Polymer Degradation and Stability 94 (2009) 9094

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Polymer Degradation and Stability

journal homepage: www.elsevier.com/locate/polydegstab

Biodegradability of poly(butylene succinate) (PBS)

composite reinforced with jute bre
Lifang Liu a, b, *, Jianyong Yu c, a, Longdi Cheng a, b, Xiaojie Yang d
a

The Key Lab of Textile Science & Technology, Ministry of Education, Donghua University, Shanghai 201620, China
College of Textiles, Donghua University, Shanghai 201620, China
c
Modern Textile Institute, Donghua University, Shanghai 200051, China
d
The Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, Shanghai 200092, China
b

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 4 August 2008
Received in revised form
6 September 2008
Accepted 7 October 2008
Available online 22 October 2008

Poly(butylene succinate) (PBS)/jute composites were prepared, and the effects of bre content, diameter,
surface modication and arrangement forms on the biodegradability were evaluated by compost-soil
burial test. The weight losses of PBS/jute composites are higher than that of pure PBS lm and bulk jute
bre, and decreased with increasing bre content. The weight loss of PBS/10% jute composite after 180
days is 62.5%. In the case of the effect of bre diameter, the weight loss is found to decrease with
decreasing bre diameter. For the effect of bre surface modication, the order of higher weight loss is
PBS/untreated jute > PBS/alkali treated jute > PBS/coupling agent treated jute. Furthermore, the
composite of PBS/woven fabric has the highest weigh loss, followed by that of PBS/nonwoven fabric and
PBS/bulk jute bre, respectively.
2008 Elsevier Ltd. All rights reserved.

Keywords:
Biodegradability
Poly(butylene succinate) (PBS)
Jute bre
Composite

1. Introduction
In recent years, the development of composites has achieved
more and more progress for environmental protection as well as
government regulations in some countries [15]. Composites are
usually fabricated with biodegradable polymers as matrix phase
and natural bres as enhancement phase. Poly(e-caprolactone)
(PCL), poly(lactic acid) (PLA), poly(butylene succinate) (PBS) and
poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) are most
commonly used as matrix phase of composites, among which PBS
particularly attracts increasing commercial interest [2,3,69]. PBS,
with excellent mechanical properties and processing capabilities, is
polymerized from butanediol and succinic acid, which may soon
both be available from bio-based renewable resources [6,8]. A great
deal of lignocellulosic bre, such as jute bre, hemp bre, sisal bre,
abaca bre, and so on, are used as reinforcement materials for
biomaterials with their good mechanical properties and low specic
mass, among which jute bre is most attractive [6,8,1012]. Jute
bre can be planted in riverats, depressions, and saline-alkali soils,
which are unavailable to plant cotton and most food corps, and no
pesticides and fertilizer are needed during the growth of jute, so jute
is a kind of pure green agro-product. Jute can also be harvested
two or three time annually, thereby resulting in signicant high
yield and low cost. Furthermore, Jute bre has nearly the highest
* Corresponding author. Tel.: 86 21 6779 2719; fax: 86 21 6779 2102.
E-mail address: lifangliu@dhu.edu.cn (L. Liu).
0141-3910/$ see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymdegradstab.2008.10.013

specic strength and modulus in lignocellulosic bre which is

especially meaningful to enhance composites. However, jute bre
also has disadvantages as a reinforcing material: the high moisture
absorption and the low processing temperature permissible
[4,6,1214]. Surface modication is often used to decrease the
moisture absorption, as well as to improve the interfacial properties
in composites. Processing temperatures have to be maintained
below 200  C to avoid deterioration of the properties due to the jute
degradation [14]. PBS, with melting point of about 90120  C can be
processed at temperatures of 140200  C [6,9]. So jute bre and PBS
were selected in this work not only for their excellent properties but
also for their processing temperature compatibility. We have
studied the mechanical properties of PBS/jute composites, but focus
only on their biodegradability in this study.

2. Experimental details
2.1. Materials
Three kinds of jute bre used in this study, with average
diameters of 55 mm, 48 mm and 40 mm, respectively, were produced
in Bangladesh. Poly(butylene succinate) (PBS), white masterbatch
with melting point of about 115  C, was kindly supplied from
Showa Highpolymer Co., Ltd. (Japan) and vacuum-dried at 40  C for
24 h prior to use. All the other chemicals used in this study were
reagent grade and used without further purication.

L. Liu et al. / Polymer Degradation and Stability 94 (2009) 9094

2.2. Surface modication of jute bre

70

Jute bre with diameter of 55 mm was cleaned and dried at 60  C

for 24 h in a vacuum oven, then pretreated with 0.2% H2SO4 solution at 55  C for 1.5 h, and then ltered off and washed. The cleaned
bre was surface modied with the following processes, respectively: (1) soaked in 5% NaOH solution at room temperature for 4 h,
which was called alkali treatment; (2) soaked in a solution of 1.5%
coupling agent KH-570 and 98.5% anhydrous ethanol at room
temperature for 4 h, which was called coupling agent treatment.
Both of the two kinds of bres were washed and dried at 60  C for
24 h in a vacuum oven.

60

91

PBS/55um jute
PBS/48um jute

Weight loss ( )

PBS/40um jute
50
40
30
20
10

2.3. Fabrication of jute woven fabric and nonwoven fabric

0
30

One part of jute bre after alkali treatment was spinning into
yarn and then woven into fabric, and another part of ones needlepunched into nonwoven fabrics. The two fabrics both have nearly
the same mass of unit area (200 g/m2).

60

90

120

150

180

Buried time (day)

Fig. 2. Weight loss of buried specimens with different bre diameters.

2.5. Biodegradability test

2.4. Fabrication of composites
2.4.1. Bulk jute bre reinforced composite
Jute bres after different treatments were chopped into about
35 mm lengths, then mixed at given contents with PBS in HAAKE
Rheometer Systems (Rheocord 90, Germany HAAKE co., Ltd., Germany) at a rotary speed 80 rpm for 15 min at 120  C to obtain the
mixture of jute bre and melting PBS. The mixture was cooled to
room temperature, and then cut to desired size and heated again at
140  C under a pressure of 15 MPa for 15 min in a at sulde
machine (Shanghai No.1 Rubber and Plastics Plant, China) to obtain
composite plates.
2.4.2. Jute fabric reinforced composites
PBS masterbatch were heated in the at sulde machine at
a temperature of 140  C and a pressure of 8 MPa for 10 min to
obtain pure PBS lms. Then one layer of jute woven or nonwoven
fabric was sandwiched between two layers of PBS lms. These
layers were pressed in the at sulde machine at 140  C and 8 MPa
for 5 min to melt PBS, then at 15 MPa for 15 min to make melted
PBS wet bres in the fabric, and nally at 10 MPa for 5 min to obtain
composite plates.

The composite plates were cut into 30  40 mm rectangular

specimens for biodegradability testing. Biodegradability was
determined by measuring weight loss of the specimens buried in
compost soil. The composition of compost soil was: 20% water, 20%
organic substance, 30% rotten leaves, 5% urea, and 5% others
(sawdust, wastepaper). Each specimen was buried in the compost
soil and incubated at environmental temperature of 30  2  C.
Water was supplied constantly to keep the compost soil humid.
Each specimen was dug out of the compost soil after buried for 30,
60, 90, 120,150, and 180 days, respectively, and then washed with
water and dried to a constant weight at 60  C in a vacuum oven. The
weight loss Wloss(%) was calculated using the formula:

Wloss

Winitial  Wfinal
 100%
Wfinal

where Winitial and Wnial are the weights of specimen before and
after buried in compost soil.
2.6. Picture and spectral analysis
The surface properties and FTIR spectra of jute bre before and
after modication were examined by scanning electron microscope

70

60

PBS/10

jute

PBS/20

jute

PBS/30

jute

70
PBS/untreated jute
PBS/alkali treated jute
PBS/coupling agent treated jute

60

50

40

Weight loss (

Weight loss(

50

Pure PBS film

Bulk jute fibre

30

20

30

20

10

0
30

40

10

60

90

120

150

Buried time(day)
Fig. 1. Weight loss of buried specimens with different bre contents.

180

30

60

90

120

150

180

Buried time (day)

Fig. 3. Weight loss of buried specimens with different surface modications.

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L. Liu et al. / Polymer Degradation and Stability 94 (2009) 9094

the tight structure of PBS lm, resulting in quicker biodegradation

than pure PBS.

Table 1
Main compositions of jute bre with different surface modication%.
Jute bres

Cellulose

Hemicellulose

Lignin

Without surface modication

With alkali treatment
With coupling agent treatment

63.2
72.9
77.6

14.5
12.6
11.4

16.8
11.7
9.6

(SEM) (JSM-5600LV, JEOL Ltd., Japan) and Fourier Transform

Infrared spectrophotometer (FTIR) (NEXUS-670, Nicolet Company,
US), respectively.
3. Results and discussion
3.1. Fibre content
Three composites specimens of untreated bulk jute bre at the
content of 10 wt.%, 20 wt.% and 30 wt.% were prepared as
mentioned above. The biodegradability of these three specimens as
well as pure PBS lm and bulk jute bre was assessed, and the
results are shown in Fig. 1. The weight loss increases with burial
period for all the specimens, and the order of higher weight loss
after burial was PBS/10% jute composite > PBS/20% jute composite > PBS/30% jute composite > pure PBS lm > bulk jute bre. The
weight loss of PBS/jute composite after 180 days is 62.5%, 54.8% and
47.3%, respectively, in accordance with the bre content of 10 wt.%,
20 wt.% and 30 wt.%. While the weight losses of pure PBS lm and
bulk jute bre are 31.4% and 24.7% respectively, showing that
compounding of jute bre and PBS accelerates the biodegradation
of either jute bre or PBS. The weight loss was also observed to
decrease with the increase of bre content, and to reach
a maximum at the bre content of 10 wt.%. It may be explained that,
in case of one component in composite degrades faster than the
other, the weight loss in biotic conditions would mostly be due to
the degradation of that component [13]. As shown by the experimental results, the degradation of PBS is faster than that of jute
bre, so the weight loss is decreased with the increase of bre
content. However, the addition of jute bre into PBS may change

3.2. Fibre diameter

Composites with jute bre of different diameters were prepared
at the same bre content of 10 wt.% and biodegradability tested as
shown in Fig. 2. The weight loss is found to decrease with the
decrease of bre diameter. There are increasing quantities of bres
in unit volume of composite at given bre content with the
decrease of bre diameter, resulting in increasing of interface area
between bre and PBS matrix, so as to improve the adhesion at the
interface and make the internal structure of composite tighter.
Good compatibility means that the composite have stronger
capabilities to resist environmental attacks that may erode it [4]. So
the weight loss of composites is decreased with the decrease of
bre diameter.
3.3. Fibre surface modication
Jute bre as well as other natural cellulose bre has inevitable
bottlenecks as enhancement materials, such as poor wettability,
high moisture absorption, incompatibility with hydrophobic polymers, and so on. These properties can be improved by physical and/
or chemical treatments [1216]. Alkali and coupling agent treatments were introduced here to modify the properties of jute bre
as mentioned above, and composites reinforced with treated bres
at 10 wt.% content were prepared. Fig. 3 shows the biodegradability
of the buried specimens in terms of weight loss. The order of higher
weight loss is PBS/untreated jute > PBS/alkali treated jute > PBS/
coupling agent treated jute. These results indicate that surface
modication can inuence the bio-disintegrability of jute bre.
Surface modication can remove a certain amount of lignin,
hemicellulose and pectin covering the external surface of the cell
wall of the bre (Table 1), making the bre cleaner and rougher
than before, as shown in Fig. 4. The removal of surface impurities is
advantageous in jute/PBS adhesion, as it facilitates both mechanical
interlocking and the bonding reaction due to the exposure of the

Fig. 4. The surface of jute bre (a) without modication, (b) with alkali treatment and (c) with coupling treatment.

L. Liu et al. / Polymer Degradation and Stability 94 (2009) 9094

93

70
PBS/bulk jute fibre
PBS/woven fabric
PBS/nonwoven fabric

60

Weight loss (

50

40

30

20

10
Fig. 5. FTIR spectra of differently treated jute bres.

hydroxyl groups to PBS [17,18]. Furthermore, surface modication

can also bring changes to the chemical compositions of jute bre.
Fig. 5 illustrates the FTIR spectra of different treated jute bres. A
broad absorption band in the region 34003200 cm1, as well as
the characteristic of hydrogen bonded OH stretching vibration,
both can be found in the FTIR spectra of jute bre treated or not.
However, the strong and sharp peak at 1740 cm1 attributed to
pC]O stretching vibration of hemicellulose is weakened after
treatment, especially after coupling agent treatment, showing that
surface treatment promotes the ionization of the hydroxyl group to
the alkoxide, as shown in Eqs. (1) and (2) that shows the reactions
between jute bre and alkali or coupling agent KH-570, respectively [17]. The hydrophilic behaviour of jute bre induced by
predominance of OH groups will thus be weakened, and its
compatibility with hydrophobic PBS will accordingly be improved
[6,17], as shown in Fig. 6. So the biodegradability of composites is
decreased as explained above. Jute bres treated with coupling
agent have more obvious changes, resulting in less weight loss of
their composites.

30

60

90

120

150

180

Buried time (day)

Fig. 7. Weight loss of buried specimens with different bre arrangement forms.

NaOH Cell-OH/Cell-O Na H2 O

(1)

CH2 ]CCH3 COOCH2 3 SiOH3 Cell  O

/CH2 ]CCH3 COOCH2 3 SiOH2 O  Cell H2 O

3.4. Fibre arrangement forms

There are mainly three forms of bre as enhancement materials
for composites, i.e., bulk bre, woven fabric, nonwoven fabric. The
jute bres after alkali treatment were used to fabricate composites
in different arrangement forms at the same content of 20 wt.%. The
weight loss of corresponding composites is illustrated in Fig. 7. The
composite of PBS/woven fabric has the highest weight loss,

Fig. 6. Fracture surface of biocomposites reinforced with (a) untreated, (b) alkali treated, and (c) coupling agent treated jute bres.

94

L. Liu et al. / Polymer Degradation and Stability 94 (2009) 9094

followed by that of PBS/nonwoven fabric and PBS/bulk jute bre,

respectively. The root reasons are the uniformity of bre distributing in composite and the interfacial compatibility of bre and
PBS. The composite reinforced with woven jute fabric have many
inner defects because the bre in every yarn are closely congregated to be fully wetted by melting PBS although there are visible
gaps between yarns in fabric. Poor compatibility leaves the
composite vulnerable to outer microorganism. Nonwoven fabric
has higher porosity and uniformity of bre distribution than woven
one, so the composite have more consistent inner-structure.
Furthermore, bulk bre reinforcing composites have the most
uniform distribution of bre and the most compatible interface in
composite, leading to the lowest weight loss.
4. Conclusions
Biodegradability of PBS/jute bre composites was investigated
by compost soil burial test. Regarding the effect of bre content
on the biodegradability of composite, the order of higher weight
loss is PBS/10% jute composite > PBS/20% jute composite > PBS/
30% jute composite > pure PBS lm > bulk jute bre. The weight
loss of PBS/10% jute composite after 180 days is 62.5%. In case of
the effect of bre diameter, the weight losses are found to
decrease with the decrease of bre diameter, because the
composite reinforced with ner bre has better inner-structure.
In the effect of surface modication of bre, the order of higher
weight loss is PBS/untreated jute > PBS/alkali treated jute > PBS/
coupling agent treated jute, since the hydrophilic behaviour of
jute bre is weakened by surface modication, and the compatibility with hydrophobic PBS is thus improved. Furthermore, the
composite of PBS/woven fabric has the highest weigh loss,
following by that of PBS/nonwoven fabric and PBS/bulk jute bre,
respectively. The root reasons are the uniformity of bre distribution in the composite and the interfacial compatibility of bre
and PBS.

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