Preparation of Dyes

By: Ann Cherian

Class and Section: 12E
Teacher in-charge: Roopa Shankar
 Table of contents
Sno. Title Pages

1 Abstract 2

2 Introduction 3

3 A study in Pigments 4

4 Types of Pigments 6

5 The Case of Dyeing 9

6 Methods of Dyeing 11

7 Process of Dyeing 13

8 Chemistry of 15
Dyeing Process
9 Experiement 18

10 Future Scope 24

11 Bibliography 25

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 Abstract
This topic was chosen because of the fascination and the science behind the
working of a pigment, and how the color of each pigment is different and has
different shades of the same color.

We wanted to know how to prepare paint pigments using various chemicals and
record the efficiency in producing them.

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 Introduction
A pigment is a colored material that is completely or nearly insoluble in water. In
contrast, dyes are typically soluble, at least at some stage in their use. Generally
dyes are often organic compounds whereas pigments are often inorganic
compounds. Pigments of prehistoric and historic value include ochre, charcoal,
and lapis lazuli.
Dyeing is the application of dyes or pigments on textile materials such
as fibers, yarns, and fabrics with the goal of achieving color with desired color
fastness. Dyeing is normally done in a special solution containing dyes and
particular chemical material. Dye molecules are fixed to the fiber by absorption,
diffusion, or bonding with temperature and time being key controlling factors. The
bond between dye molecule and fiber may be strong or weak, depending on the
dye used. Dyeing and printing are different applications; in printing, color is
applied to a localized area with desired patterns. In dyeing, it is applied to the
entire textile.
The primary source of dye, historically, has been nature, with the dyes being
extracted from animals or plants. Since the mid-19th century, however, humans
have produced artificial dyes to achieve a broader range of colors and to render the
dyes more stable to washing and general use. Different classes of dyes are used for
different types of fiber and at different stages of the textile production process,
from loose fibers through yarn and cloth to complete garments.
Acrylic fibers are dyed with basic dyes, while nylon and protein fibers such
as wool and silk are dyed with acid dyes, and polyester yarn is dyed with disperse
dyes. Cotton is dyed with a range of dye types, including vat dyes, and modern
synthetic reactive and direct dyes.

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 A Study in Pigments
What is Pigment?
A pigment is a material that changes the colour of reflected or transmitted light as
the result of wavelength-selective absorption. In other words, it’s a substance that
appears a certain colour because it selectively absorbs certain wavelength of light.
Many materials selectively absorb certain wavelengths of light. Materials that
humans have chosen and developed for use as pigments usually have special
properties that make them ideal for colouring other materials. A pigment must have
a high tinting strength relative to the materials it colours. It must be stable in solid
form at ambient temperatures.

For industrial applications, as well as in the arts, permanence and stability are
desirable properties. Pigments that are not permanent are called fugitive. Fugitive
pigments fade over time, or with exposure to light, while some eventually blacken.

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Pigments are used for coloring paint, ink, plastic, fabric, cosmetics, food and other
materials. Most pigments used in manufacturing and the visual arts are dry
colorants, usually ground into a fine powder. This powder is added to a binder (or
vehicle), a relatively neutral or colorless material that suspends the pigment and
gives the paint its adhesion.

While a dye can dissolve by itself in a liquid, pigments can be dissolved in a liquid
with the help of a binder. Dyes are primarily applied in the textile and paper
industry, pigments are used in industries such as colouring paints, inks, cosmetics,
and plastics.

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 Types of Pigments
Based on the method of their formulation, pigments can be categorized into two
types: inorganic pigments and organic pigments.
 ORGANIC PIGMENTS:
This type of pigments occurs naturally, and they’ve been used for centuries.
They’re quite simple in their chemical structure. They’re named organic as
they contain minerals and metals that give them their color. Organic pigment
manufacturers produce them through a simple process that’s made of
washing, drying, powdering, and combining into a formulation.
Compared to inorganic pigments, this usage of these pigments is less
frequent and that’s why there are limited number of organic pigment
suppliers. These pigments are used when the required color strength isn’t too
much.


INORGANIC PIGMENTS :
As you can guess by its name, this type of pigments is exactly the opposite
type of organic pigments. These pigments are also known as “synthetic
pigments.” They’re formulized in labs and offer great scope of control to

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 inorganic pigment manufacturers. Inorganic pigments are manufactured by
relatively simple chemical processes such as oxidation.
Inorganic pigment suppliers supply this type of pigments mainly to paints,
plastics, synthetic fibers, and ink industry. In uses where bright colors are
required, organic pigments are used as they bolster high color strength.
Inorganic pigments include white opaque pigments which are commonly
used to lighten other colors and to provide opacity.
 Two other types of pigments are metallic pigments and industrial
pigments:
Metallic pigments, as implied in the name, include metal pigments such as
zinc and aluminum pigments. While industrial pigments are the pigments
that are widely used in the industrial applications and include organic,
inorganic and the metallic pigments.

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8
 Principle
The principle behind the working of pigments is related with how different
substances can selectively absorb and reflect different light rays corresponding to
their different wavelengths in the visible spectrum. Pigments appear the colors they
are because they selectively reflect and absorb certain wavelengths of visible light.
White Light is a mixture of all light rays of wavelength 400 nm – 700 nm.

When this light encounters a pigment, parts of the spectrum are absorbed by the
different components of the pigment. Some other wavelengths or parts of the
spectrum are reflected and scattered. The new reflected light spectrum creates the
appearance of a color. When this reflected light encounters a Human Eye, the
Brain perceives the light as the color corresponding to its Wavelength. Pigments,
unlike fluorescent substances can only subtract wavelengths from the source light
and can never add new ones.

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 The Case of Dyeing
"The process of applying color to fiber stock, yarn, or fabric is called dyeing."
There may or may not be thorough penetration of the colorant into the fibers or
yarns.
Dyes can be used on vegetable, animal, or
man-made fibers only if they have an
affinity to them. Textile dyes include acid
dyes, used mainly for dyeing wool, silk, and
nylon, and direct or substantive dyes, which
have a strong affinity for cellulose fibers.
Mordant dyes require the addition of
chemical substances, such as salts to give
them an affinity for the material being dyed.
They are applied to cellulose fibers, wool, or
silk after such materials have been treated
with metal salts. Sulfur dyes, used to dye
cellulose, are inexpensive but produce colors
lacking brilliance. Azoic dyes are insoluble
pigments formed within the fiber by
padding, first with a soluble coupling
compound and then with a diazotized base.
Vat dyes, insoluble in water, are converted into soluble colorless compounds
employing alkaline sodium hydrosulfite. These colorless compounds are absorbed
by cellulose, which is subsequently oxidized to an insoluble pigment. Such dyes
are colorfast. Disperse dyes are suspensions of finely divided insoluble, organic
pigments used to dye such hydrophobic fibers as polyesters, nylon, and cellulose
acetates. Reactive dyes combine directly with the fiber, resulting in excellent
colorfastness. The first ranges of reactive dyes for cellulose fibers were introduced
in the mid-1950s. Today, a wide variety is available.

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 Methods of Dyeing
Objective:
The primary objective of dyeing is to apply uniform color to the substrate (fiber,
yarn, or fabric) with required color fastness. Tie-dye and printing are the methods
where the color is applied in a localized manner.
1. Bale Dyeing: This is a low-cost method to dye cotton cloth. The material is
sent without scouring or singeing, through a cold-water bath where the sized
warp has an affinity for the dye. Imitation chambray and comparable fabrics
are often dyed this way.
2. Batik Dyeing: This is one of the oldest forms known to man. It originated in
Java. Portions of the fabric are coated with wax so that only un-waxed areas
will take on the dye matter. The operation may be repeated several times and
several colors may use for the bizarre effects. Motifs show a mélange,
mottled or streaked effect, imitated in machine printing.
3. Beam Dyeing: In this method, the warp is dyed before weaving. It is wound
onto a perforated beam and the dye is forced through the perforations
thereby saturating the yarn with color.
4. Burl or speck Dyeing: This is done mostly on woolens or worsteds; colored
specks and blemishes are covered using special colored links which come in
many colors and shades. It is a hand operation.
5. Chain Dyeing: This is used when yarns and cloth are low in tensile strength.
Several cuts or pieces of cloth are tacked end-to-end and run through in a
continuous chain in the dye color. This method affords high production.
6. Cross Dyeing: This is a very popular method in which varied color effects
are obtained in the one dye bath for a cloth that contains fibers with varying
affinities for the dye used. For example, a blue dyestuff might give nylon 6 a
dark blue shade, nylon 6, 6 a light blue shade, and have no affinity for
polyester area unscathed or white.
7. Jig Dyeing: This is done in a jig, kier, vat, beck, or vessel in an open
formation of the goods. The fabric goes from one roller to another through a
deep dye bath until the desired shade is achieved.
8. Piece Dyeing: The dyeing of fabrics in the cut, bolt, or piece form is called
piece dyeing. It follows the weaving of the goods and provides a single color
for the material, such as blue serge, a green organdy.

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 9. Random Dyeing: Coloring only certain designated portions of the yarn.
There are three ways of doing this type of coloring:
10.Yarn dyeing: In yarn dyeing, the yarns are dyed first before the fabric
manufacturing stage. The yarn dyeing happens in hanks or in package
dyeing. Package dyeing is a method where yarns are wound on perforated
cones placed in a dye vessel. The dye solution is then alternatively pushed
inside out and vice versa. Examples are many stripes, patterned (checks) and
jacquard designed fabrics.
11.Dope dyeing: In dope dyeing, pigments are added to the polymer solution
itself before extruding the fibers. The process provides the dyed fibers with
excellent fastness properties. The dope dyeing applies to synthetic
fiber only. This method of dyeing is also known as solution dyeing and 'mass
coloration' or 'mass colored'. It has limited color options.
12.Raw Stock Dyeing: Dyeing of fiber stock precedes spinning of the yarn.
Dyeing follows the degreasing of wool fibers and drying of the stock.
13.Solution Dyeing: This is also called dope dyeing or spun dyeing; the
pigment color is bonded-in in the solution and is picked up as the filaments
are being formed in the liquor. Cellulosic and non-cellulosic fibers are dyed
to perfection by this method. The colors are bright, clear, clean, and fast.
14.Yarn-dyed: Yarn that has been dyed before the weaving of the goods;
follows spinning of the yarn. It may be done in either partial immersion or
total immersion of the yarn.

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 Process of Dyeing
The dyeing of textile fiber is carried out in a solution, generally aqueous, known as
the dye liquor or dye bath. For true dyeing to have taken place, the coloration of
fabric and absorption are important determinants.
 Coloration: The coloration must be relatively permanent: that is not readily
removed by rinsing in water or by normal washing procedures. Moreover,
the dyeing must not fade rapidly on exposure to light.
 Absorption: The process of attachment of the dye molecule to the fiber is
one of absorption: that is the dye molecules concentrate on the fiber surface.
There are four kinds of forces by which dye molecules are bound to the
fiber:

a. Ionic forces
b. Hydrogen bonding
c. Vander Waals' forces
d. Covalent chemical linkages
Dyeing of Wool: In the dyeing of wool which is a complex protein containing
about 20 different amino acids, the sulfuric acid added to the dye bath forms ionic
linkages with the amino groups of the protein. In the process of dyeing, the sulfate
anion (negative ion) is replaced by a dye anion. In the dyeing of wool, silk, and
synthetic fibers, hydrogen bonds are probably set up between the azo, amino,
alkylamino, and other groups and the amino Co-NH-groups. Covalent chemical
links are brought about in the dye bath by a chemical reaction between a fiber-
reactive dye molecule, one containing a chemically reactive center, and a hydro-
oxy group of cotton fiber, in the presence of alkali.
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 The Chemistry of the Dyeing Process
Exhaustion in any dyeing process, whatever the chemical class of dye being used,
heat must be supplied to the dye bath; energy is used in transferring dye molecules
from the solution to the fiber as well as in swelling the fiber to render it more
receptive. The technical term for this process is exhaustion. Levelness: An
Important Quality.

Evenness of dyeing, known as levelness is an important quality in the dyeing of all

forms of natural and synthetic fibers. It may be attained by the control of dyeing
conditions viz.
1. By agitation to ensure proper contact between dye liquor and substance
being dyed and by use of restraining agents to control the rate of dyeing or
strike. Solvent Dyeing Serious consideration has recently been given to the
methods of dyeing in which water as the medium is replaced by solvents
such as the chlorinated hydrocarbons used in dry cleaning. The technological
advantages in solvent dyeing are 1. Rapid wetting of textiles
2. Less swelling
3. Increased speed of dyeing per given amount of material
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 4. Savings in energy, as less heat is required to heat or evaporate per-chloro-
ethylene. Thus, it eliminates the effluent (pollution) problems associated
with the conventional methods of dyeing and finishing.
Machinery and Equipment: Modern dyeing machines are made from stainless steel.
Steels containing up to 4% molybdenum are favored to withstand the common acid
conditions.A dyeing machine consists essentially of a vessel to contain the dye
liquor, provided with equipment for heating, cooling, and circulating the liquor
into and around the goods to be dyed or moving the goods through the dye liquor.
The kind of machine employed depends on the nature of the goods to be dyed.
Labor and energy costs are high concerning total dyeing costs: the dyers aim to
shorten dyeing times to save steam and electrical power and to avoid spoilage of
goods.The conical-pan loose-stock machine is widely used. Fibers are held in an
inner truncated conical vessel while the hot dye liquor is mechanically pumped
through. The fiber mass tends to become compressed in the upper narrow half of
the cone, assisting in efficient circulation. Leveling problems are less important as
uniformity may be achieved by blending the dyed fibers before spinning.The
Hussong machine is the traditional apparatus. It has a long, square-ended tank as a
dye bath into which a framework of poles carrying hanks can be lowered. The dye
liquor is circulated by an impeller and moves through a perforated false bottom
that also houses the open steam pipe for heating. In modern machines, circulation
is improved at the points of contact between hank and pole. This leads to better
leveling and elimination of irregularities caused by uneven cooling. In package-
dyeing machines dye color may be pumped in rather two directions:
1. Through the perforated central spindle and outward through the package or
2. By the reverse-path into the outer layers of the package and out of the
spindle. In either case, levelness is important.
3. Some package-dyeing machines can work under pressure at temperatures up
to 130C.The winch is the oldest piece of dyeing machine and takes its name
from the slated roller that moves an endless rope of cloth or endless belt of
cloth at full width through the dye liquor. Pressurized-winch machines have
been developed in the U.S.
In an entirely new concept, the Gaston County jet machine circulates fabric in rope
form through a pipe through a high-pressure jet of dye color. The jet machine is
increasingly important in the high temperature dyeing of synthetic fibers,
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especially polyester fabrics. Another machine is the jig. It has a V-shaped trough
holding the dye color and guides rollers to carry the cloth at full width between two
external, powered rollers, the cloth is wound onto each roller alternately, that is,
the cloth is first moved forward, then back through the dye color until dyeing is
complete. Modern machines, automatically controlled and programmed, can be
built to work under pressure.

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EXPERIMENT
Aim: To dye wool and cotton clothes with malachite green.
Requirements:
 500 ml beakers
 tripod stand
 wire gauze
 glass rod
 spatula
 wool cloth
 cotton cloth
 Sodium carbonate
 tannic acid
 tartaremetic acid
 malachite green dye
 500 ml beaker
 Tripod stand
 Wire gauze
 Glass rod Sodium
 Tannic Acid
 Tartaremetic Malachite
 Carbonate Green
 Copper Sulphate
 Sodium Carbonate
Theory: Cotton fibers show good durability and utility. It is a stable material; it
stays undamaged even in conditions of high exposure to weak acids and alkalis. It
has high water absorbing capacity. Cotton fabrics are easy to dye, they have very
low elasticity characters. They are easily washable and can be ironed even at very
high temperatures. Woolen fibers are high moisture absorbers too. They take up
moisture in vapor form. It generates heat when it absorbs moisture. Each wool
fiber is a molecular coil spring, making the fiber remarkably elastic. They have
high durability and resilience. Nature has folded the chemical polypeptide chains
back upon themselves in such a way that they act like a coiled spring that elongates
when it is extended and retracts when it is released. Malachite Green is an organic
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compound that is used as a dyestuff and controversially as an antimicrobial in
aquaculture. Malachite green is traditionally used as a dye for materials such as
silk, leather, and paper. Although called malachite green, this dye is not prepared
from the mineral malachite - the name just comes from the similarity of color.
Chemical formula: [C6H5C(C6H4N(CH3)2)2]Cl (Common Name: Triarylmethane
dye).

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 Procedure
Experiment 1
1)Take about 0.5g of solid sodium carbonate and dissolve it in 250ml of water.
Preparation of tartaremetic solution:
2)Take about 0.2g of tartaremetic and dissolve it in 100ml of water by stirring with
the help of a glass rod.
3) Preparation of tannic acid solution: Take 100ml of water in a beaker and add
about 1.0g of tannic acid to it.
4)Heat the solution. On heating, a clear solution of tannic acid is obtained.
5) Preparation of dye solution: Take about 0.1g of malachite green dye and add to
it 400ml of water. Warming results in a clear solution of the dye.
6)Dyeing of wool: Take about 200ml of dye solution and dip in it the woolen cloth
to be dyed. Boil the solution for about 2 minutes. After that remove the cloth and
wash it with hot water 3-4 times, squeeze and keep it for dyeing.
7)Dyeing of cotton: Cotton does not absorb malachite green readily, therefore it
requires the use of a mordant. For dyeing, a cotton cloth dips it in sodium
carbonate solution for 10 minutes and then rinse with water. Then put the cloth in a
hot tannic solution for about 5 minutes. Now take out the cloth from the tannic acid
solution and keep it in tartaremetic solution for about 5 minutes. Remove the cloth
and squeeze it with a spatula to remove most of the solution. Now place the cloth
in the boiling solution of the dye for about 5 minutes. Remove and wash the dyed
cloth thoroughly with water, squeeze and keep it for drying.
8) Dyeing of cotton directly: Take another piece of cotton cloth and put it directly
into a boiling solution of the dye. Keep it dipped for about 2 minutes. Remove the
cloth, wash it with water, squeeze and keep it for drying.

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 Experiment 2
1. Make a solution of sodium carbonate by dissolving 5.8 grams of the salt in 55
mL of water. Stir the solution briskly, using a spatula, until the salt particles are
properly dissolved in the water.
2. Make a solution of copper sulphate by dissolving 12.5 grams of the salt in 50
mL of water. Stir the solution briskly, using a spatula, until the salt particles are
properly dissolved in the water.
3. Add sodium carbonate solution, slowly, into copper sulphate solution while
stirring briskly.
4. Leave the greenish (malachite) mixture, so formed, undisturbed for 15 minutes.
5. Prepare a gravity filter by setting a folded filter paper in the form of a cone,
which is stuck to the inner edge of a funnel, which is then set on a conical flask.
6. Pour the mixture, slowly, over the gravity filter, and allow the powder to
precipitate.
7. Once the filter paper is dried up, carefully remove the filter paper and pour the
powder in a china dish.
8. Scrape the excess powder that is stuck on the filter paper, by using a spatula.
9. The powder obtained, is the paint pigment of the Shade malachite.
10. Weigh the Powder Formed on an Electronic Weighing Scale, and calculate the
efficiency of formation.

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 Observations
1. The color of wool cloth directly by dipping in a hot solution of malachite
green dye is fast.
2. The color of cotton cloth dyed directly (without using mordant) by dipping
in a hot solution of malachite green is not fast to washing and is of low
intensity.
3. The color of cotton cloth dyed indirectly by using mordant and then by
dipping in a hot solution of malachite green is fast to washing and is of high
intensity.
4. Precautions: Let the Malachite Green solution boil properly for about 8-10
minutes to get better results.
5. While dyeing cotton directly, let the cotton cloth be present in the dye for
more than or equal to 2 minutes but not less.
6. Using solutions such as tartaremetic solution, the tannic acid solution must
be eminent.
7. Usage of gloves is preferable to ensure tidiness.
8. For Malachite:
Amount of Reactants = ____ g
Amount of Pigment formed = ____ g
Efficiency = ____ %

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 Conclusion
DYE FABRIC RESULT
Dying Malachite green dye on wool is a fast process while on cotton it is not fast to
wash and has low intensity. Using Sodium carbonate solution, tartaremetic
solution, tannic acid, and Malachite green on cotton, the result obtained was
different as it was fast to washing with a fast intensity.

Precautions

1. All apparatuses used for the experiment should be properly cleaned before use to
prevent any unnecessary addition of impurities.
2. All chemicals used should be accurately measured. If more or less than the
required amount is used, then the pigment may not be formed efficiently.
3. Make sure the right chemicals are used else an unwanted reaction may take
place, which may thus lead to incorrect results.
4. Filtration of the pigment should be done carefully to get maximum amount of
pigment.

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 Future scope

1.There is tremendous scope for paint pigments in the future.

2.Increasing experimental methods and newer technologies in preparation of
pigments has increased the quality and quantity of pigments obtained.
3. Scientists are trying to increase the efficiency of the various paint pigments by
newer experimental methods.
4. New shades of colors have been developed in laboratories.
5.Industries have increased their production of pigments and dyes through
scientific technology. 6.Pigments are now being used more widely.
6. Natural pigments / non – toxic pigments are being synthesized to avoid any
health hazards due to the dangerous chemicals contained in them.

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Bibliography
 www.google.com
 www.chemstudy.com
 www.chymist.com
 www.bing.com
 www.seminarsomnly.com
 www.archive.org
 https://en.wikipedia.org/wiki/Pigment
 https://en.wikipedia.org/wiki/Dyeing

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