PREPARATION AND APPLICATION OF NATURAL DYE ON

YARN (EXTRACTED FROM BEETROOT PEEL)

PROJECT REPORT
Submitted in partial fulfilment of the requirements to
ACHARYA NAGARJUNA UNIVERSITY
for the Award of the Degree of

BACHELOR OF TECHNOLOGY
IN
CHEMICAL ENGINEERING

by

P. SAI MOUNIKA (Y11CH841)

T. DEEPAK KUMAR (L12CH866)

Under the Guidance of

Sri. K. Ramesh Chandra,
M.Tech., MIICHE., MISTE.,
Assistant Professor

DEPARTMENT OF CHEMICAL ENGINEERING

R.V.R. & J.C. COLLEGE OF ENGINEERING
(Autonomous)
CHOWDAVARAM, GUNTUR-522019
Andhra Pradesh :: India
2014 2015
 R.V.R. & J.C. COLLEGE OF ENGINEERING
(Autonomous)
DEPARTMENT OF CHEMICAL ENGINEERING

CERTIFICATE

This is to certify that the Project Report entitled PREPARATION AND

APPLICATION OF NATURAL DYES ON YARN is a bonafide record work done

by P. Sai Mounika (Y11CH841) and T. Deepak Kumar (L12CH866) in partial

fulfillment of the requirements for the award of BACHELOR OF TECHNOLOGY IN

CHEMICAL ENGINEERING during the academic year 2014 2015.

(K. Ramesh Chandra) (Dr.M.Venkateswara Rao)

Project Guide Professor & Head
 ACKNOWLEDGEMENT

The successful completion of any task would be incomplete without a proper

suggestion, guidance and environment. Combination of these three factors acts like
backbone to our project Preparation and application of natural dye on yarn
(Extracted from beetroot peel)

We are pleased to acknowledge our heartful thanks to our project guide

K.RAMESH CHANDRA, assistant professor of Chemical Engineering for his guidance,
frequent advices, valuable suggestions and encouragement to complete this Project
Report

We whole heartedly thank Dr. M. Venkateswara Rao, Head of the department of

Chemical Engineering and all faculty members for providing the necessary facilities to
complete this term paper successfully.

We also wish to acknowledge our deep sense of gratitude to Dr. A. Sudhakar,

Principal for his help in the completion of this term paper with in the college premises.

A word of special thanks to my friends for their great help and co-operation in
bringing out this project successfully

P. SAI MOUNIKA
(Y11CH841)

T. DEEPAK KUMAR
(L12CH866)
 CONTENTS

S.NO TITLE PAGE.NO

1 INTRODUCTION

2 HISTORY OF DYES

3 WAVE LENGTH AND ABSORBANCE OF

ORGANIC DYES

4 TYPES OF DYES

5 CLASSIFICATION OF DYES

6 ORIGIN AND HISTORY OF NATURAL DYES

7 TYPES OF NATURAL DYES

8 PROCESSES EMPLOYED FOR EXTRACTION

9 STATUS OF NATURAL DYES IN INDIA

10 APPLICATION OF THE PROJECT

11 OVERVIEW OF THE PROJECT

12 MOTIVE BEHIND THE PROJECT

13 MATERIALS USED

14 EQUIPMENT USED IN THIS PROCESS

S.NO TITLE PAGE.NO

15 METHOD OF EXTRACTION

16 PROCEDURE OF EXTRACTION

17 APPLICATION TO SUBSTRATE

18 FASTNESS TESTS

19 RESULTS OF FASTNESS TESTS

20 STRENGTH TEST

21 ADVANTAGES AND DISADVANTAGES

22 COST ESTIMATION

23 LITERATURE SURVEY

24 RESULTS AND DISCUSSIONS

25 BIBLOGRAPHY
 1. INTRODUCTION

Dying is an ancient art which predates written records. It was practiced since
Bronze Age. The widely and commercially used synthetic dyes impart strong colours but
causes carcinogenicity and inhibition of benthic photosynthesis. Germany was the first to
take initiative to put ban on numerous specific azo-dyes for their manufacturing and
applications. Netherlands, India and some other countries also followed the ban. Certain
problems with the use of natural dyes in textile dyeing are colour yield, complexibility of
dyeing process, reproducibility results, limited shades, blending problems and inadequate
fastness properties. But these problems can be overcome by using chemicals called as
mordants. Mordants are metal salts which produce an affinity between the fabric and the
Dye.

Metal ions of mordants act as electron acceptors for electron donors to form co-
ordination bonds with the dye molecule, making them insoluble in water. Alum, Chrome,
Stannous Chloride, Copper Sulphate, Ferrous Sulphate etc. are the commonly used
mordants. Cotton textile dyeing was done since the medieval period using cheap natural
dyes.

Nature has gifted us more than 500 dyes-yielding plant species. Colouring agents
of these plants are derived from roots, leaves, barks, trunks or fruits. All colours of
rainbow are obtained from plants. Natural dyes have better bio degradability and
generally have higher compatibility with the environment. They are non toxic, non-
allergic to skin, non-carcinogenic, easily available and renewable.

Beets are a unique source of phytonutrients called betalains. Betanin and

vulgaxanthin are the two best-studied betalains from beets, and both have been shown to
provide antioxidant, anti-inflammatory, and detoxification support. The detox support
provided by betalains includes support of some especially important Phase 2 detox steps
involving glutathione. Although you can see these betalain pigments in other foods. The
concentration of betalains in the peel and flesh of beets gives you an unexpectedly great
opportunity for these health benefits.
 2. HISTORY OF DYES

Until the 1850s virtually all dyes were obtained from natural sources, most
commonly from vegetables, such as plant, trees, and lichens, with a few from insects.
Solid evidence that dyeing method are more than 4,000 years old has been provided by
dyed fabric in Egyptian tombs. Ancient hieroglyphs describe extraction and application
of natural dyes. Countless attempts have been made to extract dyes from brightly
coloured plants and flowers; yet only a dozen or so natural dyes found widespread use.
Undoubtedly most attempts failed because most natural dyes are not highly stable and
occur as components of complex mixtures, the successful separation of which would be
unlikely by the crude methods employed in ancient times. Nevertheless, studies of these
dyes in the 1800s provided a base for development of synthetic dyes, which dominated
the market by 1900.

Two natural dyes, alizarin and indigo have major significance. Alizarin is a red
dye extracted from the roots of the madder plant, Rubia tinctorium. Two other red dyes
were obtained from scale insects. These include kermes, obtained from Coccus ilicis,
which infects the Kermes oak and cochineal, obtained from Dactylopius Coccus, which
lives on prickly pear cactus in Mexico. One kilogram of cochineal dye can be obtained
from an estimated 200,000 insects. The principal coloured components in these dyes are
Kermesis and Carminic acids, respectively, whose similarity was established by 1920. In
their natural state many colorants are rendered water-soluble through the presence of
sugar residues. These sugars, however, are often lost during dye isolation procedures.
 3. WAVE LENGTH AND COLOUR ABSORPTION IN
ORGANIC DYES

Wavelength Absorbed Colour Absorbed Colour Observed

(nm)

400 435 Violet Yellow Green

435 480 Blue Yellow

480 490 Green Blue Orange

490 500 Blue Green Red

500 560 Green Purple

560 580 Yellow Green Violet

580 595 Yellow Blue

595 605 Orange Green Blue

605 700 Red Blue Green

 4. TYPES OF DYES

Natural dyes
Synthetic dyes

NATURAL DYES:
The word natural dye covers all the dyes derived from 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 fiber. 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/colorants when a textile
material being impregnated with such metallic salt is subjected to dying with different
natural dyes, usually having some mordantable groups facilitating fixation of such
dye/colorant. These modants after combining with dye in the fiber, it forms an insoluble
precipitate or lake and thus both the dye and mordant get fixed to become wash fast to a
reasonable level.

SYNTHETIC DYES:
The English chemist William Perkins accidently discovered the synthetic dye,
mauve, in 1856, while he was trying to synthesize quinine in aniline. Before that time, all
coloring materials were extracted from barks, roots, seeds, leaves and shellfish. Most
synthetic dyestuffs are made from coal-tar derivatives. Their manufacture is a highly
complicated technical operation, which is constantly changing. There is variation in the
manner in which different fibers respond to dyestuffs and even the same fibers do not
produce a full range of colours with a particular type of dye.
 5. CLASSIFICATION OF DYES

BASIC OR CATIONIC DYES:

This group was the first of the synthetic dyes to be taken out of coal-tar
derivatives. As textile dyes, they have been largely replaced by later developments.
However, they are still used on discharge printing, and for preparing leather, paper, wood,
and straw. More recently they have been successfully used with some readymade fibers,
especially the acrylics. The name means that these are dyes with an organic material,
which is soluble in a simple acid. Basic dyes were originally used to colour wool, silk,
linen, hemp etc., without the use of a mordant, or using agent. With a mordant like tannic
acid they were used on cotton and rayon. Basic dyes give brilliant colours with
exceptional fastness to acrylic fibers. They can be used on basic dyeable variants of nylon
and polyester. Nowadays basic dyes are no longer used to any great extent on cotton or
linen and seldom fibers. Their most important use today is on acrylics. They can also be
used on basic dyeable variants of nylon and polyester.

DIRECT DYES:

Historically, the direct dyes followed the basic dyes were and widely hailed
because they made it unnecessary to use a mordant or binder in dyeing cotton. The
colours are not brilliant as those in the basic dyes but they have better fastness to light and
washing and such fastness can be measurably improved by after treatments (diazotized
and developed). Direct dyes can be used on cotton, linen, rayon, wool, silk and nylon.
These dyes usually have azo linkage N=N and high molecular weight. They are water
soluble because of sulfonic acid groups.
ACIDIC DYES:

This is a very large and important group of dyestuffs. While an acid dye is a salt
the colour comes from the acidic component, while in the basic dye its from the organic
base. He first acid dyes were combinations of basic dyes with Sulphuric or Nitric acid.

Adding metallic salts especially chrome to the dyed fabric in an after-treatment generally
has increased colour fastness of acid dyes. Acid dyes cannot be used for wool tops but are
used in dyeing wool piece goods, silk, nylon and some of the other manmade fibers. If a
mordant is used they will successfully dye cotton and linen, though this is seldom done
today. The ordinary type of acid dye is reserved largely for apparel fabrics and for
knitting and rug yarns. A great deal of it is used on nylon carpeting.

PRE-METALIZED DYES:

This is an important group of acid dyes, which have been complexed with metallic
ions to improve light fastness on woll and nylon.

SULPHUR DYES:

The Sulphur dyes provide very deep shades, which have excellent resistance to
washing but poor resistance to sunlight. They will dye cotton, linen and rayon, but not
brightly. Sulphur dyed fabrics therefore usually must be treated with alkalis to neutralize
the acids, which have found.

AZOIC DYES:

These dyes are used primarily for bright red shades in dyeing and printing sice
most other classes of fast dyes are lacking in good red dyes. Azoic dyes, called Naphthols
in the industry, are actually manufactured in the fabric by applying one half of the dye.
The other half is then put on and they combine to form the finished colour. Unless they
are carefully applied and well washed, they have poor fastness to rubbing or crocking.
VAT DYES:

These are perhaps the best known group of dyes in use today because of their all
round fastness to washing and sunlight on cotton and rayon. The term vat comes from the
old indigo method dyeing in a vat: indigo had to be reduced to light form. Vat dyes are
made from indigo, anthraquinone and carbazole. They are successfully used on cotton,
linen, rayon, wool, silk and sometimes nylon. Vat dyes are also used in the continuous
piece of dying process sometimes called pigment application process. In this method the
dyes are not reduced before application, but after they have been introduced into the
fabric. This makes for a dyeing superior appearance and economy. There are no light red
vat dyes.

Soluble Vats: There are no water soluble preparations for dyes

Indigo: The oldest known vat dyestuff, formerly made from the indigo plant, but now
made synthetically.

COLLECTIVE DYES:

Collectives are the latest dyestuff and because they react chemically with cotton,
viscose, linen, wool and silk they are very fast to washing treatments. They can be dyed
and printed by many methods and for the first time, the whole spectrum of colour can be
put onto cloth using just one class of dyes. Substituting a reactive group on a direct dye
produces these dyes.

Dyes for Manmade Fibers:

Dyeing manmade fibers such as acetate, the polyacids, polyesters and acrylics,
etc., has proved to be a challenge to dyers. Each new fiber, as it emerges from the
laboratory, must be carefully analyzed and tested for its reaction to different dyestuffs.
The process has been continues experimentation with new developments turning up
constantly. To date both basic and acid dyes have been used as well as what is known as
disperse colours. A dispersed dye may be any one of a number of slightly soluble
dyestuffs dispersed, or held in suspension in the dye bath. Perhaps the best known
example is the dispersed dye method for colouring acetate, which cannot be dyed by any
other technique. For acetate dyes, the dye substance is derived from anthraquinone and
azoic dyes. It is ground in a colloid mill. When dispersed in dye bath (colloidal
suspension), the particles are microscopic and cannot be detected by the naked eye.

Alizarin Dyes:

These are vegetables dyes, originally derived from the madder plant and now
produced synthetically. They are used on wool and sometimes on cotton. They produce a
brilliant turkey red, among other colours.

Aniline Black:

They are produced from the chemical aniline, and are usually associate with the
colour black. Aniline black is a fast black, much used on cottons and its developed by
oxidizing the aniline on the fiber. It is very fast tot light, washing, and chlorine.

Chrome Dyes:

These are a special type of acid dyes and they are used to colour animal fibers,
especially woolens and worsteds, they will react well on a fabric with metals such as
chromium. The process, however, tends to dull the colour brilliance but does provide high
light fastness and wash fastness.

Neutral Dyes:

These are metal containing acid dyes and the metal is added in manufacture.

Acetate of Disperse Dyes:

Disperse dyes were originally developed for dyeing secondary cellulose acetate
fibers. These dyes relatively insoluble in water and are prepared for dyeing by being
ground into relatively fine powder in the presence of dispersing agents.
 6. ORIGIN AND HISTORY OF NATURAL DYES

Natural Dyes are dyes or colorants derived from plants, invertebrates, or

minerals. The majority of natural dyes are Vegetable Dyes from plant sources roots,
berries, bark, leaves, wood and other organic sources such as fungi and lichens.
Archaeologists have found evidence of textile dyeing dating back to the Neolithic period.
In China, dyeing with plants, barks and insects has been traced back more than 5,000
years. The essential process of dyeing changed little over time. Typically, the dye
material is put in a pot of water and then the textiles to be dyed are added to the pot,
which is heated and stirred until the colour is transferred. Textile fiber may be dyed
before spinning (dyed in the wool), but most textiles are yarn-dyed or piece-dyed
after weaving. Many natural dyes require the use of chemicals called mordants to bind the
dye to the textile fibers; tannin from oak galls, salt, natural alum, vinegar and ammonia
from stale urine were used by early dyers. Many mordants and some dyes themselves,
produce strong odors and large scale dye works were isolated in their own districts

Throughout history, people have dyed their textiles using common, locally
available materials but scarce dyestuffs that produced brilliant and permanent colours
such as the natural invertebrate dyes, Tyrian purple and crimson kermes, became highly
prized luxury items in the ancient and medieval world. Plant-based dyes such as woad
(Isatic tinctoria), indigo, saffron and madder were raised commercially and were
important trade goods in the economies of Asia and Europe. Across Asia and Africa,
patterned fabrics were produced using resist dyeing techniques to control the absorption
of colour in piece-dyed cloth. Such as cochineal and logwood (Haematoxylum
campechianum) were brought to Europe by the Spanish treasure fleets and the dyestuffs
of Europe were carried by colonists to America.

The discovery of man-made synthetic dyes in the mid-19th century triggered a

long decline in the large-scale market for natural dyes. Synthetic dyes, which could be
produced in large quantities, quickly superseded natural dyes for the commercial textile
production enabled by the industrial revolution and unlike natural dyes, were suitable for
the synthetic fibers that followed. Artists of the Arts and Crafts Movements preferred the
pure shades and subtle variability of natural dyes, which mellow with age but preserve
their colours, unlike early synthetic dyes and helped ensure that the old European
techniques for dyeing and printing with natural dyestuffs were preserved for use by home
and craft dyers. Natural dyeing techniques are also preserved by artisans by traditional
cultures around the world.

In the early 21st century, the market for natural dyes in the fashion industry is
experiencing a resurgence. Western consumers have become more concerned about the
health and environmental impact of synthetic dyes in manufacturing and there is a
growing demand for products that use natural dyes. The European Union, for example,
has encouraged Indonesian batik cloth producers to switch to natural dyes to improve
their export market in Europe. Dyes uses in the fashion industry.

Fiber content determines the type of dye required for a fabric:

Cellulose fibers : Cotton, Linen, Hemp, Ramie, Bamboo, Rayon

Protein fibers : Wool, Angora, Mohair, Cashmere, Silk, Soy, Leather, Suede

Cellulose fibers require fiber-reactive, direct/substantive and vat dyes, which are
colorless, soluble dyes fixed by light and/or oxygen. Protein fibers require vat, acid or
indirect/mordant dyes, that require a bonding agent. Each synthetic fiber requires its own
dyeing method. For example, Nylon requires acid, disperse and pigment dyes, rayon
acetate requires disperse and so on.
 7. TYPES OF NATURAL DYES

Natural dyes can be sorted into three categories. Natural dyes obtained from
plants, those obtained from animals and obtained from minerals. Although some fabrics
such as silk and wool can be coloured simply by being dipped in the dye, others such as
cotton require a mordant. A mordant is an element, which aids the chemical reaction that
takes place between the dye and the fiber so that the dye is absorbed. Containers used for
dyeing must be non-reactive brass, Copper or Iron pots will do their own moradanting.
Not all dyes need mordants, such as lichens and walnut hulls, they are called substantive
dyes. If they do need a mordant they are called adjective dyes.

Common mordants are: ALUM, usually used with cream of tartar, which helps
Evenness and brightens slightly; IRON which saddens or darken colours, bringing out
green shades; TIN, usually used with cream of tartar, which blooms or brightens colours,
especially reds, oranges and yellows; BLUE VITROL which saddens colours and brings
out green and TANNIC ACID used tans and browns.

One example of natural dyes obtained from is madder, which is obtained from the
roots of the madder plant. The plants are dug up, the roots are washed, dried and found
into powder. During the 19th Century, the most widely available fabrics were those which
had been dyed with madder the Turkey Red that was considered brilliant and exotic.
The madder plant continued to be used for dyeing until the mid 1800s when a synthetic
substitute was developed.

Another example of a natural dye obtained from plants is wood. Until the middle
Ages, Europeans used wood to create a blue fabric dye. The wood was widely used in
Europe. The colouring was in the leaves, which were dried and ground mixed with water,
and made into a paste. This dye was supplanted by Indigo an ancient shrub well known to
the Egyptians and Indians. Like wood, its colour lay in its leaflets and branches. The
leaves were Fermented, the sediment purified, and the remaining substance was pressed
into cakes.
 Indigo prevailed as the preferred blue dye for a number of reasons. It is
substantive dye, needing no mordant, yet the colour achieved is extremely fast to washing
and to light. The manufacture of natural Indigo lasted well into the early 1900s.

Natural dyes obtained from minerals Ocher is a dye obtained from an impure
earthy ore of iron or ferruginous clay, usually red or yellow. In addition to being the
principal ore of iron, hematite is a constituent of a number of abrasives and pigments.

Natural dyes obtained from animals:

A good example is cochineal, which is a brilliant and red dye produced from
insects living on cactus plants. The properties of the cochineal bug were discovered by
pre Colombian Indians who would dry the females in the sun and then ground the dried
bodies to produce a rich, red powder. When mixed with water, the powder produced a
deep, vibrant red colouring. In fact, most cherries today are given their bright red
appearance through the artificial colour Carmine, which comes from the cochineal
insect.

Name of Dyes from plants (Major Natural) :

ANNATO is from the pulpy part of the seeds on Indian plant. Bixa Orellana:
Fugitive orange red colour.

BRAZIL WOOD is from wood of the tree, caesalpinia Echinacea: bright red colour.

CUDBEAR comes from the lichen, Lecanora tartarea : lilac colour dye.

CUTCH is obtained from boiling the wood of Acacia catechu, native to India: rich brown
colour.

FUSTIC. OLD: Obtained from wood of tropical American tree. Chlorophora tinctoria:
gold to yellow in colour and still popular on wool.

FUSTIC. YOUNG or ZANTE: Comes from the powered wood of the Rhus cotinus, a
shrub size tree of the cashew family: yellow to dark olive in colour.
INDIGO is obtained from the plant, Indigofera tinctoria : blue colour.

KERMES is extracted from bodies of tiny insect, Coccus arborum; red dye.

LAC is obtained by boiling tree incrustation produced by tiny lac insect. Tachardia lacca;
bright red colour.

LOG WOOD comes from a Central Americans tree, Haematoxylon campechium; gives
purple on wool, blue and black in silk.

MADDER comes from the roots of the plant, Rubos tinctorum; red colour, Produces
alizarin.
 8. PROCESSES EMPLOYED FOR EXTRACTION

The essential process of dyeing requires soaking the material containing the dye
(the dyestuff) in water, adding the textile to be dyed to the resulting solution (the
dyebath), and bringing the solution to a simmer for an extended period, often measured in
days or even weeks, stirring occasionally until the colour has evenly transferred to the
textiles. Some dyestuffs, such as indigo and lichewns, will give good colour when used
alone; these dyes are called direct dyes or substantive dyes. The majority of plant dyes,
however, also require the use of a mordant, a chemical used to fix the colour in the
textile fibers. These dyes are called adjective dyes. By using different mordants, dyers can
often obtain a variety of colours and shade from the same dye. Fibers or cloth may be
pretreated with mordants, or the mordant may be incorporated in the dye bath. In
traditional dyeing, the common mordants are vinegar, tannin from oak bark, sumac or oak
galls, ammonia from stale urine, and wood-ash liquor or potash (potassium carbonate)
made by leaching wood ashes and evaporating the solution.

We shall never know by what chances primitive man discovered that salt, vinegar
from fermenting fruit, natural alum and stale urine helped to fix and enhance the colours
of his yarns but for many centuries these four substances were used as mordants. Salt
helps to fix or increase fastness of colours, vinegar improves reds and purples and the
ammonia in stale urine assists in the fermentation of indigo dyes. Natural alum
(aluminum sulfate) is the most common metallic salt mordant, but tin (stannous chloride),
copper (cupric sulfate), iron (ferrous sulfate, called copperas) and chrome (potassium
dichromate) are also used. Iron mordants Sadden colours, while tin and chrome
mordants brighten colours.

The iron mordants contribute to fabric deterioration, referred to as dye rot.

Additional chemicals or alterants may be applied after dyeing to further alter or reinforce
the colours. Textiles may be dyed as raw fiber (dyed in the fleece or dyed in the wool), as
spun yarn (dyed in the hank or yarn-dyed), or after weaving (piece-dyed). Mordants often
leave residue in wool fiber that makes it difficult to spin, so wool was generally dyed
after spinning, as yarn or woven cloth. Indigo, however, requires no mordant and cloth
manufacturers in medieval England often dyed wool in the fleece with the indigo-bearing
plant woad and then dyed the cloth again after weaving to produce deep blues, browns,
reds, purples, blacks and tawnies.

In China, Japan, India, Pakistan, Nigeria, Gambia, some other parts of West
Africa and Southeast Asia, patterned silk and cotton fabrics were produced using resist
dyeing techniques in which the cloth is printed or stenciled with starch or wax, or tied in
various ways to prevent even penentration of the dye when the cloth is piece-dyed.
Chinese ladao is dated to the 10th century; other traditional techniques include tie-dye,
batik, Roketsuzemo, Katazomo, bandhani and lecheria.

The mordants used in dyeing and many dyestuffs themselves give off strong and
unpleasant odors and the actual process of dyeing requires a good supply of fresh water
storage areas for bulky plant materials, vats which can be kept heated (often for days or
weeks) and airy spaces to dry the dyed textiles. Ancient large scale dye-works tended to
be located on the outskirts of populated areas on windy promontories.
 9. STATUS OF NATURAL DYES IN INDIA

India has a very rich tradition of using natural dyes. The art and craft producing
natural dyed textile has been practiced since ages in many villages by traditional expert
craft-persons in the country. Natural dyes, when used by themselves have many
limitations of fastness and brilliancy of shade. However, when used along with metallic
mordants they produce bright and fast colours. The use of metallic mordants is not always
eco-friendly, but the pollution problems created by metallic mordants are of very low
order and can be easily overcome. Therefore, instead of using unsustainable technology
for producing colours one can use Mild Chemistry to achieve almost similar results.
 10. APPLICATIONS OF NATURAL DYES

Natural dyes find use in the coloration of textiles, foods, drugs and cosmetics.
Small quantities of dyes are also used in coloration of paper, leather, shoe polish, wood,
cane, candles, etc. in the earlier days; dyes were derived only from natural sources. Some
processing was required but essentially the dye itself was obtained from a plant, mineral
or animal. After the accidental synthesis of mauveine by William Henry Perkin in 1856
and its subsequent commercialization, heralding the advent of coal tar dyes, the use of
natural dyes receded. A wide range of synthetic dye stuff was thrust upon the industry and
it was readily accepted for its distinct advantage over natural dyes with respect to
application, colour range and availability.
 11. OVERVIEW OF THE PROJECT

Use of natural dyes has increased several folds in the past few years due to the
eco-friendly approach of the people. This paper concerns with the purification of natural
dyestuff extracted from an abundantly occurring beet Beetroot Plant. The main colouring
agent in the Beetroot peel is Alizarin. Solvent extraction method was used for the
extraction of the dye. The Beetroot peel dye was used for dyeing of scoured cotton cloth
using two mordants-copper sulphate and ferrous sulphate in the ratio of 1:1, 1:3, 3:1.
Dying along with mordanting techniques which included pre mordanting, simultaneous
mordanting and post mordanting was carried out. Study about fastness tests of dyed
cotton yarn was undertaken. Large range was obtained because of varying mordant ratios
and combinations.

Structure of Alizarin:
 12. MOTIVE BEHIND THE PROJECT

In these days of sophisticated technology, we made many synthetic dyes to impart

colour to our cloths of which some are carcinogenic, some are allergic to skin and other
body organs. These dyes are mostly made from non biodegradable materials and thus are
so. Therefore the dyes prepared and applied to fabric are accumulating on the earth
causing a huge disposal problem. Therefore man is in search of ecofriendly materials and
methods to develop them. Hence we prefer natural dyes to synthetic dyes due to their
faster biodegradability, no or less pollution in the process preparation and wide ranges of
applications with slight modifications. In search of sources to extract dye from natural
stuff of plant and animal origin, the ruddy and attractive Beetroot Peel caught our
attention. We then started to search whether we can find a way to extract the colouring
matter from its ruddy peel, because it is usually thrown off and is a biodegradable waste.

Fortunately, we came across a research article entitled COTTON DYEING

WITH DYE EXTRACTED FROM BEETROOT PEEL. This initially disappointed us
since we thought of making this for the first time. When we had gone through the articles,
we found some scope to improve the content of the same by making necessary alterations
in the solvent used for extractions.

Hence we chose this topic with the intention to make suitable advancements
regarding the solvents used and substrates that used in the actual article. We used same
mordants and the method of dyeing and mordanting as used in the research article.
 13. MATERALS USED

Source:
Beetroot are the sources for extracting dye.

Substrate:
100% cotton yarn is the substrate.

Chemicals:
95% ethanol
Copper Sulphate
Ferrous Sulphate
 14. EQUIPMENT USED IN THE PROCESS

Weighing balance
These are widely used in weighing the substance of lower weights accurately.

Water bath:
Water bath are widely used in laboratories for boiling and general purpose work.
They are available in various types including single and double walled rectangular water
baths which can also be used for sterilizing, drying of objects and laboratory glassware.

Soxhlet apparatus:
A soxhlet extractor is a piece of laboratory apparatus invented in 1879 by
franzvon soxhlet. It was originally designed for
the extractor of a lipid from a solid materal.
However, a soxhlet extractor is a not limited to
the extraction of lipids. Typically, a soxhlet
extraction is only required where the desired
compound has a limited solubility in a solvent,
and the impurity is insoluble in that solvent. If the
desired compounds has a significant in a solvent
then a substance. An apparatus for extracting
components from a solid like extracting natural
products from plant materials. The material used
is placed in a thimble made of thick filter paper and this is held in a specially designed
reflex condenser with a suitable solvent. The chamber holding the thimble fills with warm
solvent and this is led back it the source via a side arm. The apparatus can be operated for
long periods, with components concentrating in the source vessel.

Hot air oven:

Hot air ovens are electrical devices used in sterilization. They are originally
developed by Pasteur. The oven uses dry heat to sterilize articles. Generally, they can be
operated from 50 to 300 0c .there is a thermostat controlling the temperature. These are
digitally controlled to maintain the temperature. Their double walled insulation keeps
the heart in ad conserves energy, the inner layer being a poor conductor and outer layer
being metallic.

Colorimeter:
A colorimeter is a device used in Colorimetry. In Scientific fields the word
generally refers to the device that measures the absorbance of particular wavelengths of
light by a specific solution. The device is most commonly used to determine the
concentration of a know solute in a given solution by the application of the Beer-Lambert
law, which states that the concentration of a solute is proportional to the absorbance.

The output from a colorimeter may be displayed by an analogue or digital meter

and may be shown as transmittance or as absorbance. The useful range of the absorbance
scale is from 0-2 but it is desirable to keep within the range 0-1 because, above 1, the
results become unreliable due to scattering of light.
 15. METHOD OF EXTRACTION
Solvent extraction was used for extracting the Dye

16. PROCEDURE OF EXTRACTION

Preparation of Raw material:

The peel samples were collected and washed thoroughly with water to remove any
impurities.

After drying at room temperature, the samples were ground into powder with the
help of grinder

Extraction of Crude Dyestuff:

100g of sample was weighed and taken in a round bottom flask and 500ml of
solvent (ethanol water) in the ratio of 40:60 was added to it. The flask was heated in a
water bath at 60C for 60mins. The solution was then filtered to obtain crude dyestuff.
 We used different concentrations of solvent while extracting the crude dye stuff.

Laboratory grade 95% Ethanol:

o The above procedure is followed as it is in this case of extraction.
75% Ethanol:
o The process is slightly modified in this case as the resulting solution is too
viscous to be filtered. So we employed centrifuge to separate dye from the
powder.

Calculating the yield with 95% alcohol:

Weight of sample taken = 25g
Weight of filter paper = 5.812g
Weight of sample along with paper after extraction = 26.182g
Percentage Yield = 18.52%

Calculating the yield with 75% alcohol:

Weight of sample taken = 25g
Weight of filter paper = 5.517g
Weight of sample along with paper after extraction = 27.235g
Percentage Yield = 13.12%

Purification of Crude Dyestuff:

The crude dyestuff is distilled to get 1/3rd of the solution using the Soxhlet
apparatus at 70C for 3hrs. in this process Ethanol is recovered and the concentrated dye
is obtained. The solution is kept overnight at a room temperature for precipitation. The
precipitation in ethanol water is obtained by decanting the solution. The obtained particles
are dried in the oven overnight at 60C. Water was added in the Soxhlet apparatus. By
addition of water, the boiling points of the compounds are lowered, allowing them to
evaporate at lower temperatures.
Whatever the concentration of solvent may be, the purification process remains
the same.
 17. APPLICATION TO SUBSTRATE

Scouring of cotton yarn:

Scouring of cotton yarn was done by initially washing it with a good quality
detergent, soaking it in distilled water for 24 hours and then washed to remove any traces
of seed remains and dried at room temperature. The scoured material was soaked in clean
water for 30 minutes prior to dyeing or mordanting.

Dyeing and Mordanting:

Accurately weighed cotton yarn was treated with different metal salts (Mordants
used cupric sulphate and ferrous sulphate). The process of mordanting used were
Pre mordanting:
It (Pre mordanting) is a technique that involves applying the mordant first and
then introducing the dye to the material. It is also called on-chrome treatment
Simultaneous mordanting:
Simultaneous mordanting employs the approach of combination the dye and then
mordant agent first, then applying the mixture to the material that is to be dyed. It is also
known as meta-chrome or meta-mordanting
Post mordanting:
Post mordanting involves dyeing the fabric first, then exposing the material to
mordants as a final treatment. It is also known as after-chrome treatment

After dyeing, the dyed material was washed with cold water and dried at room
temperature.
The mordanted cotton cloth was immediately used for dyeing because some mordants are
light sensitive. The chromatophore of the dye makes it resistant to photochemical attack,
but the auxochrome may alter the fastness. Good light fastness was observed in fabrics
dyed with the dye extracted from beetroot peel. This is due to the formation of complex
with the metal which protects the chromatophore from photolytic degradation. Wash
fastness of the dye is influenced by the rate of diffusion of the dye and state of the dye
inside the fiber. The fiber dyed with beetroot peel dye showed morderate wash fastness.
Good rub fastness was exhibited by the fibers dyed using the dye extracted from the
beetroot peel. Complexing the fiber with mordant has the effect of insolubilizing the dye,
making it colour fast
Conditions for dyeing and Mordanting:

Dye Mordant M:L Temperature Time

4% o.w.f. 2% o.w.f 1:40 80C 60 minutes

 18. FASTNESS TESTS

Colour fastness is the resistance of a material to change any of its colour

characteristic or extent of transfer of its colorants to adjacent white materials in touch. It
is a term used in the dyeing of textiles materials, meaning of the materials colour to
fading or running. In general, Yarns should be tested for colour fastness before using
bleach or other cleaning products. Fastness tests establish the fitness for purpose of the
fabric and help identify the appropriate care label instructions.

Colour fastness is a measure of two different properties of a textile, the degree to

which it changes colour when subjected to particular treatment or environment, and the
tendency for the textile to cause staining of other fabrics with which it comes into contact.
The colour fastness properties of a textile will be related to the type of fibers present, the
construction of the material and especially to the type of dyestuff used and the method by
which it has been applied.

Fastness properties depends on the strength of the attractive forces between the
dyes and the fiber. Light fastness, wash fastness and rub fastness that are standardized.

RUB FASTNESS TEST

DRY RUBBING:
With the dry rubbing yarn flat in place over the end of the finger of the crock
meter, some should be rubbed 10 times to and fro in a straight line along a track 10cm
long on the dry specimen in 10 seconds and with a downward force of 9 N.

WET RUBBING:
The above described procedure should be repeated with a fresh dry specimen and
with wet rubbing yarn. The wet rubbing yarn should be prepared by soaking a fresh
rubbing yarn in distilled water and squeezing the same to contain its own weight of water.
LIGHT FASTNESS:
The staining of the rubbing cotton yarn should be assessed with the help of a grey
scale. It is necessary to eliminate dyed fibers pulled out during rubbing and retained on
the surface of rubbing cotton yarn, the coloration due to staining by dye stuff only should
be considered. In case of doubt on the assessment of colour fastness rating by a single
observer, the assessment should be done by at least three observes and overall average
rating should be reported.

Factors affecting the light fastness:

Treatment of formaldehyde based cationic dye fixing agent tends to lower the
light fastness.
Light fastness lowers by half to one rating when dyes are used in combination as
compared to rating of individual component for a given depth.

Wash fastness test:

Washing Fastness Tester is used
widely for determining colour fastness of
textile materials to washings. The colour
fastness of textile material is determined by
way of mechanical hesitation of a specimen
of textile with the piece of specified adjacent
fabrics in Standard soap solution followed
by rinsing and drying. Thereafter, the
change in colour of specimen and stains of
the adjacent fabrics are assessed with standard grey scale.
 19. RESULT OF FASTNESS TEST
RUB FASTNESS:

LIGHT FASTNESS:

WASH FASTNESS:

From the pictures above, we can infer that the dye from beet root showed good quality.
 20. STRENGTH TEST
We find the strength of the yarn using this test:

Testing single yarns presents many problems due to the fine diameter of the yarns.
Yarn strength determination is further complicated by the fact that yarns are irregular and
as such their strength is strongly dependent on the testing conditions. Since the
probability of encountering a life-determining flaw increases with increasing length, yarn
with longer gauge lengths breaks at lower value of stress. Hence the strength of yarn is
not a single-valued property but a statistical variable.

Procedure:
Testing the strength of regular yarn:

1. At first one lea cotton yarn is measured by

wrap reel and in this way the sample is
taken for testing.
2. Now, the sample is fixed with the upper
jaw J1 and the lower jaw J2.
3. The m/c is started and observed the dial
until the sample is torn out.
4. When the sample is torn out the m/c is
stopped and the reading is taken. The
sample is weighted and counts are
calculated.
5. The value is nearly 42kgs
Testing the strength of coloured yarn:

1. At first one lea cotton yarn is measured by wrap

reel and in this way the sample is taken for
testing.
2. Now, the sample is fixed with the upper jaw J1
and the lower jaw J2.
3. The m/c is started and observed the dial until the
sample is torn out.
4. When the sample is torn out the m/c is stopped
and the reading is taken. The sample is weighted
and counts are calculated.
5. The value is nearly 42.5kgs
 21. ADVANTAGES AND DISADVANTAGES

Advantages:

Natural dyes are free of azo compounds

These are known as antioxidants
These dyes have the high potential to be sold at higher price
Natural Dyes consists less toxic, less pollution and less health hazardous than
Synthetic Dyes
These are non carcinogenic and non poisonous.

Disadvantages:

Natural dyes takes more time to extract dyestuff

The availability of Natural Dyes are LOW
Its dependent on the Climatic conditions, seasons etc
Synthetic fibers usually cannot be dyed with natural dyes.
 22. COST ESTIMATION

A cost estimate is the approximation of the cost of a program, project, or

operation. The cost estimate is the product of the cost estimating process. The cost
estimate has a single total value and may have identifiable component values.

COSTING OF THE BEETROOT PEEL DYE:

Cost sheet is a statement, which shows various components of total cost of a

product. It classifies and analysis the components of cost of a product. To fix the selling
price of a product or service, it is essential to prepare the cost sheet. It helps in fixing
selling price of a product or service by providing detailed information of the cost. The
costing was done taking into consideration the direct expenses, overheads and the
administration charges.
COST SHEET FOR 1Kg OF BEETROOT PEEL DYE:

TOTAL
S NO PARTICULARS RUPEES
RUPEES
Direct Material
a) Peel of Beetroot 2,500/-
1) b) Ethanol (40 L) 7,600/-
c) Water (60 L) 1,500/-
Total 11,600/-
Direct labor
2)
(Rs 500 for 5 days) 2500/-
Direct Expences
3) Oven distillation unit, Water bath and 1,800/-
Heating Mantle
Prime Cost 15,900/-
Additional over heads
4) Administrative Expenses (Including 250/-
travelling and stationary)
Packaging Materials 150/- 400/-
Total Cost 16,300/-
5) Profit Margin 10% 1,630/-
Selling Price 17,930/-
 23. LITERATURE SURVEY

1. Antibacterial Dyeing of Wool with Natural Cationic Dye Using Metal Mordants

Materials:
Woolen yarn (Nm = 400, 2 ply) was purchased from local wool spinning mill. To
remove any natural or synthetic impurities, the yarns were scoured using 2 g/l non-ionic
surfactant (Ultravon CN, Ciba) and 2 ml/l ammonia at 45 C for 30 minutes (L : G = 30 :
1) and then rinsed and air dried. L : G represents the liqour to goods ratio. 268 Fig. 1.
Chemical structure of Berberine [10] Berberis Vulgaris roots were first washed and dried
and then chopped and powdered. To prepare the original solution of the dye, each 100 g
of powder was added to 1 L of distilled water and boiled for 2 hours and then filtered.
The concentration of the resultant solution is 10 % W/V. Acetic acid and ammonia were
analytical grade reagents from Merck.
Methods:
Mordanting. The scoured wool yarns were mordanted using different amounts (1, 2, and
5 % owf) of alum, copper sulfate and potassium dichromate mordants at 80 C and L : G
= 30 : 1, for 45 minutes. Generally, mordanting was done prior to dyeing. After
mordanting the each sample was rinsed with 100 ml of distilled water. Dyeing. 100 ml of
original dye solution was mixed with 100 ml of distilled water for each 5 gram of wool (L
: G = 40 : 1). The pH of the dyebath was adjusted on 5 using acetic acid . The dyeing was
started at 40 C and the temperature was raised to final temperature (60, 70, 80, 90 C) at
the rate of 2 C per minute. Then the samples remained in that condition for appropriate
time (45, 60, 90 minute), and then rinsed and air dried. All mordanting and dyeing
processes were carried out using a laboratory dyeing machine made by Rissanj co.-Iran.

Fastness properties:
All fastness properties of dyed samples when mordanted are higher than when
nonmordanted . This increase is due to increase in size of dye molecules when connected
to metal atoms into the fiber [14]. Wet rub fastness was less than dry rub fastness because
the water molecules can dissolve some of watersoluble dye molecules and make them
easier to be removed from the fiber by rubbing. All fastness properties of mordanted and
then dyed wool fibers are generally acceptable.
2. Cotton Dyeing with Natural Dye Extracted from Pomegranate (Punica
granatum) Peel

Source: Pomegranates were purchased from Market Yard, Pune.

Substrate: 100% cotton cloth was purchased from Prakash Departmental Stores, Pune
Chemicals: Laboratory grade chemicals - 95% ethanol, copper sulphate and ferrous
sulphate
Methods:
Solvent extraction was used for extracting the dye.

Preparation of Raw Material: The samples were collected and washed thoroughly with
water to remove any impurities. After drying at room temperature, the samples were
ground into powder with the help of grinder (Win and Swe, 2008).

Extraction of Crude Dyestuff: 100 g of sample was weighed and taken in a round
bottom flask and 500ml of solvent (ethanol water) in the ratio 40:60 was added to it. The
flask was heated in a water bath at 60C for 60mins.The solution was then filtered to
obtain crude dyestuff (Win and Swe, 2008; Goodarzian and Ekrami, 2010).

Purification of Crude Dyestuff: The crude dyestuff is distilled to get 1/3rd of the
solution using the Soxhlet apparatus at 70C for 3hrs. In this process ethanol is recovered
and the concentrated dye is obtained. The solution is kept overnight at room temperature
for precipitation. The precipitation in ethanol water is obtained by decanting the solution.
The obtained particles are dried in the oven overnight at 60C (Win and Swe, 2008;
Goodarzian and Ekrami, 2010). Water was added in the soxhlet apparatus. By addition of
water, the boiling points of the compounds are lowered, allowing them to evaporate at
lower temperatures (Chowdhari et al.., 2004).

Dyeing and Mordanting: Accurately weighed cotton cloth was treated with different
metal salts (mordants used Cupric Sulphate and Ferrous Sulphate).Three processes of
mordanting were used-pre mordanting, simultaneous mordanting and post mordanting.
After dyeing, the dyed material was washed with cold water and dried at room
temperature (Pruthi et al., 2007; Jothi, 2008; Suitcharit et al., 2010).
3. Cotton Dyeing with Natural Dye Extracted from marigold flower (TAGETES
EREECTAL)
Materials: A dark yellow variety of marigold flowers were collected
Substrates: Desized and scoured cotton, bleached, and silk fabrics were used for dyeing.
Chemicals: Alum, copper sulphate, stannous chloride and ferrous sulphate.
Methods: The dyeing of cotton and silk with marigold flower was carried out in four
stages; Pre-Treatment, Extraction of dyes from flower, Mordanting (fixing dye with fiber)
and Dyeing.
Extraction of colorant:
Flowers from the plant source were crushed and dissolved in distilled water and allowed
to boil in a beaker kept over water bath for quick extraction for 2 hours. All the color was
extracted from flowers by the end of 2 hours. The solution was filtered for immediate use.
The flowers were also dried in trays, in thin layers, in a current of warm air immediately
after picking.
Scouring of Cotton and Silk: Silk and cotton fabrics and wool yarn were washed in a
solution containing 0.5 g/L sodium carbonate and 2 g/L nonionic detergent solution at 50
C for 25 min, keeping the material to liquor ratio at 1:40. The scoured material was
thoroughly washed with tap water and dried at room temperature. The scoured material
was soaked in clean water for 30 min prior to dyeing or mordanting.

Dyeing: The cotton and silk samples were dyed with dye extract, keeping M:L ratio as
1:40; however for cotton dyeing it was used directly while in the case of silk dyeing the
pH was maintained at 4 by adding a buffer solution (sodium acetate and acetic acid). The
dye extract was prepared by adding 4 gm dye powder in 100ml water (M:L: 1: 40).
Dyeing was done by the conventional dyeing method. After dyeing, the dyed material
was washed with cold water and dried at room temperature. It was then dipped in brine
for dye fixing. The color strength was determined calorimetrically using Computer
Colour Matching software at the maximum wavelength of the natural colorant.
 24. RESULTS AND DISCUSIONS

The yield of dye extracted from Beetroot peel was 19.2% in this process. The amount of
dye extracted from rind of Beetroot was 22.5%. Yields of the dye can be improved by
using sophisticated techniques. Large number of plants gives red colour (Cage). The
fabrics dyed with Beetroot peel gave different shades of Red. Similarly, red and blue
pigments were obtained from crude indigo extract of Indigofera tinctoria. Mordants play
very important role in imparting colour to the fabric. The mordants used in combination
in different ratios gave varying shades. Better colour strength results are dependent on the
metal salt used.
Strong co-ordination tendency of Fe enhances the interaction between the fiber and the
dye, resulting in high dye uptake. Ferrous sulphate and Copper sulphate have the ability
of forming coordination complexes (Coordination numbers are 6 and 4 respectively).
Functional groups such as amino and carboxylic acid on the fiber can occupy the
unoccupied sites on interaction with the fiber. Thus, a ternary complex is formed by the
metal salt on which one site is with the fiber and the other site is with the dye.
The mordants cloth was immediately used for dyeing because some mordants are light
sensitive. The chromatophore of the dye makes it resistant to photochemical attack, but
the auxochrome may alter the fastness. Good light fastness was observed in fabrics dyed
with the dye extracted from the Beetroot Peel. This is due to the formation of complex
with the metal which protects the chromatophore from the photolytic degradation. Good
rub fastness was exhibited in fabrics dyed with the extracted from the Beetroot peel.
Complexing the fiber with mordant has the effect of insolubilizing the dye, making it
colour fast. The fabrics dyed with Beetroot rind exhibit good fastness properties.
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