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Hair Colouring Composition And A Process For Preparing The Same

Abstract: ABSTRACT HAIR COLOURING COMPOSITION AND A PROCESS FOR PREPARING THE SAME The present disclosure provides a hair coloring composition comprising 1.6 to 4.1 mass% of para-phenylenediamine and 2,5-diaminotoluenesulphate as coloring agents, 1.6 to 4.0 mass% of meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene as coupling agents, 0.16 to 0.75 mass% of iso-ascorbic acid and sodium sulphate as antioxidants, 1.5 to 2.5 mass% of a surfactant, 0.09 to 0.11 mass% of ethylene diamine tetra acetate (EDTA) as chelating agent, 1.35 to 6.0 mass% of monoethanol amine as alkalizer, 0.13 to 0.9 mass% of magnesium sulphate as stabilizer, and additives selected from the group consisting of a fluid medium, emulsifiers, a fragrance, a conditioning agent and thickening agents. The mass% of each of the components is with respect to the total mass of the composition. The hair coloring composition of the present disclosure develops the color in a short duration of time and retains the color even after repeated washings.

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Patent Information

Application #
Filing Date
05 June 2018
Publication Number
49/2019
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
dewan@rkdewanmail.com
Parent Application

Applicants

HYGIENIC RESEARCH INSTITUTE PVT. LTD.
602, Supreme Chambers, Andheri (West), Mumbai – 400053, Maharashtra, India

Inventors

1. PAWAR, Ajit
Flat No 202, Bldg. No B-8, Sector 10, Near Swami Narayan Mandir, Shantinagar, Mira Road (E), Mumbai-401107, Maharashtra, India
2. GADGIL, Makarand
101, B wing , Ramchandra park, Pawar nagar , Near Smashan Bhumi, Nandiwali Pada ,Sagaon, Dombivli (E), Mumbai-421201, Maharashtra, India
3. RAI, Sadananda
Kausthubha Bolwar, Puttur D.K, Karnataka 574201, India

Specification

DESC:FIELD
The present disclosure relates to a hair coloring compositions and a process for its preparation.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Coloring of human hair is well known in view of changing styles and fashions. Dyes formulated for coloring hair fibers, are typically termed temporary, semi-permanent, or permanent. Temporary and semi-permanent dyes or hair colors last through a few shampoos, while permanent hair colors are retained for six weeks and longer.

During coloring of the hair, “keratin”, the unique protein material of hair is repeatedly subjected to both chemical and mechanical damage. Further, keratin damage also occurs from combing and brushing, as well as from sunlight, chlorinated water, shampooing, permanent waving, and other such treatments involving various chemicals. Due to such keratin damages, the distal ends of each hair fiber tend to have substantially more damage than the proximal ends nearer to the scalp based on the length of the hair fibre. This inconsistency causes variation in the dye uptake by the hair fiber, resulting in color variations along the length of the hair fiber.
Further, conventional dyes have drawbacks for the longevity or wearability of the resulting color, its ability to resist fading, and its ability to resist changes due to washing, combing, or rubbing.
If an individual does not regularly have the color reapplied, the hair fibers will develop an uneven hair color, due to the uneven distribution of the dye along the hair fibers. This produces an unnatural appearance and cast to the hair. Furthermore, the repeated use required by such product causes excess dyestuff rinsed from the hair to enter the waterways, thereby adding to the cumulative problems presently being realized in the contamination of ground water.
In spite of the long history of coloration of hair and the extensive effort that has been expended in attempting to eliminate the problems associated with the dyeing of human hair, no system has been achieved which is capable of overcoming all of the drawbacks and difficulties encountered with hair dyes.
Therefore, there is a felt a need to develop a hair coloring composition which requires short dyeing time has a rapid color development on hair, has good hair dyeing property, is safe and has good color tone and lasts for a long time.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a hair coloring composition.
Still another object of the present disclosure is to provide a hair coloring composition which is peroxide and ammonia free.
Yet another object of the present disclosure is to provide a hair coloring composition that provides rapid color development.
Yet another object of the present disclosure is to provide a process for the preparation of a hair coloring composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
In a first aspect, the present disclosure provides a hair coloring composition comprising para-phenylenediamine and 2,5-diaminotoluenesulphate as coloring agents, in an amount in the range of 1.6 to 4.1 mass%, meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene as coupling agents, in an amount in the range of 1.6 to 4.0 mass%, iso-ascorbic acid and sodium sulphate as antioxidants, in an amount in the range of 0.16 to 0.75 mass%, a surfactant, in an amount in the range of 1.5 to 2.5 mass%, ethylene diamine tetra acetate (EDTA) as chelating agent, in an amount in the range of 0.09 to 0.11 mass%, monoethanol amine as alkalizer, in an amount in the range of 1.35 to 6.0 mass%, magnesium sulphate as stabilizer, in an amount in the range of 0.13 to 0.9 mass%, at least one nourishing agent selected from the group consisting of Phyllanthus emblica extract, Eclipta prostrata extract, Hibiscus rosa-sinensis extract, Trigonella foenum-graecum extract, walnut oil and argan oil, in an amount in the range of 0.05 to 0.5 mass%, and additives selected from the group consisting of a fluid medium, emulsifiers, a fragrance, a conditioning agent and thickening agents. The mass% of each of the component in the hair coloring composition is with respect to the total mass of the composition.
In accordance with the present disclosure, the mass ratio of para-phenylenediamine and 2,5-diaminotoluenesulphate is in the range of 0.7:1 to 0.8:1.
In accordance with the present disclosure, the mass ratio of 2,4-diaminophenoxyethanol dihydrochloride to 2,5-diaminotoluene sulphate is in the range of 0.1:1 to 0.3:1, the mass ratio of meta-aminophenol to para-phenylenediamine is in the range of 0.1:1 to 0.4:1, the mass ratio of N,N-Bis-(2-Hydroxyethyl)-p-phenylenediamine sulfate to 2,5-diaminotoluene sulphate is in the range of 0.096:1 to 0.11:1, the mass ratio of para-aminophenol to para-phenylenediamine is in the range of 0.1:1 to 0.27:1, and the mass ratio of para-phenylenediamine to 1,2,4-Trihydroxy benzene is in the range of 0.5:1 to0.7:1.
In accordance with the present disclosure, the composition further comprises additives selected from the group consisting of a fluid medium in an amount in the range of 25 to 90 mass%, emulsifiers in an amount in the range of 4.0 to 7.0 mass%, a fragrance in an amount in the range of 0.25 to 0.75 mass%, conditioning agents in an amount in the range of 0.3 to 2.5 mass%, and thickening agents in an amount in the range of 4.0 to 7.0 mass%.
The present disclosure also provides a process for the preparation of a hair colouring composition. The process comprises the steps of preparing a dye phase (phase A), an oil phase (phase B ), conditioner phase (phase C) and coupler phase (phase D). The dye phase (phase A), the oil phase (phase B), conditioner phase (phase C) and coupler phase (phase D) are mixed under stirring. The pressure is reduced in the range of 300 to 650 mm/Hg to obtain hair coloring composition.
DETAILED DESCRIPTION
Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details, are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
The present disclosure envisages an autooxidative hair coloring composition that is free of peroxide and ammonia, and is capable of rapid color development on hair.
In accordance with the present disclosure, the hair coloring composition can be in a form selected from the group consisting of gel, emulsion, cream, powder, suspoemulsion and the like.
In an aspect, the hair coloring composition of the present disclosure comprises at least one coloring agent (dye), at least one coupling agent, at least one antioxidant, at least one chelating agent, an alkalizer, a stabilizer, at least one nourishing agent and additives.
Typically, the hair coloring composition comprises para-phenylenediamine and 2,5-diaminotoluenesulphate as coloring agents (dye), in an amount in the range of 1.6 to 4.1 mass%, meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene as coupling agents, in an amount in the range of 1.6 to 4.0 mass%, iso-ascorbic acid and sodium sulphate as antioxidants, in an amount in the range of 0.16 to 0.75 mass%, a surfactant, in an amount in the range of 1.5 to 2.5 mass%, ethylene diamine tetra acetate (EDTA) as chelating agent, in an amount in the range of 0.09 to 0.11 mass%, monoethanol amine as alkalizer, in an amount in the range of 1.35 to 6.0 mass%, magnesium sulphate as stabilizer, in an amount in the range of 0.13 to 0.9 mass%, at least one nourishing agent selected from the group consisting of Phyllanthus emblica extract, Eclipta prostrata extract, Hibiscus rosa-sinensis extract, Trigonella foenum-graecum extract, walnut oil and argan oil, in an amount in the range of 0.05 to 0.5 mass%, and additives selected from the group consisting of a fluid medium, emulsifiers, a fragrance, a conditioning agent and thickening agents. The mass% of each of the component in the hair coloring composition is with respect to the total mass of the composition.
Coloring agent (dye) is a primary intermediate in the hair coloring composition, which reacts with coupling agent(s)/coupler(s) to provide a desired shade upon oxidation in hair.
In accordance with the embodiments of the present disclosure, the coloring agent is at least one selected from para-phenylenediamine and 2,5-diaminotoluenesulphate.
Para-phenylenediamine and 2, 5-diaminotoluene sulphate are primary dyes. Both para-phenylenediamine and 2,5-diaminotoluene sulphate are auto-oxidation dyes, as a result of which the hair colouring composition of the present disclosure does not require use of ammonia, a foul smelling compound and an irritant, as a component.
In one embodiment the coloring agent is a combination of para-phenylenediamine and 2, 5 diamino toluene sulphate.
Para-phenylenediamine (PPD) [CAS no. 106-50-3] penetrates hair shaft and follicle and strongly binds protein. These properties of para-phenylenediamine make it an effective hair dyeing chemical that is widely used as a permanent hair dye. The primary oxidation intermediate of para-phenylenediamine is highly reactive and in combination with an auto-oxidizable dye coupler 1,2,4-trihydroxy benzene, forms an oxidation condensate, which upon application becomes trapped within the structure of hair and rapidly oxidizes upon exposure to atmospheric oxygen, to develop natural black or black brown colour. Efficacy of the hair colour composition increases with the quantity of PPD, thereby providing more coverage and reduced fading even after hair wash. However, higher quantities PPD can cause allergic and skin reactions. Therefore, in the present disclosure, the amount of PPD in the hair colouring composition is kept below 4% with respect to the total mass of the hair colouring composition.
2,5-diamino toluene sulphate [CAS Number 615-50-9] is commonly used in hair coloring. Comparatively, 2,5-diamino toluene sulphate is a safer dye, however it is more expensive and required in larger quantities. 2,5-Diaminotoluene sulphate is a substitute for phenylenediamine (1,4-diaminobenzene) in commercial hair dyes. 2,5-diaminotoluene sulphate is less reactive than the para-phenylenediamine in the presence of 1,2,4-trihydroxy benzene. In the present disclosure, 2,5 diaminotoluene sulphate is added to the composition along with para-phenylenediamine (PPD), to reduce the rate of the reaction with 1,2,4-trihydroxy benzene with para-phenylenediamine (PPD). It helps to improve the shelf life of the hair colouring composition. It is also preferred because of its lower toxicity as compared to para-phenylenediamine (PPD).
In accordance with the embodiments of the present disclosure, the mass ratio of para-phenylenediamine to 2,5-diaminotoluenesulphate is in the range of 0.7:1 to 0.8:1.
In accordance with one embodiment of the present disclosure, the mass ratio of para-phenylenediamine to 2,5-diaminotoluenesulphate is 0.75:1.
The coupling agent/coupler undergoes a coupling reaction with the colouring agents to form high molecular weight products, which are trapped in the hair matrix and cannot be readily removed during washing, which thereby helps in retaining the hair color/dye even after repeated washing. The coupling agent/coupler can be one compound or a mixture of compounds.
In accordance with the embodiments of the present disclosure, the coupling agent is at least one selected from the group consisting of meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene.
In one embodiment the coupling agent is a combination of meta amino phenol, 2,4-diaminophenoxyethanol dihydrochloride, para amino phenol, N,N Bis (2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene.
In accordance with the embodiments of the present disclosure, the ratio of para-phenylenediamine (colouring agent) to 1,2,4-trihydroxybenzene (coupling agent) is in the range of 0.3:1 to 0.7:1.
In the present disclosure, the ratio of para-phenylenediamine (colouring agent) to 1,2,4-trihydroxybenzene (coupling agent), which is in the range of 0.3: 1 to 0.7:1, is optimized to obtain desired hair colouring composition. If para-phenylenediamine content of the hair colouring composition is increased beyond this ratio, 1,2,4-trihydroxy benzene is consumed very fast and as a result the hair colouring composition has reduced shelf life.
2,4-diaminophenoxyethanol dihydrochloride [CAS 66422-95-5] reacts with para-phenylenediamine to form blue shade.
Meta-aminophenol also known as 3-aminophenol [CAS no. 591-27-5] is an organic compound. It is an aromatic amine and aromatic alcohol. It is the meta isomer of 2-aminophenol and 4-aminophenol.
N,N Bis (2-Hydroxyethyl)-p-phenylenediamine Sulfate [CAS no. 54381-16-7] is used as coupler in the composition of the present disclosure.
Para-aminophenol also known as 4-aminophenol [CAS no. 123-30-8] is an organic compound, available as a white powder. It is dye coupler. It gives brown shade. Para amino phenol accelerates the reaction rate of (coloring hair) para-phenylenediamine during dyeing the hair, which reduces the coloring time to around 50% with respect to the conventional hair color. Moreover, use of para amino phenol along with para-phenylenediamine retains the black shade and near brownish color even after repeated hair washing.
1,2,4-trihydroxybenzene [CAS No.533-73-3] is an aromatic triol that acts as a dye coupler and results in auto-oxidation of the dyes when exposed to aerial oxygen. The aromatic triol controls the speed at which the dye intermediate oxidizes in the presence of atmospheric oxygen. The aromatic triol(s) and primary oxidation intermediate(s) in combination forms the oxidation condensate, which upon application becomes trapped within the structure of hair and rapidly oxidizes upon exposure to atmospheric oxygen.
In the present disclosure, the hair coloring composition comprises 1,2,4 trihydroxy benzene, which acts as auto-oxidizable dye coupler. Therefore, the hair colouring composition of the present disclosure does not need a separate developer like ammonia or hydrogen peroxide.
In accordance with the present disclosure, the mass ratio of 2,4-diaminophenoxyethanol dihydrochloride to 2,5-diaminotoluene sulphate is in the range of 0.1:1 to 0.3:1, the mass ratio of meta-aminophenol to para-phenylenediamine is in the range of 0.1:1 to 0.4:1, the mass ratio of N,N-Bis-(2-Hydroxyethyl)-p-phenylenediamine sulfate to 2,5-diaminotoluene sulphate is in the range of 0.096:1 to 0.11:1, the mass ratio of para-aminophenol to para-phenylenediamine is in the range of 0.1:1 to 0.27:1, and the mass ratio of para-phenylenediamine to 1,2,4-trihydroxy benzene is in the range of 0.5:1 to 0.7:1.
In the present disclosure, five different couplers are used in combination to provide a hair colouring composition that provides natural black or black brown shade to the hair dyed with the composition. Each of these coupling agent reacts with the colouring agents to provide various different shades and tints, which on combination leads to formation of desired colour shade on the hair. For example, para-aminophenol provides an amber shade, meta-aminophenol provides brown shade, and 2,4 diamino phenoxy ethanol di hydrochloride provides bluish ting. However, various combinations of each of these five different coupling agents with two colouring agents, provides the desired natural black shade.
The auto oxidizing hair colour composition oxidizes in the presence of air, without addition of a developer. Therefore, it essential to add an anti-oxidant to the hair colouring composition to ensure that the packaged product does not oxidize until its use. The anti-oxidant helps in increasing the shelf life of the hair colouring composition.
Antioxidants retard the oxidation reaction during the storage of the hair colouring composition. It also helps to minimize the staining of the skin. The antioxidants inhibit the oxidation of the hair colouring composition caused by free radicals. However, larger quantity of antioxidant would result in a hair colouring composition that does not oxidize even after its application to the hair, whereas a smaller quantity of antioxidant would cause the hair colouring composition to oxidize in the package even before its application to the hair. Therefore, it is imperative that an anti-oxidant is added to the hair coloring composition at an optimum concentration to achieve the desired results.
In accordance with the embodiments of the present disclosure, the antioxidant is at least one selected from iso-ascorbic acid and sodium sulphite.
In one embodiment, the antioxidant is a combination of sodium sulphite and iso-ascorbic acid. Sodium sulphite [CAS No. 7757-83-7] is used as antioxidant /reducing agent in cosmetics and personal care products. Iso-ascorbic acid [CAS No. 89-65-6] is used as antioxidant / reducing agents in cosmetics and personal care products.
In accordance with the embodiments of the present disclosure, the mass ratio of iso-ascorbic acid and sodium sulphate is in the range of 6:1 to 7.78:1.
In accordance with one embodiment of the present disclosure, the mass ratio of iso-ascorbic acid and sodium sulphate is 6:1.
In accordance with one embodiment of the present disclosure, the mass ratio of iso-ascorbic acid and sodium sulphate is 7.5:1.
Surfactant is added to hair colouring composition to reduce the surface tension of water and also reduce the interfacial tension between oil and water. It has ability to quickly wet out the hair which allows easy penetration of dyes and dye intermediates. It ensures better and uniform spreading of the hair colouring composition on application to the hair by countering any resistance offered by natural oils present in the hair and scalp.
Surfactant also acts as an emulsifier and helps incorporate any nourishing oils (argan oil, walnut oil) that may be added to the hair colour.
The surfactant can be selected from the group consisting of sodium lauryl sulphate, coco amido propyl betaine, coco diethanolamide, sodium sarcosinate, and the like.
The surfactant used in the composition of the present disclosure is sodium lauryl sulphate. Sodium lauryl sulfate [CAS No. 151-21-3] is a synthetic organic compound with the formula NaC12H25SO4. It is an anionic surfactant used in many cleaning and hygiene products.
Chelating agents, also known as chelants, chelators, or sequestering agents, are chemical compounds that react with metal ions or contaminants by forming at least two bonds with the metal ion to form a stable, water-soluble complex, thereby allowing the metal complex to be excreted.
In one embodiment, the chelating agent is ethylene diamine tetra acetate (EDTA). EDTA [CAS no. 60-00-4] acts as a chelating agent and as a stabilizer in cosmetics to prevent ingredients in a given formula from binding with trace elements (particularly minerals) that can be present in water. EDTA also keeps other ingredients from causing unwanted changes to a product’s texture, odor, and/or consistency.
An alkalizer is a chemical compound that is used for adjusting the pH of the hair colouring composition. The alkaline pH of the formulation allows hair shaft to swell which allows the dye precursor to penetrate hair and oxidize and combine to form large molecules. These large molecules contain conjugated double bonds, which gives color to the hair.
In the present disclosure, mono-ethanolamine is added to the hair colouring composition to increase the pH of the formulation. Hair colouring composition with a pH value in the range of of 9-10 helps the dye molecules penetrate hair cuticles as they open up at an alkaline pH. Increased quantity of the alkalizer helps raise the pH of the hair colouring composition.
The alkalizer used in the cream based hair coloring composition of the present disclosure is monoethanol amine. Monoethanolamine [CAS no: - 141-43-5] is an organic chemical compound. The molecule is both a primary amine and a primary alcohol. Ethanolamine is a colorless, viscous liquid.
Stabilizer is a key ingredient of the hair colouring composition as it forms a complex with the dye and the protein (keratin) present in hair to ensure that the hair colour binds to the hair and is retained for longer time. It is known to prevent degradation of the dyes and thereby keep the hair colour stable.
The stabilizer used in the cream based hair coloring composition of the present disclosure is magnesium sulphate. Magnesium sulphate [CAS No. 7487-88-9] helps to stabilize the dyes added in the formulation. As 1,2,4-trihydroxy benzene is highly unstable, magnesium ion present in the formulation stabilizes it. It can also acts as a catalyst.
The nourishing agents that may be introduced in the cream based hair coloring composition provide nourishment to the hair and helps in its healthy growth. It is natural herbal extract and has nourishment properties. The cream based hair coloring composition of the present disclosure comprises extracts of various plants which provide nourishment to the hair.
In accordance with the embodiments of the present disclosure, the nourishing agent is at least one selected from the group consisting of Phyllanthus emblica extract, Eclipta prostrata extract, Hibiscus rosa-sinensis extract, Trigonella foenum-graecum extract, walnut oil and argan oil.
In one embodiment of the present disclosure, the nourishing agent is a combination of Phyllanthus emblica extract from whole fruits, Eclipta prostrata extract from whole shrub, Hibiscus rosa-sinensis extract from whole flower, and Trigonella foenum-graecum extract from seeds, all of which were purchased from the local market in Gujarat. Walnut oil and argan oil were imported from outside India.
Eclipta prostrata (Asteraceae), also known as false daisy, and Bhringraj grows in moist places all over the world. It is widely distributed throughout India, China, Thailand and Brazil.
Hibiscus rosa-sinensis (Malvaceae), also known as Chinese hibiscus, China rose, Hawaiian hibiscus, and shoeblack plant, is a species of tropical hibiscus, native to East Asia.
Phyllanthus emblica (Phyllanthaceae), also known as emblic, emblic myrobalan, myrobalan, Indian gooseberry, Malacca tree, and amla is a deciduous tree, indigenous to a large area ranging from Nepal, India, and Sri Lanka, throughout South-East Asia to southern China. It is widely cultivated for its fruits throughout its natural area of distribution, particularly in India, and also in the Mascarene Islands (Réunion, Mauritius), the West Indies and Japan.
Trigonella foenum-graecum (Fabaceae), also known as methi is cultivated worldwide as a semiarid crop. Major fenugreek-producing countries are Afghanistan, Pakistan, India, Iran, Nepal, Bangladesh, Argentina, Egypt, France, Spain, Turkey and Morocco.
The plant parts used in the cream based hair coloring composition of the present disclosure can be derived from the barks, roots, tubers, stigma, kernels, exudates, stolons, rhizome, leaves, seeds, nuts, berries, fruits, stems and flowers of the plants are commercially purchased from the market as value added products and therefore, the specific source of the product is unknown.
The hair coloring composition further comprises additives selected from the group consisting of fluid medium, emulsifiers, nourishing agents, a fragrance and a conditioning agent.
Typically, water is used as the fluid medium. In an embodiment of the present disclosure, demineralized water is used as the fluid medium. Typically, the fluid medium/water is used in an amount sufficient to make 100 mass% of the hair coloring composition. In an exemplary embodiment the fluid medium is in the range of 25 mass% to 90 mass%. Water dissolves many of the ingredients that impart benefits, such as conditioning agents and cleansing agents
In accordance with the embodiments of the present disclosure, the emulsifier is at least one selected from the group consisting of glyceryl stearate, polyethylene glycol ester of stearic acid (PEG 100 stearate), cetearyl alcohol, dicetyl phosphate and ceteth-10 phosphate.
In one embodiment, the emulsifier is a combination of glyceryl stearate, polyethylene glycol ester of stearic acid (PEG 100 stearate), cetearyl alcohol, dicetyl phosphate and ceteth-10 phosphate.
The combination of cetearyl alcohol [CAS No. 67762-27-0], dicetyl phosphate [CAS No. 8005-44-5] and ceteth-10 phosphate [CAS No. 50643-20-4] has unique emulsifying properties that allows to form emulsion which display markedly different characteristics than those of conventional emulsifying waxes. These emulsions exhibit a combination of natural substantivity, greater oil deposition and shear thinning (thixotrophy) in the composition.
Glyceryl stearate [CAS No. 31566-31-1] is a solid and waxy compound. It is made by reacting glycerin (a soap by-product) with stearic acid (a naturally occurring, vegetable fatty acid). Arlacel™ 165 is an acid-stable self-emulsifying glycerol monostearate.
Polyethylene glycol ester of stearic acid (PEG-100 stearate) [CAS No. 9004-99-3] is off-white, solid ester of polyethylene glycol (a binder and a softener) and stearic acid.
The conditioning agent typically attaches to the hair and creates a thin film, allowing the easier combing of wet or dry hair and imparts a silky feel to the hair.
In accordance with the embodiments of the present disclosure, the conditioning agent is at least one selected from dimethicone and polyquaternium-39.
In one embodiment, the conditioning agent is a combination of dimethicone, and polyquaternium-39. Dimethicone [CAS No. 9006-65-9] provides shine, smoothness to hair. Polyquaternium-39 [CAS no:- 25136-75-8] helps to deposit more color in to hair.
A thickening agent is a viscosity increasing agent in cosmetics and personal care products because of its capability to hold water.
In accordance with the embodiments of the present disclosure, the thickening agent is at least one selected from xanthan gum and cetostearyl alcohol.
In one embodiment, the thickening agent is a combination of xanthan gum and cetostearyl alcohol. Xanthan gum was imported from outside India.
Xanthan gum [CAS No. 11138-66-2] is a polysaccharide derived from glucose or sucrose (sugars) with many industrial uses, including use as a common food additive. Xanthan Gum is able to increase the viscosity of liquids even when used at less than 1% concentration. Xanthan gum also acts as a stabilizer to prevent ingredients from separating in the composition. Xanthan gum enhances freeze-thaw stability, and improves shelf life and helps with the stabilization of the composition. Xanthan Gum is also used as a binder, emulsion stabilizer and emulsifying surfactant.
Cetostearyl alcohol [CAS NO: ?67762-27-0] also known as cetearyl alcohol or cetylstearyl alcohol is a mixture of fatty alcohols, consisting predominantly of cetyl and stearyl alcohols and is classified as a fatty alcohol.
Fragrances are used in a wide variety of products to impart a pleasant odor, mask the inherent smell of some ingredients, and enhance the experience of using the product. The amount of fragrance can be in the range of 0.1 mass% to 2.0 mass% of the total mass of the hair coloring composition.
In one embodiment, the cream based hair coloring composition comprises 4.025 mass% of para-phenylenediamine and 2,5-diaminotoluenesulphate as coloring agents, 3.91 mass% of meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene as coupling agents, 0.161 mass% of iso-ascorbic acid and sodium sulphate as antioxidants, 2 mass% of sodium lauryl sulphate as surfactant, 0.1 mass% of ethylene diamine tetra acetate (EDTA) as chelating agent, 3.45 mass% of monoethanol amine as alkalizer, 0.138 mass% of magnesium sulphate as stabilizer, and 0.5 mass% of Amla extract (Phyllanthus emblica), Bhringraj extract (Eclipta prostrata), Jaswand extract (Hibiscus rosa-sinensis), Methi extract (Trigonella foenum-graecum), walnut oil and argan oil, as nourishing agents, 73.466 mass % of water as fluid medium, 4.5 mass% of a combination of cetearyl alcohol, dicetyl phosphate and ceteth-10 phosphate, and a combination of glyceryl stearate and polyethylene glycol ester of stearic acid (PEG 100 stearate), as emulsifiers, 0.5 mass% of a fragrance, 2.25 mass% of dimethicone and polyquaternium-39 as conditioning agents, and 5 mass % of xanthan gum and cetostearyl alcohol as thickening agents. The mass% of each of the component is with respect to the total mass of the composition.
In an exemplary embodiment, the cream based hair coloring composition comprises 1.725 mass% of para-phenylenediamine and 2.3 mass% of 2,5-diamino toluene sulphate, as coloring agents, 0.46 mass% of 2,4-diaminophenoxyethanol dihydrochloride, 0.1725 mass% of meta-aminophenol, 0.23 mass% of N,N-Bis-(2-Hydroxyethyl)-p-phenylenediamine sulfate, 0.1725 mass% of para-aminophenol and 2.875 mass% of 1,2,4-trihydroxybenzene, as coupling agents, 0.023 mass% of sodium sulphite and 0.138 mass% of iso-ascorbic acid (erythorbic acid), as antioxidants, 2 mass% of sodium lauryl sulphate as surfactant, 0.1 mass% of ethylene diamine tetra-acetic acid (EDTA) as chelating agent, 3.45 mass% of mono-ethanolamine as alkalizer, 0.138 mass% of magnesium sulphate as stabilizer, and 0.2 mass% of Amla extract (Phyllanthus emblica), Bhringraj extract (Eclipta prostrata), Jaswand extract (Hibiscus rosa-sinensis) and Methi extract (Trigonella foenum-graecum), 0.2 mass% walnut oil and 0.1 mass% argan oil, as nourishing agents, 73.466 mass % of water as fluid medium, 2.5 mass% of a combination of cetearyl alcohol, dicetyl phosphate and ceteth-10 phosphate, and 2.0 mass% of a combination of glyceryl stearate and polyethylene glycol ester of stearic acid (PEG 100 stearate), as emulsifiers, 0.5 mass% of a fragrance, 0.25 mass% of dimethicone, and 2.0 mass% of polyquaternium-39 as conditioning agents, 4.5 mass % of cetostearyl alcohol and 0.5 mass% of xanthan gum as thickening agents. The mass% of each of the component is with respect to the total mass of the composition.
The hair coloring composition is peroxide and ammonia free and hence is safe for use and is easy to apply. Further, the hair coloring composition is capable of developing the color in a short duration of time and the colour imparted to the hair is retained on the hair even after repeated washing of the hair. In accordance with the present disclosure, the color development time (on hair) of the hair coloring composition can be in the range from 10 minutes to 30 minutes.
In another aspect of the present disclosure, there is provided a process for preparing a hair coloring composition.
The process comprises mixing predetermined amount of reactants under stirring at a predetermined temperature and predetermined pressure to obtain hair color composition. In accordance with the present disclosure, the hair coloring composition can be in a form selected from the group consisting of gel, emulsion, cream, powder, suspoemulsion and the like.
In an exemplary embodiment, a process for cream based hair coloring composition is provided. The process for the preparation of cream based hair coloring composition is given in detail as below.
The process comprises the steps of preparing a dye phase (phase A), an oil phase (phase B ), conditioner phase (phase C) and coupler phase (phase D). The dye phase (phase A), the oil phase (phase B), conditioner phase (phase C) and coupler phase (phase D) are mixed under stirring. The pressure is reduced in the range of 300 to 650 mm/Hg to obtain hair coloring composition.
The process is hereinafter described in detail.
Initially, all the ingredients/raw materials are weighed and stored in individual poly bags or stainless steel vessel till use.
A dye phase (Phase A) is prepared by mixing surfactant into hot water having a temperature in the range of 80 oC to 85 oC followed by adding chelating agent, antioxidant, stabilizer, dyes, coupler, alkalizer under stirring to obtain a slurry, and adding nourishing agent into said slurry under stirring to obtain the phase A (dye phase). The nourishing agent is a combination of Phyllanthus emblica, Eclipta prostrata, Hibiscus rosa-sinensis, and Trigonella foenum-graecum.
An oil phase (Phase B) is prepared by separately mixing a nourishing agent, a thickening agent and an emulsifier to obtain a mixture, and heating the mixture to a temperature in the range of 60 oC to 75 oC under stirring to obtain a phase B (oil phase). The ratio of nourishing agent: thickening agent: emulsifier is in the range of 1:15:15. The nourishing agent is a combination of walnut oil and argan oil.
Conditioner phase (Phase C) is prepared by dissolving a conditioning agent in water to obtain a solution. The conditioning agent is polyquaternium-39.
Coupler phase (Phase D) is prepared by dissolving a coupler in water to obtain coupler solution. The coupler is 1,2,4-trihydroxy benzene.
Further, a thickening agent is mixed in a hot water having a temperature in the range of 80 oC to 85 oC, under stirring, to obtain a homogenous mixture. The thickening agent is xanthan gum.
In the next step, the homogenous mixture is mixed with the dye phase (phase A), under stirring, followed by the addition of the oil phase (phase B), at a temperature in the range of 65 oC to 75 oC, to obtain homogenized resultant slurry. Nitrogen gas is purged under reduced pressure through the homogenized resultant slurry under stirring till the temperature drops to 40 to 50 oC to obtain an emulsion. The reduced pressure is in the range of in the range of 300 to 650 mm/Hg.
Conditioner phase (Phase C) is added to the so obtained emulsion followed by addition of fragrance and coupler phase (Phase D) under stirring. The mixing is carried out under nitrogen purging and under reduced pressure in the range of 300 to 650 mm/Hg to obtain the cream based hair coloring composition. The homogenized liquid is at a reduced pressure in the range of 300 to 650 mm/Hg, to remove any trapped air bubbles, and obtain the cream based hair coloring composition.
The hair coloring composition is subjected to quality control and quality assurance tests to confirm that the finished product meets the desired standards.
The hair coloring composition is peroxide and ammonia free and hence is safe for use and is easy to apply. Further, the hair coloring composition is capable of developing the color in a short duration of time and retains the color even after repeated washing.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment, but, are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following laboratory scale experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. These laboratory scale experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial/commercial scale.
EXPERIMENTAL DETAILS
Experiment 1: Cream based hair coloring compositions (Examples 1 to 4) in accordance with process of the present disclosure:
The cream based hair coloring composition in accordance with the present disclosure was prepared by the following general process. The nourishing agent used in the present disclosure was a combination of Phyllanthus emblica extract from whole fruits, Eclipta prostrata extract from whole shrub, Hibiscus rosa-sinensis extract from whole flower, and Trigonella foenum-graecum extract from seeds, all of which were purchased from the local market in Gujarat, India. Xanthan gum, walnut oil and argan oil were imported from outside India. The quantities of the ingredients used in the preparation of the cream based hair coloring compositions are provided in Table 1.
Step-I: Preparation of Dye Phase (Phase-A)
In a clean stainless steel (SS) tank having 100 liter capacity and fitted with a mechanical stirrer, 50 kg hot water at ~83 ºC was added. Liquid sodium lauryl sulphate was added to the hot water under stirring, followed by the addition of EDTA. Sodium sulphite, iso-ascorbic acid/erythorbic acid and magnesium sulphate were then added. Next, dyes and couplers (Meta Amino Phenol, Para Amino Phenol, 2, 5 Diamino Toluene sulphate, Para-phenylenediamine, N,N Bis (2-Hydroxyethyl)-p- Phenylenediamine Sulfate and 2 ,4 -Diaminophenoxyethanol Dihydrochloride) were added under stirring followed by the addition of mono ethanol amine to obtain a slurry. The slurry was stirred for another 10 minutes till all the dye and coupler were dissolved. After the dye and the coupler were completely dissolved, Ayurprash (a combination of Amla, Bhringraj, Jaswand, and Methi extract) was added under stirring to obtain the Dye Phase.
Step-II: Preparation of Oil Phase (Phase-B)
Previously weighed oil phase ingredients, namely, Walnut oil, Argan oil, Cetostearyl alcohol, Cetearyl Alcohol (and) Dicetyl phosphate (and) Ceteth-10 phosphate, Glyceryl stearate, PEG 100 stearate, and Dimethicone were added to a clean SS tank having 100 liter capacity and fitted with a bottom nozzle, and heated to 68 to 70 °C, under stirring for uniform distribution of heat, to obtain a mixture. The same temperature was maintained when the oil phase ingredients were added to the SS tank.
Step-III: Preparation of Conditioner Phase (Phase C) (Polyquaternium-39 solution)
Previously weighed amount of Polyquaternium-39 was added to a clean SS tank having 10 liter capacity, followed by the addition of 2 kg water under stirring.
Step-IV: Preparation of Coupler Pahse (Phase-D) (1,2,4-trihydroxy benzene solution)
Previously weighed 1,2,4-trihydroxy benzene was added to a clean SS tank having 50 liter capacity fitter with a stirrer, under nitrogen atmosphere containing 25 kg water. The reaction mixture was stirred till 1,2,4-trihydroxy benzene was completely dissolved.
Step-V: Preparation of the cream based hair coloring composition
100 kg water maintained at 83 ºC was separately added to a planetary mixer. Xanthan gum was then added under stirring (Homogenize for 2-3 minutes), and stirred with anchor /shaft for 2-3 minutes to obtain a homogenous mixture. To the homogenous mixture Dye phase (Phase A) was added under stirring with anchor. This was followed by the incorporation of oil phase ( Phase B) maintained at 65 to 70 ºC to obtain a homogenous resultant slurry. The homogenous resultant slurry was stirred by rotating the anchor at 35 rpm for 2 minutes. The anchor was stopped and the reaction mixture was homogenized for 2 minutes. Nitrogen was flushed through homogenized mixture and the pressure reduced in the range of 300 to 650 mm/Hg. After nitrogen was completely flushed, the valve of the mixer was closed and the stirring under reduced pressure was continued for 10 minutes to obtain an emulsion.
The mixer was cooled by passing cold water in the jacket and stirring at 35 rpm. After 10 minutes chilled water was passed through the jacket with continuous stirring. If a drop in reduced pressure (vacuum) was observed, the vacuum pump was switched on till the desired reduced pressure (vacuum) was obtained. The speed of rotation was slowly decreased to 25 rpm to avoid air entrapment and to ensure that the emulsion was homogeneously mixed.
When the temperature of the emulsion dropped to 45 ºC or below, the vacuum was released by purging nitrogen and conditioner phase (Phase C) (Polyquaternium-39 solution) was added, followed by stirring for 2 - 3 minutes. The fragrance was slowly added under stirring, followed by stirring for 2-3 minutes. This was followed by the addition of coupler phase (Phase-D) (1, 2, 4 -Trihydroxy benzene solution). The reaction mass was stirred for 15 minutes with circulation of the bulk. Stirring was continued for another 15 minutes, under reduced pressure in the range of 300 to 650 mm/Hg, to ensure complete homogenization and obtain the cream based hair coloring composition of the present disclosure.
After analysis of the sample by QA/QC, the cream based hair coloring composition was released and filled in appropriate container (Lami tube Aluminium collapsible tube, laminate pouches depending on the requirement and market order.). The tank containing the bulk (cream based hair coloring composition) was continuously flushed with nitrogen.
The filling was carried out by transferring the bulk (cream based hair coloring composition) to a machine filling hopper. Nitrogen was continuously flushed in hopper to avoid oxidation. During filling, care was taken to flush the tubes/pouch with nitrogen prior to filing the cream based hair coloring composition. After filing the tubes/pouches were flushed with nitrogen, sealed, and stored till further use.
Table-1: Components of the hair colouring compositions of the present disclosure for providing natural black shade or black brown shade and their quantities:
S. No. Ingredients Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8
Quantity (% w/w)
Thickening agent
1 Cetostearyl alcohol 4.5 4.5 4.5 4.5 5.25 5 5.2 5.5
2 Xanthan gum 0.5 0.5 0.5 0.5 0.5 0.4 0.5 0.6
Emulsifier
3 Cetearyl Alcohol (and) Dicetyl phosphate (and) Ceteth-10 phosphate 2.5 2.5 2.5 2.5 2.75 2.5 2.75 2.95
4 Glyceryl stearate & Peg 100 stearate 2 2 2 2 2 2.5 2.75 2.95
Conditioning agent
5 Dimethicone 0.25 0.25 0.25 0.25 0.05 0.05 0.05 0.05
6 Polyquaternium-39 2 2 2 2 0.5 0.25 0.5 0.5
Surfactant
7 Sodium lauryl sulphate 2 2 2 2 2 1.5 2 2.5
Chelating agent
8 EDTA (plain) 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1
Antioxidant
9 Sodium sulphite 0.023 0.023 0.023 0.023 0.045 0.035 0.045 0.055
10 Iso-ascorbic acid (erythorbic acid) 0.138 0.138 0.17 0.138 0.35 0.25 0.35 0.4
Stabilizer
11 Magnesium Sulphate 0.138 0.138 0.25 0.138 0.75 0.5 0.75 0.9
Coloring Agent (Dye)
12 Para-phenylenediamine 0.69 0.966 1.38 1.725 1.5 0.9 1.2 1.35
13 2, 5 Diamino Toluene sulphate 0.92 1.29 1.84 2.30 2 1.25 1.65 1.8
Coupling Agent (Coupler)
14 2 ,4 -Diaminophenoxyethanol Dihydrochloride 0.184 0.257 0.368 0.46 0.34 0.25 0.325 0.4
15 Meta Amino Phenol 0.138 0.192 0.27 0.1725 0.28 0.35 0.45 0.5
16 N,N Bis (2-Hydroxyethyl)-p- Phenylenediamine Sulfate 0.092 0.129 0.185 0.23 0.2 0.12 0.16 0.2
17 Para Amino Phenol 0.069 0.096 0.14 0.1725 0.17 0.2 0.3 0.37
18 1, 2, 4 -Trihydroxy benzene 1.15 1.61 2.3 2.875 2.5 1.5 1.9 2.3
Alkalizer
19 Mono ethanol amine 1.38 1.40 1.6 3.45 3.25 2.5 3.5 3.5
Fragrance (Odor)
20 Fragrance 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5
Nourishment
21 Walnut oil 0.2 0.2 0.2 0.2 0.1 0.1 0.1 0.1
22 Argan oil 0.1 0.1 0.1 0.1 0.05 0.05 0.05 0.05
23 Ayurprash (a combination of Amla , Bhringraj , Jaswand & Methi extract) 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Solvent
24 Water QS QS QS QS QS QS QS QS
pH of the composition 9.1 9.2 9.4 9.9 9.7 9.5 9.8 9.8

The cream based hair coloring compositions for dyeing the hair in natural black shade or black brown shade, are obtained in the form of slightly viscous cream, having a pH (at 27 °C) in the range of 8.0 to 10.0, and having a pleasant and characteristic odor. Examples 1-5 provide natural black shade, while Examples 6-8 provide black brown shade. The para-phenylene diamine content in the cream based hair coloring composition of the present disclosure is not more than 4 % w/w.
Experiment 2: Study for retention of the color of the cream based hair coloring composition of the present disclosure
The cream based hair coloring compositions (Examples 1-8) of the present disclosure were tested on natural black and white hair tresses to evaluate the retention property of the colour. The cream based hair coloring compositions were applied on 5 different samples (Tresses 1 to 5) of hair, each containing 70-80 strands of mixed hair, and the result is summarized in Table 2.
Table 2: Evaluation of hair coloring composition of Example-1 for retention of the color on hair
Example No.
Sr. No. for Tresses 1st application –development time - 30 minutes After 5 wash
After 10 wash After 15 wash After 20 wash
1 1-5. Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black After 24 hrs the shade was Deeper
On grey hair soft black to darkest brown shade (gradual fading) On grey hair darkest brown shade (fading) On grey hair dark brown shade (fading) On grey hair Light brown shade (fading)
2 1-5 Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black After 24 hrs the shade was Deeper
On grey hair soft black to darkest brown shade (gradual fading) On grey hair darkest brown shade (fading) On grey hair dark brown shade (fading) On grey hair Light brown shade (fading)
3 1-5 Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black After 24 hrs the shade was Deeper
On grey hair black shade On grey hair soft black shade On grey hair soft black to darkest brown shade (gradual fading) On grey hair darkest brown shade (gradual fading)
4 1-5 Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black After 24 hrs the shade was Deeper On grey hair black shade On grey hair soft black to darkest brown shade (gradual fading) On grey hair soft black to darkest brown shade (gradual fading) On grey hair darkest brown shade (gradual fading)
5 1-5 Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black After 24 hrs the shade was Deeper On grey hair black shade On grey hair soft black shade On grey hair soft black to darkest brown shade (gradual fading) On grey hair darkest brown shade (gradual fading)
6 1-5 Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black brown After 24 hrs the shade was Deeper On grey hair black – brown shade On grey hair Dark brown shade (gradual fading ) On grey hair brown shade (fading) On grey hair light brown shade (fading)
7 1-5. Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black brown After 24 hrs the shade was Deeper On grey hair black – brown shade On grey hair Darkest brown shade On grey hair Dark brown shade (gradual fading) On grey hair brown shade (fading)
8 1-5. Natural Black & white hair tresses ( approx. gray hair up to 60 %) On grey hair natural black brown After 24 hrs the shade was Deeper On grey hair black – brown shade On grey hair Darkest brown shade On grey hair Dark brown shade (gradual fading) On grey hair brown shade (fading)

It is seen from Table-2, Example 1, that a color of the light brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 2, that a color of the light brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 3, that a color of the darkest brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 4, that a color of the darkest brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 5, that a color of the darkest brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 6, that a color of the light brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 7, that a color of the brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
It is seen from Table-2, Example 8, that a color of the brown shade is retained even after 20 washings, when the cream based hair coloring composition of the present disclosure is used.
Experiment 3: Study of color development using the cream based hair coloring composition of the present disclosure
Studies were carried to determine the color development efficacy of the cream based hair coloring compositions of the present disclosure by testing the composition on the hair of the volunteers. Volunteers in the age group of 21 to 75 years having grey hair were chosen for the study. Volunteers with scalp, skin diseases, or cut on head were not selected for the study. Prior to starting the study, details of the selected volunteers were noted down, such as natural hair color, approximate percent of grey hair, length of hair from root, and hair washing habits of the volunteers. During color /dye application and after hair wash, the feedback from the volunteer is taken and the volunteer is regularly observed for a period of 1 month. The stability of color /dye on hair is judged by visual observation. 16 volunteers (8 males (M1 to M8) and 8 females (F1 to F8)) were selected who had above 50 % grey hair and minimum 1 inch visible grey hair re-growth. All the volunteers were regular users of hair dye and had not applied hair dye /color for an average of 45 days before initiating the study. The color development efficacy of the cream based hair coloring compositions of the present disclosure (compositions of Examples 2 and 4) was determined and the results are summarized in Tables 3-6.
Composition obtained in Example 2, was applied to the hair of male volunteers using a brush and the color was allowed to develop for 30 minutes. The hair was washed with shampoo and water after 30 minutes, towel dried and finally dried with hair blow dryer. The results are presented in Table-3.
Table 3: Evaluation of longetivity of the hair coloring composition of Example-2 in male volunteers
Results on grey hair and overall shade produce in 1st application After 24 hrs
(2nd day) After 7 days After 14 days After 21 days After 28 days
Volunteer M-1
On grey hair soft black shade , overall soft black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.
Volunteer M-2
On grey hair soft black shade , overall soft black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black . Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.
Volunteer M-3
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer M-4
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer M-5
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black. Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer M-6
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black. Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer M-7
On grey hair soft black shade , overall soft black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade . No fadage observed, the shade on hair was natural black. Slight fadage observed, the shade on hair was soft black. Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.
Volunteer M-8
On grey hair soft black shade , overall soft black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade . No fadage observed, the shade on hair was natural black . Slight fadage observed, the shade on hair was soft black. Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.

Composition obtained in Example 2, was applied to the hair of female volunteers using a brush and the color was allowed to develop for 30 minutes. The hair was washed with shampoo and water after 30 minutes, towel dried and finally dried with hair blow dryer. The results are presented in Table-4.
Table 4: Evaluation of longetivity of the hair coloring composition of Example-2 in female volunteers
Results on grey hair and overall shade produce in 1st application. After 24 hrs
(2nd day) After 7 days After 14 days After 21 days After 28 days
Volunteer F-1
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-2
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-3
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-4
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-5
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-6
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-7
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-8
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened / darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.

Summary of Volunteer trails carried out
The volunteers were recalled on 2nd day, 7 day, 14 day, 21st day & 28 day and observed. The observation was as follows.
Male volunteer no M1 to M8 :-
? The immediate shade obtained on grey hair is soft black which darken /deepens on 2nd day and turn to natural black. The grey coverage is 100 % for 8 volunteers.
? After 7 days no fadage observed for all 8 volunteers and the shade on grey hair was natural black
? After 14 days slight fadage observed for all volunteers . For 4 volunteers M1, M2, M7 & M8 the shade on grey hair faded to soft black and other 4 volunteers M3, M4, M5 & M6 the shade faded between black and soft black.
? After 21 days gradual fadage observed for all volunteers. For 4 volunteers M1, M2, M7 & M8 the shade on grey hair faded from soft black to darkest brown and other 4 volunteers M3, M4, M5 & M6 the shade faded to soft black.
? After 28 days gradual fadage observed for all volunteers. For 4 volunteers M1, M2, M7 & M8 the shade on grey hair faded from darkest brown to dark brown and other 4 volunteers M3, M4, M5 & M6 the shade faded from soft black to darkest brown.
Female volunteer no F1 to F8 :-
? The immediate shade obtained on grey hair is soft black which darken /deepens on 2nd day and turn to natural black. The grey coverage is 100 % for 8 volunteers .
? After 7 days no fadage observed for all 8 volunteers and the shade on grey hair was natural black
? After 14 days slight fadage observed for all volunteers. For all 8 volunteers F1 to F8 the shade faded between black and soft black.
? After 21 days gradual fadage observed for all volunteers . For all 8 volunteers F1 to F8 shade faded to soft black.
? After 28 days gradual fadage observed for all volunteers. For all 8 volunteers F1 to F8 the shade faded from soft black to darkest brown.

Conclusion:
? The hair colouring composition of the Example 2, of the present disclosure imparts black shade on gray hair in 30 minutes with 100 % grey coverage .
? The longetivity of hair colouring composition of the Example 2, of the present disclosure is up to 28 days with gradual fading .
Composition obtained in Example 4, was applied to the hair of male volunteers using a brush and the color was allowed to develop for 30 minutes. The hair was washed with shampoo and water after 30 minutes, towel dried and finally dried with hair blow dryer. The results are presented in Table-5.
Table 5: Evaluation of longetivity of the hair coloring composition of Example-4 in male volunteers
Results on grey hair and overall shade produce in 1st application. After 24 hrs
(2nd day) After 7 days After 14 days After 21 days After 28 days
Volunteer M-1
On grey hair soft black shade , overall soft black with 100 % coverage The black shade has deepened/darkened, overall natural black shade No fadage observed, the shade on hair was natural black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown fadage observed, the shade on hair was more towards dark brown
Volunteer M-2
On grey hair soft black shade , overall soft black with 100 % coverage The black shade has deepened/darkened, overall natural black shade No fadage observed, the shade on hair was natural black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown fadage observed, the shade on hair was more towards dark brown
Volunteer M-3
On grey hair soft black shade , overall black with 100 % coverage The black shade has deepened/darkened, overall natural black shade No fadage observed, the shade on hair was natural black No fadage observed, the shade on hair was between black to soft black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown
Volunteer M-4
On grey hair soft black shade , overall black with 100 % coverage The black shade has deepened/darkened, overall natural black shade No fadage observed, the shade on hair was natural black No fadage observed, the shade on hair was between black to soft black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown
Volunteer M-5
On grey hair soft black shade , overall black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer M-6
On grey hair soft black shade , overall black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer M-7
On grey hair soft black shade , overall soft black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black . Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.
Volunteer M-8
On grey hair soft black shade , overall soft black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black . Slight fadage observed, the shade on hair was soft black. Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.

Composition obtained in Example 4, was applied to the hair of female volunteers using a brush and the color was allowed to develop for 30 minutes. The hair was washed with shampoo and water after 30 minutes, towel dried and finally dried with hair blow dryer. The results are presented in Table-6.
Table 6: Evaluation of longetivity of the hair coloring composition of Example-4 in female volunteers
Results on grey hair and overall shade produce in 1st application. After 24 hrs
(2nd day) After 7 days After 14 days After 21 days After 28 days
Volunteer F-1
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened/darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-2
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened/darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-3
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened/darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-4
On grey hair soft black shade , overall black with 100 % coverage. The black shade has deepened/darkened, overall natural black shade. No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black. Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-5
On grey hair soft black shade , overall black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.

Volunteer F-6
On grey hair soft black shade , overall black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black. No fadage observed, the shade on hair was between black to soft black Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown.
Volunteer F-7
On grey hair soft black shade , overall soft black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black . Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.
Volunteer F-8
On grey hair soft black shade , overall soft black with 100 % coverage . The black shade has deepened/darkened, overall natural black shade . No fadage observed, the shade on hair was natural black . Slight fadage observed, the shade on hair was soft black Slight fadage observed, the shade on hair was more towards darkest brown. fadage observed, the shade on hair was more towards dark brown.

The volunteers were recalled on 7th day, 14th day, 21st day, & 28th day and the hair color was observed. The observations were as follows.

Male Volunteer M1 to M8 :-
• The immediate shade obtained on grey hair was soft black which darken /deepens on 2nd day and turned to natural black. The grey coverage is 100 % for all the 8 volunteers.
• After 7 days no fadage was observed for all 8 volunteers and the shade on grey hair was natural black.
• After 14 days slight fadage was observed for all volunteers. For 4 volunteers M1, M2, M7 and M8 the shade on grey hair faded to soft black and other 4 volunteers M3, M4, M5 and M6 the shade faded between black and soft black.
• After 21 days gradual fadage was observed for all volunteers. For 4 volunteers M1, M2, M7 and M8 the shade on grey hair faded from soft black to darkest brown and other 4 volunteers M3, M4, M5 and M6 the shade faded to soft black .
• After 28 days gradual fadage was observed for all volunteers. For 4 volunteers M1, M2, M7 and M8 the shade on grey hair faded from darkest brown to dark brown and other 4 volunteers M3, M4, M5 and M6 the shade faded from soft black to darkest brown.
Female volunteer no F1 to F8 :-
? The immediate shade obtained on grey hair is soft black, which darkens /deepens on 2nd day and turns to natural black. The grey coverage is 100 % for 8 volunteers.
? After 7 days no fadage observed for all 8 volunteers and the shade on grey hair was natural black.
? After 14 days slight fadage observed for all volunteers. For 6 volunteers F1 to F6 shade faded between black and soft black, and for the other 2 volunteers F7 and F8, the shade faded to soft black.
? After 21 days gradual fadage observed for all volunteers. For 6 volunteers F1 to F6 shade faded to soft black, and for the other 2 volunteers F7 and F8, the shade faded from soft black to darkest brown.
? After 28 days gradual fadage observed for all volunteers. For 6 volunteers F1 to F6 shade faded to darkest brown , and for the other 2 volunteers F7 and F8, the shade faded to dark brown.
Conclusion:
? The hair colouring composition of the Example 4, of the present disclosure imparts black shade on gray hair in 30 minutes with 100 % grey coverage.
? The longetivity of hair colouring composition of the Example 4, of the present disclosure is up to 28 days with gradual fading.
Composition obtained in Example 6, was applied to the hair of male volunteers using a brush and the color was allowed to develop for 30 minutes. The hair was washed with shampoo and water after 30 minutes, towel dried and finally dried with hair blow dryer. The results are presented in Table-7.

Table 7: Evaluation of longetivity of the hair coloring composition of Example-6 in male volunteers
Results on grey hair and overall shade produce in 1st application. After 24 hrs
(2nd day) After 7 days After 14 days After 21 days After 28 days
Volunteer M-1
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-2
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-3
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-4
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-5
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-6
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-7
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Volunteer M-8
On grey hair natural black brown with 100 % coverage The black brown shade has deepened/darkened, overall natural black brown shade . Visually no fadage observed, the shade on hair was black brown . Gradual fadage observed, the shade on hair was dark brown. Gradual fadage observed, the shade on hair was dark brown to light brown. fadage observed, the shade on hair was more towards Light brown.
Summary of Volunteer trails carried out
The volunteers were recalled on 2nd day, 7 day, 14 day, 21st day & 28 day and observed. The observation was as follows.
Male volunteer no M1 to M8 :-
? The immediate shade obtained on grey hair is soft black - brown which darken /deepens on 2nd day and turn to blackish brown . The grey coverage is 100 % for 8 volunteers .
? After 7 days no fadage observed for all 8 volunteers and the shade on grey hair was Black brown
? After 14 days slight fadage observed for all volunteers . For all 8 volunteers M1- M8 the shade on grey hair faded to soft black to dark brown
? After 21 days gradual fadage observed for all volunteers. For all 8 volunteers M1- M8 the shade on grey hair faded to soft black to dark brown
? After 28 days fadage observed for all volunteers. For all 8 volunteers M1- M8 the shade on grey hair faded to Light brown
Conclusion:
? The hair colouring composition of the Example 6, of the present disclosure imparts black brown shade on gray hair in 30 minutes with 100 % grey coverage .
? The longetivity of hair colouring composition of the Example 6, of the present disclosure cream is up to 28 days with gradual fading .

TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of a hair coloring composition that is free of peroxide and ammonia, and is capable of rapid color development. The hair coloring composition of the present disclosure is safe and also provides nourishment to the hair and aids in its healthy growth.
The embodiments as described herein above, and various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising”, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results.
The foregoing description of specific embodiments so fully reveal the general nature of the embodiments herein, that others can, by applying current knowledge, readily modify and/or adapt for various applications of such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein. Further, it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
Having described and illustrated the principles of the present disclosure with reference to the described embodiments, it will be recognized that the described embodiments can be modified in arrangement and detail without departing from the scope of such principles.
While considerable emphasis has been placed herein on the particular features of this disclosure, it will be appreciated that various modifications can be made, and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other modifications in the nature of the disclosure or the preferred embodiments will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
,CLAIMS:WE CLAIM :

1. A hair coloring composition comprising:
a) para-phenylenediamine and 2,5-diaminotoluenesulphate as colouring agents, in an amount in the range of 1.6 to 4.1 mass%;
b) meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene as coupling agents, in an amount in the range of 1.6 to 4.0 mass%;
c) iso-ascorbic acid and sodium sulphate as antioxidants, in an amount in the range of 0.16 to 0.75 mass%;
d) a surfactant, in an amount in the range of 1.5 to 2.5 mass%;
e) ethylene diamine tetra acetate (EDTA) as chelating agent, in an amount in the range of 0.09 to 0.11 mass%;
f) monoethanol amine as alkalizer, in an amount in the range of 1.35 to 6.0 mass%;
g) magnesium sulphate as stabilizer, in an amount in the range of 0.13 to 0.9 mass%;
h) at least one nourishing agent selected from the group consisting of Phyllanthus emblica extract, Eclipta prostrata extract, Hibiscus rosa-sinensis extract, Trigonella foenum-graecum extract, walnut oil and argan oil, in an amount in the range of 0.05 to 0.5 mass%; and
i) additives selected from the group consisting of a fluid medium, emulsifiers, a fragrance, a conditioning agent and thickening agents;
wherein the mass% of each of the component is with respect to the total mass of the composition.
2. The composition as claimed in claim 1, wherein the mass ratio of para-phenylenediamine and 2,5-diaminotoluenesulphate is in the range of 0.7:1 to 0.8:1.
3. The composition as claimed in claim 1, wherein the mass ratio of 2,4-diaminophenoxyethanol dihydrochloride to 2,5-diaminotoluene sulphate is in the range of 0.1:1 to 0.3:1, the mass ratio of meta-aminophenol to para-phenylenediamine is in the range of 0.1:1 to 0.4:1, the mass ratio of N,N-Bis-(2-Hydroxyethyl)-p-phenylenediamine sulfate to 2,5-diaminotoluene sulphate is in the range of 0.096:1 to 0.11:1, the mass ratio of para-aminophenol to para-phenylenediamine is in the range of 0.1:1 to 0.27:1, and the mass ratio of para-phenylenediamine to 1,2,4-Trihydroxy benzene is in the range of 0.5:1 to 0.7:1.
4. The composition as claimed in claim 1, wherein the mass ratio of iso-ascorbic acid and sodium sulphate is in the range of 6:1 to 7.78:1.
5. The composition as claimed in claim 1, wherein said surfactant is selected from the group consisting of sodium lauryl sulphate, coco amido propyl betaine, coco diethanolamide and sodium sarcosinate.
6. The composition as claimed in claim 1, wherein said fluid medium is water, in an amount in range of 25 to 90 mass%;
7. The composition as claimed in claim 1, wherein said emulsifiers are glyceryl stearate, polyethylene glycol ester of stearic acid (PEG 100 stearate), cetearyl alcohol, dicetyl phosphate and ceteth-10 phosphate, in an amount in the range of 4.0 to 7.0 mass%.
8. The composition as claimed in claim 1, wherein said conditioning agents are dimethicone and polyquarernium-39, in an amount in the range of 0.3 to 2.5 mass%;
9. The composition as claimed in claim 1, wherein said thickening agents are xanthan gum and cetostearyl alcohol, in an amount in the range of 4.0 to 7.0 mass%;
10. The composition as claimed in claim 1, comprising:
a) 4.025 mass% of para-phenylenediamine and 2,5-diaminotoluenesulphate as coloring agents;
b) 3.91 mass% of meta-aminophenol, 2,4-diaminophenoxyethanol dihydrochloride, para-aminophenol, N,N-Bis-(2-hydroxyethyl)-p-phenylenediamine sulfate and 1,2,4-trihydroxybenzene as coupling agents;
c) 0.161 mass% of iso-ascorbic acid and sodium sulphate as antioxidants;
d) 2 mass% of sodium lauryl sulphate as surfactant;
e) 0.1 mass% of ethylene diamine tetra acetate (EDTA) as chelating agent;
f) 3.45 mass% of monoethanol amine as alkalizer;
g) 0.138 mass% of magnesium sulphate as stabilizer;
h) 0.5 mass% of at least one nourishing agents selected from the group consisting of Amla Extract (Phyllanthus emblica), Bhringraj extract (Eclipta prostrata), Jaswand extract (Hibiscus rosa-sinensis) and Methi extract (Trigonella foenum-graecum), walnut oil and argan oil; and
i) Additives;
wherein the mass% of each of the component is with respect to the total mass of the composition.
11. The composition as claimed in claim 10, wherein said additives comprise:
i. 73.466 mass % of water as fluid medium;
ii. 4.5 mass% of emulsifiers;
iii. 0.5 mass% of a fragrance;
iv. 2.25 mass% of dimethicone and polyquaternium as conditioning agents; and
v. 5 mass % of xanthan gum and cetostearyl alcohol as thickening agents;
wherein the mass% of each of the component is with respect to the total mass of the composition.
12. The composition as claimed in claim 1, comprising:
a) 1.725 mass% of para-phenylenediamine and 2.3 mass% of 2,5-diamino toluene sulphate, as coloring agents;
b) 0.46 mass% of 2 ,4 -diaminophenoxyethanol dihydrochloride, 0.1725 mass% of meta-aminophenol, 0.23 mass% of N,N-Bis-(2-Hydroxyethyl)-p- phenylenediamine sulfate, 0.1725 mass% of para-aminophenol and 2.875 mass% of 1,2,4-trihydroxybenzene, as coupling agents;
c) 0.023 mass% of sodium sulphite and 0.138 mass% of iso-ascorbic acid (erythorbic acid), as antioxidants;
d) 2 mass% of sodium lauryl sulphate as surfactant;
e) 0.1 mass% of ethylene diamine tetra-acetic acid (EDTA) as chelating agent;
f) 3.45 mass% of mono-ethanolamine as alkalizer;
g) 0.138 mass% of magnesium sulphate as stabilizer;
h) 0.2 mass% of Amla extract (Phyllanthus emblica), Bhringraj extract (Eclipta prostrata), Jaswand extract (Hibiscus rosa-sinensis) and Methi extract (Trigonella foenum-graecum), 0.2 mass% walnut oil and 0.1 mass% argan oil, as nourishing agents; and
i) Additives;
wherein the mass% of each of the component is with respect to the total mass of the composition.
13. The composition as claimed in claim 12, wherein said additives comprise:
i. 73.466 mass % of water;
ii. 2.5 mass% of a combination of cetearyl alcohol, dicetyl phosphate and ceteth-10 phosphate, and 2.0 mass% of a combination of glyceryl stearate and polyethylene glycol ester of stearic acid (PEG 100 stearate), as emulsifiers;
iii. 0.5 mass% of a fragrance;
iv. 0.25 mass% of dimethicone and 2.0 mass% of polyquaternium-39, as conditioning agents; and
v. 4.5 mass % of cetostearyl alcohol and 0.5 mass% of xanthan gum as thickening agents;
14. A process for the preparation of a hair colouring composition as claimed in claim 1, said process comprising the following steps:
a) preparing a dye phase:
i) mixing a surfactant with water at a temperature in the range of 80 oC to 85 oC, followed by adding a chelating agent, at least one antioxidant, a stabilizer, at least one colouring agent, at least one coupling agent and an alkalizer to obtain a slurry; and
ii) adding at least one nourishing agent to said slurry under stirring to obtain a dye phase;
b) preparing an oil phase:
i) mixing at least one nourishing agent, at least one thickening agent, at least one emulsifier and at least one conditioning agent, followed by heating to a temperature in the range of 60 oC to 75 oC under stirring to obtain an oil phase;
c) preparing a conditioner phase:
i) dissolving at least one conditioning agent in water to obtain a conditioner phase;
d) preparing a coupler phase:
i) dissolving at least one coupling agent in water to obtain coupler phase;
e) preparing a colouring composition:
i) mixing at least one thickening agent and water under stirring, at a temperature in the range of 80 oC to 85 oC to obtain a homogenous phase;
ii) mixing said homogenous phase with said dye phase under stirring, followed by the addition of said oil phase, at a temperature in the range of 65 oC to 75 oC to obtain homogenized slurry;
iii) purging said homogenized slurry with nitrogen gas and subjecting the purged slurry to reduced pressure in the range of 300 to 650 mm/Hg until the slurry cools to a temperature in the range of 40 to 50 oC to obtain an emulsion; and
iv) adding said conditioner phase to said emulsion under nitrogen atmosphere and under stirring, followed by adding a fragrance and said coupler phase, and subjecting the mixture to reduced pressure in the range of 300 to 650 mm/H to obtain the hair coloring composition.

15. The process as claimed in claim 14, wherein in the step (b), of preparing an oil phase, the ratio of nourishing agent: thickening agent: emulsifier is in the range of 1:15:15.

Documents

Application Documents

# Name Date
1 201821020909-STATEMENT OF UNDERTAKING (FORM 3) [05-06-2018(online)].pdf 2018-06-05
2 201821020909-PROVISIONAL SPECIFICATION [05-06-2018(online)].pdf 2018-06-05
3 201821020909-PROOF OF RIGHT [05-06-2018(online)].pdf 2018-06-05
4 201821020909-FORM 1 [05-06-2018(online)].pdf 2018-06-05
5 201821020909-DECLARATION OF INVENTORSHIP (FORM 5) [05-06-2018(online)].pdf 2018-06-05
6 201821020909-FORM-26 [06-06-2018(online)].pdf 2018-06-06
7 201821020909-Proof of Right (MANDATORY) [13-06-2018(online)].pdf 2018-06-13
8 201821020909-OTHERS(ORIGINAL UR 6( 1A) FORM 1)-140618.pdf 2018-09-26
9 201821020909-ENDORSEMENT BY INVENTORS [30-05-2019(online)].pdf 2019-05-30
10 201821020909-COMPLETE SPECIFICATION [30-05-2019(online)].pdf 2019-05-30