Textile Research Journal

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Textile Research Journal Vol 80(17): 18461858 DOI: 10.1177/0040517510369408 The Author(s), 2010. Reprints and permissions:
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Preparation and Physical Properties of Regenerated Cellulose
Fibres from Sugarcane Bagasse
Ahmed Jalal Uddin, Atsushi Yamamoto,
Yasuo Gotoh
1
, Masanobu Nagura
Faculty of Textile Science and Technology, Shinshu
University, 3-15-1 Tokida, Ueda, Nagano 386-8567, Japan
Mahito Iwata
2 Shinnaigai Textile Ltd., 2-6, 3-Chome, Bingo-Machi,
Chuo-ku, Osaka 541-0051, Japan
Conventional synthetic fibres are generally fabricated from
petroleum-based polymers and their large-scale consump-
tion has generated serious environmental problems. As a
result, much attention has recently been devoted to the
development of biodegradable and environmentally friendly
fibres for both apparel and industrial applications [1, 2].
Cellulose is one of the most abundant natural resources
on earth, and there has been extensive research on the pro-
duction of fibre from this material. The history of cellulose
fibre dates back to the 1860s, when the first rayon fibres
were commercialised.
1
But the rayon process, which included
toxic carbon disulfide treatments to block hydroxyl groups
of cellulose in order to prepare a spinnable solution, some-
times caused ecological problems. Since then, many
attempts have been made to invent new solvents to directly
dissolve cellulose. One solvent, N-methylmorpholine-N-
oxide (NMMO) hydrate, has been successfully used in the
Abstract To produce cellulose regenerated fibres
with high mechanical properties at low cost, sug-
arcane bagasse was chosen as a cheap raw mate-
rial. In this study, bagasse was dissolved in N-
methylmorpholine-N-oxide (NMMO) 0.9 hydrate,
and fibres were prepared by the dry jet-wet spin-
ning method by using dilute water/NMMO mix-
ture as a coagulant, as is done in the production
of commercial lyocell fibre. The effects of other
coagulants, including water, methanol, isopropa-
nol and ethanol, on the physical properties of the
fibres were also investigated. Among these coagu-
lants, fibres produced in ethanol and water/NMMO
mixture exhibited the superior tensile strength
and initial modulus although had some NMMO
trapped in fibre matrix. After removal of NMMO
by a simple heat treatment, much improvement in
the fibre structure and mechanical properties was
observed. The cross-sectional morphology and
surface of these two fibres reveal the occurrence
of fibrillation due to their high degree of crystal-
linity and overall high molecular orientation. The
bagasse regenerated fibres produced in this study
had a tensile strength of approximately 530 MPa
and Youngs modulus of approximately 33 GPa,
which are comparable to those of commercial lyo-
cell fibre.
Key words bagasse regenerated fibres, dry-jet
wet spinning, structure-properties
1
Corresponding author: e-mail: ygotohy@shinshu-u.ac.jp
Preparation and Physical Properties of Regenerated Cellulose Fibres A. J. Uddin et al. 1847 TRJ
production of regenerated cellulose fibres. Lyocell fibres
spun from cellulose solution in NMMO hydrate were first
investigated in the early 1980s [3, 4].
Though regenerated cellulose fibres are usually spun by
the traditional wet spinning method, the dry jet-wet spin-
ning process with an air-gap was found to produce lyocell
fibres with good physical properties [57]. Most dry jet-wet
spun lyocell fibres have been commercially successful in
the apparel field due to their good mechanical properties,
blendability with other fibres, and draping characteristics.
In comparison with viscose rayon, they show excellent
mechanical properties in the wet state [79]. The NMMO
technology provides a relatively simple, resource-conserv-
ing, and environmentally friendly method for producing
regenerated cellulose fibre. The manufacturing process is
designed to recover 99% of the solvent, which minimises
effluent. Furthermore, the solvent itself is nontoxic and the
effluent is not hazardous [10, 11].
Pulp material containing more than 90% -cellulose is
called high -cellulose pulp, and pulp containing more
than 20% hemicellulose is called high hemicellulose pulp
[12]. The cellulose of lyocell is usually derived from pulp
with only high -cellulose pulp content, which is obtained
from hardwood trees such as oak and birch. These trees
require vast areas of land and many years to grow. Conse-
quently, although the pulp of these trees guarantees a high
fibre yield, the cost of producing the pulp material is rela-
tively high [13]. In this context, a cheaper source of pulp
with high hemicellulose content would reduce the cost of
lyocell fibres. Recent investigations reported that the yield
of lyocell fibres produced from high and low hemicellulose
content was approximately equal because most of the cel-
lulose and hemicellulose can be converted into fibre in the
lyocell process [14, 15]. Moreover, higher hemicellulose
content correlates with a smaller fibril aggregation size
[1618]. Thus, the hemicellulose serves as a regulator for
the close association of cellulose and hemicellulose. This
association increases the stability of the fibril aggregation
[19, 20] that ultimately leads to the increase in fibrillation
resistance of lyocell fibres [21, 22].
Bagasse is a fibrous residue that is left after the crushing
of sugarcane stalks. Essentially, bagasse is a waste product,
and so annual production of approximately 100 million
tons requires additional disposal costs. Currently, some of
the bagasse is burned in the furnaces of sugar cane mills to
provide heat and to generate power or steam. These proc-
esses generate toxic dioxins [23]. Bagasse pulp is also used
to make several grades of paper: newspaper, writing paper,
toilet tissue, paper towels, glassine, etc. Even so, an excess
of bagasse exists, and this excess is deposited on empty
fields, altering the landscape. Bagasse contains, on aver-
age, 49% moisture, 49% fibre and 2% soluble solids. The
composition the fibrous part of bagasse is 50% cellulose,
30% hemicellulose, 18% lignin and some inorganic com-
pounds [24].
The main objective of our research is to prepare regen-
erated cellulose fibre with high mechanical properties from
a cheaper source of raw material. Fibres were prepared
from sugarcane bagasse by following conventional lyocell
processing, which entails dry jet-wet spinning using N-meth-
ylmorpholine-N-oxide (NMMO) 0.9 hydrate as a solvent. In
this study, the influence of other types of coagulants on the
mechanical properties of fibres was investigated. First, a
dilute water/NMMO mixture and only water were used as
coagulants. Then, to inhibit the rapid coagulation in water,
alcoholic coagulants miscible with the solvent NMMO-
water, such as methanol, isopropanol and ethanol, were
also examined in order to obtain a high spin-draw ratio.
Experimental
Materials
Bagasse was supplied by Okinawa Sugarcanes Research
Corporation in Japan. A commercial lyocell fibre sample
(diameter, 20 m) used for making apparel was received
from the Shinnagai Textile Ltd., Japan to compare the
mechanical properties of this sample with those of our pre-
pared fibres.
NMMO hydrate was purchased from Tokyo Chemical
Industry Co. Ltd., Japan. The 50 wt% aqueous NMMO
solution (approximately 4.8 mol/L) was condensed to
NMMO 0.9 hydrate in an evaporator with a vacuum at
120C.
Alkali Treatment of Bagasse Prior to
Spinning
To extract lignin and inorganic compounds, bagasse were
agitated at 80 rpm and temperature 90C for 24 h in an alkali
solution of concentrations of 3, 5, 7 and 10 wt% NaOH. The
elimination of lignin was confirmed by Fourier Transform
Infrared (FT-IR) Spectroscopy. The reduction of inorganic
materials after alkali treatment was examined by Thermo-
Gravimetric Analysis (TGA) and Scanning Electron Micro-
scopy/Energy Dispersive X-ray (SEM/EDX).
Preparation of Spinning Solution
The spinning solution was prepared by combining 40 ml
NMMO 0.9 hydrate (solvent), 4 g bagasse (cellulose), 10
mg propyl gallate (antioxidant) and 10 mg sodium dodecyl-
sulphate (surfactant) in a flask and stirring the solution in a
static rotary mixer at 50 rpm at 120C for 2.5 h.
Dry Jet-Wet Spinning
Dry jet-wet spinning was carried out with an air gap of 15
mm through a single-hole spinneret of diameter 0.5 mm.
1848 Textile Research Journal 80(17) TRJ TRJ
The extrusion temperature was 100C. The injection speed
was approximately 4.0 m min
1
. Coagulation took place in
water, methanol, isopropanol, ethanol and water/NMMO
mixture (10 wt%) at room temperature (20C) with a 2-m
coagulating bath followed by a water wash. It should be
noted that we previously spun bagasse fibres in water/
NMMO coagulants of various NMMO concentrations (0%
to 50%) and the water/NMMO (10 wt%) mixture showed
the best results in terms of physical properties. The entire
study will be reported in a future paper. For simplification,
the water/NMMO mixture (10 wt%) coagulant will hereaf-
ter be referred to as the water/NMMO coagulant in this
paper.
The prepared fibres were taken up at their maximum
possible speeds, between 35 and 70 m min
1
depending on
the coagulants. The spin-draw ratio d
f
/d
0
was determined
by measuring the cross-sectional diameter of the solution
dope at the spinneret exit (d
f
) over the fibre cross-sectional
diameter at the take-up point (d
0
).
Spun fibres were dried in an oven at 30C for 24 h in the
presence of silica gel to absorb water.
Hot drawing and heat treatment of fibres were carried
out with a hand-operated drawing apparatus into a hot oven.
Measurements
Structure characterization
Birefringence was obtained by measuring the refractive
indices parallel and perpendicular to the fibre axis by an
Interphako Interference Microscope, Carl Zeiss JENA
Ltd., Germany. During each measurement, five fibre speci-
mens were taken from five different locations and then
averaged.
Wide-angle X-ray diraction (WAXD) measurements
were obtained by a Rigaku Rotorflex RU-200B diracto-
meter using Ni-filtered Cu-K

radiation operated at 40 kV
and 150 mA (wavelength 1.542 ). The degree of crystallin-
ity was determined from the ratio of crystalline scattering
versus total scattering, and the amorphous contribution was
estimated by polynomial approximation [25]. The angle of
preferred orientation with respect to the fibre axis was
determined from the most intense reflection peak of equa-
torial diffraction (with the overlapping 110/200 plane at 2
= 22.6) [26, 27]. Curves derived from the azimuthal scans
were fitted onto the profiles of the mathematical model
investigated with Gauss functions [28], as shown in eq. (1),
where I
o
is the peak intensity,
o
is the azimuthal angle at I
o
,
and is the peak width. Hermans crystal orientation func-
tions, f
c
, were then obtained with eq. (2):
(1)
(2)
where
The density of the fibres was determined on small
pieces of fibres by a floatation method at 25C using a mix-
ture of carbon tetrachloride (CCl
4
) and n-heptane as the
reference solution. Each density value represented the
average of three measurements.
SEM was conducted with an Hitachi S-2380N after
sputtering the samples with platinum (Pt). SEM-EDX was
analyzed with an Hitachi S-3000N attached with an Energy
Dispersive X-ray (EDX) analyzer, Horiba EX 200-SE.
TGA was performed using a ThermoPlus II TG-DTA
8120 from room temperature to 600C in air at a scan rate
of 10C min
1
. The weight of each sample was 5 mg.
FT-IR measurements were performed by the FTIR-
8600PC, Shimadzu Ltd., Japan.
Fibrillation of fibres was carried out by taking 10 fibres
of 20 mm length. Fibres were immersed in distilled water
at room temperature (20C) and sonicated for 15 min on a
Branson ultrasonic sonifier 2510 OJ-DTH followed by
magnetic stirring for 1 hr.
Mechanical properties
The tensile properties of filament fibres (40 mm gauge
length) were measured in Tensilon Model RTC-1250A,
Japan at a crosshead speed of 40 mm min
1
. The experi-
mental results represent the average of 10 individual meas-
urements.
Dynamic mechanical properties
The dynamic viscoelastic properties were measured by an
ITK Co. DVA-225 instrument at a frequency of 10 Hz and
heating rate of 10C min
1
on fibres of 20-mm length.
Results and Discussion
Alkali Treatment of Bagasse
Several types of regenerated cellulose fibres (e.g., rayon,
acetate, triacetate and lyocell) are manufactured from
I
( )
I
o

o

--------------
\
]
| |
2

)
`

exp =
f
c
3
2
cos 1
2
-------------------------------- =

2
cos
I
( )

2
cos sin d
0
2

I
( )
sin d
0
2

------------------------------------------------ =
Preparation and Physical Properties of Regenerated Cellulose Fibres A. J. Uddin et al. 1849 TRJ
purified wood pulp. To remove the lignin and inorganic
compounds, bagasse was subjected to agitation with alkali
(NaOH) solutions of different concentrations (3, 5, 7 and
10 wt%).
Figure 1 shows the FT-IR curves of the original
(untreated) and alkali-treated bagasse. The original bagasse
sample exhibits the IR bands at approximately 1740, 1604,
1515 and 1240 cm
1
which correspond, respectively, to the
carbonyl group of carboxyl and ester group, C=C aromatic
ring of lignin, aromatic ring of lignin, and C-O stretching of
lignin [29]. These bands disappear for alkali-treated
bagasse, even at the alkali concentration of 3%. But the
treatment of bagasse with 10 wt% NaOH is necessary to
remove the inorganic matters as described below.
The remaining matter of the alkali-treated bagasse
were studied by TGA. To ascertain the presence of inor-
ganic matter after alkali treatment, original and alkali-
treated bagasse specimens were heated to 600C and kept
for 2 h until the hemicellulose, cellulose and lignin were
completely degraded, since they degrade at 180C, 340C
and 420C, respectively. After TGA scans were finished,
the weights of the remaining inorganic materials were
measured. Figure 2 plots the weight reduction of inorganic
matter as a function of alkali concentration. As seen in Fig-
ure 2, the removal of inorganic matter apparently reaches a
saturation level after treatment with 10 wt% NaOH. In the
SEM-EDX study, EDX identified inorganic materials con-
taining potassium, silica, calcium and a small amount of
iron.
Characteristics of Bagasse Fibres Prepared
in Different Coagulants
Physical Appearance
The physical appearance of the bagasse fibres prepared in
various coagulants was observed and all fibres showed the
silky sheen of commercial lyocell fibres, irrespective of the
coagulant used.
Structure Development
The structural parameters of bagasse fibres obtained in dif-
ferent coagulants are listed in Table 1 according to their
maximally achieved spin-draw ratio. In this table, it is seen
that the fibre diameter (measured in SEM) becomes thinner
with the increase in spin-draw ratio, which directly influ-
ences the structural parameters of fibres. Among all fibres,
the water/NMMO and ethanol coagulated fibres show com-
paratively better structural parameters, such as the degree
of crystallinity (X
c
), lattice spacing (d) (measured when the
intense peak corresponds to overlapping 110/200 plane at
2 = 22.6), crystal orientation (f
c
) and birefringence (n).
The n and X
c
values for these two fibres are very close,
but f
c
and d are different. In the case of the water/NMMO
coagulated fibre, X
c
value is seemingly lower, although it
possesses the highest f
c
and n among all fibres.
The densities of the 100% crystalline sample (
c
) and
100% amorphous sample (
a
) for cellulose were reported
as 1.620 and 1.415 gcm
3
, respectively [30]. But the density
value of the water/NMMO coagulated fibre was found to
be 1.43 gcm
3
, which is very close to the density of
a
of cel-
lulose; this result does not match the other structural
Figure 1 FT-IR spectra for origi-
nal (untreated) and alkali-treated
bagasse.
1850 Textile Research Journal 80(17) TRJ TRJ
parameters of that fibre, such as X
c
(56%), f
c
(0.81) and n
(19.3 10
3
)
.
Then, the low density value of this fibre was
investigated by SEM and FT-IR (described later) and this
was attributed to the remaining NMMO in the fibre along
with the formation of an interfibrillar free volume or micro-
voids during spin drawing. Such interfibrillation and the
resultant low density value of fibres were found in our previ-
ous work for highly crystallised and highly oriented polypro-
pylene (PP) fibres, when the PP fibre was drawn by laser-
heated drawing to its highest draw ratio [31]. For that reason,
in our present study we calculated the degree of crystallinity
of all bagasse fibres from their respective WAXD profiles.
The WAXD images of these fibres are shown in Figure 3.
The WAXD images show that crystal order improves with
increasing spin-draw ratio. As shown by the structural
parameters obtained in Table 1, the WAXD images of
water/NMMO and ethanol coagulated fibres show higher
crystallinity and crystal orientation. Methanol coagulated
fibres indicate comparatively lower crystal orientation. Iso-
propanol and water coagulated fibres show the lowest crys-
tal parameters and an obvious amorphous halo.
We observed the SEM images of the fractured cross sec-
tions of fibres, presented in Figure 4. The images of the
water/NMMO, methanol and isopropanol coagulated
fibres indicate some fibrillation. It is well known that during
the spinning of lyocell fibres, crystallization occurs and crys-
talline regions are separated by amorphous regions but held
together by hydrogen bonds. At a high spinning speed, the
crystals orient and the fibre fibrillates, tearing the hydrogen
bonds in the amorphous regions [32]. Such inherent phe-
Figure 2 Inorganic materials (%)
contained in original and alkali-
treated bagasse measured by TGA.
Table 1 Structural parameters of bagasse fibres prepared in various coagulants.
Coagulant
Spin-draw
ratio
d
f
/d
0
Fibre
diameter
(m)
Fibre density
(gcm
3
)
Degree of
Crystallinity*,
X
c
(%)
Lattice
Spacing, d
()
Degree of
crystal
orientation, f
c
Birefringence
n 10
3
Water/NMMO 17.5 38 1.43 56 4.272 0.81 19.3
Ethanol 17 40 1.53 60 4.235 0.71 19.0
Methanol 12.75 43 1.51 58 4.238 0.65 17.1
Isopropanol 10.5 48 1.48 56 4.263 0.60 16.5
Water 8.75 52 1.41 48 4.303 0.45 12.2
* X
c
measured from WAXD
Preparation and Physical Properties of Regenerated Cellulose Fibres A. J. Uddin et al. 1851 TRJ
Figure 3 WAXD images of bagasse fibres prepared in various coagulants.
Figure 4 SEM images of fractured cross sections of bagasse fibres prepared in various coagulants.
1852 Textile Research Journal 80(17) TRJ TRJ
nomenon of lyocell fibre spinning was also observed in our
present work. However, water/NMMO coagulated fibre
bears some indication of the remaining NMMO in the fibre
matrix. The ethanol coagulated fibre was expected to show
fibrillation due to its higher structure parameters (Table 1 and
Figure 3); instead, it shows a skin-core structure. This is pos-
sibly due to the fact that the core of this fibre was not prop-
erly coagulated because of its hard skin and some NMMO
was trapped in the core part of fibre. The SEM image of the
water coagulated fibre also does not show any fibrillation.
Since NMMO is a strongly hygroscopic substance [33], thus
the solvent NMMO might have instantly extracted from the
fibre towards water while entering into the water coagulat-
ing bath. This fact might cause the very fast coagulation and
lowest spin-draw ratio of the water coagulated fibre (Table 1)
that ultimately results in the lowest structural parameters
(Table 1 and Figure 3).
Correlation of Mechanical Properties with Fibre
Structure
Figure 5 shows the typical stress-strain curves of the fibres in
different coagulants. For all fibres, the shape of the stress-
strain curves expresses an initial linear portion, a yield point,
and a region of low or high slope up to rupture. Several ten-
sile properties such as tensile strength, initial modulus, and
elongation at break, evaluated from the stress-strain curves,
are summarised in Table 2. In close agreement with the struc-
tural development, the tensile properties of water/NMMO
and ethanol coagulated fibres also show remarkable improve-
ment in comparison to other coagulated fibres. Water/
NMMO fibre shows the highest tensile strength with tough-
ness and the ethanol fibre shows the highest initial modu-
lus. Methanol and isopropanol coagulated fibres show
somewhat lower tensile properties, whereas the water coag-
Figure 5 Typical stress-strain cur-
ves of bagasse fibres prepared in
various coagulants.
Table 2 Mechanical properties of bagasse fibres prepared in various coagulants.
Coagulant
Tensile Strength
(MPa)
Initial Modulus
(GPa)
Elongation at break
(%)
Water/NMMO 427 10 (30) 13 1 (909) 15 2
Ethanol 394 8 (26) 21 2 (1372) 4.3 1
Methanol 349 7 (23) 13 1 (861) 10 1.5
Isopropanol 349 9 (24) 17 2 (1149) 11 1.8
Water 247 6 (18) 10 1 (709) 9.3 1.6
Note: The values in parentheses are in cN/tex.
Preparation and Physical Properties of Regenerated Cellulose Fibres A. J. Uddin et al. 1853 TRJ
ulant fibre possesses the lowest of all. These overall results
support the well-known fact that the higher the spin-draw
ratio (Table 1), the higher the tensile strength and modulus
The temperature dependence in mechanical properties
is revealed by dynamic viscoelastic analyses. In Figure 6,
the temperature-dependent storage modulus (E) of all the
bagasse fibres is illustrated. Considering the structural
parameters and tensile properties, the water/NMMO and
ethanol coagulated fibres are expected to show the highest
E values across the entire temperature range. But the eth-
anol coagulated fibre shows a strange E curve. A closer
examination of the E curve of this fibre indicates an increase
of between 50 and 105 C, may be due to the removal of
trapped ethanol/water. The curve then follows a sharp
decrease, perhaps due to the plasticising effect of remain-
ing NMMO trapped inside the fibre during coagulation
(later confirmed by FTIR as illustrated in Figure 7). Since
NMMO starts to decompose at around 170C, the curve
again turns towards an increasing trend. Unlike ethanol
coagulated fibre, the E curve of water/NMMO coagulated
fibre does not show such an unusual pattern though it also
has some NMMO in its matrix (Figure 7). But the content
and the pattern of NMMO in water/NMMO and ethanol
coagulated fibres seem to be different. In the case of the
ethanol coagulated fibre, NMMO may become trapped in
the core part of fibre surrounded by its hard skin and so
NMMO in the core part decomposes at 170 C as seen in
its E curve. Such skin-core structure was found for isopro-
panol coagulated NMMO-type cellulose fibre [27]. Unlike
the ethanol coagulated fibre, the water/NMMO fibre may
not have the skin-core structure as the solvent and the
coagulant in this case are the same, NMMO. In this case,
NMMO may just randomly exist in fibre matrix and evapo-
rate slowly with the gradual increase of temperature during
the measurement of storage modulus in dynamic mood.
NMMO Removal from the Fibre Matrix
The remaining NMMO in the water/NMMO and ethanol
coagulated fibres was investigated by FT-IR spectra. As
shown in Figure 7, the stretching bands at 1260 and 800 cm
1
,
corresponding to the (-CN) and (-NO) stretching of
NMMO, were observed in these fibres. This finding is in
good agreement with our previous assumption. To elimi-
nate NMMO from the fibres, both fibres were subjected to
hot drawing and/or heat treatment. To do this, for the etha-
nol coagulated fibre, the near melting temperature of
NMMO (170C), the lowest sagging point in its E curve
(Figure 6), was selected. At 170C, this fibre could be drawn
up to 1.2 times perhaps due to plasticising effect of NMMO
and then kept for 5 min in that state with tension. In the
case of the water/NMMO coagulated fibre, the tempera-
ture at 250C, at which E begins to drop (Figure 6), was
selected. This fibre could not be drawn even at a high tem-
perature because it was already highly crystallised and ori-
ented (Table 1) as well as fibrillated (Figure 4). Hence, this
fibre was only heat treated with tension for only 5 min at
250C. The IR bands of NMMO for both fibres then disap-
Figure 6 Storage modulus of
bagasse fibres prepared in various
coagulants.
1854 Textile Research Journal 80(17) TRJ TRJ
peared (Figure 7), which confirmed the complete elimina-
tion of NMMO from the fibres.
Characteristics of Fibres after NMMO Removal
Stress-strain curves of water/NMMO and ethanol coagu-
lated bagasse fibres after NMMO removal are illustrated
in Figure 8 along with the curve of commercial lyocell
fibre. The ethanol coagulated fibre exhibits a brittle mode
of deformation behaviour with no apparent yield point,
and a regime of sharply rising stresses until rupture. Con-
versely, the water/NMMO coagulated fibre still shows a
yield point and comparatively higher strain until rupture.
The steeper initial slope for both fibres indicates their
Figure 7 FT-IR curves of water/
NMMO and ethanol coagulant
bagasse fibres, showing the elimi-
nation of NMMO after heat treat-
ment.
Figure 8 Typical stress-strain
curves of water/NMMO and etha-
nol coagulated fibres after NMMO
removal in comparison with the
curve of commercial lyocell fibre.
Preparation and Physical Properties of Regenerated Cellulose Fibres A. J. Uddin et al. 1855 TRJ
toughness, that is, their larger initial resistance to applied
stress.
The storage modulus curves (E) of these fibres are
shown in Figure 9. The sagging part of the curve of the etha-
nol coagulated fibre is completely eliminated after NMMO
removal. Moreover, after NMMO removal, the E values for
both the water/NMMO and ethanol coagulated fibres across
the entire temperature range have markedly increased. The
increase in E suggests that high levels of molecular orienta-
tion and crystallinity are achieved after NMMO removal
and heat treatment.
The WAXD images of these fibres, shown in Figure 10,
also clearly indicate the improvement in crystallinity and
crystal orientation after NMMO removal. Table 3 lists the
structural and mechanical properties of the water/NMMO
and ethanol coagulated fibres. The structural improvements
of the fibres have a strong correlation with their respective
increase in tensile properties. After NMMO removal, both
fibres show improved molecular structures, such as crystallin-
ity, lattice spacing, crystal orientation and birefringence that
noticeably enhance their mechanical properties and reduc-
tion in elongation at break. The higher tensile strength and
modulus of ethanol coagulated fibre compared with water/
NMMO coagulated fibre may be attributed to its higher
crystallinity, crystal orientation, birefringence and smaller
crystal lattice spacing. The SEM images of the fracture and
Figure 9 Storage modulus of
water/NMMO and ethanol coagu-
lated fibres after NMMO removal in
comparison with the storage mod-
ulus of commercial lyocell fibre.
Figure 10 WAXD images of water/
NMMO and ethanol coagulated
bagasse fibres after NMMO removal
and heat treatment.
1856 Textile Research Journal 80(17) TRJ TRJ
surface of these fibres, shown in Figure 11 and Figure 12,
respectively, demonstrate the higher fibrillation of ethanol
coagulated fibre in comparison with water/NMMO fibre.
As shown in Table 3, the occurrences of higher fibrillation
of the ethanol coagulated fibre can be attributed to its higher
degree of crystallinity, smaller lattice spacing and higher ori-
entation of both crystalline and non-crystalline regions of the
fibre. Such fibrillation is generally observed for highly crys-
tallised and highly oriented lyocell fibres [34, 35].
In this work, the tensile strength of 530 MPa and initial
modulus of 33 GPa are reported for bagasse regenerated
fibre. These values are comparable with those of the com-
mercial lyocell fibre used in our study (tensile strength 486
MPa and initial modulus 16 GPa) and those reported in
related literature (tensile strength 525~600 MPa, and ini-
tial modulus 8~18 GPa) [36, 37].
Conclusion
Sugarcane bagasse was dissolved in N-methylmorpholine-
N-oxide (NMMO) 0.9 hydrate, and fibres were prepared
by the dry jet-wet spinning method. We evaluated different
kinds of coagulating agents, including water/NMMO
(10%), water only, methanol, isopropanol and ethanol and
compared the structures and properties of the resulting
fibres. The fibres prepared in water/NMMO and ethanol
coagulant showed better physical properties even though
the solvent NMMO remains in the fibre matrix. After
removal of NMMO by heat treatment, further improve-
ment in the structures and properties for these fibres were
achieved. The fractured cross-sections and surfaces of
these fibres reveal the occurrence of fibrillation due to
higher crystallinity and molecular orientation.
Considering the structure and mechanical properties of
the fibres prepared in this work, it can be concluded that
Table 3 Mechanical properties and structural parameters of water/NMMO and ethanol coagulated bagasse fibres after
NMMO removal by heat treatment.
Coagulant
Tensile
Strength,
(MPa)
Initial
Modulus,
(GPa)
Elongation at
break
(%)
Degree of
Crystallinity, X
c

(%)
Lattice Spacing,
d ()
Degree of
crystal
orientation, f
c
Birefringence
n 10
3
Water/NMMO 502 (33.5) 26 (1733) 6 60 4.246 0.85 20.8
Ethanol 530 (35) 33 (2171) 2 69 4.218 0.88 23.2
Note: The values in parentheses are in cN/tex.
Figure 11 SEM images of fractured water/NMMO and ethanol coagulated bagasse fibres after NMMO removal by heat
treatment.
Preparation and Physical Properties of Regenerated Cellulose Fibres A. J. Uddin et al. 1857 TRJ
sugarcane bagasse, which is generally considered as waste
product, can produce regenerated cellulose fibres with
mechanical properties comparable to those of commercial
lyocell fibre.
Acknowledgements
The authors are indebted for support of this work by the
Grant-in-Aid for the Global COE program by the Ministry
of Education, Culture, Sports, Science and Technology of
Japan.
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