Ultrasonics Sonochemistry 16 (2009) 243249

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Ultrasonics Sonochemistry
journal homepage: www.elsevier.com/locate/ultsonch

Ultrasonic dyeing of cationized cotton fabric with natural dye.

Part 1: Cationization of cotton using Solx E
M.M. Kamel *, M.M. El Zawahry, N.S.E. Ahmed, F. Abdelghaffar
National Research Centre, Textile Research Division, El-Behoos Street, Dokki, P.O. Box 12622 Cairo, Egypt

a r t i c l e

i n f o

Article history:
Received 25 March 2008
Received in revised form 22 July 2008
Accepted 7 August 2008
Available online 15 August 2008
Keywords:
Cationization
Cotton
Ultrasound
Sonochemistry
Cochineal dye
Dyeing

a b s t r a c t
The dyeing of cationized cotton fabric with Solx E using colouring matter extracted from Cochineal dye
has been studied using both conventional and ultrasonic techniques. Factors affecting dye extraction such
as ultrasound power, particle size, extraction temperature and time were studied. The results indicated
that the extraction by ultrasound at 300 W was more effective at lower temperature and time than conventional extraction. The effect of various factors of dye bath such as pH, salt concentration, ultrasound
power, dyeing time and temperature were investigated. The colour strength values obtained were found
to be higher with ultrasound than with conventional techniques. The results of fastness properties of the
dyed fabrics were fair to good. The scanning electron microscope (SEM) images of the morphological and
X-ray analyzes were measured for cationized cotton fabrics dyed with both conventional and ultrasound
methods, thus showing the sonicator efciency.
2008 Published by Elsevier B.V.

1. Introduction
The dyeing of cotton fabrics with anionic dyes such as direct
and reactive dyes requires the presence of large quantities of electrolyte to increase dye uptake, resulting in serious environmental
problems. As a result of this process, large volumes of wastewater,
containing signicant amounts of dyes and chemicals, are discharged from a typical cotton dye house [1]. One method of avoiding this problem is to cationize the cotton bre by cationic agents
that increase the colour strength of the dyeing process and improved wash fastness [2].
Natural dyes are generally environmentally friendly and have
many advantages over synthetic dyes [3]. In recent years, there
has been an interest in the application of these dyes due to their
bio-degradability and higher compatibility with the environment
[47]. Cochineal dye which is isolated from the dried bodies of
the female scale insects was the main red dye used in Central
America before the Spanish conquest. During the 16th century, it
was imported into Europe and began to replace the domestic kermes as an artists pigment and for dyeing [8]. These insects are still
collected in Peru and India to furnish the permanent brilliant carmine for the food, drink and cosmetic industries and artists colours [8,9]. The compound responsible for the purple colour of
this dye is carminic acid [1012].
The use of ultrasound energy for dyeing textiles as a cleaner
production is very well known in the literature [1315], Although,
* Corresponding author. Tel.: +20 2 33371718; fax: +20 2 33370931.
E-mail address: mona_kamel_nrc@yahoo.com (M.M. Kamel).
1350-4177/$ - see front matter 2008 Published by Elsevier B.V.
doi:10.1016/j.ultsonch.2008.08.001

it has not been applied in the area of dyeing with natural dyes as
much as it is being used for direct and reactive dyes. Ultrasound
can enhance a wide variety of chemical and physical processes,
mainly due to the cavitation effect in liquid mediums (that is the
growth and explosive collapse of microscopic bubbles, which
causes a large increase in the pressure and temperature) that enhances the rate of dyeing process.
The aim of this work was to focus on the use of ultrasound (US)
for enhancing the dyeing efciency and fastness properties of
cationized cotton fabrics with Solx E using Cochineal as a natural
dye. Although it was previously reported that the exhaustion
method was the applicable method for cationization of cotton fabrics with Solx E [16], our present study was the rst work to
investigate using the pad dry cure cationized method for cotton
fabrics. Different factors affecting dyeability and fastness properties were thoroughly investigated. Comparative results of the dyeing efciency of cationized cotton fabrics using both the US and
conventional (CH) dyeing methods are also presented. The microscopic images obtained by SEM and X-ray diffraction techniques
were also investigated to provide visual evidence of the existence
of ultrasonic effects.
2. Materials and methods
2.1. Dyes
The whole insect part of Cochineal was used and it was supplied
from local marketing in Egypt as a powder form, which was

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imported from India. The characteristics of this commercial material were as follows: the botanical name of the Cochineal dye is
Dactylopius coccus, the C.I. name is Natural Red 4, the class is
Anthraquinone, and kmax in water is 532 nm.
2.2. Fabrics
In this work scoured and bleached cotton fabric (142 g/m2) was
supplied from Miser Spinning and Weaving Company, Mahalla
El-Kobra., Egypt. Before being used, the fabric was treated with a
solution containing 5 g/L non-ionic detergent (Hostapal CV,
Clariant), at 95 C for 4 h. Then the fabric was thoroughly washed
with water and air dried at room temperature.

ratio 1:30 at different pH values (210), concentrations of glauber

salt (015 g/L), for different durations (15240 min) and temperatures (3080 C). For comparison, the same conditions of dyeing
were carried out using US at different sonic power (100500 W).
Finally, the dyed samples were rinsed with cold water and washed
in a bath containing 3 g/L non-ionic detergent (Hostapal CV, Clariant) at 90 C for 30 min using a liquor ratio 1:30. The fabrics were
then rinsed and air dried. The optimum condition was elevated for
dyed cationized cotton fabrics.
2.9. Measurements and analysis

2.3. Cationic agents

2.9.1. Determination of nitrogen percentage

Nitrogen was determined by the Cole and Parks modication of
the semi-micro Kjeldahl method [17].

Solx E was supplied by Ciba GeigyCo., Germany as an aqueous solution of approximately 40% solid content. It is a polyaminochlorohydrin quaternary ammonium polymer with epoxide
functionality that can react with cellulose via ether formation in
the presence of alkalis [16].

2.9.2. Fourier transform infrared spectroscopic analysis

Fourier transform infrared (FTIR) spectra were recorded on a
Nexus 670 FTIR Spectrometer, Nicolet Company, USA using potassium bromide disks. A total of 32 scans for each sample were taken
with a resolution of 4 cm1, with a range of 4000400 cm1.

2.4. Ultrasound equipment

2.9.3. Colour measurements of the dyed fabrics

The colour strength of the dyed samples was evaluated by a
light reectance technique using the PerkinElmer, UVVis Spectrophotometer (Model, Lambda 3B). The relative colour strength
(K/S values) was assessed using the KubelkaMunk equation [18]

A CREST Ultrasonic, TRU-SWEEPTM ultrasonic bench top cleaner

bath, model 575 D with a capacity 5.75 L, was used. The experimental setup used was composed of an electrical generator at a
frequency of 38.5 kHz and power ranging from 135 W average/
500 W. The output power levels are from 50 up to 500 W, and
are supplied by three transducers at the bottom of the industrial
grade tank. Precise digital control of time (090 min), thermostatically controlled heater (ambient to 80 C), power level and degas
functions. The internal dimensions of the tank were 11.5  6  6
depth and 292  152  152 mm.
2.5. Conventional extraction
Conventional extraction was carried out in 100 mL water using
a varying amount of the dye materials (0.11.0 g) for different
times (15120 min) and at different temperature (50 80 C).
2.6. Ultrasound extraction
Ultrasound extraction was carried out as above in 100 mL distilled water using varying amounts of the dye materials (0.1
1.0 g) at different temperatures (5080 C) using different sonic
power (100500 W) for different time intervals (15120 min).
2.7. Cationization of cotton with the pad dry cure method
Cotton fabrics were padded at 100% wet pick up through a solution of NaOH (15 g/L) and different concentration of Solx E (0
150 g/L). To minimize reactant hydrolysis, the alkali was added
to the padding bath just prior to application. The padded samples
were then dried at 80 C for 3 min and cured at 115 C for 4 min.
Then samples were rinsed several time with water and nally neutralized with a dilute acetic acid solution (12 g/L), the fabric was
thoroughly rinsed with water, followed by soaping with 3 g/L of
non-ionic detergent at a boil for 30 min, then rinsed with water
and air dried.
2.8. Dyeing procedure
Cationized cotton fabric was dyed with natural colouring matter extracted from Cochineal insects (0.5 g/100 mL water) for
60 min using US at 80 C. The fabrics were CH dyed with a liquor

K=S

1  R2
2R

2.9.4. Scanning electron microscope

The untreated and ultrasonic treated dyed cotton fabric were
examined using a SEM Model Philips XL 30 with an EDX Unit attached, with accelerating voltage of 30 kV and magnication between 10 and 400.000. All the samples were coated with gold
before SEM testing.
2.9.5. X-ray diffraction
An X-ray diffraction analysis was performed at room temperature for the cationized cotton fabric dyed with both CH and US
method, on an X-ray diffractometer model Philips X Pert MPP with
a type PW 3050/10 goniometer. The diffractometer controlled and
operated by a PC computer with the programs P Rot and used a
Mo Ka source with wavelength 0.70930 , operating with Motube
radiation at 50 kV and 40 mA. The scan parameters range from
2 < 2h < 50 with scanning step of 0.03 in the reection geometry.
2.9.6. Particle size measurement
The mean diameters of the partially soluble Cochineal dye were
measured by particle size analyzer (Fritsch Analystte 22, Laser analyzer). All the samples were measured in the Research and Development Institute, Technical services Department.

Table 1
Effect of different concentrations of Solx E
Concentration. of Solx E (g/L)

0
25
50
75
100
125
150

Nitrogen content (%)

0.00
0.169
0.337
0.680
0.712
0.740
0.760

K/S
CH

US

0.0998
5.37
6.18
6.39
6.50
6.61
6.61

0.325
5.72
6.62
6.84
6.90
6.98
7.02

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2.9.7. Fastness properties

The dyed samples were tested according to ISO standard methods. The specic tests were ISO 105-X12 (1987), colour fastness to
rubbing; ISO 105-C02 (1989), colour fastness to washing and ISO
105-E04 (1989), colour fastness to perspiration.

3. Results and discussion

3.1. Effect of different concentrations of Solx E

Table 2
Effect of ultrasound dye extraction power level on the colour strength
Power level (W)

Particle size (lm)a

Standard deviationa

100
200
300
400
500

1.5025
1.2375
1.190
1.1475
1.2103
1.229

0.31
0.35
0.37
0.33
0.31
0.32

K/S
CH

US

4.42
6.18
6.50
6.73
6.61
6.39

5.37
6.73
7.23
7.50
7.10
6.81

The average particle size of two determinations and standard deviations.

The results in Table 1 reveal that as the concentration of Solx E

increased from 0 to 150 g/L, the nitrogen percent (N%) of the
cationized cotton fabric was also increased from 0% to 0.760%
and due to this increase the colour strength also increased. It
was observed that the maximum dye uptake with pronounced increase in K/S values was obtained at 75 g/L and above this the N%
levels off. The results also show that the colour strength values
of US dyeing methods are generally higher than those of CH dyeing
methods. This enhancement effect of US power may be due to cavitation effect [14]; this point will be discussed in detail later.

sity within 3346 and 1033 cm1 with increasing nitrogen content
of the cationized fabric.
These distinct narrow, high intensity bands (OH/N+ R3) conrm
presence of the quaternary ammonium salts. In addition, a two
splitting distinct bands can be observed in the spectrum (B) with
in 2922 and 2853 cm1, 1430 and 1373 cm1 corresponding to aliphatic CH stretching, bending deformations and rocking vibrations of the methylene groups (CH2).

3.2. FTIR analysis

3.3. Factors affecting dye extraction

FTIR spectra were obtained for the untreated (A) and treated (B)
cotton fabric with cationizing agent Solx E (nitrogen content of 0%
and 0.68%, respectively), as shown in Fig. 1. In the treated fabric
certain absorption bands can be observed in the 1116 cm1 range
(CN stretching vibration) as well as an intensive distinct band at
1059 cm1 which are characteristic of primary-COH stretching
deformation, which are not present in the untreated fabric in spectrum (A). The spectrum of the cationized cotton fabrics with Solx
E is markedly different from the uncationized fabric.
In addition, the broad absorption band within 3352 and
1032.71 cm1 for the unmodied cotton fabric revealed the presence of numerous hydroxyl groups. However, the (primary-OH)
band of the cationized cotton become narrow with a higher inten-

3.3.1. Effect of ultrasound power

The effect of US on the extractability of Cochineal dye was conducted at different power levels (100500 W). As shown in Table 2,
the results indicate that as the US power increased from 0 to
300 W, the average particle size of the Cochineal dye decreased
and due to that the concentration of the extracted colouring matter
would also increase in the dye bath and the colour strength was
also increased. However, at a higher power level (400500 W),
the average particle size increased slightly and due to that the concentration of the extracted colouring matter decreased and the colour strength of the dyed sample was also decreased. This may be
attributed to a power level (400500 W) that was too high and
would cause an increase in the bubble numbers in the dye solution

Fig. 1. FTIR spectra of (A) untreated cotton fabric and (B) treated cotton fabric.

M.M. Kamel et al. / Ultrasonics Sonochemistry 16 (2009) 243249

during the cavitation phenomenon which might reduce the efciency of the ultrasound energy transmitted into the medium
[19,20]. These results emphasize the enhancement effect of US,
which increases the rate of dye extraction from Cochineal insects
by virtue of its dispersion, degassing and diffusion capabilities
(accelerating the rate of dye desorption from the insect body). On
the other hand, it can be observed from Table 2 that US in comparison with CH extractability will enhance the dyeability as the colour strength values associated with pronounced increase using US
than CH dyeing method and this point will be discussed in detail
later.
Consequently, a power level of 300 W was chosen as an optimum power level for the dye extraction method. Some dyes extracted via US are more susceptible than others to the effect of
US with different power levels. This observation means that, for
each dye there is an optimum US power level [21].

8
7

K/S

246

CH

US

4
3
0.1

0.2

0.3

0.5

0.7

Dye amount ( w/v %)

Fig. 3. Effect of dye extraction amount on the colour strength (extraction
conditions: 300 W, at 80 C for 60 min, dyeing conditions: L.R. 1: 30, pH 4, 500 W,
at 80 C for 60 min).

7.8

3.3.3. Effect of dye amount

The extraction of Cochineal dye at different dye amounts (0.1
1.0 g/100 mL) performed using US (300 W) at 80 C for 60 min.
Fig. 3 shows that as the dye amount increased, more dye extract
also increased up to 0.5 g/100 mL water which was associated with
a higher colour strength values increment. The K/S value then levels off above this concentration when using either the US or CH
dyeing method, and shows much higher values at all points in US
extracted and dyeing methods as expected.
3.3.4. Effect of extraction time
The effect of the extraction time using US extraction of Cochineal dye was carried out for different times (15120 min). Fig. 4
shows that the K/S value increases with increased extraction time

7.4
7

K/S

3.3.2. Effect of extraction temperature

Previous studies have shown that the CH extraction of natural
dyes into an aqueous solution is temperature dependant and increases as the temperature approached the boiling point of the
solution. To fully investigate the effect of the US efciency of the
dye extraction, the temperature of the extraction mixture was reduced below its boiling point.
As shown in Fig. 2, it is clear that the concentration of colouring
matter increased when the extraction temperature was increased
up to 80 C while using US extraction method. This also produced
a pronounced increase in the colour strength of the US than the
CH dyeing method. The results emphasize the enhancement effect
of power US on reducing the dye extracted temperature of Cochineal dye.

6.6
6.2
5.8

CH

5.4

US

5
15

30

45

60

90

120

Extraction time (min)

Fig. 4. Effect of dye extraction time on the colour strength (extraction conditions:
concentration of dye 0.5 g/100 mL, 300 W, at 80 C, dyeing conditions: L.R. 1: 30, pH
4, 500 W, at 80 C for 60 min).

for both the US and CH dyed methods, with a pronounced increase

in the US case than the CH case.
The results in Fig. 4 clearly indicate that the K/S values of the
dyed cationized cotton fabric using US increased rapidly in the rst
60 min. It is worth mentioning that, as the time of dye extraction
increased; more dye was extracted, which leads to higher K/S values of dyed cationized cotton fabric. After 90120 min the K/S values began to decrease, which may be due to degradation of the dye
molecule. On the other hand, the K/S values of dyed cationized cotton using the CH method increased continuously as the extraction
time increased (15120 min). When the time of extraction reaches
120 min, the K/S values of cationized cotton are still lower than the
US dyeing method at 60 min. These results illustrate the benet of
using US waves in dye extraction due to dispersion, degassing and
diffusion (accelerating the rate of dye extraction from the insect
body).

7.6
7.4

CH

7.2

US

3.4. Factors affecting dyeing properties

K/S

6.8
6.6
6.4
6.2
6
5.8
5.6
50

60

70

80

Temperature (C)
Fig. 2. Effect of dye extraction temperature on the colour strength (extraction
conditions: concentration of dye 0.5 g/100 mL, 300 W, for 60 min, dyeing conditions: L.R. 1: 30, pH 4, 500 W, at 80 C for 60 min).

3.4.1. Effect of dye bath pH

Fig. 5 shows the effect of the pH values of the dye bath on both
the CH and US dyeing process for cationized cotton fabrics. It is
obvious that, as the pH values of the dye bath increased from 2
to 4, the colour strength values also increased in both cases, with
a slightly improvement in the dyeability in case of the US dyeing
process. As the pH increased >4, the K/S values of cationized cotton
decreased markedly. The effect of the dye bath pH can be attributed to the correlation between the dye structure and cationized
cotton bres. Since the Cochineal dye used acts as an acid dye, it
would interact ionically with the protonated terminal amino
groups of the cationized cotton bres under acidic medium (pH
4) via electrostatic dye attraction. In addition, additional interactions take place together with ionic forces. This ionic attraction

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M.M. Kamel et al. / Ultrasonics Sonochemistry 16 (2009) 243249

methods. It is clearly indicated that, in the absence of salt, the colour strength in case of the US dyeing method was higher than the
CH dyeing method. Moreover, as the salt concentration increased
from (015 g/L) the colour strength also decreased in both dyeing
methods, which is good for the environment.

K/S

6
5

CH
US

4
3

5
pH value

10

Fig. 5. Effect of dye bath pH on the colour strength of dyed cationized cotton fabrics
(extraction conditions: concentration of dye 0.5 g/100 mL, 300 W, at 80 C for
60 min, dyeing conditions: L.R. 1: 30, 500 W, at 80 C for 60 min).

would increase the dyeability of the bre, as is clearly shown in

Fig. 5. However, at a pH above 4, the ionic interaction between
the dye and cationized cotton fabric decreased due to the decreasing number of protonated terminal amino groups of the cationized
cotton fabrics, thus lowering its dyeability [14].
3.4.2. Effect of ultrasound power
The effect of ultrasonic power on the dyeability of cationized
cotton fabrics with Cochineal dye was conducted at different
power levels (100500 W). As shown in Fig. 6, the colour strength
of dyed fabrics seemed to be directly increased proportional
with the power supplied till 300 W, then a leveling off occurs.
Increasing the US power above 300 W does not have an additional
effect on the dyeability of the cationized cotton fabrics.
The improvement of the US dyeing process up to 300 W may be
due to the acoustic cavitation phenomenon, which would lead to
[13,22]: dispersion (breaking up of micelles and high molecular
weight aggregates into uniform dispersions in the dye bath),
degassing (expulsion of dissolved or entrapped gas or air molecules
from bre into liquid and removal by cavitation, thus facilitating
dye-bre contact), and diffusion (accelerating the rate of dye diffusion inside the bre by piercing the insulating layer covering the
bre and accelerating the interaction or chemical reaction between
the dye and cationized bre). Above 300 W an increase in the bubble numbers in the dye bath during the cavitation phenomenon occurs which may reduce the efciency of the US energy transmitted
into the medium [19,20].

3.4.4. Effect of dyeing temperature

The effect of temperature on the dyeability of the cationized
cotton fabrics dyed with Cochineal dye was conducted under US
and CH conditions at different temperatures (3080 C). As shown
in Fig. 8, it is clear that the colour strength (K/S) values increase
with increase in the dyeing temperature in both the US and CH
methods with a more pronounced increase in the US case than
the CH method.
Generally, in case of the US dyeing method, the K/S values increase as the temperature increased from 30 to 80 C. This result
may be due to the bre swelling effects that enhance the dye
diffusion. Also, the US power provides other additional factor of
de-aggregation of the dye molecules. This leads to a faster motion
and stirring effect in the US dyeing method, thus leading to a further enhancement of dye diffusion and better dyeability as compared to the CH dyeing method.
3.4.5. Effect of dyeing time
The effect of dyeing time was studied under US and CH conditions for different dyeing time (15240 min) to reveal the effect
of power ultrasonic on the dyeability of the cationized cotton fabrics dyed with Cochineal dye. As shown in Fig. 9, the colour
strength obtained was increased as the time increased for both
US and CH methods, with a much higher colour strength value at
all points in the US case. In both dyeing methods a plateau is attained after 60 min and then no change in K/S values was observed
beyond 90 min.

K/S

CH

3.4.3. Effect of salt addition

Fig. 7 shows the effect of the added salt concentration on the
colour strength of the dyed fabrics using both the CH and US

US

4
0

2.5

7.5

10

15

Salt conc. (g/L)

7.6

Fig. 7. Effect of salt addition on the colour strength of dyed cationized cotton
fabrics (extraction conditions: concentration of dye 0.5 g/100 mL, 300 W, at 80 C
for 60 min, dyeing conditions: L.R. 1: 30, pH 4, 300 W, at 80 C for 60 min).

7.4

6.8

K/S

K/S

7.2

6.6
6.4

CH
US

6
5
4
3

6.2
0

100

200

300

400

500

Power level (W)

Fig. 6. Effect of US power on the colour strength of cationized cotton fabric
(extraction conditions: concentration of dye 0.5 g/100 mL, 300 W, at 80 C for
60 min, dyeing conditions: L.R. 1: 30, pH 4, at 80 C for 60 min).

30

40

50

60

70

80

Temperature (C)
Fig. 8. Effect of dyeing temperature on the colour strength of dyed cationized
cotton fabrics (extraction conditions: concentration of dye 0.5 g/100 mL, 300 W, at
80 C for 60 min, dyeing conditions: L.R. 1: 30, pH 4, 300 W, no salt, for 60 min).

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M.M. Kamel et al. / Ultrasonics Sonochemistry 16 (2009) 243249

increasing more possibility for the penetration of the dye molecules into the bres. On the other hand, the US dyeing method is
associated with cavitation effects, which would lead to [11,21]:
dispersion, degassing and diffusion (accelerating the rate of dye
diffusion inside the bre by piercing the insulating layer covering
the bre and accelerating the chemical reaction between dye and
bre).

8
7.5

K/S

7
6.5

CH

US

5.5
5

15

30

45

60
90
120
Dyeing time (min)

180

240

Fig. 9. Effect of dyeing time on the colour strength of dyed cationized cotton fabrics
(extraction conditions: concentration of dye 0.5 g/100 mL, 300 W, at 80 C for
60 min, dyeing conditions: L.R. 1: 30, pH 4, 300 W, no salt, at 80 C).

3.4.6. Morphological study

The SEM technique was used to investigate the change in the
surface morphology of the dyed cationized cotton fabric with both
the CH and US dyeing methods. The results obtained are shown in
Fig. 10. It is obvious that the bres dyed with the CH method (a) are
smooth and distinct. In contrast, the bres dyed with US method
(b) are no longer smooth and become rough. These results may
be due to the creation of voids in the bre structure, lead to a physical loosening of the microstructure of the dyed bre with an

3.4.7. X-ray analyses

The X-ray diffraction patterns for the cationized cotton fabric
with Solx E dyed with both the CH and US method are shown
in Fig. 11. The CH dyed method (1) showed one major sharp peak
at 2h 10.50 with a higher intensity that represent the crystallinity together with other small broad peaks at 2h 15.60 and a

Table 3
Effect of CH and US dyeing method on crystallinity, crystallite size, 2h angle and dspacing of cationized cotton fabric
Dyeing
method

Crystallinity
(%)

2h ()

d-Spacing
()

Crystallite size
()

CH

51.35

3.87467

38.44

US

44.00

6.83, 7.59, 10.50,

15.60
6.69, 7.58, 10.43,
15.39

3.90248

20.76

Fig. 10. SEM photographs of cationized cotton fabrics (a) dyed with CH method and (b) dyed with US method.

Fig. 11. X-ray diffraction patterns of cationized cotton fabric dyeing with (1) CH dyeing method and (2) US dyeing method.

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M.M. Kamel et al. / Ultrasonics Sonochemistry 16 (2009) 243249

Table 4
Fastness properties of dyed cationized cotton fabrics using CH and US dyeing methods
Dyeing methods

Washing

Perspiration

Rubbing fastness

Acid

CH
US

Light

Alkali

Alt.

Alt.

Alt.

Dry

Wet

4
34

4
45

4
45

4
34

34
4

34
34

45
4

3
3

4
34

34
34

12
23

2
2

Alt. = alteration (change in colour), C = staining on cotton, W = staining on wool.

broad peak at 2h 6.83, 7.60 with a lower intensity. The US dyed

method (2) is characterized by four peaks, one broad peak with less
intensive percent at 2h 6.69, 7.58 which is mainly amorphous,
and a high intensive sharp peak at 2h 10.43 as well as another
small peak at 2h 15.39. The crystallinity percentage was calculated by evaluation of the area of the sharp and broad peaks in
Fig. 11 and estimated according to the following equation [23]:

IC
Cx%
 100
I C Ia
where Cx% is the crystallinity percentage and Ic and Ia are the intensities of the X-ray diffraction pattern of the crystalline and amorphous components, respectively. It is clear from Table 3 that the
US dyeing method decreased the crystallinity as well as the crystallite size than the CH dyeing method, which indicates that the amorphous region increases. An increase in the d-spacing values of the
US dyeing method as compared to CH dyeing method occurred in
the indicated region. It can be concluded that the dye uptake increased via dyeing with the US method [24].
4. Fastness properties
The fastness tests involving washing, rubbing, perspiration
(acidalkali) and light of dyed cationized cotton fabric using the
US and CH methods are shown in Table 4. The results indicate fair
to good fastness properties of the dyed samples using both the US
and CH methods. Generally in the case of washing and perspiration
fastness properties did not alter where a decrease in rubbing fastness was observed in both CH and US methods.
5. Conclusions
Ultrasound appears to be an effective technique for the extraction of Cochineal dye and gave maximum extraction value at
300 W which was associated with decreasing the average particle
size. Better K/S values were observed for dyed cationized cotton
fabrics using ultrasound compared to the results obtained via the
conventional method. The results of X-ray diffraction studies and
SEM images provided visual evidence that the ultrasound technique is useful in enhancing the dyeability as measured by K/S values, than the conventional dyeing method. Comparing the fastness

properties for the ultrasound and conventional method, the results

indicate fair to good fastness properties of the dyed samples using
both techniques.

Appendix
Ultrasound US
Conventional CH
Fourier transform infrared FTIR
Nitrogen content percent N%

References
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