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Hair Coloring Composition And A Process For Its Preparation

Abstract: The present disclosure relates to a hair coloring composition that is free of peroxide and ammonia, and is capable of rapid colour development on hair. The composition comprises a fluid medium, a thickening agent, a humectant, a chelating agent, an antioxidant, a coloring agent, a coupler, a fragrance, a conditioning agent, and a pH adjusting agent, in a pre-determined proportion with each other. The hair coloring composition is safe and non-toxic to use and provides a faster rate of colour development in comparison to known hair colour compositions.

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Notices, Deadlines & Correspondence

Patent Information

Application #
Filing Date
04 October 2019
Publication Number
35/2022
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
dewan@rkdewanmail.com
Parent Application
Patent Number
Legal Status
Grant Date
2025-09-09
Renewal Date

Applicants

HYGIENIC RESEARCH INSTITUTE PRIVATE LIMITED
602, Supreme Chambers, Off. Veera Desai Road, Andheri (West), Mumbai - 400 053, Mumbai, Maharashtra, India

Inventors

1. PAWAR, Ajit Mansingh
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) Pin code -421201, India
3. RAI Sadananda
Kausthubha Bolwar Puttur D.K. Karnataka 574201, India

Specification

Claims:
WE CLAIM:
1. A hair colouring composition comprising:
a) a coloring agent in the range of 1.2 mass% to 11 mass% of said composition;
b) at least one humectant in the range of 1.5 mass% to 5.5 mass% of said composition;
c) a coupler in the range of 0.25 mass% to 6.25 mass% of said composition;
d) at least one chelating agent in the range of 0.025 mass% to 0.3 mass% of said composition;
e) an antioxidant in the range of 0.25 mass% to 1.25 mass% of said composition;
f) a thickening agent in the range of 0.525 mass% to 8.5 mass% of said composition;
g) at least one catalyst in the range of 0.25 mass% to 2.0 mass% of said composition;
h) at least one fragnance in the range of 0.4 mass% to 1.75 mass% of said composition;
i) at least one conditioning agent in the range of 0.25 mass% to 5.0 mass% of said composition;
j) at least one pH adjusting agent in the range of 0.75 mass% to 5.0 mass% of said composition; and
k) a fluid medium in an amount sufficient to make 100 mass% of the composition.

2. The hair colouring composition as claimed in claim 1, wherein,
a) said colouring agent is a combination of para-phenylenediamine, N,N-bis(2-hydroxyethyly)-p-phenylenediamesulphate and para aminophenol;
b) said humectant is selected from the group consisting of propylene glycol, ethylene glycol, glycerol, butylene glycol, and sorbitol;
c) said coupler is selected from 2,4-diaminophenoxyethanol dihydrochloride, meta aminophenol and 1,2,4-trihydroxy benzene;
d) said chelating agent is selected from the group consisting of disodium ethylene diamine tetra acetate (EDTA), tetrasodium EDTA, trisodium citrate, and etidronic acid;
e) said antioxidant is selected from the group consisting of sodium sulphite, ascorbic acid, vitamin K, vitamin E, tocopherol acetate, butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), ascorbyl palmitate, citric acid, propyl gallate, methionine and sodium metabisulfite;
f) said catalyst is magnesium sulphate;
g) said thickening agent is selected from the group consisting of xanthan gum, gelatin,sodium alginate, hydroxyethyl cellulose, and sodium carboxy methyl cellulose;
h) at least one fragrance;
i) said conditioning agent is a mixture of amodimethicone and C-12-14 sec Pareth-7;
j) said pH adjusting agent is selected from the group consisting of monoethanolamine, triethanolamine, diethanolamine potassium hydroxide, and sodium hydroxide; and
k) said fluid medium is demineralized water.

3. The hair colouring composition as claimed in any of the preceding claims, wherein said composition comprises:
a) para-phenylenediamine in the range of 0.7mass% to 3.9mass% of said composition, N, N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate in the range of 0.05 mass% to 1.25 mass% and para amino phenol in the range of 0.025 mass% to 1.0 mass%;
b) propylene glycol in the range of 1.5 mass% to 5.5 mass% of said composition;
c) 2,4-diaminophenoxyethanol dihydrochloride in the range of 0.1 mass% to 2.0 mass% of said composition, meta amino phenol in the range of 0.1 mass% to 1.25 mass% and 1,2,4-Trihydroxy benzene in the range of 0.7 mass% to 3.0 mass%;
d) disodium ethylene diamine tetra acetate (EDTA) in the range of 0.025 mass% to 0.35mass% of said composition;
e) sodium sulphite in the range of 0.025 mass% to 0.35 mass% of said composition; iso ascorbic acid or erythorbic acid in the range of 0.1 mass% to 0.90 mass% of said composition;
f) magnesium sulphate in the range of 0.25 mass% to 2.0 mass%;
g) sodium alginate in the range of 2.0 to 6.0 mass% or hydroxyl ethyl cellulose in the range of 0.5 to 5.0 mass% and sodium carboxy methyl cellulose in the range of 0.025 mass% to 0.50 mass% of said composition;
h) said fragrance in the range of 0.4 mass% to 1.75 mass% of said composition;
i) amodimethicone and C-12-14 sec Pareth-7 in the range of 0.25 mass% to 5.0 mass% of said composition;
j) monoethanolamine in the range of 0.75 mass% to 5.0 mass% of said composition; and
k) demineralized water in an amount sufficient to make 100 mass% of the composition of said composition.
4. The hair colouring composition as claimed in claim 1, wherein the pH of said composition is in the range of 7 to 10.

5. A process for preparing a hair colouring composition as claimed in claim 1, wherein said process comprises the following steps:
a) adding a thickening agent to a fluid medium under stirring to obtain a slurry;
b) separately adding at least one humectant, at least one chelating agent, an antioxidant and a coloring agent to a fluid medium to obtain a dye phase;
c) adding a fragrance, a conditioning agent and a pH adjusting agent to said dye phase under stirring;
d) mixing said dye phase with said slurry followed by purging of nitrogen gas and stirring to obtain a homogenized mass;
e) adding a solution of a coupling agent to said homogenized mass to obtain a resultant mixture;
f) recirculating said resultant mixture to obtain a homogenized liquid; and
g) applying vacuum pressure to said homogenized liquid to obtain said hair colouring composition.

6. The process as claimed in claim 5, wherein said vacuum pressure is applied to said mixture of dye phase and slurry in the range of 200 kg/cm2 to 500 kg/cm2 to remove any trapped air bubbles to form a homogenized mass
, Description:

FIELD
The present disclosure relates to a hair coloring composition and a process for its preparation.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Hair coloring, or hair dyeing, is the practice of changing the hair color. The main reasons for changing the hair color are to cover gray or white hair, to change to a color regarded as more fashionable or desirable, to restore the original hair color after it has been discolored by hairdressing processes or sun bleaching. The use of coloring matters on human hair is well known. Hair dyeing with plants is a multicultural art practiced since ancient times. The discovery of synthetic dyes in the 19th century began to change the technology of the coloring of hair. The early processes were based on the oxidation of p-phenyl-enediamine. Commercially, ‘oxidation dyes’ are the most important class of hair colorant and provide the only satisfactory means for permanent dyeing. There are four basic ingredients, namely, ammonia, hydrogen peroxide, lauryl sulfate and alcohol that are mainly used in the hair dye.
Conventional hair dyes containing a plant extract or an organic compound typically require a long hair dyeing time. Further, the hair dyeing property and color development are not satisfactory. Still further, the color of the conventional hair dye tends to fade on exposure to sunlight.
Ammonia and hydrogen peroxide used as integral ingredients in hair colors are capable of retaining the hair color for a long duration. Without these chemicals, hair color will fade off after a few washing with shampoo. Ammonia and hydrogen peroxide are usually included only in permanent hair dyes.
However, hydrogen peroxide, if used in large quantities has a corrosive effect, has harmful side effects on the nervous system, the digestive system, and the respiratory organs. It can cause damage to the DNA and is suggested to be cancerous. Further, the use of ammonia in the hair dye composition has many disadvantages, such as hair becomes rough and brittle with a tendency to tangle easily, formation of split ends, weakening of hair, hair breakage, and hair loss. It is also suggested that ammonia causes skin allergies, irritation of the eyes, itching in the scalp, and unexplained coughing. Due to the aforestated reasons, the conventional hair dyes cannot be used by people who are sensitive to chemicals, have life-threatening illnesses, and are pregnant.
Therefore, there is felt a need to provide a safe hair coloring composition which requires short dyeing time, has good hair dyeing property and 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
The present disclosure provides a hair coloring composition. In an aspect of the present disclosure the composition comprises a coloring agent, a humectant, a coupler, a chelating agent, an antioxidant, a catalyst, a thickening agent, a fragnance, a conditioning agent, a pH adjusting agent and a fluid medium..
The hair coloring composition comprises the colouring agent in the range of 1.2 mass% to11 mass% of the composition, the humectant in the range of 1.5 mass% to 5.5 mass% of the composition, the coupler in the range of 0.25 mass% to 6.25 mass% of the composition, the chelating agent in the range of 0.025 mass% to 0.3 mass% of the composition, the antioxidant in the range of 0.25 mass% to 1.25 mass% of the composition, the thickening agent in the range of 0.525 mass% to 8.5 mass% of the composition, the fragnance in the range of 0.4 mass% to 1.75 mass% of the composition, the conditioning agent in the range of 0.25 mass% to 5.0 mass% of the composition, catalyst in the range of 0.25 mass% to 2.0 mass% of the composition, and pH adjusting agent in the range of 0.75 mass% to 5.0 mass% of the composition. The pH adjusting agent maintains the pH of the composition in the range of 7 to 10. Demineralized water is used as a fluid medium in an amount sufficient to make 100 mass% of the composition.
In another aspect of the present disclosure, a process for preparing hair colouring composition is provided. The process involves preparation of a fluid medium and a dye phase in separate vessels. The process of preparation of the fluid medium involves adding a thickening agent slowly to the fluid medium with stirring for a predetermined time. The dye phase is prepared by addition of at least one humectant, at least one chelating agent, at least one antioxidant and a coloring agent to the fluid medium under stirring till it is completely dissolved.
The hair coloring composition is peroxide and ammonia free, and hence is safe for use. 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.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
The present disclosure will now be described with the help of the accompanying drawing, in which:

Figure 1 illustrates a flow chart describing the process of preparation of the hair colouring composition.
DETAILED DESCRIPTION
Embodiments, of the present disclosure, will now be described with reference to the accompanying drawing.
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.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
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 present disclosure envisages a hair coloring composition that is free of peroxide and ammonia, and is capable of rapid color development on hair.
In an aspect of the present disclosure, there is provided a hair coloring composition. The hair coloring composition comprises a coloring agent, a thickening agent, a humectant, a chelating agent, an antioxidant, a coupler, a catalyst, a fragrance, a conditioning agent, a pH adjusting agent and a fluid medium in a pre-determined proportion with each other.
The colouring agent can be one compound or a mixture of compounds selected from para-phenylenediamine, N, N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate and para amino phenol. In an embodiment, the coloring agent is a mixture of para-phenylenediamine, N, N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate and para amino phenol. Typically the, coloring agent can be in the range of 1.2 mass% to11 mass% of the composition.
The thickening agent can be one compound or a mixture of compounds, selected from the group comprisingxanthan gum, gelatin sodium alginate, hydroxyethyl cellulose, and sodium carboxy methyl cellulose. Typically, the thickeners or viscosity modifiers can be in the range of 0.525 mass% to8.5 mass% of the composition.
The humectant can be selected from the group comprising propylene glycol, ethylene glycol, glycerol, butylene glycol, and sorbitol. Typically the hair colouring composition comprises a humectant in the range of 1.5 mass% to 5.5 mass%.
The chelating agent can be selected from the group comprising disodium ethylene diamine tetra acetate (EDTA), tetrasodium EDTA, trisodium citrate, and etidronic acid. Typically the composition comprises a chelating agent in the range of 0.025 mass% to 0.35mass%.
The antioxidant used in the hair colouring composition can be a single compound or a mixture of compounds. The antioxidants inhibit the oxidation of process caused by free radicals. The antioxidant can be selected from the group consisting of sodium sulphite, ascorbic acid, vitamin K, vitamin E, tocopherol acetate, butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), ascorbyl palmitate, citric acid, propyl gallate, methionine, and sodium metabisulfite. Typically, antioxidants in the range of 0.125 mass% to 1.25 mass% can be present in the composition.
The catalyst in the hair colouring composition performs the function of gentle opening of the cuticle to allow the hair color to penetrate the cortex of the hair. Typically the catalyst in the hair colouring composition can be in the range of 0.25 mass% to 2.0 mass%.
The coupler in the hair colouring composition undergoes a coupling reaction to form high molecular weight products, which are trapped in the hair matrix and cannot be readily removed during washing, and thereby aids in retaining the hair color/dye even after repeated washing. The coupler can be one compound or a mixture of compounds. Typically the coupler can be in the range of 0.25 mass% to 6.25 mass% of the composition.
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. Typically the conditioning agent can be in the range of 0.25 mass% to 5.0 mass% of the composition.
The pH adjusting agent maintains the pH of the hair coloring composition to lie in the range of 7 to 10. The pH adjusting agent can be selected from the group comprising monoethanolamine, triethanolamine, diethanolamine potassium hydroxide, and sodium hydroxide. The hair colouring composition comprises a pH adjusting agent (alkalizer) in the range of 0.75 mass% to 5.0 mass% of the composition to maintain the pH.
The hair colouring composition further comprises a fragnance in the range of 0.4 mass% to 1.75 mass% of the composition. 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 is used in an amount sufficient to make 100 mass% of the hair coloring composition.

In an embodiment of the present disclosure, the hair colouring composition comprises para-phenylenediamine in the range of 0.7 mass% to 3.9 mass%, N, N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate in the range of 0.05 mass% to 1.25 mass% and para amino phenol in the range of 0.025 mass% to 1.0 mass% of the composition as a colouring agent. The composition further comprises propylene glycol as a humectant in the range of 1.5 mass% to 5.5 mass%. A mixture of sodium alginate in the range of 2.0 to 6.0 mass% or hydroxyl ethyl cellulose in the range of 0.5 to 5.0 mass% and sodium carboxy methyl cellulose in the range of 0.025 mass% to 0.50 mass% of the composition can be used as thickeners or viscosity modifiers. Sodium sulphite in the range of 0.025 mass% to 0.35 mass% of the composition and iso ascorbic acid or erythorbic acid in the range of 0.1 mass% to 0.90 mass% of the composition can be used as antioxidants. Magnesium sulphate in the range of 0.25 mass% to 2.0 mass% of the composition can be used as a catalyst. 2,4-diaminophenoxyethanol dihydrochloride in the range of 0.1 mass% to 2.0 mass% of the composition, meta amino phenol in the range of 0.1 mass% to 1.25 mass% and 1,2,4-trihydroxy benzene in the range of 0.7 mass% to 3.0 mass% of the composition are present as couplers in the composition. Ethylene diamine tetra acetate (EDTA) is present as a chelating agent in the range of 0.025 mass% to 0.35mass% of the composition. The composition further comprises a fragnance in the range of 0.4 mass% to 1.75 mass%. The fragnance used in the composition is any suitable fragnance known in the art. Amodimethicone and C-12-14 sec Pareth-7 in the range of 0.25 mass% to 5.0 mass% of the composition are present as hair conditioning agents. The hair colouring composition comprises monoethanolamine in the range of 0.75 mass% to 5.0 mass% of the composition as a pH adjusting agent (alkalizer) to maintain the pH at 9.4.
In another aspect of the present disclosure, there is provided a process for preparing a hair coloring composition. The process is hereinafter described in detail. The general process for preparation of the hair colouring composition is illustrated in figure 1. Initially, all the ingredients/raw materials are weighed and stored in individual poly bags or stainless steel vessel till use.
Referring to figure 1, it is seen that a pre-determined amount of a fluid medium is added to a vessel. In an embodiment, the vessel is made of stainless steel and is fitted with a mechanical stirrer. Typically, the fluid medium is added via a bottom nozzle present in the vessel.
A thickening agent is added to the fluid medium slowly, with stirring. Care is taken that lumps are not formed during the addition of the thickening agent. The resultant mixture is stirred further for a time period in the range of 40 minutes to 60 minutes.
In a separate vessel, a dye phase is prepared. A pre-determined amount of a fluid medium is added to the vessel. In an embodiment, the vessel is made of stainless steel and is fitted with a mechanical stirrer. The temperature of the fluid medium is maintained in the range of 55 °C to 65 °C.
A humectant is added to the fluid medium, followed by the addition of a chelating agent, and antioxidant, under stirring.
After obtaining a mixture of fluid medium, chelating agent and an antioxidant, a coloring agent is added, under stirring till it is completely dissolved. This is followed by the addition of a coupler.
The fragrance, and a conditioning agent are added, followed by the addition of a pH adjusting agent, under stirring.
The dye phase is transferred to the vessel containing the thickening agent and nitrogen gas is purged into the vessel. The mixture is stirred to obtain a homogenized mass.
A freshly prepared solution of a coupling agent is added to the homogenized mass, followed by stirring. The mixture obtained is recirculated for 2 minutes to 3 minutes to obtain a homogenized liquid.
Vacuum pressure is applied to the homogenized liquid in the range of 300 kg/cm2 to 450 kg/cm2, to remove any trapped air bubbles, and obtain the 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 of the present disclosure can be present in the form of a transparent/clear gel, lotion, cream or serum and is easy to apply. The hair coloring composition is peroxide and ammonia free, and hence is safe for use. 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. In an exemplary embodiment, the hair colouring composition of the present invention is in the form of a hair colouring serum that can be easily applied.
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 experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.
EXPERIMENTAL DETAILS
Experiment 1: Preparation of hair coloring composition of the present disclosure
Preparation of hair colouring composition: The hair colouring composition in accordance with the present disclosure was prepared using the below mentioned composition. The amount of ingredients (kg) used is summarized in Table-1.
Table-1: Hair coloring compositions in accordance with the present disclosure:
Sr.no Ingredient Function Example 1
Composition
Amt in (kg) Example 2
Composition
Amt in (kg)
1 D. M. water /Aqua Base Q.S to 100 % Q.S to 100 %
2 Sodium Alginate
or
Hydroxy ethyl cellulose
Thickener /viscosity modifier 2.5
or
1.25 3
or
1.5
3 Sodium Carboxymethylcellulose Thickener /viscosity modifier 0.075 0.075
4 Propylene glycol Humectant 3.5 4.0
5 Ethylene diaminetetraacetate Chelating agent 0.15 0.2
6 Sodium Sulphite Antioxidant 0.25 0.15
7 Iso Ascorbic acid /Erythorbic acid Antioxidant 0.25 0.5
8 Magnesium Sulphate Catalyst 0.5 1.25
9 Para-phenylenediamine Dye 1.75 2.0
10 2,4-diaminophenoxyethanol dihydrochloride Coupler 0.4 0.6
11 Meta amino phenol Coupler 0.4 0.5
12 N,N-bis (2-hydroxyethyl) -p-phenylenediamine sulfate Dye 0.4 0.6
13 Para Amino Phenol Dye 0.25 0.5
14 1,2,4 -Trihydroxy benzene Coupler 2.6 2.9
15 Toluene-2,5-diamine sulphate Dye 2.0 2.5
16 Fragrance Odour 0.5 1.0
17 Amodimethicone (and) C-12-14 sec Pareth -7 Hair conditioning 0.5 1.0
18 Mono ethanol amine pH adjusting agent 3.0 added to maintain the pH between 9 and 9.5 4.0 added to maintain the pH between 9 and 9.5

Experiment-2: Evaluation of colour retention time of the hair colouring serum.
(A) Criteria for choosing volunteer:
The volunteers with a minimum age of 21 or more and an upper age limit of 75 years were selected for evaluation of grey hair coverage and colour retention time for the same. The volunteers with any scalp, skin diseases or cut on head were excluded from the study.
16 volunteers (8 male and 8 female) having above 50 % grey hairs and minimum 1 inch grey hair re-growth visible were selected for the study. The selected volunteers were regular users of hair colour. The volunteers had not applied hair colour for 45 days before the start of the study.
(B) Data collection:
The details of chosen volunteers were noted down e.g. natural hair colour, % of grey hair approximately, length of hair from root, hair washing habits of volunteers. The feedback of volunteers was taken during application of the hair colour serum and after hair wash.The stability of colour serum on hair was judged by visual observation for a period of over 1 month with regular intervals.
(C) Application of the hair colour serum on the volunteers:
The hair colour serum was applied by brush and allowed to develop for a time period of 30 minutes. The hair was washed with mild shampoo & water, towel dried and finally dried with blow dryer. This method of colouring and drying was repeated for all the applications. The formulation trial of hair colouring serum was labeled as “Sample A”. The male volunteers were numbered as M1, M2, M3, M4, M5, M6, M7 and M8. The female volunteers were numbered as F1, F2, F3, F4, F5, F6, F7 and F8.
Table 3: Application of hair colouring serum on male volunteers and study of retention time
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 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-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 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-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 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-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 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.

Table 4: Application of hair colouring serum on female volunteers and study of retention time
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.

From Table 3and 4, the observations for 2nd day, 7thday, 14thday, 21st day & 28th day can be listed as follows:
For male volunteers:
• 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 all the 8 volunteers.
• For male volunteers, 5 average hair wash per week was carried out. 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 the volunteers wherein the shade on the grey hair faded between black and soft black.
• After 21 days gradual fadage was observed for all volunteers wherein the shade on grey hair faded from soft black to darkest brown.
• After 28 days gradual fadage was observed for all volunteers wherein the shade on grey hair faded from darkest brown to dark brown.
For female volunteers:
• 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.
• For female volunteers2 average hair wash per week were carried out. 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 wherein the shade faded between black and soft black.
• After 21 days gradual fadage was observed for all volunteers wherein the shade faded to soft black.
• After 28 days gradual fadage was observed for all volunteers wherein the shade faded from soft black to darkest brown.
(B) Further, the evaluation of the composition with respect to the synergistic action of the components was determined. Comparative compositions were prepared which comprise either none of the colouring agent, or only one of the colouring agents at twice the concentration in order to keep the active matter concentration constant. And the hair colour compositions were evaluated as carried out mentioned above.
It was observed that the colour development took longer time and the developed colour was only retained till 2 washes. Therefore, it was evident from the comparative study that the components of the hair colour in when present in specific concentration was synergistically effective in developing the colour in the predetermined time period and retaining the colour fastness for the predetermined cycles.
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 is safe and also provides nourishment to the hair and aids in its healthy growth.
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. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
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 invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure 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.

Documents

Application Documents

# Name Date
1 201921040374-STATEMENT OF UNDERTAKING (FORM 3) [04-10-2019(online)].pdf 2019-10-04
2 201921040374-PROOF OF RIGHT [04-10-2019(online)].pdf 2019-10-04
3 201921040374-POWER OF AUTHORITY [04-10-2019(online)].pdf 2019-10-04
4 201921040374-FORM 1 [04-10-2019(online)].pdf 2019-10-04
5 201921040374-DRAWINGS [04-10-2019(online)].pdf 2019-10-04
6 201921040374-DECLARATION OF INVENTORSHIP (FORM 5) [04-10-2019(online)].pdf 2019-10-04
7 201921040374-COMPLETE SPECIFICATION [04-10-2019(online)].pdf 2019-10-04
8 Abstract1.jpg 2019-10-14
9 201921040374-Proof of Right (MANDATORY) [04-01-2020(online)].pdf 2020-01-04
10 201921040374-FORM 18 [27-09-2023(online)].pdf 2023-09-27
11 201921040374-FER.pdf 2024-08-22
12 201921040374-FORM 3 [21-10-2024(online)].pdf 2024-10-21
13 201921040374-FORM 4 [22-02-2025(online)].pdf 2025-02-22
14 201921040374-FORM-26 [20-03-2025(online)].pdf 2025-03-20
15 201921040374-OTHERS [22-03-2025(online)].pdf 2025-03-22
16 201921040374-MARKED COPIES OF AMENDEMENTS [22-03-2025(online)].pdf 2025-03-22
17 201921040374-FORM-26 [22-03-2025(online)].pdf 2025-03-22
18 201921040374-FORM 13 [22-03-2025(online)].pdf 2025-03-22
19 201921040374-FER_SER_REPLY [22-03-2025(online)].pdf 2025-03-22
20 201921040374-CLAIMS [22-03-2025(online)].pdf 2025-03-22
21 201921040374-AMMENDED DOCUMENTS [22-03-2025(online)].pdf 2025-03-22
22 201921040374-US(14)-HearingNotice-(HearingDate-29-04-2025).pdf 2025-04-03
23 201921040374-Correspondence to notify the Controller [22-04-2025(online)].pdf 2025-04-22
24 201921040374-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [24-04-2025(online)].pdf 2025-04-24
25 201921040374-US(14)-ExtendedHearingNotice-(HearingDate-26-05-2025)-1200.pdf 2025-04-25
26 201921040374-Correspondence to notify the Controller [15-05-2025(online)].pdf 2025-05-15
27 201921040374-Written submissions and relevant documents [10-06-2025(online)].pdf 2025-06-10
28 201921040374-MARKED COPIES OF AMENDEMENTS [10-06-2025(online)].pdf 2025-06-10
29 201921040374-FORM 13 [10-06-2025(online)].pdf 2025-06-10
30 201921040374-AMMENDED DOCUMENTS [10-06-2025(online)].pdf 2025-06-10
31 201921040374-PatentCertificate09-09-2025.pdf 2025-09-09
32 201921040374-IntimationOfGrant09-09-2025.pdf 2025-09-09

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