WO2022013100A1 - Compositions antitranspirantes en stick - Google Patents

Compositions antitranspirantes en stick Download PDF

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Publication number
WO2022013100A1
WO2022013100A1 PCT/EP2021/069171 EP2021069171W WO2022013100A1 WO 2022013100 A1 WO2022013100 A1 WO 2022013100A1 EP 2021069171 W EP2021069171 W EP 2021069171W WO 2022013100 A1 WO2022013100 A1 WO 2022013100A1
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WO
WIPO (PCT)
Prior art keywords
oil
composition according
antiperspirant
oils
solidifying agent
Prior art date
Application number
PCT/EP2021/069171
Other languages
English (en)
Inventor
Nigel John CROSS
Bruce Steven Emslie
Craig James LUCKWELL
Original Assignee
Unilever Ip Holdings B.V.
Unilever Global Ip Limited
Conopco, Inc., D/B/A Unilever
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unilever Ip Holdings B.V., Unilever Global Ip Limited, Conopco, Inc., D/B/A Unilever filed Critical Unilever Ip Holdings B.V.
Publication of WO2022013100A1 publication Critical patent/WO2022013100A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q15/00—Anti-perspirants or body deodorants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216—Solid or semisolid forms
    • A61K8/0229—Sticks
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • A61K8/064—Water-in-oil emulsions, e.g. Water-in-silicone emulsions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26—Aluminium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31—Hydrocarbons
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin

Definitions

  • the present invention relates to antiperspirant stick compositions and their method of manufacture, especially to such compositions containing an astringent antiperspirant salt and in particular to compositions in the form of solidified water-in-oil emulsions.
  • Antiperspirant stick compositions are typically characterised by being integral and self- supporting, commonly in the form of a rod or bar, usually dispensed from a tubular container having an open end and provided with a platform that is moveable towards the open end.
  • Some antiperspirant stick compositions are anhydrous, whilst others are aqueous compositions in the form of an emulsions.
  • the antiperspirant active is commonly dissolved in the aqueous phase which is typically dispersed in an oil continuous phase to form a water-in-oil emulsion.
  • the present invention relates to antiperspirant stick formulations which comprise droplets of a solution of an antiperspirant active dispersed in a continuous oil phase, such formulations being made solid by the presence of a solidifying agent or structurant.
  • emulsion stick formation has been addressed in a series of patents to Unilever, including US 6287544, US 6455056, US 6248312, and WO 2003/059307. These specifications disclose that emulsion sticks can be made using structurants, many of which are fibre-forming small molecule gelling agents. A combination of structurants has been disclosed in WO 2004/098551, also to Unilever. It is preferable for a stick composition to have a certain hardness. A stick that is relatively soft can result in increased deposition, which can be wasteful and/or give an unpleasant sensation of stickiness.
  • a further benefit that may be delivered by antiperspirant stick compositions according to the present invention is reducing staining typically white or yellow staining, on fabrics worn in proximity to the site of application of the composition.
  • Antiperspirant water-in-oil emulsions have been described in EP 1280502 in which the oil phase is structured with an ester wax. Compared with anhydrous antiperspirant compositions, such emulsions have exhibited reduced visible whitening.
  • a water-in-oil emulsion stick comprising potassium alum in the aqueous phase and in which the oil phase is gelled with polyethylene has been described in USP 6139824.
  • an antiperspirant stick composition in the form of a water-in-oil emulsion comprising an aqueous phase comprising dissolved antiperspirant active; an emulsifier and an oil phase comprising a liquid oil and a solidifying agent; wherein the solidifying agent is a hydrocarbon wax blend having average molecular weight (M w ) of from 450 to 500 (preferably from 460 to 490) and a polydispersity (Mw/Mn) of from 1.01 to 1.05 (preferably 1.02 to 1.04).
  • M w average molecular weight
  • Mw polydispersity
  • a non-therapeutic method of locally inhibiting or controlling odour or perspiration in which a stick composition according to the first aspect of the invention is topically applied to the human skin, preferably in the underarm.
  • ambient conditions refer to 20°C and 1 atmosphere pressure, unless otherwise indicated.
  • references to amounts of components such as “liquid oil” or “solidifying agent” relate to the total amount of such components present in the composition.
  • the word “comprising” is intended to mean “including” but not necessarily “consisting of’, i.e. , it is non-exhaustive.
  • cosmetic methods and compositions should be understood to mean non-therapeut methods and compositions, respectively.
  • an “aluminium-based” antiperspirant (AP) salt is one comprising aluminium.
  • a “calcium-activated” AP salt is one that has been heated in water with a water- soluble calcium salt during its manufacture.
  • solidified refers to a state of matter incapable of flow at a temperature of 25°C and a pressure of 1 atmosphere.
  • compositions according to the present invention is typically less than 20 mm, preferably less than 15 mm and more preferably less than 10 mm.
  • Such sticks can demonstrate a combination of aesthetically desirable properties, including sensory benefits such as the avoidance of excessive drag on application and sometimes lower visible marks on clothing worn in close proximity to the area of application on the skin.
  • the aqueous phase comprises an aqueous solution of an AP salt.
  • it may also comprise a polyol, as described further hereinbelow. It may also comprise other water-soluble materials, as described further hereinbelow.
  • water-soluble means having a solubility in water of at least 10 g/l at 25°C.
  • the aqueous phase typically comprises from 30 to 68% of the total composition. Preferably, it comprises from 40 to 65% and more preferably from 45 to 60% of the total composition.
  • the AP active is typically an aluminium-based astringent salt, including astringent aluminium salts and aluminium-zirconium salts.
  • Such salts typically have may have inorganic anions but may optionally have organic cations and may optionally be complexes.
  • Preferred astringent salts include aluminium and aluminium/zirconium halides and halohydrate salts, such as chlorohydrates.
  • Zirconium aluminium chlorohydrate actives may be used, such as ZAG (zirconium-aluminium-glycine) complexes, for example those disclosed in US 3,792,068 (Procter and Gamble Co.).
  • the AP salt is preferably a basic aluminium chlorohydrate salt, in particular a salt of general formula A OHe- x C , where is 0.3 to 5, preferably 1 to 2, and more preferably 1 to 1.6.
  • ASCH aluminium sesquichlorohydrate
  • Most commercial ASCH samples are of chemical formula AI 2 OH 4.7 CI 1.3 to AI 2 OH 4.9 CI 1.1 and it is especially preferred to use BAC salts of this formula.
  • Particularly preferred AP actives comprise calcium and particularly preferred actives are also complexes with glycine. This is especially the case for ASCH salts, although calcium- activated aluminium zirconium salts, such as those disclosed in EP 1,104,282 B1 (Gillette) and EP 1,653,918 B1 (Gillette), may also be advantageously employed.
  • ASCH actives comprising calcium are described in WO 2014/187685 (Unilever, 2014). The calcium is typically added in the form of calcium chloride. It is especially preferred that such actives are calcium-activated ASCH salts.
  • the molar ratio of calcium to aluminium is typically at least 1 :40, preferably at least 1 :30 and more preferably at least 1 :20. It is not advantageous to have the calcium concentration in excess of the aluminium concentration, indeed it is preferred that the calcium concentration is no more than half that of the aluminium concentration and more preferred that it is no more than a fifth of said concentration.
  • the preferred molar ratios of calcium to aluminium of at least 1 :40 and at least 1:20 it is independently preferred that this ratio is no greater than 1:2 and more preferred that it is no greater than 1 :5.
  • the molar ratio of calcium to aluminium is at least 1:15 and preferably no greater than 1:5 and in especially preferred embodiments it is at least 1:12 and preferably no greater than 1:5.
  • references to molar amounts and ratios of “aluminium” are calculated on the basis of mono-nuclear aluminium, but include aluminium present in poly-nuclear species; indeed, most of the aluminium in the salts of relevance is present in poly-nuclear species.
  • AP actives that are complexes with glycine are preferred, particularly when they are ASCH AP salts comprising calcium and/or activated by calcium.
  • the molar ratio of amino acid to aluminium is preferably at least 1:20, more preferably at least 1:15 and most preferably at least 1:10. It is not advantageous to have the amino acid concentration in excess of the aluminium concentration; hence, the molar amino acid to aluminium is preferably from 1:20 to 1:1, more preferably from 1:15 to 1:2 and most preferably from 1:10 to 1:5.
  • a calcium-activated ASCH glycine complex is used in which the molar ratio of calcium to aluminium is from 1:15 to 1:5 and the molar ratio of amino acid to aluminium is also from 1:15 to 1:5.
  • the proportion of antiperspirant salt is calculated excluding the weight of any water of hydration but including any complexing agent that may be present, such as glycine and any activating agent, such as calcium chloride.
  • the weight concentration of the antiperspirant salt in the aqueous phase is commonly not higher than 50% and is advantageously at least 10%. In preferred embodiments its weight concentration is from 15 to 40% and in more preferred embodiments it is from 20 to 30%.
  • the weight of antiperspirant salt in the entire composition is usually at least 6% and is commonly up to 30%.
  • the range of antiperspirant salt concentration for the composition is preferably from 8% to 25% and more preferably from 10 to 20%.
  • the disperse phase may contain a water-soluble polyhydric alcohol.
  • the polyhydric alcohol may serve to counteract the astringency of the antiperspirant salt, by acting as a humectant.
  • Suitable polyhydric alcohols for this purpose are glycerol or PEG oligomers having a molecular weight (weight average) of from 180 to 420. Such materials may be advantageously present at from 1% up to 20% and preferably at from 5 to 15% of the total composition.
  • compositions of the invention include licorice extract and/or vitamins, such as vitamin B3 (niacinamide) and vitamin C, that may enhance skin tone following topical application of the composition of the invention.
  • vitamins tend to be particularly sensitive to elevated temperature and the compositions of the invention are particularly well suited to their incorporation due to the relatively low melting point of the solidifying agent employed.
  • the oil phase of the compositions of the invention comprises a liquid oil and a solidifying agent.
  • the oil phase typically comprises from 30 to 70% of the total composition. Preferably, it comprises from 35 to 60% and more preferably from 40 to 55% of the total composition.
  • the emulsifier is considered to be a component of the oil phase.
  • the liquid oil may be chosen from any of wide range of such oils.
  • the oil phase may comprise one or more oils selected from volatile silicone oils, ester oils, ether oils or mineral oils.
  • the liquid oil is a water-immiscible oil having a melting point of 25°C or less. Preferably, it has a melting point of 20°C or less. In some embodiments, the liquid oil has a melting point of from -50°C to 25°C and preferably from -30°C to 20°C.
  • the oil phase may comprise more than one liquid oil as defined hereinabove.
  • amounts and ratios referring to “liquid oil” relate to all such oils present.
  • the oil phase comprises one or more volatile silicone oils.
  • volatile herein is meant having a measurable vapour pressure at 20 or 25°C.
  • the vapour pressure of a volatile silicone oil lies in a range from 1 or 10 Pa to 2 kPa at 25°C.
  • Volatile silicone oils can be linear or cyclic siloxanes, usually containing from 3 to 9 silicon atoms, and commonly from 4 to 6 silicon atoms, the silicon atoms being substituted by methyl groups.
  • volatile silicone oils in which at least 80% and particularly at least 90% contain at least 5 silicon atoms, such as cyclopentadimethylsiloxane (D5), cyclohexadimethylsiloxane (D6), dodecamethylpentasiloxane and tetradecamethylhexasiloxane.
  • volatile silicone oils may comprise at least 30% of the oil phase and normally not higher than 95% thereof. In a number of desirable compositions their weight proportion in the oil phase is up to 60%, and a preferred range in the oil phase is from 30 to 55%.
  • the liquid oil can alternatively or additionally comprise one or more non-volatile oils, which can be silicone oils and/or non-silicone oils.
  • Non-volatile silicone oils employed herein preferably contain one or more unsaturated substituents such as phenyl or diphenylethyl in replacement of the corresponding number of methyl substituents in polycyclosiloxanes or more preferably in linear siloxanes, often having 2 or 3 silicon atoms.
  • Such non-volatile oils have a higher refractive index than that of the volatile silicone oils and tend to mask the antiperspirant active when it is deposited on skin.
  • the non-volatile oils can also comprise dimethiconols, which are hydroxyl-terminated.
  • the proportion of non-volatile silicone oils in the oil phase is commonly up to 25% such as from 0.25 to 20% of the phase.
  • the oil phase comprises from 1 to 10% of the non-volatile silicone oil, and in other chosen embodiments, the non-volatile silicone oil provides from 10 to 20% of the oil phase.
  • the oil phase can alternatively or additionally comprise one or more hydrocarbon fluids, which can be either volatile or non-volatile.
  • Suitable hydrocarbon fluids include liquid aliphatic hydrocarbons such as mineral oils or hydrogenated polyisobutene, desirably selected to exhibit a low viscosity. Further examples of liquid hydrocarbons are polydecene and paraffins and isoparaffins of at least 10 carbon atoms. Hydrocarbon fluids conveniently comprise from 0 to 25% of the oil phase.
  • the oil phase comprises liquid aliphatic or aromatic ester oils.
  • oils can act as emollients and in addition can affect the sensory attributes of the resultant emulsion.
  • Suitable aliphatic esters contain at least one long chain alkyl group, such as esters derived from Ci to C2 0 alkanols esterified with a Cs to C22 alkanoic acid or C 6 to C1 0 alkanedioic acid.
  • the alkanol and acid moieties or mixtures thereof are preferably selected such that they each have a melting point of below 20°C.
  • Aliphatic esters include isopropyl myristate, lauryl myristate, isopropyl palmitate, diisopropyl sebacate and diisopropyl adipate.
  • ester oils include glyceride oils and in particular triglyceride oils derived from glycerol and fatty acids containing at least 6 carbons and especially natural oils.
  • Suitable liquid aromatic esters include fatty alkyl benzoates.
  • esters include suitable Cs to C18 alkyl benzoates or mixtures thereof, including in particular C12 to C15 alkyl benzoates e.g. those available under the trademark Finsolv TN.
  • Such benzoate esters are especially desirable for employment in an aqueous antiperspirant emulsion, and one employing a wax to gel the oil phase, relative to alkyl mono or diesters mentioned above, by virtue of their properties that promote superior aesthetic attributes.
  • An aryl benzoate, such as benzyl benzoate can also be used.
  • ester oils include oils in which a short alkylene group of 1 to 3 carbons, optionally substituted by a methyl group, is interposed between benzene and benzoate residues. It is advantageous to select an ester oil having a refractive index of at least 1.47.
  • the total proportion of ester oils is often from 0 to 50% of the oil phase, is desirably at least 5% and with benefit comprise at least 20%. Their total proportion is in many embodiments desirably from 25% up to 40% of the oil phase.
  • the weight ratio of aromatic ester oil to aliphatic ester oil is often selected in the range of from 1 :2 to 20:1 , such from 1 :1 to 8:1.
  • Natural ester oils which desirably can be employed herein comprise one or more unsaturated C18 fatty acid glycerides. In many instances, such ester oils comprise one or more triglycerides.
  • the fatty acid residues in the oils can comprise, commonly, from one to three olefinic unsaturated bonds and often one or two. Whilst in many instances the olefinic bonds adopt the trans configuration, in a number of desirable products the bond or bonds adopt the cis configuration. If two or three olefinic unsaturated bonds are present, they can be conjugated.
  • the fatty acid can also be substituted by an hydroxyl group.
  • the natural oils employable herein desirably comprise one or more triglycerides of oleic acid, linoleic acid, linolenic acid or ricinoleic acid.
  • Various isomers of such acids often have common names, including linolenelaidic acid, trans 7-octadecenoic acid, parinaric acid, pinolenic acid punicic acid, petroselenic acid and stearidonic acid. It is especially desirable to employ glycerides derived from oleic acid, linoleic acid or petroselenic acid, or a mixture containing one or more of them.
  • Natural oils containing one or more of such triglycerides include coriander seed oil for derivatives of petroselinic acid, impatiens balsimina seed oil, parinarium laurinarium kernel fat or sabastiana brasilinensis seed oil for derivatives of cis-parinaric acid, dehydrated castor seed oil, for derivatives of conjugated linoleic acids, borage seed oil and evening primrose oil for derivatives of linoleic and linolenic acids, aquilegia vulgaris oil for columbinic acid and sunflower oil, olive oil or safflower oil for derivatives of oleic acid, often together with linoleic acids.
  • Other suitable oils are obtainable from hemp, such as stearadonic acid derivatives and maize corn oil.
  • An especially preferred oil, which is a natural oil is sunflower seed oil.
  • the proportion of the natural oil viz particularly the triglyceride oils of unsaturated fatty acids, if present in the composition, is often selected in the range of from 0.1 to 10% of the oil phase, desirably at least 0.5% and in some embodiments particularly in the range of up to 8% of the oil phase.
  • Some preferred embodiments employ a natural ester oil in the oil phase together with a water-soluble humectant, such as those mentioned hereinbefore, in the aqueous phase, and particularly in a weight ratio to each other of from 3:1 to 1 :3.
  • a further class of particularly suitable oils comprises a) non-volatile liquid aliphatic ethers derived from at least one fatty alcohol that desirably contains at least 10 carbon atoms, such as myristyl ether derivatives e.g. PPG-3 myristyl ether or lower alkyl (£ Ce) ethers of polyglycols (preferably polypropylene glycol and especially 10 to 20 units, such as an ether named as PPG-14 butyl ether in the CTFA.
  • the class of non-volatile ethers additionally comprises b) dialkyl ethers derived from C8 or C10 linear aliphatic alcohols, and particularly dioctyl ether.
  • the invention emulsions herein can alternatively or additionally comprise a dialkyl carbonate derived from C8 or C10 linear aliphatic alcohols, and particularly dioctyl carbonate. It is often convenient for the aliphatic ether or dialkyl carbonate to constitute at least 0%, and especially at least 10%, particularly up to 50% and very desirably up to 30%, %s being of the oil phase.
  • a further class of oils that can be employed herein comprises water-immiscible aliphatic alcohols, and particularly those having a boiling point of higher than 100°C. These include branched chain alcohols of at least 10 carbon atoms and in many instances up to 30 carbon atoms, particularly 15 to 25, such as isostearyl alcohol, hexyl-decanol and octyl-dodecanol. It will be recognised that octyl-dodecanol is an especially favoured water-immiscible aliphatic alcohol in the present compositions, because it not only acts as an emollient oil but additionally moisturises skin by the mechanism of occlusion.
  • suitable water-immiscible alcohols include intermediate chain length linear alcohols, commonly containing from 9 to 13 carbon atoms, such as decanol or dodecanol. Such alcohols can often constitute at least 0.1% and particularly at least 0.5% of the oil phase, in many compositions being not more than 5% of the phase.
  • the present compositions preferably contain a fragrance oil.
  • a fragrance oil is normally a complex mixture of chemical classes and accordingly, its proportion is excluded from calculations of the proportion of the other constituents of the liquid oil, including specifically ester, ether and alcohol classes.
  • the total weight proportion of fragrance oils in the emulsion is normally selected in the range of from 0 to 4% of the emulsion, often from 0.3% to 2%.
  • the weight ratio of volatile to non-volatile oils is desirably from 2:1 to 1:2, and particularly from 3:2 to 2:3.
  • a solidifying agent is an essential constituent of the oil phase of compositions of the invention.
  • the solidifying agent is a hydrocarbon wax blend, meaning that it consists of various molecules consisting of solely carbon and hydrogen.
  • the blend is selected such that it preferably has a melting point of less than 73°C, more preferably of 72°C or less, as can be determined by the following DSC process.
  • the DSC melting trace also has a width at half height of at least 7.5°C, also as determined by the following DSC process.
  • the stick may be manufactured at relatively low temperature, saving energy and reducing possible damage to any heat- sensitive components used in the composition (vide infra).
  • the hydrocarbon wax blend typically has a melting of from 60°C to 73°C and preferably from 60°C to 72°C. In some embodiments, the hydrocarbon wax blend has a melting of from 65°C to 73°C and preferably from 65°C to 72°C.
  • DSC means differential scanning calorimetry and the DSC process referred to herein is performed in the following manner.
  • a sample of the material to be tested typically from 5 to 7 mg and especially 6 mg, is placed in a DSC pan and the pan is sealed.
  • the sample is then passed through a melt, re-solidify loop and it is then heated, from a temperature of 20°C or below, at 5°C per minute, until a temperature of at least 100°C is achieved.
  • melt, re-solidify is essential to provide consistent heat transfer through the pan used in the DSC instrument and, hence, consistency of results. Whilst one melt, re-solidify cycle is sufficient, more than one may be employed.
  • the pan used in the DSC instrument is typically made of aluminium or stainless steel.
  • the starting temperature for the final step mentioned in the above DSC process may be from -50 to 20°C.
  • the end temperature for the final step mentioned in the above DSC process may be from 100 to 200°C.
  • the melting point may be defined as (or is defined as) the peak temperature of a DSC trace performed in the manner described above, the trace being of the final heating step.
  • the “width at half height” of a DSC trace refers to a trace generated by a process performed in the manner described above, the trace being of the final heating step.
  • wax blend or “wax blends” may sometimes be substituted by the term “wax” or “waxes” respectively, without change of meaning.
  • Preferred hydrocarbon waxes are polyolefin waxes, in particular polyethylene waxes.
  • Such waxes are typically synthetic waxes, i.e. waxes synthesised from olefins in the case of polyolefin waxes and waxes synthesised from ethylene in the case of polyethylene waxes.
  • the hydrocarbon wax blend has a DSC melting trace having a width at half height of at least 7.5°C and preferably at least 8°C, as determined by the DSC process described above.
  • the hydrocarbon wax blend has a DSC melting trace having a width at 40% height of at least 10°C. In some embodiments, the hydrocarbon wax blend has a DSC melting trace having a width at half height of from 7.5°C to 15°C and preferably from 7.5°C to 12°C.
  • Hydrocarbon wax blends used in the present invention have an average molecular weight (M w ) of from 450 to 500 and particularly from 460 to 490.
  • the hydrocarbon wax blend also has a polydispersity (M w /M n ) of from 1.01 to 1.05, particularly 1.02 to 1.04.
  • M w /M n polydispersity
  • the amount of the hydrocarbon wax blend used in the compositions of the invention is preferably from 5%, more preferably from 7% and most preferably from 8%.
  • the upper amount is preferably up to 25%, more preferably up to 20% and most preferably up to 15%.
  • the preferred ranges of hydrocarbon wax blend may be selected from any of the lower and upper amounts indicated in this paragraph.
  • the invention composition comprises at least one emulsifier.
  • the emulsifier is preferably a dimethicone copolyol having an HLB value of up to 8, particularly from 2 to 7 and especially from 3 to 6.
  • Alkyl dimethicone copolyols are a preferred group of emulsifiers.
  • the emulsifier preferably comprises polyhydroxylated esters, polyalkylene oxide (including PEG ester, PPG esters and mixed PEG-PPG esters) or polyglyceryl esters.
  • Polyglyceryl esters are particularly preferred, especially in cold processed compositions (vide infra).
  • PEG refers to polyethylene glycol
  • PPG refers to polypropylene glycol.
  • the proportion of the emulsifier in the composition is often selected in the range of from 0.125% to 2.0% and in many embodiments from 0.5 to 1.5%.
  • compositions herein can incorporate one or more additional components.
  • additional components can include skin feel improvers, such as talc or finely divided high melting point polyethylene (>110°C), for example in an amount of up to about 6% and often in total in an amount of from 0.5 to 5%; inorganic particulates, preferably finely divided, such as fumed silica, for example in an amount of up to 2%; skin benefit agents, such as allantoin; vitamins or lipids, for example in an amount of up to 5%; colouring agents, such as titanium dioxide; preservatives, such as butylhydroxytoluene, often in an amount of from 0.01 to 0.1%; metal chelates, such as EDTA, for example in an amount of up to 1%; skin cooling agents, such a menthol and menthol derivatives, often in an amount of up to 2%, all of such percentages being of the total composition.
  • skin feel improvers such as talc or finely divided high melting point polyethylene (>110°C
  • a preferred addition component is a cosmetic skin tone modifier, particularly those selected from niacinamide, 12-hydroxystearic acid, vitamin C, licorice extract and avocado oil.
  • niacinamide, vitamin C, licorice extract and avocado oil are temperature sensitive are especially suited to incorporation into the compositions of the invention.
  • a further optional ingredient can comprise a wash-off agent, which can assist a user of the invention composition to wash it off.
  • a wash-off agent which can assist a user of the invention composition to wash it off.
  • Such an agent when employed, often comprises a non ionic surfactant, such as in an amount of from 0.1 to 2% of the emulsion, and often at least 0.5%.
  • the wash-off agent can be the same as the emulsifier it is preferably a nonionic surfactant such as POE or POP/POE ester or ether (or mixture) having an HLB that is at least 10.
  • the invention stick compositions can be made in a process comprising: in step 1, making an aqueous phase by blending together the water and water-soluble ingredients, including the antiperspirant astringent salt, at least a fraction of which may be in the form of a pre-formed aqueous solution; in step 2, forming an oil phase comprising the solidifying agent and the liquid oil or oil mixture, which normally entails heating the wax and oils to a temperature at which wax particles are no longer visible, commonly in the region of the melting point of the wax; and in a step 3, mixing the aqueous phase and the oil phase together at elevated temperature such that the solidifying agent remains in a liquid state dissolved in the liquid oil, and preferably shear mixing the two phases, in the presence of the emulsifier, and in step 4, filling the resultant mixture into a dispenser whilst it is still mobile and thereafter cooling or allowing the composition to cool, initially until the mixture solidifies and then attains ambient temperature.
  • Steps 1 and 2 in the process described above can be carried out simultaneously or sequentially.
  • the oil is often heated to a temperature in the region of 70 to 80°C, preferably 70 to 75°C.
  • the aqueous phase, prepared in step 1 is mixed with the oil phase in step 3, it preferably heated to temperature in the region of 60 to 70°C, more preferably 65 to 70°C and most preferably 68 to 69°C.
  • the temperature is maintained at preferably 65 to 80°C, more preferably 65 to 75°C and most preferably 66 to 74°C.
  • the wax or waxes, or a fraction of them can be heated externally, for example melted, prior to introduction into the oil phase or emulsion.
  • any temperature sensitive ingredients such as certain fragrance components
  • an antiperspirant composition is manufactured by the steps of (i) making an aqueous phase by blending together water and an antiperspirant active and heating said phase to a temperature of 60°C or greater; (ii) forming an oil phase comprising the solidifying agent and a liquid oil and heating said phase to a temperature of 70°C or greater; (iii) with the aqueous phase and oil phase at the temperatures as indicated in steps (i) and (ii) respectively, mixing these phases together in the presence of an emulsifier; (iv) filling the resultant mixture into a dispenser whilst it is still mobile and (v) cooling the composition until the mixture solidifies; the solidifying agent being a hydrocarbon wax blend having a melting point of 73°C or less and a DSC melting trace having a width at half height of at least 7.5°C.
  • the process described in the paragraph immediately above may be performed by batch or continuous (including semi-continuous) processes.
  • the oil and aqueous phases are made separately and typically held with gentle agitation in separate vessels.
  • the oil phase may be held at any suitable temperature, typically within the range 60 to 80°C.
  • the aqueous phase temperature should be adjusted such that when the two phases are combined, the temperature of the mixture is sufficiently high to avoid premature solidification. Typically, this will be in excess of 65°C.
  • the two phases (streams) can then be combined at any point upstream of (or in) a device capable of providing intensive mixing (the primary intensive mixing device) which leads to the formation of the emulsion. Suitable devices include Sonolators and devices where the streams are brought together through impinging jets.
  • the combined streams can be pumped through the primary intensive mixing device under the required conditions to form the desired emulsion while ensuring that the temperature of the mixture exceeds the solidification temperature.
  • the emulsion formed in this manner may be packed directly into stick packs or sent to a holding vessel where the emulsion droplet size can be maintained or adjusted, by use of a second intensive mixing device (of similar or different design to the primary intensive mixing device) situated either inside the vessel or in a recirculation loop around the vessel, prior to packing the emulsion by filling into stick packs.
  • a second intensive mixing device of similar or different design to the primary intensive mixing device
  • fragrance may be added to the mixture (emulsion) either as a third stream upstream or downstream of (or in) the primary intensive mixing device or directly into the holding vessel if used.
  • step (i) making an aqueous phase by blending together water and an anti perspi rant active; (ii) forming an oil phase; (iii) mixing the aqueous phase and the oil phase together, preferably at high shear, to form an emulsion at ambient temperature in the presence of an emulsifier; (iv) adding a solidifying agent, in solid form, to the emulsion formed in step (iii) and heating the mixture to a temperature of 70°C or greater in order to melt/dissolve the solidifying agent; (v) filling the resultant mixture into a dispenser whilst it is still mobile and (vi) cooling the composition until the mixture solidifies; the solidifying agent being a hydrocarbon wax blend having a melting point of 73°C or less and a DSC melting trace having a width at half height of at least 7.5°C.
  • the solidifying agent being a hydrocarbon wax blend having a melting point of 73°C or less and a DSC melting trace having a width at half
  • a dispenser for a stick composition often comprises a tubular barrel, having a side wall that surrounds the composition and defines at a first end an opening through which the composition can pass and a second, opposed end within which is fitted a piston, located within the barrel, that is capable of being impelled towards the first end.
  • the means for impelling the piston can comprise a finger or like implement that is pressed by the user against the exposed side of the piston, or a mechanism for imparting axial movement to the piston.
  • Such a mechanism can comprise a threaded spindle that engages with a threaded aperture in the piston, the spindle being mounted on an exposed rotor wheel or fitted with a cog that can be rotated by engagement with a button via a ratchet.
  • the rotor wheel or button is mounted on the barrel adjacent to the second end.
  • Suitable dispensers for firm sticks are described, for example in US 4232977, WO09818695, WO09305678, and 2002/03830.
  • the present invention includes the non-therapeutic use of compositions according to the invention to inhibit or control perspiration, especially in the armpit.
  • the composition is wiped across the skin to apply it topically, typically at ambient temperature. The action can be repeated until the user considers that sufficient composition has been deposited, often in the region of 3 to 8 wipes per armpit.
  • the composition is commonly applied shortly after the armpit has been washed or shaved.
  • the composition is thereafter left in place, conventionally, for a period of time commonly between 5 and 24 hours until it is washed off.
  • the weight of antiperspirant active applied per armpit is preferably in the range of from 0.15 to 0.5 grams.
  • the AASCH solution used in the following examples was a 27% aqueous solution prepared in the following manner.
  • ASCH (12 parts), calcium chloride (1.5 parts) and glycine (1.9 parts) were heated together for 2 hours at 87°C, in an aqueous solution having a total solids content of 27%.
  • the indicated parts and total solids content refer to the content of the components as anhydrous materials, even though the ASCH and calcium chloride raw materials comprised some water of hydration.
  • the AASCH in the resulting solution had a molar ratio of glycine to aluminium of 10: 90 and a molar ratio calcium to aluminium of 9: 91.
  • Example 1 and Comparative Examples A and B as detailed in Table 1 were prepared by the following method.
  • the oil phase ingredients (cyclopentasiloxane, sunflower seed oil, C12-15 alkyl benzoate, emulsifier, and solidifying agent) were mixed and heated to 80°C whilst stirring at approximately 2500 rpm.
  • the aqueous phase ingredients (AASCH solution and glycerol) were mixed together and heated to 80°C. Once the solidifying agent had melted/dissolved into the oil phase, the aqueous phase was slowly added to the oil phase whilst increasing the stirring rate up to 7500 rpm. The mixture was then sheared for 5 minutes at 7500 rpm whilst cooling to 74°C. The fragrance was then added, and the mixture was furthered cooled to 72°C before pouring into stick barrels and being allowed to cool to ambient temperature.
  • Example 2 and Comparative Example C were prepared by the following method.
  • the oil phase ingredients cyclopentasiloxane, sunflower seed oil, C12-15 alkyl benzoate, emulsifier
  • the oil phase ingredients cyclopentasiloxane, sunflower seed oil, C12-15 alkyl benzoate, emulsifier
  • the aqueous phase ingredients AASCH solution and glycerol
  • the aqueous phase was then slowly added to the oil phase whilst increasing the stirring rate up to 7500 rpm.
  • the mixture was then sheared for 5 minutes at 7500 rpm before the solidifying agent was added and heated to 80°C. Once the solidifying agent had melted/dissolved the mixture was cooled to 74°C and fragrance added.
  • the mixture was further cooled to 72°C before pouring into stick barrels and being allowed to cool to ambient temperature.
  • Polarwachs N670 obtained from Morre-Tec Industries, NJ, is a synthetic polyethylene wax having a melting point of 70.94°C and a DSC trace showing a width at half height of approximately 9°C.
  • the DSC melting trace also had a width at 40% height of approximately 10.5°C.
  • Accumelt 8719A obtained from The International Group, is a synthetic wax having a melting point of about 68.5°C and a DSC trace showing a relatively narrow width at half height of about 5°C.
  • PerformaleneTM M70 obtained from Baker Hughes Co., is a neutral synthetic hard wax having a melting point of 68.89°C and a DSC trace showing a relatively narrow width at half height of approximately 6°C.
  • the DSC melting trace also had a width at 40% height of 7°C.
  • Synkos 2050 obtained from Koster Keunen, is a synthetic wax having a melting point of about 70°C and a DSC trace showing a relatively narrow width at half height of about 5°C.
  • the DSC traces used to characterise the Polarwachs N670 and Performalene M70 waxes were generated on a Perkin Elmer Diamond DSC. 5-7mg samples were weighed into a stainless steel pans which were then hermetically sealed. Two cycles were performed, heating from 5°C to 100°C at 5°C/min.
  • the DSC traces used to characterise the Accumelt 8719A and Synkos 2050 waxes were generated using a Discovery-DSC from TA Instruments with a T4P calibration and regular Tzero pans.
  • the sample weights were 4.19 mg for the Synkos 2050 and 5.28 mg for the Accumelt 8719A.
  • Samples were cooled to -50°C and held at that temperature for 2 minutes. The samples were then heated from 15°C to 200°C at 10°C per minute and then cooled from 200°C to 15°C at 5°C per minutes. Finally, the samples were heated from 15°C to 200°C at 10°C per minute.
  • the profiles from the second heating cycle were used to estimate the melting point (peak temperature) and the width at have height.
  • Example 1 was much harder than Comparative Examples A and B. Further, Comparative Example B was grey in colour and Comparative Example A was off-white, whilst Example 1 was white. When a microscopy study of the sticks was performed, Example 1 had a smooth, even appearance, whereas Comparative Example B showed the presence of plate-like crystalline structures, indicating poor incorporation of the solidifying agent.
  • Example 2 was only marginally harder than the Comparative Example C, it had a further benefit in that the Comparative Example C stick was off-white, whereas the Example 2 stick was white.
  • Examples 3 to 7 as detailed in Table 2 may be prepared by the following method.
  • the cyclopentasiloxane, C12-15 alkyl benzoate, emulsifier and solidifying agent are mixed and heated to 75°C whilst stirring at approximately 2500 rpm.
  • the aqueous phase ingredients AASCH solution and glycerol
  • the aqueous phase is slowly added to the oil phase whilst increasing the stirring rate up to 7500 rpm and not allowing the temperature to drop below 69°C.
  • the mixture is then sheared for 5 minutes at 7500 rpm whilst cooling to 66 to 68°C.
  • the fragrance and sunflower seed oil (when used) are then added, and the mixture was pouring into stick barrels at 66 to 68°C and then allowed to cool to ambient temperature.

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Abstract

L'invention concerne une composition antitranspirante en stick sous la forme d'une émulsion eau dans l'huile, comprenant une phase aqueuse comprenant une substance active anti-transpirante dissoute ; un émulsifiant et une phase huileuse comprenant une huile liquide et un agent de solidification ; l'agent de solidification étant un mélange de cires hydrocarbonées ayant un poids moléculaire moyen (Mw) de 450 à 500 et une polydispersité (Mw/Mn) comprise entre 1,01 et 1,05.
PCT/EP2021/069171 2020-07-13 2021-07-09 Compositions antitranspirantes en stick WO2022013100A1 (fr)

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WO1998018695A1 (fr) 1996-10-25 1998-05-07 The Procter & Gamble Company Dispositif distributeur simplifie, unidirectionnel et a torsion possedant un dosage incremental
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US3792068A (en) 1971-04-02 1974-02-12 Procter & Gamble Dry powder aerosol antiperspirant composition incorporating dry powder antiperspirant active complex and process for its preparation
US4232977A (en) 1978-10-18 1980-11-11 The Procter & Gamble Company Package for antiperspirant/deodorant
WO1993005678A1 (fr) 1991-09-16 1993-04-01 The Procter & Gamble Company Emballage du type a remplissage et a retournement, comprenant un systeme de levage sans fuite et a etancheite particuliere
WO1998018695A1 (fr) 1996-10-25 1998-05-07 The Procter & Gamble Company Dispositif distributeur simplifie, unidirectionnel et a torsion possedant un dosage incremental
US6139824A (en) 1998-07-17 2000-10-31 L'oreal S.A. Deodorant composition
EP1104282B1 (fr) 1998-08-19 2005-10-19 The Gillette Company Sels antisudoraux ameliores stabilises avec du calcium et solutions aqueuses concentrees de ces sels
US6287544B1 (en) 1999-04-12 2001-09-11 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Antiperspirant compositions
US6248312B1 (en) 1999-04-12 2001-06-19 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Cosmetic compositions
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WO2002003830A1 (fr) 2000-07-07 2002-01-17 Unilever Plc Produit en baton s'utilisant comme cartouche de remplissage ou comme baton deodorant a poussoir
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EP1653918B1 (fr) 2003-08-14 2014-07-02 The Gillette Company COMPOSITIONS ANTITRANSPIRAnTes A EFFICACITE ACCRUE CONTENANT DU STRONTIUM OU DU CALCIUM
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