Claims:We Claim:

1. A kit comprising silicone active based hair conditioning formulation atleast in two parts comprising:
(A) first part of the hair conditioning formulation comprising 1 to 50% of a reactive organopolysiloxane of structure (i)

………………….(i)

where, Z is the carbinol group having functionality like –CpH2p-OA; where p is an integer selected from 0 to 20 and A is either Hydrogen or an alkyl group,
m is from 0 to 5000, n is from 1 to 5000,
R’ is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group; and
an organic solventwherein the reactive organopolysiloxane of structure (i) is clearly soluble in the solvent;

(B) Second part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (ii)

…………………….(ii)

where, Y is the anhydride group and not limited to the said functionalities,
R" is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group,
b is atleast 10 and a is more than or equal to 0; and
an organic solvent, wherein the reactive organopolysiloxane of structure (ii) is clearly soluble in the organic solvent.

2. A kit comprising silicone active based hair conditioning formulation as claimed in claim 1 comprising directions of use for application of said first and second part of the hair conditioning formulation for in-situ generation of resulting hair conditioning organopolysiloxane molecule within the hair cortex and remain entrapped for a longer time even after consecutive hair wash cycles.

3. A kit comprising silicone active based hair conditioning formulation as claimed in anyone of preceding claims 1 or 2 wherein said first and second part of the hair conditioning formulation are adapted to first enter in the hair cortex and then react with each other to in-situ generate ~CH2-CO-O–CH2~ linkage at the a, ? position of the resulting organopolysiloxane molecule of high viscosity of at least 100 mPa.s at 25 oC to favour entrapment within the hair cortex for a longer time even after consecutive hair wash cycles.

4. A kit comprising silicone active based hair conditioning formulation as claimed in anyone of preceding claims 1 to 3 wherein the solvent in said formulation is selected to make a clear solution of the reactive organopolysiloxanes and toprovide low surface tension of uptoabout 25 dynes/sec more preferably upto 20 dynes/sec to favour effective uniform spreading of the actives (A) and (B) on hair surface when applied in small amounts for initiation of the in-situ reaction.
5. A kit comprising silicone active based hair conditioning formulation as claimed in anyone of preceding claims 1 to 4 wherein said organic solvent is selected from cyclomethicone or mixtures thereof, short chain volatiles selected from trimethylsiloxy terminated polydimethylsiloxane (dimethicone), short chain alkanes or mixtures thereof.

6. A kit comprising silicone active based hair conditioning formulation as claimed in anyone of preceding claims 1 to 5 wherein said ingredient (A) of organopolysiloxane of structure (i) preferably has n equal to 3 and A is hydrogen wherein said ingredient (B) has the functionality Y preferably derived of succinic anhydride.

7. A method of hair conditioning involving
(A) first part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (i)

………………….(i)

where, Z is the carbinol group having functionality like –CpH2p-OA; where p is an integer selected from 0 to 20 and A is either Hydrogen or an alkyl group,
m is from 0 to 5000, n is from 1 to 5000,
R’ is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group; and
an organic solvent wherein the reactive organopolysiloxane of structure (i) is clearly soluble in the solvent;

(B) Second part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (ii)

…………………….(ii)

where, Y is the anhydride group and not limited to the said functionalities,
R" is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group,
b is atleast 10 and a is more than or equal to 0; and
the organic solvent, wherein the reactive organopolysiloxane of structure (ii) is clearly soluble in the organic solvent, comprising the steps of:
(a) applying said first and second part of the hair conditioning formulation to hair to be conditioned in combination or individually one after the otherin the presence of a catalyst to initiate the reaction between carbinol silicone and anhydride silicone; and
(b) allowing the said first and second part of the hair conditioning formulation to enter the hair cortex for in-situ generation of resulting hair conditioning organopolysiloxane molecule within the hair cortex to thereby remain entrapped for desired conditioning even after several wash cycles.

8. A method of hair conditioning as claimed in preceding claim 7
wherein said first part of the hair conditioning formulation (A) involving reactive organopolysiloxane of structure (i) that is hydroxyl silicone polymer of a,? hydroxy propyl polydimethylsiloxane is obtained by reacting hydrogen siloxane containing polymer with allyl alcohol; and
wherein said second part of the hair conditioning formulation (B) involving reactive organopolysiloxane of structure (ii) is a a,? anhydride polydimethylsiloxane obtained by reacting hydrogen siloxanecontaining polymer with allyl succinic anhydride.

9. A method of hair conditioning as claimed in anyone of preceding claims 7 and 8 comprising the steps of:
(I) intimately mixing with carbinol silicone solution (A) with anhydride silicone solution (B) in a selective ratio range preferably in the range of 10:90 to 90:10;
(II) applying the said mix on the hair ensuring entire coverage of the hair with the solution (A) and (B);
(III) leaving the hair with the said mix at ambient temperature for atleast 5 minutes for favouring the entry of carbinol silicones and anhydride silicones in the cortex of the hair to in-situ react and yield a high viscosity organopolysiloxane polymer involving ~CH2-CO-O–CH2~ linkage of viscosity of at least 100 mPa.s at 25 oC adapted for conditioning the hair having lasting conditioning effect over several consecutive wash cycles.

10. A method of hair conditioning as claimed in anyone of preceding claims 7-9 wherein
step (I) involving intimately mixing carbinol silicone solution (a) with anhydride silicone solution (b) is preferably done at the selective ratio range of 50:50;
step (III) involving leaving the hair with said mix of carbinol silicone (A) and anhydride silicone solution (B) at ambient temperature is preferably left for 15-30 minutes for favouring the entry of carbinol silicone and anhydridesilicones in the cortex of the hair to react with each other in-situ adapted to form hydrophobic silicone coating on hair.

11. A method of hair conditioning as claimed in anyone of preceding claims 7-10 wherein step (II) of applying said mix on the hair ensuring entire coverage of the hair involves application ofcarbinol silicone solution (A) and anhydride silicone solution (B) at the levels of upto10 gm per 100 gm of hair wherein preferably atleast 1% of carbinol silicone solution (A) and atleast 1% of anhydride silicone solution (B) are applied on 100 gram of clean hair to favour optimum hydrophobic coating on hair having lasting effect over several consecutive wash cycles.

12. A method of hair conditioning as claimed in anyone of preceding claims 7-11 wherein the catalyst is selected from basic catalysts including triethanolamine to initiate the reaction between that carbinol silicone and anhydride silicone in basic condition at room temperature of 25 ?C.

Dated this the 16th September, 2015 Anjan Sen
Of Anjan Sen and Associates
(Applicants Agent)

, Description:
PATENT OF ADDITION TO PARENT APPLICATION NO. 158/KOL/2011 dt. 04.02.2011

FIELD OF INVENTION
The present invention relates to a hair conditioning composition/agent/ kit adapted to favour long lasting conditioning effect on the hair and maintain lively hair for a longer period of time comprising formulations of selective organopolysiloxane molecules, with carrier solvent and more particularly, relates to long lasting hair conditioning formulation adapted to favour entering of reactive silicones in the hair cortex through hair cuticles to generate reacted high viscosity polymer which could be retained in the narrow passage between the hair cuticles for a longer time on hair surface even after number of hair wash and keep the hair more lively for a longer duration. The present invention is further directed to not only save unnecessary organopolysiloxane drainage in rinse water but also aid rinse waste water treatment more facile in waste water treatment plant. Therefore, the present invention in other words is addressed not only to keep the hair more lively for longer time but also helps to recycle the huge amount of rinse water as a part of responsible care.

BACKGROUND ART
Globally, most of the people wash the hair with 2-in-1 shampoo or wash with standard shampoo and use conditioner separately or use leave on conditioner in dry hair after washing the hair with shampoo. In all cases, the conditioner used after cleaning the hair to give a conditioning effect is not permanent. Therefore, it is important during hair washing to ensure that the hair gets cleaned first while washing the hair and then during rinsing, the conditioner gets transferred to the hair. Silicone use in 2-in-1 shampoo or conditioner or leave on silicone (silicone gum blend in volatile solvent) are apparently distributed on hair surface and every time during hair washing, the same gets partly or fully cleaned from hair surface and get drained out with rinsed waste water.
Standard hair conditioner like 2-in-1 shampoo ideally works in two stages during application of shampoo. In the 1st stage upon application of shampoo in washing stage, only detergent part of the shampoo emulsify all dirt and residual conditioning polymers gets retained in the hair and the conditioner molecules present in the shampoo should not get deposited on the hair at the washing stage. In the second stage, all emulsified dirt particles gets washed in the water used for rinsing and conditioning molecule present in the shampoo immediately settles on the hair. In today’s world, silicone is one of best conditioning polymer used in most of the conditioning shampoos and therefore, during each application of conditioning shampoo, some quantity of silicone polymer in the form of emulsified dirt gets washed out through rinse water and gradually accumulates from a small quantity to noticeable quantity in waste water. Moreover, conditioning properties in hair is also dependent on how efficiently conditioning molecule stay in shampoo solution and not deposit on hair during washing period. Additionally, conditioning properties in hair also depend on how fast conditioning silicone molecule settles on the hair during rinsing. Furthermore, most of the rinse off hair conditioning product available in the market transfer conditioning silicone molecule as high as 40 to 50% on hair surface while the rest of the silicone gets washed away in the water used for rinsing with increase of silicone quantity in waste water.
Presently available silicone leave-on hair conditioner contains high viscous silicone polymer dissolved in either cyclomethicone or other organic solvent. After application of such leave on conditioner, Silicone gum form a smooth film in hair and solvent in the conditioner helps for spreading high viscosity silicone dimethicone or dimethiconol polymer on hair surface and later the solvent evaporates from the hair. Hence, the hair gets coated with fine silicone film and does not lose silicone conditioner during application. Presently available silicones doesn’t have any entrapping or bonding with hair surface and as a result, during hair washing with shampoo, silicone film from hair surface gets washed off easily during hair rinsing. Therefore, this type of leave on conditioner also does not last permanently on the hair and after each hair wash such type of hair conditioners are applied again on the hair to get the desired conditioning effect.

US 5646214describe a coating composition containing polyester polymers with terminal carbamate groups and polymeric polyol derived from ethylenically unsaturated monomers.

WO2013070302A1 describes a cosmetic composition of reactive blend copolymer for imparting transfer-resistant film on integument comprises, in vehicle, first phase polymer having pendant maleic anhydride functional group and second phase polymer having complementary reactive functional group. This application is not related to a two-part system but is a transfer resistant composition specially used in transfer resistant lipsticks, creams etc.

US6492455 describes the use of maleic anhydride co-polymers as film formers discloses the use of co-polymers with maleic anhydride functional groups and amine functional polymers as a heat cured coating within cosmetics. The use of maleated olefin copolymers as fixatives for personal care products such as hair sprays is disclosed in U.S. Patent No. 6,025,501 to Ulmer et al. U.S. Patent No. 6,706,817 discloses a bioadhesive resulting from a cross-linked maleic anhydride polymer gel. Multiple functionalized maleic anhydride/olefin co-polymers as enhanced film- forming agents are disclosed in PCT Application No. PCT/IT06/00661 to Rando et al. In each of the above- mentioned patents and patent applications, the maleic anhydride group is incorporated into the backbone of the polymer.

EP 1377621 disclosed Amino silicone containing amino groups in branch as well in alpha omega position. Therefore, such amino structure after reaction with organic epoxide or silicone epoxide have atleast two epoxy groups results vesicles or gels which is difficult to use in uniform hair coating for long lasting hair conditioner. EP 11625132 disclosed a highly cross linked silicone polymer emulsion is produced after make oil-in-water and water-in-oil emulsions and microemulsions containing elastometicsilanes or siloxanes having quaternary ammonium groups in their molecule as the oil phase of emulsion or microemulsion, comprosing reacting (i) an organic quaternary ammonium compound having epoxide groups or halohydrin groups in its molecule, with (ii) a silane or siloxane having amino groups in the molecule, in presence of (iii) a crosslinking agent and (IV), a surfactant, dispersed in (V) an aqueous polar phase resulting a cross linked polymer solution that is difficult to use in uniform hair coating for long lasting hair conditioner
US 7863397 disclosed a amino and/or ammoniopolysiloxanecomprising a reaction product of epoxy silicone, disocynate and organic amino compound resulting high molecular weight polymer and difficult to make semi-permanent coating on hair for long lasting hair conditioning effect. US 20100310491disclosed a personal care composition suitable for hair treatment comprising a composition of reaction product of oxirane or oxetane and amino silane. Hair treatment composition is an emulsion comprising a continuous phase which comprises the reaction product of oxirane or oxetane and amino silane and a discontinuous phase which comprises water or a non-aqueous hydroxylic solvent. Reacted product of oxirane or oxetane and amino silane is difficult to make a uniform homogeneous coating on hair surface and resulting no anchoring of silicone molecule in the hair cuticle due to increase in molecular weight.
Reference is invited to parent co-pending patent application no. 158/KOL/2011 dt. 04.02.2011disclosing a hair conditioning kit comprising selective silicone actives based hair conditioning formulation atleast in two parts adapted to favour achieving the desired lasting conditioning effect on the hair and maintain lively hair for a longer period of time involving formulations of selective organopolysiloxanes adapted to enter in thehair cortex and then react with each other to in-situ generate ~CH(OH)-CH2-NH–CH2~ linkage at the a, ? position of the resulting organopolysiloxane molecule enabling viscosity of at least 100 mPa.s at 25 oCto favour entrapment within the hair cortex for a longer time even after consecutive hair wash cycles.
Therefore, there is still a strong need in the art for a hair conditioning composition/kit to achieve a long lasting effect of hair conditioning whereby the conditioner would get retained on the hair even after number of hair washing cycles to favour proper conditioning and lively hair. Furthermore, such long lasting hair conditioning composition/ kit could also substantially reduce silicone wastage in rinsed water and to have minimum impact on the environment, render rinse waste water treatment in waste water treatment plant more facile and help recycling huge amount of rinse water.

OBJECTS OF THE INVENTION
It is thus the basic object of the present invention to provide for a long lasting hair conditioning formulation which could favour entry of reactive silicones in the hair cortex through hair cuticles to generate reacted high viscosity polymer which could then be retained in the narrow passage between the hair cuticles for a longer time on hair surface even after number of hair wash and thus keep the hair more lively for a longer duration.

Another object of the present invention is to provide for a hair conditioning composition/agent/ kit comprising formulation involving reactive organopolysiloxane molecules in association with a solvent adapted to favour long lasting conditioning effect on the hair by getting retained on the hair after several wash cycles.

Another object of the present invention is to provide for a hair conditioning formulation comprising reactive organopolysiloxane molecules in association with organic solvents that would react in-situ on the cortex of the hair to generate desired high viscosity organopolysiloxane polymer and further achieve good spread ability thereof with low surface tension of the said solvent to favour effective spreading on the hair surface and a long lasting conditioning effect.

Another object of the present invention is to provide for a process of conditioning the hair by employing the said hair conditioning composition/agent/ kit favouring long lasting and consistent conditioning effect on the hair after multiple hair wash cycles and at the same time avoiding any negative sensory effect.

Yet another object of the present invention is to provide for a hair conditioning formulation that would uniformly spread on the hair surface when applied in small amounts with the provision of penetrating inside the hair cuticle when applied in said small amounts.

Another object of the present invention is to provide for a hair conditioning formulation adapted to favour molecular growth involving reaction of reactive organopolysiloxanes inside the hair cuticles when applied in small amounts as oil.

Yet another object of the present invention is to provide for a hair conditioning formulation favouring generating of the selective conditioning silicone molecule of size big enough that too to be formed within the cuticle of the hair which would be difficult to rinse off from the hair surface cuticle even after consecutive hair wash cycles due to its big molecular size and being entrapped inside the cuticle of the hair.

Still another object of the present invention is to provide for a hair conditioning composition/ kit that would favour minimal loss of organopolysiloxane conditioner molecule in rinse water during hair washing.

Yet further object of the present invention is directed to not only save unnecessary organopolysiloxane drainage in rinse water but also help for the rinse waste water treatment more easy in waste water treatment plant and thus directed not only to keep the hair more lively for longer time but also help to recycle the huge amount of rinse water as a part of responsible care.

SUMMARY OF THE INVENTION
Thus according to the basic aspect of the present invention there is provided a kit comprising silicone active based hair conditioning formulation atleast in two parts comprising

(A) first part of the hair conditioning formulation comprising 1 to 50% of a reactive organopolysiloxane of structure (i)

………………….(i)

where, Z is the carbinol group having functionality like –CpH2p-OA; where p is an integer selected from 0 to 20 and A is either Hydrogen or an alkyl group,
m is from 0 to 5000, n is from 1 to 5000,
R’ is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group; and
an organic solventwherein the reactive organopolysiloxane of structure (i) is clearly soluble in the solvent;
(B) Second part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (ii)

…………………….(ii)

where, Y is the anhydride group and not limited to the said functionalities,
R" is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group,
b is atleast 10 and a is more than or equal to 0; and
an organic solvent, wherein the reactive organopolysiloxane of structure (ii) is clearly soluble in the organic solvent.

Preferably said kit comprising silicone active based hair conditioning formulation comprising directions of use for application of said first and second part of the hair conditioning formulation for in-situ generation of resulting hair conditioning organopolysiloxane molecule within the hair cortex and remain entrapped for a longer time even after consecutive hair wash cycles.

According to another preferred aspect of the present invention there is provided said kit comprising silicone active based hair conditioning formulation wherein said first and second part of the hair conditioning formulation are adapted to first enter in the hair cortex and then react with each other to in-situ generate ~CH2-CO-O–CH2~ linkage at the a, ? position of the resulting organopolysiloxane molecule of high viscosity of at least 100 mPa. s at 25 oC to favour entrapment within the hair cortex for a longer time even after consecutive hair wash cycles.

More preferably, is said kit comprising silicone active based hair conditioning formulation said solvent in said formulation is selected to make a clear solution of the reactive organopolysiloxanes and toprovide low surface tension of uptoabout 25 dynes/sec more preferably upto 20 dynes/sec to favour effective uniform spreading of the actives (A) and (B) on hair surface when applied in small amounts for initiation of the in-situ reaction. The surface tension of any liquid sample by using DCAT instrument. For surface tension measurement the liquid sample is taken in the Petri dish provided alongwith the machine. Attach the Wilhelmy plate at the holder, and the surface tension value is displayed by the instrument in dyne per second and no calculations are needed.

According to another preferred aspect of the present invention there is provided a kit comprising silicone active based hair conditioning formulation wherein said organic solvent is selected from cyclomethicone or mixtures thereof, short chain volatiles selected from trimethylsiloxy terminated polydimethylsiloxane (dimethicone), short chain alkanes or mixtures thereof.

According to yet another preferred aspect of the present invention there is provided said kit comprising silicone active based hair conditioning formulation wherein said ingredient (A) of organopolysiloxane of structure (i) preferably has n= 3 and A as hydrogen wherein said ingredient (B) has the functionality Y preferably derived of succinic anhydride.

According to another aspect of the present invention a method of hair conditioning is provided involving
(A) first part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (i)

………………….(i)

where, Z is the carbinol group having functionality like –CpH2p-OA; where p is an integer selected from 0 to 20 and A is either Hydrogen or an alkyl group,
m is from 0 to 5000, n is from 1 to 5000,
R’ is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group; and
an organic solvent wherein the reactive organopolysiloxane of structure (i) is clearly soluble in the solvent;

(B) Second part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (ii)

…………………….(ii)

where, Y is the anhydride group and not limited to the said functionalities,
R" is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group,
b is atleast 10 and a is more than or equal to 0; and
the organic solvent, wherein the reactive organopolysiloxane of structure (ii) is clearly soluble in the organic solvent, comprising the steps of:
(a) applying said first and second part of the hair conditioning formulation to hair to be conditioned in combination or individually one after the otherin the presence of a catalyst to initiate the reaction between carbinol silicone and anhydride silicone; and
(b) allowing the said first and second part of the hair conditioning formulation to enter the hair cortex for in-situ generation of resulting hair conditioning organopolysiloxane molecule within the hair cortex to thereby remain entrapped for desired conditioning even after several wash cycles.

Preferably in said method of hair conditioning said first part of the hair conditioning formulation (A) involving reactive organopolysiloxane of structure (i) that is hydroxyl silicone polymer of a,? hydroxy propyl polydimethylsiloxane is obtained by reacting hydrogen siloxane containing polymer with allyl alcohol; and
wherein said second part of the hair conditioning formulation (B) involving reactive organopolysiloxane of structure (ii) is a a,? anhydride polydimethylsiloxane obtained by reacting hydrogen siloxanecontaining polymer with allyl succinic anhydride.

According to another preferred aspect of the present invention there is provided said method of hair conditioning comprising the steps of:
(I) intimately mixing with carbinol silicone solution (A) with anhydride silicone solution (B) in a selective ratio range preferably in the range of 10:90 to 90:10;
(II) applying the said mix on the hair ensuring entire coverage of the hair with the solution (A) and (B);
(III) leaving the hair with the said mix at ambient temperature for atleast 5 minutes for favouring the entry of carbinol silicones and anhydride silicones in the cortex of the hair to in-situ react and yield a high viscosity organopolysiloxane polymer involving ~CH2-CO-O–CH2~ linkage of viscosity of at least 100 mPa.s at 25 oC adapted for conditioning the hair having lasting conditioning effect over several consecutive wash cycles.

Preferably said method of hair conditioning is provided wherein
step (I) involving intimately mixing carbinol silicone solution (a) with anhydride silicone solution (b) is preferably done at the selective ratio range of 50:50;
step (III) involving leaving the hair with said mix of carbinol silicone (A) and anhydride silicone solution (B) at ambient temperature is preferably left for 15-30 minutes for favouring the entry of carbinol silicone and anhydridesilicones in the cortex of the hair to react with each other in-situ adapted to form hydrophobic silicone coating on hair.

More preferably in said method of hair conditioning said step (II) of applying said mix on the hair ensuring entire coverage of the hair involves application ofcarbinol silicone solution (A) and anhydride silicone solution (B) at the levels of upto10 gm per 100 gm of hair wherein preferably atleast 1% of carbinol silicone solution (A) and atleast 1% of anhydride silicone solution (B) are applied on 100 gram of clean hair to favour optimum hydrophobic coating on hair having lasting effect over several consecutive wash cycles.

According to yet another preferred aspect of the present invention there is provided said method of hair conditioning wherein the catalyst is selected from basic catalysts including triethanolamine to initiate the reaction between that carbinol silicone and anhydride silicone in basic condition at room temperature of 25 ?C.

BRIEF DESCRIPTION OF FIGURES

Figure 1: illustrates SEM images for hair treated with the anhydride/ carbinol silicone system a) After zero wash, b) after ten washes;

DETAILED DESCRIPTION OF THE INVENTION
As discussed hereinbefore the present invention provides for the desired conditioning kit/formulation/actives that imparts improved and long lasting conditioning effect by way of reactive silicones with solvent/s entering in the hair cortex through hair cuticles to get entrapped in hair cortex due to selective increase of polymer chain by addition / condensation reaction of the silicone polymers and retained in the narrow passage between the hair cuticles for a longer time on hair surface even after number of hair wash and thus keep the hair more lively for a longer duration due to longer retaining hydrophobic silicone coating on hair surface

According to an aspect of the present invention, there is provided a hydrophobic hair treatment composition/agent comprising silicone formulation wherein the said long lasting hydrophobic treatment on hair would favour generating selective highly viscous organopolysiloxane molecule involving ~ CH2-CO-O–CH2~ linkage.

According to another aspect of the present invention there is provided a hair conditioning composition/ agent comprising hair conditioning formulation of reactive organopolysiloxanes in two parts based on different solvent medium comprising
(A) first part of the hair conditioning formulation comprising 1 to 50% of a reactive organopolysiloxane of structure (i)

………………….(i)

where, Z is the carbinol group having functionality like –CpH2p-OA; where p is an integer selected from 0 to 20 and A is either Hydrogen or an alkyl group,
m is from 0 to 5000, n is from 1 to 5000,
R’ is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group; and
an organic solventwherein the reactive organopolysiloxane of structure (i) is clearly soluble in the solvent;
The preferred method of preparing this type of reactive hydroxyl silicone polymer is by the reaction of hydrogensiloxane (H-siloxane) containing polymer with allyl alcohol to obtain organopolysiloxane of structure (i). The organopolysiloxane of structure (i) which is a a,?hydroxy propyl polydimethylsiloxane.

(B) Second part of the hair conditioning formulation comprising:
1 to 50% of a reactive organopolysiloxane of structure (ii)

…………………….(ii)

where,Y is the anhydride group and not limited to the said functionalities,
R" is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group,
b is atleast 10 and a is more than or equal to 0; and
an organic solvent, wherein the reactive organopolysiloxane of structure (ii) is clearly soluble in the organic solvent.

The reactive organopolysiloxane of structure (ii) which is a a, ? anhydride polydimethylsiloxane, which is a reaction product of hydrogen siloxane (H-siloxane) with allyl succinic anhydride.

According to another aspect of the present invention there is provided a hair hydrophobic treatement kit comprising ingredients
(a) less than 50 % reactive organopolysiloxane of structure (i)

……………………….(i)

where, Z is the carbinol group having functionality like –CpH2p-OA; where p is an integer selected from 0 to 20 and A is either Hydrogen or an alkyl group,
m is from 0 to 5000, n is from 1 to 5000,
R’ is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group; and
an organic solventwherein the reactive organopolysiloxane of structure (i) is clearly soluble in the solvent;
(b) less than 50 % reactive organopolysiloxane of structure (ii)

…………………………….(ii)

where, Y is the anhydride group and not limited to the said functionalities,
R" is monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably similar to R or different in carbon number,
R is the monofunctional, saturated or unsaturated alkyl group with 1 to 20 carbon atoms or monofunctional aryl group with 6 to 20 carbon atoms, most preferably methyl group,
b is atleast 10 and a is more than or equal to 0; and
an organic solvent, wherein the reactive organopolysiloxane of structure (ii) is clearly soluble in the organic solvent wherein the said organic solvent can be cyclomethicone or mixtures thereof or short chain volatiles trimethylsiloxy terminated polydimethylsiloxane (dimethicone) or short chain alkanes in which structure (ii) is clearly soluble,
(c) providing for directions of use for achieving effective hair hydrophobic hair treatment involving the formulation comprising ingredients (a) and (b).

The viscosity of the fluids, its mixture and the emulsion prepared by the fluid is measured at 25ºC by Anton PaarRheometer; model MCR101, geometry single gap cylinder: CC27 spindle and shear rate 1 s-1 for 2 minutes at 250C is used for measuring viscosity at 25ºC. Three measurements are made for each sample and the viscosity value is taken at 60 secs. A MCR Rheometer Series product works as per USP (US Pharmacopeia Convention) 912 – Rotational Rheometer methods.

According to yet another aspect of the present invention there is provided a method of silicone hydrophobic coating on hair involving the above said composition/ kit comprising the steps of:
(I) intimately mixing anhydride silicone solution (a) with carbinol silicone solution (b) in a selective ratio range preferably in the range of 10:90 to 90:10; most preferably 50:50 ratio. Each component of silicone solution (a) & (b) is applied as high as 10 gm per 100 gm hair and quantity of hair solution (a) & (b) always greater than zero. Most preferably, less than 7% of anhydride silicone solution (a) and less than 7% carbinol silicone (b) applied after mixing of two component on 100% gram clean hair results optimum long lasting hydrophibic coating on hair
(II) applying the said mix on the hair ensuring entire coverage of the hair with the solution (a) and (b);
(III) leaving the hair with the said mix at ambient temperature for atleast 5 minutes for favouring the entry of anhydride silicones and carbinol silicones in the cortex of the hair to react and yield a high viscosity polymer involving ~CH2-CO-O–CH2~ linkage adapted for conditioning the hair having lasting effect over several consecutive wash cycles. Preferably, leaving the hair with said mix (mixture of anhydride silicone (a) & carbinolsilicone (b) at ambient temperature for 15-30 minutes for favouring the entry of anhydride silicones and carbinol silicones in the cortex of the hair to react.

According to a preferred aspect of the present invention there is provided for a hair coating composition/ agent comprising long lasting hair hydrophobic treatment formulation wherein in the said formulation the solvent is selectively provided to benefit effective high spreading on the hair surface having low surface tension below or equivalent to 25 dynes/sec. Most preferably, surface tension of the solvent is below 20 dynes/sec.

According to another preferred aspect of the present invention there is provided a hair hydrophobic coating composition/ agent on hair comprising silicone formulation wherein the reactive organopolysiloxanes in the said formulation are selectively provided to react with each other at ambient condition.

According to yet another preferred aspect of the present invention there is provided a hair coating composition/ agent comprising silicone formulation wherein the solvents including the reactive organopolysiloxane make a clear solution (i.e. silicones are soluble in solvent) and surface tension of the solution (solvent&silicones) is below 25 dynes/cm and optimally below 20 dynes/cm so that solution spread uniformly on hair surface when applied in small amounts.

According to an embodiment of the present invention, the same involves mixing of a 1st part of anhydride silicone solution with 2nd part of carbinol silicone in the ratio of 10:90 to 90:10. The said mix solution of atleast 0.1 gm per gm of hair is then applied properly so that all hair surface is coated with the oil i.e. mix solution of anhydride silicone solution and carbinol silicone solution. The hair is allowed to stay in this condition at ambient condition for atleast 15 min. During this time, mixed oil with reactive silicones are found to enter in the hair cortex through hair cuticles and both the silicones i.e. anhydride silicone &carbinol silicone after mixing gets reacted in solvent medium to form ~CH2-CO-O–CH2~linkage inside the cortex and to yield a high viscosity polymer. After completion of reaction, the polymer molecular weight was found to become high enough which did not allow polymer to return back from the narrow passage between the cuticles. Therefore high molecular weight silicone polymer could thus get retained on the surface by way of being entrapped inside cuticle for longer time till the passage in between the cuticles become big enough to allow the polymer to come out from inside the cuticles.
Therefore, according to an embodiment of the present invention, the same favoured the desired in-situ formation of the silicone polymer involving ~CH2-CO-O–CH2~ linkage which could get retained for longer time on hair surface even after number of hair wash to keep hair more lively.
The triethanol amine or any other basic catalystacts as a catalyst to initiate the reaction between that alcohol group of carbinol and anhydride in basic condition at room temperature of 25 oC.

The present invention is described hereunder in greater details in relation to the following non-limiting exemplary illustrations and Figures:

Example 1:In accordance with the present invention (anhydride silicone and carbinol silicone system)
Two part system:
1) Part A system:
a,? anhydride polydimethylsiloxaneand C13-C15 alkane(from total petrochemical,France)
2) Part B system:
a,?hydroxy propyl polydimethylsiloxaneand C13-C15 alkane and small amount of pure triethanol amine (available from Sigma Aldrich)

Table 1: Components in accordance with the presentinvention(anhydride silicone and carbinol silicone system)
Component A
INGREDIENTS % QTY
a,? anhydride polydimethylsiloxane 20
GEMSEAL 25(INCI C-13-15 Alkane) 80
100
Component B
INGREDIENTS % QTY
a,?hydroxy propyl polydimethylsiloxane 19.6
Triiethanolamine 0.4
GEMSEAL 25(INCI C-13-15 Alkane) 80
100

On mixing Component A and Component B the colour turns yellow first then becomes hazy and on further stirring becomes clear transparent. On mixing the viscosity is 992 mPa.s at 25 oC and after 35 minutes at 25oC the viscosity becomes 2400 mPa.s at 25 oC.

Example 3: Application process
Take 2.4 gmof hair swatch (Indian Hair), and then weigh 0.036 gm of component A and 0.036 gm of component B in a small Petridish both from Table 1 of current invention. The two components weighed in the petridish are mixed completely with fingers and silicone mixture is formed. The silicone mixture is applied on the hair entirely along the length for 1 minute.The hair swatch is hanged for 25 minutes. After 25 minutes some portion of this treated hair is kept aside.Rest hair is taken for shampoo wash. The hair swatch portion taken for shampoo wash is weighed and then wetted under tap water with a water flow rate of 50 ml/sec for 10 sec. Apply @ 0.1 gm blank shampoo as in Table 3 (0.2% JC13S base) per gram of hair.Apply for 60 secs and hold it for 60 secs. Then wash the hair for with water for 30 sec for two times with defined water flow rate of 50 ml/s and dry the hair under room temperature.
Washing is done for 10 times. Remove small quantity of hair tresses each time from the bunch after 1st wash, 5th wash, 10th wash.
Measure the silicone deposition of unwashed hair sample, hair from 1st wash, 5th wash & 10th wash.
Table 3: Shampoo Composition
Serial No Ingredients Quantity(wt%)
a Demineralised water 25.47
* 4% Carbopol 980 slurry 10.34

b Sodium Lauryl ether sulphate 40.98
Cocoamidopropylbetaine 4.31

c Ethylene glycol mono stearate 0.98
PEG - 45 0.025

d Jaguar C13S (Guar Hydroxylpropyltrimonium chloride) 0.2
Glycerine 0.98

e 50% Sodium hydroxide solution 0.049
Demineralised water 7.09
? Pearliser 0.98

f Cosmetic grade mica 0.147

g 50% Sodium hydroxide solution 0.31
Demineralised water 0.31

h Glydant (DMDM Hydantoin ) 0.098
Kathon CG 0.021
Disodium EDTA 0.049

i Perfume 0.049

j 15% Sodium chloride solution 1.66

Example 4: Silicone Deposition on Hair post application process
Silicone deposition is measured by Spectrophotometer of manufacturer-Spectro,Model- Xepos
Supplier-Ametek Materials Analysis Division in parts per million of weight of hair.
Table 4: Silicone deposition
Anhydride/carbinol silicone system (ppm)
Zero wash 7200
5 washes 4600
10 washes 3900

Example 5: Evaluation of hair’s surface coating by Scanning Electron Microscopy (SEM) after the application process

It can be thus clearly concluded from the deposition test results of Table 4 above and SEM results of Figure 1 that the anhydride/ carbinol silicone system of the present invention (Figure 1: SEM images for hair treated with the anhydride/ carbinol silicone systema) After zero washb)after ten washes)is not only effective in keeping the hair more lively for a longer duration of time due to longer retention of hydrophobic silicone coating on hair surface, the same is also found to impart improved conditioning as far as the long lasting conditioning effect after several was cycles are concerned.

It is thus possible by way of the present invention to provide for a hair conditioning kit comprising selective silicone actives based hair conditioning formulation atleast in two parts adapted to favour achieving the desired lasting conditioning effect on the hair and maintains lively hair for a longer period of time involving formulations of selective organopolysiloxane molecules as discussed hereinbefore. Advantageously, the present invention provides for long lasting conditioning formulations and method of hair conditioning such as to in-situ generate desired high viscosity silicone polymer involving ~CH2-CO-O–CH2~ linkage at the a, ? position of the resulting organopolysiloxanepolymermolecule of high viscosity of at least 100 mPa.s at 25 oCand higher molecular weighttofavour its entrapment and retention within the hair cortex for a longer period of time suitably adapted for conditioning the hair to keep it lively even after consecutive washes thereby providing lasting conditioning effect over several consecutive wash cycles by favourably avoiding any negative sensory effect.