transition of starch rich phase.33 These studies
showed that phase separation occurred in TPS with
glycerol as plasticiser. Table 2 reveals that all
blends exhibited three distinct glass transition
temperatures corresponding to the glycerol rich phase,
the PBS phase and the starch rich phase respectively.5
However, these peaks approached each other with
the increment of rPBS content. It was indicated
that TPS and PBS were partially compatible, but it
had no positive influence on improving mechanical
properties. In addition, rPBS enhanced the interfacial
compatibilisation. A further reduction in Tg of starch
rich phase was found in Table 2 compared to the other
two phases. It was attributed to the reaction between
anhydride in rPBS and hydroxyl in starch.18 Moreover,
rPBS acted as a plasticiser in TPS/PBS. The two factors
above were the main driving forces to enhance the
compatibility of TPS/PBS blends.34
Phase behaviour plays a vital role on mechanical
properties of polymer blends. Phase morphology elab-
orates the relationship between microstructure and the
mechanical properties. Figure 6 displays the

Table 1 Melting and crystallisation results of neat polymer and binary blends: a: TPS/PBS (40/60); b: TPS/PBS/rPBS (40/58/2);
c: TPS/PBS/rPBS (40/55/5); d: TPS/PBS/rPBS (40/50/10); e: pure PBS; f: TPS (25% glycerol)

Tm/8C

Sample Tc/8C DHc/J g21 L H DT DHm/J g21 Xc/%

a 93.15 40.66 105.98 113.26 7.28 35.93 54.2

b 93.60 41.23 105.75 112.88 7.13 37.89 57.1
c 93.77 39.68 105.50 112.59 7.09 37.30 56.3
d 93.83 45.97 105.32 112.21 6.89 38.02 57.3
e 95.80 61.42 109.82 115.45 5.63 66.41 60.1
f ... ... 118.53 1.10 ...

Plastics, Rubber and Composites 2015 VOL 44 NO 9 365

Yin et al. Fabrication and characterisation of TPS/PBS

5 Second heating DSC thermograms for neat polymer and 7 Water absorption of blends contained different contents
binary blends at 108c min21: a TPS/PBS (40/60); b TPS/ of rPBS: a TPS/PBS (40/60); b TPS/PBS/rPBS (40/58/2);
PBS/rPBS (40/58/2); c TPS/PBS/rPBS (40/55/5); d TPS/ c TPS/PBS/rPBS (40/55/5); d TPS/PBS/rPBS (40/50/10)
PBS/rPBS (40/50/10); e pure PBS; f TPS (25% glycerol)

morphology of TPS/PBS blends. Residual granular

structure and uneven block structure were observed on
Table 2 Glass transition temperatures of neat polymer and the fracture surface of non-compatibilised blends. Starch
binary blends: A: TPS/PBS/rPBS (40/50/10); B: TPS/ granules were detached from PBS matrix, suggesting
PBS/rPBS (40/55/5); C: TPS/PBS/rPBS (40/58/2); that phase separation occurred. With the addition of the
D:TPS/PBS (40/60); E: pure PBS; F: TPS (25% gly- rPBS, no visible starch granules were detected in Fig.
cerol) 6b–d. It can be indicated that rPBS weakened the
Tg (glycerol Tg (PBS Tg (TPS rich
interfacial tension between TPS and PBS and led to the
Sample rich phase)/8C phase)/8C phase)/8C smaller size of phase domain.35 Starch phase distributed
more evenly with the increase of rPBS content. There-
A 258.6 218.9 13.0 fore, when the compatibilised blends were subjected to
B 256.5 221.0 11.2 an external force, deformation of interfacial layer was
C 255.0 224.0 13.3 transferred and the stress was dispersed effectively due
D 253.9 222.1 20.1
to their stronger interfacial adhesion, especially in PBS
E ... 223.4 ...
F 259.5 ... 22.1 domains.

Water absorption
Figure 7 shows the equilibrium water absorption of TPS/
PBS blends. The incorporation of hydrophobic PBS
dramatically lowered the water absorption of TPS and
reduced the water sensitivity of TPS/PBS blends.27 As
illustrated in Fig. 7, the equilibrium water uptake in
blends containing rPBS was lower than those blends
without rPBS. It is attributed to the good dispersion,
homogeneous microstructure of starch and well dis-
persion of starch particles restricting the diffusion of
water molecules in TPS/PBS blends.36 The result also
demonstrated that the content of compatibiliser has no
effect on water resistance of TPS/PBS.

6 SEM images of fractured surface of TPS/PBS: a TPS/PBS
(40/60); b TPS/PBS/rPBS (40/58/2); c TPS/PBS/rPBS
(40/55/5); d TPS/PBS/rPBS (40/50/10)
Conclusions
An interfacial compatibiliser rPBS was successfully
synthesised by grafting the MAH onto PBS. Fully bio-
degradable binary blends of TPS and PBS with different
contents of rPBS were prepared using a two-step
extrusion process. The mechanical properties, mor-
phology and compatibility of blends were investigated.
Results showed that rPBS greatly improved the strength
and elongation at break of blends, especially for the
PBS that occupied the main ingredients. TPS/PBS/rPBS
(40/55/5) possessed the highest tensile strength and

366 Plastics, Rubber and Composites 2015 VOL 44 NO 9

Yin et al. Fabrication and characterisation of TPS/PBS
elongation at break. The rPBS in PBS blends helped to
improve interfacial miscibility. Good adhesion of TPS/
PBS interface and small evenly dispersed starch particles
were observed with higher content of rPBS. rPBS
enhanced the water resistance of TPS/PBS/rPBS. The
results suggested that compatibilised TPS/PBS blends,
with the combination of biodegradability, high strength
and water resistance, can be a strong candidate of
packing material.
Acknowledgements
This investigation was supported by the National Sci-
ence & Technology Pillar Program during the Twelfth
Five-Years Plan Period (grant no. 2012BAD32B01). The
authors gave thanks to Dr Yichen Du in the Guelph
Food Research Centre Agriculture and Agri-Food
Canada for his help in improving the English of the
paper.
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