Title of Invention

A PROCESS FOR PREPARING TEXTILE ARTICLES SELECTED FROM COTTON, SILK AND WOOL DYED BY COLOURING MATERIALS ISOLATED FROM FLOWERS.

Abstract In the conventional mode of dyeing textile materials, chemical dyes are being used some of which cause environmental pollution, apart from having adverse physiological actions, which has led to search for safe colouring materials from natural objects like flowers. The present invention provides a process for preparing textile articles dyed by colouring materials isolated from flowers which comprises- (i) simmering shredded flowers in water for 1.5 to 2 hours at a temperature between 70° and 85Oc under occasional agitation, followed by decantation or straining of the supernatant coloured liquid ; (ii) soaking textile material in the coloured extract in presence of al least one mordanting chemical selected from alum, chrome alum. K2Cr2O7 K2Cr2O4. NaCL MgSO4, SnCl2 and CuSO4 present in an amount of around 100 - 200 gms per 5 litres of extract for a period of 1 to 1.5 hours : (iii) removing gummy materials, if any and washing the textile material in water. (iv) drying the colured textile article and pressing, if needed, to remove wrinkles. Pre-mordanting and simultaneous mordanting are also within the scope of this invention using flowers like Marigold. Aparajita. Palash. Sheuli, Bougainvillea. China Rose, Alkanet and Kolaboti as colour source.
Full Text The present invention relates to a process for preparing textile articles selected from cotton silk and wool , by colouring materials isolated from flowers. More particularly the present invention deals with isolation and extraction of colouring matters from flowers, preparation of a dye-bath from the extracted water-soluble pigments and textile materials like silk, wool or cotton dyed by being treated in the said dye-bath.
Dyeing of textile materials will mean imparting a colour which is light fast forms a fairly steadfast bond with the substrate to which it is applied so that it is not easily washed away on laundering and is fairly resistant to hoth acid and
alkali.
These days from chemical dye industry it has been observed that factory effluents contain toxic chemicals which invariably cause environmental pollution. Besides, some of the chemicals going out in factory effluents like 'Benzidinc Red' "Metanil yellow". "Phthalocyanine Blue", etc. have been found to be carcinogenic in nature and some other dyes have adverse allergic dermatological syndrome on human and animals alike. When such deleterious chemicals are released in water bodies or dumped in soil, they become a major source of environmental pollution and lead to health hazard.
Even though textile colouration and dyeing industry is still using chemical dye, search for dyestutts from natural vegetative sources has been on for some time. Developed countries like European Stales. Japan and United States of America have issued embargoes on the unrestricted use of chemical dyestuffs in view of the potential environmental hazard posed by such colouring compounds. In India and also in a number of tropical and sub-tropical countries there is a vast resource of coloured flowers, the colouring pigments of which may gainfully be employed for colouring textile materials and these are eco-friendly flowers in large quantities go waste everyday in India, from which colouring matters may be isolated using suitable technology. Some of these natural vegetative sources may be subjected to extraction and isolation of dyes therefrom, which when applied to textile fabric produce exquisite shades at far less cost in comparison with synthetic

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chemical dyes, apart from being non-toxic, easily available and having no adverse reaction when in contact with human skin. Due mainly to easy availability and cheap labour, most of the textiles dyed with colouring matters obtained from vegetative sources are imported from Third World Countries, India being one of the major players. Flowers growing abundantly in India, particularly in the Eastern Region, may be selected from, inter alia. Marigold (a flower of the plant of genus Calendula or Tagetas), China Rose., Aparajita. Bougainvillea, Cineraria. Alkanei. Palash, Sheuli, and the like flowers, from which colouring matters may be easily extracted.
Heretofore indigenously available flowers like Palash and Sheuli (or Shefali) have been widely used for colouring textile materials, particularly cotton articles, simply by boiling the flowers in hot water and dipping (he textile materials in the dye leached out from flowers. The quality of dyeing was often not satisfactory, non-uniform patches of colour being produced after drying of the textile material. Moreover, the intensity of colour tended to fade on washing in weakly alkaline bath and/or being exposed to sunrays.
The present invention aims at overcoming the foregoing disadvantages of conventional mode of extraction and dyeing of textile materials with colouring materials isolated from flowers.
The principal object of this invention is to provide a process for preparing textile articles dyed by colouring materials isolated from flowers.
A further object of this invention is to provide a process for preparing dyed textile articles by using colouring materials isolated from flowers and enhancing fastness of colour by employing selected type of mordanting chemical(s).
A still further object of the present invention is to provide a process which substantially eliminates all possibilities of environmental pollution.
Another object of this invention is to evolve a process which is cost effective and uses indigenously available raw materials.

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The foregoing objects are achieved by the present Invention which relates to a process for preparing textile articles selected from cotton silk and wool dyed by colouring materials isolated from flowers such as herein described- which comprises.

(a) gradually heating or blanching freshor dried flowers in shredded form in water (20 -
30gm of flower per 100 ml of water ) with the addition of 4-6 % by wi. of
sodium chloride for a period of around I to 1.5 hours at a temperature
between around 70f> and 85°C under occasional stirring, followed by
decantation or straining of supernatant coloured liquid ;
(b) soaking textile material in the coloured extract obtained from step (a) in
presence of a mordanting solution prepared by adding 100 - 200 gms of
mordant per litre of water, said mordant being selected from the group of
alum, chrome alum, K2Cr207. K2O2O4, NaCl, MgSO4, SnCI2 and CuSO4,
wherein the ratio of extract to mordanting solution is varied between
around 1-2:1 and textile material to extract or liquor ratio is varied from 1
: 20 to 1 : 30, and soaking is carried out for a period of I to 1.5 hours, maintaining a temperature of between around 80° and 90°C.
(c) removing gummy materials, if any, from the extract in step (b) after
soaking of the textile material in the supernatant liquid ;
(d) washing the coloured textile material in water;
(e) ageing the textile material for 5 to 7 days and then soaping the said material
with around 1.5 - 2.5g/l of non-ionic detergent at room temperature for 5 to
10 minutes, followed by washing with water, and
(f) drying the coloured textile material and pressing it. if needed, to remove
wrinkles.
Volume of water used for blanching may optionally be varied between 2 to 3 parts for every unit amount of flower taken. In other words, for each kilogram of flower, 2-3 litres of water at ambient temperature may be used for blanching.
There is an element of flexibility in addition of mordanting chemicals. In point of fact, all three possible variations may be adopted, namely-i) pre-mordanting, ii) simultaneous mordanting and iii) post mordanting.

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However, the first mode, namely, pre-mordanting is usually applied in textile coloration, as it is time saving and uses less mordant (s). The amount of mordanting chemical has to be carefully controlled and it usually varies between 100 and 200 gms per litre of water.
It has been found to obtain satisfactory adhesion of colouring materials to the textile articles in the event of 'simultaneous mordanting1 if the mixture of water, mordanting chemieal(s) and shredded flowers are subjected to gentle stirring between, Say, 30 and 50 r.p.m.
It is to be noted that selection of mordant as well as colouring material plays an important part in dyeing of textile materials, as these factors tend to influence the shade, tint and depth of the coloured substrate.
The textile materials may be divided into three broad categories, namely, cotton, wool and silk, depending on their origin, texture and nature of fibres. Most of the natural dyes belong to acid mordant group, as a result of which they show affinity for silk and wool. Some other natural dyes have affinity for cellulosic fibres. Pure fibres have been used for the purpose of this invention, chemical composition of which are being discussed briefly herein below.
(i) Cotton: Cotton is a natural fibre chemicaiy known as cellulose, having an empirical formula of (C^-l,o05)n. available from vegetative sources. Pure cellulose is a white substance having a specific gravity of 1.5. Cold water causes cotton to swell but has no chemical action on it. The body of cotton fibre consists of (a) primary wall, (b) secondary wall and (c) lumen. The outer surface of fibre is made of cuticle comprising wax and pectic material.
(ii) Wool : Wool has a complex structure composed mainly of three tissues, cuticle, cortex and medulla. There is no basic difference between wool and human and animal hair. Wool is primarily composed of a special type of protein called keratin which differs from other proteins on account of its high sulphur content, it usually consists of carbon { ~ 50 %) . oxygen (22-25 %) . nitrogen (16- 17%), hydrogen (~ 7 %) and sulphur (3-4 %).
(iii) Silk : Silk possesses many a desirable features of textile fibre, such as, inter alia, strength, elasticity, softness, shine, affinity for dyes, etc. Silk is a solidified viscous fluid secreted from special organs of silkworm. It consists of silk fibroin or inner layer and outer layer of silken filament. These two components are found to be present in silk fibre in proportions of about 70 %

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fibroin (C15H26N5O6) and 25 % sericin (C15H23N5O6). Outside the sericin layer there is a thin layer of albumen and in the outermost surface there is a coat of gelatin. Fibroin is known to be composed of a number of amino acids, some of which are mentioned below along with their respective amounts : i) Glycine [ NH2. CU2. COOH ] - 38 % ii) Alanine [ CH3. CM. (NH2) COOH ] - 22 % iii) Serine [ HO. CH2. CH (NH2). COO)] ] - 15 % iv) Tyrosine [ HO. C6H,0- CH2. CH (NH2) COOH ] - 9 % v) Other amino acids with bulky substituents - 16 %
As mentioned earlier, flowers yielding coloured pigments have been selected from blooms growing abundantly and mostly of indigenous origin like -
Marigold (Tagetes patula L) , Joba (Hibiscus rosa-sinensis L) . Sheuli (Nyctanthes arbortristis L) . Aparajita (Chilorea ternatea). Bougainvillea (Bougainvillea sp.), Alkanet (Alkanna tinetoria), Palash (Bulea monosperma) and Kolaboti (Canna indica L) Such coloured flowers contain a large number of chemical substances like carbohydrates, minerals, mucilage, vitamins (specially riboflavin and thiamin). pigments like anthocyanin. crocin. carotene, lycopene. zigzantin, xanthenes, etc. Pigments from flowers may be of water soluble or water-insoluble varieties, and these need to be extracted for colouring fibres. It has been found that addition of a little alcohol, say 5-10 % by volume of 70 % ethanol computed on the total volume of the blanching liquid, enhances extraction of pigments from shredded flowers in the course of blanching.
It has surprisingly been found that adhesive materials obtained by boiling in water pieces of'Ladies finger', green Wood apple (Bael). Babool gum, and such other substances from vegetative sources, when added to the textile materials along with the mordanting chemicals, produce a dyed material with a pronounced colour fastness.
For obtaining satisfactory natural dyeing, one needs to have both extracts from flower and mordanting chemicals usually from inorganic sources. In order to obtain deeper colour shades, stronger dye extract and greater proportions of mordants are to be used, it has been observed that less amounts of mordant(s) help in producing pale shades of colour.
The invention will now be described by means of the undernoted example which is aiven by way of illustration and not by way of limitation.

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Example
2.0 kg of Marigold flowers are washed well with running water to remove adhering mud and dirt. The washed flowers are subjected to shredding in a cutting machine or a shredder and the shredded flowers are transferred to a closed vessel equipped with a heating arrangement and a thermostalic control. Around 10 litres of water with of 5 % of sodium chloride are poured into the vessel and the temperature is slowly raised to around 80 C and held there for around 2 hours with occasional stirring. 5 - 10% by volume of 70 % ethanol may be added in the course of blanching or simmering to ensure better extraction of colouring pigments in greater amounts. The strength of coloured liquor can be increased by vacuum distillation to attain desired intensity of colour.
For working with a smaller quantity of flowers, one may use a soxhlei apparatus for extraction of pigments ihererrom under controlled conditions.
In a separate bath, the textile article is soaked in a colour fixative (mordant) which attaches itself to the textile fibres and the dye molecules attach themselves to the mordant. The mordant used is common alum |K2SO4; Al2 (SO4)3, 24 H2O] or NaCl selected for their non-toxic nature. 500 gm of alum is added to around 3 litres of water and textile material to be dyed is dipped therein and simmered for around an hour at about 85 °C; then the whole is slowly brought down "to ambient, cooled overnight and rinsed and squeezed to remove excess liquid. Material io liquor ratio was maintained around 1 : 25
Thereafter the textile article is dipped into the extracted dye solution obtained by straining or by simply decanting of the liquid in which (lowers were simmered. The entire mass is heated to a temperature between 80(l and 90°C for around one hour or until the colour has attained the desired level of depth and intensity. It is to be noted that the textile material should have room to be moved freely in the dyebath to ensure homogeneous dyeing. If it is felt that the colour is not of desired intensity, more dyestuffis to be used.
The dyed textile article is then subjected to "ageing" for 5 to 7 days followed by soaping the material with around 1,5 - 2.5 g/1 of non-ionic

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detergent at room temperature for 5 to 10 minutes, followed by washing with water and
(f) Drying the coloured textile article and pressing it, if needed, to remove wrinkles.
The dyed samples were tested for colourfastness to wash and light. Wash fastness of cotton was tested according to the procedure as given in IS: 764 - 1984 and that of silk and wool as given in IS : 687 - 1984. The ratings for change of colour and staining on adjacent fabrics were given with the help of Grey Scales.
Light fastness property was tested by following the procedure as given in IS: 686 - 1984. The extent of fading of samples was assessed by using Grey Scales.
Colour fastness to washing and light for cotton was around 3. Colour fastness to washing of silk and wool textiles was around 4 but colour fastness to light was around 4 on silk and wool.
If it: is desired to modify the colour, "after mordants" can be used. this, however, is likely to add to the cost of production:
The inherent advantages of the present invention may be summarised as follows:
I) this ensures a gainful utilisation of our natural resources like flowers;
ii) the process ensures prevention of wastage of vegetative produce :
iii) the process produces natural colours which are not only eco-friendly but
also have no deleterious effects on human skin ; iv) the solid residue from flowers left after extraction of colouring material
may be used as cattle feed or as bio-fertilizer ; v) the evolved technology can create fresh job opportunities, particularly in
rural areas ; vi) the process does not need any sophisticated machinery or imported
reactants and vii) the technology evolved is extremely cost effective.

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While the invention has been described in detail and with specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without deviating or departing from the scope and spirit of the invention. Thus the disclosure contained herein includes within its ambit obvious equivalents and substitutes as well.
Having described the invention in detail with particular reference to the appended example, it will now be more specifically defined by means of claims appended hereinafter.

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I claim:
1. A process for preparing textile articles selected from cotton silk and wool dyed by colouring materials isolated
from (lowers such herein described, which comprises : -
(a) gradually heating or blanching^flowers in shredded form in water (20 - 30gm,
of flower per 100 ml of water ) with the addition of 4-6 % by wt. of sodium
chloride for a period of around 1 to 1.5 hours at a temperature between around
70 and 85 C under occasional stirring, followed by decantation or straining of
supernatant coloured liquid ;
(b) soaking textile article in the coloured extract obtained from step (a) in presence
of a mordanting solution prepared by adding 100 - 200 gms of mordant per
litre of water, said mordant being selected from the group of alum, chrome
alum, K2Cr2O7. K2Cr2O4. NaCl, MgSO4, SnCl2 and CuSO4? wherein the ratio of
extract to mordanting solution is varied between around 1-2:1 and textile article to
extract or liquor ratio is varied from 1 : 20 to 1 : 30. and soaking is carried out for a
period of 1 to 1.5 hours, maintaining a temperature of between around 80 and 90 C.

(c) removing gummy materials, if any. from the extract in step (b) after as soaking of
the textile material in the supernatant liquid :
(d) Washing the coloured textile material in water;
(e) ageing the textile material for 5 to 7 days and then soaping the said material
with around 1.5 - 2.5 g/1 of non-ionic detergent at room temperature for 5 to
10 minutes, followed by washing with water, and
(g) drying the coloured textile material and pressing it, if needed, to remove wrinkles.
2. A process as claimed in Claim I. wherein the proportion of flower and water for blanching or simmering optimally varies between 1 : 4-6.

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3- A process as claimed in Claims 1 and 2 . wherein the said mordanting chemical is added in the course of simmering or blanching of flowers with gentle stirring at around 30 to 50 r.p.m.
4. A process as claimed in Claims 1 to 3. wherein the textile article is treated
with mordanting chemical, dried and thereafter dipped in the aqueous
extract of (he coloured pigments obtained from flowers.
5. A process as claimed in Claims 1 and 4. wherein the amount of mordanting
chemical is varied between around 100 and 200 gms for every litre of
water.
6. A process as claimed in any of the preceding claims, wherein the colouring
material is extracted from the flowers selected from the group of Marigold
(Tagetes sp.) Aparajita (Clitoria linctoria), China Rose (Hibiscus rosa-
sinensis). Bougainvillea (Bougainvillea sp.), AJkanet (Alkanna tictoria).
Palash (Butea mpnosperma), Sheuli (Nyctanthes arbortrislis L) and
Kolaboti (Canna indica L), optionally in the presence of 5 - 10 % by
volume of 70 % ethanol in the course of blanching.
7. A process as claimed in any of the preceding claims, wherein adhesive
materials obtained by boiling in water pieces of'Ladies linger', green Wood
Apple (Baei), Babool gum and such other substances from vegetative
sources are added to the textile articles in the course of mordanting,
thereby enhancing colour fastness.

8. A process for preparing textile anicies selected from cotton silk and wool dyed by colouring materials isolated
from flowers, substantially as hereinbefore described.
In the conventional mode of dyeing textile materials, chemical dyes are being used some of which cause environmental pollution, apart from having adverse physiological actions, which has led to search for safe colouring materials from natural objects like flowers.
The present invention provides a process for preparing textile articles dyed by colouring materials isolated from flowers which comprises-
(i) simmering shredded flowers in water for 1.5 to 2 hours at a temperature between 70° and 85Oc under occasional agitation, followed by decantation or straining of the supernatant coloured liquid ;
(ii) soaking textile material in the coloured extract in presence of al least one mordanting chemical selected from alum, chrome alum. K2Cr2O7 K2Cr2O4. NaCL MgSO4, SnCl2 and CuSO4 present in an amount of around 100 - 200 gms per 5 litres of extract for a period of 1 to 1.5 hours :
(iii) removing gummy materials, if any and washing the textile material in water.
(iv) drying the colured textile article and pressing, if needed, to remove wrinkles.
Pre-mordanting and simultaneous mordanting are also within the scope of this invention using flowers like Marigold. Aparajita. Palash. Sheuli, Bougainvillea. China Rose, Alkanet and Kolaboti as colour source.

Documents:

00633-kol-2004-abstract.pdf

00633-kol-2004-claims.pdf

00633-kol-2004-correspondence.pdf

00633-kol-2004-description(complete).pdf

00633-kol-2004-form-1.pdf

00633-kol-2004-form-18.pdf

00633-kol-2004-form-2.pdf

00633-kol-2004-form-3.pdf

00633-kol-2004-letters patent.pdf

00633-kol-2004-p.a.pdf

00633-kol-2004-reply f.e.r.pdf

633-KOL-2004-CORRESPONDENCE-1.1.pdf

633-KOL-2004-CORRESPONDENCE.pdf

633-KOL-2004-FORM 27.pdf

633-kol-2004-granted-abstract.pdf

633-kol-2004-granted-claims.pdf

633-kol-2004-granted-description (complete).pdf

633-kol-2004-granted-form 2.pdf

633-kol-2004-granted-specification.pdf


Patent Number 208564
Indian Patent Application Number 633/KOL/2004
PG Journal Number 31/2007
Publication Date 03-Aug-2007
Grant Date 02-Aug-2007
Date of Filing 06-Oct-2004
Name of Patentee SIDDHARTHA DATTA.
Applicant Address P.O. JADAVPUR UNIVERSITY, DEPTT. OF CHEMICAL ENGINEERING, KOLKATA 700 032
Inventors:
# Inventor's Name Inventor's Address
1 SIDDAHARTHA DATTA P.O. JADAVPUR UNIVERSITY, KOLKATA-700 032.
PCT International Classification Number C09B 69/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA