Description:TECHNICAL FIELD:
The present disclosure relates to acosmetic application. More specifically, the present disclosure relates to ahair colouring compositioncomprising at least one direct dye and analkylamine cationic surfactant in presence of a reducing agent, which delivers 100% grey hair coverage.The present disclosure also relates to the hair colouring composition comprising at least one alkylamine cationic surfactant, co-acting with specific direct dyes and reducing agents thatimparts superior colour uptake with good grey hair coverage. Further, the present disclosure providesasynergistichair colouring composition that upon single application provides hair a long-lasting colour and withminimal colour bleeding.The present hair colour composition is safe, easy to use, simple to apply,free of dye precursors / intermediates, ammonia, and hydrogen peroxide.

BACKGROUND:
The need for hair colour composition, present &future:
Information provided in the “Background” section is included for setting the context and for understanding of the present invention. It is not an admission that any of the data included in the present application is previous knowledge or is currently being claimed or is part of any publication directly or implicitly referred to herein.
The permanent / long term alteration in the colourof keratinous fibers by the oxidative coloring process is well known in literature. In order to achieve the desired intensity and shade, the oxidative coloring process involves primary dye intermediates, couplers, and an oxidizing agent. The dye precursors (dye intermediates and couplers)used are small, polar, and soluble molecules that are easy to diffuse into the hair shaft.When activated by peroxide under basic conditions, the primary intermediates react with other dye precursors (couplers) to form larger colored moieties within the hair shaft as a result the same cannot come out easily from said hair shaft.
Since colouringof hair is one of the beauty routines, it is highly desirable to have a physical dyeing process, which excludes bleaching of hair. Direct dyes can be used for formulations involving physical dyeing process. But the challenge is to meet the other requirements including wash fastness, or no bleeding of color from the hair. Many attempts have been made to increase the wash fastness of direct dyes by either forming a covalent bond between chromophores and proteins inside hair or increasing the number of binding sites on the dyes. Attempts to form the covalent bond between chromophores and proteins result in uneven color uptake along the length of the hair and reduced dye penetration into the hair fibers since the dyes are typically twice as large as common oxidative dye precursors. If the number of binding sites is increased on the dyes, then the penetration into the cortex becomes impossible because of difficulty to diffuse through negatively charged networks of keratin proteins. This results in excess color bleeding and fading. Also, it is difficult to produce darker shades with polycationic dyes due to limited binding sites on the surface of hair. Reference is invited for few of the related prior attempts reported in the literature.
US10478643B2 relates to a hair dyeing composition comprising selected hair dyes and a reducing agent in order to color hair homogeneously, intensively, and durably. Said hair dyeing compositionis a two-part aqueous hair coloring composition comprising parts A and B for mixing prior to application onto hair, wherein part A is an aqueous composition containing one or more selected direct dyes and part B is an aqueous composition with one or more reducing agents selected from the group consisting of thioglycolic acid and its salts, thiolactic acid and its salts, dihydrolipoate, thioglycerol, mercaptopropionic acid and its salts, cysteine and its salts, N substituted cysteins, cystamines, thioethanol, sulfite salts, bisulfite salts and metabisulfite salts.The prior art discloses the use of direct dyes of different classes but does not cover or discuss about any additional ingredients or feature which reduce color bleeding.
US10456341B2 discusses a ready to use composition for the reshaping and direct coloring of hair comprising glyoxylic acid, a glyoxyloyl amino acid or a mixture thereof and a direct dye and a method for reshaping and coloring of hair by means of the said compositions. The pH of the composition is acidic, below the isoelectric point of hair.Thepreferred pH is between 3 and 4.5. The composition can either be a ready to use composition or it can be provided as a kit containing a two-agent type hair cosmetic comprising a first agent containing glyoxylic acid and the second agent containing at least a direct dye. The processing time required is between 5 and 45min. Dyes could be selected from anionic, cationic or nonionic dyes.The patent does not discuss wash fastness of the achieved color and does not discuss about the problem of color bleeding.
US007087096B2 concerns a dyeing composition for keratinous fibers, comprising of at least a direct cationic coloring agent, a quaternary ammonium salt in an appropriate dyeing medium, which contains an anionic surfactant. These are capable of giving intense and only slightly selective colors, which are resistant to various attacks on hair. The patent does not discuss about the wash fastness of the achieved color and does not discuss about the problem of color bleeding.
US10441521B2 describes a method for straightening and dyeing keratinous fibers with the following steps: (i) treating the fibers with a straightening agent (G), (ii) treating the fibers with a conditioner (K), and (iii) treating the fibers with a coloring agent (F). The straightening composition (G) includes at least one alkalizing agent selected from sodium hydroxide, potassium hydroxide, lithium hydroxide, magnesium hydroxide, calcium hydroxide, and / or guanidinium hydroxide, the conditioner (K) and / or the coloring agent (F) include at least one reducing agent selected from thiolactic acid, thioglycolic acid, cysteine, sodium sulfide, sodium sulfite, sodium thiosulfate, sodium dithionite, and / or cosmetically acceptable salts thereof, and the coloring agent (F) includes at least one direct acid dye.This method was claimed to be less damaging. The prior art describes multi-step application for the treatment and coloring. First step involves application of straightening agent for a period of 30 sec to 45 min, followed by rinsing of the hair, then application of the conditioner for a period of 30 sec to 45 min, again followed by rinsing and finally applying the colorant and leaving it for a period of 30 sec to 45 min and rinsing. The cited art does not address the problem of colour bleeding associated with the direct dyes.
US2019/0160000A1 describes a hair coloring composition for providing a film on keratin fibres comprises in a cosmetically acceptable carrier, a film forming aminosilicone polymer and a hair coloring agent. The aminosiliconepolymers tightly bind any hair coloring agent, eg: pigment and / or colored material and / or direct dyes and / or oxidation dyes onto the hair fibers in a durable fashion. Hence, the film–forming aminosilicone polymer provides an excellent film.The coloring agent may be selected from the group consisting of pigment, colored material, direct dye, oxidation and mixtures thereof. Post coloring, water dipping test was carried to prove the efficacy of the film forming amino siliconepolymers.The prior artdisclosesamino silicone polymers as the film former and does not use any reducing agents in the hair coloring composition.Moreover, the prior art does not disclose the color bleeding associated with the direct dyes.
US10034823B2 describes a method of dyeing hair. The method includes applying a hair color composition including one or more direct dye compounds and rinsing the hair with water. The one or more direct dye compounds each include a blue-violet or blue chromophore (imidazolium dyes), one or two permanent cations, one to four incipient cations, and one or more hydrophobic moieties. The incipient cations are pendant to the core structure and are neutral. The direct dye compounds enter the hair shaft after the hair color composition is applied to the hair. The hair color composition has a pH between about 6 to about 11. The pH of the hair after rinsing is from about 3.5 to about 6. The rinsing of the hair causes one or more of the one to four incipient cations to change from neutral to positively charged entities inside of the hair shaft, resulting in better wash fastness.This prior art uses both permanent and incipient cations, does not use any reducing agents in the composition and silent about the problem of color bleeding associated with the direct dyes.
US9504639B2 discloses a composition for treating keratinous fibers, more particularly human hair, comprising in a cosmetically appropriate vehicle a) at least one organic and/or inorganic acid, b) at least one direct dye and c) at least one compound of the formula (I) as shown below.

(i) x and y independently stand for numbers from 1 to 100; (ii)z stands for a number from 0 to 100and (iii) R1 and R2 independently stand for a linear orbranched, saturated, unsaturated, or multiply unsaturated C5-C20 alkyl group, a hydroxyl group, a C1-C30alkoxy group, a carboxy C1-C30alkyl group, or a C1-C6, alkyl-(O-CH-CH2)n O- group, where n stands for an integer from 1 to 60.The direct dyes are selected from non-ionic nitro dyes or their combinations thereof. The cited prior art does not use reducing agents nor it addresses the problem of color bleeding in the composition.
US20180021239A1 discloses a method for dyeing hair by applying a polyvinyl amine copolymer solution followed by a hair dye composition to the hair. A hair dye composition includes an aqueous base fluid; a polyvinyl amine copolymer; and an anionic or cationic hair dye. The application is sequential where the polyvinyl amine copolymer solution is sprayed onto hair followed by the dye composition.The process is multi-step and no washing is done post spraying.
US10328016B2 relates to a cosmetic agent for changing the colour of keratinic fibres, comprising in a cosmetically acceptable carrier comprising of at least one compound selected from the group of oxidation dye precursors, direct dyes and mixtures thereof and a first linear non-ionic silicone polymer with the formula,

Wherein, R2 and R7, in each case independently of one another, stand for a methyl group or a hydroxyl group and x represent integers from 1650 to 8500 and a second linear non-ionic silicone polymer with the formula,

Wherein, R2 and R7, in each case independently of one another, stand for a methyl group or a hydroxyl group and y stand for integers from 40 to 1300. This is used in combination with an oxidising agent. The use of the at least one non – ionic linear silicone polymer leads to an improved colourfulness and / or depth of shades. The prior art does not disclose the use of reducing agents, or the problems associated with direct dyes such as colour bleeding.
None of the above prior arts disclose a combination of direct dyes along with at least one alkylamine cationic surfactantand reducing agent that shows minimal color bleeding and excellent colour retention.Therefore, there remains a scopefordevelopment of a hair colouring composition that would provide 100% grey coverage,besafe, free of ammonia, and hydrogen peroxide, has minimal colour bleeding, excellent colour retention, and good hair coloring properties based on the above combination of direct dyes along with alkylamine cationic surfactant and reducing agent.

OBJECTIVES:
The primary objective of the present disclosure is to provide a hair colouring composition comprising at least one direct dye and one or more alkylamine cationic surfactant in the presence of a reducing agent that delivers excellent grey hair coverage.
Another object of the present disclosure is to provide said hair colouring composition which would comprise at least one C18-C40chain length alkylamine cationic surfactant synergistically co-acting with the specific direct dyes and reducing agents, imparting superior colour uptake with excellent (100%)grey hair coverage.
Yet another object of the present disclosure is to provide said hair colouring composition which would be a synergistic composition with long-lasting colour and minimal colour bleeding.
Further object of the present disclosure is to provide said hair colour composition that is safe, easy to use, simple to apply andfree of dye precursors / intermediates for oxidative dyes, ammonia and hydrogen peroxide.

SUMMARY:
The present disclosureprovides a hair colouring composition comprising at least one direct dye/s and one or morealkylamino cationic molecule/s with a long chain fatty acid moiety in the presence of reducing agent/s that delivers excellent grey hair coverage and provides a synergistic composition with long lasting colour and minimal colour bleeding.
A preferred aspect of present disclosure provides a multi-component hair colour composition with minimal colour bleeding comprising: (i) 0.1 to 6 mass % of direct dye/s; (ii) 0.1% to 5 mass % of alkylamine cationic agent/s; (iii) 0.1 to 25 mass % reducing agent/s and (iv) cosmetically acceptable base with scalp and hair benefit agents.
The present disclosure provides a multi-component hair colour composition comprisingdirect dye/s, alkylamine cationic agent/s, and reducing agent/s, wherein the individual components may be present by themselves or in any chemically compatible combination, in a cosmetically acceptable base with scalp and hair benefit agents.
Various features, aspects and advantages of the inventive subject matter will become more apparent from the following detailed description of preferred embodiments.

DETAILED DESCRIPTION OF DRAWINGS:
The accompanying drawings are included to provide a further understanding of the present disclosure and are incorporated in and constitute a part of this specification. The drawings illustrate exemplary embodiments of the present disclosure and, together with the description, serve to explain the principles of the present disclosure. The diagrams are for illustration only, which thus is not a limitation of the present disclosure:
Figure 1 shows UV-vis absorption valueofComposition without any adjuvants (Experiment No: 79) and Composition with CutissentialBehenyl TMS 50 (Experiment No: 9).
DETAILED DESCRIPTION:
It is to be understood that the present disclosure is not limited in its application to the details of construction and the arrangement of components set forth in the following description or illustrated in the drawings. The present disclosure is capable of other embodiments, of being practiced, or of being carried out in various ways. Also, it is to be understood that the phraseology and terminology used herein is for the purpose of description and should not be regarded as limiting.
Definition:
• All technical and scientific words used herein, unless otherwise defined, have the same meaning as commonly known by one having ordinary ability in the relevant field. The words "a" and "an" designate one or more (i.e., at least one) of the article's grammatical objects. Unless otherwise stated, weight is used to determine all percentages and ratios. All percentages and ratios are calculated based on the total final composition unless otherwise indicated.
• As used herein, whether in a transitional phase or the body of a claim, the terms “comprise(s)” and “comprising” are to be interpreted as having an open-ended meaning. That is, the terms are to be interpreted synonymously with the phrases “having at least” or “including at least”. When used in the context of a process, the term “comprising” means that the process includes at least the recited steps but may include additional steps. When used in the context of a composition, the term “comprising” means that the composition includes at least the recited features or components but may also include additional features or components.
• All composition described herein can be performed in suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., “such as”) provided with respect to certain embodiments herein is intended merely to better illuminate the disclosure and does not pose a limitation on the scope of the invention otherwise claimed. No language in the specification should be construed as indicating any non-claimed element essential to the practice of the disclosure.

The present disclosure will now be described in greater detail including various specific details which are to be regarded as merely exemplary. Accordingly, those of ordinary skill in the art will recognize that without departing from the scope and spirit of the present disclosure and its various embodiments there may be any number of changes and modifications described herein.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer, or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the disclosure unless there is a statement in the specification to the contrary. The above-mentioned composition of the invention can be incorporated in hair coloring composition/ kit and is adapted for use in cosmetically acceptable forms such as cremes/shampoo/lotions/gels and the like.
The term “formulation” used herein refers to a mixture prepared according to a formula.
a. Rating of Visual Assessment of Colour Uptake on Hair:0-19% = No uptake; 20-59% = Poor; 60-84% = Moderate; 85-94% = Good; 95-100% = 100% where the numerical values represent any and all values including fractions till the next numerical value.
b. Concentrations: The tabulated concentrations in the tables are in the form of active percentages and recorded as "mass%" of the total composition.
c. Compositions & Preparation: Unless mentioned otherwise, all experimental compositions were prepared in crème format as per Format 1 Crème #1 following process conditions as described under experimental section.
d. ColouringProcess: In all experiments, unless mentioned otherwise, the colour development was assessed on hair swatches and after application to hair, 30 min of developmental time was provided, and the hair swatches were washed after application of colouring mixture as per experimental procedure.
Aspects of the present disclosure are further understood in light of the following examples, which should not be considered as limiting the scope of the present disclosure.
Primaryaspect of the present disclosureprovides a multi-component hair colour composition with minimal colour bleeding comprising(i) 0.1 to 6 mass % of direct dye/s; (ii) 0.1% to 5 mass % of alkylamine cationic agent/s; (iii) 0.1 to 25 mass % reducing agent/s and (iv) cosmetically acceptable base with scalp and hair benefit agents. Prior to the application on hair, the differentcomponents / parts are mixed and thereby forms the composition of the present disclosure.
A further aspect of the present disclosure provides a multi-component hair colour composition comprising direct dye/s, alkylamine cationic agent/s, and reducing agent/s, wherein the direct dye/s and the reducing agent/s must be kept separated till the point of mixing and the alkylamine cationic agent/s can be combined with either of the individual components or it can be provided separately as an additional component to be combined with the other components at the time of mixing. Each of these components can be in a cosmetically acceptable carrier system with or without hair / scalp benefit agents. In the non-limiting examples disclosed herein, the alkylamine cationic component has been combined with the direct dyes.
Another aspect of the present disclosure provides a multi-part/component hair colour composition comprising direct dye/s, alkylamine cationic agent/s, and reducing agent/s, wherein the individual parts may be mixed prior to application to hair for providing the inventive hair colouring composition and delivering the desired colouring benefits.
In an embodiment of present disclosure, the direct dye is selected from Basic Brown 16, Basic red 76, Blue 12, Basic Brown 17, Basic red 51, Basic Blue 99, Basic Violet 1, Basic Violet 2, Basic Violet 3, Basic Yellow 57, Basic Red 2, Basic Red 12, Basic Red 22, HC Blue 2, HC Blue 4, HC Blue 5, HC Blue 6, HC Blue 7, HC Blue 8, HC Blue 9, HC Blue 10, HC Blue 11, HC Blue 12, BC Blue 13, HC Blue 16, HC Brown 1, HC Brown 2, HC Green 1, HC Orange 1, HC Orange 2, HC Orange 3, HC Orange 5, HC Red 1, HC Red 3, HC Red 7, HC Red 54, HC Red BN, HC Violet 1, HC Violet 2, HC Yellow 2, HC Yellow 4, HC Yellow 5, HC Yellow 6, HC Yellow 7. HC Yellow 8, HC Yellow 9, HC Yellow 10, HC Yellow 11, HC Yellow 12, HC Yellow 13, HC Yellow 14, HC Yellow 15or combination thereof.
In another embodiment of the present disclosure, thealkylamine cationic agent is selected from Trimethyl-n-octylammoniumChloride, Trimethylstearylammonium Bromide, Trimethyltetradecylammonium Chloride, Heptadecyltrimethylammonium Bromide, Hexadecyltrimethylammonium Bromide, Trimethylnonylammonium Bromide, Domiphen Bromide, Di(C12-C18)-alkyldimethylammonium chloride, Di(C12-C18)-alkyldimethylammoniumbromide, (C12-C18)-alkyldimethylbenzyl -ammonium chloride, (C16-C18)-alkylpentaoxyethylammonium chloride, Dioctadecyl -dimethylammoniumbromide, Distearoylethyldimonium chloride, Cetyltrimethyl -ammonium chloride, Cetyltrimethylammonium bromide, Cetyltrimethylammonium methosulfate, Stearyltrimethylammoniumchloride, Cocamidopropyltrimonium Chloride, UndecyleneamidopropyltrimoniumMethosulfate, BehentrimoniumMethosulfate, C10-C40IsoalkylamidopropylethyldimoniumEthosulfate, Acrylamidopropyltrimonium Chloride/Acrylamide Copolymer, Dihydrogenated tallow dimethyl ammonium chloride, Di(palmitic carboxyethyl)hydroxyethyl methyl ammonium methylsulfate, Benzalkonium chloride, polyquaterium-53, polyquaternium-10 or combinations thereof.

In another embodiment of the present disclosure, the reducing agent is selected from thioglycolic acid and its salts, thiolactic acid and its salts, dihydrolipoate, thioglycerol, mercaptopropionic acid and its salts, cysteine and its salts, N substituted cysteins, cystamine and its salts, thioethanol, sulfite salts, bisulfite salts and metabisulfite salts, dithionite salts, (2-carboxyethyl) phosphine and its salts, glyoxylic acid and its salts, ascorbic acid and its salts as well as derivatives or combination thereof.
Yetanother embodimentof the present disclosure providesthe cosmetically acceptable bases selected from a rheology modifier and a pH modifier, and other hair/scalp benefiting agents includingconditioning agent, a penetration aid, a humectant, anemollient, anemulsifier, a surfactant anda softening agent or combination thereof.
In yet another embodiment said rheology modifier of the present disclosure is selected from Acrylates Copolymer, Acrylates/C10-C30 Alkyl Acrylate Crosspolymer, Acrylates/Beheneth-25 Methacrylate Copolymer, Acrylates/Steareth-20 Itaconate Copolymer, Acrylates/Ceteth-20 Itaconate Copolymer, Sodium alginate, Cellulose derivatives such as Methyl cellulose, Hydroxyethyl cellulose, Hydroxymethyl cellulose, Hydroxypropyl cellulose or combination thereof.
Certain embodiment of the present disclosure provides, thepH modifier is selected from phosphoric acid, ascorbic acid and lactic acid, and alkalis such as ethanolamine, triethanolamine, 2-amino-2-methyl-1-propanol,soda lye, ammonia, potash lye, tris(hydroxymethyl)aminomethane or combination thereof.
In some embodiment of the present disclosure provides, the composition pHranges from 7 - 12.
Furthermore, embodiment of the present disclosure provides, the composition developmental time is 5 minutes to 60 minutes.
In a further embodiment of the present disclosure provide,the pH of the composition is maintained by using alkalizersuch as ethanolamine (MEA). The pH of the mixture after mixing was maintained between 9 - 11.
The present disclosure provides a synergistic composition with long lasting colour and minimal colour bleeding. Further, the present hair colour composition is safe, easy to use, simple to apply and free ofdye precursors for oxidative dyes and hydrogen peroxide.
EXAMPLES
The following examples are illustrated to describe the scope of the disclosure.
While hair colouring of the present invention can be performed with multi-component systems, that is with 2 or more than 2 components, for convenience formulations of different examples/prototype products incorporating the inventive compositions in a two-component systemare prepared as discussed below.
EXAMPLE 1
Preparation of Hair Coloring Composition of the Present Disclosure
Component A: Crème Format: The term Crème means a viscous liquid or semi-solid that does not readily drip when applied to the hair. It may be in the solution or emulsion form.
The general formulation for Component A is given in Table 1. This formula is a typical one, but can be varied by a person skilled in the art.
Table 1: General Formulation for Component A (Colorant)
General Formulation (ComponentA)
Oil Phase Cocamide MEA 3.50
Lauryl alcohol 3.50
Water Phase Sodium laureth sulfate 3.00
Acrylates/C10-C30 Alkyl Acrylate Crosspolymer 4.00
Cationic Compounds As per relevant experiment (see tables)
Direct Dyes As per relevant experiment (see tables)
Fragrance 0.50
Ethanolamine 2.40
Water QS to 100

Method of Preparation: Oil phase and the alkylamine cationic component are heated together at a temperature of 75C. Water phase containing surfactants is added to the melted oil-phase mixture at 75C and stirred for 10 min to form the emulsion. Water dispersed rheology modifiers are added to the emulsion. The direct dyes are dissolved in water/pH modifier (ethanolamine) mixture and subsequently added to the emulsion. The mixture is then agitated and cooled to 30C, and the fragrance was added.
Component B:
This general formula of Component B is a typical one but can be varied by a person skilled in the art.
Table 2: General Formulation for Component B (reducing component)
Acrylates/C10-C30 Alkyl Acrylate Crosspolymer 1.2
Reducing Agent As per relevant experiment (see tables)
Ethanolamine 12
Fragrance 0.5
Water QS to 100

Method of Preparation:The rheology modifier is dispersed in water. Reducing agents and the remaining ingredients are added at room temperature.

Component C and D
This general formula of Component C (devoid of Cationic Compounds) and D (contains only cationic compound) in the case of a 3-component system is a typical one but can be varied by a person skilled in the art.
Table 3: General Formulations for Component C and D
Component C
General Formulation (Component C)
Oil Phase Cocamide MEA 3.50
Lauryl alcohol 3.50
Water Phase Sodium laureth sulfate 3.00
Acrylates/C10-C30 Alkyl Acrylate Crosspolymer 4.00
Direct Dyes As per relevant experiment (see tables)
Fragrance 0.50
Ethanolamine 2.40
Water QS to 100

Component D
Acrylates/C10-C30 Alkyl Acrylate Crosspolymer 1.2
Cationic alkylamine agents As per relevant experiment (see tables)
Fragrance 0.5
Water QS to 100

EXAMPLE 2
Preparation of Hair Swatches: For the preparation of grey hair tresses, the hair was washed prior to use with non-conditioning shampoo and then dried. 5 g hair swatches were prepared for the experiments. The tresses were sorted based on the L* values before colouring. L* of the selected swatches were 60.5 ± 4.
EXAMPLE3
Hair Colouring Process
Two component system
General Method: The prepared formulations (Colorant- Component A) were mixed with reducing component (Component B) in 1:0.2 to 1:3, preferably in the ratio 1:1 to 1:2. For all the tabulated experiments, mixing ratio of Component A to B is 1:1. The mixture was applied immediately on the grey hair swatches with the help of an applicator brush or with the help of gloved hands. It is recommended to use gloves to cover the hands to prevent staining of hands as well as to prevent exposure to the chemicals. After application of the mixture, the grey hair swatches were left for 30 min and then washed.
A detailed method of colouring the hair involving hair colouring composition comprise the steps of:
a) Preparing the colorant component (Component A) including the direct dyes, and alkylamine cationic agents in the form of cream and the like at the desired pH by using pH modifiers;
b) Intimately mixing the said Component A formulation with the reducing component (Component B) in the ratio as mentioned in the general method section when the component Aandcomponent Bare provided separately or as a compartmentalized container including sachet in the kit to provide for a ready to use colouring composition mix; and
c) Applying the said mixture on hair ensuring complete coverage of the hair especially the roots following the guidelines of the general method and
d) Washing after 30 min of developmental time under flowing water or shower.

3-Component System
General method: The prepared formulations (Colorant- Component C) were mixed with reducing component (Component B) and Component D in 1:0.2:0.2 to 1:3:3, preferably in the ratio 1:1:1 to 1:2:2. The mixture was applied immediately on the grey hair swatches with the help of an applicator brush or with the help of gloved hands. It is recommended to use gloves to cover the hands to prevent staining of hands as well as to prevent exposure to the chemicals. After application of the mixture, the grey hair swatches were left for 30 min and then washed.
A detailed method of colouring the hair involving hair colouring composition comprise the steps of:
a) Preparing the colorant component (Component C) including the direct dyes, in the form of cream and the like at the desired pH by using pH modifiers;
b) Intimately mixing the said Component C formulation with the reducing component (Component B) and the adjuvant composition (Composition D) in the ratio as mentioned in the general method section when the component B, C and Dare provided separately or as a compartmentalized container including sachet in the kit to provide for a ready to use colouring composition mix; and
c) Applying the said mixture on hair ensuring complete coverage of the hair especially the roots following the guidelines of the general method and washing after 30 min of developmental time under flowing water or shower.
Visual Assessment of Hair Colour and Grey Hair Coverage:
The visual assessment of the hair colour and grey hair coverage was carried out under normal day light conditions with the help of an expert panel of hair color.

EXAMPLE4
ColourBleeding Evaluation:
The swatches post colouring with the respective compositions were washed and dried. The swatches were allowed to stir in 120 ml water for 2 min. The grey hair swatch was removedand the liquor was taken for UV-vis absorbance. The intensity of the wash liquor was recorded using UV-vis absorption spectroscopy. For UV-vis data, 200 microliters were diluted to 1 ml and spectra were recorded. Absorbance of less than 0.1 = 1 (minimal bleeding), 0.1 - 0.2 = 2, >0.2 - 0.3 = 3, >0.3 - 0.4 =4 and above 0.4 it was denoted as 5 (the highest bleeding).
Study of Different Components fortheir selective Role:
Study A: Role ofDifferent Blue Direct Dyes onthe Colour Uptake
In order to study the selectivity of different coloured direct dyes in hair colouring, experiments were undertakenwith 3 different blue direct dyesfollowingthe procedure as described under Example 3 (Two component system).The results are given in Table 4.Unless mentioned otherwise, the mixing ratio of the colorant and reducing components were maintained as 1:1.
Table 4: Effect of Different Blue Direct Dyes on Grey Hair Coverage.
(The formulations of Component A and Component Bas given in Table 1 and Table 2)
Expt No 1 2 3
Components in Table 1 & Table 2
Blue Direct Dyes HC Blue 16 4.0 0.0 0.0
Blue 12 0.0 4.0 0.0
Basic Blue 99 0.0 0.0 4.0
Alkylamine cationic agent (as active percentage) Incroquat™ Behenyl TMS – 50 1.2 1.2 1.2
Reducing Agent Potassium thioglycolate 14 14 14
Observation on Hair Colouring (Mixing Ratio of Components A& B = 1:1)
Grey hair coverage 100% Poor Poor
Colour of Hair Intense blue Pale blue Pale blue
Color Bleeding 1 1 1

Three different types of direct blue dyes were used for 3 different experimentsinvolving Component A and the reducing component (Component B) following the general formulation as already mentioned. From Table 4, it is clear that HC Blue-16 delivers 100% grey hair coverage with minimal colour bleeding. But the other two blue dyes, both Basic Blue 12 and Basic Blue 99 delivered only pale blue shade with poor grey hair coverage.
Study B: Role of Reducing Agents
Selection of reducing agents played a crucial role in the development of colour on hair. This is illustrated in the experiments 74 to 85 listed in Table 5.
Table 5: EffectofDifferent Reducing Agents on Grey Hair Coverage
(The formulations of Component A and Component B as given in Table 1 and Table 2)
Expt No 74 75 76 77 78 79 80 81 82 83 84 85
Ingredients (in Component A; as in Expt 5)
Basic Brown 16 4 4 4 4 4 4 4 4 4 4 4 4
HC Blue 16 4 4 4 4 4 4 4 4 4 4 4 4
Basic Red 76 2 2 2 2 2 2 2 2 2 2 2 2
Adjuvant 0 0 0 0 0 0 0 0 0 0 0 0
Reducing Agents (in Component B)
Potassium thioglycolate 6 8 9 10 12 14 0
Sodium sulfite 8 0
Ascorbic acid 15 0
Glyoxylic acid (50%) solution 40 0
Cysteamine HCl 14 0
Tris (2-carboxyethyl) phosphine hydrochloride 2 0
Observation on Hair Colouring (Mixing Ratio of Components A & B = 1:1)
Grey Hair Coverage (%) 100 100 100 100 100 100 Poor Good Poor 100 100 0
Colour of Hair Dark Brown Dark Brown Dark Brown Dark Brown Dark Brown Natural Black Greyish Black Natural Black Greyish Black Natural Black Natural Black* Grey
Color Bleeding 4 4 4 4 4 5 2 5 5 5 5 1
* Hair was brittle
For all the experiments described in Table 5, Component A used was as in Expt 5 (See table 6), where there were no alkylamine cationic agent (adjuvants). With no reducing agent(Expt No 85), when just Component A (Expt No 5) was mixed with formulation for Component B, no colour uptake was there. The colours washed off (Expt No 85). From the results, it was evident that the effective reducing agents were potassium thioglycolate and cysteamine HCl. Though Tris (2-carboxyethyl)phosphine hydrochloride was found to be effective, hair texture changedsignificantly. Hence, was not used for further experiments. It was also noted that while there was excellent colour uptake, colour bleeding was high.
Study C: Role of Adjuvants on Colour Bleeding and Grey Hair Coverage
Further studies on the use of adjuvants to influence colouring and colour bleeding were initiated usingdifferent adjuvantsat different concentrations in the Component A. The results are given in Table 6, PartsA, B and C.
Table 6: Influence of Different Adjuvants on the Grey Hair Coverage and Color Bleeding
(The formulations of Component A and Component B as given in Table 1 and Table 2)
Table 6, Part A
Expt No 5 6 8 9 11 12
Basic Brown 16 4 4 4 4 4 4
HC Blue 16 4 4 4 4 4 4
Basic Red 76 2 2 2 2 2 2
Adjuvants
CutissentialBehenyl 18-MEA1 0.5 1 1.2 2 3
Ingredients (In Component B)
Potassium thioglycolate 14 14 14 14 14 14
Observation on Hair Coloring (Mixing Ratio of Components A & B = 1:1
Grey Hair Coverage (%) 100% 100% 100% 100% 100% 100%
Colour of Hair Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black
Color Bleeding 5 3 3 1 1 1

Table 6, Part B
Expt No 20 22 24 26 31 33 35 37
Ingredients (in Component A)
Basic Brown 16 4 4 4 4 4 4 4 4
HC Blue 16 4 4 4 4 4 4 4 4
Basic Red 76 2 2 2 2 2 2 2 2
Adjuvants
NDurhance AA20002 0.5 1 1.5 3
Incroquat™ Behenyl TMS3 0.5 1 1.5 3
Ingredients (in Component B)
Potassium thioglycolate 14 14 14 14 14 14 14 14
Observation on Hair Colouring (Mixing Ratio of Components A & B = 1:1)
Grey Hair Coverage (%) 100% 100% 100% 100% 100% 100% 100% 100%
Colour of Hair Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black
Color Bleeding 5 5 4 4 3 3 1 1

Table 6, Part C
Expt No 38 40 42 44 45 47 48 49 51
Ingredients (in Component A)
Basic Brown 16 4 4 4 4 4 4 4 4 4
HC Blue 16 4 4 4 4 4 4 4 4 4
Basic Red 76 2 2 2 2 2 2 2 2 2
Adjuvants
Silsoft AX-E4 0.5 1 1.5 3
ChromapolColorPOP polymer5 0.5 1 1.2 1.5 3
Ingredients (in Component B)
Potassium thioglycolate 14 14 14 14 14 14 14 14 14
Observation on Hair Colouring (Mixing Ratio of Components A & B = 1:1)
Grey Hair Coverage (%) 100% 100% 100% 100% 100% 80% 80% 70% Poor
Colour of Hair Natural Black Natural Black Natural Black Natural Black Natural Black Dull Black Dull Black Dull Black Dull Black
Color Bleeding 5 4 4 3 3 3 1 1 1
Notes:
1 = INCI Name: BehentrimoniumMethosulfate (and) C10-40IsoalkylamidopropylethyldimoniumEthosulfate (and) Cetyl Alcohol) - 40 % cationic actives (Behenyl and C10-40Isoalkylamidopropylquat);2 = INCI Name: Acrylamidopropyltrimonium Chloride/Acrylamide Copolymer) - 20% active;3 = INCI Name: BehentrimoniumMethosulfate (and) Cetearyl Alcohol) - 50% active;
4 = INCI Name: Bis-Cetearyl Amodimethicone (and) Ceteareth-7 (and) Ceteareth-25) - 45% active;5 = Polyurethane-10 - % Active 40%

A perusal ofTable 6(Parts A, B and C)showed that not all adjuvantsprevent the colour bleeding.Some of the adjuvants such as the ColorPOP arrest the colourbleeding,but hinder the colour deliveries (Expt no: 45, 47, 48, 49 and51). All the other adjuvants evaluated gave good colour to hair. But it was observed that the adjuvants CutissentialBehenyl 18-MEA1and Incroquat™ Behenyl TMS3 gave the least colour bleeding while colour deliveries were excellent.Both theseadjuvants containBehentrimoniumMethosulfate. This suggeststhat the ingredients containing alkylamino cationic molecules of certain chain lengths only can prevent colour bleeding.In these cases, Behentrimoniummethosulfate, which is a C22 chain length alkylamine cationic surfactant were involved. Synergy between the dyes andBehentrimoniummethosulfate, work effectively for 100% grey hair coverage and minimalcolor bleeding.
In order to assess the generality of this observation, several alkylamino cationic molecules were evaluated. To evaluate the efficacy of different chain length alkyl amine surfactant/compounds in reducing the colour bleeding, experiments were carried out with Fentacare DHT21, FentacareTEP, BKC, polyquaterium-53, and polyquaternium-10. The results are tabulated in Table 7. From theTable 7 (Parts A and B), Fentacare DHT21, Fentacare TEP and Polyquaternium-53, deliver minimal color bleeding with 100% grey hair coverage and natural black shade. Though BKC gives minimal color bleeding, the shade was dull black with 80% grey hair coverage. From the results, it can be concluded that the chain length of the alkyl groups should be more than C18 to get minimal colour bleeding.
Table 7: Effectiveness of Different Alkylamine Surfactant/Compounds on the Grey Hair Coverage and Colour Bleeding.
(The formulations of Component A and Component B as given in Table 1 and Table 2)
Table 7, Part A
Expt No 52 53 52 53 54 55 56 57 58
Ingredients (in Component A)
Basic Brown 16 4 4 4 4 4 4 4 4 4
HC Blue 16 4 4 4 4 4 4 4 4 4
Basic Red 76 2 2 2 2 2 2 2 2 2
Adjuvants
Fentacare DHT21a 1 1.2 1.5
Fentacare ® TEPb 1 1.2 1.5
BKCc 1 1.2 1.5
Ingredients (in Component B)
Potassium thioglycolate 14 14 14 14 14 14 14 14 14
Observation on Hair Colouring (Mixing Ratio of Components A & B = 1:1)
Grey Hair Coverage (%) 100% 100% 100% 100% 100% 100% 80% 80% 80%
Colour of Hair Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black Dull Brownish Black Dull Brownish Black Dull Brownish Black
Color Bleeding 3 3 1 3 3 1 1 1 1
Notes:
a = Dihydrogenated tallow dimethyl ammonium chloride
b = Di(palmiticcarboxyethyl)hydroxyethyl methyl ammonium methylsulfate
c = Benzalkonium chloride

Table 7, Part B
Expt No 33 34 35 59 60 61 62 63 64
Ingredients (in Component A)
Basic Brown 16 4 4 4 4 4 4 4 4 4
HC Blue 16 4 4 4 4 4 4 4 4 4
Basic Red 76 2 2 2 2 2 2 2 2 2
Adjuvants
Incroquat™ Behenyl TMS 1 1.2 1.5
Polyquaterium-53 1 1.2 1.5
Polyquaternium-10 1 1.2 1.5
Ingredients (in Component B)
Potassium thioglycolate 14 14 14 14 14 14 14 14 14
Observation on Hair Colouring (Mixing Ratio of Components A & B = 1:1)
Grey Hair Coverage (%) 100% 100% 100% 100% 100% 100% 80% 80% 80%
Colour of Hair Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black Natural Black
Color Bleeding 3 1 1 2 1 1 4 4 3

Thus, it is demonstrated that many alkylamino cationic molecules can effectively work as an adjuvant to the dyes and provide good grey hair coverage as well as minimum colour bleeding.
It is further shown that such combinations also work effectively for other colour shades and provide excellent grey hair coverage as well as minimum bleeding. Detailed results are presented in Table 8.
Table 8: Effectiveness of Selected Alkylamino Cationic Moleculestowards Grey Hair Coverage and Colour Bleeding with Different Direct Dyes.
(The formulations of Component A and Component B as given in Table 1 and Table 2)
Expt No 65 66 67 68 69 70
Ingredients (in Component A)
Basic Brown 16 4
HC Blue 16 4
Blue 12 4
Basic Brown 17 4
Basic red 51 4
HC Yellow 2 4
Adjuvants
Incroquat™ Behenyl TMS 1.2 1.2 1.2 1.2 1.2 1.2
Ingredients (in Component B)
Potassium thioglycolate 14 14 14 14 14 14 14 14 14
Observation on Hair Colouring (Mixing Ratio of Components A & B = 1:1)
Grey Hair Coverage (%) 100% 100% 100% 100% 100% 100%
Colour of Hair Intense Blue Dark Brown Dark Blue Dark Brown Brick red Yellow
Color Bleeding 1 1 1 1 1 1
Table 8 shows the other shades which can be obtained with different direct dyes. Wide range of shades could be obtained with minimal colour bleeding.
Table 9 shows the efficacy of a 3-component system containing dyes, reducing agents and alkylamine cationic agents towards grey hair coverage and colour bleeding. Even if Cationic alkylamine agents are used as a third component, the grey hair coverage is not compromised and color bleeding is minimal as shows in Table 9.
Table 9: Effectiveness of 3-component System Towards Grey Hair Coverage and Colour Bleeding
(The formulations of Component B, Component C and Component Das given in Table 2, and Table 3)
Expt No 86
Basic Brown 16 4
HC Blue 16 4
Basic Red 76 2
Ingredients (In Component B)
Potassium thioglycolate 14
Ingredients (In Component C)
IncroquatTMBehenyl TMS 1.2
Observation on Hair Coloring (Mixing Ratio of Components B:C:D = 1:1:1)
Grey Hair Coverage (%) 100%
Colour of Hair Natural Black
Color Bleeding 1

Table 10: UV-Vis absorbance value to show the role of Behentrimoniummethosulfate in color bleeding
Dyes Cutissentialbehenyl 18-MEA Absorbance Value max(nm)
Dye Composition in Expt79 0 0.7 582
Dye Composition in Expt 9 1.2 0.05 582
Table 10 shows the UV-vis absorbance values for the dye composition used to achieve natural black shade with and without Cutissential™ Behenyl18-MEA. Referring Figure 1 shows UV-vis absorption value of Composition without any adjuvants (Experiment No: 79) and Composition with CutissentialBehenyl TMS 50 (Experiment No: 9).
As a result, an embodiment of the present disclosure includes figures and tables demonstrating a synergistic composition of direct dyes, reducing agents and alkylamino cationic molecules for hair colouring giving long lasting colour, excellent colour retention, 100% grey hair coverage, and minimal colour bleeding.
Therefore, it was evident from the comparativestudy that the components of the hair colour when present in specific concentrationwas synergistically effective in developing the colour on hair with 100% grey hair coverage in a predeterminedtimeperiod and retaining the colour fastness with minimal color bleeding.

ADVANTAGES:
1. The present disclosure provides a synergistic composition that is safe.
2. The present disclosure provides a synergistic composition that is easy to use.
3. The present disclosure provides a synergistic composition that is simple to apply.
4. The present disclosure provides a synergistic composition giving excellent colour delivery to hair with complete (100%) grey hair coverage.
5. The present disclosure provides a synergistic composition giving excellent colour retention.
6. The present disclosure provides a synergistic composition with long lasting colour.
7. The present disclosure providesa synergistic composition giving that gives minimal colour bleeding.
8. The present synergistic hair colour composition is free of dye precursors / intermediates and hydrogen peroxide.
, Claims:We Claim:
1. Amulti-component hair colour composition with minimal colour bleeding comprising:
(i) 0.1 to 6 mass % of direct dye/s;

(ii) 0.1% to 5 mass % of alkylamine cationic agent/s;

(iii) 0.1 to 25 mass % reducing agent/s and

(iv) cosmetically acceptable base with scalp and hair benefit agents.

2. The composition as claimed in claim 1, wherein the direct dye is selected from Basic Brown 16, Basic red 76, Blue 12, Basic Brown 17, Basic red 51, Basic Blue 99, Basic Violet 1, Basic Violet 2, Basic Violet 3, Basic Yellow 57, Basic Red 2, Basic Red 12, Basic Red 22, HC Blue 2, HC Blue 4, HC Blue 5, HC Blue 6, HC Blue 7, HC Blue 8, HC Blue 9, HC Blue 10, HC Blue 11, HC Blue 12, BC Blue 13, HC Blue 16, HC Brown 1, HC Brown 2, HC Green 1, HC Orange 1, HC Orange 2, HC Orange 3, HC Orange 5, HC Red 1, HC Red 3, HC Red 7, HC Red 54, HC Red BN, HC Violet 1, HC Violet 2, HC Yellow 2, HC Yellow 4, HC Yellow 5, HC Yellow 6, HC Yellow 7. HC Yellow 8, HC Yellow 9, HC Yellow 10, HC Yellow 11, HC Yellow 12, HC Yellow 13, HC Yellow 14 and HC Yellow 15or combination thereof.

3. The composition as claimed in claim 1, wherein the alkylamine cationic agent is selected from Trimethyl-n-octylammonium Chloride, Trimethylstearylammonium Bromide, Trimethyltetradecylammonium Chloride, Heptadecyltrimethylammonium Bromide, Hexadecyltrimethylammonium Bromide, Trimethylnonylammonium Bromide, Domiphen Bromide, Di(C12-C18)-alkyldimethylammonium chloride, Di(C12-C18)-alkyldimethylammoniumbromide; (C12-C18)-alkyldimethylbenzylammonium chloride, (C16-C18)-alkylpentaoxyethylammonium chloride, dioctadecyldimethylammonium bromide, distearoylethyldimonium chloride, cetyltrimethylammonium chloride, cetyltrimethylammonium bromide, cetyltrimethylammoniummethosulfate, stearyltrimethylammonium chloride, Cocamidopropyltrimonium Chloride, UndecyleneamidopropyltrimoniumMethosulfate, BehentrimoniumMethosulfate, C10-C40Isoalkylamidopropyl-ethyldimoniumEthosulfate, Acrylamidopropyltrimonium Chloride/Acrylamide Copolymer, Dihydrogenated tallow dimethyl ammonium chloride, Di(palmitic carboxyethyl)hydroxyethyl methyl ammonium methylsulfate, Benzalkonium chloride, polyquaterium-53 and polyquaternium-10 or combinations thereof.

4. The composition as claimed in claim 1, wherein the reducing agent is selected from thioglycolic acid and its salts, thiolactic acid and its salts, dihydrolipoate, thioglycerol, mercaptopropionic acid and its salts, cysteine and its salts, N substituted cysteins, cystamine and its salts, thioethanol, sulfite salts, bisulfite salts and metabisulfite salts, dithionite salts, (2-carboxyethyl) phosphine and its salts, glyoxylic acid and its salts, ascorbic acid and its salts as well as derivatives or combination thereof.

5. The composition as claimed in claim 1, wherein the cosmetically acceptable bases is selected from a rheology modifier and a pH modifier and other hair/scalp benefiting agents such as a conditioning agent, a penetration aid, a humectant, an emollient, an emulsifier, a surfactant and a softening agent or combination thereof.

6. The composition as claimed in claim 5, wherein the rheology modifier is selected from Acrylates Copolymer, Acrylates/C10-C30 Alkyl Acrylate Crosspolymer, Acrylates/Beheneth-25 Methacrylate Copolymer, Acrylates/Steareth-20 Itaconate Copolymer, Acrylates/Ceteth-20 Itaconate Copolymer, sodium alginate; cellulose derivatives such as methyl cellulose, hydroxyethyl cellulose, hydroxymethyl cellulose, hydroxypropyl cellulose or combination thereof.

7. The composition as claimed in claim 5, wherein the pH modifier is selected from phosphoric acid, ascorbic acid and lactic acid, and alkalis such as monoethanolamine, triethanolamine, 2-amino-2-methyl-1-propanol,ammonia, soda lye, potash lye, and tris(hydroxymethyl)aminomethane or combination thereof.

8. The composition as claimed in claim 1, wherein the composition pHranges from7 - 12.

9. The composition as claimed in claim 1, wherein the composition developmental time is 5 minutes to 60 minutes.

Dated this the 10thDay of March, 2023 Anjan Sen
Of Anjan Sen and Associates
(Applicants Agent)
IN/ PA-199