Review of Literature On Natural Dyes

CHAPTER- II
REVIEW OF LITERATURE
Promotion of natural dyes along with the use of metal mordant is of

major concern due to non eco-friendly nature of mordants. It is necessary to
develop new techniques of coloration with the help of modern scientific inputs
so that these dyes can offer themselves as effective eco-option.
The present study has focused on elimination of the use of non eco
friendly mordant and improvement in colour fastness by the use of eco-
friendly mordant.
The literature reviewed has been presented in the following sequence.
2.1 Environment pollution from synthetic dyes

2.2 Natural dyes and mordants
2.2.1 Advantages and disadvantages of natural dyes
2.2.2 Classification of natural dyes
2.2.3 Mordants and Fixation
2.2.4 Mordanting methods
2.2.5 Types of mordants
2.3 Studies on natural dyes
2.3.1 Natural dyes for cellulose
2.3.2 Natural dyes for protein
2.3.3 Natural dyes for polyamide
2.3.4 Natural dyes for printing
2.4 Details of dyes used in the study
2.4.1 Tropical Almond or Indian Almond(Terminalia Catappa)
2.4.2 Malabar semul or red cotton tree(Bombax Ceiba)
2.4.3 Mast tree or Asopalav(Polyalthia longifolia)
2.4.5 Neem tree(Azadirachta indica)
2.5 Studies of ecofriendly finishes on dyed fabric
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2.1 Environment pollution from synthetic dyes

Until the latter half of the 19th century people were using natural dyes
(Parkes, 2002) for colouring of textiles. Different parts of the plant were used
to obtain various shades.
After invention of synthetic dyes, natural dyes are not used because of
the advantage of synthetic dye over natural dye in respect of application,
colour range, fastness properties, and availability. But, some synthetic dyes are
hazardous, carcinogenic and also release vast amount of pollutant in the
environment during their manufacturing (Gulrajani et al. 1999; Nagia and
Mohamedy, 2007)
The world is slowly realizing the damaging effects of several
chemicals that are synthesized by men in laboratory. Ecology and pollution
have therefore become a major concern to all (Nimkar, 2004). Green house
effect, ozone layer depreciation, water pollution and improper waste disposal
have become important issues (Teli et al., 2002a). So, all developed countries
are looking for safe environment. In this context, the textile industry, which
uses hundreds of chemicals in production, from raw material to disposal, is
generally regarded among the most polluting industry (Nimkar, 2004).
To promote a clean environment and safety to the manufacture and
users of textile products Germany has banned certain dyes and the entire
European Union (EU) is promoting the concept of eco friendly textiles. This
concept is based on the cradle-to-grave approach i.e. it analysis entire life
cycle of production distribution and utilization and disposal after use
(Subramanian and Phalgunani, 1995). In this context, natural dyes are being
promoted but with a word of caution (Chavan, 1995) to keep the revival
activities for natural dyes to a limited scale in order to maintain the balance
between environment and trade.
Dyes can be of many different structural varieties like acidic, basic,
disperse, azo, anthraquinone based and metal complex dyes among others. The
textile industry is the largest consumer of dye stuffs. During the coloration
process a large percentage of the synthetic dye does not bind and is lost to the
waste stream (Weber and Adams, 1995).
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Approximately 10-15% dyes are released into the environment during

dyeing process making the effluent highly colored and aesthetically
unpleasant. The effluent from textile industries thus carries a large number of
dyes and other additives which are added during the colouring process (Wang
et al., 2002). These are difficult to remove in conventional water treatment
procedures and can be transported easily through sewers and rivers especially
because they are designed to have high water solubility. They may also
undergo degradation to form products that are highly toxic and carcinogenic
(Rinde & Troll, 1975).
It is in the textile industry that the largest quantities of aqueous wastes
and dye effluents are discharged from the dyeing process, with both strong
persistent colour and a high biological oxygen demand (BOD), both of which
are aesthetically and environmentally unacceptable (Wang et al., 2007).
Recently, a number of commercial dyers and small textile export
houses have started looking at the possibilities of using natural dyes for
regular basis dyeing and printing of textiles to overcome environmental
pollution caused by the synthetic dyes (Glover and Pierce, 1993).
2.2Natural dyes and mordants
Natural dyes comprise those colourants (dyes and pigments) that are
obtained from animal or vegetable matter without chemical processing
(Gulrajani & Gupta, 1992).
The word ‘natural dye’ covers all the dyes derived from the natural
sources like plants, animal and minerals. Natural dyes are mostly non-
substantive and must be applied on textiles by the help of mordants, usually a
metallic salt, having an affinity for both the colouring matter and the fibre.
Transition metal ions usually have strong coordinating power and/or capable
of forming week to medium attraction/interaction forces and thus can act as
bridging material to create substantivity of natural dyes when a textile material
being impregnated with such metallic salt (i.e.mordanted) is subjected to
dyeing with different natural dyes, usually having some mordantable groups
facilitating fixation of such dye. These metallic mordants after combining with
dye in the fibre, forms an insoluble precipitate or lake and thus both the dye
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and mordant get fixed to become washing fast to a reasonable level (Samanta
and Konar, 2011).
2.2.1Advantages and disadvantages of natural dyes
In the recent years, there has been a trend to revive the art of natural
dyeing. This is mainly because in some aspects natural dyes are advantageous
against synthetic dyes. Some of these advantages along with some limitations
(disadvantages) are listed below:
Advantages of natural dyes
 The shades produced by natural dyes are usually soft, lustrous and
soothing to the human eye.
 Natural dyestuff can produce a wide range of colours by mix and match
system. A small variation in the dyeing technique or the use of different
mordants with the same dye (polygenetic type natural dye) can shift the
colours to a wide range or create totally new colours, which are not
easily possible with synthetic dyestuffs.
 Natural dyestuffs produce rare colour ideas and are automatically
harmonizing.
 Unlike non-renewable basic raw materials for synthetic dyes, the natural
dyes are usually renewable, being agro-renewable/vegetable based and at
the same time biodegradable.
 In some cases like harda, indigo etc., the waste in the process becomes
an ideal fertilizer for use in agricultural fields. Therefore, no disposal
problem of this natural waste.
 Many plants thrive on wastelands. Thus, wasteland utilization is an
added merit of the natural dyes. Dyes like madder grow as host in tea
gardens. So there is no additional cost or effort required to grow it.
 This is a labour intensive industry, thereby providing job opportunities
for all those engaged in cultivation, extraction and application of these
dyes on textile/food/leather etc.
 Application of natural dyes has potential to earn carbon credit by
reducing consumption of fossil fuel (petroleum) based synthetic dyes.
 Some of its constituents are anti-allergens, hence prove safe for skin
contact and are mostly non-hazardous to human health.
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 Some of the natural dyes are enhanced with age, while synthetic dyes
fade with time.
 Natural dyes bleed but do not stain other fabrics, turmeric being an
exception.
 Natural dyes are usually moth proof and can replace synthetic dyes in
kids garments
Despite these advantages, natural dyes do carry some inherent
disadvantages, which are responsible for the decline of this ancient art of
dyeing textiles.
Limitation/ disadvantages of natural dyes
 It is difficult to reproduce shades by using natural dyes/colourants, as
these agro-products vary from one crop season to another crop season,
place to place and species to species, maturity period etc.
 It is difficult to standardize a recipe for the use of natural dyes, as the
natural dyeing process and its colour development depends not only on
colour component but also on materials.
 Natural dyeing requires skilled workmanship and is therefore expensive.
Low colour yield of source natural dyes thus necessitates the use of more
dyestuffs, larger dyeing time and excess cost for mordants and
mordanting.
 Scientific backup of a large part of the science involved in natural dyeing
is still need to be explored.
 Lack of availability of precise technical knowledge on extraction and
dyeing techniques.
 The dyed textile may change colour when exposed to the sun, sweat and
air.
 Nearly all-natural dyes with a few exceptions require the use of mordants
to fix them on to the textile substrate. While dyeing, a substantial portion
of the mordant remains unexhausted in the residual dye bath and may
pose serious effluent disposal problem.
 With a few exceptions, most of the natural dyes are fugitive even when
applied in conjunction with a mordant. Therefore, sometimes their colour
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fastness performance ratings are inadequate for modern textile usage.

(Samanta and Konar,2011)
2.2.2 Classification of natural dyes
Natural dyes can be classified (Gulrajani & Gupta, 1992) in a number
of ways. The earliest classification was according to alphabetical order or
according to the botanical names. Later, it was classified in various ways, e.g.
on the basis of hue, chemical constitution, application class etc.
A. In “Treatise on Permanent Colours” by Bancroft (1775), natural dyes are
classified into two groups: ‘Substantive Dyes’ such as indigo, turmeric etc.
which dye the fibers directly and ‘Adjective Dyes’ such as logwood,
madder etc. which are mordanted with a metallic salt.
B. Natural dyes are classified according to hue (Predominating colour). Hue
of the natural dyes is assigned as with number by Colour Index
International started in 1924. The database is jointly maintained by SDC
and AATCC. The number of dyes in each hue is given in table-2.1
Table 2.1 Showing the number of natural dyes in each hue as per the Colour Index
(Samanta and Konar, 2011)
CI Natural No. of Dyes Percent
Yellow 28 30.4
Orange 6 6.5
Red 32 34.8
Blue 3 3.3
Green 5 5.5
Brown 12 13
Black 6 6.5
On the basis of hues, natural dyes can be classified as follows:

 Red colour dyes: Most red dyes are hidden in roots or barks of plants
or camouflaged in the bodies of dull grey insects. They are almost
invariably based on anthraquinone and its derivatives. These dyes are
stable to light and washing.
 Yellow colour dyes: Yellow is the liveliest and perhaps the most
abundant of all hues in nature. About 90% of the yellow dyes are
flavonoids. Generally, they produce pale shade with quicker fading
except turmeric, which produce dull deep shade. Wash fastness rating
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of natural yellow dyes ranges from fair to excellent, e.g., tesu,

turmeric, kapila.
 Blue colour dyes: Indigo and woad are blue colour dye which gives
excellent fastness to light and washing.
 Black colour dyes: Black shades, generally obtained from tannin rich
plant natural dyes and appreciably substantive towards cellulosic and
protein fibre, imparts good overall fastness properties. Examples –
logwood, harda, custard apple etc.
C. On the basis of origin, natural dyes are broadly classified into three
Categories: vegetable, mineral and animal origin. There are about 500
vegetable origin dyes, in these the colouring matter is derived from root,
leaf, bark, trunk or fruit of plants, details are given in table-2.2
Table-2.2 Some common natural dyestuffs obtained from different vegetable origin
Part of the Plant Dyestuffs
Root Turmeric, Madder (Manjistha), Onions, Beet-root
Bark/ Branches Purple bark, Sappan wood, Shillicorai, Khair,
Red bark, Sandalwood
Leaf Indigo, Henna, Eucalyptus, Tea,
Cardamon, Coral Jasmine, Lemon Grass
Flowers (Petals) Marigold, Dahlia, Tesu, Kusum
Fruits/Seeds Latkan, Pomegranate rind, Beetle nut, Myrobolan
(Harda)
Mineral origin dyes are derived from specific mineral natural source
or so-called mineral colours are produced from purified inorganic
compounds. Some of the important mineral dyes are chrome-yellow, iron-
buff, narkin-yellow, Prussian-blue and manganese brown. Animal origin lac,
cochineal and kermes have been the principal natural dyes yielding from the
insect.
D. On the basis of their chemical constitution (Dedhia, 1998).
i. Indigoid dyes: Indigo, tyrian purple and woad are the most common
examples of this class.
ii. Anthraquinone dyes: Almost all the red natural dyes are based on the
anthraquinoid structure having both plant and mineral origin. Madder,
lacs, kermes, cochineal are some of the dyes. These are generally
mordant dyes.
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iii. Alphanaphthoquinones: Typical examples of this class are lawsone

(henna) and juglone, obtained from the shells of unripe walnuts. These
dyes are generally dispersing dyes and give shades of orange.
iv. Flavonoids, which yield yellow dyes, can be classified under flavones,
isoflavones, aurones and chalcones. Flavones are colourless organic
compounds. Most of the natural yellows are derivatives of hydroxyl
and methoxy substituted flavones and isoflavones. Common example
is weld (containing luteolin pigment) giving brilliant and fast colours
on both wool and silk.
v. Di-hydropyrans: Closely related in chemical structure to the flavones
are substituted di-hydropyrans, viz. haematin and its leuco form,
haematoxylin. These are important natural dyes for dark shades on
silk, wool and cotton. Logwoods, brazil wood and sappan-wood are
the common example.
vi. Anthocyanidins: The naturally occurring member of this class
includes carajurin, a direct orange dye for wool and cotton. It is
obtained from the leaves of bignonia chica.
vii. Carotenoids: The class name carotene is derived from the orange
pigment found in carrots. In these, the colour is due to the presence of
long conjugated double bonds.
E. On the basis of the method of application (Gulrajani & Gupta, 1992).
i. Mordant dyes are dyestuffs which require a mordant in their
application as they have no affinity for the fiber being dyed. A
mordant dye should have electron donating groups capable of forming
a complex with the transition metal salt, e.g., madder, fustic, Persian,
berries, kermes, cochineal etc.
ii. Vat dyes are water insoluble dyes which are first converted to their
water soluble form (reducing with sodium hydrosulphite and then
solubilising it with alkali) and then applied to the fibers. The true
colour is produced only on oxidation followed by treatment with a hot
soap solution, e.g., indigo.
iii. Direct dyes are those dyes that have tremendous affinity for the
cellulosic fibers. They are dyed from a boiling dye bath. Turmeric,
harda, pomegranate rind etc. are the few of the direct natural dyes.
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iv. Acid dyes are applied from an acidic medium. The dye molecules
have either sulphonic or carboxylic group (s) which can form an
electrovalent bond with amino groups of wool and silk. An after
treatment with tannic acid known as back tanning improves the
fastness of these type of dyes, e.g., saffron.
v. Disperse dye has a relatively low molecular mass, low solubility and
no strong solubilizing groups. Disperse dyes can be applied on to
hydrophobic synthetic fibre from neutral to mildly acidic pH. They can
also be applied to silk and wool. These dyes can be post-mordanted
with chromium, copper and tin salts, e.g., lawsone and many other
flavones and anthraquinone dyes.
vi. Basic or cationic dyes on ionization give coloured cations and form
an electrovalent bond with the –COOH group of wool and silk. These
dyes are applied from neutral to mildly acidic pH. These dyes have
poor light fastness, e.g., berberine.
The same dyestuffs can produce many different colours and shades
depending on the soil type, cultivation method, environment, weather, season,
material to be dyed, and the source of water being used (Chakrabarti &
Vignesh, 2011). As a result, it is one of the reasons to explain why the
synthetic dyes are adopted in the manufacturing industry instead of natural
dyes. The standardization of the natural dyes can enhance the competitiveness
in the market.
2.2.3 Mordant and Fixation
The word "mordant" comes from the French word "Mord" or "to bite"
and mordants can be described as metallic salts with affinity for both fiber and
dyes stuffs and that improves the colour fastness. Even some of the fugitive
dyes have been used successfully with the help of mordants. (Vankar, 2007)
A mordant is substance used to set dyes on fabrics or tissue sections by
forming a coordination complex with the dye which then attaches to the fabric
or tissue. The mordant is a sort of bridge between the fibre and the dyestuffs
that are extracted from the plants or animals (Bohmer, 2002).
However, most of the natural dyestuffs which are known as subjective
dyes require some mordants to fix the colour on the fibers and form strong
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chemical bonds. The mordant enters deeply into the fibre and combines with
dyestuff to form the colour (Brennan, 2004).
Mordants help the fibre receive the dyestuff well and form bonding.
Compounds of alum (potassium alum), tannin (tannic acid), and iron (ferrous
sulphate) are the safest choices (Brennan, 2004).
Mordant can help the dyestuffs achieve a strong and bright colour on
cellulose fibers. They combine with the dyestuff and are then permanently
fixed onto the fibre. Intensity of the hue and the fastness of the resultant colour
can be improved (Dalby, 1992).
However, mordants have their own colours which may affect the
colour of the dyed textile. In addition, the mordants combined with the dyeing
molecules lead to a significant influence on the hue produced with a particular
dyestuff (Horrocks &Anand, 2000).
2.2.4 Mordanting Methods:

Mordanting can be achieved by pre-mordanting (before dyeing),
simultaneously mordanting and dyeing or post mordanting system (after
dyeing).
A. In the pre-mordanting method, the textile material is first immersed into the
mordant solution for 30 to 60 minutes at the room temperature or higher
temperature with a liquor ratio of 1:5 to 1:20. The textile material treated
with mordant is then dyed. After dyeing, the dyed material is washed with a
non-ionic detergent. It is the most frequently used procedure by natural
dyers because large quantities of textile can be treated and stored until
dyeing.
B. As for the simultaneous mordanting and dyeing, the textile material is
immersed in a dyebath solution containing both mordant and dye. Dyeing
auxiliaries can be added during the dyeing process. For the optimization of
dyeing condition, dyeing process variables can be studied for the specific
fibre-mordant-natural dye system in order to improve the colour yield of
textiles. After dyeing, the textile material is washed with non-ionic
detergent.
C. With regard to the post-mordanting method of natural dyeing, the dyeing
process is carried out on the bleached textiles in the dyebath without
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mordant. The dyed fabric then is treated in another bath called saturator
containing the mordanting solution. Treatment condition may vary
depending on the type of fibre, dye and mordant system being used. After
dyeing, the textile material is washed properly with non-ionic detergent.
When using this mordanting method, the colours are usually different and
often less strong.
In all these three applications, mordants act as dye setters that will
prevent the colour from running or streaking after dyeing (Yee, 2013).
2.2.5 Types of mordants
Limitation on colour yield and poor fastness properties prompted a
search for ideal mordants, the chemicals which increase natural dye uptake by
textile fibers. Different types of mordants yield different colours even for the
same natural dye. Therefore, final colour, their brilliance and colour fastness
properties are not only dependant on the dye itself but are also determined by
varying concentration and skillful manipulation of the mordants. Thus, a
mordant is more important than the dye itself. Moreover, the ideal mordant for
bulk use should produce appreciable colour yield in practicable dyeing
conditions at low cost, without seriously affecting physical properties of fibre
or fastness properties of the dyes. Also, It should not cause any noxious effect
during processing and the dyed textile material should not have any
carcinogenic effect during use. Mordants can be classified into the following
categories:
A. Metallic mordants
They are generally metal salts of aluminum,chromium,iron,copper and
tin. The metallic mordants are of two types.
i. Brightening mordants
a) Potash alum: Among all types of alum, potash alum is cheap, easily
available and safe to use mordant. It usually produces pale versions of the
prevailing dye colour in the plant.
Alum or other metallic mordants fix dyes on fibre by chemically
combining with the functional groups of the natural dyes to form covalent
bonds, hydrogen bonds and other interactional forces as shown in figure
2.1
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Figure: 2.1 Bondings between alum and dye (Samanta & Konar, 2011)
Alum occurs in nature but is also found in many plants. Alum reacts
chemically with water first, whereby the aluminum forms a mildly basic
hydroxide which is no longer soluble in water. Alum attaches itself to the
mildly acidic groups of the protein molecules of the wool or silk fibers and
heat can accelerate the process. During dyeing, the aluminum then binds
the molecules of mildly acidic dyestuff, thereby creating the so-called lac
which is insoluble. Hence, the dyed material is colourfast when washed.
(Bohmer, 2002).
b) Chrome (potassium dichromate): It is also referred to as red chromate.
It is relatively more expensive. However, Cr3+ or Cr6+ is considered to be
harmful for human skin as objectionable heavy metal beyond a certain
limit of its presence. Its use has been limited as per the norms of the eco-
standards. Chrome is known as potassium dichromate and is a kind of
brightening mordant. It produces a deep version of the prevailing dye
colour, and leaves wool with beautiful softness, while other mordants will
harden wool (Dyer, 1976; Salvendy & Ji, 2012).
c) Tin (stannous chloride): It gives brighter colours than any other mordant.
However, they are oxidized on exposure to air and may impart a stiff hand
to the fabric. Stannous chloride also causes higher loss of fabric tenacity
(tensile strength) if applied beyond a certain concentrations.
ii. Dulling mordants
a) Copper (cupric sulphate): Known as blue vitriol available as bright blue
crystals. it is readily soluble in water and easy to apply. It gives some
special effects in shades, which otherwise cannot be obtained. However,
copper beyond a certain limit is also under the eco-standard norms as
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objectionable heavy metal. Copper mordant also reacts with water to form
a mildly basic hydroxide (Bohmer, 2002).Copper mordant is less
frequently used than the other mordants as it is toxic. (Liles, 1990).
b) Iron (ferrous sulphate): It is also known as green vitriol and is readily
soluble in water. It is used for darkening /browning and blackening of the
colours/ shades. It is easily available and one of the oldest mordants
known. It is extensively used to get grey to black shades.
B. Tannins
The term ‘tanning agent’ is given initially to those water-soluble
cellulosic materials that predicates gelatin from solution. But all gelatin
precipitation did not identified as tanning agent. Tannins are polyphenolic
compounds having capacity of gelling under certain conditions. Among the
tannins, myrobalan (harda) and galls/sumach are most important.
Tannic acid is available in its natural form and can be extracted
from number of vegetables. Oak galls, sumach, cutch and some barks are all
rich in tannic acid. Dyestuffs that contain tannin such as black oak,
pomegranate, cutch, fustic, etc. do not need an additional tannin mordant.
Some of these tannic acid rich sources may also contain dyes, and so this may
affect the resultant colour after dyeing has taken place, resulting in darker and
less brilliant colour. (Bohmer, 2002). Tannic acid extracted from the vegetable
sources for natural dyeing is more natural than those metal salts or the
chemical tannic acid (Dalby, 1992).During dyeing, the tannin combines with
the cellulose on one side and then binds with another mordant such as alum or
iron mordant. The chemical processes involved in the use of tannic mordant
are not entirely clear.
C. Oil type mordants
Vegetable oils or Turkey red oil (TRO) are such type of mordants.
TRO as mordant is mainly used in the dyeing of deep red colour from madder.
The main function of TRO as oil mordant is to form a complex with alum
when used as a main mordant. Sulphonated oil posses better binding-capacity
than the natural oils. Oil mordanted samples exhibit superior fastness and hue.
2.3 Studies on natural dyes
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In the last fifteen to twenty years many scientific research studies on

natural dyes have been carried out very systematically. These studies mainly
deal with identification of dye, extraction procedure standardization,
application method and colour fastness test. Some important ones are grouped
and summarised below.
2.3.1 Natural dyes for cellulosic fibre
Most of the studies reported on dyeing of cotton with natural dyes are
mainly on use of different mordants, pre, post and simultaneous mordanting
techniques, standardization of dyeing condition, influence of pH on colour,
mordant mixing along with use of sonicator for optimum extraction technique.
Some important and recent ones are given below.
Deo and Desai (1999) dyed cotton and jute fabrics with an aqueous
extract of tea, containing tannins as the main colorant species. The dyeing was
carried out with and without metal salts as mordants, using three different
dyeing methods: pre-mordanting, meta-mordanting and post-mordanting. The
resulting wash and light fastnesses of the dyed fabrics were good to excellent.
The colour of the fabrics was investigated on computer colour matching
system in terms of K/S, and CIELAB colour-difference values. Deep shades
(K/S = 3.9) were obtained for jute in acidic media, while cotton fabrics got
dyed in medium depths (K/S = 2.0) under identical conditions of dyeing.
Gulrajani (2001) evaluated cotton dyeing by using various natural dyes
alone and in combination to yield six basic shades: blue, yellow, red, black,
green and fawn. These dyed fibers were then blended in various proportions
along with undyed cotton fibers and spun on a rotor-spinning machine to
produce 204 coloured yarns. The fastness properties of the six basic shades
were determined. The L*a*b* and L*C*h values of the yarns having 50%
dyed fibre and 50% un dyed cotton fibre was also determined. The values
were plotted to obtain the colour gamut of natural dyes on cotton yarns.
Teli et al. (2002) used water borne extracts of madder and tea to dye
cotton fabric using conventional single dip dyeing method with different
mordanting methods. The results were compared with a new method that uses
ferrous sulphate and tannic acid as mordants in a multiple dip process. Results
show that the multiple dip method was capable of producing deeper shades,
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uses less dye and indicates a potential for industrial use. Ferrous sulphate
mordant produced the deepest shades.
In a study by Samanta et al. (2003) cotton fabric was dyed with four
different natural dyes (turmeric, myrobolan, madder, red sandalwood) using
pre, post and simultaneous-mordanting techniques. Aluminium sulphate was
used as a mordant. Some samples were also dyed with a combination of
turmeric with madder or red-sandalwood and a combination of myrobolan
with madder or red sandalwood in different proportions. Selected mordanted
and dyed samples were after-treated with a cationic dye fixing agent. Turmeric
being a direct dye type, gave maximum colour strength when applied by the
simultaneous-mordanting method, either singly or in combination with other
dyes. Turmeric also showed poor wash fastness, which was improved to some
extent by after-treatment with a cationic dye fixing agent and on combination
of turmeric with other dyes of better fastness. Combined dye application of
turmeric with the other dyes by the simultaneous-mordanting method resulted
in a better shade development as the observed colour strength values were
always higher than the calculated or the expected values. However, myrobolan
on combination with other dyes gave higher colour strength when applied by
the post-mordanting method. In the case of the simultaneous-mordanting
method, myrobolan did not show a synergistic effect in terms of the observed
and calculated K/S values.
Garima et al. (2004) efficiently dyed cotton yarns with a plant dye,
Ornamental Mustard (Brassica juncea) using certain optimum variables.
Medium of dye extraction, wave length, extraction time, dye material
concentration, dyeing temperature, dyeing time, and dyeing pH were
standardized. Ornamental mustard leaves were extracted in aqueous, alkaline,
and alcoholic mediums, and the best color was obtained in the alkaline
medium. The results showed that the optical density increased with increased
extraction time up to 30 minutes, and further decreased with increase in
extraction time. The maximum dye absorption was observed at 7% dye
material concentration, and increased with increase in dyeing temperature. The
dye absorption also increased with increasing pH, and thus the optimum pH
selected for dyeing was 10. Thus, dye extraction in an alkaline medium with
optimum wave length of 360nm, extraction time 30 minutes, dye material
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concentration 7%, dyeing temperature 100°C, dyeing time 45 minutes, and

dyeing pH 10, gave excellent results for dyeing cotton yarns.
Study on cotton fabric using Eclipta as natural dye in both
conventional and sonicator methods has been reported byVankar et al. (2007).
The effects of dyeing showed higher color strength values obtained by the
latter. Dyeing kinetics of cotton fabrics were compared for both the methods.
The time/dye uptake reveals the enhanced dye uptake showing sonicator
efficiency. The results of fastness properties of the dyed fabrics were fair to
good. CIELAB values have also been evaluated.
Teli and Paul (2006) have highlighted the creative potential, non-
pollutant nature, and soft lustrous colors of coffee seed coat as a natural dye
enabling it to be used in eco-friendly dyeing of textiles. For the study natural
dye from coffee-seed coat was extracted for its application in dyeing cotton.
Dye extract and filtered after boiling coffee-seed coat in 5 liter water for 4
hours and kept overnight. Dyeing was carried out by pre-mordanting, meta-
mordanting and post-mordanting, using several mordants including myrobolan
and ferrous sulphate. The fastness properties of dyeing were satisfactory give
different tones and higher depth of dyeing. The result indicated that coffee-
seed extract develops a range of shades with good fastness properties on
cotton.
Lee (2007) extracted natural colorant from Coffea arabica L., using
water as extradant at 90°C for 90 min. Studies have been made on the dyeing,
color fastness, and deodorization properties of cotton fabric dyed with Coffea
arabica L. extract solutions, The best mordants were found to be FeSO4,
CuSO4, and SnSO4 for improving the color strength (K/S) of cotton fabric.
Perspiration fastness for mordants MnSO4, ZnSO4, and NiSO4 for cotton was
rated 3. It was found that cotton fabric dyed with the Coffea arabica L. extract
showed good deodorization performance.
Natural dye was extracted by Shanker and Vankar (2007) from
Hibiscus mutabilis (Gulzuba)/Cotton rose/ belonging to family Malvaceae for
dyeing cotton. Pretreatment with 2-4 % metal mordants and keeping M:L ratio
as 1:40 for the weight of the fabric to plant extract is optimum showing very
good fastness properties for cotton. Aqueous extract of Gulzuba flowers yield
25
shades with good fastness properties. It was concluded that the dye had good
scope in the commercial dyeing of cotton for garment industry.
Dayal et al. (2008) isolated natural dye from parthenium hysterophorus
weed and applied on cotton. The dye was extracted by boiling 1 kg weed with
10 liter water for 60 min at 95-98ºC. The study indicates that its aerial part
may be used for the isolation of dye in solid form (13%).The dyebath was set
with 4 gram per liter of dye with M:L ratio 1:100 at 95-98ºC for 60 minute.
Post mordanting method was used with common mordants like CuSO4, alum
and SnCl2.The dyed cotton fabric was immersed in mordant bath (0.5%) by
keeping M:L ratio 1:100 at 95-98ºC for 45 minute. which imparts a number of
shades on cotton with good fastness properties.
Indi & Chinta (2008) have studied application and properties of natural
dye phyllanthus reticulatus on cotton. Dye was extracted from the fruit of
phyllanthus reticulatus. Cotton fabric (M:L ratio 1:20) was premordanted with
alum (8%) and tannic acid (4%) at 80ºC for 1 hr. Same conditions was applied
for post mordanting. Dyeing was carried out for 10% shade at 80ºC for 45
minute at pH range from 3 to 7 followed by post treatment with soap 0.5 gpl
for 20 minute at 60ºC. It was concluded that colour obtained totally depends
on the type of mordant and method of mordanting used and pH conditions
Light fastness was poor for all application methods used in this experiment but
slight improvement was observed in post mordanting methods. overall wash
fastness for all application methods of dyeing remained same. Rubbing
fastness was very good for all the application methods.
Saha & Dutta (2008) have studied the use of marigold flower as floral
dye because huge amount of unsold flowers are wasted everyday. These unsold
flowers create a big problem for disposal as well as these can create environment
pollution also. These unsold flowers can be used for dyeing purpose for cotton
fibre and residuals after dyeing can be used as bio-fertilizers. In the study cotton
was mordanted before dyeing. For mordanting, low concentration of eco-friendly
mordanting agents: Alum, Copper Sulphate, Ferrous Sulphate, Stannous
Chloride were used. The mordanted samples were immersed in dye bath for 2
hour at a temperature range of 80ºC.After dyeing, soaping was done with 2g/l
non-ionic soap at room temperature for 10 minute, and then dried in shade.
Various shades of yellow, brown, grey and grey black were obtained using
26
different mordants. Good wash fastness properties were noted and so the
flowers were recommended for use in industry. This floral dye has no side
effects on skin and it has no harmful effect on environment also.
Vankar & Shanker (2008) studied ultrasonic dyeing of cotton with
Nerium oleander flower. The scoured fabric was soaked in clean water for 30
minute prior to dyeing and mordanting. Mordanting with metal salts such as
FeSO4, SnCl2, CuSO4, SnCl4, K2Cr2O7and alum was carried out at 60ºC for 30
minute. Cotton was then dyed with dye extract, keeping M:L ratio as 1:30 and
pH was maintained at 4 by adding buffer solution. It was concluded that
aqueous extract of nerium flowers yield cream to green to purple shades on
cotton fabrics with good fastness properties the colour strength (K/S value) were
good particularly for cotton mordanted by stannic chloride. The dye showed
good scope in commercial dyeing of cotton fabric for garment industry.
An attempt was made by Gahlot and others (2008) to optimize various
dyeing variables such as extraction medium, extraction time, dyeing time,
mordants concentration and methods of mordanting for dyeing of cotton with
jatropha flower dye. Four metallic mordants: alum, chrome, copper sulphate
and ferrous sulphate were taken in various concentrations. Dyeing was carried
out at optimized dyeing time (60 minute) and 4-6 pH. Various tones of peach,
brown and grey were obtained. The dyed materials had good colour fastness
properties also. The processing of dye materials was found to be easy as well
as safe from the point of environment.
An attempt was made to dye cotton with areca nut extract by Mhale
(2008). Mordanting was done by mixing two mordants in different
proportions. Alum + potassium dichromate, alum+ copper sulphate, alum+
ferrous sulphate, potassium dichromate + copper sulphate, potassium
dichromate + ferrous sulphate were used in 1:1,1:3 and 3:1 ratio. Mordant
combination was done in such a way that amount of mixed mordant did not
exceed 5grams per 100grams of cotton fabric. Shades obtained were light,
medium and dark rust, sand brown, brown, olive green and leaf green. It was
concluded that samples post mordanted with potash alum: potassium
dichromate 1:1 and 1:3 combinations had better fastness to sunlight, washing,
rubbing and perspiration in alkaline media. Simultaneously mordanted sample
with potash alum : copper sulphate 1:1 and potash alum: ferrous sulphate 3:1
27
combinations exhibited better fastness. Pre mordanted samples with potassium

dichromate copper sulphate 1:3 and copper sulphate: ferrous sulphate 1:3,
1:1 and 3:1 combination showed better fastness to sunlight, washing,
rubbing and perspiration. Areca nut dyed cotton post mordanted with
potassium dichromate: ferrous sulphate 1:1 combination gave excellent results
to colour fastness.
Prusti, et. al. (2009), have studied Terminalia catappa as a suitable
natural dye for cotton yarn. Process development for the extraction of natural
dye in pure form, from the waste leaves of Indian almond (Terminalia
catappa) and its application on different yarns have been carried out
successfully. Cotton yarn was dipped in mordant such as alum + turmeric,
ferrous sulphate, stannous chloride, copper sulphate, potassium dichromate.
The mordanted cotton yarn was dyed at 80ºC-90ºC. Golden yellow, slate gray,
pale yellow and brown colours were obtained. It was concluded from the study
that it was possible to obtain various intensities of colour shades for cotton
yarn by using a known quantity of isolated dye materials, which is not possible
in case of the traditional method.
Mukherjee et. al. (2009) studied modification of natural yellow dyes
for improvement of washing and light fastness. Cotton fabric was
premordanted with aluminium sulphate, zinc sulphate, copper sulphate,
magnesium sulphate, copper sulphate and sodium dichromate. Dyeing was
carried out at 90ºC for 45 minute with M:L ratio 1:20. Modifications of dyes
were performed using poly carboxylic acid (oxalic acid, tartaric acid citric
acid) and cyanuric chloride in liquid dye. Most of the natural dyes namely
Turmeric (Curcuma longa); Palas (Butca mnnosperma), Ganda (Tagetes
Erects) and shruh (Nyctanethes Arbortristis) are having poor to moderate
washing fastness and very poor light fastness owing to their inbuilt dye
structure. They contain -OH groups along with -OCH3 which intensify the
depth of shade according to t hei r increased numbers in one dye molecule.
These -OH groups are prone to metallic mordants to produce shades of
different tones. On the other hand, these groups are the common path way to
UV rays of sunlight and therefore, colour fades quickly due to a photo
chemical reaction. In this research work, attempts were made to block the -OH
groups of the dye with poly carboxylic acid for improvement of light fastness
28
along with improvement in intensity of color and washing fastness. It was

concluded that all yellow dyes having -OH group in their structure can be
improved for their washing and light fastness through modification of the dye
with Cyanuric Chloride. For controlling of tone of yellow, prior introduction
of -COOH group may be helpful. Further investigation in this regard is
necessary so that fast natural yellow with brighter hue and purity of tone can
be achieved.
Patel (2009)successfully dyed cotton in presence and in absence of
mordants in different hues and tones at various concentration levels of babool.
SnCl2, FeSO4, CuSO4 and mix of FeSO4, + CuSO4were selected for pre
mordanting. The sample were treated in mordant solution at boil for 1 hour
and then entered in the dyebath; in meta mordanting process mordanting and
dyeing was carried out simultaneously. The increase in the colour strength
value of cotton dyed with babool was possible with selection of metallic
mordants and varieties of shades were produced on cotton. Shade ranging from
cream to medium brown to dark brown can be readily produced on cotton
without mordants. Mixed mordant system (i.e. FeSO4, + CuSO4 ) was found to
be the best in pre mordanting method as far as the colour strength was
concerned while copper sulphate was found to be the best in case of
metamordanting technique. Thus selection of mordanting technique was found
to be equally important. Pre mordanting technique was found superior than
metamordanting technique. The all round fastness properties of various
samples dyed using exhaust dyeing method were adequate and quite
comparable with control dyed samples.
Process development for the extraction of natural dyes from the waste
leaves of jack fruit plant (Artocarphs heterophyllus) and their application on
cotton yarn have been carried out successfully by Purohit, et al (2009).
Cotton yarn was treated in the prepared mordant solution (alum + turmeric
powder) for 30-45 minute at 50-60°C. Then mordanted yarn was air dried
for 15 min. The mordanted cotton yarn was then treated in the dye bath for
45-60 minute at 90-95°C. The dyed yarn was left for 30 minutes for air
oxidation. The various fastness studies such as washing, rubbing, perspiration
and light fastness were undertaken. It was observed that the traditional way
of dyeing is a time consuming and laborious method, whereas the isolated
29
dye obtained from the waste leaves of Artocarphs heterophyllus and its
applications on textiles is economical, time saving and easy to handle. It is
possible to obtain various intensities of colours shades such as golden yellow,
maroon for cotton yarns, which are not possible in case of the traditional
method. Different shades in cotton yarn were obtained using the isolated
colouring materials. Further the present investigation deals with the waste
utilization of the natural resources.
Mahangade et al. (2009) extracted natural dye from the leaves of plant
namely (Maba angustifolia)known as Kalindrin in Malvanj. It was utilized for
coloration of cotton fabric. Two mordanting techniques were explored to
study their effect on the colour strength and fastness properties of the dyed
samples.
(a)The conventional mordanting technique consisted of a sequential
treatment with tannic acid followed by alum solution. In the above sequence
normal tap water as well as water modified with specific salts was employed
at both acidic pH(3.7) and alkaline conditions pH(11.6). Fabric was treated
with hot tannic acid (20% owf) for 1 h. followed by treatment in alum
solution (60% owf) for 30 min. at room temperature. The treated fabric was
washed with respective water employed for preparing the solutions and dried
at room temperature.
(b) In the modified technique the sequence adopted was alum, tannic
acid and the used alum solution. In the modified technique also normal tap
water as well as water modified with specific salts was employed at both acidic
pH (3.7) and alkaline pH (11.6) conditions. Fabric was treated with alum (60%
owf) solution for 30 minutes at room temperature, hot tannic acid (20% owf)
treatment for 1 hour, followed by treatment with used alum from the earlier
step for 30 min. Fabric sample was washed with respective water employed for
preparing the solutions and dried at room temperature.
Dyeing was carried out under acidic and alkaline conditions at different
temperatures. Colour strength and fastness properties were found to be superior
in the modified mordanting technique as compared to the conventional
mordanting technique.
Goel et. al. (2010)extracted dye from onion peels in acidic medium for
dyeing cotton. Metallic mordants(alum, ferrous sulphate and stannous
30
chloride) were used to enhance the colourfastness of the dyed cotton yarns.
Brown, rust green, dark green and golden yellow shades were obtained.
Colourfastness was evaluated against washing, rubbing, perspiration and light
according to ISO standards. It was concluded that for all the dyed yarns,
mordants improved the colourfastness properties.
Kulkarni et. al. (2011) studied dyeing of cotton with natural dye
extracted from Pomegranate (Punica granatum) peel. Accurately weighed
cotton cloth was treated with different metal salts cupric sulphate (2%) and
ferrous sulphate(2%).Three processes of mordanting were used: pre
mordanting, simultaneous mordanting and post mordanting. Dye concentration
was 4% and M:L ratio 1:40 at 80°C for 60minutes. After dyeing, the dyed
material was washed with cold water and dried at room temperature. The
fabric dyed with pomegranate peel gave different shades of yellow, brown and
black. The obtained results have shown the dyeing potential of pomegranate
peel as source for cotton dyeing. Good fastness was exhibited by the dyed
cloth mainly because of the mordants used. It was concluded that there is a lot
of scope to use pomegranate peel as dye for obtaining various color shades
using safe mordants under eco-friendly textile dyeing. The process of
production of pomegranate peel dye was found to be cost-effective as
compared to the cost of dyes in local market.
Srivastava et. al. (2012) found that the required scientific studies and
systematic reports on dyeing of textiles with natural dyes are still insufficient.
There are numerous natural products still unexplored and untouched. As a
result, more such studies need to be conducted. In this study, litchi peels were
utilized for imparting color on selected cellulosic fabrics. Dyeing was done on
the chosen fabrics with multiple trials, and by treating it like other vegetable
dyes to achieve satisfying results. A series of experiments were conducted to
determine the dyeing variables, such as extraction medium, optimum
concentration of dye material, extraction time, and concentration of mordants
and methods of mordanting. After the tests following recipe was finalized:
Dye materials: 5 gm
Water: 100 ml
Temperature: 60°C (as per the experiment conducted)
Time: 60 min. (as per the experiment conducted)
Mordants : FeSO4, alum and tannic acid, post mordanting 45 min. at 90 °C
31
During the study, a wide range of colors were obtained on jute

selected for the study. Mordants were capable of improving the shades and
the fastness in many cases. Litchi dye gave best fastness towards
perspiration, crocking and then towards washing, while just satisfactory
results for light fastness were achieved. However, it has been revealed in
many studies that light fastness of many natural dyes are found to be poor to
medium. From the obtained results, it was concluded that cellulose can be
successfully dyed with the discarded peel of litchi fruit, giving acceptable
fastness results, with or without mordants. Further researches can be done to
explore the possibility of dyeing with litchi dye on other textile materials.
Because only the discarded fruit peel was used for the purpose, its use will
have no adverse effect on the bio-diversity. Researcher and scientists thus
have a good opportunity to make pollution free environment by using these
source on textile materials, as the processing of these dyes involved no toxic
chemicals.
Jain (2013) extracted colourant from jamun leaves, bark, bark peel and
fruit and dyeing was carried out on cotton premordanted with natural mordants:
amar chal, arjun chal and babul barkat following conditions:
Dye extraction time : 45min.
Dye material concentration: 20ml/150mlof water
Mordanting time: 60 min.
Mordanting temperature: 60 ºC
Dyeing time: 60 min.
Dyeing temperature: 60-75ºC
Best shades on cotton fabric were obtained by using jamun leaves

mordanted with babul bark, jamun fruit mordanted with arjun bark and jamun
bark mordanted with amar stem gave good colour yield. Babul bark exhibited
good light and wash fastness. And amar stem exhibited fair to good light
fastness.
2.3.2 Natural dyes for protein fibre
Wool and silk are two important protein natural fibers obtained from
animal and insect. Extensive literatures have been reviewed on dyeing of wool
and silk with natural dyes. These studies mainly deal with dye extraction
process, extraction time, concentration of dye, dyeing time, method of
32
mordanting, shades obtaining and colour fastness properties. Some important

studies of natural dyes on wool and silk are summarised below.
The advent of natural dyes has necessitated search of new dye
sources and natural mordants. Keeping this in to consideration researchers
(Gill and Singh, 2002) conducted a study to optimize the process of dyeing
wool with gum from simal, Bombax ceiba Linn. syn. Bombax
malabaricum DC. and application of natural mordants. During experiment
natural dye was obtained by boiling 1g powder of the Semal bark in 50 ml
water at seven different pH values, i.e. 4,5,6,7,8,9 and 10 for 45 minutes.
natural mordants used for study were bark of arjun, Babool, Eucalyptus,
Indian Blackberry, Mango tree, fruits of Chebulic myrobalan and Indian
gooseberry and pomegranate fruit rind. These were used in dried and
powder form. The results showed that Semal dye could be used on wool in
combination with different natural mordants to produce different shades of
pink (grayish pale red to light maderia). All natural mordants helped in
increasing the colour strength of the dye on wool
Mathur and Gupta (2003) obtained natural mordant from concentrating
the aqueous solution extract of banana flower petaloide under reduced
pressure and evaporating it to dryness. Bharat merino sheep wool yarn dyed
with turmeric (Curcuma longa) was subjected to mordanting separating with
natural mordant and chromium under identical condition. Out of the different
concentration of the mordants used 3.5% natural mordant and 1.55 %
chromium on the weight of yarn show similar color fastness, reflectance, color
shade and K/S values. The chromium mordant in high concentration damaged
wool while natural mordant does not cause damage to wool. Since the nature
of turmeric colourant and banana petaloids is ecofriendly, their use in dyeing
and mordanting will not cause any harm to the environment.
Extraction of natural colourant from neem (Azadirachta indica) for
dyeing of wool yarn was studied by Mehtab et al. (2003). Neem bark
colourant showed two absorption maxima at 275 and 374 nm. Dyeing of wool
yarn under the optimum conditions (pH, 4.5; colourant conc., 0.05g per gram
of wool; treatment time, 60 min; and treatment temp., 97.5°C) showed very
good light and wash fastness properties without deteriorating the quality of
wool.
33
Paul et al. (2003) have described walnut bark as a good source of

brown colour and relatively eco friendly. Application process is easy and so
was found to be useful for rural population. Dyeing variables in using walnut
dye to dye wool were tested, and the colourfastness of selected dye on woollen
yarns was also investigated. Experiments were conducted to determine the
optimization of dyeing variables - medium of dye extraction, and optimization
of dye extraction time, dye concentration and dyeing time. Preparation of final
samples and colourfastness testing were covered. Walnut bark was found to be
a good source of brown colour, with a variety of fast shades using different
mordants.
Agarwal and Gupta (2003) discussed the conditions for dyeing of wool
with a vegetable dye from the roots of the herb Madder (Rubia cordifolia).
The optimized conditions included the concentration of dye, extraction time,
dyeing time, concentration of the mordants, and method of mordanting for
wool fibers. The dyed samples were subjected to tests for fastness to light and
washing. From optical density data, the optimum concentration of the dye was
found to be 5 grams per 100 ml of water, while the optimum extraction and
dyeing time were found to be 120 minutes and 90 minutes, respectively.
Simultaneous method of mordanting was observed to give the best results in
terms of luster, depth of shade, evenness of the dye, and the overall
appearance.
Detailed work on wool dyeing using reinwardtia flowers and poplar
leaves in the ratio of 50:50 each as natural dye was done by Garima et al.
(2004). Different variables viz. wave length, dye material combination, dye
extraction time, dye material concentration, dyeing time, pH and mordants
were standardized. 7% dye material, extracted and dyed for 45 minutes each
using 1% and 4% of copper sulphate, chrome and ferrous sulphate as
mordants gave excellent colours ranging from yellow ochre to military green.
The fastness grades in terms of washing as colour change were 3-4/5 and
colour staining from 3-5, light fastness from 3/4 to 4/5, rubbing fastness 4-5
and perspiration from 3/4 to 4/5. Hence the source explored was found
suitable for dyeing of wool.
Wool fabric was dyed with an aqueous extract from the bark of Acacia
pennata containing tannin as the major colourant by Shukla et al. (2000).
34
Dyeing with the combination of extracts of Acacia pennata and banana stem
has also been carried out and improvement in depth of colour without altering
the tone was observed. The colour of the fabrics has been evaluated on
computer colour matching system in terms of K/S and L* a* b* colour
coordinates. The dyeing shows moderate to good fastness to washing, light
and rubbing.
Bechtold et al. (2006) described that food and beverage industry
releases considerable amounts of wastes which contain natural dyes. Such
wastes could serve as a source for the extraction of natural dyes for textile-
dyeing operations. The extraction of brilliant yellow and red colours from
fruits and vegetables is of particular interest. Wastes, e.g. pressed berries,
pressed grapes, distillation residues from strong liquor production, and wastes
and peels from vegetable processing, have been extracted with boiling water
and test dyeing on wool yarn were performed. Colour strength, shade and
fastness properties of the dyeing have been tested. The extracts were applied
as direct dyes and in the presence of Fe+2and alum mordants. The results prove
the potential of such wastes as a source for natural dyestuff extraction.
Das et al. (2006) studied the application of dye obtained from Punica
granatum fruit rind on wool and silk fabric in the presence and absence of
environment-friendly mordanting agents. The dyeing of wool and silk with
pomegranate solution was found to be effectively accomplished at pH 4.0.
Pre- and post-mordanting employing ferrous sulphate and aluminium sulphate
improve the colour uptake, light fastness and colour retention repeated
washing. The use of such mordants, however, does not improve wash fastness
property of dyed substrates.
Bechtold et al.(2007) used the aqueous extract of ash-tree bark
(Fraxinus excelsior L.) as a model to study the shade reproducibility of dyeing
on wool. A meta-mordanting process using FeSO4·7H2O mordant was chosen
as a system with particular potential for industrial application. The exhaust
dyeing process with immediate use of the extracts as a dyebath and direct
addition of FeSO4·7H2O stock solution as a meta-mordant process showed
good shade reproducibility and satisfying levelness of the dyed material. An
increase of Fe+2mordant above a dyebath concentration of 2-3 gm did not result
in further colour depth. Extraction of 1-2 gm of bark was found sufficient to
35
dye 1 gm wool yarn to the darkest colour possible; use of higher amounts of
bark did not yield substantially higher colour depth. The quality of bark and
the extraction step were found to be of significant importance for the colour
depth; thus, in an optimized process, conditions of extract formation have to
be well controlled.
Koyuncu (2007) studied the dyeing of wool yarn using Rheum ribes
roots as natural dye in conventional method. The effects of dyeing show
higher colour strength values obtained by the latter. Dyeing with Rheum ribes
roots has been shown to give good dyeing results. The results of washing
fastness properties of the dyed wool yarn were fair to good. CIELAB values
have also been evaluated.
Lu et al. (2007) performed experiment on dyeing wool fabric with
sorghum red as natural dye by mordant dyeing method. The process
conditions of premordant and post-mordant dyeing were determined in
quadrature experiments. The experimental results were as follows: the
consistency of the dye was the key factor on dyeing depth in pre-mordant
process, the dyeing depth enhanced with consistency of the dye solution
increase; the pH value was the second factor that affected the depth, the depth
improved with the increase of pH value. The consistency of Fe2+ played an
important role in post-mordant dyeing process. The depth enhanced with the
increase of consistency of Fe2+. The depth improved with the temperature
rising. The rubbing and washing color fastness of dyed wool fabric were all 4
or up to 4. It indicated that sorghum red dye was suitable to dye wool fabric.
Javalakshmi. and Amsamani (2008) applied annatto and catechu for
dyeing wool using bio-mordants. The method of dyeing woollen yarn with
annatto and catechu was standardized by determining the optimum dyeing
conditions, namely dye material concentration, dye material extraction time,
dyeing time, mordant concentration and mordanting method. Two bio
mordants namely myrobalan and karavelum bark were used in 1%
concentration and two natural fixing agents such as liquor of tamarindus
indica linn. and boiled off liquor of green tea were used. Dye extracted from
annatto and catechu were soaked 24 hours in aqueous medium. Mordanting
and dyeing was carried out at room temperature for 30 minutes. Fixing
treatment was given at room temperature for 10 minutes. The washing,
36
rubbing, light and perspiration fastness of the dyed samples was evaluated,
giving fair to excellent fastness grades. Hence, an attempt by using natural
Bio-Mordant and natural fixing agent has achieved both good wash fastness
and good fastness to light.
An attempt was made by Gahlot et. al. (2008) to optimize various
dyeing variables such as extraction medium, extraction time, dyeing time,
mordants concentration and methods of mordanting for dyeing of wool and
silk with jatropha flower dye. Four metallic mordant alum, chrome, copper
sulphate and ferrous sulphate were used in various concentrations. Dyeing was
carried out at optimized dyeing time (60 minute) and 4-6 pH. Various tones
of different colours like peach, light peach, light brown and grey shade were
obtained. The dyed materials had good colour fastness properties also. The
processing of dye materials was easy as well as safe from the point of
environment.
Comprehensive dyeing of wool using natural sources in alkaline
condition was done by Raja, (2008). Fine wool from Bharat Merino sheep was
dyed with seven different natural resources such as tanners senna bark, silver
oak leaves, wattle myrobolan bark, myrobolan, carrot leave, indigo, and
catechu at different pH conditions with different mordants(alum, aluminium
sulphate, stannous chloride, ferrous sulphate, potassium dichromate) using
post-mordanting technique. The shades obtained were grey, brown, yellow and
light green with moderate high washing fastness. Selected dyed samples were
tested for bundle strength to know the effect of alkaline pH on dyeing and
concluded bundle strength was reduced. It was also concluded that wide range
of shades except pure red and green can be developed using the above listed
natural sources and mordants using the same recipe. If the pH conditions are
changed probably more shades can be developed for wool in all cases fastness
was satisfactory.
Optimization of dyeing procedure on wool yarn with Pistacia
integerrima leaves dye using synthetic(alum, copper sulphate, stannous
chloride) and natural mordant (Alnus nepalensis) was studied by Badoni
(2009). Premordanted marino wool sample was treated in dyebath at room
temperature for 45 minute. New colour shades like grey, yellow, dark golden,
steel blue was obtained. He concluded that P. integemma (leaves) have
37
excellent dye property and can be utilized for commercial purposes. However
a number of color shades were obtained with different mordants that were
found stable against light and washing factors. Moreover the sample dyed with
natural mordant was safer and eco-friendly and can be a source of mordant in
textile industry.
In the study by Karolia (2010) dyeing of wool was done with natural dye
extracted from bark, leaf and fruit of walnut tree. From the study an interesting
aspect was obtaining, an array of colors which could be easily done by varying
different mordants (alum, copper sulphate, ferrous sulphate, tannic acid, tea,
coffee, Pomegranate) and with change of pH. It was concluded that the colors
produced by natural dyes- Walnut are interesting and attractive due to tonal
effects created by them. Bark dyed samples had mixture of yellow and green.
Strong presence in the red and yellow quadrant was observed in acidic and self
pH. In leaf dyed samples the shades obtained in self, alkaline pH were mostly
green and yellow. In fruit dye, red – yellow was the dominant color quadrant.
All the three pH gave mild shades and a strong presence of brown, showing
the more of red being present. All colors showed fair to excellent wash, rub
and light fastness properties.
Khan et.al., (2010)extracted natural dye from Acacia catechu. This dye
was used for dyeing mordanted wool with eco-friendly mixture of mordants
(Iron and Tin). By using different permutations and combinations of mordants
with cutch, forty eight shades were developed. Fastness properties (light ,wash
and rub/crocking) were studied on these samples. It was concluded that by
changing the concentration of the dye and mordants, shade variation in wool
sample were observed. Most of the dyed wool samples had fairly good to good
fastness rating. It was concluded from the study that cutch can be used as an
ecofriendly natural colourant for dyeing woolen yarn.
Khan et.al.,(2012)concluded that the colourant extracted from henna
leaves was found to possess acceptable dyeing performance and produced
orange yellow to reddish brown shades on woolen yarn. Dyeing was carried
out by using 1%, 5%, 10% and 20% of dye concentrations. Material to liquor
(M:L) ratio was kept 1:40 maintaining neutral pH (7) at 30°C.Thirty six
shades with appreciable change in hue and tone were obtained by varying
mordant combinations as well as dye concentrations. Dyeing of wool with
38
extract of henna leaves in the absence of mordent, displayed good light

fastness, good to very good wash fastness but moderate fastness to rubbing.
Mordanting with mixed mordant (5% alum + 2.5% iron and 2.5% iron+0.5%
tin) does not have any significant effect on fastness property, depth of shades
for both unmordanted as well as mordanted woolen yarn follow a commonly
increasing trend with increasing concentration of dye. Dyeing on mordanted
woollen yarns showed high colour strength which displayed good all-round
fastness properties. It was also concluded from the study that extract of henna
leaves applied on woollen yarns mordanted with mixed metal mordants can
successfully be used to obtain a range of soft and soothing shades on woollen
yarns.
Kaur et al. (2012) investigated the use of green tea as a natural
colourant for dyeing of wool with good fastness results. The dyeing process
was carried out with dye extracted from three different qualities of tea leaves
using three solvent (Methanol, Acetone, Acetonitrile ). Washing fastness, light
fastness, K/S and reflectance was measured. Colour yield and washing
fastness properties are moderate to good, where as light fastness rating varies
from 3-6.
In the study by Srivastava et al. (2012) litchi peels were utilized for
imparting color on wool fabrics. Dyeing was done on the chosen fabrics with
multiple trials, a series of experiments were conducted to determine the dyeing
variables, such as extraction medium, optimum concentration of dye material,
extraction time, and concentration of mordants and methods of mordanting.
After the tests following recipe was finalized:
Dye materials : 5 gm
Water: 100 ml
Temperature : 60°C (as per the experiment conducted)
Time: 60 min. (as per the experiment conducted)
Mordants : ferrous sulphate, alum and tannic acid
Mordanting: Post mordanting for 45 min at 90 °C
During the study, a wide range of colors were obtained on wool
fabric. Mordants were capable of improving the shades and the fastness in
many of the cases. Litchi dye gave best fastness towards perspiration,
crocking and then towards washing, while just satisfactory results for light
fastness were achieved. However, it has been revealed in many studies that
39
light fastness of many natural dyes are found to be poor to medium. From
the obtained results, it was concluded that wool fabric can be successfully
dyed with the discarded peel of litchi fruit, giving acceptable fastness
results, with or without mordants.
Dyeing of woolen yarn with lac dye has been studied using ferrous
sulphate, stannous chloride and their combination by Mohammad et.al.,
(2012). Eco-friendly mordants (5% Fe, 1% Sn) and their combination (2.5%
Fe + 0.5%Sn) on the depth of shades, colour values and fastness properties
of woolen yarns dyed with lac dye were measured. The temperature of
mordant bath and dye bath was 91-93ºCwith M:L ratio was 1:40. It was
concluded that application of lac dye on wool substrate produces a range of
fifty four shades varying from light orange-bright red-dark scarlet
depending on the amount of lac dye, eco-friendly mordant and their
combination used. Very good light fastness, good wash fastness and
moderately good to good rubbing fastness properties were obtained.
Devi et al. (2002) identified Eclipta prostrata, a common weed found
in most of the fields in Andhra Pradesh as a good source of natural dye for silk
for production of green shades. Alkaline medium was suitable for extraction
of dye from the plant and pleasant yellowish-green shades were obtained on
silk. The extraction and dyeing procedures were standardized based on the
optical density before and after dyeing silk and visual appearance judged by a
panel of 30 scientists. All four mordants namely alum, chrome, copper
sulphate and ferrous sulphate were found to be suitable for application on silk.
15% and 20% of alum, 3% of chrome, 2% of copper sulphate and 1 and 2%
of ferrous sulphate were found to produce fast yellowish green shades on silk.
Mostly dark shades were obtained by post mordanting method, followed by
simultaneous and premordanting methods. Exposure to alkali had either
deepened the hue or added green tinge to the silk samples when subjected to
washing and alkali perspiration. Loss of colour was found with acidic
perspiration. Excellent to outstanding fastness to sunlight was found in all
mordanted samples. There was no absolute staining for washing. Colour
change was not found in samples subjected to crocking in dry and wet
conditions. Only slight staining was found. This dye can easily be
recommended for use on silk fabrics for producing light green shades.
40
Phukan and Phukan (2004) standardized the condition of dyeing

mulberry silk yarn with the bark of Arjun tree, Terminalia Arjuna. Mordants
such as alum, chrome, copper sulfate, and ferrous sulfate were used for the
study for the fixation of the dye molecule with the fiber. To remove the
sericin, degumming was done before dyeing, with washing soda, alkaline and
acidic methods were employed for dye extraction. Alum mordant and pre-
mordanting method showed the best results in both alkaline and acidic
medium of dye extraction. Yarns dyed with Arjun dyes showed color fastness
to washing, rubbing, light, and perspiration.
The natural dyes which were selected for the study by Grover et al.
(2005)included Jatropha, Lantana, Hamelia, Euphorbia, Kilmora, and Walnut.
Silk was initially degummed prior to dyeing, to make the fabric free from
sericin, which obstructs the penetration of dyestuffs into the fiber. A series of
experiments were conducted to determine the dye-extraction medium,
optimum concentration of dye, extraction time, dyeing time, mordant
concentration, and methods of mordanting. The acidic media exhibited
maximum percent absorption for Jatropha, Lantana, Hamelia, and Euphorbia
dye, while Kilmora and Walnut dye showed good results in alkaline medium.
The results obtained from different experiments lead to the optimization of a
standard recipe for dyeing of silk with each dye source.
Silk yarn was dyed with Peach leaves by Mahajan et al. (2005)using
six combinations of mordants namely Alum/ Chrome, Alum/ Copper
Sulphate; Alum/ Ferrous Sulphate; Chrome/ Copper Sulphate; Chrome/
Ferrous Sulphate and Copper Sulphate/ Ferrous Sulphate in the ratio of 1:3, 1:1
and 3:1. Dyeing was carried out according to the optimized dyeing conditions,
which were standardized beforehand. These optimized conditions were dye
extraction time, dye concentration, dyeing medium, dyeing time etc. The
dyeing was done using these optimized conditions and the abovementioned six
combinations in three ratios with three mordanting methods namely pre,
simultaneous and post mordanting. This resulted in a total of 54 shades. The
dyed samples were then evaluated for colour fastness to washing, light,
rubbing and perspiration fastness according to ISO standards. On evaluation it
was concluded that silk dyed with Peach leaves showed excellent washing
41
fastness except for few samples, very good light fastness and fair to good
rubbing and perspiration fastness.
Ukalkar and Karanjkar (2005) optimized dyeing variables of silk by
using flame of forest flowers (Butea monosperma). The petals were selected
as a dye source and were removed when the flowers were fresh and dried
under shade. Optimization of dyeing silk comprised of optimization of dye
material concentration, dyeing time and concentration of mordant. Based on
percent dye absorption and visual appearance, aqueous medium was found to
be most suitable for extraction of dye. The percent absorption increased with
the increase in the concentration of flower petals from 1-5g and maximum
percent absorption by 1 g of silk was obtained with 5g dye/100ml water. On
the basis of percent dye absorption, optimized dye extraction time was 30
minutes, as optical density value was around 0.3. Higher dye absorption time
was found after dying silk for 30 minutes. The 0.3 percent concentration of
copper sulfate and ferrous sulfate, and 0.15 percent of alum gave higher
percent dye absorption values in the three methods of mordanting.
Rawat et al. (2005) studied the application of poinsettia leaf dye, an
environmental friendly natural dye, on silk fabric. The fastness properties
were found satisfactory. Silk fabric, which was degummed using a solution of
genteel and water, was dyed with poinsettia leaves and the dyed fabric was
subjected to color fastness testing. During the colorfastness test, the samples
were washed in a Laundrometer for 45 minutes at a constant temperature of
50° C. The colorfastness of the dyed samples to acidic solution was found
much better than the alkaline solution. The dye may be useful in imparting
number of fast shades on silk using common mordants such as FeSO4 and
CuSO4 with good fastness properties except alkaline perspiration.
Sudhakar et al. (2006) extracted natural dye from the nuts of Areca
catechu grown abundantly in India and utilized for coloration of silk fabric.
Different mordants at varying concentrations were used on silk for pre-
mordanting to study their effect on the colour value and fastness properties of
the dyed samples. Silk fabrics were also dyed with different mordanting
techniques using lowest concentration of mordants. Colour values with respect
to K/S, L* a* b* and fastness properties were found to be influenced by the
42
type of mordant and technique of mordanting with very low concentrations of

the mordant.
An attempt was made to extract natural dye from coffee-seeds for its
application in dyeing silk by Teli and Paul (2006). Dye extract was filtered
after boiling the coffee-seed coat in 5 liter water for 4 hours and kept
overnight. Dyeing was carried out by pre-mordanting, meta-mordanting and
post-mordanting, using several mordants including myrobolan and ferrous
sulphate. The fastness properties of dyeing are continuously achieving the
range of satisfactory level and give different tones and higher depth of dyeing.
The result indicated that coffee-seed extract develops a range of shades with
good fastness properties on silk.
Lee (2007) extracted natural colorant from Coffea arabica L., using
water as extradant at 90°C for 90 min. Studies were made on the dyeing, color
fastness, and deodorization properties of silk fabric dyed with Coffea arabica
L. extract solutions, The best mordants were found to be FeSO4, CuSO4, and
SnSO4 for improving the color strength (K/S) of silk, fabric
MnSO4showedrating of 3. It was found that FeSO4 and CuSO4 were the best
mordants for the improvements of color strength (K/S) and light fastness for
silk fabric. In addition, it was found that silk fabrics dyed with the Coffea
arabica L. extract showed good deodorization performance.
Shanker and Vankar (2007) extracted natural dye of Hibiscus mutabilis
(Gulzuba)/Cotton rose belonging to family Malvaceae which was used for
dyeing textiles. Aqueous extract of Gulzuba flowers yielded shades with good
fastness properties.. In the present study dyeing with gulzuba has been shown
to give good dyeing results. Pretreatment with 2-4 % metal mordants and
keeping M:L ratio as 1:40 for the weight of the fabric to plant extract is
optimum showing very good fastness properties for silk. The dye has good
scope in the commercial dyeing of silk for garment industry
Sharma et al. (2007) explored the herbaceous plant Eupatorium
adenophorum as a very good green color source for dyeing of silk yarn with
excellent fastness properties. Leaves of the Eupatorium plants were collected
and shade dried, crushed and packed. Sericin was removed from silk fabric so
as not to interfere with luster and dye absorption. The dye material was
entered into the dye liquor and boiled. Four mordants were used with three
43
methods of mordanting. A mordant ranged from 1-5% was selected for the
study. The concentration of dye material was optimized by taking seven
concentration prepared by boiling. Yarn was dyed in the dye bath for varying
time. The time at which the absorption high was selected as optimum dyeing
time and then evaluated for color fastness. Results show that 10% alum with
post mordanting method has yielded yellowish green shade while with 4%
chrome in pre-mordanting sap green color has been obtained. Light army
green and dark army green shades on silk were obtained with 4% CuSO4 and
4% FeSO4 using post-mordanting method. Excellent fastness to light and
outstanding fastness to washing was shown by dyed silk yarn using 4%
chrome. Little noticeable staining and color change was found for dry and wet
crocking samples.
Vankar and Shanker (2008) studied ultrasonic dyeing of silk with
Nerium oleander flower. Mordanting with metal salts such as FeSO4, SnCl2,
CuSO4, SnCl4, K2Cr2O7and alum was carried out at 60ºC for 30 minute. Silk
was dyed with dye extract, keeping M:L ratio as 1:40 and pH was maintained
at 4 by adding buffer solution. It was concluded that aqueous extract of nerium
flowers yield cream to green to purple shades on silk fabrics with good fastness
properties the colour strength (K/S value) were good particularly for silk
mordanted by ferrous sulphate. The dye showed good scope in commercial
dyeing of silk fabric for garment industry.
Sidhu and Jastesh, (2008) studied silk dyeing with Goldendrop
(Onosma echioides) dye.Dyeing of silk was done using four mordants namely
alum, chrome, copper sulphate and ferrous sulphate in three concentration
each. For 100 gram degummed silk 5,10,15 grams alum and 1,2,3 gm chrome,
copper sulphate and ferrous sulphate were used. Optimum dye: material
concentration was 1gm/1gm silk. Dyeing was carried out at room temperature
for 45 minute. It was found that goldendrop dye can be successfully used for
dyeing of silk to obtain a wide range of soft, pastel and bright colours such as
olive green, light and dark grey, brownish, bronze and blackish brown. With
regards to colour fastness test, samples exhibited excellent fastness to
washing; poor to fairly good fastness to light; fair to excellent fastness to
rubbing and good to excellent fastness to perspiration in both acidic and
alkaline medium.
44
Prusti, et al (2009), have studied Terminalia catappa as a suitable

natural dye for silk yarn. Process development for the extraction of natural dye
in pure form, from the waste leaves of Indian almond (Terminalia catappa)
and its application on different yarns have been carried out successfully. Silk
yarn was treated with mordant such as alum, turmeric powder, alum +
turmeric powder, ferrous sulphate, stannous chloride, copper sulphate,
potassium dichromate; then mordanted silk yarn was dyed at 80ºC-90ºC.
Golden yellow, slate gray, pale yellow, brown colour shades were obtained. It
is possible to obtain various intensities of colour shades for silk yarn by using
a known quantity of isolated dye materials, which is not possible in case of the
traditional method. Different colour shades have been achieved for silk
materials using different mordants.
Washing fastness of natural colourant is comparatively low so attempt
was made to improve the fastness properties of natural dyes with the help of
mordant on silk fabric by Sundrarajan et. al. (2009). Three natural colourant (
Hibiscus flower, Onion skin, and Eucalyptus bark) were selected for dyeing
silk fabric and fastness was improved with the use of synthetic mordants:
Alum, copper sulphate and potassium dichromate and natural mordant:
Pomegranate rind and tannin. Dyeing was done at optimized condition ( 6%
dye solution at 80ºC for 45 minute). Combinations of two and three mordants
were also used. Yellow brown and green shades were obtained on silk fabric.
It was concluded that premordanted fabrics produced good dye uptake and
wash fastness than the unmordanted fabric. Two and three combinations
mordanted fabrics produced better dye uptake and also better washing fastness
than single mordanted and unmordanted fabrics. Three colorants produced
better improvement in washing fastness property with tannin and
pomegranate mordants. Combinations of two and three mordants gave almost
same results.
Abu Sayeed et al. (2009) isolated natural dye (2-hydroxy 1,4
napthoquinone) from the leaves of Lawsonia Inermis Linn. The dye was
characterized by chemical analysis and spectroscopic analysis like FTIR,1H
13
NMR and C NMR. The isolated dye was applied on degummed silk fiber
with alum mordant at 80ºC and pH-3 for 60 minute in M:L ratio 1:40. The
colour of dyed silk was deep orange yellow. It was concluded that leaves of
45
heena contain extractible dye constituents which is more than 0.923%on the
wet basis. Dyeability of degummed silk fiber with dye was very good in
aqueous medium. The colour of dyed silk fabric was pleasant and fast to
sunlight, detergent wash, organic acid and alkalis.
Process development for the extraction of natural dyes from the waste
leaves of jack fruit plant (Artocarphs heterophyllus) and their application on
silk yarns have been carried out successfully by Purohit, et al (2009). Silk
yarns was premordanted with alum, alum + turmeric powder, alum + NaNO2,
alum + FeSO4, alum +(NH4)2SO4, alum + K2Cr207 for 30-45 minute at 50-
60°C,then air dried for 15 minutes. The mordanted silk yarn was then dyed for
45-60 minute at 50-60°C with extract from leaves of jack fruit plant. The
dyed yarn was left for 30 minutes for air oxidation. The various fastness
studies such as washing, rubbing, perspiration and light fastness was carried
out. It was observed from the above experiments that the traditional way of
dyeing is a time consuming and laborious method, whereas the isolated dye
obtained from the waste leaves of jack fruit plant and its applications on
textiles is economical, time saving and easy to handle. It is possible to obtain
various intensities of colours shades such as golden yellow, orange yellow,
maroon, slate grey, chocolate, brown for silk yarns, which are not possible in
case of the traditional method..Further the present investigation deals with the
waste utilization of natural resources.
Goel et. al. (2010) extracted dye from onion peals in acidic medium for
dyeing mulberry and tussah silk. Metallic mordants(alum, ferrous sulphate and
stannous chloride) were used to enhance colourfastness of dyed silk yarns.
Brown, rust green, dark green and golden yellow shades were obtained.
Colourfastness was evaluated against washing, rubbing, perspiration and light
according to ISO standards. It was concluded that for all the dyed yarns,
mordants improved the colourfastness properties.
Waste leaves of Tectonagrandis as a suitable natural dye for textile has
been studied by Prusti et. al. (2010). Process development for the extraction of
natural dye from the waste leaves of teak plant (Tectona grandis) and their
application on silk yarns has been carried out successfully using following
condition. Silk yarn (0.5 g) was treated in 20 ml of prepared mordant solution
46
at 1:30 MLR (material to liquor ratio) at 60-70 °C for 30-45 min. Then the
mordanted yarn was air dried for 15 minutes.
Light salmon and maroon colour shade for silk yarns has been
achieved using the isolated colouring materials. The dying experiments were
carried out adopting premordanting technique using different parameters with
silk yarns. It was observed that the isolated colouring material produces
excellent shade on silk yarn. The solvent used for the extraction process can
be recovered and reused for subsequent extraction. They concluded that the
dyeing procedure is time saving and economical as compared to the traditional
way of dyeing. In this method, it is possible to obtain various intensities of
colour shades for silk yarns by using known quantity of dye materials, which
is not possible in case of the traditional method. It is also observed that
different shade: light salmon and maroon are achieved without any mordant.
while, brick red, brown, golden red, slate grey and olive were obtained by
different mordents.
Kumaresan et al. (2011) studied application of eco-friendly natural dye
on silk using combination of mordant such as myrobolan+nickel sulphate,
myrobolan+aluminium sulphate,myrobolan+potassium dichromate,myrobolan
+ferrous sulphate, myrobolan+stannous chloride. They found that flower of
Cordia Sebestena can be successfully used for dyeing of silk to obtain a wide
range of soft and light brown shade by using combination of mordants; with
regards to colour fastness, test samples exhibited excellent fastness to washing
(except for pre‐mordanting using myrobolan + Potassium dichromate
combination); excellent fastness to rubbing (except for pre‐ mordanting using
Myrobolan + Potassium dichromate combination); good to excellent fastness
to perspiration in both acidic and alkaline media and fairly good fastness to
light.
In the study by Rastogi & Rastogi (2012) one co-friendly dyeing with
ayurvedic herbs on silk fabric revealed that sandalwood and manjistha gave
good colour on silk fabrics, while sandalwood and neem gave good
colorfastness on silk fabrics. On the other hand alum produced very even and
deep shades on fabric in comparison with MgCl2. Ironing and washing
fastness of all the dyes on silk fabrics with all mordants gave excellent results.
Light fastness of sandalwood and neem gave better fastness as compared to
47
Sandalwood and manjistha. Rubbing fastness of all herbs was found very good
to excellent. Thus it was concluded that alum could be used as a better
substitute for MgCl2 to improve colorfastness of Ayurvedic herbs.
2.3.3 Natural dyes for polyamide fibre
Nylon is synthetic fiber containing amide link known as polyamide

fiber. Literature has been reviewed has shown limited studies on dyeing of
nylon with natural dyes. Studies mainly deal with extraction process, dyeing
process, method of mordanting, shades obtained and colour fastness
properties. Some important studies of natural dyes on nylon are presented
below:
Gulrajni (2001) demonstrated possibilities of nylon dyeing by using
vegetable dyes like Annatto, Ratanjot and Berberine. Furthermore evaluation
of sample fastness and colour value was undertaken. Anlab Colour Space plots
for each dye was prepared by plotting their a*b* values. K/.S values were
discussed and the percentage exhaustion dye absorbance reported. Wash
fastness was good for Rajantot, very good for Annatto and poor for Berberine.
Light fastness values were included. Nylon could be dyed with these vegetable
dyes at pH 4 (Rajanjot), 6 (Annatto) and 9 (Berberine). Good to moderate light
and wash fastness resulted.
Gupta (2004) purified two components of Indian madder, purpurin
(1,2,4-trihydroxyanthraquinone) and munjistin (1,3-dihydroxy-2-
carboxyanthraquinone) and dyed nylon fabric with these two component. The
light and wash fastness of dyed and mordanted samples has been studied.
Purpurin showed much better resistance to photo fading than munjistin. It was
found that the type of mordant and the method of mordanting significantly
affected the rate and extent of photo fading. The use of copper or ferrous
sulphate gave high resistance to fading, whereas stannous chloride or alum did
not. On the other hand, light fastness was improved when post mordanting
was conducted with copper or ferrous iron, but pre-mordanting was superior in
the case of stannous chloride and alum.
Mashaly (2006) studied dyeing of nylon fabrics using lac as a natural
dye in both conventional and ultrasonic techniques. The extractability of lac
dye from natural origin using power ultrasonic was also evaluated in
48
comparison with conventional heating. The results of dye extraction indicate

that power ultrasonic is rather effective than conventional heating at low
temperature and short time. The effect of dye bath pH, salt concentration,
ultrasonic power, dyeing time and temperature were studied and the resulting
shades obtained by dyeing with ultrasonic and conventional techniques were
compared. Colour strength values obtained were found to be higher with
ultrasonic than with conventional heating. The results of fastness properties of
the dyed fabrics were good to very good. Dyeing kinetics of nylon fibre with
lac dye using conventional and ultrasonic conditions was compared. The
time/dye-uptake isotherms revealed enhanced dye-uptake in the second phase
of dyeing (diffusion phase). The values of dyeing rate constant, half-time of
dyeing and standard affinity and ultrasonic efficiency have been calculated
and discussed.
Two different natural dyes extracted from vegetable sources, namely:
Calendula and Casuarina. were selected by Mohamed (2009) and applied as a
dye on polyamide fibre, i.e. nylon 6 successfully. He concluded that the
behavior of natural dyes during dyeing of nylon fabric was similar to that of
acid dyes. The rate of dyeing was found to increase as the temperature,
increased till it reached its maximum at boiling for the two applied natural
dyes. Temperature breaks down the aggregate of dyes and increases their
solubility as well as opening up the fibre structure and thus accelerates the
diffusion of dye molecules inside the fibre. The pH of dyeing was found to
play a great role since maximum colour strength was achieved at strong acidic
medium which may be attributed to the high electrostatic attraction between
positively charged basic groups in the nylon fibre and the dye anions.
Teli et al. (2010) have studied dyeing of nylon with natural colourants,
the research mainly focuses on application of natural dyes such as turmeric,
madder, catechu, Indian rhubarb, heena, tea and pomegranate rind on nylon.
Three different methods of application namely pre-mordanting, meta-
mordanting and post-mordanting were used in which case contribution of
copper sulphate, ferrous sulphate, Potassium dichromate and Tannic acids was
studied in terms of enhancement in depth of dying. These dyes have affinity
for nylon and bright deep shades of yellow, grey, and black were obtained.
They concluded that most suited mordants in general are ferrous sulphate and
49
tannic acid. Moreover, toxicity of ferrous sulphate as compared to copper sul-

phate and potassium dichromate is very less and tannic acid is also
biodegradable in nature. Therefore in other words the process of dying of
synthetic fibers with selected natural dyes has potential of becoming
environmentally safe process.
2.3.4 Natural dyes for printing
Tawfik (2002) explained the suitability of turmeric in the fine powder
form as natural dye in printing cotton, polyester and their blended fabrics
using pigment-printing technique. Variable studied included concentration of
the colour, nature of thickening agent, type of fixation and pH of the printing
paste. The printed goods were evaluated by measuring the K/S and the overall
fastness properties. The data obtained indicated that regardless of the nature of
the fabrics used, type of fixation or of the time elapsed before commencing
printing, the K/S increased by increasing the concentration of turmeric and/or
decreasing the pH to 6.3. Thermo fixation is more suitable than steaming. It
can be concluded that turmeric can be used as natural dye for printing
successfully.
Maulik and Mandal (2010) reported printing of handloom cotton fabric
with vegetable colourants in presence of different inorganic salts, like
aluminium sulphate, ferrous sulphate and copper sulphate and to assess
different colourfastness properties of printed textile. Camellia sinensis (tea
leaf), Allium cepa (onion skin), Tagetes erecta (marigold flower) and Butea
monosperma (palas flower) were used as vegetable colourant. Aqueous
solution was prepared by adding 50 g of dried vegetable matter boiled for 60
minutes, allowed to stand for 15 minutes and filtered through nylon bolting
cloth. Evaporated water was replaced by fresh water. Dyeing was carried out
by pad-dry technique at nearly 100% wet pick-up in a laboratory model two
bowl padding mangle. The impregnated fabrics were then dried at room
temperature before printing. Printing of cotton fabrics treated with natural
colourant was carried out with the help of print paste containing inorganic
salts (5 g/l) and gum indulka thickener. The impressions were made with the
help of wooden blocks of various designs. After printing the fabrics were dried
at room temperature, followed by steaming for 15 minutes at a temperature of
102ºC in a cottage steamer. After steaming the printed fabrics were
50
immediately washed with 2 g/l non-ionic detergent at 60ºC for 10 minutes in

order to remove gum and the strong mineral acid (sulphuric acid) produced
during the steaming process. After soaping the printed fabrics were washed
with hot water, followed by cold wash and finally dried in air. It was
concluded that in presence of different inorganic salts with the objectives of
achieving an improvement in the fastness properties of the printed materials,
making them higher performing and enhancing scope for their use in different
value-added niche handloom products. Ferrous sulphate, aluminium sulphate
and copper sulphate when used as inorganic salts produce most balance
improvements in colourfastness of the printed cotton fabrics.
In the study by Jayalakshmi and Varshitha (2010)bleached woven
organic cotton fabric was block printed with vegetable dyes and treated with
mintage wash, crushing process and gulf voll wash to adhere strongly,
improve the general appearance of the fabric and impart wrinkled effect to
organic cotton fabric. Vegetable dyes were extracted by combination of carrot,
beetroot and red cabbage each of 200 gms were taken, boiled, smashed and
added in 1:40 ml of M: L ratio maintaining a temperature of 60ºC for a
duration of 1 hour. Later it was dried, filtered and the thick dye solution was
extracted. Printing paste was prepared by mixing one kg of binder, two gms of
prepared thick vegetable dye colour. On the previous day of printing, hundred
gms of gum were diluted with 4-5 liters of water in a big trough so as to make
the water into a thick viscous solution. Later, a minimum amount of three gms
of binder was mixed with this diluted gum solution. The binder acts as the
medium which is sometimes replaced by kerosene. The ratio of binder to
kerosene is 1: 8 for good quality of print. Printing operation was carried out at
room temperature following the block printing procedure. The treated organic
cotton fabric was converted into garment and wear study revealed that it was
comfortable during wear, without creating any irritation to the skin.
Maulik and Biswas(2011)research on dyeing and printing of jute
yarn/fabric with Camellia sinensis (tea leaf), Tagetes erecta (Marigold), Rubia
tinctorum (Manjistha), Cedrela toona (Mahogany), Terminalia chebula
(Harda) and Acacia catechu (Khair) in absence and presence of different
inorganic salts with the objectives of achieving an improvement in the
fastness properties of the printed materials, making them higher performing
51
and enhancing scope for their use in different value-added jute diversified
products. Extraction was done by adding 100 g of each vegetable matters to
one liter of water. The mixture was stirred, heated and kept at boiling point for
45 min, allowed to stand for 15 min and finally filtered through nylon bolting
cloth. Dyeing of jute with vegetable colour in absence of inorganic salt at a
material to liquor ratio of 1:20. The dye bath temperature was kept at 800C for
45 min. The dyed materials were then washed with 2 g/l non-ionic detergent at
600C for 10 min, Dyeing was also carried out in presence of inorganic salt
such as aluminium sulphate and ferrous sulphate by post-mordanting method
at 800C for 45 min followed by cold wash and finally dried. Printing of jute
fabrics dyed with vegetable colourants was carried out with the help of print
paste containing inorganic salts (5 g/1000 g of print paste) and gum indulka
thickener, whereas for printing on bleached jute fabric the print paste was
prepared by mixing inorganic salts, vegetable colourants and gum indulka
thickener. The impressions were made with the help of wooden blocks and the
fabrics were dried at room temperature, followed by steaming for 10 min at a
temperature of 1000C in a cottage steamer. The fabrics were then immediately
washed with 2 g/l non-ionic detergent at 500C for 10 min in order to remove
the gum and the strong mineral acid (Sulphuric acid) produced during the
steaming process. After soaping the printed fabrics were further washed with
cold water and finally dried in air. Colourfastness of the printed jute fabrics
was improved by inorganic salts such as ferrous sulphate and aluminium
sulphate.
2.4 Details of dyes used in the study
Waste material of four plants namely Tropical almond (waste leaves),
Shimalo (Bark), Asopalav (waste leaves), Neem (waste leaves) were selected
for the present research study. General information, brief introduction,
physical appearance, chemical composition of plant waste is given below.
52
2.4.1 Tropical Almond or Indian Almond(Terminalia Catappa)
Photograph- 2.1 Tropical Almond (Terminalia Catappa)
Tropical Almond tree Tropical Almond leaf front side Tropical Almond leaf back side
Source of images: Google Images

General information:
Family: Combretaceae
Scientific/Botanical name: Terminalia catappa
English name: Tropical-Almond, Indian-Almond
Common name(s): Badamlili, Desi badam
Part used as dye: Waste leaves
Brief introduction:
It is a large, spreading tree now distributed throughout the tropics in
coastal environments. It grows to about 35 meter tall, with an upright
structure. During the dry season (autumn), the leaves turn into colours of red,
copper, gold. The tree usually sheds all its leaves twice a year in January-
February and July-August. The tree first drops its leaves when it reaches 3-4
years old and then every year.
The leaves are large, 15–25 centimeters (5.9–9.8 inch) long and 10–14
centimeters (3.9–5.5 inch) broad, ovoid, glossy dark green and leathery.
Before falling, they turn pinkish-red or yellow-brown, due to pigments such as
violaxanthin, lutein, and zeaxanthin. The leaves contain several flavonoids
(like kaempferol or quercetin), several tannins (such as punicalin, punicalagin
or tercatin), saponines and phytosterols.
The leaves are found to have strong anti-bacterial properties and
promote fish breeding, curing sick fish and speed up healing of damage. The
dried leaves act as a "black water extract" which gradually turns the water
brown like tea and effectively reduces the pH levels in water, releasing
organic compounds such as humic acids, flavanoids and tannins into the water
which absorb harmful chemicals. (Thomson and Evans,2006).
53
2.4.2Malabar semul or red cotton tree (Bombax Ceiba)

Photograph-2.2Malabar semul or Red cotton tree (Bombax Ceiba)
Tree Stem with conical prickle conical prickle
Family: Bombacaceae
Scientific/Botanical name: Bombax ceiba Linn
English name: Malabar semul , Red cotton tree, Indian kapok tree
Common name(s): Shimalo, Semal
Part used as dye Dry bark with trunk
Brief introduction:
It is the large beautiful and deciduous tree found throughout India
and other parts of tropical and sub-tropical Asia, Australia and Africa. The
tree is mentioned in Mahabharata proving its presence since a long time.
The tree is large sized, tall, deciduous, having straight, buttressed
trunk with a clear bole and widespread branches. The trunk and branch
bark is gray in colour having hard, sharp and conical prickles.
Preliminary tests show the presence of glycosides and tannins from

root, stem and leaf. In the stem some alkaloids and in root proteins are
identified. The stem bark contains lupeol and b-sitostrol.(Jain et al.,2009)
54
2.4.3 Mast tree or Asopalav(Polyalthia longifolia)
Photograph-2.3 Mast tree or Asopalav(Polyalthia longifolia)
Asopalav whole tree Asopalav close view Asopalav leaves

Family: Annonaceae
Scientific/Botanical name: Polyalthia longifolia
English name: Mast tree
Common name(s): Asopalav
Part used as dye Dry leaves
Brief introduction:
It is a lofty evergreen tree, native to Indiaand Sri Lanka, commonly
planted due to its effectiveness in alleviating noise pollution. It is introduced
in gardens in many tropical countries around the world. It exhibits
symmetrical pyramidal growth with willowy weeping pendulous branches and
long narrow lanceolate leaves with undulate margins. The tree is known to
grow over 30 ft in height. It grows naturally (without trimming the branches
out for decorative reasons) into a normal large tree with plenty of shade. The
plant was found to contain alkaloids, flavonoids, saponins, carbohydrates, fats
and oils, tannins, steroids and terpenoids.(Chen et al., 2000)
Fresh leaves are a coppery brown colour and are soft and delicate to
touch, as the leaves grow older the color becomes a light green and finally a
dark green. The leaves are shaped like a lance and have wavy edges. The
leaves are use for ornamental decoration and are used in festivals. In past, the
flexible, straight and light-weight trunks were used in the making of masts for
sailing ships. That is why the tree is also known as the Mast Tree.
55
2.4.4 Neem tree (Azadirachta indica)
Photograph-2.4Neem tree(Azadirachta indica)
Neem whole tree Neem close view Neem dry leaves

Family: Meliaceae
Scientific/Botanical name: Azadirachta indica
English name: Neem tree
Common name(s): Limdo, Neem
Part used as dye: Dry leaves
Brief introduction:
Azadirachta indica (neem) belonging to Meliaceae family is very
important medicinal plant which is traditionally used to treat different
diseases. It is a large evergreen tree, 12 to 18 meter in height and 1.8 to 2.4
meter in girth with a straight bole and long spreading branches forming a
broad crown as much as 20 meters across, commonly found throughout greater
parts of India. Neem is a native tree of India, found in every part in
India especially in semi-arid conditions. The Neem Tree is an incredible
plant that has been declared the "Tree of the 21st century" by the United
Nations. It is one of the major components in Ayurvedic medicine. The neem
is an ancient Indian cure-all due to its antibacterial, antifungal, antiviral,
antihistamine and antiseptic properties. In fact the people of India call the
Neem Tree "The Village Pharmacy".
Identiﬁcation and characterization of chemical compounds in crude
extracts from leaves of Omani neem has been carried out by Hossain et al.,
(2013).
The crude extracts of the leaves contain normal hydrocarbons, phenolic
compounds, terpeniods, alkaloids and glycosides.(Bukhari et al.,2014) The
56
important chemical constituents were present in the leaf crude extracts of

neem that can be endorsed to cultivation on a domestic plantation.
2.5 Studies of ecofriendly finishes on dyed fabric
Textile fiber or fabrics are deficient in one or more properties or

improved properties are desired for the fiber or fabric. Textile finishing
provides a method whereby deficiencies in the textile can be corrected or
specific properties can be introduced. A finish is a treatment given to a fabric,
to change its appearance, handling /touch or performance. Its purpose is to
make the fabric more suitable for its end use (Jahid & Pervez , 2015).
To improve those performance properties, cotton fabric often are given
a chemical treatment called durable press finishing. This treatment involves
the use of crosslinking agents. Most important ecofriendly crosslinking agents
are butanetetracarboxylic acid (BTCA) and citric acid (CA). Many research
studies on durable press finishing with ecofriendly crosslinking agents have
been carried out. Few studies are given below.
Schramm et al. (2002) used polycarboxylic acids 1,2,3,4-
butanetetracarboxylic acid and citric acid as non-formaldehyde durable press
finishing agents instead of formaldehyde-releasing N-methylol compounds. In
this study, isocratic HPLC is applied in an attempt to quantify the
polycarboxylic acids that react with cellulosic material dyed with CI Reactive
Red 195, CI Reactive Yellow 145 and CI Reactive Blue 221. Subsequently,
the fabrics were cured with formulations containing butanetetracarboxylic acid
and citric acid or a combination of both. The pre-weighed, dyed fabric was
impregnated in a treatment bath containing a crosslinking agent and a catalyst.
No softener was used. The catalyst was added to the formulation immediately
before application. Subsequently, the sample (30 × 50 cm) was passed through
a two-roll laboratory padder (air pressure 1 bar, fabric speed 3 m/min). This
treatment gave a wet pick-up of about 100–109%, depending on the original
weight of the fabric treated. After drying (2 min, 100 °C) the fabric was cured
for a specified time at 180 °C in a laboratory dryer, washed with occasional
stirring (sodium carbonate 1 g/l, 10 min, 50 °C, wash liquor 1 l) and finally
dried again (3 min, 80 °C). The chromatographic determination reveals that an
increase in the depth of shade results in a decrease of the amount of
57
butanetetracarboxylic acid, except in the case when cotton is dyed with CI

Reactive Blue 221, a copper formazan complex-based dyestuff. Colour
measurements indicate that the ∆E* values decrease in the order CI Reactive
Yellow 145, CI Reactive Red 195 and CI Reactive Blue 221. The dyestuffs
react with the hydroxyl groups of the cellulose and consequently fewer
hydroxyl groups are available for the esterification reaction with
polycarboxylic acids. This phenomenon is confirmed by the fact that the
application of higher depths of shade results in a decrease in the amount of
cotton-bound PCA, except with CI Reactive Blue 221.
Concurrent dyeing and finishing of cotton with natural colour and
citric acid in the presence of NaH2PO4 as catalyst under thermal treatment by
Maulik et al. (2011) has been reported. Cotton fabric was simultaneously
modified and dyed with citric acid and Camellia sinensis, and citric acid and
Punica granatum in the presence of sodium di-hydrogen phosphate
(NaH2PO4) as the catalyst using a pad–dry–cure technique. Treatment with
10% citric acid, 15% NaH2PO4 and dye at 100% wet pickup, followed by
drying at 95°C for 5 min and curing of the dried fabric at 140°C for 5 min
produced most balanced improvements in respect of the depth of shade,
wrinkle recovery and colour fastness to light, wash and rubbing with retention
of more than 70% of the original strength. Infrared analysis of the dyed cotton
fabric indicated that the treatment of cotton with citric acid and either
Camellia sinensis or Punica granatum under the influence of an esterification
catalyst led to the esterification of carboxyl groups of citric acid and of
hydroxyl groups of cotton cellulose and with that of both the dyes. The said
process also led to some degree of cross-linking of polymeric chains of cotton.
Effect of different cross-linking agents on cotton fabric dyed with
caspian natural dyes was studied by Sheth et al.(2003). Mill bleached
mercerized cotton fabric was used. The fabric was pretreated with potash
alum, stannous chloride or tartaric acid at 80ºC for 30 minutes at M:L 1:20.
Undyed and dyed fabrics were padded with conventionally used dimethyl
dihydroxyethylene urea. Color depth and color difference of dyed and cross-
linked fabric was measured on a Macbeth Colour Eye 7000A. The results
observed that the color difference of differently cross-linked fabric was
comparable of slightly higher than that for conventionally used DMDHEU
58
cross-linked fabric. Trisuccinimidyl citrate (TSC) fabrics showed drastic

change in shade, while very low formaldehyde (VLF) cross-linked fabric
showed less comparable color difference to that of DMDHEU depending on
type of mordant used during dyeing. Wrinkle recovery angle was found to be
between 233-258. While tear and tensile strength retention was between 51-
100 depending on type of mordant used during dyeing and type of cross-
linking agent applied. Generally, from the results obtained it was found that in
case of most of the natural dyes and different mordants when dyed on cotton
fabric and cross-linked with organic acid in presence of trisodium citrate, color
difference was higher than that for conventionally used cross-linked fabric.
Influence of microwaves on non-formaldehyde DP finished dyed
cotton fabrics has been reported by Vukusic et al. (2003). An alternative
approach to the application of formaldehyde releasing conventional N-
methylol compounds is based upon the use of non-formaldehyde Durable
Press (DP) finishing agents – polycarboxlic acids (PCA). The application of
microwave energy to impart durable crease resistance to dyed cotton fabric.
Bifunctional dyes: C.I. Reactive Red 195, C.I. Reactive Yellow 145 and C.I.
Reactive Blue 221 were applied in the study. Isocratic HPLC method was
applied to quantify the PCA reacted with the cellulosic material under two
different curing procedures.Microwave way of curing imparts higher levels of
wrinkle resistance of dyed as well as of undyed cotton materials treated with
PCA. General trend noticed when microwave curing is used a lower amount of
PCA bound. This opposite trend between elastic recovery and quantity of PCA
bound can be attributed to a greater number of least di-ester linkages which
can improve DP properties and cannot be distinguished from mono-ester
linkages with the HPLC technique. The chromatographic determination
reveals the decrease in PCA, in almost all the cases studied, caused by the
increase in shade depth with both ways of curing. These results confirmed the
reduced cellulose affinity for further crosslinking with PCA molecules,
because of the partial blockage of cellulose reactive groups with the dye
molecules. Regarding the evaluation of the color differences, they are more
prominent when microwave treatment is included in the experiment. Shade
changes are primarly caused by the catalyst applied, which is a strong
reducing agent. Azo chromogen is decomposed by the action of the reducing
59
agent, which causes most prominent shade changes, particulary with yellow
hue. Primarily in the wrinkle recovery and resistance to deformation,
microwave way of curing offers much better results.
60

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CHAPTER- II

Promotion of natural dyes along with the use of metal mordant is of

2.1 Environment pollution from synthetic dyes

2.1 Environment pollution from synthetic dyes

Approximately 10-15% dyes are released into the environment during

fastness performance ratings are inadequate for modern textile usage.

On the basis of hues, natural dyes can be classified as follows:

of natural yellow dyes ranges from fair to excellent, e.g., tesu,

iii. Alphanaphthoquinones: Typical examples of this class are lawsone

2.2.4 Mordanting Methods:

In the last fifteen to twenty years many scientific research studies on

concentration 7%, dyeing temperature 100°C, dyeing time 45 minutes, and

combinations exhibited better fastness. Pre mordanted samples with potassium

along with improvement in intensity of color and washing fastness. It was

During the study, a wide range of colors were obtained on jute

Best shades on cotton fabric were obtained by using jamun leaves

mordanting, shades obtaining and colour fastness properties. Some important

Paul et al. (2003) have described walnut bark as a good source of

extract of henna leaves in the absence of mordent, displayed good light

Phukan and Phukan (2004) standardized the condition of dyeing

type of mordant and technique of mordanting with very low concentrations of

Prusti, et al (2009), have studied Terminalia catappa as a suitable

2.3.3 Natural dyes for polyamide fibre

Nylon is synthetic fiber containing amide link known as polyamide

comparison with conventional heating. The results of dye extraction indicate

tannic acid. Moreover, toxicity of ferrous sulphate as compared to copper sul-

immediately washed with 2 g/l non-ionic detergent at 60ºC for 10 minutes in

2.4.1 Tropical Almond or Indian Almond(Terminalia Catappa)

Photograph- 2.1 Tropical Almond (Terminalia Catappa)

Source of images: Google Images

2.4.2Malabar semul or red cotton tree (Bombax Ceiba)

Tree Stem with conical prickle conical prickle

Source of images: Google Images

Preliminary tests show the presence of glycosides and tannins from

2.4.3 Mast tree or Asopalav(Polyalthia longifolia)

Photograph-2.3 Mast tree or Asopalav(Polyalthia longifolia)

Asopalav whole tree Asopalav close view Asopalav leaves

2.4.4 Neem tree (Azadirachta indica)

Photograph-2.4Neem tree(Azadirachta indica)

Neem whole tree Neem close view Neem dry leaves

important chemical constituents were present in the leaf crude extracts of

2.5 Studies of ecofriendly finishes on dyed fabric

Textile fiber or fabrics are deficient in one or more properties or

butanetetracarboxylic acid, except in the case when cotton is dyed with CI

cross-linked fabric. Trisuccinimidyl citrate (TSC) fabrics showed drastic

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