HAIR TREATMENT COMPOSITION

专利摘要:
application of a surfactant-soluble anti-dandruff agent. it is a hair care composition having from about 14% to about 40% of one or more surfactants; from about 0.1% to about 10% of one or more surfactant-soluble antidandruff agents; where, when the hair care composition is diluted to 1.3%, the surfactant concentration has a ratio between surfactant diffusion coefficient and soluble agent diffusion coefficient less than 0.6 or greater than 1.4.
公开号:BR112017022021B1
申请号:R112017022021-0
申请日:2016-04-22
公开日:2021-07-06
发明作者:Debora W. Chang；Eric Scott Johnson；Robert Wayne Glenn, Jr.；Todd Ryan Thompson；Allison Lynn Edwards；Michelle Lynn Carter
申请人:The Procter & Gamble Company；
IPC主号:

专利说明:

FIELD OF THE INVENTION
[0001] The present invention relates to the application of a surfactant soluble scalp agent of a composition for hair treatment. BACKGROUND OF THE INVENTION
[0002]For years, anti-dandruff shampoos have been widely used to treat dandruff and cleanse hair and scalp, but there still remains a need for optimized anti-dandruff shampoos. In general, antidandruff shampoos are formulated with antidandruff agents in combination with surfactants and aqueous systems that are intended to deposit the antidandruff agents on the scalp. Anti-dandruff agents can be insoluble particulates such as zinc pyrithione and/or surfactant-soluble substances such as climbazol or octopirox. Many dandruff shampoos use cationic polymers with anionic surfactants to form coacervates that aid in the deposition of insoluble particulate agents. However, in general, coacervates do not affect the deposition of soluble agents as soluble agents do not associate with coacervates formed between cationic polymers and anionic surfactants. In fact, it can be difficult to deposit much more than 1 to 2% of the soluble agents present in antidandruff shampoos onto the scalp while the remaining 98 to 99% of the soluble agents in the formulas are rinsed off. As many of the antidandruff agents can be relatively expensive, allowing >97% of the soluble agents to be rinsed off is tantamount to throwing money away, and so there is a need for a shampoo that can more efficiently deposit soluble antidandruff agents. Also, as consumers continue to desire a shampoo that offers superior antidandruff efficacy and less dandruff agent deposition results in lower antidandruff efficacy, there remains a need for a shampoo that can deposit a higher percentage of soluble agents present in the scalp on the scalp. anti-dandruff shampoos.
[0003]The association of different classes of surfactants in micellar aggregates is a well-known phenomenon. Micelles are often drawn as static spherical aggregates, but actually micelles are in dynamic equilibrium with individual surfactant molecules (monomers) that are constantly being exchanged between the bulk and the micelles. Additionally, the micelles themselves are continually disintegrating and reassembling. There are two relaxation processes involved in micellar solutions. The first is a rapid relaxation process called T1 which is associated with the rapid exchange of monomers between micelles and the surrounding mass phase. The second relaxation time, T2, is attributed to the micelle formation and dissolution process (ie, the micelle lifetime). The extensive experimental research on micellization kinetics by Shah et al. (Patist, A., Jha, B.K., Oh, S.G., and Shah, D.O., J. Surfactants Deterg. 2, 317, 1999). James-Smith, M.A., Shekhawat, D., and Shah, D.O., Tenside Surf. Det. 44, (2007) 142) showed a strong correlation of T2 with various detergency properties including oil solubilization in micellar solutions and droplet size in emulsions, as well as surface active properties such as dynamic surface tension and micelle stability. Their research also revealed a strong inverse correlation of T2 with other properties, such as foaming ability and concentration of submicellar aggregates. Specifically, they showed that a maximum T2 and thus maximum micellar stability corresponded to both a maximum rate of oil solubilization and maximum amount of solubilized oil. Logic, therefore, might suggest that a cleaning composition with longer T2, more stable micelles and faster solubilization rate might be preferable, as such a system can clean better, more quickly solubilize larger amounts of oils or surfactant-soluble materials and it should be more stable. Surprisingly, however, it has been found that a composition with a shorter T2 surfactant system, less stable micelles and a slower rate of solubilization, as demonstrated in Figure 1, is preferred. SUMMARY OF THE INVENTION
[0004] In an embodiment of the present invention, it relates to a composition for treating hair, comprising from about 14% to about 40% of one or more surfactants; from about 0.1% to about 10% of one or more surfactant-soluble antidandruff agents; where, when the hair care composition is diluted to a surfactant concentration of 1.3%, it has a ratio between surfactant diffusion coefficient and soluble agent diffusion coefficient less than 0.6 or greater than 1.4. BRIEF DESCRIPTION OF THE DRAWINGS
[0005] Figure 1 is a graph of the solubilization rate of octopirox as a function of the surfactant composition. DETAILED DESCRIPTION OF THE MODALITIES OF THE INVENTION
[0006]All percentages and ratios used in this document are expressed in weight of the total composition, except where otherwise indicated. All measurements are understood to be made under ambient conditions, where "ambient conditions" means conditions at about 25°C, under about one atmosphere of pressure and about 50% relative humidity, unless otherwise noted. All numeric ranges include narrower ranges; the delineated upper and lower range boundaries are combinable to create additional ranges not explicitly delineated.
[0007] The compositions of the present invention may comprise, consist essentially of, or consist of essential ingredients, as well as optional ingredients described herein. For use herein, the term "consists essentially of" means that the composition or component may contain additional ingredients, but only if these do not substantially alter the basic and novel characteristics of the claimed compositions or methods.
[0008] "Apply" or "applying", as used in reference to a composition, means applying or spreading the compositions of the present invention onto a keratinous tissue such as hair.
[0009] "Dermatologically acceptable" means that the compositions or components described are suitable for use in contact with human skin tissue without undue toxicity, incompatibility, instability or allergic response, and the like.
"Safe and effective amount" means an amount of a compound or composition sufficient to significantly elicit a positive benefit.
[0011] Although the specification ends with claims that specifically mark and distinctly claim the invention, it is believed that the present invention will be better understood from the following description.
[0012]As used herein, the term "fluid" includes liquids and gels.
[0013] For use in the present invention, articles including "a" and "an", when used in a claim, are understood to mean one or more of what is claimed or described.
[0014]As used herein, "comprising" means that other steps and other ingredients that do not affect the end result may be added. This term covers the terms "consisting of" and "consisting essentially of".
[0015]For use in the present invention, the term "blends" is intended to include a unique combination of materials and any compounds that may result from that combination.
[0016] As used herein, "molecular weight" or "MW" refers to weight average molecular weight unless otherwise specified. Molecular weight is measured using industry standard method, gel permeation chromatography ("GPC").
[0017] Where ranges of amounts are given, these shall be understood as the total amount of said ingredient in the composition or, where more than one species falls within the scope of the ingredient definition, as the total amount of all ingredients present in the composition that correspond to that definition.
[0018] For example, if the composition comprises 1% to 5% fatty alcohol, then a composition comprising 2% stearyl alcohol and 1% cetyl alcohol and no other fatty alcohol would fall within the scope.
[0019] The amount of each specific ingredient or mixtures thereof, described later in this document, may account for up to 100% (or 100%) of the total amount of the ingredient(s) in the hair care composition.
[0020] As used herein, "personal care compositions" include products such as shampoos, shower gels, liquid hand cleansing creams, hair dyes, facial cleansing creams and other liquid surfactant-based compositions
[0021] As used herein, the terms "include", "includes" and "including" are intended to be non-limiting and are understood to mean "comprise", "comprises" and "comprising", respectively.
[0022] All percentages, parts and ratios are based on the total weight of the compositions of the present invention, except where otherwise specified. All of these weights, as long as they belong to the ingredients on the list, are based on the active content and therefore do not include vehicles or by-products that might be included in commercially available materials.
[0023] Except where otherwise specified, all component or composition contents refer to the active portion of that component or that composition and exclude impurities, for example, residual solvents or by-products, which may be present in commercially available sources of such components or compositions.
[0024] It should be understood that each numerical upper limit presented throughout this descriptive report includes each of the lower numerical limits, as if such lower numerical limits were expressly written in this document. Each numerical lower limit presented throughout the specification includes each of the upper numerical limits, as if such upper numerical limits were expressly written in this document. Each numerical range presented in this descriptive report includes each narrower numerical range that falls within such broader numerical range, as if such narrower numerical ranges were expressly written in this document.
[0025] Although the T2 and stability of a surfactant system and the solubility of soluble agents in surfactant in that system are important, the stability and solubility of the surfactant micelle and the rate of solubilization of agents in the system after dilution are of equal importance , such as when cleaning composition is applied to the head during use. One way to understand the solubility and associations of the soluble agent in the surfactant system through dilution is to measure by NMR the diffusion coefficients of the surfactant and the surfactant soluble agents in a diluted sample. If the diffusion coefficients of the surfactant and the agent are similar such that the ratio between the two coefficients is close to 1.0, it can be inferred that the surfactant-soluble agent is in or in close association with surfactant micelles. However, if the diffusion coefficients of the surfactant and the agent are too different such that the ratio between the two coefficients is significantly greater or less than 1.0, then it can be inferred that the surfactant-soluble agent is not within or associated with the surfactant micelles. This, in turn, implies that the surfactant-soluble agent is less soluble in the diluted surfactant of the second case.
[0026] It was found that a soluble antidandruff agent containing cleaning composition, which when diluted to 1.3% surfactant concentration has a ratio of surfactant diffusion coefficient to soluble agent diffusion coefficient of less than 0.8 or greater than 1.2, which can deposit this soluble agent with ~1.4X or greater efficiency than a composition containing soluble antidandruff agent, whose diffusion coefficient ratio is close to 1.0.
[0027] Without sticking to theory, the increased deposition efficiency exhibited by the embodiments of the present invention can, surprisingly, be further increased by incorporating an additional oil phase that separates upon dilution in combination with a cationic polymer, which forms coacervates upon dilution. Coacervate aids in the deposition of oil within which the surfactant-soluble agent must be at least partially soluble, thus resulting in an increase in the total percentage of soluble agent deposited.
[0028] Surfactant-soluble agents are defined as materials that are insoluble in water, but soluble at a concentration of 0.1% or higher in a 10% aqueous solution of sodium laureth-1 sulfate. A conventional method can be used to determine solubility. Such a method may include a material, in which solubility can be determined by first visually evaluating that the material containing sodium laureth-1 sulfate mixture is homogeneous, followed by filling a glass container with the material containing the laureth-1 sulfate mixture then placing a Class 2 red standard laser pointer such as the Quartet Class 2 standard laser pointer (model MP-1202Q) against the side of the container and flashing the laser through the container. If the material is soluble in the sodium laureth-1 solution, the laser light will not be scattered, resulting only in an observable red dot appearing on the side of the container opposite the laser pointer and the red non-visible laser beam will be observed passing through. of the solution. Soluble anti-dandruff agent
The anti-dandruff agent may be a material or a mixture selected from the group consisting of: azoles such as climbazol, ketoconazol, itraconazol, econazol and elubiol; hydroxy pyridones such as octopirox (piroctone olamine), cyclopirox, rilopirox and MEA-Hydroxyoctyloxypyridinone; keratolytic agents such as salicylic acid and other hydroxy acids; strobilurins such as azoxystrobin and metal chelating agents such as 1,10-phenanthroline.
[0030] In one embodiment, azole antimicrobials are an imidazole selected from the group consisting of benzimidazole, benzothiazole, bifonazole, butaconazole nitrate, climbazole, clotrimazole, croconazole, eberconazole, econazole, elubiol, fenticonazole, fluconazole, flutimazole, isoconazole, ketoconazole, lanoconazole, metronidazole, miconazole, neticonazole, omoconazole, oxiconazole nitrate, sertaconazole, sulconazole nitrate, tioconazole, thiazole and mixtures thereof, or azole antimicrobials are a triazole selected from the group consisting of: terconazole, itraconazole and mixtures of the same. In one embodiment, the azole antimicrobial agent is ketoconazole. In one embodiment, the only antimicrobial agent is ketoconazole.
[0031] In one embodiment, the soluble antidandruff agent may be present in an amount of about 0.1% to 10%, in another embodiment, from about 0.25% to 8%, in yet another embodiment, of about 0.5% to 6%. A. Detersive surfactant
[0032] The hair care composition may comprise more than about 14% by weight of a surfactant system that provides cleaning performance to the composition, in one embodiment, greater than 20% by weight of a surfactant system that provides a cleaning performance to the makeup. The surfactant system contains an anionic surfactant and/or a combination of anionic surfactants and/or a combination of anionic and cosurfactant surfactants selected from the group consisting of amphoteric, zwitterionic, nonionic surfactants and mixtures thereof. Various examples and descriptions of detersive surfactants are given in US Patent No. 8,440,605; US Patent Application Publication No. 2009/155383 and US Patent Application Publication No. 2009/0221463, which are incorporated herein by reference in their entirety.
[0033] In one embodiment, the hair care composition may comprise from about 14% to about 40%, from about 15% to about 36%, from about 18% to about 32%, or from about 18% to about 32%. about 20% to about 28% by weight of one or more surfactants.
[0034] Suitable anionic surfactants for use in the compositions are alkyl and alkyl ether sulfates. Other suitable anionic surfactants are the water-soluble salts of organic products from the sulfuric acid reaction. Further suitable anionic surfactants are the reaction products of fatty acids esterified with isethionic acid and neutralized with sodium hydroxide. Other similar anionic surfactants are described in US Patent Nos. 2,486,921; 2,486,922; and 2,396,278, which are incorporated herein by reference in their entirety.
[0035]Examples of anionic surfactants for use in the hair care composition include ammonium lauryl sulfate, ammonium laureth sulfate, paret C10-15 ammonium sulfate, C10-15 alkyl ammonium sulfate, C11-15 alkyl ammonium sulfate, decyl ammonium sulphate, ammonium decet sulphate, ammonium undecyl sulphate, ammonium undecet sulphate, triethylamine lauryl sulphate, triethylamine lauryl sulphate, triethanolamine lauryl sulphate, triethanolamine lauryl sulphate, monoethanolamine lauryl sulphate, monoethanolamine lauryl sulphate, lauryl sulphate diethanolamine, diethanolamine laureth sulfate, sodium lauric monoglyceride sulfate, sodium lauryl sulfate, sodium lauryl sulfate, sodium C10-15 sulfate, sodium C10-15 alkyl sulfate, sodium C11-15 alkyl sulfate, sodium decyl sulfate sodium, sodium decet sulfate, sodium undecyl sulfate, sodium undecet sulfate, potassium lauryl sulfate, potassium lauret sulfate, paret C1015 potassium sulfate, C1 alkyl 0-15 potassium sulphate, C11-15 alkyl potassium sulphate, potassium decyl sulphate, potassium decet sulphate, potassium undecyl sulphate, potassium undecet sulphate, sodium lauryl sarcosinate, sodium lauroyl sarcosinate, lauryl sarcosine, cocoyl sarcosine , cocoyl ammonium sulfate, ammonium lauroyl sulfate, sodium cocoyl sulfate, sodium lauroyl sulfate, potassium cocoyl sulfate, potassium lauryl sulfate, triethanolamine lauryl sulfate, triethanolamine lauryl sulfate, monoethanolamine cocoyl sulfate, monoethanolamine lauryl sulfate , sodium tridecyl benzene sulfonate, sodium dodecyl benzene sulfonate, sodium cocoyl isethionate and combinations thereof. In one embodiment, the anionic surfactant is sodium lauryl sulfate or sodium laureth sulfate.
[0036] The composition of the present invention may also include anionic surfactants selected from the group consisting of: a) R1 O(CH2CHR3O)y SO3M; b) CH3(CH2)z CHR2CH2O(CH2CHR3O)y SO3M; and c) mixtures thereof, wherein R1 represents CH3 (CH2)10, R2 represents H or a hydrocarbon radical comprising from 1 to 4 carbon atoms so that the sum of the carbon atoms in z and R2 is 8, R3 is H or CH3 , y is 0 to 7, the average value of y is about 1 when y is not (0), and M is a positively charged monovalent or divalent cation.
Suitable anionic alkyl sulfate and alkyl ether sulfate based surfactants include, but are not limited to, those having branched alkyl chains, which are synthesized from C8 to C18 branched alcohols that can be selected from the group consisting of: Guerbet alcohols, alcohols derived from aldol condensation, oxo alcohols and mixtures thereof. Some non-limiting examples of branched alcohols including 2-alkyl oxo alcohols like 2-methyl-1-undecanol, 2-ethyl-1-decanol, 2-propyl-1-nonanol, 1-octanol 2-butyl, 2-methyl-1 -dodecanol, 2-ethyl-1-undecanol, 2-propyl-1-decanol, 2-butyl-1-nonanol, 2-pentyl-1-octanol, 2-pentyl-1-heptanol, and those sold under the trade names LIAL® (Sasol), ISALCHEM® (Sasol), and NEODOL® (Shell), and Guerbet and aldolic condensation derivative alcohols such as 2-ethyl-1-hexanol, 2-propyl-1-butanol, 2-butyl- 1-octanol, 2-butyl-1-decanol, 2-pentyl-1-nonanol, 2-hexyl-1-octanol, 2-hexyl-1-decanol, and those sold under the trade name ISOFOL® (Sasol) or sold as alcohol ethoxylates and alkoxylates under the trade names LUTENSOL XP® (BASF) and LUTENSOL XL® (BASF).
Anionic alkyl sulfates and alkyl ether sulfates may also include those synthesized from branched alcohols derived from C8 to C18 butylene or propylene which are sold under the trade names EXXAL™ (Exxon) and Marlipal® (Sasol). This includes anionic surfactants from the subclass sodium tridecet-n sulfates (STnS), where n is between about 0.5 and about 3.5. Examples of surfactants in this subclass are sodium tridecet-2 sulfate and sodium tridecet-3 sulfate. The composition of the present invention can also include sodium tridecyl sulfate.
[0039] The composition of the present invention may also include anionic alkyl and alkyl ether sulfosuccinates and/or dialkyl ether and dialkyl sulfosuccinates and mixtures thereof. The dialkyl and dialkyl ether sulfosuccinates can be linear or branched C6-15 dialkyl and dialkyl ether sulfosuccinates. The alkyl moieties can be symmetric (i.e., the same alkyl moieties) or asymmetric (i.e., different alkyl moieties). Some non-limiting examples include: disodium lauryl sulfosuccinate, disodium lauryl sulfosuccinate, sodium bistridecyl sulfosuccinate, sodium dioctyl sulfosuccinate, sodium dihexyl sulfosuccinate, sodium dicyclohexyl sulfosuccinate, sodium diamyl sulfosuccinate, sodium diisobutyl sulfosuccinate linear bis(tridecyl) sulfosuccinate and mixtures thereof.
[0040] The hair care composition may comprise a co-surfactant. The cosurfactant can be selected from the group consisting of amphoteric surfactant, zwitterionic surfactant, nonionic surfactant and mixtures thereof. The cosurfactant may include, but is not limited to, lauramide propyl betaine, cocoamido propyl betaine, lauryl hydroxy sultaine, sodium lauroamphoacetate, disodium cocoamphodiacetate, cocamide and mixtures thereof.
[0041] The hair care composition may further comprise from about 0.25% to about 15%, from about 2% to about 14%, from about 3% to about 13% by weight of one or more amphoteric, zwitterionic, non-ionic co-surfactants, or a mixture thereof.
Amphoteric or zwitterionic surfactants suitable for use in the hair care composition of the present invention include those that are known for their use in shampoo or other hair care and hygiene products. Non-limiting examples of suitable zwitterionic or amphoteric surfactants are described in US Patent Nos. 5,104,646 and 5,106,609, which are incorporated herein by reference in their entirety.
[0043] Amphoteric cosurfactants suitable for use in the composition include the described surfactants, such as derivatives of secondary and tertiary aliphatic amines, in which the aliphatic radical can be a straight or branched chain, and in which one of the aliphatic substituents contains from about 8 to about 18 carbon atoms, and one contains an anionic group, such as carboxy, sulfonate, sulfate, phosphate, or phosphonate. Suitable amphoteric surfactants include, but are not limited to, those selected from the group consisting of: sodium cocaminopropionate, sodium cocaminodipropionate, sodium cocoamphoacetate, sodium cocoamphodiacetate, sodium cocoamphohydroxypropylsulfonate, sodium cocoamphopropionate, sodium coramphopropionate, sodium lauraminopropionate, sodium lauroamphoacetate, sodium lauroamphoacetate, sodium lauroamphohydroxypropylsulfonate, sodium lauroamphopropionate, sodium coramphopropionate, sodium laurimine dipropionate, ammonium cocaminopropionate, ammonium cocaminodipropionate, cocoamphoamphoacetate cocoamphoacetate ammonium hydroxypropyl sulfonate, ammonium cocoamphopropionate, ammonium cornamphopropionate, ammonium lauraminopropionate, ammonium lauroamphoacetate, ammonium lauroamphohydroxypropyl sulfonate, ammonium lauroamphopropionate, ammonium cornamphopropionate, ammonium lauraminodipropionate co-thionate, amine, triethanolamine cocaminodipropionate, triethanolamine cocoamphoacetate, triethanolamine cocoamphohydroxypropylsulfonate, triethanolamine cocoamphopropionate, triethanolamine cornamphopropionate, triethanolamine lauraminopropionate, triethanolamine lauroamphoacetate, triethanolamine lauroamphopropionate, triethanolamine triethanolamine sulfonate, triethanolamine triethanolamine sulfonate acid cocoanfodipropiônico, caproanfodiacetato, disodium caproanfoadipropionato, disodium capriloanfodiacetato, disodium capriloanfodipriopionato, disodium cocoanfocarboxietil-hidroxipropilsulfonato, disodium cocoamphodiacetate, disodium cocoanfodipropionato, disodium dicarboxietilcocopropilenodiamina, disodium laureth-5 carboxianfodiacetato, disodium lauriminodipropionato, disodium lauroanfodiacetato of disodium, disodium lauroamphodipropionate, disodium oleoamphodipropionate, PPG-2-isodecetyl-7 carboxyamphod disodium iacetate, lauraminopropionic acid, lauroamphodipropionic acid, lauryl aminopropylglycine, lauryl diethylenediaminoglycine and mixtures thereof.
[0044] The composition may comprise a zwitterionic cosurfactant, in which the zwitterionic cosurfactant is a derivative of aliphatic quaternary ammonium compounds, phosphonium and sulfonium, in which the aliphatic radicals may be straight-chain or branched and in which one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic group such as carboxy, sulfonate, sulfate, phosphate, or phosphonate. The zwitterionic surfactant can be selected from the group consisting of cocamido ethyl betaine, cocamido propylamine oxide, cocamido propyl betaine, collagen hydrolyzed with cocamido propyl dimethylaminohydroxypropyl, collagen hydrolyzed with cocamido propyl dimonium hydroxypropyl hydroxy, cocamido propyl hydroxypropyl sultaine, cocobetaine coco-betaine, coco-hydroxy sultaine, coco/oleamidopropyl betaine, coco-sultaine, lauramide propyl betaine, lauryl betaine, lauryl hydroxy sultaine and lauryl sultaine and mixtures thereof.
Nonionic surfactants suitable for use in the present invention include those described in Detergents and Emulsifiers ("Detergents and Emulsifiers"), by McCutcheon, US edition (1986), by Allured Publishing Corp., and in Functional Materials ( "Functional materials"), by McCutcheon, North American edition (1992). Suitable nonionic surfactants for use in the personal care compositions of the present invention include, but are not limited to, polyoxyethylene alkyl phenols, polyoxyethylene alcohols, polyoxyethylene polyoxypropylene glycols, glyceryl esters of alkanoic acids, polyglyceryl esters of alkanoic acids, esters of propylene glycol of alkanoic acids, sorbitol esters of alkanoic acids, polyoxyethylenated sorbitol esters of alkanoic acids, polyoxyethylene glycol esters of alkanoic acids, polyoxyethylenated alkanoic acids, alkanolamides, N-alkyl pyrrolidones, alkyl glycosides, alkyl polyglycosides alkylamine and polyoxyethylene silicones.
[0046] The cosurfactant can be a nonionic surfactant selected from the group including alkanolamides: Cocamide, methyl MEA cocamide, DEA cocamide, MEA cocamide, MIPA cocamide, DEA lauramide, MEA lauramide, MIPA lauramide, DEA myristamide, MEA myristamide, MEA PEG-20 cocamide, PEG-2 cocamide, PEG-3 cocamide, PEG-4 cocamide, PEG-5 cocamide, PEG-6 cocamide, PEG-7 cocamide, PEG-3 lauramide, PEG-5 lauramide, PEG-3 oleamide, PPG-2 cocamide, PPG-2 hydroxyethyl cocamide, PPG-2 hydroxyethyl isostearamide and mixtures thereof.
Representative polyoxyethylenated alcohols include alkyl chains in the range of C9-C16 and having from about 1 to about 110 alkoxy groups including, but not limited to, lauret-3, lauret-23, cete-10, stearete- 10, stearete-100, behenet-10, all commercially available from Shell Chemicals, Houston, Texas, USA under the tradenames Neodol® 91, Neodol® 23, Neodol® 25, Neodol® 45, Neodol® 135, Neodo® 167, Neodol® PC 100, Neodol® PC 200, Neodol® PC 600, and mixtures thereof.
Also commercially available are polyoxy ethylene fatty ethers, commercially available under the tradename Brij®, from Uniqema, Wilmington, Delaware, USA, including but not limited to Brij® 30, Brij® 35, Brij® 52, Brij® 56, Brij® 58, Brij® 72, Brij® 76, Brij® 78, Brij® 93, Brij® 97, Brij® 98, Brij® 721 and mixtures thereof.
[0049] Suitable alkyl glycosides and alkyl polyglycosides can be represented by the formula (S)n-O-R where S is a sugar moiety such as glucose, fructose, mannose, galactose and the like; n is an integer from about 1 to about 1,000, and R is a C8-C30 alkyl group. Examples of long-chain alcohols from which the alkyl group can be derived include decyl alcohol, lauryl alcohol, myristyl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol and the like. Examples of such surfactants include alkyl polyglycosides where S is a glucose moiety, R is a C8-20 alkyl group, and n is an integer from about 1 to about 9. Commercially available examples of such surfactants include decyl polyglycoside and lauryl polyglycoside, available under the trade names APG® 325 CS, APG® 600 CS, and APG® 625 CS) from Cognis, of Ambler, Pa, USA. Also useful in the present invention are sucrose ester based surfactants such as sucrose cocoate and sucrose laurate as well as alkyl polyglycosides, available under the trade names Triton™ BG-10 and Triton™ CG-110, from the Dow Chemical Company, from Houston, TX, USA.
[0050] Other nonionic surfactants suitable for use in the present invention are glyceryl esters and polyglyceryl esters, including but not limited to C12 glyceryl monoesters, glyceryl monoesters of -22 saturated, unsaturated and chain fatty acids branched as glyceryl oleate, glyceryl monostearate, glyceryl monopalmitate, glyceryl monobehenate C12 and mixtures thereof, and polyglyceryl esters of -22 saturated, unsaturated and branched chain fatty acids as polyglyceryl-4 isostearate, polyglyceryl-3 oleate polyglyceryl-2 sesquioleate, triglyceryl diisostearate, diglyceryl monooleate, tetraglyceryl monooleate and mixtures thereof.
[0051] Also usable here as non-ionic surfactants are sorbitan esters. C12 sorbitan esters of -22 saturated, unsaturated and branched chain fatty acids are useful in the present invention. Such sorbitan esters generally comprise mixtures of mono-, di-, tri-esters, etc. Representative examples of suitable sorbitan esters include sorbitan monolaurate (SPAN® 20), sorbitan monopalmitate (SPAN® 40), sorbitan monostearate (SPAN® 60), sorbitan tristearate (SPAN® 65), sorbitan monooleate (SPAN® 80), sorbitan trioleate (SPAN® 85) and sorbitan isostearate.
Also suitable for use in the present invention are alkoxylated derivatives of sorbitan esters including, but not limited to, polyoxy ethylene (20) sorbitan monolaurate (Tween® 20), polyoxy ethylene (20) sorbitan monopalmitate (Tween®) 40), polyoxy ethylene (20) sorbitan monostearate (Tween® 60), polyoxy ethylene (20) sorbitan monooleate (Tween® 80), polyoxy ethylene (4) sorbitan monolaurate (Tween® 21), polyoxy monostearate ethylene (4) sorbitan (Tween® 61), polyoxy ethylene (5) sorbitan monooleate (Tween® 81) and mixtures thereof, all available from Uniqema.
Also suitable for use in the present invention are alkyl phenol ethoxylates including but not limited to nonylphenol ethoxylates (TERGITOL™ NP-4, NP-6, NP-7, NP-8, NP-9, NP- 10, NP-11, NP-12, NP-13, NP-15, NP-30, NP-40, NP-50, NP-55, NP-70 available from The Dow Chemical Company, Houston, TX, USA ) and octyl phenol ethoxylates (TRITON™ X-15, X-35, X-45, X-114, X-100, X-102, X-165, X-305, X-405, X-705 available together to The Dow Chemical Company, Houston, TX, USA).
[0054] Also suitable for use herein are tertiary alkylamine oxides, including lauramine oxide and cocamine oxide.
[0055] Non-limiting examples of other additional anionic, zwitterionic, amphoteric and non-ionic surfactants suitable for use in hair care compositions are described in McCutcheon's article, Emulsifiers and Detergents, 1989 yearbook, published by MC Publishing Co., and in US patents no. 3,929,678, 2,658,072; 2,438,091; 2,528,378, which are incorporated herein by reference in their entirety.
Suitable surfactant combinations comprise an average % by weight of alkyl branch from about 0.5% to about 30%, alternatively from about 1% to about 25%, alternatively from about 2 % to about 20%. The combination of surfactants may have an average cumulative weight % of C8 to C12 alkyl chain lengths from about 7.5% to about 25%, alternatively from about 10% to about 22.5%, alternatively , from about 10% to about 20%. The combination of surfactants may have an average C8-C12/C13-C18 alkyl chain ratio of from about 3 to about 200, alternatively from about 25 to about 175.5, alternatively from about 50 to about 150, alternatively about 75 to about 125. B. Cationic polymers
[0057] The hair care composition also comprises a cationic polymer. Such cationic polymers can include at least one of (a) a cationic guar gum polymer, (b) a cationic non-guar galactomannan polymer, (c) a cationic tapioca polymer, (d) a cationic copolymer of acrylamide monomers and cationic monomers, and/or (e) synthetic uncrosslinked cationic polymer, which may or may not form lyotropic liquid crystals in combination with the detersive surfactant (f) a cationic cellulose polymer. Additionally, the cationic polymer can be a mixture of cationic polymers.
[0058] The hair care composition may comprise a cationic guar gum polymer, which is a cationically substituted galactomannan gum (guar) derivative. Guar gum for use in preparing such guar gum derivatives is typically obtained as a naturally occurring material from the seeds of the guar plant. The guar gum molecule itself is a straight-chain mannan, which is branched at regular intervals with single-membered galactose units into alternative mannose units. The mannose units are linked together via β(1-4) glycosidic bonds. The branching of galactose takes place through an α(1-6) bond. The cationic derivatives of guar gums are obtained through the reaction between the hydroxyl groups of polygalactomannan and reactive quaternary ammonium compounds. The degree of substitution of cationic groups on the guar gum structure should be sufficient to provide the cationic charge density described above.
[0059] In one embodiment, the cationic polymer including but not limited to a cationic guar gum polymer has a weight average molecular weight less than 1.5 million g/mol, or from about 150,000 to about 1.5 million g/mol, or from about 200,000 to about 1.5 million g/mol, or from about 300,000 to about 1.2 million g/mol, or from about 750,000 thousand to about 1 million g/mol. In one embodiment, the cationic guar gum polymer has a charge density of from about 0.2 to about 2.2 meq/g or from about 0.3 to about 2.0 meq/g or from about 0.4 to about 1.8 meq/g; or from 0.5 meq/g to about 1.7 meq/g.
[0060] According to one embodiment, the cationic guar gum polymer has a weight average molecular weight less than about 1.5 million g/mol and has a charge density of about 0.1 meq/g about 2 .5 meq/g. In one embodiment, the cationic guar gum polymer has a weight average molecular weight less than 900,000 g/mol or from about 150,000 to about 800,000 g/mol or from about 200,000 to about 700,000 g/mol. mol or from about 300,000 to about 700,000 g/mol or from about 400,000 to about 600,000 g/mol, from about 150,000 to about 800,000 g/mol or from about 200,000 to about 700,000 g/mol or from about 300,000 to about 700,000 g/mol or from about 400,000 to about 600,000 g/mol. In one embodiment, the cationic guar gum polymer has a charge density of from about 0.2 to about 2.2 meq/g or from about 0.3 to about 2.0 meq/g or from about 0.4 to about 1.8 meq/g; or from 0.5 meq/g to about 1.5 meq/g.
The hair care composition may comprise from about 0.05% to about 1%, from about 0.05% to about 0.9%, from about 0.1% to about from 0.8%, or from about 0.2% to about 0.7% cationic polymer (a), by total weight of the composition.
[0062] Cationic guar gum polymer can be formed from quaternary ammonium compounds. In one embodiment, the quaternary ammonium compounds to form the cationic guar gum polymer fit the general formula:
wherein R3, R4 and R5 are methyl or ethyl groups; R6 is an epoxy alkyl group with the following general formula 2
or R6 is a halohydrin group with the following general formula 3:
wherein R7 is a C1 to C3 alkylene; X is chlorine or bromine and Z is an anion such as Cl-, Br-, I- or HSO4-.
[0063] In one embodiment, the cationic guar gum polymer conforms to general formula 4:
where R8 is guar gum; and wherein R4, R5, R6 and R7 are as defined above; and where Z is a halogen. In one embodiment, the cationic guar gum polymer conforms to formula 5:

[0064] Other suitable cationic guar gum polymers include cationic guar gum derivatives such as hydroxypropyl triammonium guar gum chloride. In one embodiment, the cationic guar gum polymer is a hydroxypropyl triammonium guar gum chloride. Specific examples of guar hydroxypropyltrimonium chlorides include the Jaguar® series commercially available from Solvay, for example Jaguar® C-500, commercially available from Solvay. Jaguar® C-500 has a charge density of 0.8 meq/g and a molecular weight of 500,000 g/mol. Other suitable guar hydroxypropyltrimonium chlorides are: guar hydroxypropyltrimonium chloride, which has a charge density of about 1.1 meq/g and a molecular weight of about 500,000 g/mol, is available from ASI, a density of loading of about 1.5 meq/g and a molecular weight of about 500,000 g/mol is available from ASI. Other guar hydroxypropyltrimonium chlorides are suitable: Hi-Care 1000, which has a charge density of about 0.7 meq/g and a molecular weight of about 600,000 g/mol and is disposed with the Solvay; N-Hance 3269 and N-Hance 3270, which have a charge density of about 0.7 meq/g and a molecular weight of about 425,000 g/mol and are available from ASI; Hi-Care 3196, which has a charge density of about 0.8 meq/g and a molecular weight of about 1,100,000 g/mol and is available from ASI; AquaCat CG518 has a charge density of about 0.9 meq/g and a molecular weight of about 50,000 g/mol and is arranged close to the ASI. BF-13, which is a borate (boron) free guar gum of charge density of about 1.1 meq/g and molecular weight of about 800,000 and BF-17, which is a borate (boron) free guar gum of charge density of about 1.7 meq/g and molecular weight of about 800,000, both available from ASI.
The hair care compositions of the present invention may comprise a galactomannan polymer derivative with a mannose to galactose ratio greater than 2:1 on a monomer to monomer basis; the galactomannan polymer derivative selected from the group consisting of a cationic galactomannan polymer derivative and an amphoteric galactomannan polymer derivative having a net positive charge. For use herein, the term "cationic galactomannan" refers to a polymer of galactomannan to which a cationic group is added. The term "amphoteric galactomannan" refers to a polymer of galactomannan to which a cationic group and an anionic group are added so that the polymer has a net positive charge.
[0066] Galactomannan polymers are present in the endosperm of seeds of the Legume family. Galactomannan polymers are created from a combination of mannose monomers and galactose monomers. The galactomannan molecule is a straight-chain mannan branched at regular intervals with single-membered galactose units into specific mannose units. The mannose units are linked together via β(1-4) glycosidic bonds. The branching of galactose takes place through an α(1-6) bond. The ratio of mannose monomers to galactose monomers varies according to plant species and is also affected by climate. The non-guar galactomannan polymer derivatives of the present invention have a mannose to galactose ratio greater than 2:1 on a monomer to monomer basis. Suitable mannose to galactose ratios can be greater than about 3:1 and the mannose to galactose ratio can be greater than about 4:1. Analysis of mannose to galactose ratios is well known in the art and is typically based on measuring the galactose content.
[0067] The gum for use in preparing the non-guar galactomannan polymer derivatives is typically obtained in the form of a naturally occurring material such as seeds or grains from plants. Examples of various non-guar galactomannan polymers include but are not limited to tara gum (3 parts mannose/1 part galactose), carob or locust bean (4 parts mannose/1 part galactose) and cassia gum (5 parts mannose/1 part galactose ).
[0068] In one embodiment of the invention, the non-guar galactomannan polymer derivatives have a molecular weight of from about 1,000 to about 10,000,000 and/or from about 5,000 to about 3,000,000.
The hair care compositions of the invention may also include galactomannan polymer derivatives having a cationic charge density from about 0.5 meq/g to about 7 meq/g. In one embodiment of the present invention, the galactomannan polymer derivatives have a cationic charge density from about 1 meq/g to about 5 meq/g. The degree of substitution of cationic groups on the galactomannan structure needs to be sufficient to provide the cationic charge density described above.
[0070] The galactomannan polymer derivative can be a cationic derivative of the non-guar galactomannan polymer, which is obtained by the reaction between the hydroxyl groups of the polygalactomannan polymer and reactive quaternary ammonium compounds. Suitable quaternary ammonium compounds for use in forming the cationic galactomannan polymer derivatives include those according to general formulas 1 to 5 as defined above:
[0071] Cationic non-guar galactomannan polymer derivatives formed from the reagents described above are represented by the general formula:
where R is the gum. The cationic galactomannan derivative may be a hydroxypropyltrimethylammonium chloride gum, which may be more specifically represented by general formula 7:

[0072] Alternatively, the galactomannan polymer derivative may be an amphoteric galactomannan polymer derivative having a net positive charge, obtained when the cationic galactomannan polymer derivative further comprises an anionic group.
Cationic non-guar galactomannan may have a mannose to galactose ratio greater than about 4:1, a molecular weight of about 1,000 g/mol to about 10,000,000 g/mol, and/or of about 50,000 g/mol to about 1,000,000 g/mol, and/or from about 100,000 g/mol to about 900,000 g/mol, and/or from about 150,000 g/mol to 400,000 g/mol and about a cationic charge density of about 1 meq/g to 5 meq/g, about, and/or about 2 meq/g to 4 meq/g, and can be derived from a cassia plant.
Hair care compositions may comprise at least about 0.05% of a galactomannan polymer derivative by weight of the composition, alternatively from about 0.05% to about 2% by weight of the composition of a polymer derivative of galactomannan.
Hair care compositions may comprise water-soluble cationically modified starch polymers. For use herein, the term "cationically modified" refers to a starch to which a cationic group is added prior to degradation of the starch to a lower molecular weight, or to a starch to which a cationic group is added after modification. of the starch to obtain a desired molecular weight. The definition of "cationically modified starch" encompasses amphoterically modified starches. The term "amphoterically modified starch" refers to a hydrolyzed starch to which a cationic group and an anionic group are added.
Hair care compositions may comprise cationically modified starch polymers in a range of from about 0.01% to about 10% and/or from about 0.05% to about 5% by weight of the composition .
[0077] The cationically modified starch polymers presented in the present invention have a percentage of bound nitrogen from about 0.5% to about 4%.
The cationically modified starch polymers for use in hair care compositions can have a molecular weight from about 850,000 g/mol to about 1,500,000 g/mol and/or from about 900,000 g/mol to about of 1,500,000 g/mol.
Hair care compositions may include cationically modified starch polymers having a charge density of about 0.2 meq/g about 5 meq/g and/or about 0.2 meq/g about 2 meq/g. Chemical modification to obtain such charge density includes, but is not limited to, the addition of amino groups and/or ammonium groups to starch molecules. Some non-limiting examples of these ammonium groups may include substituents such as hydroxy propyl trimonium chloride, trimethyl hydroxy propyl ammonium chloride, dimethyl stearyl hydroxy propyl ammonium chloride and dimethyl dodecyl hydroxy propyl ammonium chloride. See Solarek, D.B., Cationic Starches in Modified Starches: Properties and Uses, Wurzburg, O.B., Ed., CRC Press, Inc., Boca Raton, Florida, USA. 1986, pages 113 to 125. Cationic groups may be added to starch prior to degradation to a lower molecular weight or may be added after such modification.
[0080] Cationically modified starch polymers generally have a degree of cationic group substitution from about 0.2 to about 2.5. For use in the present invention, the "degree of substitution" of cationically modified starch polymers is the average of the number of hydroxyl groups on each anhydroglucose unit that is derivatized by substituent groups. Since each anhydroglucose unit has three hydroxyl groups potentially available for substitution, the maximum possible degree of substitution is 3. The degree of substitution is expressed as the number of moles of substituting groups per mole of anhydroglucose units, on an average molar basis . The degree of substitution can be determined using proton nuclear magnetic resonance ("sup.1H NMR") spectroscopy methods well known in the art. The techniques of.sup. 1 H NMR include those described in "Observation on NMR Spectra of Starches in Dimethyl Sulfoxide, Iodine-Complexing, and Solvating in Water-Dimethyl Sulfoxide", Qin-Ji Peng and Arthur S. Perlin, Carbohydrate Research, 160 (1987), 57 at 72; and "An Approach to the Structural Analysis of Oligosaccharides by NMR Spectroscopy", J. Howard Bradbury and J. Grant Collins, Carbohydrate Research, 71, (1979), 15 to 25.
[0081]The starch source before chemical modification can be chosen from a variety such as tubers, legumes, cereals and grains. Some non-limiting examples of these sources may include corn starch, wheat starch, rice starch, waxy corn starch, oat starch, cassava starch, waxy barley, waxy rice starch, glutenous rice starch, rice starch candy, amioca, potato starch, tapioca starch, oat starch, sago starch, rice pudding, or mixtures of these items.
[0082] Cationically modified starch polymers can be selected from degraded cationic corn starch, cationic tapioca, cationic potato starch, and mixtures thereof. Alternatively, the cationically modified starch polymers are cationic corn starch and cationic tapioca.
[0083] Starch, before degradation or after modification to a lower molecular weight, may comprise one or more additional modifications. For example, such modifications can include cross-linking, stabilization reactions, phosphorylations and hydrolysations. Stabilization reactions can include alkylation and esterification.
[0084] Cationically modified starch polymers can be incorporated into the composition in the form of hydrolyzed starch (for example, acid, enzyme, or alkaline degradation), oxidized starch (for example, peroxide, peracid, hypochlorite, alkaline, or any other oxidizing agent), physically or mechanically degraded starch (eg through thermomechanical energy input from processing equipment), or combinations thereof.
[0085] An optimal form of starch is one that is readily soluble in water, and forms a substantially clear solution (% transmittance of about 80 to 600 nm) in water. The transparency of the composition is measured by ultraviolet/visible (UV/VIS) spectrophotometry, which determines the absorption or transmission of UV/VIS light by a sample, using a Gretag Macbeth Color i 5 colorimeter, according to the related instructions. A wavelength of light of 600 nm proved to be suitable for characterizing the degree of clarity of cosmetic compositions.
[0086] Cationically modified starch suitable for use in hair care compositions is available from known starch suppliers. Also suitable for use in hair care compositions is non-ionic modified starch which can be further derivatized to a cationically modified starch as is known in the art. Other suitable modified starch-based starting materials can be quaternized, as is known in the art, to produce the cationically modified starch polymer suitable for use in hair care compositions.
[0087] Starch Degradation Procedure: An aqueous starch slurry can be prepared by mixing granular starch in water. The temperature is raised to about 35°C. An aqueous solution of potassium permanganate is then added at a concentration of about 50 ppm, based on the amount of starch. The pH is raised to about 11.5 with sodium hydroxide, and the aqueous slurry is stirred enough to prevent the starch from settling. Next, a solution of hydrogen peroxide diluted to about 30% in water is added to a content of about 1% peroxide, based on the amount of starch. The pH of about 11.5 is then restored by adding additional sodium hydroxide. The reaction is complete after a period of about 1 to about 20 hours. The mixture is then neutralized with dilute hydrochloric acid. Degraded starch is recovered by filtration followed by washing and drying.
[0088] The hair care composition may comprise a cationic copolymer of an acrylamide monomer and a cationic monomer, wherein the copolymer has a charge density of about 1.0 meq/g to about 3.0 meq/g . The cationic copolymer can be a synthetic cationic copolymer of acrylamide monomers and cationic monomers.
[0089] The cationic copolymer may comprise: (i) an acrylamide monomer of the following formula AM:
Formula AM where R9 is H or C1-4 alkyl; and R10 and R11 are independently selected from the group consisting of H, C1-4 alkyl, CH2OCH3, CH2OCH2CH(CH3)2 and phenyl, or together are C3-6 cycloalkyl; and (ii) a cationic monomer according to formula CM:
Formula CM where k =1, each of v, v' and v'' is independently an integer from 1 to 6, w is zero or an integer from 1 to 10, and X- is an anion.
[0090] The cationic monomer can adapt to the formula CM and where k = 1, v = 3 and w = 0, z = 1 and X- is Cl- to form the following structure:

[0091] The above structure can be called diquaternary. Alternatively, the cationic monomer can adapt to the formula CM and where v and v'' are each 3, v' = 1, w =1, y = 1 and X- is Cl-, such as:

[0092]The structure above can be called triquaternary.
Suitable acrylamide monomer includes, but is not limited to acrylamide or methacrylamide.
[0094] The cationic copolymer (b) can be AM:TRIQUAT which is a copolymer of acrylamide and 1,3-Propandiammonium, N-[2-[[[dimethyl[3-[(2-methyl-1-oxo-2) - propenyl)amino]propyl]ammonium]acetyl]amino]ethyl]2-hydroxy-N,N,N',N',N'-pentamethyl-, trichloride. AM:TRIQUAT is also known as polyquaternium 76 (PQ76). AM:TRIQUAT can have a charge density of 1.6 meq/g and a molecular weight of 1.1 million g/mol.
[0095] In an alternative embodiment, the cationic copolymer is an acrylamide monomer and a cationic monomer, in which the cationic monomer is selected from the group consisting of: dimethylaminoethyl (meth)acrylate, dimethylaminopropyl (meth)acrylate, ( ditert-butylaminoethyl meth)acrylate, dimethylaminomethyl (meth)acrylamide, dimethylaminopropyl (meth)acrylamide; ethylenimine, vinyl amine, 2-vinylpyridine, 4-vinylpyridine; ethyl ( trimethyl ammonium meth)acrylamide, propyl (meth)acrylamide of trimethyl ammonium chloride, vinylbenzyl trimethyl ammonium chloride, diallyl dimethyl ammonium chloride and mixtures thereof.
[0096] The cationic copolymer may comprise a cationic monomer selected from the group consisting of: cationic monomers which include trimethylammonium ethyl (meth)acrylate chloride, trimethylammonium ethyl (meth)acrylate methyl sulfate, ethyl benzyl (meth) acrylate dimethylammonium acrylate, 4-benzoylbenzyl dimethylammonium ethyl acrylate chloride, trimethylammonium ethyl(meth)acrylamide chloride, trimethylammonium propyl(meth)acrylamide chloride, vinylbenzyl trimethylammonium chloride, diallyl dimethylammonium chloride and mixtures thereof.
[0097] The cationic copolymer can be soluble in water. The cationic copolymer is formed from (1) copolymers of (meth)acrylamide and cationic monomers based on (meth)acrylamide and/or cationic hydrolysis stable monomers, (2) terpolymers of (meth)acrylamide, monomers based on cationic (meth)acrylic acid esters and (meth)acrylamide-based monomers and/or stable hydrolysis cationic monomers. Cationic (meth)acrylic acid ester-based monomers can be cationized (meth)acrylic acid esters containing a quaternized N atom. In one embodiment, the cationized (meth)acrylic acid esters containing a quaternized N atom are dialkyl amino alkyl (meth)acrylates quaternized with C1 to C3 in the alkyl and alkylene groups. Suitable cationized esters of (meth)acrylic acid containing a quaternized N atom may be selected from the group consisting of: ammonium salts of dimethylaminomethyl (meth)acrylate, dimethylaminoethyl (meth)acrylate, dimethylaminopropyl (meth)acrylate, ( diethylaminomethyl meth)acrylate, diethylaminoethyl (meth)acrylate; and diethylaminopropyl (meth)acrylate quaternized with methyl chloride. In one embodiment, cationized esters of (meth)acrylic acid containing a quaternized N atom, dimethylaminoethyl acrylate, which is quaternized with an alkyl halide, or with methyl chloride or benzyl chloride or dimethyl sulfate (ADAME-Quaternary) , the cationic monomer when based on (meth)acrylamides can be dialkyl (meth)acrylamides quaternized with C1 to C3 in the alkyl and alkylene groups, or dimethyl aminopropylacrylamide, which is quaternized with an alkyl halide, or methyl chloride or benzyl chloride or dimethyl sulfate.
Suitable cationic monomer based on a (meth)acrylamide includes a quaternized dialkyl amino alkyl(meth)acrylamide with C1 to C3 in the alkyl and alkylene groups. The cationic monomer based on a (meth)acrylamide can be dimethylaminopropylacrylamide, which is quaternized with an alkyl halide, specifically methyl chloride or benzyl chloride or dimethyl sulfate.
[0099] The cationic monomer can be a cationic monomer with stable hydrolysis. Cationic monomers with stable hydrolysis can be, in addition to dialkyl amino alkyl(meth)acrylamide, all monomers which can be observed as stable by the OECD hydrolysis test. The cationic monomer can be hydrolysis stable and the hydrolysis stable cationic monomer can be selected from the group consisting of: diallyl dimethylammonium chloride and water soluble cationic styrene derivatives.
[0100] The cationic copolymer can be a terpolymer of acrylamide, 2-dimethylammoniomethyl(meth)acrylate quaternized with methyl chloride (ADAME-Q) and 3-dimethylammoniopropyl(meth)acrylamide quaternized with methyl chloride (DIMAPA-Q). The cationic copolymer can be formed from acrylamide and acrylamidopropyltrimethylammonium chloride, where acrylamidopropyltrimethylammonium chloride has a charge density from about 1.0 meq/g to about 3.0 meq/g.
[0101] The cationic copolymer can have a charge density of about 1.1 meq/g or about 2.5 meq/g or about 1.1 meq/g about 2.3 meq/g or about 1.2 meq/g about 2.2 meq/g or about 1.2 meq/g about 2.1 meq/g or about 1.3 meq/g about 2.0 meq/g g or from about 1.3 meq/g to about 1.9 meq/g.
[0102] The cationic copolymer can have a molecular weight from about 100,000 g/mol to about 1.5 million g/mol or from about 300,000 g/mol to about 1.5 million g/mol or from about 500,000 g/mol to about 1.5 million g/mol or from about 700,000 g/mol to about 1.0 million g/mol or from about 900,000 g/mol to about 1, 2 million g/mol.
[0103]The cationic copolymer can be a copolymer of trimethylammoniopropylmethacrylamide chloride-N-acrylamide, which is also known as AM:MAPTAC. AM:MAPTAC can have a charge density of about 1.3 meq/g and a molecular weight of about 1.1 million g/mol. The cationic copolymer can be AM:ATPAC. AM:ATPAC can have a charge density of about 1.8 meq/g and a molecular weight of about 1.1 million g/mol. (a) Synthetic Cationic Polymers
[0104] The hair care composition can comprise a synthetic polymer that can be formed from i) one or more cationic monomeric units, and optionally ii) one or more monomeric units that have a negative charge, and/or iii) a non-ionic monomer, the subsequent charge of the copolymer being positive. The ratio between the three types of monomers is given by "m", "p" and "q", where "m" is the number of cationic monomers, "p" is the number of monomers that have a negative charge, and "q " is the number of non-ionic monomers.
[0105] Cationic polymers can be water-soluble or dispersible, not cross-linked, and cationic synthetic polymers that have the following structure:
where A, can be one or more of the following cationic moieties:
Where @ = starch, alkyl starch, ester, ether, alkyl or alkyl aryl. Where Y = C1-C22 alkyl, alkoxy, alkylidene, alkyl or aryloxy Where y = C1-C22 alkyl, alkyloxy, alkyl aryl or alkyl aryloxy. Where Z = C1-C22 alkyl, alkyloxy, aryl or aryloxy Where R1 = H, linear or branched C1-C4 alkyl Where s = 0 or 1, n = 0 or > 1 Where T and R7 = C1-C22 alkyl and Where X - = halogen, hydroxide, alkoxide, sulfate or alkyl sulfate Where the monomer that has a negative charge is defined by R2' = H, linear or branched alkyl C1-C4 and R3 as:
where D is O, N or S; Where Q = NH2 or O Where u = 1-6 Where t = 0-1 and Where J = oxygenated functional group containing the following elements P, S, C Where nonionic monomer is defined by R2'' = H, linear alkyl or C1-C4 branched, R6 = straight or branched alkyl, alkyl aryl, aryloxy, alkyloxy, alkyl aryloxy and β is defined as
Where G' and G'' are, independently of each other, O, S or N-H and L = 0 or 1.
[0106]Examples of cationic monomers include (meth)acrylamides; monomers comprising at least one secondary, tertiary or quaternary amine function, or a heterocyclic group containing a nitrogen, vinyl amine or ethylenimine atom; diallyl dialkyl ammonium salts; their mixtures, their salts, and macromonomers that derive from them.
[0107] Additional examples of cationic monomers include dimethyl amino ethyl(meth)acrylate, dimethyl aminopropyl(meth)acrylate, diterthiobutylaminoethyl(meth)acrylate, dimethylaminomethyl(meth)acrylamide, dimethylaminopropyl(meth)acrylamide, ethylenimine , vinyl amine, 2-vinylpyridine, 4-vinylpyridine, ethyl trimethyl ammonium chloride (meth)acrylate, ethyl trimethyl ammonium methyl sulfate (meth)acrylate, ethyl dimethyl ammonium benzyl chloride ethyl (meth)acrylate, 4-benzoylbenzyl dimethyl chloride ethyl ammonium acrylate, ethyl trimethyl ammonium chloride (meth)acrylamide, propyl trimethyl ammonium chloride (meth)acrylamide, vinylbenzyl trimethyl ammonium chloride, diallyl dimethyl ammonium chloride.
[0108] Suitable cationic monomers include those comprising a quaternary ammonium group of the formula -NR3+, where R, which is identical or different, represents a hydrogen atom, an alkyl group comprising from 1 to 10 carbon atoms, or a benzyl group, optionally bearing a hydroxyl group, and comprise an anion (counterion). Examples of anions are halides such as chlorides, bromides, sulphates, hydrosulphates, alkylsulphates (eg comprising 1 to 6 carbon atoms), phosphates, citrates, formates and acetates.
[0109] Suitable cationic monomers include ethyl trimethyl ammonium chloride (meth)acrylate, ethyl trimethyl ammonium methyl sulfate (meth)acrylate, ethyl dimethyl ammonium benzyl chloride (meth)acrylate, 4-benzoylbenzyl dimethyl ammonium acrylate ethyl chloride, ethyl (meth)acrylamide trimethyl ammonium chloride, propyl (meth)acrylamide trimethyl ammonium chloride, vinylbenzyl trimethyl ammonium chloride.
[0110] Additional suitable cationic monomers include propyl (meth)acrylamide trimethyl ammonium chloride.
[0111]Examples of monomers with a negative charge include ethylenically unsaturated alpha monomers comprising a phosphate or phosphonate group, alpha ethylenically unsaturated monocarboxylic acids, alpha ethylenically unsaturated dicarboxylic acid monoalkylesters, alpha ethylenically unsaturated dicarboxylic acid monoalkylamides, alpha ethylenically saturated dicarboxylic acids, ethylenically insaturated dicarboxylic acids monoalkylamides comprise a sulfonic acid group, and salts of ethylenically unsaturated alpha compounds that comprise a sulfonic acid group.
[0112] Suitable monomers with a negative charge include acrylic acid, methacrylic acid, vinyl sulfonic acid, vinyl sulfonic acid salts, vinylbenzene sulfonic acid, vinylbenzene sulfonic acid salts, alpha-acrylamidomethyl propane sulfonic acid, acid salts alpha-acrylamidomethyl propanesulfonic acid, 2-sulfoethyl methacrylate, 2-sulfoethyl methacrylate salts, acrylamido-2-methylpropanesulfonic acid (AMPS), acrylamido-2-methylpropanesulfonic acid salts, and styrene sulfonate (SS).
[0113]Examples of nonionic monomers include vinyl acetate, ethylenically unsaturated alpha carboxylic acid amides, ethylenically unsaturated alpha monocarboxylic acid esters with a hydrogenated or fluorinated alcohol, polyethylene oxide (meth)acrylate (i.e., acid (meth) polyethoxylated acrylic), ethylenically unsaturated alpha dicarboxylic acid monoalkylesters, ethylenically unsaturated alpha dicarboxylic acid monoalkylamides, vinyl nitriles, vinyl amine amides, vinyl alcohol, vinyl pyrrolidone, and vinyl aromatics.
[0114] Preferred nonionic monomers include styrene, acrylamide, methacrylamide, acrylonitrile, methyl acrylate, ethyl acrylate, n-propylacrylate, n-butyl acrylate, methyl methacrylate, ethyl methacrylate, n-propyl methacrylate, n-butyl methacrylate 2-ethyl hexyl acrylate, 2-ethyl hexyl methacrylate, 2-hydroxy ethyl acrylate and 2-hydroxy ethyl methacrylate.
[0115] The anionic counterion (X-) in association with synthetic cationic polymers can be any known counterion, as long as the polymers remain soluble or dispersible in water, in the hair care composition, or in a coacervated phase of the treatment composition of the hair, and provided that the counterions are physically and chemically compatible with the essential components of the hair care composition or otherwise do not unduly impair the performance, stability or aesthetics of the product. Some non-limiting examples of these counterions include halides (eg, chlorine, fluorine, bromine, iodine), sulfate, and methylsulfate.
[0116] The cationic polymer described in the present invention, can assist in providing damaged hair, particularly chemically treated hair, a replacement hydrophobic layer F. The microscopically thin F-layer provides natural weather resistance while helping to retain moisture and prevent further damage. Chemical-based treatments damage the hair cuticle and remove its protective F-layer. As layer F is removed, hair becomes increasingly hydrophilic. It has been found that when lyotropic liquid crystals are applied to chemically treated hair, the hair becomes more hydrophobic and younger, both in appearance and in feel. Without being bound by any particular theory, it is believed that the lyotropic liquid crystal complex creates a hydrophobic layer or film that coats the hair fibers and protects it, much like the natural F-layer does. The hydrophobic layer restores hair to a generally new, healthier looking state. Lyotropic liquid crystals are formed by combining the synthetic cationic polymers described herein with the aforementioned anionic detergent surfactant component of the hair care composition. Synthetic cationic polymer has a relatively high charge density. It should be noted that some synthetic polymers that have a relatively high cationic charge density do not form lyotropic liquid crystals, mainly due to their abnormal linear charge densities. Such synthetic cationic polymers are described in WO 94/06403 by Reich et al. The synthetic polymers described in the present invention can be formulated into a stable hair care composition that provides optimized conditioning performance with respect to damaged hair.
[0117] Cationic synthetic polymers that can form lyotropic liquid crystals have a cationic charge density from 2 meq/gm to about 7 meq/gm and/or from about 3 meq/gm to about 7 meq/gm and/or from about 4 meq/gm to about 7 meq/gm. In some embodiments, the cationic charge density is about 6.2 meq/gm. Cationic polymers also have a molecular weight of from about 1,000 to about 5,000,000 and/or from about 10,000 to about 1,500,000 and/or from about 100,000 to about 1,500,000.
[0118] In another embodiment of the invention, cationic synthetic polymers that provide greater conditioning and deposition of benefit agents, but do not necessarily form lyotropic liquid crystals have a cationic charge density of about 0.7 meq/g to about 7 meq µgm and/or from about 0.8 meq/gm to about 5 meq/gm and/or from about 1.0 meq/gm to about 3 meq/gm. Polymers also have a molecular weight of from about 1,000 to about 1,500,000, from about 10,000 to about 1,500,000, and from about 100,000 to about 1,500,000.
[0119]Suitable cationic cellulose polymers are hydroxyethylcellulose salts reacted with substituted trimethylammonium epoxide, referred to in the industry (CTFA) as Polyquaternium 10 and available from Dow/Amerchol Corp. (Edison, N.J., USA) in their LR, JR and KG polymer series. Non-limiting examples include: JR-30M, KG-30M, JP, LR-400, and mixtures thereof. Other suitable types of cationic cellulose include the polymeric quaternary ammonium salts of hydroxy ethyl cellulose reacted with lauryl dimethyl ammonium substituted epoxide, referred to in the industry (CTFA) as Polyquaternium 24. These materials are available from Dow/Amerchol Corp. under the trade name Polymer LM-200. Other suitable types of cationic cellulose include polymeric quaternary ammonium salts of hydroxyethylcellulose reacted with lauryl dimethylammonium substituted epoxide and lauryl trimethylammonium substituted epoxide, referred to in the industry (CTFA) as Polyquaternium 67. These materials are available from Dow/Amerchol Corp. under the trade names SoftCAT Polymer SL-5, SoftCAT Polymer SL-30, Polymer SL-60, Polymer SL-100, Polymer SK-L, Polymer SK-M, Polymer SK-MH and Polymer SK-H.
[0120] The concentration of cationic polymers is in the range of from about 0.025% to about 5%, from about 0.1% to about 3% and/or from about 0.2% to about 1 % by weight of the hair care composition. ç. Viscosity reducing agents.
[0121] In one embodiment, the hair treatment composition described herein may comprise from about 0.1% to about 35%, alternatively from about 0.25% to about 30%, and alternatively from about from 0.5% to about 25% of a viscosity reducing agent, by weight of the hair care composition. Some non-limiting examples of suitable viscosity reducing agents include Class A materials, Class B materials, water miscible solvents, hydrotropes, and mixtures thereof.
[0122] The hair treatment composition described herein may have a liquid phase viscosity of from about 1 centipoise to about 6,000 centipoise, alternatively, from about 1 centipoise to about 4,500 centipoise, alternatively, from about 1 to about from 3,000 centipoises and, alternatively, from about 5 and to about 2,000 centipoises. 1. Class of viscosity reducing agents
[0123] Class A viscosity reducing agents may have a partition dispersion coefficient from about -3.1 to about -0.7, alternatively from about -3 to about -0.85 and, alternatively, from about -2.92 to about -0.92. Class A viscosity reducing agents may have a partition dispersion coefficient from about -3 to about -1.9, alternatively from about -2.9 to about -2, wherein one or more reducing agents of viscosity have at least 2 polar groups, or have 1 polar group and less than 5 sp3acyclic hybridized carbon atoms that are connected to each other in an adjacent group. Class A viscosity reducing agents may have a partition dispersion coefficient from about -3 to about -1.9, alternatively from about -2.9 to about -2, wherein one or more reducing agents of viscosity have 2 to 4 polar groups, or have 1 polar group and 1 to 3 acyclic sp3 hybridized carbon atoms that are connected to each other in an adjacent group. Class A viscosity reducing agents may have a partition dispersion coefficient from about -3 to about -1, alternatively from about -2.9 to about -2, wherein one or more viscosity reducing agents have 2 to 4 polar groups or have 1 polar group and 2 acyclic sp3 hybridized carbon atoms that are connected to each other in an adjacent group. Class A viscosity reducing agents can provide unexpected viscosity reduction when used in the hair care composition described herein.
[0124]The partition dispersion coefficient (PDC) is defined by the following equation: PDC= logP - 0.3001 * (δD)2 + 10.362 * δD - 93.251 where logP is the partition coefficient between octanol and water as calculated by the Consensus algorithm implemented in ACD/Percepta version 14.02 by Advanced Chemistry Development, Inc (ACD/Labs, Toronto, Canada), and where δD is the Hansen solubility dispersion parameter in (MPa)1/2 calculated using- is the program "HSPIP - Hansen Solubility Parameters in Practice" by Abbott Hiroshi and Yamamoto 4th Edition, version 4.1.07.
[0125] Viscosity reducing agents can be organic compounds containing 1 polar group, alternatively, at least 1 polar group, alternatively 2 to 4 polar groups, and alternatively, at least 2 polar groups. Polar groups can be selected from the group consisting of alcohols, aldehydes, esters, lactones, coumarins, ethers, ketones, phenols, phenyl, oxides, alkenyl, alkynyl, and combinations thereof. Viscosity reducing agents can have a molecular weight between 100 daltons and 300 daltons, alternatively from about 125 daltons to about 300 daltons. Additionally, viscosity reducing agents can have a water solubility between 23 and 25 degrees Celsius of about 900 to 50,000 mg/l.
[0126] Viscosity reducing agents may be selected from the group consisting of raspberry ketone, triethyl citrate, 5-methyl-3-heptanone oxime, hydroxycitronellal, camphor gum, 2-isopropyl-5-methyl-2-hexenal, eucalyptol , 1,1-dimethoxyoctane, isobutyl hexanoate, dihydro isojasmonate, and combinations thereof. Alternatively, viscosity reducing agents may be selected from the group consisting of raspberry ketone, triethyl citrate, hydroxycitronellal, camphor gum, and combinations thereof. Alternatively, the viscosity reducing agent can be selected from the group consisting of raspberry ketone, triethyl citrate, hydroxycitronellal, and combinations thereof. 2. Class B viscosity reducing agents
[0127] Class B viscosity reducing agents may have a partition dispersion coefficient from about 0.05 to about to about 5.1, alternatively, from about 0.08 to about 4.5, alternatively from about 0.09 to about 4.4, alternatively from about 0.05 to about 2.0, alternatively from about 0.08 to about 1.8, alternatively from about 0 .09 to about 1.7 and, alternatively, from about 0.095 to about 1.68. Class B viscosity reducing agents can provide unexpected viscosity reduction when used in the hair care composition described herein.
[0128]The partition dispersion coefficient (PDC) is defined by the following equation: PDC= logP - 0.3001 * (δD)2 + 10.362 * δD - 93.251 where logP is the partition coefficient between octanol and water calculated by Consensus algorithm implemented in ACD/Percepta version 14.02 by Advanced Chemistry Development, Inc (ACD/Labs, Toronto, Canada), and where δD is the Hansen solubility dispersion parameter in (MPa)1/2, calculated using - and the program "HSPIP - Hansen Solubility Parameters in Practice" by Abbott Hiroshi and Yamamoto, 4th Edition, version 4.1.07.
[0129] Viscosity reducing agents can be organic compounds comprising 1 polar group, alternatively at least 1 polar group, alternatively 2 to 4 polar groups, and alternatively at least 2 polar groups. Polar groups can be selected from the group consisting of alcohols, aldehydes, esters, lactones, coumarins, ethers, ketones, phenols, phenyl, oxides, alkenyl, alkynyl, and combinations thereof. Viscosity reducing agents can have a molecular weight between 100 daltons and 300 daltons, alternatively from about 125 daltons to about 300 daltons. Additionally, the viscosity reducing agents can have a water solubility between 23 and 25 degrees Celsius of about 10 to 900 mg/l.
[0130]Class B viscosity reducing agents may be selected from the group consisting of veloutone, isoamyl salicylate, gamma-terpinene, linalyl isobutyrate, alpha-terpinene, limonene, dipentene, phenyl geranyl acetate, isopropyl myristate, hexadecane, and combinations thereof. Alternatively, Class B viscosity reducing agents may be selected from the group consisting of veloutone, gamma-terpinene, linalyl isobutyrate, alpha-terpinene, limonene, dipentene, phenyl geranyl acetate, isopropyl myristate, hexadecane, and combinations thereof. Alternatively, Class B viscosity reducing agents may be selected from the group consisting of veloutone, isoamyl salicylate, gamma-terpinene, linalyl isobutyrate, alpha-terpinene, limonene, dipentene, phenyl geranyl acetate, and combinations thereof. 3. Water miscible solvents
[0131] Vehicles useful in some embodiments of the hair care composition include water and water solutions of lower alkyl alcohols, polyhydric alcohols, ketones having 3 to 4 carbon atoms, C1C6 esters of C1-C6 alcohols, sulfoxides , amides, carbonate esters, and ethoxylated and propoxylated C1-C10 alcohols, lactones, pyrrolidones, and mixtures thereof. Examples of non-limiting lower alkyl alcohols are monohydric alcohols that have 1 to 6 carbons, such as ethanol and isopropanol. Some non-limiting examples of polyhydric alcohols useful in the present invention include propylene glycol, dipropylene glycol, butylene glycols, hexylene glycol, glycerine, propanediols and mixtures thereof.
[0132] In one embodiment of the present invention, the hair care composition may comprise a hydrotrope/viscosity modifier which is an alkali metal or ammonium salt of an alkylbenzene sulfonate such as sodium xylene sulfonate, cumene sulfonate or sulfonate of sodium toluene.
[0133] In a further embodiment of the present invention, the hair care composition may comprise silicone/PEG-8 silicone/PEG-9 silicone/PEG-n silicone/silicone ether (n may be another integer), whereupon non-limiting examples include PEG8-dimethicone A208) MW 855, PEG8-dimethicone D208 MW 2706. D. Propellant or blowing agent
[0134] The concentrated hair care composition described herein may comprise from about 1% to about 10% propellant or blowing agent, alternatively from about 2% to about 8% propellant by weight of the concentrated composition to hair treatment.
[0135] The propellant or blowing agent may comprise one or more volatile materials which, in a gaseous state, may carry the other components of the concentrated hair care composition in particulate form or in droplets or as a foam. The propellant or blowing agent can have a boiling point within the range of about -45°C to about 5°C. The propellant or blowing agent can be liquefied when packaged in conventional aerosol containers under pressure. Rapid boiling of the propellant or blowing agent upon exiting the aerosol foam dispenser can aid in the atomization or foaming of the other components of the concentrated hair care composition.
[0136] Aerosol propellants or blowing agents that may be employed in the aerosol composition may include chemically inert hydrocarbons such as propane, n-butane, isobutane, cyclopropane and mixtures thereof, as well as halogenated hydrocarbons such as dichlorodifluoromethane, 1,1- dichloro-1,1,2,2-tetrafluoroethane, 1-chloro-1,1-difluoro-2,2-trifluoroethane, 1-chloro-1,1-difluoroethylene, 1,1-difluoroethane, dimethyl ether, monochlorodifluoromethane, trans -1,3,3,3-tetrafluoropropene and mixtures thereof. The propellant or blowing agent can comprise hydrocarbons such as isobutane, propane and butane - these materials can be used for their low reactivity to ozone and can be used as individual components where their vapor pressures at 21.1°C are in the range from about 1.17 bar to about 7.45 bar, alternatively from about 1.17 bar to about 4.83 bar and alternatively from about 2.14 bar to about 3.79 bar. E. Scalp Health Agents.
[0137] In one embodiment of the present invention, one or more scalp health agents can be added to provide benefits to the scalp in addition to the fungicidal/antidandruff efficacy provided by surfactant-soluble antidandruff agents. This group of materials is diverse and provides a wide range of benefits including hydration, barrier enhancement, fungicide, antimicrobial and antioxidant, anti-itch and sensory elements, and antidandruff agents such as zinc pyrithione (ZPT) or selenium sulfide. Such scalp health agents include, but are not limited to: Vitamins E and F, salicylic acid, niacinamide, caffeine, panthenol, zinc oxide, zinc carbonate, glycols, glycolic acid, PCA, PEGs, erythritol, glycerin, triclosan, lactates, hyaluronates, allantoin and other ureas, betaines, sorbitol, glutamates, xylitols, menthol, menthyl lactate, isocyclomon, benzyl alcohol, a compound comprising the following structure:
R1 is selected from H, alkyl, amino alkyl, alkoxy; Q=H2, O, -OR1, -N(R1)2, -OPO(OR1)x, -PO(OR1)x, -P(OR1)x, where x = 1-2; V=NR1, O, -OPO(OR1)x, -PO(OR1)x, -P(OR1)x, where x = 1-2; W=H2, O; X, Y = independently selected from H, aryl, naphthyl, for n=0; X, Y = aliphatic CH2 or aromatic CH for n > 1 and Z is selected from aliphatic CH2, aromatic CH, or heteroatom; A = lower alkoxy, lower alkylthio, aryl, substituted aryl or fused aryl; and the stereochemistry is variable at the positions marked with *. and natural extracts/oils including spearmint, mint, argan, jojoba and aloe. F. Optional Ingredients.
[0138] According to embodiments of the present invention, the hair care composition may further contain one or more optional ingredients, including suitable benefit agents include benefit agents, but are not limited to conditioning agents, cationic silicone polymers , anti-dandruff agents, gel nets, chelating agents, and natural oils such as sunflower oil or castor oil. Other suitable optional ingredients include, but are not limited to, perfumes, perfume microcapsules, dyes, particles, antimicrobials, defoamers, antistatic agents, rheology modifiers and thickeners, suspension materials and builders, pH adjusting agents and buffers , preservatives, pearlizing agents, solvents, thinners, antioxidants, vitamins and combinations thereof.
[0139] Such optional ingredients must be physically and chemically compatible with the components of the composition and must not otherwise unduly impair the stability, aesthetics, or performance of the product. The CTFA Cosmetic Ingredient Handbook, 10th Edition (published by Cosmetic, Toiletry, and Fragrance Association, Inc., Washington, DC, USA) (2004) (hereafter "CTFA"), describes a wide variety of non-limiting materials that can be added to the composition of the present invention. 1. Conditioning agents
[0140] The conditioning agent of the hair care compositions may be a silicone-based conditioning agent. The silicone-based conditioning agent can comprise volatile silicone, non-volatile silicone or combinations of these substances. The concentration of the silicone-based conditioning agent typically ranges from about 0.01% to about 10% by weight of the composition, from about 0.1% to about 8%, from about from 0.1% to about 5% and/or from about 0.2% to about 3%. Some non-limiting examples of suitable silicone-based conditioning agents, and optional suspending agents for the silicone, are described in reissue US Patent No. 34,584 and in US Patent No. 5,104,646 and US Patent No. 5,106,609. which descriptions are incorporated herein by reference.
[0141] Silicone-based conditioning agents for use in the compositions of the present invention may have a viscosity, as measured at 25°C, of from about 20 to about 2,000,000 centistokes ("cSt"), of about 1,000 at about 1,800,000 cSt, from about 10,000 to about 1,500,000 cSt, and from about 20,000 to about 1,500,000 cSt.
[0142] Dispersed silicone-based conditioning agent particles typically have an average diameter value in the range of about 0.01 micrometer to about 60 micrometer. For application of small particles to hair, the volume average particle diameters are typically in the range of from about 0.01 micrometers to about 4 micrometers, from about 0.01 micrometers to about 2 micrometers, from about 0 .01 micrometers to about 0.5 micrometers.
[0143] Additional material on silicones including sections discussing silicone fluids, gums and resins, as well as the manufacture of these, can be found in Encyclopedia of Polymer Science and Engineering, vol. 15, 2nd. ed., pp. 204 to 308, John Wiley & Sons, Inc. (1989), incorporated herein by reference.
[0144] Silicone emulsions suitable for use in the embodiments of the present invention include, but are not limited to, insoluble polysiloxane emulsions prepared in accordance with the descriptions given in US Patent No. 6,316,541 or US Patent No. 4,476,282 or in US patent application publication no. 2007/0276087. Accordingly, suitable insoluble polysiloxanes include polysiloxanes such as alpha, omega hydroxy terminated polysiloxanes or alpha, omega alkoxy terminated polysiloxanes which have an internal phase viscosity of about 5 cSt to about 500,000 cSt. For example, the insoluble polysiloxane can have an internal phase viscosity of less than 400,000 cSt, preferably less than 200,000 cSt, more preferably from about 10,000 cSt to about 180,000 cSt. The insoluble polysiloxane can have an average particle size within the range of about 10 nm to about 10 microns. The average particle size can range from about 15 nm to about 5 microns, from about 20 nm to about 1 micron, from about 25 nm to about 500 nm.
[0145] The average molecular weight of the insoluble polysiloxane, the internal phase viscosity of the insoluble polysiloxane, the viscosity of the silicone emulsion, and the particle size comprising the insoluble polysiloxane are determined by methods commonly used by those skilled in the art, such as the methods of present invention disclosed in Smith, AL The Analytical Chemistry of Silicones, John Wiley & Sons, Inc.: New York, 1991. For example, the viscosity of the silicone emulsion can be measured at 30°C with a Brookfield viscometer with spindle 6 to 2.5 rpm. The silicone emulsion may also contain an additional emulsifier together with the anionic surfactant,
[0146] Other classes of silicones suitable for use in the compositions of the present invention include, but are not limited to: i) silicone fluids, including, but not limited to, silicone oils, which are flowable materials having a lower viscosity that about 1,000,000 cSt measured at 25 °C; ii) aminosilicones, which contain at least one primary, secondary or tertiary amine; iii) cationic silicones, which contain at least one quaternary ammonium functional group; iv) silicone gums which include materials having a viscosity greater than or equal to 1,000,000 cSt measured at 25°C; v) silicone resins, which include highly cross-linked polymeric siloxane systems. vi) silicones with a high refractive index, having a refractive index of at least 1.46, and vii) mixtures thereof.
[0147] The conditioning agent of the hair treatment compositions of the present invention may also comprise at least one organic conditioning material such as oil or wax, either alone or in combination with other conditioning agents, such as the silicones described above. The organic material can be non-polymeric, oligomeric or polymeric. It can be in the form of oil or wax and can be added in the pure formulation or in a pre-emulsified form. Some non-limiting examples of organic conditioning materials include, but are not limited to: i) hydrocarbon oils; ii) polyolefins, iii) fatty esters, iv) fluorinated conditioning compounds, v) fatty alcohols, vi) alkyl glycosides and alkyl glycoside derivatives; vii) hydrophobic quaternary ammonium compounds; viii) polyethylene glycols and polypropylene glycols having a molecular weight of up to about 2,000,000, such as those whose CTFA names are PEG-200, PEG-400, PEG-600, PEG-1000, PEG-2M, PEG-7M, PEG-14M , PEG-45M, and mixtures thereof. 2. Emulsifiers
[0148]Several anionic and nonionic surfactants can be used in the compositions of the present invention. Anionic and nonionic emulsifiers can be monomeric or polymeric in nature. Monomeric examples include, by way of illustration and not limitation, alkyl ethoxylates, alkyl sulfates, soaps, derivatives thereof, and acids and esters. Polymeric examples include, by way of illustration and not limitation, polyacrylates, polyethylene glycols, block copolymers and, and derivatives thereof. Naturally occurring emulsifiers like lanolins, lecithin and lignin and their derivatives are also some non-limiting examples of useful emulsifiers. 3. Chelating Agents
[0149] The hair care composition may also contain a chelator. Suitable chelators include those mentioned in AE Martell & RM Smith, Critical Stability Constants, Vol. 1, Plenum Press, New York & London (1974) and AE Martell & RD Hancock, Metal Complexes in Aqueous Solution, Plenum Press, New York & London (1996) both incorporated herein by reference. When relating to chelators, the term "salts and derivatives thereof" means those salts and derivatives which comprise the same functional structure (e.g., the same chemical structure) as the chelator to which they refer and which have similar or better chelating properties. This term includes salts of alkali metals, alkaline earth, ammonium, substituted ammonium (ie, monoethanol ammonium, diethanol ammonium, triethanol ammonium), chelating esters with an acid portion and mixtures thereof, in particular, all sodium salts , potassium or ammonium. The term "derivatives" also includes "chelating surfactant" compounds, such as those exemplified in US Patent No. 5,284,972, and large molecules that comprise one or more chelating groups that have the same functional structure as the original chelators, such as polymeric EDDS (acid disuccinic ethylenediamine), described in US Patent No. 5,747,440.
[0150] The contents of the EDDA chelator in hair care compositions can be low, up to about 0.01% by weight, or even high, up to about 10% by weight, but above the higher content ( i.e. 10% by weight) there may be formulation and/or human safety concerns. In one embodiment, the content of the EDDS chelator can be at least about 0.05% by weight, at least about 0.1% by weight, at least about 0.25% by weight, at least about 0.5% by weight, at least about 1% by weight, or at least about 2% by weight of the hair care composition. Levels above about 4% by weight can be used but may not result in additional benefit. 4. Water carrier vehicle
[0151] Hair care compositions may be in the form of pourable liquids (under ambient conditions). Such compositions will therefore typically comprise a vehicle, which is present at an amount of from about 40% to about 85%, alternatively from about 45% to about 80%, alternatively from about 50% to about 75% by weight of the hair care composition. The vehicle may contain water or a miscible mixture of water and organic solvent, and, in one aspect, may comprise water with little or no significant concentration of organic solvent, except when subsequently incorporated into the composition, as minor ingredients of other essential or optional components .
[0152] The carrier usable in embodiments of the hair care compositions of the present invention includes water and aqueous solutions of lower alkyl alcohols and polyhydric alcohols. Lower alkyl alcohols useful in the present invention are monohydric alcohols having from 1 to 6 carbons, in one aspect, ethanol and isopropanol. Exemplary polyhydric alcohols usable in the present invention include propylene glycol, hexylene glycol, glycerine and propanediol. G. Foam dispenser.
[0153] The hair care composition described herein can be supplied in a foam dispenser. The foam dispenser can be an aerosol foam dispenser. The aerosol foam dispenser may comprise a reservoir for containing the hair care composition. The reservoir can be made of any suitable material selected from the group consisting of plastic, metal, alloy, laminate and combinations thereof. In one modality, the reservoir can be used only once. In one embodiment, the reservoir may be removable from the foam aerosol dispenser. Alternatively, the reservoir can be integrated into the aerosol foam dispenser. In one modality, there can be two or more reservoirs.
[0154]The foam can also be a mechanical foam dispenser. The mechanical foam dispenser described can be selected from the group consisting of compressible foam dispensers, pump foam dispensers, other mechanical foam dispensers and combinations thereof. In one embodiment, the mechanical foam dispenser is a compressible foam dispenser. Non-limiting examples of suitable pump dispensers include those described in WO 2004/078903, WO 2004/078901 and WO 2005/078063 and can be supplied by Albea (60 Electric Ave., Thomaston, CT 06787, USA) or Rieke Packaging Systems (500 West Seventh St., Auburn, Indiana 46706).
[0155] The mechanical foam dispenser may comprise a reservoir to contain the concentrated hair care composition. The reservoir can be made of any suitable material selected from the group consisting of plastic, metal, alloy, laminate and combinations thereof. The reservoir can be a refillable reservoir such as a pour-on or screw-on reservoir, or the reservoir can be a single-use reservoir. The reservoir can also be removable from the mechanical foam dispenser. Alternatively, the reservoir can be integrated with the mechanical foam dispenser. In one modality, there can be two or more reservoirs.
[0156] In one embodiment, the reservoir may be comprised of a material selected from the group consisting of rigid materials, flexible materials and combinations thereof. The reservoir may be comprised of a rigid material so as not to flatten under external atmospheric pressure when subjected to an internal partial vacuum. H. Product shape
[0157] The hair care compositions of the present invention may be presented in typical hair care formulations. They can be in the form of solutions, dispersions, emulsions, powders, talcs, encapsulates, spheres, sponges, solid dosage forms, foams and other application mechanisms. The compositions of the embodiments of the present invention can be hair tonics, leave-in hair products such as hair care and styling products, rinse-off hair products such as shampoos and personal care products and care products; and any other way that can be applied to hair. I. Applicator
[0158] In one embodiment of the present invention, the hair care composition can be dispensed from an applicator for dispensing directly into the scalp area. Direct dispensing onto the scalp, through the targeted application of an applicator, allows the deposition of undiluted cleaning agents directly where cleaning needs are greatest. This also minimizes the risk of eye contact with the cleaning solution.
[0159]The applicator is attached or can be attached to a bottle containing the hair care cleansing composition. The applicator can consist of a base that retains or extends to a single tip or a plurality of tips. The tips have openings that can be located at the end, or at any point between the tip and the base. These openings allow the product to be dispensed from the bottle directly onto the hair and/or scalp.
[0160]Alternatively, the applicator can also consist of fixed or brush-shaped bristles or extending from a base. In this case, the product can be dispensed from the base and the bristles can allow the product to be distributed through the movement of combing or brushing.
[0161]The applicator and tip design and materials can also be optimized to allow scalp massage. In this case, it may be beneficial for the geometry of the tip or bristles at the ends to be more rounded similar to the ball applicator used for eye creams. It may also be beneficial for the materials to be smoother and softer; for example, metal or metal-like finishes, "rubber materials". viscosity measurement
[0162]Shampoo viscosities can be measured in a 2.5 ml sample using a Brookfield RS cone and plate rheometer with a C75 cone for 1 to 2 s-1 at 27°C for 3 min. Measurement of diffusion coefficients by NMR
[0163] Cleaning compositions containing surfactant soluble agent are diluted with deionized water to a surfactant concentration of about 1.3%. The dilution factor is believed to be representative of a cleaning composition when applied to a head during use. Diluted samples are introduced into 5 mm NMR tubes without further preparation. No deuterated solvents are present, so all experiments are run unlocked. Diffusion coefficients are determined using the vendor supplied pulse sequence ("ledbpgppr2s", echo stimulated with bipolar gradients, longitudinal eddy current delay, presaturation and 2 degraded gradients) using a Bruker Avance 700 MHz equipped NMR spectrometer with a BBO z gradient probe. Gradient pulse durations ranged from 3,000 to 6,000 us, with diffusion periods of 150 ms. 32 linearly spaced gradient values are used in the 2% to 95% range of 10 A current from a GREAT 3/10 amplifier, with resultant gradient forces given by 5 Gauss/cm/A. Data is processed using software available from vendors.
[0164]The diffusion coefficient of the micelle surfactant is designated as DS and the diffusion coefficient of the surfactant soluble agent is designated as DA. The ratio between the diffusion coefficient of the surfactant and the diffusion coefficient of the surfactant soluble agent can be calculated using the following equation:
Measurement of Soluble Agent Deposition in Surfactants
[0165] The deposition of the surfactant-soluble agent in vivo on the scalp can be determined by extracting the agent into ethanol after the scalp has been treated with a cleaning composition containing surfactant-soluble agent and rinsed. The agent concentration in the ethanol extraction solvent is measured by HPLC. Quantification is done by reference to a standard curve. The concentration detected by HPLC is converted to a collected amount using the concentration in grams multiplied by volume.
[0166]The percentage of agent deposited can be calculated using the following equation:

[0167]Deposition efficiency can be calculated using the following equation;
Preparation of shampoo compositions
[0168]Shampoo compositions are prepared by adding surfactants, anti-dandruff agents, perfumes, viscosity modifiers, cationic polymers, and the remainder of the water with ample agitation to ensure a homogeneous mixture. The mixture can be heated to 50 to 75°C to accelerate solubilization of the soluble agents, then cooled. The pH of the product can be adjusted as needed to obtain shampoo compositions of the present invention that are suitable for application to human hair and scalp, and can vary based on the selection of detersive surfactants, fatty alcohols and/or other components specific. Non-limiting examples
[0169] The compositions illustrated in the Examples below are prepared by conventional formulation and mixing methods. All exemplified amounts are stated as percent by weight on an active basis and exclude minor materials such as diluents, preservatives, color solutions, imaging ingredients, botanicals and so on, unless otherwise specified. All percentages are based on weight unless otherwise noted.
Discussion of Results for Examples 1 to 2
[0170] For Example 1, the diffusion coefficient ratio (DS/DA) is close to 1.0, which indicates that piroctone olamine is diffusing at the same rate as the SLE1S micelles, implying that piroctone olamine is within the SLE1S micelles. However, the (DS/DA) ratio for Example 2 is significantly greater than 1.0, which indicates that piroctone olamine is diffusing at a different rate than sodium undecyl sulfate micelles, suggesting that piroctone olamine is not diffusing. finds sodium undecyl sulfate within micelles. The implications of piroctone olamine not being within the surfactant micelles in Example 2 are reflected in the greatly increased deposition efficiency of Example 2 which is 3.6X that of Example 1 (control).


Discussion of Results for Examples 3 to 8
[0171] Not even decreasing the surfactant contents, as in Examples 4 and 6, and decreasing the product viscosity, as in Example 8, significantly impacted the deposition efficiency versus their respective controls, Examples 3, 5 and 7. In fact, Examples 4, 6, and 8 demonstrate deposition efficiencies in the 0.9 to 1.2X range as their respective controls.
[0172] Examples 9 to 13 below further exemplify embodiments of the present invention.


Sample preparation method for microscopy
[0173]10:1 Dilution Sample Preparation: Weigh 10.00 ± 0.05 g of tap water into a glass vial. Add 1.00 ± 0.02 g of shampoo to tap water. Tightly close the bottle cap, and shake vigorously 20 times back and forth. Allow the sample to settle for 5 to 24 hours until the milky phase has split to the top.
[0174] 5:1 Dilution Sample Preparation: Weigh 10.00 ± 0.05 g of tap water into a glass vial. Add 2.00 ± 0.02 g of shampoo to tap water. Tightly close the bottle cap, and shake vigorously 20 times back and forth. Allow the sample to settle for 5 to 24 hours until the milky phase has split to the top.
[0175] Microscope Slide Preparation: Use a plastic pipette of 1 ml of milky phase sample from the top of the dilution sample and place a drop on a microscope slide, then place a microscope slide cover on top of the sample.
[0176] Dilution samples are evaluated under a 40X objective lens using differential interference contrast (DIC) microscopy. Images are captured by the camera using AxioVs40 V 4.7.2.0 imaging software available from Carl Zeiss Imaging Solutions. Discussion of results for examples 11 to 13
[0177] Microscopy of the dilutions of Examples 11, 12 & 13 shows the presence of limonene oil droplets trapped in the coacervate. This is evidence that upon dilution of the shampoo, both the coacervate and the limonene oil phase separate.

Discussion of results for examples 14 to 15
[0178] For Example 14 (control), the ratio between diffusion coefficients (DS/DA) is close to 1.0 which indicates that piroctone olamine is diffused at the same rate as the SLE1S micelles, which allows us to infer that piroctone olamine is within the SLE1S micelle. However, in Example 15 where SLE1S is replaced by sodium undecyl sulfate, the ratio (DS/DA) is greater than 1.0. This change in DS/DA indicates that piroctone olamine is diffusing at a different rate than sodium undecyl sulfate micelles, which allows us to infer that piroctone olamine is not found within the micelles. The implication of piroctone olamine not being within the surfactant micelles in Example 15 is reflected in an increase in deposition efficiency of Example 15 versus Example 14 (control).
Discussion of Results from Examples 16 to 18
[0179] For Example 16 (control), the ratio between the diffusion coefficients (DS/DA) is close to 1.0 which indicates that the climbazol is diffusing at the same speed as the SLE1S micelles, which allows us to infer that climbazol is within the SLE1S micelle. However, in Examples 17 to 18 where SLE1S is replaced by sodium undecyl sulfate, the ratio (DS/DA) is significantly greater than 1.0. This change in DS/DA indicates that climbazol is diffusing at a different rate than sodium undecyl sulfate micelles, which allows us to infer that climbazol is not inside the micelles. Accordingly, Examples 17 to 18 are representative of the present invention and exhibit significantly greater deposition efficiency which is 1.9X to 2.5X than that of Example 16 (control). This demonstrates that the present invention can be broadly applied to a variety of soluble antidandruff agents.

Discussion of Results for Examples 19 to 23
[0180]This set of examples demonstrates that diffusion coefficient ratios (DS/DA) greater than 1.2 is important to achieve the desired increased deposition efficiency. Examples 20 to 22 are representative of the present invention and demonstrate that it is possible to obtain diffusion coefficient ratios (DS/DA) greater than 1.2 with a variety of surfactants. Consequently, Examples 20 to 22 show greater deposition efficiency (1.4 to 2.0X) than that of Example 19 (control). Example 23 is a comparative example and shows that even when the formula contains sodium undecyl sulfate, if DS/DA is close to 1.0 the deposition efficiency will be low and similar to that of the control (Example 19).
[0181]In the examples, all concentrations are listed in terms of percent by weight, except where otherwise specified, and may exclude secondary materials such as thinners, fillers and others. The formulations mentioned herein, therefore, contain the mentioned components and any secondary materials associated with such components. As will be evident to one of skill in the art, the selection of these secondary elements will vary depending on the physical and chemical characteristics of the specific ingredients selected to produce the hair care composition.
[0182] The dimensions and values disclosed in the present invention are not to be understood as being strictly limited to the exact numerical values mentioned. Instead, except where otherwise noted, each of these dimensions is intended to mean both the stated value and a range of functionally equivalent values around that value. For example, a dimension revealed as "40 mm" is intended to mean "about 40 mm".
[0183] Each document cited in the present invention, including any patent or patent application by cross-reference or related, and any patent or patent application in which this application claims priority or benefit thereof, is hereby incorporated in its entirety by reference. , except as expressly excluded or otherwise limited. Mention of any document is not an admission that it constitutes prior art in relation to any invention disclosed or claimed in the present invention, nor that by itself or in any combination with any other reference or references, it teaches, suggests or describes such invention . In addition, if there is a conflict between any meaning or definition of a term mentioned in this document and any meaning or definition of the same term in a document incorporated by reference, the meaning or definition ascribed to that term in this document shall take precedence.
[0184] Although specific embodiments of the present invention have been illustrated and described, it will be evident to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that fall within the scope of the present invention.

权利要求:
Claims (22)
[0001]
1. Hair care composition, CHARACTERIZED by comprising: a) 14% to 40% of one or more surfactants, in which one or more of the surfactants is an anionic surfactant or combinations of anionic surfactants; b) from 0.1% to 10% of one or more surfactant-soluble anti-dandruff agents; where, when the hair care composition is diluted to 1.3%, a surfactant concentration has a ratio of surfactant diffusion coefficient to soluble agent diffusion coefficient of from 1.4 to 2.5.
[0002]
2. Hair care composition according to claim 1, CHARACTERIZED in that the surfactant is an anionic surfactant selected from the group consisting of anionic alkyl sulfates and alkyl ether sulfates having linear or branched alkyl chains and mixtures thereof.
[0003]
3. Composition for hair treatment, according to claim 1 or 2, CHARACTERIZED in that the surfactant is an anionic surfactant selected from the group consisting of: a) R1 O(CH2CHR3O)y SO3M; b) CH3(CH2)z CHR2CH2O(CH2CHR3O)y SO3M; and c) mixtures thereof, wherein R1 represents CH3 (CH2)10, R2 represents H or a hydrocarbon radical comprising from 1 to 4 carbon atoms so that the sum of the carbon atoms in z and R2 is 8, R3 is H or CH3 , y is 0 to 7, the average value of y is 1 when y is not (0), and M is a positively charged monovalent or divalent cation.
[0004]
4. Hair care composition according to claim 1, CHARACTERIZED in that the surfactant is a surfactant or combination of surfactants selected from the group consisting of sodium lauryl sulfate, sodium laureth-n sulfate, where n is between 0.5 to 3.5, sodium C10-15 alkyl sulfate, where the alkyl chain may be straight or branched, paret-n C10-15 sodium sulfate, where n is between 0.5 to 3 .5 and the alkyl chain may be straight or branched, sodium decyl sulfate, sodium decet-n sulfate where n is between 0.5 to 3.5, sodium undecyl sulfate, sodium undecet-n sulfate where n is between 0.5 to 3.5, sodium tridecyl sulfate, sodium tridecet-n sulfate where n is between 0.5 to 3.5, an anionic surfactant selected from the group consisting of: a) R1 O(CH2CHR3O)y SO3M; b) CH3(CH2)z CHR2CH2O(CH2CHR3O)y SO3M; and c) mixtures thereof, wherein R1 represents CH3(CH2)10, R2 represents H or a hydrocarbon radical comprising from 1 to 4 carbon atoms so that the sum of the carbon atoms in z and R2 is 8, R3 is H or CH3 , y is 0 to 7, the average value of y is 1 when y is not (0), and M is a positively charged monovalent or divalent cation.
[0005]
5. Composition for hair treatment, according to claim 1, CHARACTERIZED by additionally comprising from 0.25% to 15% of one or more amphoteric, non-ionic or zwitterionic co-surfactants.
[0006]
Hair care composition according to claim 1, characterized in that the surfactant-soluble agent is a hydroxyl pyridine.
[0007]
A hair care composition according to claim 1, characterized in that the hydroxyl pyridone is piroctone olamine.
[0008]
8. Hair care composition according to claim 1, characterized in that the surfactant-soluble agent is an azole.
[0009]
A hair care composition according to claim 8, CHARACTERIZED in that the azole is climbazol.
[0010]
10. Composition for hair treatment, according to claim 1, CHARACTERIZED in that the composition further comprises a cationic polymer.
[0011]
A hair care composition according to claim 1, characterized in that the composition additionally comprises a conditioning agent.
[0012]
A hair care composition according to claim 11, characterized in that the conditioning agent is a silicone.
[0013]
A hair care composition according to claim 1, characterized in that it additionally comprises one or more scalp health agents.
[0014]
A hair care composition according to claim 13, characterized in that the scalp health agent is zinc pyrithione.
[0015]
A hair care composition according to claim 13, characterized in that the scalp health agent is salicylic acid.
[0016]
The hair care composition according to claim 13, characterized in that the scalp health agent is menthol and/or mint lactate.
[0017]
The hair care composition according to claim 1, characterized in that it additionally comprises from 1% to 7% of a perfume.
[0018]
The hair care composition of claim 1, wherein the hair care composition is dispensed as a foam.
[0019]
The hair care composition of claim 18 wherein the hair care composition is dispensed as an aerosol foam.
[0020]
The hair care composition of claim 19 wherein a propellant or blowing agent for dispensing the composition as an aerosol foam is a chemically inert hydrocarbon, a halogenated hydrocarbon and mixtures thereof.
[0021]
The hair care composition of claim 18, wherein the hair care composition is dispensed as a pumped foam.
[0022]
The hair care composition of claim 1, characterized in that the hair care composition is applied using an applicator.

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法律状态:
2019-10-15| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2021-04-27| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-07-06| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 22/04/2016, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US201562151702P| true| 2015-04-23|2015-04-23|

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US62/151,702|2015-04-23|

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