FORM 2
THE PATENTS ACT 1970
(Act 39 of 70)
COMPLETE SPECIFICATION
(See SectionlO)
TITLE OF INVENTION:
HAIR COLORING SHAMPOO COMPOSITION AND A METHOD FOR THE PREPARATION OF THE SAME
APPLICANT(S):
Name: EMAMI LIMITED
Nationality: An Indian Company registered under the Companies Act, 1956
Address: Emami Limited, 701, Express Zone, Western Express Highway, Goregoan
(East), Mumbai - 400 063.

Title:
Hair Coloring Shampoo Composition and a process for the preparation of the same
Field of Invention
The present invention relates to a shampoo composition and particularly a coloring shampoo composition which on regular use gives gradual and long lasting grey coverage with minimal hair damage
Background
A large section of today's population makes use of hair color for combating problems associated with premature graying of hair. Over the years, numerous permanent hair color compositions for gray coverage have been made available in the public domain. But the hair damage associated with these compositions is intense and very often leaves color stains on hands, scalp, towels and pillows.
The conventional permanent hair color compositions in general constitute primary intermediates (mostly Para-phenylenediamine (PPD)), Coupling agents (mostly meta substituted anilines) and bleaching / oxidizing agents (mostlythCh for cream colors and Barium Peroxide and perborates for powder colors). Coloring process is performed in aqueous medium for powder colors and in an alkaline medium for cream colors. Although these compositions are effective in grey coverage and hair coloring, most commonly used ingredients like H2O2, Ammonia and PPD are known to be potential allergens causing allergies

primarily to the skin, eyes and scalp apart from hair damage due to their harsh nature.
Prior art suggests the existence of hair coloring shampoo compositions which are available without H2O2, Ammonia and PPD. However the compositions still largely remain anionic surfactant based, at a higher pH and with direct dyes / cationic dyes.
European Application EP 1656967 Bl discloses a color enhancing composition comprising at least one anionic surfactant and at least one non-ionic surfactant, at least one cationic direct dyestuff and at least one hydroxyl carboxylic acid and/or dicarboxylic acid. Apart from enhancing color the composition intends to improve hair shine, manageability and softness of the hair.
European Application EP 1504749 Al discloses that the presence of sulfated anionic surfactants reduces the color enhancing performance, but they should be present at minor concentrations in the color shampoo compositions. Therefore suitable anionic surfactants of the carboxylate type are used not exceeding 50 % of the total concentration, thereby retaining the non-ionic and amphoteric as the main component.
Australian Application AU 200131256 B2 discloses a color depositing composition comprising alkyl glucoester as an anionic surfactant along with at least one cationic dye. Therefore, it is a foaming anionic based coloring shampoo. The alkyl glucoester also lends conditioning effects to the shampoo.

US Application US 578857 Bl (Color Shampoo Formula) discloses a shampoo based formulation which typically makes use of a cationic dye, an anionic surfactant and an amphoteric surfactant. This composition is for the coloring of grey hair which has not been subjected to a prior oxidation process or other chemical treatments.
Now considering time and again anionic surfactants have been the single most effective constituent of shampoo or shampoo based systems due to their intensive foaming and cleansing properties it also has to be understood that this is not the case with coloring shampoos. The cationic components like cationic dyes which form an important base of coloring systems in hair care products do not give the intended results in terms of the amount of color to be deposited,when in combination with anionic surfactants as they are not compatible. There is a need for adopting parallel surfactant systems which in combination with the cationic components are efficacious in maximum gray coverage and also delivers cleansing benefits.
It is therefore desirable to address the disadvantages associated with the use of anionic surfactant as seen in the prior art apart from delivering a damage free composition, which have been overcome in the present invention by providing an anionic-surfactanf free hair coloring composition with cleansing properties
Objects of Invention: 1. It is a primary object of the invention to provide a water based hair coloring shampoo composition and particularly a coloring shampoo

composition which on regular use gives gradual and long lasting grey coverage with minimal hair damage apart from delivering cleansing benefits.
2. It is another object of the invention to provide a safe hair coloring shampoo composition which is devoid of conventional damage causing compounds like Ammonia, Hydrogen peroxide, PPD, Sulphates and other bleaching / oxidizing agents.
3. It is another object of the invention to provide a hair coloring shampoo which overcomes the problems of eye irritation, allergies and hair damage.
4. It is another objective of the invention to provide a hair coloring composition close to neutral pH(6 to 7) with added advantages with respect to mildness and safety.
5. It is another objective of the invention to make the color application process hassle free and a very easy one like a shampooing process and delivers benefits in situ.
6. It is another object of the invention to provide a process for the preparation of a water based hair coloring shampoo.
Summary of Invention:
The present invention relates to a hair coloring shampoo composition and the process of preparation of the same. The aqueous hair coloring shampoo

composition comprises a non-ionic surfactant, at least one amphoteric surfactant,at least one betaine surfactant and a cationic dye associated with a pigment. There is no anionic surfactant. There are no damage causing ingredients such as H2O2, Ammonia, Sulphate and PPD. The pH of the composition is close to neutral (6 to 7) and gives added advantages with respect to mildness and safety. This being hair coloring shampoo, grey coverage / hair coloring benefits are delivered in situ and hence overall process is very simple as shampoo and hassle free / less messy.
This hair coloring shampoo composition delivers on shampoo benefits viz. mainly cleaning and also on regular use gives gradual and long lasting grey coverage with minimal hair damage. Foam height is comparable to conventional marketed shampoo formulations.
Detailed description of the Invention:
The present invention is an aqueous hair coloring shampoo composition wherein "aqueous" denotes that the composition has water or an aqueous solution as a major component. Therefore, the composition comprises a range of 55 to 60 percent by weight of the total weight of the composition.
The shampoo composition primarily consists of anon-ionic (Decyl Glucoside) and amphoteric (Betaine and Disodium Cocoamphodiaceate) surfactants as the primary and secondary surfactants respectively. Anionic surfactants which are

generally the foam producing ingredients in shampoo compositions are absent in the present composition and thereby the non-ionic surfactant in combination with the amphoteric surfactants generate foam quantity comparable to that of anionic surfactants.
The Primary surfactant suitable for use in the composition of the invention includes alkyl glucosides namely decyl glucoside, contributing to a range of 4 to 10 % weight of the composition.
The secondary surfactant suitable for use in the composition of the invention includes Sodium Cocoamphoacetate, Sodium Cocoamphopropionate, Disodium Cocoamphodiacetateand Disodium Cocoamphodipropionate, preferably, the betaine surfactant which is yet another Secondary surfactant in the present invention is a cocamido alkyl betaine such as cocamido propyl betaine. These secondary/auxiliary surfactants function as foam boosters or foam modifiers.
The composition includes the secondary surfactant; amphoteric surfactant from a range of 6 to 10 % by weight of the composition and the betaine surfactant in the range of 10 to 20 % by weight of the composition.
The overall range of surfactant levels in the composition should not exceed 26 % of the weight of the composition beyond which, poor color delivery is possible.
The concentration of cationic dyes in the composition ranges from 0.2 to 1.0 percent of the weight of the composition. The cationic basic dyes useful in the present composition of the invention include Basic Red 76 (CI No-12245), Basic

Blue 99, basic Brown 16, Acid Violet 43, Basic Red 76, Basic Yellow which further enhances the coloring capacity of the shampoo composition. The trade names under which these cationic dyes are available are Arianor Ebony 306020 and Madder Red. A high pigment concentration in the form of dispersion is included in the composition under the trade name Covarine Black WS 9199 and the concentration of the same ranges between 0.2 to 1 % of the weight of the composition. Covarine Black WS 9199 is the key pigment responsible for grey coverage. A combination of cationic dyes and the pigment results in an optimized synergy giving extensive grey coverage.
Main black color delivery/ grey coverage is through Covarin Black WS 9199 pigment (CI 77266). Other basic dyes are to enhance black effect delivered by Covarin WS 9199.
The hair coloring composition also includes an acrylates copolymer to function as a rheology modifier in order to function as a structuring agent and to increase the viscosity of the composition.to increase the
Furthermore the composition includes the surfactants combined with a conditioning polymer. The polymers which find suitability here are known by their CTFA category name Polyquaternium which further includes samples like Polyquaternium-53, Polyquaternium 57, Polyquaternium 67 and Polyquaternium 76.

The hair coloring shampoo composition also includes other conventional ingredients like moisturizers, chelating agents, UV Filters and sunscreens and< humectants due to various functionalities associated with the same.
The moisturizer or moisturizing agent used in the composition may include a component selected from D-panthenol and similar compounds and it contributes to a range of 0.1 to 0.5 % of the weight of the composition.
The preferred chelating agent found in the range of 0.01 to 1.0 % of the weight of the composition is ethylene diamine tetra acetic acid.
A suitable humectant used in the composition in the range of 1.0-5.0 % of the weight of the composition is Hydrogenated starch hydrolysate.
Performance of Hair coloring shampoo composition:
The present composition gives good cleansing benefits in terms of performance levels. Foam height values obtained by BIS method indicates foam generation is comparable to already existing prior art and the relevant compositions.
On conducting a performance study it was observed that, 50% grey hair swatches are transformed to 100 % black hairs after 5 washes with the present hair coloring shampoo composition. Similar results were achieved for 50 to 100 % grey hairs also.
An added advantage of the present composition is that post application this coloring shampoo does not stain object or surfaces, for example scalp, towel, pillows, most likely to come in contact during the application process.

The present invention also provides a process for the preparation of a hair coloring shampoo composition which comprises the following three main steps as each step constitutes a phase:
a. Phase A:DM water, Acrylates Copolymer, Disodium Cocoamphodiacetate,
DecylGlucoside,Polyquaternium-53,Triethanolamine, cocamidopropylbetaine
Preparing of a homogeneous solution by mixing the ingredients of Phase A one by one under continuous stirring.
b. Phase B: DM water, Ethylenediamine tetra acetic acid,
EthylhexylMethoxycinnamate / Butyl Methoxydibenzoylmethane / PPG-26-
Buteth-26 / Ethylhexyl Salicylate / PEG-40-Hydrogenated Castor Oil,
Hydrogenated starch hydrolysate, D-Panthenol, Methylchloroisothiazolinone
(and) Methylisothiazolinone.
Weighing of Phase B water separately, for the addition of Phase B ingredients one by one under continuous stirring to prepare a homogenous solution followed by admixing of Phase A in to Phase B under constant stirring.
c. Phase C: Basic Red 76(CI No-12245), CI-772266 & glycerine & aqua &
PVP, Basic blue 99 & Basic brown 16 & Acid violet 43 & Basic red 76 and
Basic yellow 57, Fragrance Ultra Gloss
Mixing of Phase C ingredients one by one under continuous stirring.

The following examples illustrate the present invention. The compositions described below are expressed as weight percentages of the components.
Example 1

s.
No Phase INCI Name Range
(% weight)
1.
2. .
3. A DM Water 45-40%

Acrylates Copolymer 7-8%

Cocamidopropyl betaine 13-14%
4.
Disodium Cocamphodiacetate 6-8%
5.
DecylGlucoside 6-8%
6.
Polyquaternium-39 0.5-1%
7. B Tri ethanol Amine 1.5-2%
8. C DM water 20-15%
9. 10.
Ethylene di amine tetra acetic acid 0.05-0.2%

D-Panthenol 0.3-0.8%
11.
Basic Red 76(CI No-12245)-Madder Red 0.05-1.0%
12. 13.
CI-772266 & glycerine & aqua&PVP 0.2-1%

Arianor Ebony 306020 0.4-1%


Example 2
S.
No Phase INCIName Range
( % weight)
1. 2. 3. 4.
5. 6. A DM Water 55-25%


Acrylates Copolymer 6-10%


Cocamidopropyl betaine 10-20%


Disodium Cocamphodiacetate 6-10%


Decyl Glucoside 4-10%


Polyquaternium-53 0.2-1%
7. B Tri ethanol Amine 1.0-3.0%
8.
9.
10.
11. C Ethylhexyl
Methoxycinnamate / Butyl Methoxydibenzoylmethane / PPG-26-Buteth-26 / Ethylhexyl Salicylate / PEG-40-Hydrogenated Castor Oil 0.2-1.0%


Methylchloroisothiazolinone (and) Methylisothiazolinone. 0.01-0.5%


Hydrogenated starch hydolysate 1.0-5.0%


Fragrance 1.0-3.0%
12. 13.
14. D DM water 15-5%


Ethylene di amine tetra acetic acid 0.01-0.2%


D-Panthenol 0.1-1%


S.
No Phase INCI Name Range
(% weight)
15. Basic Red 76(CI No-12245)-Madder Red 0.2-1.0%
16.
CI-772266 & glycerin& aqua & PVP 0.2-1%
17.
Arianor Ebony 306020 0.2-1%

Exan ple 3
S.
No Phase INCI Name Range( % weight)
1. A DM Water 45-40%
2.
Acrylates Copolymer 7-8%
3.
Cocamidopropyl betaine 13-14%
4.
Sodium Cocoamphopropionate 6-8%
5.
Decyl Glucoside 6-8%
6.
Polyquaternium 67 0.5-1%
7. B Tri ethanol Amine ■1.5-2%
8. C DM water 20-15%
9.
Ethylene di amine tetra acetic acid 0.05-0.2%
10.
D-Panthenol 0.3-0.8%

s.
No Phase INCI Name Range
(% weight)
11. C Basic Red 76(CI No-12245)-Madder Red 0.05-1.0%
12.
CI-772266 & glycerine & aqua & PVP 0.2-1%
13.
Arianor Ebony 306020 0.4-1%
Suitable humectants, UV Filters, Sunscreens and Preservatives may be added as per requirement.
Test Example Procedure:
1. The DM water of phase A is charged in to a beaker.
2. Ingredients of Phase A are added one by one under continuous stirring to prepare a homogenous transparent solution.
3. Similarly Phase B ingredient solution is added to Phase A solution under continuous stirring.
4. Phase C is added to Phase A+B under continuous stirring.
5. Lastly the color properties are checked for and transferred in to suitable container.

We claim:
1. An aqueous coloring shampoo composition with a water base, comprising: -at least one amphoteric surfactant; -a betaine surfactant; -at least one non-ionic surfactant; and -at least one basic dye associated with a pigment.
2. The aqueous coloring shampoo composition according to claim 1, wherein the amphoteric surfactant is selected from the group consisting of Sodium Cocoamphoacetate, Sodium Cocoamphopropionate, Disodium Cocoamphodiacetate, Disodium Cocoamphodipropionate.
3. The aqueous coloring shampoo composition according to claim 1, wherein the betaine surfactant is selected from a group of cocamido alkyl betaines.
4. The aqueous coloring shampoo composition according to claim 3, wherein the betaine surfactant is cocamido propyl betaine.
5. The aqueous coloring shampoo composition according to claim 1, wherein the non- ionic surfactant is selected from a group of alkyl glucosides.
6. The aqueous coloring shampoo composition according to claim 5, wherein the non-ionic surfactant is decyl glucoside.

7. The aqueous coloring shampoo composition according to claim 1 includes one or more cationic basic dye components selected from a group consisting of Basic Red 76, Basic Blue 99, basic Brown 16, Acid Violet 43, Basic Red 76, Basic Yellow.
8. The aqueous coloring shampoo composition as claimed in claim 1, wherein the water base is in the range of 30 % -70 % by weight of the composition.
9. The aqueous coloring shampoo composition as claimed in claim 4, wherein the amphoteric surfactants are in the range of 6 % to 10% by weight of the composition.

10. The aqueous coloring shampoo composition as claimed in claim 3, wherein the betaine surfactants are in the range of 10 % to 20% by weight of the composition.
11. The aqueous coloring shampoo composition as claimed in claim 5, wherein the non-ionic surfactants are in the range of 4 % to 10% by weight of the composition.
12. The aqueous coloring shampoo composition as claimed in claim 7, wherein the cationic basic dyes are in the range of 0.2 % to 1% by weight of the composition.
13. The aqueous coloring shampoo composition as claimed in claim 1, wherein the shampoo composition pH is in the range of 6 to 7.

14. A method for the preparation of the aqueous coloring shampoo composition comprises the following steps:
-Preparing of a homogeneous solution by mixing the ingredients of Phase A one by one under continuous stirring.
-Weighing of Phase B water separately, for the addition of Phase ingredients one by one under continuous stirring to prepare a homogenous solution followed by admixing of Phase A in to Phase B under constant stirring.
-Mixing of Phase C ingredients one by one under continuous stirring.