COMPOSITIONS AND PROCESSES FOR TREATMENT OF KERATINOUS SUBSTRATES

A synergistic network of alkali carbonates and polyols in compositions addresses the issue of short-lived hydration in keratinous substrates, achieving durable moisture retention and improved cosmetic benefits.

FR3145478B1Active Publication Date: 2026-02-13LOREAL SA
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Patent Information

Application Number
FR2023001019
Authority / Receiving Office
FR · FR
Patent Type
Patents
Current Assignee / Owner
Filing Date
2023-02-03
Publication Date
2026-02-13
Estimated Expiration
2043-02-03

AI Technical Summary

Technical Problem

Current products fail to provide long-lasting hydration and moisturization to keratinous substrates like skin and hair, as humectants on the surface are easily removed, leading to moisture imbalance and dryness.

Method used

A synergistic combination of alkali carbonates and polyols forms an associated network within compositions, enhancing moisture penetration and retention in keratinous substrates.

Benefits of technology

The compositions significantly increase and maintain moisture content in keratinous substrates, providing long-lasting hydration and improved cosmetic benefits without a greasy feel.

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Abstract

Compositions and Processes for Treating Keratinous Substrates: The disclosure relates to compositions and processes for treating keratinous substrates, such as skin and / or hair, where the compositions comprise (a) at least one alkali carbonate, (b) at least one polyol, (c) water and / or at least one non-aqueous solvent, and (d) optionally at least one pH adjuster. The at least one carbonate and the at least one polyol are present in the composition as an associated network. Figure for the abstract: none
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Description

Title of the invention: COMPOSITIONS AND METHODS FOR TREATMENT OF KERATINOUS SUBSTRATES technical field

[0001] This disclosure relates to compositions and processes for treating keratinous substrates, such as skin or hair. BACKGROUND

[0002] Consumers wish to improve the appearance and / or feel of their skin and / or hair. For example, people with dry skin or hair may want to moisturize and / or hydrate their skin or hair to improve its appearance and feel. Attributes desired by consumers include, for example, deep and lasting hydration and / or moisturization without a greasy feel. Furthermore, improved conditioning or long-lasting cosmetic benefits are also desired.

[0003] Current products and technologies aim to hydrate and / or moisturize the skin and hair by superficially coating the surface with humectants and / or oils. The humectants remain on the surface of the skin or hair, acting as a conduit between the skin or hair and the external environment. However, while the objective is to increase the moisture content of the skin or hair, the opposite effect, such as dry skin or dry, frizzy hair, can often occur due to an imbalance of water between the skin or hair fibers and the external environment. Furthermore, the superficial coating can be easily removed by rinsing or washing, so long-term hydration and its associated benefits are not achieved.

[0004] The present inventors have now discovered, in an astonishing way, a synergistic combination of ingredients which unexpectedly provides excellent hydration to keratinous substrates such as skin and hair, the benefits of which are long-lasting. SUMMARY

[0005] It has been discovered in an astonishing and unexpected manner that the compositions and processes according to the disclosure can increase and / or improve the moisture content of keratinous substrates, can reduce the moisture loss of keratinous substrates and / or can offer beneficial cosmetic properties to keratinous substrates.

[0006] In various embodiments, the disclosure relates to compositions for the treatment of keratinous substrates, such as skin and / or hair, compositions comprising (a) at least one alkali carbonate, (b) at least one polyol, (c) water and / or at least one non-aqueous solvent, and (d) optionally at least one pH adjuster, wherein at least one alkali carbonate and at least one polyol are present in the composition in the form of an associated network. In various embodiments, the molar ratio of alkali carbonate(s) to polyol(s) in the composition and / or network ranges from less than 1:3 to about 1:50, for example from about 1:4 to about 1:20, preferably from about 1:5 to about 1:15, more preferably from about 1:7 to about 1:13, more preferably still from about 1:9 to about 1:11, or is most preferably about 1:10.

[0007] Optionally, at least one alkali carbonate may be selected from sodium carbonate, calcium carbonate, potassium carbonate, magnesium carbonate, lithium carbonate, sodium bicarbonate, potassium bicarbonate, or combinations of two or more of these. For example, in one embodiment, potassium carbonate is selected. In various embodiments, the total amount of alkali carbonates and / or associated network may range from approximately 0.1% to approximately 10%, preferably from approximately 0.25% to approximately 8%, more preferably from approximately 0.5% to approximately 6%, more preferably still from approximately 0.75% to approximately 4%, most preferably from approximately 1% to approximately 1.5% by weight, relative to the total weight of the composition.

[0008] Optionally, at least one polyol may have a molar mass less than approximately 500 g / mol, preferably less than approximately 400 g / mol, more preferably less than approximately 300 g / mol, more preferably still less than approximately 200 g / mol, and most preferably less than approximately 150 g / mol. For example, in one embodiment, glycerol is chosen. In various embodiments, the total amount of polyols and / or associated network ranges from approximately 1% to approximately 25%, preferably from approximately 2% to approximately 18%, more preferably from approximately 3% to approximately 15%, more preferably from approximately 4% to approximately 13%, and most preferably from approximately 5% to approximately 11% by weight, relative to the total weight of the composition.

[0009] In various embodiments, the compositions comprise (a) at least one alkali carbonate, preferably including potassium carbonate, (b) at least one polyol, preferably including glycerol, (c) water, and (d) at least one pH adjuster, wherein the at least one alkali carbonate and the at least one polyol are present in the composition in the form of an associated network, and the molar ratio of the alkali carbonate(s) to the polyol(s) in the network ranges from about 1:4 to about 1:20, such as from about 1:5 to about 1:15, preferably from about 1:7 to about 1:13, more preferably from about 1:9 to about 1:11, or most preferably from about 1:10.

[0010] The disclosure also relates to processes for treating ke- substrates For keratinous substrates such as skin and / or hair, the composition as disclosed may be applied, for example, by increasing the moisture content of the keratinous substrates. In some embodiments, a composition as disclosed may be applied to the keratinous substrate, optionally left on the keratinous substrate for a period ranging from approximately 30 seconds to approximately 48 hours, preferably from approximately 1 minute to approximately 24 hours, more preferably from approximately 5 minutes to approximately 12 hours, most preferably from approximately 10 minutes to approximately 9 hours, and optionally the removal of the composition after the application period, for example, by rinsing or wiping the keratinous substrates. The keratinous substrates may optionally be cleaned after the application period.For example, in an embodiment where the keratinous substrates are keratinous fibers such as hair, the hair can be cleaned with shampoo after the application period.

[0011] The disclosure also relates to a simplex solution comprising (a) at least one alkali carbonate, (b) at least one polyol, and (c) optionally water, wherein the at least one alkali carbonate and the at least one polyol are present in the simplex solution in the form of an associated network. In some embodiments, the molar ratio of alkali carbonate(s) to polyol(s) in the simplex solution ranges from less than 1:3 to about 1:50, for example, from about 1:4 to about 1:20, such as from about 1:5 to about 1:15, preferably from about 1:7 to about 1:13, more preferably from about 1:9 to about 1:11, or most preferably about 1:10.In some embodiments where the simplex solution includes water, the molar ratio of alkali carbonate(s) to water in the simplex solution ranges from about 1:10 to about 10:1, preferably from about 5:1 to about 1:5, more preferably from about 3:1 to about 1:3, more preferably still from about 2:1 to about 1:2, or most preferably is about 1:1. In some embodiments, at least one alkali carbonate is selected from sodium carbonate, calcium carbonate, potassium carbonate, magnesium carbonate, lithium carbonate, sodium bicarbonate, potassium bicarbonate, or combinations of two or more of these, and preferably includes potassium carbonate.In some embodiments, at least one polyol has a molar mass of less than about 500 g / mol, preferably less than about 400 g / mol, more preferably less than about 300 g / mol, more preferably still less than about 200 g / mol, most preferably less than about 150 g / mol, and preferably comprises glycerol.

[0012] In various embodiments, the simplex solutions comprise (a) at least one alkali carbonate, preferably including potassium carbonate, (b) at least one polyol, preferably including glycerol, and (c) optionally water, and the ratio molar of alkali carbonate(s) on polyol(s) ranges from about 1:4 to about 1:20, such as from about 1:5 to about 1:15, preferably from about 1:7 to about 1:13, more preferably from about 1:9 to about 1:11, or most preferably is about 1:10.

[0013] The disclosure also relates to processes for preparing compositions for treating keratinous substrates, the processes comprising (i) preparing a simplex solution by combining at least one alkali carbonate, at least one polyol, and optionally water, wherein the molar ratio of alkali carbonate(s) to polyol(s) in the simplex solution ranges from less than 1:3 to about 1:50, for example from about 1:4 to about 1:20, preferably from about 1:5 to about 1:15, more preferably from about 1:7 to about 1:13, most preferably from about 1:9 to about 1:11, to form an associated network of alkali carbonate(s) and polyol(s); (ii) optionally heating the simplex solution; (iii) the addition of at least one solvent selected from water and / or non-aqueous solvents to the simplex solution to form the composition; and (iv) the optional addition of at least one pH corrector to the composition.The processes in some embodiments include heating the simplex solution in (ii) to a temperature from about 35 °C to about 100 °C, preferably from about 50 °C to about 100 °C, most preferably from about 75 °C to about 90 °C, and subsequently cooling the simplex solution. The processes in some embodiments include adding at least one pH adjuster to the composition to achieve a pH from about 7 to about 14, such as from about 7 to about 11, preferably from about 7.5 to about 10.5, more preferably from about 8 to about 10. The processes in some embodiments include adding at least one additional component selected from the active agents and auxiliary components to the composition.The disclosure also relates to keratinous substrate treatment compositions prepared by the processes, as well as processes for treating keratinous substrates with compositions prepared by the processes. DETAILED DESCRIPTION

[0014] The disclosure relates to compositions and processes for treating keratinous substrates, such as skin and hair. The compositions and processes disclosed provide increased moisture and moisture retention to the keratinous substrates, which has proven surprisingly and unexpectedly durable. The disclosure also relates to manufacturing processes for the compositions. I. COMPOSITIONS

[0015] The compositions according to this disclosure comprise (a) at least one alkali carbonate, (b) at least one polyol, (c) water and / or at least one non-alkali solvent aqueous, and (d) optionally at least one pH adjuster. Compositions may optionally include at least one active agent and / or at least one auxiliary component.

[0016] The alkali carbonate(s) and polyol(s) are present in the composition as an associated network, and therefore, the compositions comprise an associated network of alkali carbonate(s) and polyol(s). As used herein, the terms "network" and "associated network" are used interchangeably to signify that the components in the composition are associated with one another rather than being present in the composition separately. The association of components in a network may be chemical or physical. For example, the components may be hydrogen-bonded to one another. However, it should be understood that the compositions according to the disclosure may also include one or more of the network components when that component or those components are not part of the network.For example, compositions may include one or more networks of alkali carbonate(s) and polyol(s), and compositions may include one or more alkali carbonates and / or polyols separated from the network(s). Alkaline carbonates

[0017] The compositions according to the disclosure comprise at least one alkali carbonate. In some embodiments, the compositions and / or the associated network may comprise more than one alkali carbonate, for example at least two alkali carbonates, at least three alkali carbonates, etc.

[0018] In various embodiments, at least one alkali carbonate may be selected from alkali carbonates, alkali bicarbonates, or combinations thereof. For example, alkali carbonates may be selected from sodium carbonate, calcium carbonate, potassium carbonate, magnesium carbonate, lithium carbonate, or combinations of two or more of these. Alkaline bicarbonates may, for example, be selected from sodium bicarbonate, potassium bicarbonate, or combinations thereof. In preferred embodiments, the alkali carbonate comprises, consists essentially of, or consists of potassium carbonate.

[0019] In various embodiments, the total amount of alkali carbonates in the composition and / or in the associated network ranges from approximately 0.1% to approximately 10%, as from approximately 0.1% to approximately 9%, from approximately 0.1% to approximately 8%, from approximately 0.1% to approximately 7%, from approximately 0.1% to approximately 6%, from approximately 0.1% to approximately 5%, from approximately 0.1% to approximately 4%, from approximately 0.1% to approximately 3%, from approximately 0.1% to approximately 2.5%, from approximately 0.1% to approximately 2%, from approximately 0.1% to approximately 1.5%, from approximately 0.25% to approximately 10%, from approximately 0.25% to approximately 9%, from approximately 0.25% to approximately 8%, from approximately 0.25% to approximately 7%, from approximately 0.25% to approximately 6%, from approximately 0.25% to approximately 5%, from approximately 0.25% to approximately 4%, from approximately 0.25% to approximately 3%, from approximately 0.25% to approximately 2.5%, from approximately 0.25% to approximately 2%, from approximately 0.25% to approximately 1.5%, from approximately 0.5% to approximately 10%, from approximately 0.5% to approximately 9%, from approximately 0.5% to approximately 8%, from approximately 0.5% to approximately 7%, from approximately 0.5% to approximately 6%, from approximately 0.5% to approximately 5%, from approximately 0.5% to approximately 4%, from approximately 0.5% to approximately 3%, from approximately 0.5% to approximately 2.5%, from approximately 0.5% to approximately 2%, from approximately 0.5% to approximately 1.5%, from approximately 0.75% to approximately 10%, from approximately 0.75% to approximately 9%, from approximately 0.75% to approximately 8%, from approximately 0.75% to approximately 7%, from approximately 0.75% to approximately 6%, from approximately 0.75% to approximately 5%, from approximately 0.75% to approximately 4%, from approximately 0.75% to approximately 3%, from approximately 0.75% to approximately 2.5%, from approximately 0.75% to approximately 2%, from approximately 0.75% to approximately 1.5%, from approximately 1% to approximately 10%, from approximately 1% to approximately 9%, from approximately 1% to approximately 8%, from approximately 1% to approximately 7%from about 1% to about 6%, from about 1% to about 5%, from about 1% to about 4%, from about 1% to about 3%, from about 1% to about 2.5%, from about 1% to about 2%, from about 1% to about 1.5%, from about 1.25% to about 10%, from about 1.25% to about 9%, from about 1.25% to about 8%, from about 1.25% to about 7%, from about 1.25% to about 6%, from about 1.25% to about 5%, from about 1.25% to about 4%, from about 1.25% to about 3%, from about 1.25% to about 2.5%, from about 1.25% to about 2%, or from about 1.25% to about 1.5% by weight, relative to total weight of the composition. In some embodiments, the total amount of alkali carbonates in the composition and / or in the associated network ranges from approximately 0.2% to approximately 2.5%, from approximately 0.3% to approximately 2.4%, from approximately 0.4% to approximately 2.3%, from approximately 0.5% to approximately 2.2%, from approximately 0.6% to approximately 2.1%, from approximately 0.7% to approximately 2%, from approximately 0.8% to approximately 1.9%, from approximately 0.9% to approximately 1.8%, approximately 1% to approximately 1.7%, approximately 1.1% to approximately 1.6%, relative to the total weight of the composition. In some preferred embodiments, the total amount of alkali carbonates in the composition and / or in the associated network may range from approximately 0.5% to approximately 2.5%, or from approximately 0.75% to approximately 1.75%, or from approximately 1% to approximately 1.5% by weight, relative to the total weight of the composition. Polyols

[0020] The compositions according to the disclosure comprise at least one polyol. In some embodiments, the compositions and / or the associated network may comprise more than one polyol, for example at least two polyols, at least three polyols, etc.

[0021] The term "polyol," as used here, refers to an organic molecule comprising at least two hydroxyl groups, such as, for example, at least three hydroxyl groups. In various embodiments, polyols may have from 2 to 32 carbon atoms, such as 3 to 16 carbon atoms, or 3 to 12 carbon atoms. Optionally, the polyols are chosen from alkane polyols. In some embodiments, the polyols are not chosen from sugar alcohols or their derivatives.

[0022] In various embodiments, the polyols that may be chosen include polyols with a molar mass less than about 500 g / mol, for example less than about 450 g / mol, less than about 400 g / mol, less than about 350 g / mol, less than about 300 g / mol, less than about 250 g / mol, less than about 200 g / mol, less than about 175 g / mol, less than about 150 g / mol, less than about 125 g / mol, or less than about 100 g / mol.

[0023] By way of example only, the polyols that may be selected include glycerol (glycerin), 1,2,6-hexanetriol, trimethylolpropane, ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, pentaethylene glycol, dipropylene glycol, 2-butene-1,4-diol, 2-ethyl-1,3-hexanediol, 2-methyl-2,4-pentanediol, caprylyl glycol, 1,2-hexanediol, 1,2-pentanediol, 4-methyl-1,2-pentanediol, or a mixture of two or more of these. In various embodiments, the solvent comprises, consists essentially of, or consists of glycerol.

[0024] In various embodiments, the total amount of polyols present in the composition and / or in the associated network ranges from approximately 1% to approximately 25%, as from approximately 1% to approximately 20%, from approximately 1% to approximately 15%, from approximately 1% to approximately 14%, from approximately 1% to approximately 13%, from approximately 1% to approximately 12%, from approximately 1% to approximately 11%, from approximately 1% to approximately 10%, from approximately 1% to approximately 9%, from approximately 1% to approximately 8%, from approximately 1% to approximately 7%, from approximately 1% to approximately 6%, from approximately 1% to approximately 5%, from approximately 2% to approximately 25%, from approximately 2% to approximately 20%, from approximately 2% to approximately 15%, from approximately 2% to approximately 14%, from approximately 2% to approximately 13%, from approximately 2% to approximately 12%, from approximately 2% to approximately 11%, from approximately 2% to approximately 10%, from approximately 2% to approximately 9%, from approximately 2% to approximately 7%, from approximately 2% to approximately 7%, from approximately 2% to approximately 6%, from approximately 2% to approximately 5%, from approximately 3% to approximately 5%, from approximately 3% to approximately 20%, from approximately 3% to approximately 15%from approximately 3% to approximately 14%, from approximately 3% to approximately 13%, from approximately 3% to approximately 12%, from approximately 3% to approximately 11%, from approximately 3% to approximately 10%, from approximately 3% to approximately 9%, from approximately 3% to approximately 8%, from approximately 3% to approximately 7%, from approximately 3% to approximately 6%, from approximately 3% to approximately 5%, from approximately 4% to approximately 25%, from approximately 4% to approximately 20%, from approximately 4% to approximately 15%, from approximately 4% to approximately 14%, from approximately 4% to approximately 13%, from approximately 4% to approximately 12%, from approximately 4% to approximately 11%, from approximately 4% to approximately 10%, from approximately 4% to approximately 9%, from approximately 4% to approximately 8%, from approximately 4% to approximately 7% from approximately 4% to , about 6%, from about 4% to about 5%, from about 5% to about 25%, from about 5% to about 20%, from about 5% to about 15%, from about 5% to about 14%, from about 5% to about 13%, from about 5% to about 12%, from about 5% to about 11%, from about 5% to about 10%, from about 5% to about 9%, from about 5% to about 8%, from about 5% to about 7% by weight, from about 5% to about 6% by weight, relative to the total weight of the composition. In some embodiments, the total amount of polyols in the composition and / or in the associated network ranges from about 5 to about 12%, such as from about 5.5% to about 11%, from about 6% to about 10%, from about 6.5% to about 9.5%, from about 7% to about 9%, or from about 8% to about 9% by weight, relative to the total weight of the composition.

[0025] In certain embodiments, it may be particularly advantageous to choose quantities of alkali carbonates and polyols such that the molar ratio of the alkali carbonate(s) to polyol(s) present in the composition and / or in the associated network is less than 1:3 and greater than approximately 1:50, for example, ranging from approximately 1:4 to approximately 1:50, from approximately 1:4 to approximately 1:45, from approximately 1:4 to approximately 1:40, from approximately 1:4 to approximately 1:35, from approximately 1:4 to approximately 1:30, from approximately 1:4 to approximately 1:25, from approximately 1:4 to approximately 1:20, from approximately 1:4 to approximately 1:15, from approximately 1:4 to approximately 1:10, from approximately 1:5 to approximately 1:50, from approximately 1:5 to about 1:45, from about 1:5 to about 1:40, from about 1:5 to about 1:35, from about 1:5 to about 1:30, from about 1:5 to about 1:25, from about 1:5 to about 1:20, from about 1:5 to about 1:15, or from about 1:5 to about 1:10.In some preferred embodiments, the molar ratio of alkali carbonate(s) to polyol(s) may range from about 1:4 to about 1:20, from about 1:5 to about 1:15, from about 1:7 to about 1:13, or from about 1:9 to about 1:11, for example a molar ratio of about 1:4, about 1:5, about 1:6, about 1:7, about 1:8, about 1:9, about 1:10, about 1:11, about 1:12, about 1:13, about 1:14, about 1:15, about 1:16, about 1:17, about 1:18, about 1:19, or about 1:20, or may be in a range having any of the above as upper and lower bounds. pH adjusters

[0026] The compositions according to this disclosure have a pH greater than 7, such as a pH in the range of approximately 7 to approximately 14, approximately 7 to approximately 13, approximately 7 to approximately 12, approximately 7 to approximately 11, approximately 7 to approximately 10, approximately 7 to approximately 9, approximately 7.5 to approximately 14, approximately 7.5 to approximately 13, approximately 7.5 to approximately 12, approximately 7.5 to approximately 11, approximately 7.5 to approximately 10, approximately 7.5 to approximately 9, approximately 7.5 to approximately 10.5, or approximately 8 to approximately 10. For example, the pH of the composition may be approximately 7.5, approximately 8, approximately 8.5, approximately 9, approximately 9.5, of about 10, about 10.5, about 11, about 11.5, about 12, about 12.5, about 13, about 13.5 or about 14, or may be in a A range having any of the above as upper and lower bounds. Accordingly, where appropriate, the compositions according to the disclosure may optionally include at least one pH adjuster. In various embodiments, the pH adjuster is chosen from compounds that can lower the pH of the composition, for example, commonly used inorganic or organic acids such as citric acid, lactic acid, maleic acid, malonic acid, hydrochloric acid, etc. Solvents

[0027] The compositions according to this disclosure comprise at least one solvent selected from water and / or non-aqueous solvents. In various embodiments, the compositions comprise water in an amount of at least 70% by weight, such as from about 60% to about 98%, from about 70% to about 95%, or from about 80% to about 90% by weight, relative to the total weight of the composition.

[0028] Optionally, the compositions according to the disclosure include at least one non-aqueous solvent. If present, the non-aqueous solvent(s) may be selected from, for example, monoalcohols, polyols other than those described above, fatty alcohols, fatty ethers, fatty esters, glycols, vegetable oils, mineral oils, silicone oils, liposomes, laminar lipid materials, or any mixture thereof. Active agents

[0029] Optionally, the compositions may comprise one or more active agents. In some embodiments, the compositions comprise at least two active agents, at least three active agents, etc.

[0030] By way of non-limiting example, the active agents may be selected from amino acids, aminosulfonic acids, and their salts. The amino acids, aminosulfonic acids, and their salts may be selected from acidic, basic, or neutral amino acids, aminosulfonic acids, and their salts. For example, one or more of the following may be included: alanine, arginine, asparagine, aspartic acid, cysteine, glutamic acid, glutamine, glycine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, taurine, threonine, tryptophan, tyrosine, valine, or their salts. By way of non-limiting example only, the compositions may comprise one or more of betaine, taurine, glycine, or salts thereof; one or more salts of non-acidic amino acids; or combinations of two or more of these.

[0031] As other non-limiting examples, vitamins and vitamin derivatives or probiotics, as well as their salts, may be included. By way of example only, compositions may include panthenol, tocopherol, ascorbic acid, salts thereof, or combinations thereof.

[0032] By way of further examples, phenolic and polyphenolic compounds may be included. For example, lignans, humates, flavones, chalcones, tannins, phenolic acids, catechins, anthocyanidins, stilbenoids, curcuminoids, or phenylpropanenoids may be chosen. Some non-limiting examples are baicalin, resveratrol, ferulic acid, ellagic acid, and salicylic acid.

[0033] Other examples of facultative active agents include acid salts (e.g. sodium citrate and / or sodium lactate), ceramides, cholesterols, sphingosines, C-glycosides, sugars, nucleic acids, α- and α-hydroxy acids, botanical extracts, silicates, aminopropyl triethoxysilane (APTES), dihydroxyacetone (DHA), peptides, their derivatives and mixtures thereof.

[0034] In some embodiments, the compositions comprise one or more active agents selected from vitamins, vitamin derivatives, vitamin prodrugs, sol-gel agents, peptides, amino acids or their salts, aminosulfonic acids or their salts, acid salts, polyphenolic compounds, moisturizing agents or combinations of two or more thereof.

[0035] If present, the total quantity of the active agent(s) and / or the quantity of individual active agents may be in the range of about 0.001% to about 10%, such as about 0.001% to about 9%, about 0.001% to about 8%, about 0.001% to about 7%, about 0.001% to about 6%, about 0.001% to about 5%, about 0.001% to about 4%, about 0.001% to about 3%, about 0.001% to about 2%, about 0.001% to about 1%, about 0.001% to about 0.5%, from approximately 0.001% to approximately 0.1%, from approximately 0.01% to approximately 10%, from approximately 0.01% to approximately 9%, from approximately 0.01% to approximately 8%, from approximately 0.01% to approximately 7%, from approximately 0.01% to approximately 6%, from approximately 0.01% to approximately 5%, from approximately 0.01% to approximately 4%, from approximately 0.01% to approximately 3%, from approximately 0.01% to approximately 2%, from approximately 0.01% to approximately 1%, from approximately 0.01% to approximately 0.5%, from approximately 0.01% to approximately 0.1%, from approximately 0.1% to approximately 10%, from approximately 0.1% to approximately 9%, from approximately 0.1% to approximately 8%, from approximately 0.1%, from approximately 7% %, from about 0.1% to about 6%, from about 0.1% to about 5%, from about 0.1% to about 4%, from about 0.1% to about 3%, from about 0.1% to about 2%, from about 0.1% to about 1%, or from about 0.1% to about 0.5% by weight, relative to the total weight of the base composition.For example, in various embodiments, the total amount of active agent(s) and / or the amount of individual active agents may be less than approximately 10%, less than approximately 9%, less than approximately 8%, less than approximately 7%, less than approximately 6%, less than approximately 5%, less than approximately 4%, less than approximately 3%, less than approximately 2%, or less than approximately 1% by weight, relative to the total weight of the composition. In some embodiments... In composition, the total quantity of individual active agents and / or the quantity of individual active agents may range from about 0.001% to about 5%, such as, for example, about 0.001% to about 3%, about 0.005% to about 5%, about 0.005% to about 3%, about 0.01% to about 5%, or about 0.01% to about 3% by weight, relative to the total weight of the composition. Auxiliary components

[0036] The compositions according to the disclosure may optionally include one or more auxiliary components. Useful auxiliary components include, but are not limited to, dyes and / or pigments for coloring the composition, rheology modifying agents (thickeners), humectants, structuring agents, gloss enhancers, antioxidants, penetrants, sequestrants, perfumes, opacifiers, sunscreens, etc.

[0037] Optional auxiliary components may be present in an amount of up to about 15%, such as from about 0.01% to about 10%, or from about 0.1% to about 5% by weight, relative to the total weight of the composition.

[0038] The compositions according to the disclosure may be in any form, such as a serum, an emulsion, a gel, a liquid, etc., and may be leave-on or rinse-off compositions. II. PROCESSES

[0039] The disclosure also relates to processes for treating keratinous substrates with compositions as disclosed. For example, the processes may include processes for increasing or improving moisture in keratinous substrates, processes for reducing moisture loss in keratinous substrates, processes for revitalizing keratinous substrates, etc. The processes may also be processes for treating hair with compositions as disclosed, for example by increasing or improving moisture in hair fibers, reducing moisture loss from hair fibers, revitalizing hair such as by improving smooth texture, manageability (e.g., fewer flyaways) and strength of hair, reducing frizz and / or improving curl definition and / or the evenness of curly hair.

[0040] Typically, processes for treating keratinous substrates with compositions according to the disclosure include applying the composition to the keratinous substrates and optionally removing the composition after a certain period of time, for example by rinsing or wiping the composition off the keratinous substrate. The period of time during which the composition is left on the keratinous substrate ("resting period" or "exposure period") may vary, but can range from about 30 seconds to about 48 hours, such as from about 30 seconds to about 24 hours, from about 30 seconds to about 12 hours, from about 30 seconds to about 6 hours, from about 30 seconds to about 2 hours, from about 30 seconds to about 1 hour, from about 30 seconds to about 45 minutes, from about seconds to about 30 minutes, from about 30 seconds to about 20 minutes, from about 30 seconds to about 15 minutes, from about 30 seconds to about 10 minutes, from about 30 seconds to about 5 minutes, or from about 30 seconds to about 2 minutes. For example, in some preferred embodiments, the rest period can range from about 1 minute to about 2 hours, from about 5 minutes to about 1 hour, from about 10 minutes to about 45 minutes, or from about 15 minutes to about 40 minutes, such as about 30 minutes.In other preferred embodiments, the resting period can range from about 1 hour to about 24 hours, from about 2 hours to about 12 hours, or from about 3 hours to about 9 hours; for example, the composition can be left on the keratinous substrate overnight.

[0041] Optionally, the composition can be applied to the keratinous substrate and left on the keratinous substrate until the keratinous substrate is subsequently washed off as part of ordinary personal cleansing. As such, in certain embodiments, the composition can be considered a "pre-wash" or "pre-shampoo" treatment composition.For example, an exemplary and non-limiting process according to the disclosure includes applying a composition according to the disclosure to the skin or hair and leaving it for a period of time, for example, for a period ranging from about 1 minute to about 24 hours, such as about 5 minutes to about 12 hours, or about 15 minutes to about 9 hours, for example, overnight, or about 1 minute to about 2 hours, about 5 minutes to about 1 hour, about 10 minutes to about 45 minutes, or about 15 minutes to about 40 minutes, such as about 30 minutes, and then washing the skin or hair.

[0042] Surprisingly, the compositions and processes for treating keratinous substrates according to the disclosure have proven extremely effective not only in increasing the moisture content of keratinous substrates, but also in maintaining their moisture content, for example, by reducing the amount of moisture lost from the keratinous substrates. This would be the result of an unexpected synergistic interaction of the components described herein. Furthermore, although the compositions are alkaline, they do not harm the keratinous substrates, for example, keratinous fibers such as hair. This would also be the result of the synergistic interaction of the components described herein.

[0043] Without being linked to any theory, it is thought that the alkali carbonate(s) and the polyol(s) form a unique network which allows increased penetration into the substrates ke- The network also remains within the keratinous substrates, maintaining an ideal level of moisture even under conditions such as high or low humidity, which would otherwise cause water to enter or leave the keratinous substrates. Thus, the network reduces the influence of the external environment on the moisture content of the keratinous substrate, allowing the optimal level of moisture and / or hydration to be maintained within the keratinous materials.

[0044] The manufacturing processes for compositions according to the disclosure therefore include the preparation of an associated network of alkali carbonate(s) and polyol(s). For example, a simplex solution of alkali carbonate(s) and polyol(s) may be prepared, which may include added water, but is preferably prepared with a minimal amount of added water, or even without added water. Without being limited to any one theory, it is believed that by preparing a simplex solution as described, the alkali carbonate(s) and the polyol(s) form a hydrogen-bonded network.

[0045] For example, a simplex solution of alkali carbonate(s) and polyol(s) can be prepared by combining the alkali carbonate(s), the polyol(s), and optionally a small amount of water and stirring until the alkali carbonate dissolves and the network forms. In various embodiments, the amount of water in the simplex solution can be in the range of up to about 10%, for example, from about 0.01% to about 10%, from about 0.01% to about 5%, from about 0.01% to about 3%, from about 0.01% to about 2%, from about 0.01% to about 1%, from about 0.1% to about 10%, from about 0.1% to about 5%, from about 0.1% to about 3%, from about 0.1% to about 2%, from about 0.1% to about 1%, based on the total weight of the simplex solution. In some embodiments, no water is added to the simplex solution.Optionally, one or more of the active agents described above may also be included in the simplex solution, and the active agent(s) may therefore also be present in the network.

[0046] The process may optionally take place at room temperature or may be elevated, for example, may go from about 22 °C to about 25 °C, from about 25 °C to about 100 °C, from about 35 °C to about 100 °C, from about 50 °C to about 100 °C, from about 75 °C to about 100 °C, from about 25 °C to about 90 °C, from about 35 °C to about 90 °C, from about 50 °C to about 90 °C, or from about 75 °C to about 90 °C.

[0047] Preferably, the simplex solution is prepared by including quantities of alkali carbonate(s) and polyol(s) such that the molar ratio of alkali carbonate(s) to polyol(s) present in the simplex solution, and therefore the lattice, is less than 1:3 to greater than approximately 1:50, for example, ranging from approximately 1:4 to approximately 1:50, from approximately 1:4 to approximately 1:45, from approximately 1:4 to approximately 1:40, from approximately 1:4 to approximately 1:35, from approximately 1:4 to approximately 1:30, from approximately 1:4 to approximately 1:25, from approximately 1:4 to about 1:20, from about 1:4 to about 1:15, from about 1:4 to about 1:10, from about 1:5 to about 1:50, from about 1:5 to about 1:45, from about 1:5 to about 1:40, from about 1:5 to about 1:35, from about 1:5 to about 1:30, from about 1:5 to about 1:25, from about 1:5 to about 1:20, from about 1:5 to about 1:15, or from about 1:5 to about 1:10.For example, in some preferred embodiments, the molar ratio of alkali carbonate(s) to polyol(s) in the simplex solution may range from about 1:4 to about 1:20, from about 1:5 to about 1:15, from about 1:7 to about 1:13, or from about 1:9 to about 1:11, for example a molar ratio of about 1:4, about 1:5, about 1:6, about 1:7, about 1:8, about 1:9, about 1:10, about 1:11, about 1:12, about 1:13, about 1:14, about 1:15, about 1:16, about 1:17, about 1:18, about 1:19, or about 1:20, or may be within a range using any of the above as upper and lower bounds. Preferably, the molar ratio of alkali carbonate(s) to polyol(s) in the simplex solution is approximately 1:10.

[0048] In some embodiments, the simplex solution comprises water and the molar ratio of the alkali carbonate(s) to water ranges from about 10:1 to about 1.10, such as from about 5:1 to about 1.5, for example from about 4:1 to about 1:4, from about 3:1 to about 1:3, from about 2.5:1 to about 1.2.5, from about 1:2 to about 2:1, from about 1.75:1 to about 1:1.75, from about 1.5:1 to about 1:1.5, from about 1.25:1 to about 1:1.25, from about 1.2:1 to about 1:1.2, or from about 1.1:1 to about 1:1.1. For example, the molar ratio of alkali carbonate(s) to water may be about 5, about 4.5, about 4, about 3.5, about 3, about 2.5, about 2, about 1.9, about 1.8, about 1.7, about 1.6, about 1.5, about 1.4, about 1.3, about 1.2, about 1.1, about 1, about 0.9, about 0.8, about 0.7, about 0.6 or about 0.5, or may be within a range using any of the above as upper and lower bounds.Optionally, if present, the amount of water in the simplex solution is such that the molar ratio of the alkali carbonate(s) to the water is approximately the same, i.e., approximately 1:1.

[0049] Once the alkali carbonate(s) and polyol(s) network is formed, the network can be included in the compositions as disclosed, as described above. For example, a simplex solution of alkali carbonate(s) and polyol(s) can be prepared as described here, and the simplex solution can then be added to or diluted with water and / or a non-aqueous solvent to form a composition as disclosed. The pH of the composition can optionally be adjusted to the target pH by adding a pH adjuster. Several alkali carbonate(s) and polyol(s) networks can be included in the compositions, where the alkali carbonate(s) and / or polyol(s) in each network can be identical or different from those in the other network(s). Additional components such as one or more active agents and / or auxiliary components may also be optionally included in the compositions. However, a qualified person will ensure that no components or quantities of components are included in the simplex solution and / or composition that could diminish the network interaction of the alkali carbonate(s) and the polyol(s).

[0050] After describing in detail the numerous embodiments of the present invention, it will become apparent that modifications and variations are possible without departing from the scope of the disclosure defined in the appended claims. Furthermore, it should be noted that all the examples in this disclosure, while illustrating numerous embodiments of the disclosure, are provided by way of non-limiting examples and should therefore not be considered as limiting the various aspects thus illustrated. It is understood that all definitions in this document are provided solely for the purposes of this disclosure.

[0051] As used herein, the terms "comprising", "having" and "including" (or "comprehension", "having" and "include") are used in their open, non-limiting sense.

[0052] In this application, the use of the singular includes the plural, unless specifically stated otherwise. The singular forms "a," "an," "the," "the," and "at least one" are understood to encompass both the plural and the singular, unless the context clearly indicates otherwise. The expressions "one or more" and "at least one" are interchangeable and expressly include individual components as well as mixtures / combinations. Similarly, the expression "a salt of this one" also refers to "salts of this one."Thus, when the disclosure refers to "at least one item selected from the group consisting of A, B, C, D, E, F, a salt of these, or mixtures of these", it indicates that one or more of A, B, C, D and F may be included, one or more of a salt of A, a salt of B, a salt of C, a salt of D, a salt of E and a salt of F may be included, or a mixture of any two of A, B, C, D, E, F, one or more salts of A, one or more salts of B, one or more salts of C, one or more salts of D, one or more salts of E and one or more salts of F may be included.

[0053] The expression "and / or" should be understood as including both the conjunctive and the disjunctive. For example, "amino acids and / or their salts" means "amino acids and their salts" as well as "amino acids or their salts," and expressly covers cases of either.

[0054] As used herein, the expressions "and mixtures of these", "and a mixture of these", "and a combination of these", "or mixtures of these", "or a mixture of these", "or combinations of these", and "or a The phrases "combination of these" are used interchangeably to indicate that the list of components immediately preceding the phrase, such as "A, B, C, D, or mixtures thereof," means that the component(s) can be chosen from A, B, C, D, A + B, A + B + C, A + D, A + C + D, etc., without limitation on the variations thereof. Thus, the components can be used individually or in any combination thereof.

[0055] For the purposes of this disclosure, it should be noted that, to provide a more concise description, some of the quantitative expressions given in this document are not qualified with the term "approximately". It is understood that, whether the term "approximately" is used explicitly or implicitly, each quantity given herein is intended to refer to the actual value given, and it is also intended to refer to the approximation of that value given that would be reasonably deduced by a person skilled in the art, including approximations due to experimental and / or measurement conditions for that value.

[0056] All ranges and quantities indicated herein are intended to include subranges and quantities using any disclosed point as a boundary, and all boundaries are intended to be inclusive unless expressly stated otherwise. Thus, a range of "1% to 10%, such as 2% to 8%, such as 3% to 5%" is intended to encompass ranges of "1% to 8%", "1% to 5%", "2% to 10%", and so on. All numbers, quantities, ranges, etc., are intended to be modified by the term "approximately", whether or not expressly stated, unless expressly stated otherwise. Similarly, a given range of "approximately 1% to 10%" is intended to have its boundaries of both 1% and 10% modified by the term "approximately". The term "approximately" is used in this document to indicate a difference of up to + / - 10% from the stated number, such as + / - 9%, + / - 8%, + / - 7%, + / - 6%, + / - 5%, + / - 4%, + / - 3%, + / - 2%, or + / - 1%.Similarly, all range boundaries are understood as being disclosed individually, such that, for example, a range of 1:2 to 2:1 is understood as disclosing a ratio of 1:2 and 2:1.

[0057] As used here, if a component is described as being present "in an amount less than or equal to" a certain amount, it is expected that this component is in fact present in the composition, namely, present in an amount greater than 0%.

[0058] All quantities and ratios indicated herein are given on the basis of the total weight of the composition, unless otherwise stated. Unless otherwise stated, all percentages indicated herein are by weight of active ingredient.

[0059] As used herein, the terms "application of a composition to keratinous substrates" and their variations are intended to designate the contacting of keratinous substrates keratinous substances, particularly hair and skin, may be affected by contact with at least one of the disclosed compositions, in any manner whatsoever. This may also mean bringing keratinous substrates into contact with a significant amount of the composition.

[0060] In this document, the term "salts" throughout the disclosure may include salts containing a counterion such as an alkali metal, an alkaline earth metal, or an ammonium counterion. This list of counterions, however, is not exhaustive. Salts also include a dissociated form of a compound, for example, in an aqueous solution.

[0061] As used in this document, the expressions "substantially free" or "essentially free" mean that the specific material may be present in small amounts that do not significantly affect the basic and novel characteristics of the compositions as disclosed. For example, there may be less than 2% by weight of a specific material added to a composition, relative to the total weight of the compositions (provided that an amount less than 2% by weight does not significantly affect the basic and novel characteristics of the compositions as disclosed). Similarly, the compositions may include less than 2%, less than 1.5%, less than 1%, less than 0.5%, less than 0.1%, less than 0.05%, or less than 0.01%, or none of the specified materials.All components positively presented in this disclosure may be negatively excluded from the claims; for example, a claimed composition may be "free," "substantially free" (or "significantly free") of one or more components that are positively presented in this disclosure. The term "substantially free" or "essentially free" as used here may also mean that the specific material is not added to the composition, but it may still be present in a raw material included in the composition.

[0062] As used herein, the term "treat" (and its grammatical variations) refers to the application of the compositions of this disclosure to the surface of keratinous substrates, such as skin and / or hair.

[0063] Unless expressly stated otherwise, no process presented herein is intended to be interpreted as requiring its steps to be performed in a specific order. Accordingly, where a process claim does not expressly state an order to be followed by its steps, or where it is not specifically stated in the claims or descriptions that the steps must be limited to a specific order, no particular order is to be inferred. EXAMPLES

[0064] The following examples are only intended to be non-limiting in nature and ex plicative. In Examples, unless otherwise indicated, quantities are expressed as a percentage by weight (% by weight) of active ingredients, relative to the total weight of the composition.

[0065] Example 1 – Simplex Solutions

[0066] The following three simplex solutions were prepared to form three different associated networks of potassium carbonate and glycerol.

[0067] Example IA - Simplex solution with water

[0068] Potassium carbonate, glycerol, and deionized water were mixed in a molar ratio of approximately 1:10:1 while stirring at a temperature of approximately 80 °C until the potassium carbonate was dissolved and the solution was substantially homogeneous. The solution was allowed to cool to room temperature. It was observed that the solution was highly viscous.

[0069] Example IB - Simplex solutions without water

[0070] Two separate simplex solutions were prepared. Potassium carbonate and glycerol were mixed in a molar ratio of approximately 1:10 while stirring at a temperature of approximately 80 °C until the potassium carbonate was dissolved and the solution was substantially homogeneous. The solution was allowed to cool to room temperature. The procedure was repeated, but the molar ratio of potassium carbonate to glycerol was approximately 1:5. In both procedures, the solutions were observed to be highly viscous. Example 2 - Compositions

[0071] The inventive and comparative compositions in Table 1 have been prepared.

[0072] [Tables 1] Comparative Inventory 2A 2B Cl C2 Glycerol 8.6 8.6 8.6 8.6 Potassium Carbonate 1.3 1.3 1.3 Hydrochloric Acid QS at pH 8 Lactic Acid QS at pH 8 QS at pH 8 Water Qs per 100 Qs per 100 Qs per 100 Qs per 100 pH 8 8 7 8

[0073] Compositions 2A and 2B according to the disclosure were prepared by diluting the simplex solution prepared in Example IA with water and a pH corrector.

[0074] Composition Cl was prepared by mixing water and glycerol. The pH of the mixture was measured at 7.

[0075] Composition C2 was prepared by mixing all the specified components at the same time to prepare the composition in the form of an adjuvant of potassium carbonate and glycerol in water.

[0076] Example 3 - Tests

[0077] The following tests were carried out to evaluate the moisture and cosmetic benefits provided to the hair by the inventive and comparative compositions in Table 1. Example 3A-1

[0078] Two strands of very curly hair were rinsed, washed, rinsed again, and left to air dry overnight under ambient conditions. Equal amounts (approximately 0.4 grams per gram of hair) of composition 2A or Cl were applied to separate strands and massaged into the hair. The strands were left overnight (approximately 12 hours) under ambient conditions. Afterward, the strands were shampooed, rinsed, and left to air dry overnight under ambient conditions.

[0079] In accordance with the manner in which these properties are typically evaluated in the art, an expert assessed the visual and tactile properties of each strand to determine whether various properties of the strand treated with inventive composition 2A or the strand treated with comparative composition Cl were superior. The expert concluded that the strand treated with inventive composition 2A exhibited significantly better hydration, curl regularity and definition, and slightly better smooth texture and frizz reduction than the strand treated with comparative composition CL Example 3A-2

[0080] Composition 2A or Cl was applied to dry, curly hair on two mannequin heads with the hair divided into four quadrants, each quadrant having a different curl pattern. The compositions remained on the hair for a processing period of approximately 30 minutes, after which the hair was shampooed and rinsed, a detangling solution was applied, and the hair was then rinsed again and dried under a roller dryer for approximately one hour.

[0081] In accordance with the manner in which these properties are generally evaluated in the art, an expert assessed the visual and tactile properties of each head of hair to determine whether various properties of the hair treated with the inventive composition 2A or with the comparative composition Cl were better. The expert assessed three of the four quadrants on each mannequin head, the least curly quadrant and the two curliest quadrants, for a total of 3 assessments for the Hair treated with inventive composition 2A and 3 evaluations for hair treated with comparative composition Cl. Each quadrant of hair on the mannequin head treated with inventive composition 2A was assigned a rating of 1 (slightly better), 2 (notably better), or 3 (significantly better) to quantify the improvement of the parameter compared to the corresponding quadrant of hair on the mannequin head treated with comparative composition Cl. The mean (n=3) of these ratings is presented in Table 2 below.

[0082] [Tables2] Parameter Rating of Improvement Dryness Reduction (Tactile) 2.3 Shape Control 2.3 Discipline 2 Hydration 2 Smooth Texture (Tactile) 2 Smooth Texture (Visual) 1.7 Split End Reduction (Visual) 1.7 Strength 1.7

[0083] The expert also observed that the two quadrants of the curliest hair treated with the inventive composition 2A had significantly better detangling effects upon application than the same quadrants of hair treated with the comparative composition CL

[0084] Examples 3A-1 and 3A-2 therefore confirm that the compositions according to the disclosure comprising an associated network of alkali carbonate(s) and polyol(s) surprisingly offer hair significant moisture, revitalization and cosmetic benefits compared to compositions comprising a polyol but no alkali carbonate. Example 3B

[0085] Half-head studies were conducted on dry, curly hair from six volunteers. For each volunteer, the inventive composition 2B was applied to one half of the head of hair and the comparative composition C2 was applied to the other half. The compositions were applied and massaged through the hair to distribute them evenly, and left on the hair for 30 minutes, after which the hair was shampooed and rinsed, a detangling solution was applied, and the hair was then rinsed again and dried under a roller dryer for approximately one hour.

[0086] In accordance with the way these properties are generally evaluated in the art, an expert assessed the visual and tactile properties of each half-head of hair to determine whether various properties of the hair treated with the inventive composition 2B or the hair treated with the comparative composition C2 were superior. Each half-head of hair treated with the inventive composition 2B was assigned a rating of 1 (slightly better), 2 (notably better), or 3 (significantly better) to quantify the improvement in the parameter compared to the hair treated with the comparative composition C2. The mean (n=6) of these ratings is presented in Table 3 below.

[0087] [Tables3] Parameter Rating of Improvement Smooth Texture (Tactile) 1.7 Curl Definition 1.5 Hydration 1.5 Strength 1.5 Dryness Reduction (Tactile) 1.5

[0088] The expert also observed that the volunteers with the curliest hair (n=4) showed significantly better curl resilience on the half of the head treated with the inventive composition 2B compared to the half of the head treated with the comparative composition C2.

[0089] Example 3B therefore demonstrates that the compositions according to the disclosure comprising an associated network of alkali carbonate(s) and polyol(s) surprisingly offer hair significant moisture, revitalization and cosmetic benefits compared to compositions comprising the same components but not in the form of an associated network.

[0090] The above examples confirm that the compositions and processes according to the disclosure provide surprisingly and unexpectedly improved moisture, revitalization and cosmetic benefits to keratinous substrates compared to the compositions and processes not in accordance with the disclosure.

Claims

Demands

1. A process for preparing a keratinous substrate treatment composition, the process comprising: (i) preparing an associated network of alkali carbonate(s) and polyol(s) by combining at least one alkali carbonate, at least one polyol, and water in an alkali carbonate(s):polyol(s) molar ratio of less than 1:3 to about 1:50 to form a simplex solution; (ii) heating the simplex solution; (iii) adding at least one solvent selected from water and / or non-aqueous solvents to the simplex solution to form the composition; and (iv) adding at least one pH adjuster to the composition.

2. A preparation process according to claim 1, wherein the molar ratio of alkali carbonate(s): polyol(s) ranges from about 1:4 to about 1:20, more preferably from about 1:5 to about 1:15, more preferably still from about 1:7 to about 1:13, most preferably from about 1:9 to about 1:

11.

3.

4. Composition prepared according to the process of claim 1 or 2. Method for treating a keratinous substrate, the method comprising: i. applying the composition according to claim 3 to the keratinous substrate, and ii. optionally, removing the composition from the keratinous substrate after a period of exposure ranging from about 30 seconds to about 48 hours, preferably from about 1 minute to about 24 hours, more preferably from about 5 minutes to about 12 hours, most preferably from about 10 minutes to about 9 hours.