Cellulose (2009) 16:481–489
DOI 10.1007/s10570-009-9279-z
Dyeing behaviour of lyocell fabric: effect of NaOH
pre-treatment
Parikshit Goswami Æ Richard S. Blackburn Æ
Jim Taylor Æ Patrick White
Received: 6 November 2007 / Accepted: 25 January 2009 / Published online: 11 February 2009
Ó Springer Science+Business Media B.V. 2009
Abstract To understand the effect of alkali pre-
treatment on the dyeing of lyocell fabrics, samples
are pre-treated with 0.0–7.0 mol dm-3 NaOH using
a pad-batch process and then dyed with different
types of reactive dyes. Exhaustion, fixation, and
visual colour strength (K/S values) are measured. It is
observed that sodium hydroxide pre-treatment signif-
icantly improves the colour yield, exhaustion, and
fixation for all dyes used. Highest K/S values are
obtained when the fabrics are pre-treated with 2.0–
2.5 mol dm-3 NaOH. Cross-sectional analysis shows
that below this optimum concentration the core fibres
in the yarn are not dyed; at optimum concentration all
fibres in yarn cross-section are homogeneously dyed.
Cross-sectional analysis shows that as the pre-treat-
ment concentration of NaOH increases above
2.5 mol dm-3, the fibres change progressively from
a circular to angular cross-section, forming a solid
unit. The decrease in K/S above the treatment
concentration of 2.5 mol dm-3, though the %E and
%F remains almost constant, is attributed to the
This paper was presented at the 2nd International Cellulose
Conference, Tokyo, Japan, 24th October 2007.
P. Goswami
R. S. Blackburn (&)
Green Chemistry Group, Centre for Technical Textiles,
University of Leeds, Leeds LS2 9JT, UK
e-mail: r.s.blackburn@leeds.ac.uk
J. Taylor
P. White
Lenzing Fibers, Lenzing, Austria
distribution of dye over a larger surface area of the
outer fibres in the yarn cross section, forcing the K/S
at kmax to decrease.
Keywords Regenerated cellulose

Cellulose II
Sodium hydroxide
Swelling

Reactive dyes
Diffusion
Morphology
Introduction
Cellulose is the most abundant biopolymer (Klemm
et al. 2005) and of particular interest in providing
renewable, sustainable, biodegradable biopolymers
for industrial applications. Cellulose is a linear 1,4-b-
glucan polymer; the units are able to form highly
ordered structures, as a result of extensive interaction
through intra- and intermolecular hydrogen bonding of
the three hydroxyl groups in each glucose unit. We
have recently provided (Goswami et al. 2009) an
extensive review of the treatment of cellulose with
sodium hydroxide (NaOH); alkali has a substantial
influence on morphological, molecular and supramo-
lecular properties of cellulose, causing changes in
crystallinity, pore structure, accessibility, stiffness,
unit cell structure and orientation of fibrils in cellulosic
fibres. Treatment with alkali can improve mechanical
and chemical properties of cellulose fibres such as
dimensional stability, fibrillation tendency, dyeability,
reactivity, lustre and fabric smoothness. Factors such
as the concentration of NaOH, treatment temperature,
123
482
applied tension, residence time, source of cellulose,
physical state of cellulose (fibril, fibre, yarn or fabric),
and degree of polymerisation have an effect on the
properties and degree of change upon treatment
(Heinze and Wagenknecht 1998; Colom and Carrillo
2002; Jaturapiree et al. 2006; Manian et al. 2008). In
general, there is limited research in this area on
cellulose II polymers; researchers have concluded that
when cellulose I is converted to cellulose II the
crystallinity index decreases, therefore, it is interesting
to understand the change in crystallinity of cellulose II
polymers when treated in alkali, particularly consid-
ering the increasing demand for lyocell fibres.
Lyocell fibres may be defined as cellulosic fibres
that are produced by regenerating cellulose into fibre
form out of a solution in an organic solvent (Albrecht
et al. 1997). Solvent spun lyocell fibres consist of
crystalline cellulose II and amorphous cellulose
and have a higher degree of crystallinity (80%) in
comparison with other regenerated cellulosic fibres,
such as modal (49%) and viscose (41%) (Colom and
Carrillo 2002). The high degree of crystallinity in
lyocell is a consequence of higher orientation during
stretching and formation of fibres; lyocell fibres have
the thinnest and longest crystallites, even the amor-
phous regions are oriented along the fibre axis (Kreze
and Malej 2003). Lyocell fibres spun from cellulose
solution in N-methylmorpholine-N-oxide (NMMO)
hydrate have proven commercially successful in
textile and nonwoven products due to their excellent
mechanical properties in the wet state, when com-
pared with viscose rayon (Loubinoux and Chaunis
1987; Lenz et al. 1993; Mortimer and Peguy 1996;
Chae et al. 2002). The manufacturing process is
environmentally benign because the non-toxic, bio-
degradable NMMO solvent used is almost completely
recycled (Woodings 1995; Albrecht et al. 1997;
Schuster et al. 2004). Additionally, the spinning baths
are filtered, cleaned, upgraded and then fed back into
the system and the proportion of used NMMO
recovered in practice is over 99.5%. The efficiency
of the system developed is such that the consumption
of NMMO can be kept down to a few kilograms per
tonne of fibre produced (Lennox-Kerr 1994; Albrecht
et al. 1997). The life cycle of a lyocell fibre has
minimal environmental impact and it is argued that
the fibre is significantly more sustainable than oil-
derived synthetic fibres (e.g., polyester, nylon,
acrylic) and natural fibres such as cotton (which
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Cellulose (2009) 16:481–489
requires significant areas of land, irrigation, pesticides
and fertilizers to grow, which the eucalyptus trees,
from which lyocell is made, do not; White et al. 2005).
Due to the unique highly crystalline structure of
lyocell, and weaker lateral links between the crystal-
lites, the fibres undergo localized separation of fibrous
elements at the surface known as fibrillation, mainly
under conditions of wet abrasion (Zhang et al. 2005;
Abdullah et al. 2006). Fibrillation is the longitudinal
splitting of a single fibre into microfibres of typically
less than 1–4 lm in diameter (Chavan and Patra
2004). This fibrillation behaviour restricts the appli-
cations of lyocell; in particular, fabric dyed in dark
hues, as medium/heavy depths can develop a ‘frosty’
(greying) appearance caused by very fine fibrils that
are visually transparent; we have demonstrated pre-
viously (Goswami et al. 2007) that fibrillated lyocell
shows lower visual colour yield in comparison with
non-fibrillated lyocell, independent of exhaustion and
fixation. If fibrillation is not controlled, these micro-
fibres become entangled giving a serious problem of
‘pilling’. Processing of lyocell is more technically
challenging in fabric and garment form compared to
other regenerated cellulosic fibres due to fibrillation
(Bates et al. 2004), and for overall success in the
textile industry, it is important to understand the
dyeing behaviour of fibrillated lyocell thoroughly to
overcome this problem.
Colom and Carrillo (2002) studied the effect of
sodium hydroxide treatment on crystallinity in the
cellulose II polymers lyocell, modal and viscose, and
followed this with a separate study comparing
lyocell, acid-hydrolysed lyocell, and standard crys-
talline cellulose I (Carrillo et al. 2004). Recently, we
have observed (Goswami et al. 2009) that sodium
hydroxide treatment causes the density, orientation
and crystallinity of lyocell fibre to decrease with
increasing sodium hydroxide concentration, and that
the greatest change in fibre properties occurs between
3.0 and 5.0 mol dm-3 NaOH. This was attributed to
the onset of formation of sodium(Na)-cellulose II at
3.0 mol dm-3 NaOH; a fully formed Na-cellulose II
structure was observed above 6.8 mol dm-3 NaOH.
The work concluded that formation of Na-cellulose II
causes plasticization of the lyocell fibres as both
inter- and intra-molecular hydrogen bonds are broken
by these higher sodium hydroxide concentrations.
In this study, lyocell fabrics were pre-treated with
varying concentrations of sodium hydroxide and then
Cellulose (2009) 16:481–489
dyed with nine different types of reactive dyes
in order to ascertain the optimum concentration of
NaOH that can afford high colour yield.
Experimental
Materials
De-sized, 100% lyocell, 2 9 1 twill, ring spun warp
(1/22 Ne; 40 ends cm-1), open end spun weft (1/12
Ne; 22 picks cm-1), 240 g m-2 was supplied by
Lenzing Austria. Samples of Procion Deep Red
H-EXL, Procion Red H-E3B (C.I. Reactive Red 120),
Procion Yellow H-E6G (C.I. Reactive Yellow 135),
Procion Yellow H-EXL (C.I. Reactive Yellow 138:1),
Procion Navy H-EXL, and Procion Orange H-ER
(C.I. Reactive Orange 84) were kindly supplied by
DyStar, Germany. Samples of Cibacron Brilliant Red
4G-E, Cibacron Navy W-B (C.I. Reactive Black 5),
and Cibacron Orange 4R (C.I. Reactive Orange 35)
were kindly supplied by Ciba, Switzerland. The
dyeing auxiliary Sandozin NIN (non-ionic surfactant)
was supplied by Clariant, UK. Embedding liquor
JB-4 was supplied by Agar Scientific. All other
chemicals were supplied by Aldrich.
Methods
Scouring
Lyocell fabric was scoured in a Roaches Rotohose
rotary drum dyeing machine for 15 min at 60 °C with
1 g dm-3 Sandozin NIN and 2 g dm-3 sodium car-
bonate using a liquor ratio of 20:1.
Alkali pre-treatment
Lyocell fabrics were treated with aqueous concentra-
tions of NaOH between 0.0–7.0 mol dm-3 by a pad-
batch process. Samples were immersed in an aqueous
NaOH solution, passed through an Ernst Benz
padding mangle applying a pressure of 10 kg cm-2,
and then batched for 30 min by wrapping around a
glass rod and enveloping the sample in poly(ethylene)
sheet. The samples were subsequently removed from
the glass rod, rinsed in hot water for 5 min, and then
immersed in 5% aqueous acetic acid at room
temperature for 60 min. Samples were then rinsed
483
in cold water for 5 min and dried. The pH of the
samples was measured by a Werner Mathis Morapex-
A machine, which passes distilled water through the
sample at 40 °C and measures the pH of the resultant
solution. Wet pick-up of the samples is calculated
using Eq. 1, where W is the weight of the sample
after padding and D is the dry weight of the sample:
 
W D
Wet pick up ¼ 100 ð1Þ
D
Dyeing
Lyocell fabric samples (10 g) were dyed with reactive
dyes at 2% on mass of fibre (omf) in a Mathis Air Boy
dyeing machine, using a liquor ratio of 20:1, according
to the methods shown in Figs. 1 and 2 for Procion and
Cibacron dyes, respectively. After dyeing the fabric
samples were thoroughly rinsed with cold water, then
washed for 30 min at 95 °C using a liquor ratio of 20:1,
and dried flat at ambient conditions.
Colour measurement
After drying, samples were measured using a Data-
color SF600 Spectraflash colour spectrophotometer
connected to a personal computer using DCI Colour
Tools software. From reflectance values (R) at a
specified wavelength (k) of the dyeings, the colour
strength (K/S) of the sample was calculated using the
Kubelka-Munk equation (Eq. 2; McDonald 1980):
ð1  Rk Þ2
K=S ¼ ð2Þ
2Rk
Fig. 1 Dyeing profile for dyeing lyocell with Procion dyes
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484 Cellulose (2009) 16:481–489

170 47

160 46

150 45

140 44

% wet pick-up

x c (%)
130 43

120 42

110 41

100 40
% wet pick-up
90 39
xc (%)
80 38
0 2 4 6
-3
NaOH (mol dm )

Fig. 2 Dyeing profile for dyeing lyocell with Cibacron dyes
UV/visible spectrophotometry
The exhausted dyebaths, and wash-off liquors were
measured using a Perkin–Elmer Lambda 9 UV/
Visible/NIR spectrophotometer in the visible region
of the spectrum (400–700 nm), at 2 nm intervals.
Concentrations were calculated from calibration
graphs at the wavelength of maximum absorption
(kmax). The residual dye solutions were diluted using
distilled water and measured at kmax and the concen-
tration of residual dye in solution calculated from
calibration plots, and dye adsorbed by the fibre
calculated from the difference before and after
exhaustion. No difference in the shape of the absorp-
tion spectrum before and after dyeing was noted.
Fig. 3 Comparison of % crystallinity (xc; Goswami et al.
2009) and % wet pick-up with increasing NaOH concentration
in the pre-treatment bath
in the pre-treatment bath xc decreases, accompanied
by a corresponding increase in % wet pick-up. It is
logical that as crystallinity of the cellulose II fibre
(and associated hydrogen bonding) decreases, the
sorption of water by the lyocell fibre will increase, as a
result of a greater potential for hydrogen bonding
between water molecules and the fibre and increased
swelling of the fibre.
Exhaustion (%E), fixation (%F) and K/S values at
kmax (colour strength) of NaOH pre-treated lyocell
dyed with Procion and Cibacron reactive dyes were
calculated, and it is found that, in general, the trends
observed were similar for each dye. A representative
example is shown in Fig. 4 for C.I. Reactive Red

Cross-sectional analysis

After dyeing, alkali pre-treated samples were embed-

ded in resin using a JB-4 embedding kit and 6 lm
cross-sections cut using a Beck Microtome. These
sections were analysed and pictures taken using an
Olympus BH-2 optical microscope attached to a
digital camera system.

Results and discussion

It is noted that all alkali pre-treated samples show very

little variation in pH (6.5–6.8) after neutralisation.
Figure 3 shows a comparison between % crystallinity
(xc; Goswami et al. 2009) and % wet pick-up, and it is
observed that with increasing concentration of NaOH
Fig. 4 Comparison of K/S values at kmax, % Exhaustion, and
% Fixation for lyocell treated with different concentrations of
NaOH for C.I. Reactive Red 120 (structure shown)

123
Cellulose (2009) 16:481–489 485

120, where it is observed that NaOH pre-treatment
improves the colour strength at all concentrations
with respect to the untreated sample. The trend
observed is that initially as concentration of NaOH in
the pre-treatment stage increases, resultant colour
strength also increases accompanied by similar
increases in %E and %F, to a maximum at around
2.0–2.5 mol dm-3 NaOH.
Cross-sectional analysis was performed on alkali
pre-treated lyocell yarns taken from the fabrics that had
been dyed with Cibacron Brill Red 4G-E (Fig. 5) and
C.I. Reactive Black 5 (Fig. 6). It is observed that the
fibres in the core of the yarn have significantly less dye
when the lyocell had not been pre-treated with alkali
(Figs. 5a, 6a) and when the alkali concentration in the
pre-treatment bath was low (up to 1.5 mol dm-3;
Figs. 5b, 6b), and most of the dye adsorbed is located at
the periphery of the yarn. However at a concentration
of 2.0 mol dm-3 NaOH (Figs. 5c, 6c), is it seen that all
the fibres in the yarn cross-section are uniformly dyed;

Fig. 5 Optical cross-

sections of lyocell filaments
in a yarn dyed with 2% omf
Cibacron Brilliant Red
4G-E following pre-
treatment with:
a 0.0 mol dm-3 NaOH;
b 1.5 mol dm-3 NaOH,
c 2.0 mol dm-3 NaOH,
d 5.0 mol dm-3 NaOH,
and e 7.0 mol dm-3 NaOH.
Scale bar is 20 lm

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486 Cellulose (2009) 16:481–489

Fig. 6 Optical cross-

sections of lyocell filaments
in a yarn dyed with 2%
omf C.I. Reactive
Black 5 following
pre-treatment with:
a 0.0 mol dm-3 NaOH,
b 1.5 mol dm-3 NaOH,
c 2.0 mol dm-3 NaOH,
d 5.0 mol dm-3 NaOH, and
e 7.0 mol dm-3 NaOH.
Scale bar is 20 lm

this finding is in agreement with the findings of Bui
et al. (2008), where they reported an increase in
porosity and accessibility in lyocell fibres after
treatment with NaOH solution. The increase in %E,
%F, and K/S from concentrations of 0.0–2.0 is
attributed to a decrease in density and crystallinity
of lyocell fibre with increasing concentration of
NaOH in the pre-treatment bath (Goswami et al.
2009); as adsorption and diffusion of dyes only occurs
in the amorphous regions of a fibre this decrease in
crystallinity affords the corresponding increase in dye
sorption.
In spite of this phenomenon, at concentrations of
NaOH above 2.0–2.5 mol dm-3, the K/S values
decrease with increasing NaOH concentration to a
plateau around 5.0 mol dm-3 NaOH. %E and %F, in
general, are constant after 2.5–3.0 mol dm-3 NaOH,
hence, the observed decrease in K/S values must be

123
Cellulose (2009) 16:481–489
due to some other reason. Observing the location of
the dyes through the yarn cross-section at NaOH pre-
treatment concentrations of 5.0 mol dm-3 (Figs. 5d,
6d) and 7.0 mol dm-3 (Figs. 5e, 6e), it is observed
again that there is a higher concentration of dye
located in the peripheral fibres in comparison with the
fibres in the centre of the yarn, even though the
overall %E is higher in comparison with lower
concentrations.
It was also observed from the cross-sections that
with increasing NaOH concentration, the fibres in the
yarn cross-section changed from a circular shape to a
more angular shape; deformation of the fibres occurs
because, in the presence of NaOH, the fibres swell
(Goswami et al. 2009). It is proposed that with
increasing NaOH concentration the extent of hydrogen
bonding in cellulose is reduced and the degree of
swelling increases; the internal voids in the twisted
yarns become limited, neighbouring fibres are
squeezed together with increasing pressure, the fibres
deform to occupy the voids forming a solid unit, and the
fibres lose there circular cross-section. After the pre-
treatment process and subsequent rinsing the fibres
contract again opening up voids once more, but the
fibres retain their angular shape and do not revert to a
circular cross-section. On subsequent dyeing of lyocell
fabrics that have been pre-treated at higher NaOH
concentrations, in the aqueous dyebath the lyocell
reforms the solid unit on swelling and it becomes
difficult for the dye molecules to diffuse within the
interior of the yarn. Only the surface fibres are dyed
where the cellulose sorption surface is exposed to the
dye solution; the core of the yarn is virtually undyed.
However, even though the fibres in the core of the
yarn remain undyed the exhaustion and fixation
remain almost the same above 2.5–3.0 mol dm-3
NaOH. We have observed previously (Goswami et al.
2009) that the greatest change in lyocell fibre
properties, when treated with NaOH occurs between
3.0 and 5.0 mol dm-3. This is attributed to the onset
of the formation of Na-cellulose II at 3.0 mol dm-3
NaOH; a fully formed Na-cellulose II structure is
expected above 6.8 mol dm-3 NaOH. Formation of
Na-cellulose II causes plasticization of lyocell fibres
as both inter- and intra-molecular hydrogen bonds are
broken by these higher NaOH concentrations. This
decrease in the density and crystallinity of the fibre
enhances the sorption properties of the outer fibres of
the yarn cross-section. It was demonstrated in our
487
Fig. 7 Comparison between the change in cross-sectional area
and K/S at kmax for samples dyed with Procion Deep Red H-
EXL over the concentration range 2.0–6.0 mol dm-3 NaOH
previous work that above a pre-treatment concentra-
tion of 5.0 mol dm-3 NaOH there is very little, if
any, further change in density and crystallinity, hence
explaining the observation herein that %E and %F
remain constant above 3.0 mol dm-3 NaOH.
Figure 7 shows the relationship between the
change in cross-sectional area (Goswami et al.
2009), and the change in K/S at kmax (example is
Procion Deep Red H-EXL) including the critical
range of 3.0–5.0 mol dm-3 NaOH, where cellulose II
is converted to Na-cellulose II. Sigmoidal fitting of
the experimental results in Fig. 7 enables correlation
between variations of these parameters with sodium
hydroxide concentration. From the sigmoidal fitting,
Eq. 3 is derived, where COH(s) is the sodium hydro-
xide concentration in aqueous solution and Y refers to
the physical property (i.e., cross-sectional area or K/S
at kmax), all the other parameters are constants and
their values given in Table 1, which also provides the
R2 value of each sigmoidal fit:
A1  A0
Y ¼ A0 þ   ð3Þ
C B
1 þ exp OHðsÞB1 0
Both cross-sectional area and K/S show very high
correlation with the sigmoidal fit over the concentra-
tion range, where it is observed that as NaOH
concentration increases, cross-sectional area increases
and K/S decreases;. It is proposed that in the range 2.0–
6.0 mol dm-3 NaOH, as the cross-sectional area
increases, the adsorbed dyes are distributed over a
greater surface area of the fibres, which causes a visual
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488
Table 1 Constants in above equation and correlation (R2) for sigmoidal fitting of experimental data based on various parameters
Y A0 A1
Cross sectional area 112.78421 146.49800
K/S at kmax 19.13863 15.93243
effect of the dyeing appearing lighter, explaining the
decrease in K/S within this range.
Conclusions
It was observed that NaOH pre-treatment significantly
improves the colour yield, exhaustion, and fixation for
all dyes used. Highest K/S values are obtained when
the fabrics are pre-treated with 2.0–2.5 mol dm-3
NaOH. Cross-sectional analysis shows that, below this
optimum concentration, the core fibres in the yarn are
not dyed; at optimum concentration, all fibres in yarn
cross-section are homogeneously dyed. Cross-sec-
tional analysis shows that as the pre-treatment
concentration of NaOH increases the fibres change
progressively from a circular to angular cross-section,
forming a solid unit. The decrease in K/S above the
treatment concentration of 2.5–3.0 mol dm-3, though
the %E and %F remain almost constant, is attributed to
the distribution of adsorbed dye over a larger surface
area of the outer fibres in the yarn cross section,
causing the decrease in K/S.
Acknowledgments The authors would like to thank Lenzing
AG and The UK Government (Overseas Research Scholarship
Awards Scheme) for the provision of a PhD scholarship to
Mr. Goswami.
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