Journal of Natural Fibers

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Microwave-assisted improvement in dyeing

behavior of chemical and bio-mordanted silk
fabric using safflower (Carthamus tinctorius L)
extract

Shahid Adeel, Khadija Naseer, Sadia javed, Saqib Mahmmod, Ren-Cheng

Tang, Nimra Amin & Saba Naz

To cite this article: Shahid Adeel, Khadija Naseer, Sadia javed, Saqib Mahmmod, Ren-Cheng
Tang, Nimra Amin & Saba Naz (2018): Microwave-assisted improvement in dyeing behavior of
chemical and bio-mordanted silk fabric using safflower (Carthamus tinctorius L) extract, Journal of
Natural Fibers, DOI: 10.1080/15440478.2018.1465877

To link to this article: https://doi.org/10.1080/15440478.2018.1465877

Published online: 25 Apr 2018.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2018.1465877

Microwave-assisted improvement in dyeing behavior of chemical

and bio-mordanted silk fabric using safflower (Carthamus
tinctorius L) extract
Shahid Adeela, Khadija Naseerc, Sadia javedc, Saqib Mahmmodc, Ren-Cheng Tangd,
Nimra Aminb, and Saba Nazb
a
Department of Chemistry, Government College University, Faisalabad, Pakistan; bDepartment of Applied Chemistry,
Government College University, Faisalabad, Pakistan; cDepartment of Biochemistry, Government College University,
Faisalabad, Pakistan; dNational Engineering Laboratory for Modern Silk, College of Textile and Clothing Engineering,
Soochow University, Suzhou, China
ARTICLE HISTORY
Received 25 August 2017
ABSTRACT
Revised 23 March 2018
The resurgence of natural colorant in textile dyeing is gaining popularity Accepted 10 April 2018
due to their ecofriendly benefits. The current study has been concerned
with dyeing of silk fabric using extract obtained from safflower (Carthamus KEYWORDS
tinctorius L.) which was microwave irradiated for 1–5 min. To make dyeing Bio-mordant; carthamin;
process more ecofriendly, bio-mordants and chemical mordants have been curcumin; lawsone;
employed at optimal conditions. It is found that microwave treatment to microwave; silk
the extract for 3 min is suitable to get darker shades with acceptable color 关键词
characteristics using un-irradiated silk. It has been found that dyeing of un- 生物媒介; 微波; 丝绸
irradiated silk fabric for 60 min using acidic extract of Safflower (pH 2) has
given high color strength. Rating of colorfastness reveals that 7% of curcu-
min and lawsone as bio-mordant has not only given high color depth but
also rated excellent fastness properties as compared to chemical mordants
used. It is found that microwave treatment has not only improved the
dyeing behavior of carthamin but also enhanced the color characteristics.

摘要
天然染料在纺织印染死灰复燃的日益普及，由于其生态友好的好处。目前
的研究已涉及丝绸织物通过红花提取物染色（carthamustinctoriusl），1-5
分钟照射使染色工艺更环保的微波，生物和化学媒染剂媒染剂已在最佳条
件下。结果表明，微波处理3分钟后，用未经辐照处理的真丝织物，可获得
色泽较佳的较暗色调。结果表明，用红花酸浸提液（pH 2）对未辐照真丝
织物进行60分钟染色，赋予了较高的染色强度。评色牢度表明7%的姜黄素
和指甲花醌作为生物媒介不仅给高色彩深度也堪称优秀的牢度性能相比，
使用化学媒染剂。发现微波处理不仅提高了红花的染色性能也提高了颜色
特征。

Introduction
Plant-derived natural dyes have been used for coloration of textile since ancient time. By the introduction
of synthetic dyes, the frequent use of conventional dyeing has been reduced (Adeel et al. 2018a). After the
population explosion and industrial revolution, demand of synthetic dyes also increased dramatically as a
result the production of synthetic dyes that reached about 700,000 mt annually in the world (Baban,
Yediler, and Ciliz 2010; Ogugbue and Sawidis 2011). But the environmental pollution associated with

CONTACT Shahid Adeel shahidadeel@gcuf.edu.pk Department of Chemistry, Government College University, Faisalabad
38000, Pakistan.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/wjnf.
© 2018 Taylor & Francis
2 S. ADEEL ET AL.

synthetic dyes which cause series and fatal health hazards to the global community has given a great
tendency to revive the art of natural dyes in various fields (Adeel et al. 2018b; Khan et al. 2017). The
studies show that synthetic dyes cause harmful effect on global community due to carcinogenic,
cytotoxic, allergic, toxic, and mutagenic in nature (Khandare and Govindwar 2015; Gulzar et al. 2015).
Due to these carcinogenic effects, people have forced the industrialist and traders to introduce eco-
friendly and eco-label natural dyed green products in various walks of life (Feriel et al. 2018; Yin, Liang,
and Wang 2017).
Natural dyes obtained from different biodegradable and renewable sources such as fungi (Chadni
et al. 2017), mineral (Jihad 2014), plants (Arora, Agarwal, and Gupta 2017), microbes (Raju and
Radha 2015), Animals (Hasan et al. 2015), insect (Nejad and Nejad 2013), herbs (Annapoorani and
Divya 2015), and algae (El-Khatib, Ali, and El-Mohamedy 2016). These dyes also have antioxidant,
antibacterial, antiallergic, antiviral, antifungal, and anti-UV properties due to presence of different
functional group present in their structure which are very helpful for ecosystem (Baaka, Ksibi, and
Mhenni 2016; Brodowska 2017). Moreover, natural dyes are ecofriendly, nontoxic, nonpoisonous,
noncarcinogenic, and nonhazardous in nature (Pervaiz et al. 2016a, 2016b). Hence, due to such
beneficial aspects, the revival of natural dyes has been welcomed in applied fields.
Beside the advantages of natural dyes, they are also facing extraction problems regarding its yields and
coloring behavior. Researchers are trying to improve the extraction, coloring behavior, and its functional
properties. These methods include conventional extraction and dyeing process that are much cost and
energy consuming. Nowadays, there is a spreading knowledge about the utilization of modern trends
such as radiation technologies which are ecofriendly. These technologies such as UV radiation (Rehman
et al. 2017), gamma radiation (Adeel et al, 2017), plasma treatment (Zhou et al. 2017), microwave
radiation (Hussaan et al. 2017; Yusoff and Leo 2017), ultrasound radiation (Baaka et al. 2017; Manimozhi
and Kanakarajan 2017; Sheikh, Jagtap, and Teli 2016), mercerization, cationization, enzymatic extraction
(Vankar, Shukla, and Wijayapala 2017), supercritical fluid extraction (Talib et al. 2016), etc. show high
treatment speed. Among these tools, microwave radiation has its own importance in natural dyeing due
to clean, uniform, and leveled heating nature as it makes dyeing process cost, time, and energy efficient
by mass transfer of kinetics (Adeel et al. 2016; Belwal et al. 2016; Vega et al. 2016). Keeping in view the
advantage of microwave treatment, the current study is undertaken to improve the dyeing process of silk
fabric using safflower as a sources of natural dyes.
Safflower is an annual seed plant species belong to the Asteraceae family. It is cultivated around the globe
due to its edible oil utilization (Lulin et al. 2012). Since prehistoric time, safflower was used for the treatment
of various diseases such as gynecological, cardiovascular, and cerebrovascular (Asgarpanah and Kazemivash
2013) as well as to decorate the tombs of Egyptian mummies. Petals of safflower also contain carthamin as
coloring component (structure given below) which give red and yellow color onto silk and wool fabric. It is
also used to color the toys, cakes, and biscuits. It is fugitive dye to light and air and is said to be possible
substitute of saffron dye. Such advantages of safflower in different fields have compelled our research group
to color the natural fabrics with an improvement in its dyeing behavior under microwave treatment.

Carthamin (C I Natural Yellow 5)

 JOURNAL OF NATURAL FIBERS 3

The aim of current study is not only to improve dyeing behavior of bio-mordanted and chemical
mordanted silk fabric but also to enhance the rating of color characteristics using safflower as a
source of natural colorant.

Materials and methods

Sample preparation
Safflower flowers (Carthamus tinctorius L.) have been selected for extraction of natural colorant
carthamin (C I 75140) as an ecofriendly natural dye. Fresh flowers of C. tinctorius L. were collected
from the Botanical Garden of Govt. College University Faisalabad, Pakistan. Silk fabric (mulberry,
width 114 cm) were provided by National Engineering Laboratory for Modern Silk, College of
Textile and Clothing Engineering, Soochow University, 199 Renai Road, Suzhou 215123, China. The
chemicals used during extraction, dyeing, and mordanting were of commercial grade. Turmeric
(Curcuma longa) and Henna (Lawsonia innermis) as sources of bio-mordant were purchased from
the local herbal market of Faisalabad.

Preparation of powders and bio-mordants

For the preparation of powder, safflowers (C. tinctorius L.) were washed with distilled water to
remove the dust and others types of impurities. After washing, flowers were dried under shade.
After drying, flowers were ground into fine powder using food grade grinding machine
(Panasonic, 550 W). The ground powder was then used for further studies for extraction and
dyeing purposes (Sumithra and Amutha 2016). For bio-mordants, freshly available leaves of henna
and turmeric rhizomes were procured from local herbal market, subjected for grinding to get
uniform particle size powder. For obtaining bio-mordants, the plant materials were boiled in
distilled water for 1 h, keeping material-to-liquor ratio of 1:25. After boiling, the materials were
filtered and filtrates were oven dried. The dried powder lawsone and curcumin were then used as
bio-mordants.

Extraction and irradiation process

For effective extraction of natural colorant carthamin from safflower, two extraction media such as
acidic and aqueous were used boiling the powder for 1 h keeping material-to-liquor ratio of 1:25. For
this purpose, 4 g of powder has been boiled with 100 ml of distilled water and 2% acidic solution for
1 h. After extraction, the crude materials were filtered and extracts obtained were irradiated for
1–5 min using microwave oven of Orient (700 W, 2450 Hz). To get optimal irradiation condition,
the dyeing of irradiated and un-irradiated fabric was carried out at 80°C for 60 min by employing
irradiated and un-irradiated aqueous and acidic extracts.

Optimization of dyeing and mordanting condition

Dyeing of silk fabric was carried out using exhaust dyeing method. For optimization of dye bath
nature, irradiated acidic extract of various pH (1–7) was employed for 20–70 min keeping M:L
ratio of 1:25 at 80°C. In the current study, two bio-mordants curcumin from turmeric and lawsone
from henna (structures given below) and two chemical mordants (iron sulfate and aluminum
sulfate) were used to improve color depth (k/s) and fastness properties. The prepared chemical and
bio-mordants were used keeping 1%, 3%, 5%, 7%, and 9% at optimal irradiation and dyeing
conditions (Yusuf et al. 2017).
4 S. ADEEL ET AL.

Lawsone

Curcumin

Evolution of color fastness properties

The color strength of un-irradiated and irradiated silk fabric dyed with safflower extract was
investigated through Kulbeka Munk equation completed in spectra flash SF 600 with illuminant
D6510° observer at Eco-Friendly Textile Lab., Govt. College University Faisalabad, Pakistan. In order
to assess the effect of MW treatment on colorfastness, different ISO methods such as ISO 105 BO2
for light using fadometer, ISO 105 CO3 for washing using rota wash, and ISO X 12 for rubbing using
crock meter were rated to observe the effect of chemical and bio-mordant using optimal extract onto
un-irradiated silk.

Result and discussion

The acidic and aqueous extract obtained from safflower petals have shown various effects onto silk
fabric under the influence of Mw treatment. The result gives in Figure 1 using aqueous extract
showed irradiated extract has given highest k/s values onto irradiated silk. But the result given in
Figure 2 showed that irradiated acidic extract (RE, 3 min) gave high k/s values onto un-irradiated silk
fabric (NRS). This is because in acidic medium, the function group of silk were more viable to
interact with colorant as compared to dyeing in aqueous medium (Shabbir et al. 2016) and also
microwave treatment adds many more values in getting darker shades via mass transfer kinetics.
Previous studies show that the mass transfer kinetics i.e. shifting of colorant from cell wall of plant to
the solvent without changing its physiological characteristics is rapid via microwave radiation instead
of conventional heating (El-Khatib, Ali, and El-Mohamedy 2016; Karabegovic et al. 2014; Sivakumar,
Rani, and Kumari 2017). The acidic medium of dye bath for silk dyeing is very useful for attaining
maximum color strength because the ionic or covalent bindings formed during dyeing remains
stable between amino group of silk and hydroxyl group of colorant (Shabbir et al. 2016). Low time
 JOURNAL OF NATURAL FIBERS 5

0.9 NRE/NRS NRE/RS RE/RS RE/NRS

0.8

0.7

0.6

0.5
K/S

0.4

0.3

0.2

0.1

0
1 2 3 4 5
Microwave Irradiation (Min)

Figure 1. Effect of microwave radiation on dyeing behavior of silk fabric using aqueous extract of safflower flowers.

NRE/NRS NRE/RS vvRE/RS RE/NRS

4
K/S

0
1 2 3 4 5
Microwave Irradiation (Min)

Figure 2. Effect of microwave radiation on dyeing behavior of silk fabric using acidic extract of safflower flowers.

microwave treatment does not stimulate the colorant to evolve into medium while for long time,
treatment may cause involvement of other moieties along with actual colorant to interact with the
fabric. During dyeing process, the actual ability of carthamin is reduced to interact with fabric that
results into low k/s value. Hence, 3-min Mw treatment to acidic extract is recommended for dyeing
and getting darker shades on to un-irradiated silk fabrics (NRS).
The result given in Figure 3 reveals that irradiated acidic extract (RE, 3 min) having pH 2 has
given darker shade onto un-irradiated fabric (NRS). This is because moving toward alkalinity the
stability of zwitterion is disturbed which in turn may favor the desorption due to transformation
into ionic form thereby yielding low color strength (Uslu and Bamufleh 2016). Hence, acidic dye
bath of pH 2 is recommended for dyeing of un-irradiated silk fabric.
The results given in Figure 4 reveal that dyeing of un-irradiated silk (NRS) for 60 min using
acidic irradiated extract (RE, 3 min) gives high color strength. This is because contact time
always plays a good role in leveled natural dyeing of silk. Low contact time always reduces
6 S. ADEEL ET AL.

2.5

K/S 2

1.5

0.5

0
1 2 3 4 5 6 7
Dyeing pH

Figure 3. Relationship between dyeing pH and k/s value of un-irradiated silk using irradiated acidic extract of safflower flowers.

5
K/S

0
20 30 40 50 60 70
Dyeing time (min)

Figure 4. Relationship between dyeing time and k/s value of un-irradiated silk using irradiated acidic extract of safflower flowers.

kinetic energy of colorant to rush toward the fabric whereas for high time not only hydrolytic
degradation occurs but also desorption is favored. This may also be explained that heating for
long time may weaken the H bonding of attraction between dye and silk fabric which results
into low color strength (Sun and Tang 2011; Yusuf et al. 2015). Hence, 60 min is the optimal
dyeing time for getting acceptable color characteristics.
The dyeing behavior of silk fabric using chemical and bio-mordanting was investigated
using Mw irradiated acidic extract of safflower. The use of bio-mordants has not only made
the process more ecofriendly but also has given high color strength with beautiful shades. The
result given in Figure 5 using pre-mordant shows that lawsone from henna and curcumin
from turmeric as bio-mordants have given high k/s values and excellent fastness character-
istics with bright yellow shades as compared to chemical mordants used. This is because Al
and Fe form metal dye complex with irradiated extract onto un-irradiated fabric, but during
complex formation, the other impurities also show that their appearance onto fabric results
into sadden shades with low k/s values (Hasan et al. 2015; Hosseinnezhad et al. 2017). But the
 JOURNAL OF NATURAL FIBERS 7

Al Fe Curcumin Lawsone
18
16
14
12
K/S 10
8
6
4
2
0
1 3 5 7 9
PRE MORDANT CONC (%)

Figure 5. Pre-chemical and bio-mordanting of un-irradiated silk using irradiated acidic extract of safflower flowers.

utilization of bio-mordant has added more value due to intra-molecular H-bonding with
colorant and fabric. This extra bonding has made dyeing process more ecofriendly and
green process that results into darker shades. Similarly, the result given in Figure 6 for
post-mordanting shows that bio-mordants have given excellent colors with good k/s values.
Hence, bio-mordants have given darker shades where 7% of curcumin and lawsone has been
optimized as pre-mordant and post-mordant as compared to chemical mordant used. The
reduction in the amount of mordant shows that Mw treatment is a cost-effective tool.
The rating results of pre-mordanting and post-mordanting given in Tables 1 and 2 show that bio-
mordants have improved the fastness characteristics. Bio-mordanting is gaining popularity due to
their green nature and as an alternative to chemical mordants because due to presence of OH. Group
in bio-mordant helps to make more firm interactions thereby giving high rating of color fastness
properties. This is attributed to the presence of benzene ring and conjugated system in the colorant
(carthamin) and bio-mordant which upon exposure to detergent, heat, light, crocking resist to fade
(Arora, Agarwal, and Gupta 2017), whereas the formation of coordinate metal complex with color-
ant and fabric before and after dyeing also adds more resistance to fade the color. Hence, microwave
treatment of acidic extract of Safflower has improved the colorfastness characteristics upon applica-
tion on un-irradiated silk fabric.

Al Fe Curcumin Lawsone
14
12
10
8
K/S

6
4
2
0
1 3 5 7 9
POST MORDANT CONC(%)

Figure 6. Post-chemical and bio-mordanting of un-irradiated silk using irradiated acidic extract of safflower flowers.
8 S. ADEEL ET AL.

Table 1. Effect of pre-mordanting on colorfastness of silk fabric dyed with irradiated acidic extract of safflower flowers.
Mordant used Mordant conc Light fastness Wash fastness Dry rubbing fastness Wet rubbing fastness
AL 1 3/4 4 4 3/4
3 4 4/5 4/5 4
5 4 4 4 4
7 4/5 4 4 4
9 4 4/5 4/5 4/5
Fe 1 4 4/5 4/5 4
3 4/5 4 3/4 4
5 4 4/5 4 3/4
7 4/5 4 4 4
9 4/5 4 4/5 ¾
Curcumin 1 4 4/5 4/5 4
3 4 4 4 4
5 4/5 4/5 5 4/5
7 4/5 4 5 4/5
9 4 4 4/5 4
Lawsone 1 4/5 4 4/5 4
3 4 4/5 4 3/4
5 4 4/5 4 3/4
7 4/5 4 4/5 4
9 4/5 4 4 4

Table 2. Effect of post-mordanting on colorfastness of silk fabric dyed with irradiated acidic extract of safflower flowers.
Mordant used Mordant conc Light fastness Wash fastness Dry rubbing fastness Wet rubbing fastness
Al 1 3/4 3/4 4 4
3 4 4 4/5 3/4
5 3/4 3/4 4 3/4
7 4/5 4/5 4 4
9 4 4 4/5 4
Fe 1 3/4 4 3/4 4
3 4 3/4 4 4/5
5 4/5 4 3/4 4
7 4/5 4/5 4 4
9 4 4 4 4/5
Curcumin 1 4 3/4 4 3/4
3 4/5 3/4 4/5 4
5 4/5 4 4 4
7 5 4/5 5 4
9 4/5 4/5 4/5 4/5
Lawsone 1 3/4 3/4 4 3/4
3 3/4 3/4 4/5 4
5 4 4 4/5 4
7 4/5 4 4 3/4
9 4 4/5 4 4

Conclusion
Mass transfer kinetics driven by microwave treatment during dyeing and extraction has made the
natural dyeing process more eco-label, green, coat and time effective. The present study concluded
that natural dye (carthamin) extracted from safflower and its stimulation by microwave treatment
followed by dyeing of chemical and bio-mordanting of silk can be used as a possible substitute of
yellow synthetic dyes. It has been found that microwave treatment to acidic extract of pH 2 for 3 min
has given darker shades and high color strength by dyeing un-irradiated silk for 1 h. Furthermore,
bio-mordants, i.e., lawsone from henna and curcumin from turmeric have not only improved the
colorfastness properties from good to excellent but also have given new shades. It is found that
microwave treatment can also be used to improve the color characteristics of other natural fabrics
using various natural dyes. Moreover, the addition of bio-mordants can be done to make dyeing
process more green and eco-label.
 JOURNAL OF NATURAL FIBERS 9

Acknowledgments
We are grateful to Mr. Zafar Iqbal Manger QA & QC of Noor Fatima fABRICS (Pvt.) Limited, Faisalabad, and
Muhammad Abbas Director Harris Dyes and Chemical (Pvt.) Limited, Faisalabad, for providing the technical
assistance and facilities of fastness testers and spectra flash (SF650).

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