PREPARATION

Of
CHEMICAL
DYES
 THE INDIAN COMMUNITY SCHOOL KUWAIT
(DEPARTMENT OFCHEMISTRY)
BONAFIDE CERTIFICATE
CERTIFIED TO BE THE BONAFIDE RECORD OF
WORK DONE BY MISS Hrithika Ratheesh
OF CLASS 12-a
IN THE INDIAN COMMUNITY SCHOOL KUWAIT
DURING THE YEAR 2022-2023
P.G.T IN CHEMISTRY
THE INDIAN COMMUNITY SCHOOL KUWAIT.
SUBMITTED FOR ALL INDIA SENIOR
SECONDARY CERTIFICATE EXAMINATION IN
CHEMISTRY AT THE INDIAN COMMUNITY
SCHOOL ,
KUWAIT.
DATE: 5/7/23
 DECLARATION
I hereby declare that the project entitled
“PREPARATION OF CHEMICAL DYES“
to the Indian Community School,Kuwait is a
record of an original work by me by gaining
the knowledge related to the project from
certain resources.

INDEX
1. Axo dye
INTRODUCTION
1. HISTORY
2. SYNTHESIS
3. PROCEDURE
4. HEALTH HAZARDS

2. Vat dyes
1. Introduction
2. History
3. Process
4. PRETREATMENT OF VAT DYING
5. Application of vat dyes
6. precautions

AZO DYES
INTRODUCTION
 Human's love of color reaches back almost to
prehistoric times, yet it is not actually until the
modern era that the full range of the rainbow has
been accessible to the majority of people in their
clothes and other textiles. Ancient or medieval times
have often been described as being quite splendid
with their "Tyrian Purple" and medieval scarlet, but
closer examination shows that some of these colours
were quite dull by today’s standards.
 HISTORY
The history of dyeing can be divided into two great
periods, the "pre-aniline," extending to 1856 and
the "post-aniline" period. The former was
characterized by a rather limited range of colors
that were based on dye-producing animals and
plants. The main vegetable dyes available were
extracted from madder root (Asia and Europe),
producing a brilliant red and leaves of the indigo
plant (India), yielding the blue dye still used today
in jeans. Among the most important animal based
dyes is the famous and expensive "Tyrian Purple"
which was obtained from the small shellfish nurez.
We have the ancients' word that this dye was
unbelievably beautiful, but evidence taken from
ancient samples prove that it ranges through a
rather uninspiring series of reds and purples. After
seeing it, we wish that Homer had written about
some of today's inexpensive coal-tar purples and
reds. A far more beautiful natural color was
introduced to Europe from Mexico in 1518, the
brilliant scarlet dye cochineal, which had been
produced from tiny lice which infest certain types
of cactus.

SYNTHESIS
 Today’s experiments deal with a class of
compounds called Azo dyes, compounds that
contain two aromatic fragments connected by a
N=N double bond. You may have encountered
these in chemistry experiments as they are typical
pH indicators. Methyl yellow, methyl orange,
methyl red, congo red and alizarine yellow are
some of the examples. They are straightforward to
make and of industrial importance. Azo dyes are
prepared in a two step reaction, the first being the
synthesis of an aromatic diazonium ion from an
aniline derivative. The next step is coupling of the
diazonium salt with an aromatic compound (shown
below is the preparation of methyl yellow). The
colours of azo dyes include different shades of
yellow, red, orange, brown, and blue.
 aim
preparation of an azo dye and use it to
dye a piece of cotton.
 Apparatus 
 Beakers, 10 cm3, x3
 Thermometer
 Tweezers
 Chemicals
 Ice
 Aminobenzene (aniline)
 Hydrochloric acid (concentrated)
 Sodium nitrite
 2-Naphthol (also called β-Naphthol; naphthalene-2-
ol)
 Sodium hydroxide solution, 2 mol dm–3
 Ethanol
 Urea

PROCEDURE
Put eight drops of aminobenzene in a 10 cm3 beaker and add 30
drops of deionised water followed by 15 drops of concentrated
hydrochloric acid. Swirl the beaker and then put it in an ice bath.
 Weigh 0.15 g of sodium nitrite into another beaker and add 1 cm3
of deionised water. Cool the beaker in the ice bath. Add one
spatula of urea (this prevents side reactions occurring).
 Mix the contents of the two beakers together and keep in the ice
bath.
  Weigh 0.45 g of 2-naphthol into another beaker and add 3 cm3 of
sodium hydroxide solution. Swirl to dissolve.
 Take a piece of cotton cloth 2 × 2 cm2 and, using tweezers, dip it
into the 2-naphthol solution. Allow the solution to completely soak
the cotton.
 Dip the cloth completely into the diazonium salt solution. A red
dye forms in the fibres, dyeing the cloth.
 Take the cloth out, wash it under the tap and leave to dry.

Observations

The orange-red azo dye forms in the fibres of the cotton, dyeing the cloth. The
melting point of 1-phenylazo-2-naphthol is 133 °C.

Health, safety and technical notes

 Read our standard health and safety guidance.

 Students must wear suitable eye protection (splash resistant goggles to BS

EN166 3).

 This experiment should be done in a fume cupboard.

 Aminobenzene (aniline) is TOXIC by all routes, a carcinogen and mutagen,

a skin sensitiser, causes eye damage and is toxic to aquatic life .

 Hydrochloric acid, HCl(aq), is CORROSIVE and a respiratory irritant (see

CLEAPSS HazCard HC047a).

 Sodium nitrite, NaNO2, is an OXIDISER, toxic if swallowed and hazardous

to aquatic life (see CLEAPSS HazCard HC093).

 2-Naphthol is HARMFUL if swallowed or in contact with skin and toxic to

aquatic life (see CLEAPSS HazCard HC070b).

 Sodium hydroxide solution, NaOH(aq), 2 mol dm–3 is CORROSIVE (see

CLEAPSS HazCard HC091a).
  Ethanol is highly FLAMMABLE (see CLEAPSS HazCard HC040a).

VAT DYES
INTRODUCTION
The name ‘vat’ comes from the wooden vessel which
was first used for the reduction and application of vat
dyes. Vat dyes are made from naturally not synthetically.
Vat dyeing is widely used for coloration of cellulose
materials such as cotton. Vat dye can’t be directly
applied and required vatting because it is insoluble in
water. However, they can be made soluble by reduction
in alkaline solution which allows them to affix to
the textile fibers. Subsequent oxidation or exposure to
air restore the dye to its insoluble form. Indigo is the
original vat dye. These dyes are the fastest dyes for
cotton, linen and viscose. They are used with mordants to
dye other fabrics such as wool, nylon, polyesters and
acrylics. But vat dyes fastness properties is good among
the all dyes. The dye takes their generic name from
vatting. The vat dyes are naturally obtained coloring
materials from the ancient time and kept into wooden vat
and make soluble in vat by the process of fermentation-
 so it is called vat dye

HISTORY
The first synthetic vat dye (indigo) was
discovered in 1880 by Adolf von Baeyer. In
1901, indanthrene was the first vat dye to be
sold commercially. In general, vat dyes are
very resistant to washing and sunlight. They
are used on Cotton, Linen, Rayon, and
Cellulose acetate. Other examples of vat
 dyes include several anthraquinone
derivatives such as synthetic alizarin and
Alizarin yellow.
What is Vatting?
Vatting is the process of converting the
insoluble vat dyes into its soluble form.
Because our ultimate goal is to dye the
substrate evenly in an aqueous medium. And
the insoluble vat dye displays no
substantivity towards cellulose, but the
soluble form does. With the help of a
suitable reducing agent and alkali, we can
convert the insoluble vat dye into its soluble
leuco form. This usually results in a change of color.

Pretreatment for Vat Dyeing:

Before vat dyeing, pretreatment is very important; it
should ensure that the substrate has a high and uniform
dye uptake and absorbency, is virtually free of husks, has
 a sufficiently high standard of whiteness, but must not
cause any significant damage to the cellulose.
Pretreatment is carried out by boiling off in the presence
of alkali and dispersing and sequestering agents. Further
improvement in the absorbency can be achieved by a
treatment with a high concentration of alkali (causticising
or mercerizing). Prior to dyeing, size is removed from
woven fabrics by the usual methods.

Aim
Preparation of vat dyes.

Typical Recipe for Vat Dyeing:

A typical recipe for a dye liquor would be:
1. Caustic soda (27% by weight), 5 ml l–1;
2. Hydrosulphite, 1.5 g l–1;
3. Stock vat, 62.5 ml l–1.
4.

Application of Vat Dye:

The application of a vat dye consists of the following
steps:
 Application of the vat dye in insoluble, disperse form
(pigmentation)
 Reduction of the dyestuff by appropriate reduction
agents
 Dissolution of the reduced (leuco) form of the dye
 Exhaustion of the dye from the dyebath/adsorption of
the reduced dye in continuous dyeing processes
 Levelling of the dye to achieve uniform dyestuff
distribution
 Oxidation of the reduced dye into the insoluble
pigment form
 Soaping to achieve the final particle distribution and
tone
 Rinsing to remove chemicals and neutralise the
material
Precautions in Vat Dyeing:
To get uniform level dyeing results, the concentration
of sodium hydro sulphite and caustic soda must be in
exact quantity to reduce the dye bath during whole the
process. Excessive quantity of reducing agent and alkali
decrease the exhaustion rate of the dyeing. Similarly
insufficient quantity of chemicals produce adverse
effect on dyeing so to control this balance
Phenolphthalien paper and Hydro papers are used.
Phenolphthalien Paper: It is white paper which turns in
pink color while contact with caustic soda.
Vat Yellow Paper: It is gold yellow paper which turn in
blue-violet color if hydro is available in dye bath.
It is also advisable that dyeing with two or three dyes
combination must be from same group of dyes. So
behavior of dyes is an important chapter to get uniform
results. Vat dyeing is the most difficult dyeing as
compared to other dyeings.