Title of Invention

POWDER KERATIN COLOURING COMPOSITION AND A METHOD OF PREPARATION FOR THE SAME

Abstract

Disclosed herein is stable powder hair dye compositions with improved fragrance and colour deposition for colouring keratin fibers comprising of (i) Primary intermediates and couplers , (ii) Powder oxidizing component, (iii) Powder anionic surfactant, (iv) Cellulose gum, (v) Hydroxy acids,(vi) Filler or diluent material,(vi) Silicon elastomer blended with silicon dioxide and (vii) encapsulated volatile organic compounds. The invention further discloses a method for preparation of stable powder hair dye compositions.

Full Text

FORM 2 THE PATENT ACT 1970 (39 of 1970) AND The Patents Rules, 2003 COMPLETE SPECIFICATION (See section 10 and rule!3) 1. Title of the invention: "POWDER KERATIN COLOURING COMPOSITION AND A METHOD OF PREPARATION FOR THE SAME" 2. Applicant (s) (a) Name: Godrej Consumer Products Limited (b) Nationality: Indian company incorporated under the Indian Companies Act, 1956 (c) Address: Pirojshanagar, Eastern Express Highway, Vikroli (East), Mumbai - 400079, Maharashtra, India. 3. Preamble to the description The following specification particularly describes the invention and the manner in which it is to be performed. 1978 2008 17 SEP Field of invention: The present invention relates to a novel powder hair color / dye composition with improved fragrance and colour deposition and a method of preparation of the said composition. Background of the invention: Permanent hair dye systems have commonly been comprised of a combination of a dye material and a developer or activator solution, most commonly hydrogen peroxide. Additive materials including thickeners, fillers and perfumes are sometimes included in the hair dye system. Typically, the two parts of the system are packaged separately until use, when they are combined in one container, then mix well and activate the product and carefully pouring the mixed solution onto the roots of the hair and combing or working the solution into the hair by hand to thoroughly and completely saturate the hair. The mixture is usually left on the hair for about 15 to 30 minutes, depending upon the shade and color depth desired. Finally, the dye solution is shampooed out of the hair and the hair is dried. Care must be taken to prevent run offs onto clothing, furnishings, etc. Once the two solutions are mixed together, the mixture must be used within a relatively short time, such as within one hour. Such a conventional system has a variety of shortcomings, including: (1) problems in mixing the components together; (2) the added time needed to prepare the working dye solution; (3) the harshness of the systems to the hair due to ammonia; (4) the additional processing steps, packaging, shipping expenses, and waste generated due to multiple containers. Two types of powder hair dyes are generally known. One is a so- called one component type, that is a mixture of a powdered oxidation dye and a powdered oxidizing agent packaged together. The powder dye is mixed with water and applied to head to colour the hair and the mixture is kept on hair for 30 to 45 minutes to get the desired colour. The 2 other is a so-called two component type, that is a powdered oxidation dye and a powdered oxidizing agent separately packaged. The two component mixture is mixed just prior to their use to prepare a colouring mixture. Both types of dyes can be stored without deterioration until being prepared as the tinting mixture. Incorporation of conditioners and perfumes, in this type product is difficult because of compatibility issue and in powder form. Also incorporation of perfume in presence of oxidizing agent is also a stability issue. Method of preparation plays an important role in stability of the product. Embodiments of the present invention are directed towards these and other objectives. There is ample literature available on synthetic dyes, precursors to dyes, coupling agents, oxidizing agents etc. in powder form. European Patent EP1733761 describes an oxidative hair colouring composition comprising yogurt powder for improving combability of hair and further relates to process of coloring hair using said composition in combination with an oxidizing agent, preferably hydrogen peroxide. US Patent 4,808,189 discloses a powdered hair dye comprising an admixture of an oxidative dye component and an amount of a powdered oxidizing agent, wherein said dye component is present in the form of a cyclodextrin inclusion complex, which will give high stability for longer shelf life, color-fastness and deeper color. US patent 6,488,918 describes methods of making the powdery cosmetic composition using cross-linked silicone elastomer to improve the storage stability. US Patent 6,613313 describe an oxidation hair dye composition containing aniline compound which exhibits excellent spreadability, applicability, level-dyeing property and shampoo resistance and a method of dyeing hair with the hair dye composition. US 5,769,901 describe a powdered hair dye composition comprising: an oxidative dye component in powdered form in an amount effective for coloring hair; 3 an oxidizing component in powdered form in an amount effective to activate the oxidative dye component; an effective amount of a thickening component in powdered form; and sucrose in powdered form, wherein the sucrose is present in the hair dye composition in an amount of approximately 30-65 weight percent, based on the total weight of the powdered hair dye composition, wherein said powdered hair dye composition is mixed with water before application to the hair. Although the above prior arts claim powdered hair dye formulations, however, the problems such as free flowing properties of the formulation, avoiding dusting while manufacturing and application of the powder hair dyes with ease remain a problem till date. Further, incorporation of fragrance in the powdered hair dye is not possible as most of the fragrances are reported to be liquids. Therefore, the present inventors have attempted to overcome the aforementioned problems by incorporating silicone conditioners as well as encapsulated volatile organic compounds to improve the conditioning together with long lasting encapsulated fragrance and improved colour deposition. The invention further aims to provide improved process for manufacturing hair dye formulation for better stability & efficacy of the product. Object of the invention: Therefore, the object of the present invention is to obviate the aforesaid drawbacks by providing a stable composition resulting into a definite keratin colouration with improved conditioning and long lasting fragrance and process for preparation thereof. Summary of the invention: In accordance with the above objective, the present invention discloses a powder hair colour composition for colouring keratin fibers comprising of (i) 1 to 30 % w/w primary intermediates and couplers , (ii) 10 to 45 % w/w powder oxidizing component, (iii) 0.1 to 10 % w/w powder anionic surfactant, (iv) 0.1 to 20% w/w cellulose gum, (v) 0.1 to 10 % w/w hydroxy acids,(vi) 1 to 40 % w/w filler or diluent material,(vi)0.1 to 5% w/w 4 silicon elastomer blended with silicon dioxide and (vii) 0.1 to 2 % w/w encapsulated volatile organic compounds. In another aspect, the invention provides a method of preparation of encapsulated fragrance that can be used in the composition of the invention to improve the fragrance and colour deposition on keratin fibres. In yet another aspect, the process for preparation of the powder hair colour composition is described. Detailed description of the invention: The invention will now be described in detail in connection with certain preferred and optional embodiments, so that various aspects thereof may be more fully understood and appreciated. Accordingly, the present invention describes a novel cosmetic composition for dyeing keratin fibers, as well as process for preparation of the said composition. A typical composition of the present invention comprises primary dye intermediates and couplers along with oxidizing agents, surfactants, thickening agents, pH adjusting agents, spreadability agents, fillers or diluents, cellulose gums and encapsulated volatile organic compounds. Thus, the present invention encompasses an improvement to powdered hair dye composition which comprises encapsulated volatile organic compounds. The perfume compound is adsorbed in the cyclodextrin cavity. The complex when dissolved in water, cyclodextrin releases the fragrance. In accordance with the above, the present invention discloses a powder hair colour composition for colouring keratin fibers comprising of (i) 1 to 30 % w/w primary intermediates and couplers , (ii) 10 to 45 % w/w powder oxidizing component, (iii) 0.1 to 10 % w/w powder anionic surfactant, (iv) 0.1 to 20% w/w cellulose gum, (v) 0.1 to 10 % w/w hydroxy acids,(vi) 1 to 40 % w/w filler or diluent material,(vi) 0.1 to 5% w/w 5 silicon elastomer blended with silicon dioxide and (vii) 0.1 to 2 % w/w encapsulated volatile organic compounds. Thus, the stable powder hair colour composition with encapsulated fragrance and colour deposition for colouring keratin fibres according to the present invention is characterized by having 0.1 to 2% w/w encapsulated volatile organic compounds. In a preferred embodiment, the essential components of the present composition comprises at least one primary dye intermediate and coupler or only primary intermediates, in an amount between 1 and 30 percent, by weight relative to the total weight of the said composition. Representative primary dye intermediates include, for instance, p-phenylene diamine, p-toluene diamine, o-phenylene diamine, methoxy paraphenylene diamine, ortho aminophenol, para aminophenol, of a salt of said compound for example a mono, di or tri hydrochloride or hydro bromide or even sulphate thereof. The composition of the invention may comprise mixture of the above. Couplers used in the present invention may include resorcinol, 2-methyl resorcinol, meta amino phenol, alpha naphthol and meta phenylene diamine, of a salt of said compound for example a mono, di or tri hydro chloride or hydro bromide or even sulphate thereof or combinations thereof. The hair dye support used in the composition is in the form of a powder which comprises 10-45 percent of powder oxidizing agents. Representative oxidizing agents include for instance Sodium percarbonate, potassium percarbonate, sodium perborate, potassium perborate, sodium peroxide, potassium peroxide, magnesium peroxide, barium peroxide, calcium peroxide, strontium peroxide, urea peroxide. Among them sodium perborate, potassium perborate, sodium percarbonate, potassium carbonate are preferred. The composition of the invention comprises 0.10 to 10 percent weight of anionic surfactant. Surfactant useful in the present invention is selected from sodium lauryl 6 sulfate, ammonium lauryl sulphate, or potassium lauryl sulphate. A combination of different surfactants can be used to impart particular viscosity and foaming properties. The composition further optionally comprises a thickening agent in a concentration of about 0.1 to about 20 weight percent of the composition, used to thicken the composition. The thickening agent selected among, carboxymethyl cellulose, carboxy vinyl polymers, hydroxyl ethyl cellulose, hydroxy] propyl cellulose, methyl cellulose, xanthan gum, carrageenan, alginic acid salts, pectin, gum Arabic, gatch gum, karaya gum, tragacanth gum, agar powder, bentonite and cross linking polyacrylic acid salts. Among them carboxymethyl cellulose, hydroxyl ethyl cellulose, xanthan gum are preferred. The composition of the invention comprises 0.10 to 15 percent weight of hydroxy organic acids. The acids selected from among lactic acid, citric acid, succinic acid, tartaric acid, malic acid, or sodium and potassium or ammonium salts of them. Preferably citric acid or tartaric acid can be employed in an amount of from 2 to 10 weight percent to adjust the pH. The composition of the present invention comprises 0.1 to 5 weight percent of a mixture of Silicone elastomer with Silicone dioxide. The invention also comprises mixing the silicone elastomer ingredient in a suitable mixing unit with the silicone dioxide at room temperature (about 10 degree to 35 degree. C) in order to provide better distribution in the said composition. The preferred silicone elastomers include dimethicone / vinyl dimethicone cross polymer and cyclo penta siloxane and dimethicone cross polymer. The above composition, which may also, includes a sufficient amount of fillers, selected from the group salts of sodium, potassium, magnesium or calcium. In a preferred embodiment, the invention discloses a method of preparing encapsulated volatile organic compounds, wherein said method comprises mixing and pulverizing volatile organic compounds 1.0 to 43 parts in 100 parts of the cellulose gum, such as cyclodextrin, in a ribbon blender; sieving the pulverized mixture to obtain powder having 7 particle size of 80 microns to 200 microns, preferably 100 microns sieve. The molar ratio of volatile organic compounds to cellulose gum is in the range of 0.01: 0.99 to 1: 2.33. The perfume compound is adsorbed in the cyclodextrin cavity and when the complex dissolved in water, cyclodextrin releases the fragrance. The composition of the present invention comprises 0.1 to 2 % weight percent of encapsulated fragrance. In another preferred embodiment, the invention describes a method of preparing the composition, wherein said method comprises: a) coating 10 to 45 % w/w powder oxidizing component with 1.0 to 40% w/w fillers in a ribbon blender for 10 to 15 minutes at room temperature and keeping the mixture aside; b) adding 0.1 to 10 % w/w powder anionic surfactant, 0.1 to 20% w/w cellulose gum, 0.1 to 10 % w/w hydroxy acids and 0.1 to 5% w/w silicon elastomers blended with silicon dioxide, one by one into the ribbon blender; c) blending the mixture for 10 to 15 minutes at room temperature and adding 1.0 to 30 % primary intermediates and couplers into said mixture; followed by 0.1 to 2 % w/w encapsulated fragrance; and d) blending the whole mass in a ribbon blender at room temperature (about 15 degree to 30 degree. C) for 45 to 60 minutes, preferably 50 minutes. In yet another preferred embodiment, the invention provides an alternate method for preparing the hair dye composition which comprises: a) coating 10 to 45 % w/w powder oxidizing component with 1 to 40% w/w fillers followed by adding 1 to 30 % primary intermediates and couplers into said mixture together with 0.1 to 10 % w/w powder anionic surfactant; 0.1 to 20% w/w cellulose gum, 0.1 to 10 % w/w hydroxy acids; 0.1 to 5% w/w silicon elastomer blended with silicon dioxide and 0.1 to 2 % w/w encapsulated volatile organic compounds and b) blending the whole mass in a ribbon blender at room temperature at about 15 degree to 30 degree for 30 to 60 minutes. 8 A typical composition according to the present invention comprises: 1 to 30 % w/w primary intermediates and couplers; 10 to 45 % w/w powder oxidizing component; 0.1 to 10 % w/w powder anionic surfactant; 0.1 to 20% w/w cellulose gum; 0.1 to 10 % w/w hydroxy acids; 1.0 to 40 % w/w filler or diluent material; 0.1 to 5% w/w silicon elastomer blended with silicon dioxide and 0.1 to 2 % w/w encapsulated volatile organic compounds. The incorporation of encapsulated volatile organic compounds improves the colouration of keratin fibers by 5 to 10%. The cellulose gum used in the hair dye composition according to the invention is cyclodextrin may be selected from alpha, beta or gamma form of cyclodextrin. The volatile organic compounds used in the present invention may be selected from terpenoids, benzenoids, aldehydes, alcohols, esters, ketones, lactones or mixture thereof. The performance of the composition improves significantly when mixed with water. The following examples, which include preferred embodiments, will serve to illustrate the practice of this invention, it being understood that the particulars shown are by way of example and for purpose of illustrative discussion of preferred embodiments of the invention and in no way limit the scope of the invention. EXAMPLES: Example 1 Composition of the powder hair dye /colour is prepared having the following formulation: Ingredients Weight percent Sodium Perborate 30 Para Pheneylene diamine 12 Resorcinol 4 Meta aminophenol 1 Cellulose gum 15 9 Tartaric acid 4 Sodium Lauryl Sulphate 3 Magnesium sulphate 23.5 Silicon dioxide 5 Dimethicone 2 Encapsulated Fragrance 0.5 Example 2 Composition for the powder hair dye prepared having the following formulation: Ingredients Weight percent Sodium Perborate 30 Para Pheneylene diamine 18 Resorcinol 4 Meta aminophenol 1 Para aminophenol 2 Cellulose gum 15 Tartaric acid 4 Sodium Lauryl Sulphate 3 Magnesium sulphate 23.5 Silicon dioxide 5 Dimethicone 3 Encapsulated Fragrance 0.75 To use the above formulations, preferably about 1 part of the above compositions are mixed with eight parts of water to obtain a smooth consistency and applied to freshly shampooed hair. Keep it for 30 minutes and then rinse with plain water. Hair treated with above compositions of this invention will show luster, brownish black hair. Enhancement in colour improvement test: 10 The above composition (with encapsulated fragrance) and (without encapsulated fragrance) were used for dyeing human grey hair tresses. The mixture is prepared by mixing one (gram) part of the powder dye and eight parts of water were, left on one gram of human grey hair for a period of 30 minutes at 30 degree on the hair and then rinsed off with water. The hair was dried and colour difference was measured by TECHKON Spectro Dense A802030 Advance to obtain Lab value. The colour readings shows 5 to 10 % more colour deposition on the hair by using claimed invention with encapsulated fragrance as compared to without encapsulated fragrance. Advantages of the invention: 1) Powdered hair dye which possesses high stability for long shelf life. 2) Provides good conditioning benefit to the human hair and the keratin fibers. 3) Provides a natural looking soft colour to grey human hair and keratin fibers. 4) It has an improved fragrance stability 5) Improved colour deposition. 6) Convenient to use. It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative examples and that the present invention may be embodied in other specific forms without departing from the essential attributes thereof, and it is therefore desired that the present embodiments and examples be considered in all respects as illustrative and not restrictive, reference being made to the appended claims, rather than to the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. 11 We Claim, 1. Stable powder hair colour composition with improved fragrance and colour deposition for colouring keratin fibers comprising (i) primary intermediates and couplers, (ii) powder oxidizing component, (iii) powder anionic surfactant, (iv) cellulose gum, (v) hydroxy acids, (vi) filler or diluent material, (vi) silicon elastomer blended with silicon dioxide and (vii) encapsulated volatile organic compounds. 2. A method of preparing encapsulated volatile organic compound according to claim 1, wherein said method comprises mixing and pulverizing volatile organic compounds 1.0 to 43 parts in 100 parts of the cellulose gum in a ribbon blender and sieving the pulverized mixture to obtain powder having particle size of 80 microns to 200 microns. 3. The method as claimed in claim 3, wherein the molar ratio of volatile organic compounds to cellulose gum is 0.01: 0.99 to 1: 2.33. 4. The method as claimed in claims 3 and 4, wherein said cellulose gum is cyclodextrin. 5. A method of preparing the powder hair colour composition according to claim 1, wherein said method comprises: a) coating 10 to 45 % w/w powder oxidizing component with 1.0 to 40% w/w fillers in a ribbon blender for 10 to 15 minutes at room temperature and keeping the mixture aside; b) adding 0.1 to 10 % w/w powder anionic surfactant, 0.1 to 20% w/w cellulose gum, 0.1 to 10 % w/w hydroxy acids and 0.1 to 5% w/w silicon elastomers blended with silicon dioxide, one by one into the ribbon blender; c) blending the mixture for 10 to 15 minutes at room temperature and adding 1.0 to 30 % primary intermediates and couplers into said mixture, followed by 0.1 to 2 % w/w encapsulated volatile organic compounds; and d) blending the whole mass in a ribbon blender at room temperature (about 15 12 degree to 30 degree. C) for 45 to 60 minutes, preferably 50 minutes to obtain powder hair colour composition. 6. A method of preparing the powder hair colour composition according to claim 1, wherein said method comprises: a) coating 10 to 45 % w/w powder oxidizing component with 1 to 40% w/w fillers followed by adding 1 to 30 % primary intermediates and couplers into said mixture together with 0.1 to 10 % w/w powder anionic surfactant; 0.1 to 20% w/w cellulose gum, 0.1 to 10 % w/w hydroxy acids; 0.1 to 5% w/w silicon elastomer blended with silicon dioxide and 0.1 to 2 % w/w encapsulated volatile organic compounds and b) blending the whole mass in a ribbon blender at room temperature at about 15 degree to 30 degree for 30 to 60 minutes to obtain powder hair colour composition. 7. The powder hair colour composition for colouring keratin fibers as claimed in claim 1, wherein said encapsulated volatile organic compounds improves the colouration of keratin fiber by 5 to 10%. 8. The powder hair colour composition for colouring keratin fibers as claimed in claim 1, wherein the volatile organic compounds are selected from the group consisting of terpenoids, benzenoids, aldehydes, alcohols, esters, ketones, lactones or mixture thereof. 9. Stable powder hair colour composition with improved fragrance and colour deposition for colouring keratin fibers comprising (i) 1 to 30 % w/w primary intermediates and couplers, (ii) 10 to 45 % w/w powder oxidizing component, (hi) 0.1 to 10 % w/w powder anionic surfactant, (iv) 0.1 to 20% w/w cellulose gum, (v) 0.1 to 10 % w/w hydroxy acids,(vi) 1 to 40 % w/w filler or diluent material,(vi) 0.1 to 5% w/w silicon elastomer blended with silicon dioxide and (vii) 0.1 to 2 % w/w encapsulated volatile organic compounds. 13 10. A powder hair colour composition for colouring keratin fibers according to any one of the preceding claims, wherein the performance of the composition improves significantly when mixed with water. Dated this 17th day of September 2008 Dr. Gopakumar G. Nair Agent for the Applicant 14

Documents:

1978-mum-2008 abstract.pdf

1978-mum-2008 claims.pdf

1978-mum-2008 correspondence.pdf

1978-mum-2008 descraption(complete).pdf

1978-mum-2008 form 1.pdf

1978-mum-2008 form 2(title page).pdf

1978-mum-2008 form 2.pdf

1978-mum-2008 form 3.pdf

1978-mum-2008 form 5.pdf

1978-mum-2008-abstract.doc

1978-mum-2008-claim.doc

1978-MUM-2008-CLAIMS(AMENDED)-(3-10-2013).pdf

1978-MUM-2008-CLAIMS(MARKED COPY)-(3-10-2013).pdf

1978-MUM-2008-CORRESPONDENCE(1-10-2008).pdf

1978-MUM-2008-CORRESPONDENCE(19-8-2010).pdf

1978-mum-2008-desecription (complete).doc

1978-MUM-2008-FORM 1(1-10-2008).pdf

1978-MUM-2008-FORM 18(19-8-2010).pdf

1978-mum-2008-form 2.doc

1978-MUM-2008-FORM 26(1-10-2008).pdf

1978-MUM-2008-REPLY TO EXAMINATION REPORT(3-10-2013).pdf