Cationic Modification of Cotton Fabrics and Reactive
Dyeing Characteristics
Neboja Risti, Ivanka Risti
High Professional School of Textile, Leskovac, Jablanicki Okrug Serbia And Montenegro
Correspondence to:
Nebojsa Ristic email: bojana1998@ptt.rs
ABSTRACT
The effect of cationic modification of cotton fabrics,
using commercial agent Sintegal V7conc, on reactive
dyeing characteristics was studied in this work. The
changes after cationization and their effects on
practical application of reactive dyes were identified
by various methods. Cationically modified fabrics
have more positive zeta potential, compared to
untreated fabrics, which has a favorable influence on
reactive dyeing in the absence or presence of salt.
Color intensities of reactive dyes reached their
maximum on samples treated with the highest
concentration of Sintegal V7conc solution and dyed
in the presence of standard salt concentration. The
results obtained indicate that color intensity increase
is a combined contribution of both salt and cationic
agent on adsorption and fixation of reactive dyes on
cotton.
Keywords: Cationic modification, cotton, zeta
potential, reactive dye, dyeing.
INTRODUCTION
For cotton dyeing, reactive dyes have been used very
often and they are, by consumption, the most
important textile dyes [1]. High popularity of reactive
dyes is based on producing brilliant and fast colors
with a wide range of shades using various
environmentally friendly procedures. Reactive dyes
stand out from other dyes by their ability to make
covalent bonds between carbon atoms of dye reactive
group and oxygen atoms of cotton hydroxyl groups
under alkaline conditions [2]. Reactive dyes are
divided, according to the structure of reactive group,
in haloheterocycle and vinyl sulfone based dyes,
which react with cellulose through nucleophilic
substitution and addition mechanisms, respectively.
Commercially, the widest used systems are: vinyl
sulfone (VS), monochlorotriazine (MCT),
bifunctional dyes, difluoro chloropyridine (DFCP),
monofluorotriazine (MFT) and dichlorotriazine
(DCT). In addition to reacting with fiber, reactive
dyes also react with water (dye hydrolysis) in a form
which cannot bond to cotton, but behaves as a
Journal of Engineered Fibers and Fabrics
Volume 7, Issue 4 2012
substantive dye and affects color fastness on fabric.
The most important parameters affecting exhaustion
and fixation of reactive dyes are temperature, salt
concentration, alkali concentration, and liquid ratio
[3]. The main drawback of reactive dyes is low
equilibrium exhaustion, due to low dye affinity for
cotton, requiring high amounts of salt and alkali in
the dyeing bath, which, when released into the water
streams, produce disturbances in delicate
biochemistry of water organisms.
The purpose of physical and chemical procedures for
modification of cellulose fibers is to increase reactive
dye exhaustion and fixation degree and saving
electrolytes. The pretreatment to improve
functionality and dyeing ability of cellulose fibers,
using cationic agents, has attracted attention recently
[4-7]. The reason for such treatment is improvement
of cationic activities of cellulose fibers and reduction
of electrostatic repulsion of negative ions resulting in
a positive effect on absorption of anionic dyes and
poly electrolytes. Recently reported were the results
of chemical, structural and morphological changes of
cotton after treatment with triazine derivatives
containing cationic and anionic groups [8], and the
effects of the treatment on dyeing with reactive dyes
[9]. A number of changes are identified on modified
cotton: formation of new molecular structures
containing cationic and anionic groups, very low
reduction of crystallinity degree, and modification of
surface morphology. Modified cotton was dyed with
reactive dyes and a higher exhaustion and fixation
degree of reactive dyes was achieved as a result of
reaction with new groups. The pretreatment of cotton
fabrics with cationic polyvinyl amino-chloride
increases dye reactivity and induces the Freundlich
type of isotherm to be replaced by Langmuir type
after modification [10]. The increased yield of
reactive dye on cotton fabrics treated with
commercial cationic agent is explained by positive
surface charge of cationized cotton fiber [11].
Moreover, introduction of amine groups in the cotton
structure increases reactive dye yields due to ionic
113 http://www.jeffjournal.org
attraction between cationic groups and reactive dye
anions [12]. Precationization of cotton using
commercial agents containing epoxide group gave
better color yield during printing of cotton fabrics
with pigments and anionic dyes and lower loss of
color after several washing cycles [13]. It was found
that during cationization of cotton, etherification of
primary hydroxyl groups on cellulose takes place
[14]. The reaction is superficial since X-ray
diffraction showed that cationization has no effect on
cotton crystalline structure [15]. Dyeing of cationized
cotton without salt indicated that reactive group type
did not affect the dye yield on cationized cotton and
color fastness was not changed [16]. Commercial
cationic agents can also be successfully used to
enhance cotton dyeing with natural dyes in acidic
medium with ultrasound [17, 18].
In this study, cotton fabric was treated with
commercial cationic agent in order to enhance dyeing
ability of cotton with reactive dyes of various
functional groups. The dyeing was performed both
with and without salt. Identification of cationic agent
on cotton fabric samples was done by measuring
fabric zeta potential, retained water quantity, and the
use of scanning electron microscopy. The aim of this
work was to determine the changes on the surface of
cationized cotton fabrics and to correlate them with
reactive dyeing characteristics to improve reactive
dye utilization.
EXPERIMENTAL
Materials
Bleached cotton fabric with surface mass of 204.5
g/m2 was used in the experiment. Pretreatment was
made using commercial cationic agent Sintegal
V7conc (Chemapol, Czech Republic). Sintegal
V7conc is quaternized polyglykol ether of fatty
amine with cationic character. For dyeing the samples
the following dyes were used: monochloro triazine
reactive dyes Ostazin Red H-3B (C.I. Reactive Red
45:1) and Ostazin Blue H-BR (C.I. Reactive Blue 5)
(Chemapol, Czech Republic) and vinyl sulfone
reactive dyes Remazol Red B (C.I. Reactive Red 22)
and Remazol Brilliant Blue R (C.I. Reactive Blue 19)
(Dy Star, Germany). The dyes used were of
commercial grade.
Cationization of Cotton Fabric
The cotton fabric was treated with cationic agent
Sintegal V7conc solutions with three concentrations
(0, 5 g/L, 1 g/L and 2 g/L) by exhaustion method at
50oC without salt. After 30 minutes, 10 g/L Na2CO3
was added and the treatment prolonged for an
additional 30 minutes. The cationized samples were
neutralized with diluted acetic acid solution, rinsed
Journal of Engineered Fibers and Fabrics
Volume 7, Issue 4 2012
with water and dried at room temperature. Table I
shows sample labels and treatment parameters.
TABLE I. Sample labels and treatment parameters.
MEASUREMENTS AND ANALYSIS
Zeta Potential Measurement
The Zeta potential of cotton fibers was measured by
the streaming method using an electrokinetic
analyzer (EKA, A. Paar) in a cylinder cell adjusted
for textile fiber measurement. Measurement was
performed in relation to pH values of electrolyte
solution (10-3 mol/dm3 KCl). The fiber sample, 1 g
mass, is placed in the instrument measuring cell
between two electrodes (Ag/AgCl). Under the
influence of the given pressure, electrolyte solution
flows through the measuring cell with the stationary
sample. As a result of hydrodynamic streaming of
liquid through the sample, a streaming potential (Up)
or streaming current (Ip) arises which is then
measured on an electrokinetic analyzer. From the
given values, zeta potential is calculated according to
the Helmholtz-Smoluchowsky equation [19]:
U p L
(1)
0 Q R p
or
I p L
(2)
0 Q R p
where, zeta potential (mV), Up streaming
potential (mV), Ip streaming current (mA),
permittivity electrolyte solution (Fm-1)(kgm-3s4A2), 0
vacuum permittivity (Fm-1)(kgm-3s4A2),
dynamic viscosity of solution (Pas)(kgm-1s-1), p
pressure difference between capillary ends (Pa)
(Nm-2), L capillary length (m), R electrical
resistance (), Q capillary cross-section (m2).
To measure zeta potential, the samples of cotton
fabric were washed in deionized water to
conductivity of 1-4 S/cm.
SEM Analysis
For the characterization of surface morphological
changes, the scanning electron microscope JEOL
JCM 5300 (Jeol-Japan) was used. The samples were
prepared for scanning using the standard preparation
114 http://www.jeffjournal.org
procedure applying gold vapor to fiber surface for K
five minutes to make it conductive for cathode
S T
deposition of gold vapor. F 100% (5)
K
Water Retention Value
To determine the water retention, the samples of S 0
cotton fabrics were immersed in distilled water for 24
hours and then centrifuged at 7800 min-1 for 2 Where subscript T refers to fabric treated in soap
minutes. After weighing (Ww) and drying at 105oC, solution and subscript 0 to untreated fabric.
the mass of dry samples (Wd) was measured and
water retention values calculated from: Percentage of dye intensity increase (I) on cationized
samples compared to untreated sample is given by
WRV Ww Wd / Wd (3) the following equation:

K / S k K / S o
Dyeing and Colo r Measurements I= 100% (6)
The dyeing of 4 g samples was carried out in an K / S o
Ahiba type G7B laboratory apparatus with vertical
movement of material at a bath ratio of 1:45. Where subscript k refers to cationized fabric samples
and subscript 0 to untreated fabric.
All dyeing was carried out using the All-in method.
Dye concentration was 1% based on material mass, Color uniformity was calculated by measuring K/S
Na2CO3 20 g/L and NaCl concentrations were 0, 10 values on 20 random sample spots at maximum
and 50 g/L. absorption wave lengths using Eq. (7) and Eq. (8):
Dyeing was carried out at 80oC (Ostazin dyes) and 2

( K / S ) ( K / S )
60oC (Remazol dyes) for two hours, reaching n

temperatures in 20 min. Dyeing start was at room i,

temperature. After dyeing, the samples were washed ( ) i 1
(7)
and divided in two parts. One sample part was treated n 1
in anionic washing agent solution Jugopon 50
(sodium salt of alkyl benzene sulfonate, Chromos, n
Croatia) with 2 g/L concentration at 95oC for 10 min. K / S 1
n K / S i, (8)
After rinsing and drying at room temperature, i 1
coloristic measurements were made on both sample
parts on reflexion spectrophotometer Spectraflash SF Where () is the standard deviation of each random
600X (Datacolor, USA) to determine color intensity spot K/S value with (K/S), is the maximum
(K/S), fixation degree F, percentage increase in color absorption wave length, n is the number of measured
intensity (I), and color uniformity (). spots, and (K/S)i, is the K/S value of each random
spot.
Color intensities (K/S) were determined at maximum
dye absorption wave length (Ostazin Red H-3B, = Color uniformity expressed by () is improved when
550 nm; Ostazin Blue H-BR, = 630 nm; Remazol () value decreases [20].
Red B, = 520 nm and Remazol Brilliant Blue R, =
610 nm) using Kubelka-Munk equation: Wash fastness was determined according to ISO 105-
CO6 (1994).
K 1 R
2
(4) RESULTS AND DISCUSSION
S 2R Zeta Potential
The surface of textile fibers in neutral water solutions
where: K light absorption coefficient, S light is negatively charged due to dissociation of
scattering coefficient, R D65/10 light reflection. functional groups and adsorption of ions from the
solution, inducing formation of electrical double
K/S values were calculated based on reflection values layer in water solutions of electrolytes. Dissociated
of untreated and soap solution treated sample, and carboxyl groups formed by oxidation of aldehyde
fixation degree was calculated from Eq. (5): groups on terminal glucoside units also contribute to

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Volume 7, Issue 4 2012
the negative charge of the cotton surface apart from
dissociation of functional hydroxyl group. The
negative surface charge of textile fibers, known as
zeta potential (), hampers anionic dye adsorption on
the fiber surface [21] and has a greater significance
for dye utilization if dye affinity is lower. The Zeta
potential of cotton fabric was measured by streaming
current method depending on pH values of 0,001 M
KCl solution in a pH range of 2, 5 to 10.
Measured zeta potential values, shown in Figure 1,
indicate dissociation of functional groups (-OH and
COOH) of cotton cellulose inducing negative fabric
charge. At all solution pH values, untreated cotton
fabric had the lowest zeta potential value and the
lowest pH value when = 0. Negative charge of
cationized cotton fabrics is significantly lower
irrespective of treatment agent concentration. It is
obvious, from measured zeta potential values at pH
10, that all cationized fabrics are much more
positively charged and, therefore, show better
adsorption of anionic dyes [22, 23]. In this work, a
long chain cationic compound, commercial product
Sintegal V7conc was used at three different
concentrations. Binding of cationic surfactant during
the treatment leads to the change of fabric surface
charge. The change appears first inside the so called
Stern's layer. Due to long hydrophobic chain, the next
step of adsorption is tail-to-tail binding resulting in
orientation of positive molecule part toward solution,
so the positive charge appears to be more positive
zeta potential. It was shown that this molecular
orientation increases zeta potential of cotton fabrics
cationized with Sintegal V7conc from = -19 mV for
P0 to = -15,3 mV for P0,5, to = -14,9 for P1 and
to = -13,7 mV for P2 at pH 10, which are reactive
dyeing conditions.
10
[m V ]
5 dyeing and hygienic properties during product
pH
0
2 3 4 5 6 7 8 9
-5
-10
P0
-15 P0,5
P1
P2
-20
FIGURE 1. Zeta potential () of cotton fabric cationized with
different concentrations of Sintegal V7conc in relation to pH of
electrolyte 0,001M KCl.
Journal of Engineered Fibers and Fabrics
Volume 7, Issue 4 2012
Surface Morphology
Cotton fiber surface structure was examined by
scanning electron microscopy in order to estimate the
cationization effect on surface morphology. Figure
2(a) shows a micrograph of untreated cotton fiber
surface where a system of shallow parallel grooves
can be seen. Figure 2(b) and Figure 2(c) depict
micrographs of cationized fiber surface. It can be
noticed, based on these micrographs, that there are no
big changes in surface morphology, though the
cationized fiber surfaces are slightly rougher than that
of untreated cotton fiber, due to cationization agent
deposits. Apart from increased roughness of modified
cotton fibers, it can be concluded that the extent of
cationization did not affect the fiber physical
structure, so the hand of treated samples remained
unchanged. This is an advantage of the treatment
compared to polymer material treatment which
produces certain stiffness of fabrics.
Water Retention Value
Wetting and soaking of liquids is especially
important in industrial processes such as dyeing and
finishing. Wetting, transport and retention of liquids
in porous textile materials are complex phenomena
depending on fiber surface morphology and geometry
of fabric pores. Changes of chemical composition,
fiber surface morphology, and structure of fiber pores
can modify fabric hydrophilic characteristics. Figure
3 shows retained water values for untreated and
cationically modified fabrics. On cationically
modified cotton fabrics, water retention value is
minimally reduced because cationization occurs
mainly on primary hydroxyl groups of C-6 atom of
cotton cellulose [24], so certain number of functional
groups is blocked for water molecules. Probably, the
fabric pore structure is slightly changed, resulting
also in slightly reduced water retention values. Very
small change of hydrophilicity of cationized samples
cannot negatively affect cotton fiber swelling during
exploitation.
10
116 http://www.jeffjournal.org
 0,5

0,4

0,3

WRV (g/g)
0,2

0,1

0
P0 P0,5 P1 P2

(a)
FIGURE 3. Retained water value of cationized cotton fabrics.

Dyeing Characteristics
As already mentioned in the introduction, reactive
dyes have a low affinity for cotton and, therefore,
high salt (NaCl or Na2SO4) concentrations are added
to the dyeing bath, which with deep shades amount
up to 100 g/L. Although high quantities of salts are
added, utilization of these dyes, in practical systems,
amounts up to 50-60%. From this reason, increasing
reactive dye utilization would have great
environmental and economic importance, which is
(b) why cationic modification of cotton is suggested.

In this work, standard commercial dyes with different

functional groups and a commercial cationic agent
were used in order to evaluate precationization
efficiency and effect on reactive dye absorption and
fixation, and to estimate application possibilities in
actual industrial systems.

Figures 4-7 clearly indicate the color intensities of

(c)
FIGURE 2. SEM micrographs of untreated cotton (a) and cotton
treated with 1 g/l (b) and 2 g/l Sintegal V7conc solution (c).
Ostazin and Remazol reactive dyes on cationized
fabrics are much higher than untreated cotton fabrics
in the presence or absence of salt. With untreated
samples the lowest intensity is obtained without salt.
Salt addition progressively increases reactive dye
color intensity, indicating the importance of using
salt in conventional dyeing of cotton with reactive
dyes. High quantities of salt are necessary to reduce
negative surface potential of cotton and to overcome
potential barrier which exists in absorption of dyes
from solution to the fiber surface. With cationized
samples, the lowest dye intensities were obtained in
the absence of salt and the highest ones with the
highest concentrations of cationized agent and salt.

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Volume 7, Issue 4 2012
Color intensities on cationized samples dyed in the 0,8

absence of salt are higher than to color intensities of 0 g/L NaCl

0,7
untreated samples dyed with the addition of 10 g/L 10 g/L NaCl
50 g/L NaCl
NaCl. Untreated samples dyed in the presence of 0,6

standard salt quantity (50 g/L) have higher color 0,5

intensities compared to cationized samples dyed in

K/S
0,4
the absence of salt and, therefore, increased
intensities of cationized samples dyed in the presence 0,3

of salt can be explained as a mutual contribution of 0,2

salt and cationic agent to reactive dye adsorption. On

0,1
cationized samples, apart from reaction of dye
reactive group and cotton functional hydroxyl group, 0
P0 P0,5 P1 P2
increased reactive dye adsorption takes place due to
ionic attraction of surfactant cationic groups and
FIGURE 6. C.I. Reactive Red 22 intensity on cationized cotton
reactive dye molecule anionic groups [20]. The fabrics in relation to salt concentration.
increased dye utilization with precationized samples
could be explained by detected zeta potential
reduction due to the presence of cationic surfactant 3

(Figure 1). 0 g/L NaCl

2,5
10 g/L NaCl
50 g/L NaCl

3,5 2

K/S
0 g/L NaCl
3 10 g/L NaCl 1,5
50 g/L NaCl

2,5
1

2
K/S

0,5

1,5

0
1 P0 P0,5 P1 P2

0,5
FIGURE 7. C.I. Reactive Blue 19 intensity on cationized cotton
0
fabrics in relation to salt concentration
P0 P0,5 P1 P2

In Tables II and III given are values of the increase in

FIGURE 4. C.I. Reactive Red 45:1 intensity on cationized cotton color intensity, I, fixation degree, F, color uniformity,
fabrics in relation to salt concentration. (), and wash fastness. From the results presented, a
rapid increase of color intensities on cationized fabric
1,4
0 g/L NaCl is obvious compared to untreated fabric. On the
1,2
10 g/L NaCl
50 g/L NaCl
fabrics dyed with Ostazin dyes, the highest intensity
increase was detected with dyeing without salt, while
1
in case of Remazol dyes; the highest color intensity
0,8
increase percentage was on the samples dyed in the
presence of minimum salt quantity.
K/S

0,6

0,4
Cationized fabrics contain positive groups which
increase reactive dye exhaustion due to ionic
0,2 attraction and this is most distinctive when the dye is
0
in dissociated form in the solution, i.e. with minimum
P0 P0,5 P1 P2 salt content. At higher salt concentrations the dye
dissociation is progressively suppressed and,
FIGURE 5. C. I. Reactive Blue 5 intensity on cationized cotton therefore, the ionic attraction is lower and the color
fabrics in relation to salt concentration. intensity increase is also reduced. Irrespective of
described effect, cationization efficiency for reactive
dye adsorption is complemented with salt action in
the way that dye chemical potential in the solution is
increased, i.e. the dye affinity for fiber is increased

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Volume 7, Issue 4 2012
shifting dye distribution equilibrium to the fiber side.
Moreover, dyeing characteristics of cationized fabrics
using reactive dyes in the presence of salt are the
result of both salt and cationic agent action,
simultaneously reducing cotton zeta potential and
increasing dye affinity for fiber.
Fixation degree, F, of reactive dyes applied on
cationic modified fabrics is 5-12% lower compared to
untreated samples. Lower percentage of fixed dye on
modified fabrics is the consequence of reactive dye
cationic agent complex formation [25] which, due to
steric hindrance, can block dye diffusion in the fiber
and prevent access of dye molecules to cotton
cellulose functional hydroxyl groups. It is possible to
remove (by washing in soap solution) the dye
remaining in the complex form on cotton surfaces,
giving lower fixation degree. Despite lower values of
fixation degree, F, the amount of fixed reactive dye
TABLE II. Color characteristics of cationized cotton fabrics dyed with Ostazin reactive dyes.
Journal of Engineered Fibers and Fabrics
Volume 7, Issue 4 2012
on cationized cotton fabrics is significantly higher
than on untreated fabrics because dye exhaustion is
higher on cationized fabrics.
Standard deviation values () in Tables II and III
clearly indicate that higher color uniformity is
obtained on cationized samples. The high level of
color uniformity can be attributed to new embedded
cationic groups in cotton outer layer, because non
polymer cationic agent can penetrate the cotton fiber
increasing the number of substantive groups toward
reactive dye ions and molecules, positively
influencing the color uniformity.
The level of dye fastness on samples, after one or
more washing cycles, has identical values which is
evidence of stable covalent bonds formed on
modified samples as well as in conventional dyeing.
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 TABLE III. Color characteristics of cationized cotton fabrics dyed with Remazol reactive dyes.
CONCLUSION
The main purpose of this work focuses on increasing
reactive dye utilization by cationizing cotton fabrics
using a commercial agent. By cationizing with
different concentrations of commercial agent Sintegal
V7conc, the extent of negative surface charge is
significantly reduced, which is explained as a more
positive zeta potential of fabrics. Nevertheless, all
cotton fabrics have negative charge in alkaline
conditions (pH 10) in reactive dye application.
Retained water quantity of precationized fabrics is
minimally reduced due to partially blocked hydroxyl
groups of fiber surface layer.
Dyeing of cationized fabrics using reactive dyes, in
the absence of salts, increases color intensities
progressively with the increase of cationic agent
concentration. Dye exhaustion is increased due to
ionic attraction of Sintegal V7conc cationic groups
and reactive dye anionic groups. Presence of salt in
the dye bath positively affects the exhaustion and
fixation of reactive dyes on all fabrics. With salt
addition, reactive dye affinity is increased and the
most intense dyeing is achieved. The achieved color
intensities on cationized samples, in the presence of
salt, are the result of mutual contribution of salt and
cationic agent activities on reactive dye absorption
and fixation. Fixation degree on modified fabrics is
Journal of Engineered Fibers and Fabrics
Volume 7, Issue 4 2012
slightly reduced due to formation of dye-surfactant
complex on fiber surface which, because of steric
hindrance, blocks dye diffusion into fiber. Compared
with original fabric, cationized samples have higher
color uniformity and standard fastness level,
indicating that surfactant cationic groups have an
importance for reactive dye absorption and that dye
fixation is realized by covalent bonding with cotton
hydroxyl groups, similar to standard dyeing.
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AUTHORS' ADDRESSES
Neboja Risti
Ivanka Risti
High Professional School of Textile
Vilema Pusmana 17
Leskovac, Jablanicki Okrug 16000
SERBIA AND MONTENEGRO
121 http://www.jeffjournal.org