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PREPARATION OF DYES
JACOB BABU
18-PCH-010
I take this opportunity to express my deep sense of gratitude to all those
who have contributed significantly by sharing their knowledge and
experience in the completion of this project work. I am greatly obliged to,
for providing me with the right kind of opportunity and facilities to
complete this venture.
I take this opportunity to express my heartfelt gratitude, an appreciation
to the management of KIRI DYES AND CHEMICALS PRIVATE
LIMITED.
Lastly, I bow my head before my father Mr. Rajendra Babu and my
mother Mrs. Beena Babu for their supreme sacrifice and eternal
benediction in evolving my personality. Their inspiration has made this
industrial training a great success.
JACOB BABU
18 PCH -010
INDEX
Sr. No. CONTENTS Page No.
1. INTRODUCTION
4. ● DIAZOTIZATION
● COUPLING
● CYNURATION
● CONDENSATION
5. QUALITY CONTROL
9. REFRENCES
INTRODUCTION
● Kiri Industries Limited (KIL) is one of the largest manufacturer and exporter of wide
range of Dyes, Intermediates and Chemicals from India. KIL, a fully integrated Dyes
and Chemicals company is a winner of several CHEMEXCIL and GDMA performance
awards. KIL is a preferred resource centre for many of the most extensive product
lines in textile dyes.
● The company came into being in 1998 with the setting up of Dyes manufacturing unit
at Vatva, Ahmedabad. KIL is an ISO 9001:2008-certified company listed on Bombay
Stock Exchange and National Stock Exchange of India. In 2007, KIL embarked upon
two stage backward integration by setting up India’s largest Dyestuff intermediate
manufacturing facility and largest basic chemicals facility at Padra (Baroda,
Gujarat). To strengthen its competitive edge in the Dyes vertical, KIL formed Joint
Venture with Long Sheng (China) and set up manufacturing facility for Dyes at Padra
( Baroda, Gujarat ).
● In the 15 years of its corporate journey, KIL is focusing on providing products of high
quality, collaborations and strategic acquisitions, application & environment aligned
R&D, innovative solution-centric and all-encompassing customer care. KIL is
accredited with many revolutionary innovations in the process and chemistry of
producing dyes and dyes intermediates.These have enabled it to contribute towards
cost rationalizations for customers, improved compliance with sustainability norms.
● All initiatives taken by KIL have enabled it to set its footprint in over 50 countries
across 7 continents.
Direct Dyes
• Direct dyes are cheap and easy to apply, but of poor fastness
quality.
• These dyes are also known as „salt dyes‟ or cotton colours.
• They are readily soluble in water.
• They are applied to Cellulose fibres from aqueous liquor in which
an electrolyte is added, which is usually Sodium Chloride as it accelerates
the rate at which the dye is picked up by the fibres.
Acid Dyes
• These are soluble in water and are applied under acidic conditions.
• The acid dyestuff is mostly used for wool and silk and to a less extent
nylon and acrylic fibres.
• Acid dyes are inexpensive dyes.
• They are fast to light, but they are not fast to washing.
Vat dyes
• They are insoluble in water, but they are made
soluble by the use of a strong reducing agent, such
as Sodium hydrosulphite dissolved in sodium
hydroxide.
• These are the fastest dyes for cotton, linen and
rayon.
• They also may be applied to wool, nylon,
polyester etc.
• Vat dyes are hot water dyes.
• Hot water dyes are available in both powder and liquid form.
Basic dyes
• The first coal tar dye was a basic dye.
Disperse dyes
• The fibres that are most commonly
dyed with disperse dyes are
cellulose diacetate, cellulose
triacetate and polyester fibres. To a
lesser extent acrylic and nylon fibres
are also dyed with disperse dyes.
• Polyester fibres being hydrophobic
and with significant crystalline
content, the assistance of high
temperature, high pressure and carriers (which swell the fibre) is taken to
achieve satisfactory dyeing.
Reactive dyes
• They were first developed in 1956 by I.C.I., U.K.
• The dye is retained by means of a chemical reaction between the dye and
the fibre. As such their fastness properties are excellent.
• The fibres most readily coloured with reactive dyes are natural and man
made cellulosic fibres, natural protein fibres and polyamide fibres.
• With some reactive dyes, the dyeing can be carried out at room
temperature. However with most reactive dyes, the dyeing is carried out at
high temperatures (upto the boil).
• Reactive Dyes are the most versatile and popular class of Organic Dyes
for importing color on cellulosic fibers. As the name suggests, these dyes
chemically react with cellulose to form a covalent bond between dye
molecule and cellulose.
• The salient features of
Reactive Dyes are,
Overall good fastness
properties.
Economy.
Ease of application.
Their brilliant shades.
• The entire production process of dye is carried out in four steps :
1. Diazotisation.
2. Coupling.
3. Cynuration.
4. Condensation.
These are the four main process which has been used for preparation of
dye. But it is not compulsory that this should be in specific order. They can
be used according to their necessity like in some preparation cynuration is
done earlier and diazotization done later.
For making ice firstly they pass the cold ammonia from container 1 to the
machine which is worked as refrigerator. In that machine the condenser
and a large coil is set in that ammonia is passed and water is also passed
there in small amount. Because of that liquid (water) is converted to ice. Ice
is deposited on the wall of coil. Then there are shafts which moves in
circular motion and remove all the ice from coil and get stored in a
container or it is directly produced it is required. We use the cold ammonia
but after making ice it became hot. So it is again collected to container 2
and cool it for next use.
BASIC DEFINATIONS
DIAZOTISATION
• The diazonium salts have the general formula R-N2+ X- where R stands
known as diazotisation.
COUPLING
• In organic chemistry coupling reactions are reactions where two
hydrocarbon fragments are joined together with the aid of a metal catalyst.
CYNURATION
• Cynuration can be defined as the process of treatment of dye material
• After the Diazotisation and Coupling is done Cynuric Chloride is added
• Cynuration is carried out in a reactor in the controlled temp. condition
(below 5°C).
• Calsoline oil and octonol oil is used as a foaming agent such that cynuric
amount.
CONDENSATION
• It is the final step of the process in which cynurated product is cooled
down.
• Later on the dye is sent to the plate and frame unit, followed by R.O.
System.
PROCEDURES OF EACH PLANT:
1. Diazotization process :-it is the main process where diazo compound
is formed for making dye. For the specific color of dye specific raw
material are used. There are 2 main things which we have to be very
careful about temperature and pH. The normal reaction of
diazotization is as follows :-
Firstly water is taken and add concentrate HCL as per the raw
material is used then start the stirrer.
Then add raw material as per requirement of dye product. Let it stir
for 10-15 min (time may vary according to weight of raw material).
Now add the ice to the container to maintain temperature 0-5°c.
after maintaining the temperature now we add the nitric acid for the
diazo compound. We have to add in a very small-small portion and
after each addition we have to check the theph by congo red paper
(take a piece of congo red paper and put a drop of thethat solution
and that paper should turn blue in the whole process).
After each addition of the nitric acid we should also see the
diazotization is done properly or not. We can check it by the starch
iodide paper. For that we have taken a small drop of the solution
and that will turn to dark bluebut after some time it will disappear
so we have to add the nitric acid till that dark blue color will not
disappear. Now it is the indication that our diazo compound is
formed.
In this whole process temperature should remain 0-5°c if it will
increase then ice should be added and pH is also maintained by
adding concentrate HCL.
The reaction mechanism for
diazotization is:-
completely formed.
After 10-15 min of stirring we can now add the sodium
to 4.5 actually it has to rise at 5.5 but SBC and other
solution it has been raised till 4.5 and after coming to room
When we add SBC it starts making form so there is the
Thin-layer chromatography
Thin-layer chromatography is performed on a sheet of glass, plastic, or
aluminium foil, which is coated with a thin layer of adsorbent material,
usually silica gel, aluminium oxide (alumina), or cellulose. This layer of
adsorbent is known as the stationary phase.
After the sample has been applied on the plate, a solvent or solvent mixture
(known as the mobile phase) is drawn up the plate via capillary action.
Because different analytes ascend the TLC plate at different rates,
separation is achieved.[2] The mobile phase has different properties from
the stationary phase. For example, with silica gel, a very polar substance,
non-polar mobile phases such as heptane are used. The mobile phase may
be a mixture, allowing chemists to fine-tune the bulk properties of the
mobile phase.
After the experiment, the spots are visualized. Often this can be done
simply by projecting ultraviolet light onto the sheet; the sheets are treated
with a phosphor, and dark spots appear on the sheet where compounds
absorb the light impinging on a certain area. Chemical processes can also
be used to visualize spot.
To quantify the results, the distance traveled by the substance being
considered is divided by the total distance traveled by the mobile phase.
(The mobile phase must not be allowed to reach the end of the stationary
phase.) This ratio is called the retardation factor (Rf).
Quality Control
Quality control is set of technique in
which the application of dye is checked.
The dye is only important when it can be
used and this company make dye for
coloring cotton cloth, paper, etc.
For this it had to go from many test which
decide the dye is good or bad.
Some properties are there which is
necessary to check for dye before distributing to customer which are as
follows:-
1. Color fastness:- this measure the rasistance of the textiles when they
are exposed to various agencies. The usual practice is to apply the
dye on the fabric in specified strength and subjected to the various
agencies. Here is the machine where the tubes are filled with the dye
a cotton fabric is putted in it. According to the dye some retarders,
fixatives and other chemicals added for good coloration.
2. Light fastness:- the dye is subjected to different wavelenght light and
we had to see that color on the cloth has been changed (fad) or not.
According to the to change that has been given no. between 1-5.
3. Sublimation test:- they colored dye fabric is placed near the
uncolored dye fabric and alteration in color and degree are noted.
Gives the grade between 1-5.
4. Washing test:- in this test we will check the dye by washing that it
will not go with the water. And it stays on the cloth because we wash
the cloth regularly and if the color removes then it has no use. So the
colored cloth taken and washed 2-3 times and at last we check the
color.
INTRODUCTION OF RE BLACK B DYE
• Pigments or dyes that absorb light rather than reflecting it back
to the eye "looks black" i.e. complete absorption of visible
light.
• The most common early dyes were made from bark, roots or
fruits of different trees.
• Since the mid-19th century, synthetic black dyes have largely
replaced natural dyes. One of the important synthetic
blacks is “Nigrosin”. A mixture of synthetic black dyes (CI
50415, Solvent black 5) made by heating a mixture of
nitrobenzene, aniline and aniline hydrochloride in the
presence of a copper or iron catalyst.
• The main industrial application of black dye is as a colorant,
lacquers, varnishes and in “marker-pen inks”.
• The first commercial black dye “aniline black” was discovered
and found to be Water insoluble.
• Then the discovery of water soluble aniline black was done, also
known as “nigrosin”( C.I. Acid black 2)
• “C.I. reactive black 5” is the world‟s largest selling reactive dye,
Introduced by Hoechst in 1957 as Ramazol Black B. It is a
“di- azo dye” containing two vinyl sulphone groups.
It is the plant where the black and dark blue colour is prepared. they
have different plant for this dark colour because they are dark and they
can’t be prepared in same container where other colour dye is prepared.
But we use different raw material and different intermediate for this
dark color. As for example copper sulphate is used for blue colour dye.
The prepared dye is then pass to the filter press as same as reactive
plant where the mother liquid and pure dye product will be separated.
Then the cake of the dye product is formed.
After this the dye product is transfered for the quality analysis.
Where the dye is made correctly or not is checked. By the HPLC, GC, TLC
technique which are fully automatic software machinery program and give
the idea about product is formed as compared to the standard value. These
are values is checked in every steps.
Then it is transfer for the Quality control. In the quality control the
application mode of the dye is checked on the fabric. In which the some
most important properties are examine such as light fastness, washing,
color, sublimation property, moisture in it every thing is checked before
packing and giving it to the customers.
Raw materials used in Black plant:
• Caustic Lye
• Sodium Nitrite (NaNO2)
• Hydrochloric Acid (HCl)
• Ice (Ice Water – Cold Water) & Ammonia (NH3)
• Sulfamic Acid
• Acetic Acid (CH3COOH) & Sodium Acetate (CH3COONa)
• Soda Ash (Sodium Carbonate – Na2CO3) & Sodium per sulphate
(Sodium hydrogen sulphate – NaHSO4)
• Sodium bi carbonate (Sodium hydrogen carbonate – NaHCO3)
• Vinyl Sulphone
• H – Acid
• Cyanuric Chloride
• Meta Phenylene Di Sulphonic Acid (M.P.D.S.A.)
• Copper Sulphate (CuSO4)
• Hydrazone
• Caustic Soda flakes (NaOH powder)
• EDTA – 2Na (disodium salt of Ethylene Diamine Tetra Acetic acid –
E.D.T.A.)
• Oxalic Acid & Reverse Osmosis (R.O.)
• Celsolene Oil
• Octanol & Filter Press (Plate & Frame – P & F filter)
• Sulphuric Acid (H2SO4) & Oleum (H2SO4 + SO3 gas = H2S2O7 – Oleum)