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Journal of Natural Fibers, 8:289–307, 2011
Copyright © Taylor & Francis Group, LLC
ISSN: 1544-0478 print/1544-046X online
DOI: 10.1080/15440478.2011.627114
INTRODUCTION
Wool fibers consist of keratin proteins that are made of 18 amino acids, and
these amino acids bring both free amino and carboxylic acid groups into
289
290 M. M. Kamel et al.
wool proteins. The free amino groups existing in the proteins have been
employed as main sites for interactions in acid dyeing of wool fibers, since
the amino groups could form cationic amine salts under acidic conditions
(Zhu and Sun 2004).
Natural dyes are generally environmentally friendly and have many
advantages over synthetic dyes (Deo and Paul 2003). In recent years, there
has been an interest manifested towards the application of these dyes due
to their bio-degradability and higher compatibility with the environment, as
such, the demand for natural dyes is increasing day by day (Teli et al. 2000;
El-Zawahry and Kamel 2001; Paul et al. 2005; Kamel et al. 2009). Although
vegetable dyes cannot replace synthetic dyes, they have several advantages
over synthetic dyes with regard to health, safety, and ecology.
Nowadays, the use of natural mordant dyes is mostly confined to
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MADDER ROOT
Fabrics
Scoured and bleached wool fabrics (plain weave, 300 g/m2 ) were sup-
plied by Misr Co. for spinning and weaving (Mehalla El- Kubra). The fabric
samples were scoured before use as discussed below.
FIGURE 1 The structure and photo of Terminalia arjuna fruits used in this study (color
figure available online).
292 M. M. Kamel et al.
FIGURE 2 The structure and photo of Madder dyes used in this study (color figure available
online).
Mordants
The mordants used for dyeing were potassium aluminum sulfate, potassium
dichromate, chromic chloride, copper sulfate, copper acetate, stannous
chloride, ferrous sulfate, and ferric chloride, which were of pure laboratory
grades.
Methods
SCOURING OF WOOL
The fabric was washed for 30 min in a bath containing 0.5 g/L sodium
carbonate and 2 g/L of a non-ionic detergent (Hostapal C.V., Hoechest) at
40–45◦ C, to remove any impurities. The fabric was then thoroughly washed
with water and air-dried at ambient temperature. The scoured fabric was
soaked in tap water for 5 min prior to dyeing or mordanting.
To extract the coloring matter, 5 g/L of a mixture of T.a. fruits and Madder
dyes (M) (wt/wt) were mixed well in different percentages (80:20%, 70:30%,
50:50%) and then boiled in 100 mL water for 60 min. The extract solution
was filtered before using as a dyebath.
Eco-friendly Dyeing of Wool 293
MORDANTING METHOD
Different common mordant salts are used with the permitted concentrations
that are given in the literature (Corbman 1985; Cannon and Cannon 1994) for
environmentally friendly textiles [1.6 g/L for aluminum salts + 2mL formic
acid, 0.6 g/L for chrome salts + lactic acid, 0.4 g/L for copper salts + glacial
acetic acid, 0.8 g/L for tin salts and 1 g/L for iron salts]. The three mordanting
methods that were carried out are as follows:
Pre- mordanting (I): The mordant was dissolved and added to a bath
of water with L.R. 1:50. The pH of the bath was adjusted to 4 with acetic
acid. The soaked wool fabrics were entered into the mordant solution and
the whole bath was brought slowly to boil for 1 h. It was then allowed
to cool at room temperature and the fabrics were removed and squeezed.
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Mordant fabrics should be used at once because some mordant are very
sensitive to light.
Simultaneous mordanting and dyeing (II): The mordant was first dis-
solved and then added to a bath containing the extracted dye, and then
pH of the bath was adjusted to 4 with acetic acid. The soaked fabrics were
then added and the whole bath was brought slowly to nearly boil for 1 h.
The fabrics were then rinsed under tap water and washed as usual.
Post-mordanting (III): First, the soaked fabric was added to a bath
containing the extracted dye in which the pH was adjusted to 4 with
acetic acid at boil for 50 min. Secondly, the dyed fabric was lifted out
while the dissolved mordant salts were added to the bath for the final
10 min of the dyeing process. Finally, the dyed fabric was rinsed and
washed with tap water.
MORDANT COMBINATIONS
The following seven mordant combinations were used for wool dyeing:
CONCENTRATION OF MORDANTS
amount of the two mordants in each combination was used in the following
concentration:
Each of the seven mordant combinations mentioned above were used with
all the three mordanting methods namely pre-mordanting (I), simultaneous
mordanting (II), and post-mordanting for dyeing (III).
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Dyeing
DYEING OF WOOL
Wool fabric (0.5 g) was dyed with a mixture of natural coloring matter
extracted from T.a. fruits and Madder root in three different percentages
as mentioned above using L.R. 1:50. This study was employed at different
pHs, concentrations of glauber salt, dyeing durations, and temperatures as
shown later. The fabrics were added to the dyeing bath at 40◦ C; then the
temperature was raised to 60◦ C during 10 min; after that, the temperature
was raised to 100◦ C during 30 min.
The fabrics were then dyed for 1 h at the boil, then rinsed with cold
water, and washed for 30 min in a bath containing 2 g/L of a non-ionic
detergent at 50–60◦ C at L.R. 1:50. Finally, the fabrics were then rinsed and
air dried.
Fastness Properties
The dyed samples were tested according to ISO standard methods. The
specific tests were ISO 105-X12 (1987), color fastness to rubbing; ISO 105-
C02 (1989), color fastness to washing; and ISO 105-E04 (1989), color fastness
to perspiration.
As shown in Figure 3, it is clear that the mustard brown shade of T.a. 100%
is significantly shifted to a more reddish brown color as the percentage of
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Madder in natural dye mixture increased from 20% to 50% and due to that
the K/S value also increased. This bathochromic shift (red shift) of the T.a.
dye solution in the mixture of T.a. and Madder with different percentage
from λmax 355 nm to 395 nm visible absorption band may be attributed
mainly to alizarin present in Madder, which contains eight conjugated π -
electron pairs that shift the mustard brown color to reddish brown color
as the concentration of Madder in the dye mixture increased and the K/S
values increased accordingly.
The effect of extraction time on the extractability of the mixture of T.a. fruits
and Madder (5 g mixture wt/wt/100 mL water) with different percentages
12
10
6
K/S
4
0
355 370 380 395 410
T.a. :Madder
T.a. :Madder
T.a. :Madder
100% T.a.
80:20%
70:30%
50:50%
Madder
100%
Wavelength (nm)
FIGURE 3 Effect of different percent of natural dye (color figure available online).
296 M. M. Kamel et al.
7.5
7
6.5
6
5.5
K/S 5
4.5
4
80:20 % T.a.:M
3.5
70:30 % T.a.:M
3 50:50 % T.a.:M
2.5
10 20 30 60 90 120
Extraction time (min)
T.a.: Terminalia arjuna, M: Madder
[80:20, 70:30, and 50:50] was noted at different time intervals (10–120 min).
Dyeing was carried out using 10 g/L glauber salt, pH 4, and L.R. 1:50 for
60 min at the boil. The dyed samples were rinsed and washed for 30 min in
a bath containing 3 g/L of a non-ionic detergent at 90◦ C.
As shown in Figure 4, it is clearly indicated that the color strength
maximum value is at 60 min extraction time. A further increase in time results
in decrease in color strength. This may be attributed to the decomposition
of coloring component at longer times at high temperature (100◦ C).
The dyeing of wool fabric was carried out using the optimum value of
extractability (10 g mixture/100 mL water) with different percentages of T.a.
fruits and Madder for 60 min at the boil.
Eco-friendly Dyeing of Wool 297
9
8
7
6
K/S
5
80:20 % T.a.:M
4
70:30 % T.a.:M
3 50:50 % T.a.:M
2
1.5 2.5 5 10 15 20 25
Dye amount (g/100ml)
T.a.: Terminalia arjuna, M: Madder
8.5
8
7.5
7 80:20 % T.a.:M
6.5 70:30 % T.a.:M
K/S 50:50 % T.a.:M
6
5.5
5
4.5
4
4 4.5 5 5.5 6 6.5 7
pH
T.a.: Terminalia arjuna, M: Madder
Figure 6 shows the effect of the pH values (4–7) of the dyebath on the
color strength obtained by different dye mixture extract. As can be observed,
the highest color strength is obtained at pH 4. The effect of dyebath’s pH
can be attributed to the correlation between the dye structure and wool.
Since the mixtures of the two natural dyes used act as an acid dye, it would
interact ionically with the protonated terminal amino groups of the wool
fabrics at acidic medium (pH 4) via electrostatic dye attraction. In addi-
tion, additional interactions take place together with ionic forces. However,
above pH 4 this ionic interaction decreased due to the decreasing number
of protonated terminal amino groups of wool fabrics and thus lowering its
dyeability.
298 M. M. Kamel et al.
10
7
K/S
6
5
80:20 % T.a.:M
4 70:30 % T.a.:M
50:50 % T.a.:M
3
0 0.25 0.5 1 1.5 2 3 4
Concentration of salt (g/100ml)
T.a.: Terminalia arjuna, M: Madder
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The effect of temperature on the dyeability of the wool fabrics with mixture
of T.a. fruits and Madder with different percentages was conducted at differ-
ent temperatures (60–100◦ C). As shown in Figure 8, it is clear that the color
strength (K/S) values increases with increasing the dyeing temperature and
reaches a maximum value at 100◦ C. Generally, the increase in dye uptake at
100◦ C can be explained by fiber swelling which enhanced the dye diffusion.
9.5
8.5
7.5
6.5
K/S
5.5
10
7
K/S
6
5 80:20 % T.a.:M
70:30 % T.a.:M
4 50:50 % T.a.:M
3
15 30 40 50 60 90
Dyeing time (min)
T.a.: Terminalia arjuna, M: Madder
EFFECT OF MORDANTS
The wool fabrics dyed with mixture of T.a. fruits and Madder (80:20%) at the
optimum value obtained as described earlier were mordanted with different
mordants using three method: pre-mordanting (I), simultaneous mordanting
and dyeing, (II) and post-mordanting (III). The different common mordant
salts are used with the permitted concentration as given in the literature for
environmentally friendly textiles.
Almost impairing a percentage of Madder root in T.a. fruit dyeing
bath with 20% increased the complexing of the ionized O–dihydroxy groups
with metal salts (mordant) additionally to O–dihydroxy groups of T.a. fruits
300 M. M. Kamel et al.
TABLE 1 Effect of Different Types of Mordants on the Color Strength (K/S) of Wool Fabric
Dyed with Natural Coloring Matter Extracted from Mixture of T.a. Fruits and Madder Dyes
(80:20%)
Concentration Mordanting method (K/S)
of mordant
Mordant g/L I II III
with metal salts. These mordants are mainly responsible for fixation of the
dye on the fabrics and improved wash and light fastness. Besides, a wide
range of color can be obtained by using different mordants thus leading to
change in color strength.
Table 1 shows that potassium aluminum sulfate salt produces the
lower K/S values using the three mordanting methods. This result may
be attributed to aluminum salt forming weak coordination complexes with
the dye, tending to form quite strong bonds with the dye but not with the
fiber. Thus they block the dye and reduce its interaction with the fiber. This
is in accordance with the observed low K/S values in presence of aluminum.
The results from Table 1 also indicate that the higher value of color strength
in case of aluminum salt was obtained using pre-mordant (I) method.
On the other hand, copper and iron exhibited the highest K/S values
due to their ability to form coordination complexes with the dye molecules.
Since, the coordination numbers of copper and iron are 4 and 6 respectively,
some coordination sites remained unoccupied when they interacted with the
fiber. Due to that, active sites of wool fabric (–COOH and –CONH2 ) will
occupy these sites (Bhattacharya and Shah 2000). This strong coordination
tendency leads to enhancing the interaction between the fiber and the dye,
resulting in higher dye uptake. It was also observed that copper and iron
changed shades of dyed fabrics producing deep colors, while all other metals
show similar coordination.
The wool fabrics dyed with mixture of T.a. fruits and Madder (80:20%) were
mordanted using combination of mordants. In order to determine the effects
of the combinations to produce different shades on wool and also the effects
Eco-friendly Dyeing of Wool 301
TABLE 2 Effect of Combination of Mordants on the Color Strength (K/S) of Wool Fabrics
Dyed with Natural Coloring Matter Extracted from Mixture of T.a. Fruits and Madder Dyes
(80:20%)
Mordanting method
Concentration (K/S)
of mordant
Mordant g/L I II III
of all the metal salts on dyeing activity to improve the fastness properties,
the assay mixture was performed by mixture of metal ions each at the ratio
of 1:1 using the three mordant methods as given in Table 2.
On the other hand, the addition of stannous chloride to copper, iron,
and potassium dichromate salts increased the activity of stannous chloride,
the majority of the samples was revealed by having the color strength of
the combination, which was approximately the same as that obtained with
metals, but with alum the stannous chloride enhanced the color value of
alum in the case of pre-mordant (I) method from 4.93 to 6.61 and in the
case of simultaneous (II) method and post-mordant (III) method the results
were the same.
The same holds true for the addition of potassium dichromate to copper,
iron and alum metal salt. However, it could be seen that the combination
of mordants decreases the amount of mordant salts than that applied sep-
arately. In this process, it may decrease the concentration of mordant
salts used in dyeing with less environmentally challenging combination of
mordant salts to improve the fastness properties.
Dyebath Reuse
A trial was undertaken to take benefit of the residual dyeing bath to produce
a full range of different color strength when a mixture of T.a. fruits and
Madder (80:20%) (10 g/100 mL water) was boiled for 60 min.
Three successive dyeing times are used for untreated and mordant wool
fabric. It is very interesting to obtain different hues using successive dyeing
regardless of color strength; the results are tabulated in Table 3. Generally,
it seems that, from both economic and environmental points of view, reuse
of the dyebath is of great importance.
302 M. M. Kamel et al.
K/S
Concentration
of mordant Mordanting First Second Third
Mordant g/L methods reuse reuse reuse
Fastness Properties
For better fastness to light and washing, the use of mordants may be essential
for most of natural dyes. The function of the mordant is to assist the adsorp-
tion of the dye and promote good bonding of dye and fiber as a bridge,
which helps to bond fiber and natural dyes at the molecular level. From
Tables 4 and 5, it can be inferred that the dyed samples that were treated
with mordants and combination of mordants had better fastness properties
(washing and light) than the dyed samples without mordants.
In general, it can be seen that wool fabrics dyed with mixture of T.a.
fruits and Madder (80:20%) exhibit good fastness properties. Comparing the
fastness ratings of the samples as given in Tables 4 and 5, fastness values
were improved with mordanting combination method.
CONCLUSIONS
TABLE 4 Color Fastness of Standing Dyebath of Wool and Mordant Wool Dyed with a Mixture of T.a. and M. (80:20%)
Rubbing
Number Wash fastness Alkali perspiration Acid perspiration fastness Light fastness
of reuse
∗ ∗∗ ∗ ∗∗ ∗ ∗∗
Mordant dyebath St.. St.. Alt St.. St.. Alt St.. St.. Alt Dry Wet 35 h 50 h 65 h
Control (100% T.a.) 1 3 3 3–4 3–4 3–4 4 4 4–5 4 4 3–4 4–5 5 5
2 3 2–3 3–4 3–4 2–3 3–4 4 4 4 3–4 3 5 4–5 3–4
3 2–3 2–3 4 3–4 2–3 4 4 3–4 4 3 3 4–5 4 3–4
Blank (80:20% T.a.:M) 1 3 3 3–4 2–3 2 3 3–4 3 3–4 3 2–3 3–4 4 3
2 3 2–3 3–4 2–3 2 3–4 4 3–4 3–4 3 3 3–4 3–4 3
3 3–4 3 4 3–4 3 3–4 4 3 3–4 3–4 2–3 3–4 4 3
Chromic chloride 1 3 2–3 3 2 2 3 3 2 3 2–3 2 3–4 3 2
2 3 3 3–4 2–3 2 3 3–4 3 3–4 3 3 3–4 3 2
3 3 3 3–4 2–3 2–3 3–4 3–4 3 3–4 4 2–3 3 3–4 2–3
Potassium dichromate 1 3 3 3–4 4 3–4 4 3–4 3–4 4 3 3 4 4–5 4
2 3–4 3 3–4 3 2–3 3–4 3–4 3–4 3–4 3 2–3 4–5 4 3
3 3–4 3 4 3 3 4 4 3–4 4 3–4 3 3–4 3 3
Stannous chloride 1 4 3–4 3–4 3–4 3–4 4 4 4 4 3–4 3 4–5 4–5 3–4
303
2 3 3 3–4 3 2 2–4 3–4 3–4 4 3 3 4 3–4 2
3 3–4 3 3–4 3–4 2–3 3–4 4 3–4 4 3–4 2–3 3–4 3 2
Ferrous sulfate 1 3–4 4 3–4 3–4 3 4 3–4 3–4 4 3 2–3 5–6 5 4
2 3–4 3–4 4 3–4 3 3–4 4 3–4 4 3 2–3 5 4–5 4
3 4 3–4 3–4 4 3–4 4 4 3–4 4 4 3 5 4–5 3–4
Ferric chloride 1 3 3 3–4 3 2–3 3–4 3–4 3 3–4 3 2–3 4–5 5 3–4
2 3–4 3–4 3 3–4 3 3–4 4 3–4 4 3 3 5 4–5 4
3 4 4 4 4 4 4 4 4 4 2–3 3 4–5 4 3–4
Potassium alum. sulfate 1 3 3 3–4 2 2 3–4 3 3 4 2 2 3–4 3–4 2–3
2 3 2–3 3–4 3 2–3 3–4 3 3 4 3 2 3 3 2
3 3 2–3 3–4 3 2–3 3–4 3–4 3–4 4 3 2–3 3–4 3 2–3
Copper sulfate 1 4 3–4 4 3–4 3 3–4 4 3–4 4 3 2–3 4–5 4–5 4–5
2 4 4 3–4 3 3 3–4 4 3–4 3–4 3 3 4 4 4
3 4 3–4 3–4 4 3 3–4 4 3–4 4 3 3 3–4 3–4 3–4
Copper acetate 1 4 4 3–4 3–4 3 3–4 4 3–4 4 3 2–3 4 4–5 4
2 4 4 3–4 3 2–3 4 4 4 4 3 3 4 4 3–4
3 3–4 4 3–4 3 2–3 3–4 4 3–4 4 3–4 2–3 4–5 4 4
St.. ∗ = Staining on cotton; St..∗∗ = Staining on wool; Alt. = Alteration.
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TABLE 5 Color Fastness of Standing Dyebath of Combination of Mordant Wool Dyed with a Mixture of T.a. and M. (80:20%)
Rubbing
Number Wash fastness Alkali perspiration Acid perspiration fastness Light fastness
of reuse
∗ ∗∗ ∗ ∗∗ ∗ ∗∗
Mordant dyebath St.. St.. Alt St.. St.. Alt St.. St.. Alt Dry Wet 35h 50h 65h
304
Potassium 1 3 2–3 3–4 3–4 3 3–4 4 4 4 2–3 2 4–5 5 4
dichromate + 2 3 2–3 3–4 3–4 3 3–4 3–4 3–4 4 3 2–3 4 4–5 3–4
stannous chloride 3 3 3 3–4 3–4 3 3–4 4 4 4 3–4 3 4–5 4–5 4
Copper sulfate + 1 4 4 4 4 3–4 3–4 4 4 4 2–3 2 5–6 5 4–5
Potassium 2 3–4 4 3–4 3–4 3 3–4 4 3–4 4 3–4 2–3 5 4 4–5
dichromate 3 3–4 3–4 4 3–4 3–4 4 4 3–4 4 3 3 5–6 3–4 4
Ferrous Sulfate + 1 3 2–3 3–4 4 3 4 4 3–4 4 2 2 5 5 4–5
Potassium 2 3 2–3 3 3 2–3 3–4 4 3–4 4 3–4 2–3 5 3–4 3
dichromate 3 3 3 3–4 3–4 3–4 4 3–4 3–4 3–4 3 2–3 5 3–4 3
Copper sulfate + 1 4 3–4 3 4 3–4 4 4 4 4 3–4 2 5–6 4–5 4–5
Ferrous sulfate 2 4 3–4 3–4 4 3–4 4 4 3–4 4 3–4 2–3 5 4 4
3 4 3–4 3–4 4 3 3–4 4 4 4 3–4 2–3 4–5 4–5 4
St.. ∗ = Staining on cotton; St..∗∗ = Staining on wool; Alt. = Alteration.
Eco-friendly Dyeing of Wool 305
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Eco-friendly Dyeing of Wool 307
APPENDIX
Pre-mordant I
Simultaneous mordant II
Post-mordant III
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