WO2012089819A1 - Alcohol-free fragrancing capsule - Google Patents
Alcohol-free fragrancing capsule Download PDFInfo
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- WO2012089819A1 WO2012089819A1 PCT/EP2011/074253 EP2011074253W WO2012089819A1 WO 2012089819 A1 WO2012089819 A1 WO 2012089819A1 EP 2011074253 W EP2011074253 W EP 2011074253W WO 2012089819 A1 WO2012089819 A1 WO 2012089819A1
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- Prior art keywords
- phase
- gelled
- oily
- composition
- capsule
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- 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
- A61K8/11—Encapsulated compositions
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- 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
- A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
- A61K8/463—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
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- 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
- A61K8/73—Polysaccharides
- A61K8/733—Alginic acid; Salts thereof
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- 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
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q13/00—Formulations or additives for perfume preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/30—Characterized by the absence of a particular group of ingredients
Definitions
- the present invention relates to perfume compositions in the form of perfume capsules, to a process for their preparation and to their use for an application in the field of cosmetics. It also relates to cosmetic compositions comprising said perfume capsules.
- the preparation of perfume compositions is based mainly on the dissolution of aromatic compounds in a hydroalcoholic solution (mixture of water and alcohol, typically ethanol).
- a hydroalcoholic solution mixture of water and alcohol, typically ethanol.
- alcohol typically ethanol
- the use of an alcohol such as ethanol makes it possible, by virtue of its solvent properties, to solubilize aromatic compounds which are generally insoluble or poorly soluble in water.
- alcohol has many disadvantages: it is a dermocensitizer, desiccant, irritant. Moreover, its use is not recommended for young children. In addition, environmental protection regulations have recently become stricter on volatile compounds such as ethanol.
- microemulsions comprising surfactants in the lipophilic perfuming phase, which is disadvised in the case of fragile or atopic skin.
- these microemulsions are sensitive to dilution and easily destabilize, which makes it difficult to incorporate them into other products such as cosmetics. They also contain a high level of surfactants, which is recognized as being an irritating factor, especially when the lipophilic perfume phase is high.
- the present invention aims to provide new perfume compositions for replacing current hydroalcoholic compositions.
- the present invention also aims to provide new perfume compositions without alcohol and comprising a reduced amount of surfactants, including perfume capsules.
- the present invention relates to a fragrance capsule without alcohol, comprising:
- an internal phase formed of an oil-in-water emulsion consisting of a dispersed oily phase consisting of at least one drop of an oily composition comprising a perfuming agent, and a continuous aqueous phase, totally encapsulating the or said drops of the oily phase; and an outer gelled phase comprising at least one polyelectrolyte in the gelled state, completely encapsulating said internal phase at its periphery.
- ily phase means a phase having the property of solubilizing apolar compounds, such as fatty substances, oils, lipids.
- the oily phase is insoluble in water.
- the oily compositions constituting the oily phase preferably comprise a fatty substance, an oil or a mixture of oils of vegetable, animal or mineral origin.
- a vegetable oil mention may for example be made of sweet almond oil, jojoba oil, palm oil or phytosqualane.
- fatty substances examples include esters of fatty alcohols and / or fatty acids, such as isopropyl myristate, glycerol myristate, isononyl isononanoate and acid triglycerides. caprylic or capric acid, isopropyl palmitate and ethyl palmitate.
- mineral oil mention may be made, for example, of hydrogenated polyisobutylene, isododecane, paraffin oils or silicone oils.
- the perfuming agent contained in each oily composition may also be in the form of a mixture.
- the proportion by weight of perfuming agent in each oily composition is generally from 10 to 50%, preferably from 15 to Among the perfuming agents, mention may be made of any type of perfume or fragrance, these terms being used here indifferently.
- perfumes or fragrances are well known to those skilled in the art and include, in particular, those mentioned, for example, in S. Arctander, Perfume and Flavor Chemicals (Montclair, NJ, 1969), S. Arctander, Perfume and Flavor Materials of Natural Origin (Elizabeth, NJ, 1960) and in "Flavor and Fragrance Materials," 1991 (Allured Publishing Co. Wheaton, III, USA).
- the perfumes used in the context of the present invention may comprise natural products such as extracts, essential oils, absolutes, resinoids, resins, concretes, etc., as well as basic synthetic substances such as hydrocarbons, alcohols, aldehydes, ketones, ethers, acids, esters, acetals, ketals, nitriles, etc., including saturated and unsaturated compounds, aliphatic, alicyclic and heterocyclic compounds.
- aqueous phase means a phase having the property of solubilizing polar compounds.
- the continuous aqueous phase of the internal phase is in contact with the external phase and keeps each drop of the oily phase out of contact with the external phase.
- the gelled outer phase is distinct from the continuous aqueous phase of the inner phase.
- the gelled outer phase is an aqueous phase, and typically a hydrogel of the polyelectrolyte in the gelled state.
- the dispersed oily phase and the continuous aqueous phase constitute the emulsion forming the internal phase of the capsules according to the invention and are distinct and immiscible with each other.
- the inner phase and the outer phase of the capsules according to the invention are free of alcohol. More generally, the capsules according to the invention are free of alcohol.
- alcohol is understood to mean a hydrocarbon compound, linear or branched, comprising from 1 to 20 carbon atoms, in which at least one hydrogen atom is replaced by a hydroxyl function.
- Such an alcohol is typically ethanol, isopropanol, n-butanol or any other usual alcohol in the field of cosmetics.
- the inner phase and the outer phase of the capsules according to the invention comprise a reduced amount of surfactant, generally tolerated in the context of a cosmetic application.
- the inner phase is totally free of surfactant.
- the mass percentage of surfactants included in the external phase is generally less than or equal to 0.5%, preferably less than or equal to 0.2% and preferably less than 0.1%, relative to the mass of the phase. external.
- surfactant means an amphiphilic molecule having two parts of different polarity, one lipophilic and apolar, the other hydrophilic and polar.
- a surfactant may be of ionic type (cationic or anionic), zwitterionic or nonionic.
- the capsules according to the invention have a size of 1 to 6 mm, preferably 2 to 5 mm.
- the subject of the invention is also the method for preparing such perfume capsules, comprising the following steps:
- At least one oily composition comprising a perfuming agent, a first aqueous composition and a second aqueous composition, different from the first aqueous composition and comprising at least one polyelectrolyte and at least one surfactant;
- an internal phase formed of a dispersed oily phase consisting of at least one drop of said oily composition, in a continuous aqueous phase, formed of said first aqueous composition, and totally encapsulating the dispersed oily phase, and
- multicomponent drop means a drop consisting of an internal phase, formed of a phase dispersed in a continuous phase completely encapsulating the dispersed phase, and of an external liquid phase. , encapsulating completely at its periphery the internal phase. The continuous phase is in contact with the external phase and keeps the dispersed phase out of contact with the external phase.
- the first aqueous composition and the second aqueous composition are different, so that the liquid external phase and the continuous aqueous phase have different compositions, and have different properties, for example vis-à-vis the reagent of the gelling solution.
- This type of drop is generally carried out by coextrusion of different compositions, namely at least one oily composition, a first aqueous composition and a second aqueous composition, as defined in the aforementioned process.
- the production of multi-component drops by coextrusion can be done for example by separate conveying in a double jacket of a first stream consisting of drops of the oily composition dispersed in the first continuous aqueous composition, and a second stream consisting of of the second aqueous composition.
- the first stream consisting of drops of oily composition dispersed in the first continuous aqueous composition, is for example obtained by injecting the oily composition into a stream of the first aqueous composition circulating in the jacket to form the drops of oily composition. dispersed.
- This injection is for example made through an inner conduit disposed in the jacket, the inner conduit opening preferably recessed from the output of the jacket.
- the double envelope then forms a multi-component drop, the first flow constituting the internal phase and the second flow constituting the liquid external phase.
- the inner phase and the liquid outer phase correspond to the internal phase and the external liquid phase as defined in the aforementioned method.
- the production of multi-component drops by coextrusion can also be carried out by separate conveying in a triple envelope of three streams: a first stream consisting of the oily composition, a second stream consisting of the first aqueous composition and a third stream consisting of the second aqueous composition.
- a first stream consisting of the oily composition
- a second stream consisting of the first aqueous composition
- a third stream consisting of the second aqueous composition.
- each multi-component drop is detached from the double jacket or triple jacket and falls into a volume of air, before being immersed in a gelling solution containing a reagent capable of gelling the polyelectrolyte of the external liquid phase, to form the gelled outer phase of the capsules according to the invention.
- the reagent capable of gelling the polyelectrolyte present in the gelling solution then forms bonds between the different polyelectrolyte chains present in the liquid external phase, then passing to the gelled state. , thus causing the gelling of the liquid external phase.
- the individual polyelectrolyte chains present in the liquid external phase are connected to each other to form a crosslinked network.
- the polyelectrolyte present in the gelled external phase is in the gelled state and is also called gelled polyelectrolyte or gelled polyelectrolyte.
- a gelled external phase suitable for retaining the internal phase is thus formed.
- This gelled outer phase has a proper mechanical strength, that is to say that it is capable of completely surrounding the internal phase and to retain the continuous phase and the dispersed phase present in this internal phase to prevent it from diffusing through the gelled external phase, especially when the capsule is disposed in a gas such as ambient air or in an aqueous or oily composition.
- the gelled outer phase is in the form of a monolayer envelope, completely encapsulating the internal phase at its periphery.
- the perfume capsules according to the invention remain in the gelling solution until the outer phase is completely gelled.
- the gelled perfume capsules are then collected and immersed in an aqueous rinsing solution, generally consisting essentially of water, whereby the gelled capsules are rinsed.
- an aqueous rinsing solution generally consisting essentially of water, whereby the gelled capsules are rinsed.
- This rinsing step makes it possible to extract from the gelled external phase any excess of the reagent suitable for gelling the gelling solution, and all or part of the surfactant initially contained in the second aqueous composition.
- the presence of a surfactant in the second aqueous composition makes it possible to improve the formation and gelation of the multiple drops according to the process as described above.
- the perfume capsules of the invention are rinsed and comprise a reduced amount of surfactant.
- the weight percentage of surfactant included in a capsule according to the invention is generally less than or equal to 0.050%, preferably less than or equal to 0.025% and preferably less than or equal to 0.010%, or even less than or equal to 0.005%, by relative to the total mass of the capsule.
- the perfume capsules according to the invention are then collected and immersed in an aqueous or oily storage composition.
- aqueous solution comprising cosmetic active agents and an aqueous gel optionally comprising such active agents.
- the gelled external phase of the capsules according to the invention comprises at least one polyelectrolyte in the gelled state, advantageously chosen from multivalent ion-reactive food polyelectrolytes.
- polyelectrolyte reactive with multivalent ions means a polyelectrolyte capable of passing from a liquid state in an aqueous solution to a gelled state under the effect of contact with a gelling solution containing multivalent ions such as ions of an alkaline earth metal chosen for example from calcium, barium or magnesium ions.
- the individual polyelectrolyte chains are substantially free to flow relative to one another.
- An aqueous solution of 2% by weight of polyelectrolyte then exhibits a purely viscous behavior at the shear gradients characteristic of the forming process.
- the viscosity of this zero shear solution is between 50 mPa.s and 10,000 mPa.s, advantageously between 3000 mPa.s and 7000 mPa.s.
- the individual polyelectrolyte chains in the liquid state advantageously have a molar mass greater than 65,000 g / mol.
- Said gelling solution is, for example, an aqueous solution of a salt of the type X n M m where X is for example a halide ion such as a chloride, bromide, iodide or fluoride ion, or a tartrate ion, and M is advantageously a multivalent cation an alkaline earth such as calcium, magnesium or barium, and n and m are greater than or equal to 1.
- the concentration of salt of type X n M m in the gelling solution is advantageously from 5% to 20% by weight.
- the individual polyelectrolyte chains together with the multivalent ions form a coherent three-dimensional network which retains the internal phase and prevents its flow.
- the individual chains are held together and can not flow freely relative to each other.
- the viscosity of the formed gel is infinite.
- the gel has a threshold of stress to the flow. This stress threshold is greater than 0.05 Pa.
- the gel also has a modulus of elasticity that is non-zero and greater than 35 kPa.
- the polyelectrolyte is preferably a biocompatible polymer that is harmless to the human body. It is for example produced biologically.
- polysaccharides synthetic polyelectrolytes based on acrylates (sodium, lithium, potassium or ammonium polyacrylate, or polyacrylamide), or synthetic polyelectrolytes based on sulfonates (poly (styrene) sulfonate), for example).
- the polyelectrolyte is chosen from food polysaccharides reactive with multivalent ions.
- the polyelectrolyte is chosen from alkaline alginates, such as sodium alginate or potassium alginate, gelans and pectins.
- the reaction that occurs during gelation is as follows:
- Alginates are produced from brown algae called “laminaria”, referred to as “sea weed”.
- the polyelectrolyte is an alkali metal alginate advantageously having an ⁇ -L-guluronate block content of greater than 50%, especially greater than 55%, or even greater than 60%.
- the polyelectrolyte is, for example, sodium alginate.
- the total weight percentage of polyelectrolyte in the gelled external phase is from 0.5% to 5%, preferably less than 3%.
- the total weight percentage of polyelectrolyte in the gelled external phase is, for example, equal to 2%.
- the gelled outer phase of the capsules according to the invention has a thickness of from 10 to 500 ⁇ , preferably from 20 to 200 ⁇ , and advantageously from 50 to 100 ⁇ .
- the fineness of the thickness of the gelled external phase generally makes it possible to make this external phase transparent, so that the drop or drops of the dispersed oily phase of the internal phase are thus distinctly visible.
- the capsules according to the invention generally have a volume ratio between the internal phase and the external phase greater than 2, and preferably less than 50.
- the capsules according to the invention generally have a volume ratio between the internal phase and the external phase of between 5 and 10.
- the continuous aqueous phase of the inner phase of the capsules according to the invention generally comprises at least one polyelectrolyte of molecular weight greater than
- the continuous aqueous phase is generally substantially water-based, and is typically an aqueous solution or a hydrogel, i.e. a liquid or viscous aqueous composition.
- the continuous aqueous phase may be in the gelled state, but remains distinct from the gelled external phase and its composition remains different from that of the gelled external phase.
- the continuous aqueous phase is not reactive to the reagent capable of gelling the external phase.
- a continuous aqueous phase in the gelled state has the advantage of allowing the oily phase to remain out of contact with the external phase of the capsules.
- polyelectrolytes of high molecular weight suitable for the implementation of the invention, mention may be made of sodium hyaluronate and carrageenan.
- the viscosity of the aqueous phase is generally from 0.1 to 4 Pa.s.
- the aqueous phase may also contain hydrophilic active ingredients, moisturizing agents, or agents for modifying the remanence of the perfuming agent once applied to the skin.
- the dispersed oily phase of the capsules according to the invention generally consists of at most 20 drops, preferably at most 10 drops, advantageously between 1 and 5 drops and for example 1 drop.
- the dispersed oily phase is generally liquid at room temperature and optionally comprises, in addition to at least one perfuming agent, lipophilic active principles, such as anti-wrinkle, anti-aging, protective / anti-free radical active agents, antioxidants, soothing, softening, anti-irritant, tensor / smoothing, emollient, slimming, anti-cellulite, firming, shaping, draining, anti-inflammatory, depigmenting, self-tanning, exfoliating, stimulating cell renewal or stimulating cutaneous microcirculation, absorbing or filtering the UV, anti-dandruff.
- lipophilic active principles such as anti-wrinkle, anti-aging, protective / anti-free radical active agents, antioxidants, soothing, softening, anti-irritant, tensor / smoothing, emollient, slimming, anti-cellulite, firming, shaping, draining, anti-inflammatory, depigmenting, self-tanning, exfoliating, stimulating cell renewal or stimulating cutaneous microcirc
- the oily compositions constituting the drops of the oily phase are generally transparent and optionally comprise a coloring agent, which is identical or different depending on the oily compositions.
- the oil-in-water emulsion of the internal phase consists of a dispersion of at most 20 drops of oily phase in the continuous aqueous phase.
- the drops of the oily phase are identical, that is to say that they consist of the same oily composition.
- the emulsion of the internal phase consists of a single drop of oily phase dispersed in the continuous aqueous phase.
- the dispersed oily phase is kept out of contact with the gelled external phase by the continuous aqueous phase.
- the oily phase is dispersed in the form of at least one drop or distinct drops, of macroscopic size visible to the naked eye.
- the drop or drops constituting the dispersed oily phase of the capsules according to the invention have a diameter of between 0.025 and 4 mm, preferably between 0.2 and 2 mm.
- the total volume of the dispersed oily phase of the capsules represents less than 60%, preferably between 2.5 and 30%, and advantageously between 10 and 20% of the overall volume of said capsule.
- the invention also relates to the use of perfume capsules as described above for the preparation of a perfuming cosmetic composition.
- the capsules according to the invention store in a sealed manner the perfume agent (s) contained in the dispersed oily phase.
- the invention also relates to a perfume cosmetic composition, without alcohol, comprising capsules according to the invention, identical or different, and a cosmetically acceptable vehicle.
- the cosmetically acceptable vehicle is generally based on a predominantly aqueous phase or on the contrary a predominantly oily phase.
- the cosmetically acceptable vehicle optionally contains hydrophilic or lipophilic active ingredients.
- the overall volume of the perfume capsules represents more than 5% and less than 80% of the overall volume of the perfuming cosmetic composition, advantageously more than 33%.
- the perfuming agent When using the cosmetic perfume compositions according to the invention, typically by application to the skin, the perfuming agent is released during the rupture of the gelled outer phase of the capsules.
- perfume compositions according to the invention are typically applied according to a mechanical type of breaking method.
- the perfuming cosmetic composition is applied by compression and direct shearing on the skin of at least one perfume capsule, or by means of a pump bottle which breaks at least one perfume capsule and mixes the different phases, or using a spray bottle that breaks at least one capsule, mixes the different phases and vaporizes the mixture in the form of droplets.
- FIG. large-scale view, in section along a median vertical plane of a perfume capsule according to the invention.
- a perfume capsule 10 according to the invention comprises an internal phase 15 consisting of drops 20 forming an oily phase 25 dispersed in a continuous aqueous phase 30, and a gelled external phase 40 encapsulating the entire external surface of the internal phase 15 to retain the internal phase 15.
- a food capsule 10 according to the invention is spherical in shape and advantageously has an outside diameter of less than 6 mm and of 2 mm to 5 mm.
- the capsule manufacturing process is based on the concentric coextrusion of solutions to form multi-component drops.
- An oily composition is injected into a stream of a first aqueous composition circulating in a first compartment of a double jacket.
- the set of drops of the oily composition dispersed in the first continuous aqueous composition constitutes the first flow.
- a second aqueous composition circulating in the second compartment of the jacket constitutes the second flow.
- a multi-component drop is formed, the first stream constituting the internal phase and the second stream constituting the liquid external phase of the multi-component drop.
- Each multi-component drop is detached from the jacket and falls into a volume of air, before being immersed in a gelling solution of calcium lactate.
- the formed capsules are rinsed in a water-based rinse solution and stored in water.
- the size of the internal phase, the number of drops of the oily phase dispersed and the thickness of the external phase of the capsules formed are controlled by the use of several independent syringe pumps, regulating the injection rates of the various oily compositions. and aqueous.
- the oily composition constituting the dispersed oily phase of the inner phase of the capsules is a perfuming agent as described in the description.
- the first aqueous composition constituting the continuous aqueous phase of the inner phase of the capsules is an aqueous solution of sodium hyaluronate at 1.0% by weight.
- the second aqueous composition constituting the gelled outer aqueous phase of the capsules is an aqueous solution having a weight percentage of sodium alginate of 2.0% and a weight percentage of sodium dodecyl sulphate (SDS) of 0.1%.
- the flow rate of the oily composition is set at 2 ml / h.
- the flow rate of the first aqueous composition is set at 16.75 ml / h.
- the flow rate of the first aqueous composition is set at 2 mL / h.
- Fragrance capsules are obtained, the mass percentage of each component being given relative to the total mass of a capsule.
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Abstract
Description
Capsule parfumante sans alcool Perfume capsule without alcohol
La présente invention concerne des compositions parfumantes sous forme de capsules parfumantes, leur procédé de préparation et leur utilisation pour une application dans le domaine de la cosmétique. Elle a également pour objet des compositions cosmétiques comprenant lesdites capsules parfumantes. The present invention relates to perfume compositions in the form of perfume capsules, to a process for their preparation and to their use for an application in the field of cosmetics. It also relates to cosmetic compositions comprising said perfume capsules.
La préparation de compositions parfumantes repose principalement sur la dissolution de composés aromatiques dans une solution hydroalcoolique (mélange d'eau et d'alcool, typiquement de l'éthanol). L'utilisation d'un alcool tel que l'éthanol permet, grâce à ses propriétés de solvant, de solubiliser les composés aromatiques qui sont généralement insolubles ou peu solubles dans l'eau. The preparation of perfume compositions is based mainly on the dissolution of aromatic compounds in a hydroalcoholic solution (mixture of water and alcohol, typically ethanol). The use of an alcohol such as ethanol makes it possible, by virtue of its solvent properties, to solubilize aromatic compounds which are generally insoluble or poorly soluble in water.
Cependant, l'alcool présente de nombreux inconvénients : il est un dermo- sensibilisant, desséchant, irritant. Par ailleurs, son utilisation est déconseillée pour les enfants en bas âge. De plus, la réglementation concernant la protection de l'environnement est récemment devenue plus stricte au sujet des composés volatils tels que l'éthanol. However, alcohol has many disadvantages: it is a dermocensitizer, desiccant, irritant. Moreover, its use is not recommended for young children. In addition, environmental protection regulations have recently become stricter on volatile compounds such as ethanol.
Il existe à ce jour des compositions parfumantes à base de particules polymériques (EP 0 334 490). Toutefois, ces compositions ont un aspect opaque, les particules sont difficilement applicables par spray en raison de leur viscosité élevée, et ne sont pas résorbables sur la peau, ce qui leur confèrent un toucher désagréable lors de leur utilisation. To date, there are perfuming compositions based on polymeric particles (EP 0 334 490). However, these compositions have an opaque appearance, the particles are difficult to apply by spray because of their high viscosity, and are not resorbable on the skin, which gives them an unpleasant feel during use.
La demande EP 0 572 080 décrit la préparation de microémulsions comprenant des tensio-actifs dans la phase lipophile parfumante, ce qui est déconseillé dans le cas de peaux fragiles ou atopiques. De plus, ces microémulsions sont sensibles à la dilution et se déstabilisent facilement, ce qui rend difficile leur incorporation dans d'autres produits tels que les produits cosmétiques. Elles contiennent également un fort taux de tensio-actifs, ce qui est reconnu comme étant un facteur irritant, notamment lorsque le taux de phase lipophile parfumante est élevé. The application EP 0 572 080 describes the preparation of microemulsions comprising surfactants in the lipophilic perfuming phase, which is disadvised in the case of fragile or atopic skin. In addition, these microemulsions are sensitive to dilution and easily destabilize, which makes it difficult to incorporate them into other products such as cosmetics. They also contain a high level of surfactants, which is recognized as being an irritating factor, especially when the lipophilic perfume phase is high.
Ainsi, il existe à ce jour un besoin dans le domaine de la parfumerie et plus généralement de la cosmétique pour remplacer les compositions hydroalcooliques et fournir des compositions parfumantes sans alcool et comprenant une quantité réduite de tensio-actifs par rapport aux compositions actuelles. La présente invention a pour but de fournir de nouvelles compositions parfumantes permettant de remplacer les compositions hydroalcooliques actuelles. Thus, there is to date a need in the field of perfumery and more generally cosmetics to replace hydroalcoholic compositions and provide perfume compositions without alcohol and comprising a reduced amount of surfactants compared to current compositions. The present invention aims to provide new perfume compositions for replacing current hydroalcoholic compositions.
La présente invention a également pour but de fournir de nouvelles compositions parfumantes sans alcool et comprenant une quantité réduite de tensio-actifs, contenant notamment des capsules parfumantes. The present invention also aims to provide new perfume compositions without alcohol and comprising a reduced amount of surfactants, including perfume capsules.
Ainsi, la présente invention concerne une capsule parfumante sans alcool, comprenant : Thus, the present invention relates to a fragrance capsule without alcohol, comprising:
- une phase interne formée d'une émulsion de type huile dans eau, constituée d'une phase huileuse dispersée constituée d'au moins une goutte d'une composition huileuse comprenant un agent parfumant, et d'une phase aqueuse continue, encapsulant totalement la ou lesdites gouttes de la phase huileuse ; et une phase externe gélifiée comprenant au moins un polyélectrolyte à l'état gélifié, encapsulant totalement ladite phase interne à sa périphérie. an internal phase formed of an oil-in-water emulsion, consisting of a dispersed oily phase consisting of at least one drop of an oily composition comprising a perfuming agent, and a continuous aqueous phase, totally encapsulating the or said drops of the oily phase; and an outer gelled phase comprising at least one polyelectrolyte in the gelled state, completely encapsulating said internal phase at its periphery.
Dans le cadre de la présente description, on entend par « phase huileuse >> une phase ayant la propriété de solubiliser des composés apolaires, tels que des corps gras, des huiles, des lipides. For the purposes of the present description, the term "oily phase" means a phase having the property of solubilizing apolar compounds, such as fatty substances, oils, lipids.
La phase huileuse est insoluble dans l'eau. Les compositions huileuses constituant la phase huileuse comprennent de préférence un corps gras, une huile ou un mélange d'huiles d'origine végétale, animale ou minérale. The oily phase is insoluble in water. The oily compositions constituting the oily phase preferably comprise a fatty substance, an oil or a mixture of oils of vegetable, animal or mineral origin.
A titre d'huile végétale, on peut par exemple citer l'huile d'amande douce, l'huile de jojoba, l'huile de palme ou le phytosqualane. As a vegetable oil, mention may for example be made of sweet almond oil, jojoba oil, palm oil or phytosqualane.
A titre de corps gras, on peut par exemple citer les esters d'alcools gras et/ou d'acides gras, tels que le myristate d'isopropyle, le myristate de glycérol, l'isononanoate d'isononyle, les triglycérides d'acide caprylique ou d'acide caprique, le palmitate d'isopropyle et le palmitate d'éthyle. Examples of fatty substances that may be mentioned include esters of fatty alcohols and / or fatty acids, such as isopropyl myristate, glycerol myristate, isononyl isononanoate and acid triglycerides. caprylic or capric acid, isopropyl palmitate and ethyl palmitate.
A titre d'huile animale, on peut par exemple citer le squalène. By way of animal oil, mention may be made, for example, of squalene.
A titre d'huile minérale, on peut par exemple citer le polyisobutylène hydrogéné, l'isododécane, les huiles de paraffine ou les huiles de silicone. As mineral oil, mention may be made, for example, of hydrogenated polyisobutylene, isododecane, paraffin oils or silicone oils.
L'agent parfumant contenu dans chaque composition huileuse peut également être sous la forme d'un mélange. La proportion massique d'agent parfumant dans chaque composition huileuse est généralement comprise de 10 à 50%, de préférence de 15 à Parmi les agents parfumants, on peut notamment citer tout type de parfum ou de fragrance, ces termes étant utilisés ici de façon indifférente. Ces parfums ou fragrances sont bien connus de l'homme du métier et incluent notamment ceux mentionnés, par exemple, dans S. Arctander, Perfume and Flavor Chemicals (Montclair, N.J., 1969), S. Arctander, Perfume and Flavor Materials of Natural Origin (Elizabeth, N.J., 1960) et dans "Flavor and Fragrance Materials", 1991 (Allured Publishing Co. Wheaton, III. USA). The perfuming agent contained in each oily composition may also be in the form of a mixture. The proportion by weight of perfuming agent in each oily composition is generally from 10 to 50%, preferably from 15 to Among the perfuming agents, mention may be made of any type of perfume or fragrance, these terms being used here indifferently. These perfumes or fragrances are well known to those skilled in the art and include, in particular, those mentioned, for example, in S. Arctander, Perfume and Flavor Chemicals (Montclair, NJ, 1969), S. Arctander, Perfume and Flavor Materials of Natural Origin (Elizabeth, NJ, 1960) and in "Flavor and Fragrance Materials," 1991 (Allured Publishing Co. Wheaton, III, USA).
Les parfums utilisés dans le cadre de la présente invention peuvent comprendre les produits naturels comme les extraits, les huiles essentielles, les absolus, les résinoïdes, les résines, les concrètes, etc .. ainsi que les substances basiques de synthèse comme les hydrocarbures, les alcools, les aldéhydes, les cétones, les éthers, les acides, les esters, les acétals, les cétals, les nitriles, etc ., y compris les composés, saturés et insaturés, les composés aliphatiques, alicycliques et hétérocycliques. The perfumes used in the context of the present invention may comprise natural products such as extracts, essential oils, absolutes, resinoids, resins, concretes, etc., as well as basic synthetic substances such as hydrocarbons, alcohols, aldehydes, ketones, ethers, acids, esters, acetals, ketals, nitriles, etc., including saturated and unsaturated compounds, aliphatic, alicyclic and heterocyclic compounds.
Dans le cadre de la présente description, on entend par « phase aqueuse >> une phase ayant la propriété de solubiliser des composés polaires. In the context of the present description, the term "aqueous phase" means a phase having the property of solubilizing polar compounds.
La phase aqueuse continue de la phase interne est au contact de la phase externe et maintient chaque goutte de la phase huileuse hors de contact de la phase externe. The continuous aqueous phase of the internal phase is in contact with the external phase and keeps each drop of the oily phase out of contact with the external phase.
La phase externe gélifiée est distincte de la phase aqueuse continue de la phase interne. De préférence, la phase externe gélifiée est une phase aqueuse, et typiquement un hydrogel du polyélectrolyte à l'état gélifié. The gelled outer phase is distinct from the continuous aqueous phase of the inner phase. Preferably, the gelled outer phase is an aqueous phase, and typically a hydrogel of the polyelectrolyte in the gelled state.
La phase huileuse dispersée et la phase aqueuse continue constituent l'émulsion formant la phase interne des capsules selon l'invention et sont distinctes et non miscibles l'une dans l'autre. The dispersed oily phase and the continuous aqueous phase constitute the emulsion forming the internal phase of the capsules according to the invention and are distinct and immiscible with each other.
La phase interne et la phase externe des capsules selon l'invention sont exemptes d'alcool. Plus généralement, les capsules selon l'invention sont exemptes d'alcool. The inner phase and the outer phase of the capsules according to the invention are free of alcohol. More generally, the capsules according to the invention are free of alcohol.
Dans le cadre de la présente description, on entend par « alcool >> un composé hydrocarboné, linéaire ou ramifié, comprenant de 1 à 20 atomes de carbone, dans lequel au moins un atome d'hydrogène est remplacé par une fonction hydroxyle. Un tel alcool est typiquement l'éthanol, l'isopropanol, le n-butanol ou tout autre alcool usuel dans le domaine de la cosmétique. In the context of the present description, the term "alcohol" is understood to mean a hydrocarbon compound, linear or branched, comprising from 1 to 20 carbon atoms, in which at least one hydrogen atom is replaced by a hydroxyl function. Such an alcohol is typically ethanol, isopropanol, n-butanol or any other usual alcohol in the field of cosmetics.
La phase interne et la phase externe des capsules selon l'invention comprennent une quantité réduite de tensio-actif, généralement tolérée dans le cadre d'une application cosmétique. The inner phase and the outer phase of the capsules according to the invention comprise a reduced amount of surfactant, generally tolerated in the context of a cosmetic application.
De préférence, la phase interne est totalement exempte de tensio-actif. Le pourcentage massique de tensio-actifs compris dans la phase externe est généralement inférieur ou égal à 0,5%, de préférence inférieur ou égal à 0,2% et préférentiellement inférieur à 0,1 %, par rapport à la masse de la phase externe. Dans le cadre de la présente description, on entend par « tensio-actif >> une molécule amphiphile présentant deux parties de polarité différente, l'une lipophile et apolaire, l'autre hydrophile et polaire. Un tensio-actif peut être de type ionique (cationique ou anionique), zwitterionique ou non-ionique. Les capsules selon l'invention possèdent une taille comprise de 1 à 6 mm, de préférence de 2 à 5 mm. Preferably, the inner phase is totally free of surfactant. The mass percentage of surfactants included in the external phase is generally less than or equal to 0.5%, preferably less than or equal to 0.2% and preferably less than 0.1%, relative to the mass of the phase. external. In the context of the present description, the term "surfactant" means an amphiphilic molecule having two parts of different polarity, one lipophilic and apolar, the other hydrophilic and polar. A surfactant may be of ionic type (cationic or anionic), zwitterionic or nonionic. The capsules according to the invention have a size of 1 to 6 mm, preferably 2 to 5 mm.
L'invention a également pour objet le procédé de préparation de telles capsules parfumantes, comprenant les étapes suivantes : The subject of the invention is also the method for preparing such perfume capsules, comprising the following steps:
- la mise en contact d'au moins une composition huileuse comprenant un agent parfumant, d'une première composition aqueuse et d'une deuxième composition aqueuse, différente de la première composition aqueuse et comprenant au moins un polyélectrolyte et au moins un tensio-actif, contacting at least one oily composition comprising a perfuming agent, a first aqueous composition and a second aqueous composition, different from the first aqueous composition and comprising at least one polyelectrolyte and at least one surfactant; ,
- la formation d'une goutte multi-composante constituée : the formation of a multi-component drop constituted by:
- d'une phase interne, formée d'une phase huileuse dispersée constituée d'au moins une goutte de ladite composition huileuse, dans une phase aqueuse continue, formée de ladite première composition aqueuse, et encapsulant totalement la phase huileuse dispersée, et an internal phase, formed of a dispersed oily phase consisting of at least one drop of said oily composition, in a continuous aqueous phase, formed of said first aqueous composition, and totally encapsulating the dispersed oily phase, and
- d'une phase externe liquide formée de ladite deuxième composition aqueuse, encapsulant totalement à sa périphérie la phase interne, an external liquid phase formed of said second aqueous composition, totally encapsulating at its periphery the internal phase,
- l'immersion de ladite goutte multi-composante dans une solution gélifiante contenant un réactif propre à gélifier le polyélectrolyte de la phase externe liquide, ce par quoi on obtient la phase externe gélifiée, the immersion of said multi-component droplet in a gelling solution containing a reagent capable of gelling the polyelectrolyte of the external liquid phase, whereby the gelled external phase is obtained,
- le rinçage des capsules gélifiées formées dans une solution de rinçage, ce par quoi on obtient des capsules gélifiées rincées, et - la récupération des capsules gélifiées rincées. Dans le cadre de la présente description, on entend par « goutte multi- composante >> une goutte constituée d'une phase interne, formée d'une phase dispersée dans une phase continue encapsulant totalement la phase dispersée, et d'une phase externe liquide, encapsulant totalement à sa périphérie la phase interne. La phase continue est au contact de la phase externe et maintient la phase dispersée hors de contact de la phase externe. the rinsing of the gelled capsules formed in a rinsing solution, whereby rinsed gelled capsules are obtained, and the recovery of the gelled rinsed capsules. In the context of the present description, the term "multicomponent drop" means a drop consisting of an internal phase, formed of a phase dispersed in a continuous phase completely encapsulating the dispersed phase, and of an external liquid phase. , encapsulating completely at its periphery the internal phase. The continuous phase is in contact with the external phase and keeps the dispersed phase out of contact with the external phase.
La première composition aqueuse et la deuxième composition aqueuse sont différentes, de sorte que la phase externe liquide et la phase aqueuse continue possèdent des compositions différentes, et présentent des propriétés différentes, par exemple vis-à- vis du réactif de la solution gélifiante. The first aqueous composition and the second aqueous composition are different, so that the liquid external phase and the continuous aqueous phase have different compositions, and have different properties, for example vis-à-vis the reagent of the gelling solution.
La production de ce type de goutte est généralement effectuée par co-extrusion de différentes compositions, à savoir au moins une composition huileuse, une première composition aqueuse et une deuxième composition aqueuse, telles que définies dans le procédé précité. The production of this type of drop is generally carried out by coextrusion of different compositions, namely at least one oily composition, a first aqueous composition and a second aqueous composition, as defined in the aforementioned process.
La production de gouttes multi-composante par co-extrusion peut se faire par exemple par convoyage séparé dans une double enveloppe d'un premier flux constitué de gouttes de la composition huileuse dispersées dans la première composition aqueuse continue, et d'un deuxième flux constitué de la deuxième composition aqueuse. The production of multi-component drops by coextrusion can be done for example by separate conveying in a double jacket of a first stream consisting of drops of the oily composition dispersed in the first continuous aqueous composition, and a second stream consisting of of the second aqueous composition.
Le premier flux, constitué de gouttes de composition huileuse dispersées dans la première composition aqueuse continue, est par exemple obtenu par l'injection de la composition huileuse dans un courant de la première composition aqueuse circulant dans la double enveloppe pour former les gouttes de composition huileuse dispersées. The first stream, consisting of drops of oily composition dispersed in the first continuous aqueous composition, is for example obtained by injecting the oily composition into a stream of the first aqueous composition circulating in the jacket to form the drops of oily composition. dispersed.
Cette injection est par exemple réalisée à travers un conduit interne disposé dans la double enveloppe, le conduit interne débouchant de préférence en retrait de la sortie de la double enveloppe. This injection is for example made through an inner conduit disposed in the jacket, the inner conduit opening preferably recessed from the output of the jacket.
A la sortie de la double enveloppe, se forme alors une goutte multi-composante, le premier flux constituant la phase interne et le deuxième flux constituant la phase externe liquide. La phase interne et la phase externe liquide correspondent à la phase interne et la phase externe liquide telles que définies dans le procédé précité. At the exit of the double envelope, then forms a multi-component drop, the first flow constituting the internal phase and the second flow constituting the liquid external phase. The inner phase and the liquid outer phase correspond to the internal phase and the external liquid phase as defined in the aforementioned method.
Selon une variante, la production de gouttes multi-composante par co-extrusion peut également se faire par convoyage séparé dans une triple enveloppe de trois flux : un premier flux constitué de la composition huileuse, un deuxième flux constitué de la première composition aqueuse et un troisième flux constitué de la deuxième composition aqueuse. A la sortie de la triple enveloppe, les trois flux entrent en contact et se forme alors une goutte multi-composante, le premier et le deuxième flux constituant la phase interne et le troisième flux constituant la phase externe liquide. Selon le mode de production, chaque goutte multi-composante se détache de la double enveloppe ou de la triple enveloppe et chute dans un volume d'air, avant d'être immergée dans une solution gélifiante contenant un réactif propre à gélifier le polyélectrolyte de la phase externe liquide, pour former la phase externe gélifiée des capsules selon l'invention. According to one variant, the production of multi-component drops by coextrusion can also be carried out by separate conveying in a triple envelope of three streams: a first stream consisting of the oily composition, a second stream consisting of the first aqueous composition and a third stream consisting of the second aqueous composition. At the exit of the triple envelope, the three flows come into contact and then form a multi-component drop, the first and the second stream constituting the inner phase and the third stream constituting the liquid external phase. Depending on the production method, each multi-component drop is detached from the double jacket or triple jacket and falls into a volume of air, before being immersed in a gelling solution containing a reagent capable of gelling the polyelectrolyte of the external liquid phase, to form the gelled outer phase of the capsules according to the invention.
Lorsque la goutte multi-composante entre en contact de la solution gélifiante, le réactif propre à gélifier le polyélectrolyte présent dans la solution gélifiante forme alors des liaisons entre les différentes chaînes de polyélectrolyte présentes dans la phase externe liquide, passant alors à l'état gélifié, provoquant ainsi la gélification de la phase externe liquide. When the multi-component drop comes into contact with the gelling solution, the reagent capable of gelling the polyelectrolyte present in the gelling solution then forms bonds between the different polyelectrolyte chains present in the liquid external phase, then passing to the gelled state. , thus causing the gelling of the liquid external phase.
Sans vouloir être lié à une théorie particulière, lors du passage à l'état gélifié du polyélectrolyte, les chaînes individuelles de polyélectrolyte présentes dans la phase externe liquide se raccordent les unes aux autres pour former un réseau réticulé. Without wishing to be bound to a particular theory, during the transition to the gelled state of the polyelectrolyte, the individual polyelectrolyte chains present in the liquid external phase are connected to each other to form a crosslinked network.
Dans le cadre de la présente description, le polyélectrolyte présent dans la phase externe gélifiée est à l'état gélifié et est également appelé polyélectrolyte à l'état gélifié ou encore polyélectrolyte gélifié. In the context of the present description, the polyelectrolyte present in the gelled external phase is in the gelled state and is also called gelled polyelectrolyte or gelled polyelectrolyte.
Une phase externe gélifiée, propre à retenir la phase interne est ainsi formée. Cette phase externe gélifiée présente une tenue mécanique propre, c'est-à-dire qu'elle est capable d'entourer totalement la phase interne et de retenir la phase continue et la phase dispersée présentes dans cette phase interne pour l'empêcher de diffuser à travers la phase externe gélifiée, notamment lorsque la capsule est disposée dans un gaz tel que l'air ambiant ou dans une composition aqueuse ou huileuse. A gelled external phase suitable for retaining the internal phase is thus formed. This gelled outer phase has a proper mechanical strength, that is to say that it is capable of completely surrounding the internal phase and to retain the continuous phase and the dispersed phase present in this internal phase to prevent it from diffusing through the gelled external phase, especially when the capsule is disposed in a gas such as ambient air or in an aqueous or oily composition.
De manière générale, la phase externe gélifiée se présente sous la forme d'une enveloppe monocouche, encapsulant totalement la phase interne à sa périphérie. In general, the gelled outer phase is in the form of a monolayer envelope, completely encapsulating the internal phase at its periphery.
Les capsules parfumantes selon l'invention séjournent dans la solution gélifiante le temps que la phase externe soit complètement gélifiée. The perfume capsules according to the invention remain in the gelling solution until the outer phase is completely gelled.
Les capsules parfumantes gélifiées sont ensuite collectées et plongées dans une solution aqueuse de rinçage, généralement essentiellement constituée d'eau, ce par quoi les capsules gélifiées sont rincées. Cette étape de rinçage permet d'extraire de la phase externe gélifiée un éventuel excès du réactif propre à gélifier de la solution gélifiante, et tout ou partie du tensio-actif contenu initialement dans la deuxième composition aqueuse. La présence d'un tensio-actif dans la deuxième composition aqueuse permet d'améliorer la formation et la gélification des gouttes multiples selon le procédé tel que décrit précédemment. The gelled perfume capsules are then collected and immersed in an aqueous rinsing solution, generally consisting essentially of water, whereby the gelled capsules are rinsed. This rinsing step makes it possible to extract from the gelled external phase any excess of the reagent suitable for gelling the gelling solution, and all or part of the surfactant initially contained in the second aqueous composition. The presence of a surfactant in the second aqueous composition makes it possible to improve the formation and gelation of the multiple drops according to the process as described above.
Après cette étape de rinçage, les capsules parfumantes de l'invention sont rincées et comprennent une quantité réduite de tensio-actif. After this rinsing step, the perfume capsules of the invention are rinsed and comprise a reduced amount of surfactant.
Le pourcentage massique de tensio-actif compris dans une capsule selon l'invention est généralement inférieur ou égal à 0,050%, de préférence inférieur ou égal à 0,025% et préférentiellement inférieur ou égal à 0,010%, voire inférieur ou égal à 0,005%, par rapport à la masse totale de la capsule. The weight percentage of surfactant included in a capsule according to the invention is generally less than or equal to 0.050%, preferably less than or equal to 0.025% and preferably less than or equal to 0.010%, or even less than or equal to 0.005%, by relative to the total mass of the capsule.
Les capsules parfumantes selon l'invention sont ensuite collectées et plongées dans une composition de stockage, aqueuse ou huileuse. The perfume capsules according to the invention are then collected and immersed in an aqueous or oily storage composition.
A titre de composition de stockage, on peut citer une solution aqueuse comprenant des actifs cosmétiques et un gel aqueux comprenant éventuellement de tels actifs. As a storage composition, mention may be made of an aqueous solution comprising cosmetic active agents and an aqueous gel optionally comprising such active agents.
La phase externe gélifiée des capsules selon l'invention comprend au moins un polyélectrolyte à l'état gélifié, avantageusement choisi parmi les polyélectrolytes alimentaires réactifs aux ions multivalents. Dans le cadre de la présente description, on entend par « polyélectrolyte réactif aux ions multivalents >> un polyélectrolyte susceptible de passer d'un état liquide dans une solution aqueuse à un état gélifié sous l'effet d'un contact avec une solution gélifiante contenant des ions multivalents tels que des ions d'un métal alcalino-terreux choisis par exemple parmi les ions calcium, baryum ou magnésium. The gelled external phase of the capsules according to the invention comprises at least one polyelectrolyte in the gelled state, advantageously chosen from multivalent ion-reactive food polyelectrolytes. In the context of the present description, the term "polyelectrolyte reactive with multivalent ions" means a polyelectrolyte capable of passing from a liquid state in an aqueous solution to a gelled state under the effect of contact with a gelling solution containing multivalent ions such as ions of an alkaline earth metal chosen for example from calcium, barium or magnesium ions.
A l'état liquide, les chaînes individuelles de polyélectrolyte sont sensiblement libres de s'écouler les unes par rapport aux autres. Une solution aqueuse de 2% en masse de polyélectrolyte présente alors un comportement purement visqueux aux gradients de cisaillement caractéristiques du procédé de mise en forme. La viscosité de cette solution à cisaillement nul est entre 50 mPa.s et 10000 mPa.s, avantageusement entre 3000 mPa.s et 7000 mPa.s. In the liquid state, the individual polyelectrolyte chains are substantially free to flow relative to one another. An aqueous solution of 2% by weight of polyelectrolyte then exhibits a purely viscous behavior at the shear gradients characteristic of the forming process. The viscosity of this zero shear solution is between 50 mPa.s and 10,000 mPa.s, advantageously between 3000 mPa.s and 7000 mPa.s.
Les chaînes individuelles de polyélectrolyte à l'état liquide présentent avantageusement une masse molaire supérieure à 65 000 g/moles. The individual polyelectrolyte chains in the liquid state advantageously have a molar mass greater than 65,000 g / mol.
Ladite solution gélifiante est par exemple une solution aqueuse d'un sel de type XnMm où X est par exemple un ion halogénure tel qu'un ion chlorure, bromure, iodure ou fluorure, ou bien encore un ion tartrate, et M est avantageusement un cation multivalent d'un alcalino-terreux tel que le calcium, le magnésium ou le baryum, et n et m sont supérieurs ou égaux à 1 . Said gelling solution is, for example, an aqueous solution of a salt of the type X n M m where X is for example a halide ion such as a chloride, bromide, iodide or fluoride ion, or a tartrate ion, and M is advantageously a multivalent cation an alkaline earth such as calcium, magnesium or barium, and n and m are greater than or equal to 1.
La concentration en sel de type XnMm dans la solution gélifiante est avantageusement comprise de 5 % à 20 % en masse. The concentration of salt of type X n M m in the gelling solution is advantageously from 5% to 20% by weight.
A l'état gélifié, les chaînes individuelles de polyélectrolyte forment, avec les ions multivalents, un réseau tridimensionnel cohérent qui retient la phase interne et empêche son écoulement. Les chaînes individuelles sont retenues les unes par rapport aux autres et ne peuvent pas s'écouler librement les unes par rapport aux autres. Dans cet état, la viscosité du gel formé est infinie. De plus le gel a un seuil de contrainte à l'écoulement. Ce seuil de contrainte est supérieur à 0,05 Pa. Le gel possède également un module d'élasticité non-nul et supérieur à 35 kPa. In the gelled state, the individual polyelectrolyte chains together with the multivalent ions form a coherent three-dimensional network which retains the internal phase and prevents its flow. The individual chains are held together and can not flow freely relative to each other. In this state, the viscosity of the formed gel is infinite. In addition, the gel has a threshold of stress to the flow. This stress threshold is greater than 0.05 Pa. The gel also has a modulus of elasticity that is non-zero and greater than 35 kPa.
Le polyélectrolyte est de préférence un polymère biocompatible inoffensif pour le corps humain. Il est par exemple produit biologiquement. The polyelectrolyte is preferably a biocompatible polymer that is harmless to the human body. It is for example produced biologically.
Avantageusement, il est choisi parmi les polysaccharides, les polyélectrolytes de synthèse à base d'acrylates (polyacrylate de sodium, de lithium, de potassium ou d'ammonium, ou polyacrylamide), ou les polyélectrolytes de synthèse à base de sulfonates (poly(styrène sulfonate) de sodium, par exemple). Advantageously, it is chosen from polysaccharides, synthetic polyelectrolytes based on acrylates (sodium, lithium, potassium or ammonium polyacrylate, or polyacrylamide), or synthetic polyelectrolytes based on sulfonates (poly (styrene) sulfonate), for example).
De préférence, le polyélectrolyte est choisi parmi les polysaccharides alimentaires réactifs aux ions multivalents. Preferably, the polyelectrolyte is chosen from food polysaccharides reactive with multivalent ions.
Plus particulièrement, le polyélectrolyte est choisi parmi les alginates d'alcalin, tel qu'un alginate de sodium ou un alginate de potassium, les géllanes et les pectines. More particularly, the polyelectrolyte is chosen from alkaline alginates, such as sodium alginate or potassium alginate, gelans and pectins.
Dans le cas où le polyélectrolyte est un alginate de sodium (NaAIg), et où le réactif est le chlorure de calcium, la réaction qui se produit lors de la gélification est la suivante : In the case where the polyelectrolyte is a sodium alginate (NaAIg), and where the reagent is calcium chloride, the reaction that occurs during gelation is as follows:
2NaAlg + CaCI2 Ca(Alg)2 + 2NaCI 2NaAlg + CaCI 2 Ca (Alg) 2 + 2NaCI
Les alginates sont produits à partir d'algues brunes appelées « laminaires >>, désignées par le terme anglais « sea weed >>. Alginates are produced from brown algae called "laminaria", referred to as "sea weed".
De préférence, le polyélectrolyte est un alginate d'alcalin ayant avantageusement une teneur en bloc α-L-guluronate supérieure à 50%, notamment supérieure à 55%, voire supérieure à 60%. Preferably, the polyelectrolyte is an alkali metal alginate advantageously having an α-L-guluronate block content of greater than 50%, especially greater than 55%, or even greater than 60%.
Le polyélectrolyte est par exemple un alginate de sodium. The polyelectrolyte is, for example, sodium alginate.
Selon un mode de réalisation préféré, le pourcentage massique total en polyélectrolyte dans la phase externe gélifiée est compris de 0,5% à 5%, de préférence inférieur à 3%. According to a preferred embodiment, the total weight percentage of polyelectrolyte in the gelled external phase is from 0.5% to 5%, preferably less than 3%.
Le pourcentage massique total en polyélectrolyte dans la phase externe gélifiée est par exemple égal à 2%. De préférence, la phase externe gélifiée des capsules selon l'invention possède une épaisseur comprise de 10 à 500 μηι, de préférence de 20 à 200 μηι, et avantageusement de 50 à 100 μηι. The total weight percentage of polyelectrolyte in the gelled external phase is, for example, equal to 2%. Preferably, the gelled outer phase of the capsules according to the invention has a thickness of from 10 to 500 μηι, preferably from 20 to 200 μηι, and advantageously from 50 to 100 μηι.
La finesse de l'épaisseur de la phase externe gélifiée permet généralement de rendre cette phase externe transparente, de sorte que la ou les gouttes de la phase huileuse dispersée de la phase interne sont ainsi visibles distinctement. The fineness of the thickness of the gelled external phase generally makes it possible to make this external phase transparent, so that the drop or drops of the dispersed oily phase of the internal phase are thus distinctly visible.
Les capsules selon l'invention présentent généralement un rapport volumique entre la phase interne et la phase externe supérieur à 2, et de préférence inférieur à 50. The capsules according to the invention generally have a volume ratio between the internal phase and the external phase greater than 2, and preferably less than 50.
Selon un mode de réalisation particulier, les capsules selon l'invention présentent généralement un rapport volumique entre la phase interne et la phase externe compris entre 5 et 10. According to a particular embodiment, the capsules according to the invention generally have a volume ratio between the internal phase and the external phase of between 5 and 10.
La phase aqueuse continue de la phase interne des capsules selon l'invention comprend généralement au moins un polyélectrolyte de poids moléculaire supérieur àThe continuous aqueous phase of the inner phase of the capsules according to the invention generally comprises at least one polyelectrolyte of molecular weight greater than
5.105 g/mol, de préférence supérieur à 1 .106 g/mol, avantageusement compris entre 1 et5.10 5 g / mol, preferably greater than 1 .10 6 g / mol, advantageously between 1 and
2.106 g/mol. 2.10 6 g / mol.
La phase aqueuse continue est généralement essentiellement à base d'eau, et est typiquement une solution aqueuse ou un hydrogel, c'est-à-dire une composition aqueuse liquide ou visqueuse. La phase aqueuse continue peut être à l'état gélifié, mais reste distincte de la phase externe gélifiée et sa composition reste différente de celle de la phase externe gélifiée. The continuous aqueous phase is generally substantially water-based, and is typically an aqueous solution or a hydrogel, i.e. a liquid or viscous aqueous composition. The continuous aqueous phase may be in the gelled state, but remains distinct from the gelled external phase and its composition remains different from that of the gelled external phase.
Typiquement, la phase aqueuse continue n'est pas réactive au réactif propre à gélifier la phase externe. Typically, the continuous aqueous phase is not reactive to the reagent capable of gelling the external phase.
Une phase aqueuse continue à l'état gélifié présente l'avantage de permettre le maintien de la phase huileuse hors de contact avec la phase externe des capsules. A continuous aqueous phase in the gelled state has the advantage of allowing the oily phase to remain out of contact with the external phase of the capsules.
Parmi les polyélectrolytes de haut poids moléculaire adapté à la mise en œuvre de l'invention, on peut citer le hyaluronate de sodium et le carraghénane. Among the polyelectrolytes of high molecular weight suitable for the implementation of the invention, mention may be made of sodium hyaluronate and carrageenan.
La viscosité de la phase aqueuse est généralement comprise de 0,1 à 4 Pa.s. The viscosity of the aqueous phase is generally from 0.1 to 4 Pa.s.
La phase aqueuse peut également contenir des principes actifs hydrophiles, des agents hydratants, ou encore des agents permettant de modifier la rémanence de l'agent parfumant une fois appliqué sur la peau. La phase huileuse dispersée des capsules selon l'invention est généralement constituée d'au plus 20 gouttes, de préférence au plus 10 gouttes, avantageusement entre 1 et 5 gouttes et par exemple 1 goutte. The aqueous phase may also contain hydrophilic active ingredients, moisturizing agents, or agents for modifying the remanence of the perfuming agent once applied to the skin. The dispersed oily phase of the capsules according to the invention generally consists of at most 20 drops, preferably at most 10 drops, advantageously between 1 and 5 drops and for example 1 drop.
La phase huileuse dispersée est généralement liquide à la température ambiante et comprend éventuellement, en plus d'au moins un agent parfumant, des principes actifs lipophiles, tels que des actifs anti-rides, anti-âge, protecteurs/anti-radicalaires, antioxydants, apaisants, adoucissants, anti-irritants, tenseurs/lissants, émollients, amincissants, anti-capitons, raffermissant, gainants, drainants, anti-inflammatoires, dépigmentants, autobronzants, exfoliants, stimulant le renouvellement cellulaire ou stimulant la microcirculation cutanée, absorbants ou filtrants les UV, antipelliculaires. The dispersed oily phase is generally liquid at room temperature and optionally comprises, in addition to at least one perfuming agent, lipophilic active principles, such as anti-wrinkle, anti-aging, protective / anti-free radical active agents, antioxidants, soothing, softening, anti-irritant, tensor / smoothing, emollient, slimming, anti-cellulite, firming, shaping, draining, anti-inflammatory, depigmenting, self-tanning, exfoliating, stimulating cell renewal or stimulating cutaneous microcirculation, absorbing or filtering the UV, anti-dandruff.
Les compositions huileuses constituant les gouttes de la phase huileuse sont généralement transparentes et comprennent éventuellement un agent colorant, identique ou différent selon les compositions huileuses. The oily compositions constituting the drops of the oily phase are generally transparent and optionally comprise a coloring agent, which is identical or different depending on the oily compositions.
Selon un premier mode de réalisation, l'émulsion de type huile dans eau de la phase interne est constituée d'une dispersion d'au plus 20 gouttes de phase huileuse dans la phase aqueuse continue. According to a first embodiment, the oil-in-water emulsion of the internal phase consists of a dispersion of at most 20 drops of oily phase in the continuous aqueous phase.
De préférence, au sein d'une même capsule, les gouttes de la phase huileuse sont identiques, c'est-à-dire qu'elles sont constituées de la même composition huileuse. Preferably, within the same capsule, the drops of the oily phase are identical, that is to say that they consist of the same oily composition.
Selon une variante, au sein d'une même capsule, se trouvent des gouttes différentes, que ce soit en taille ou en composition, par exemple suivant la nature des agents parfumants, des principes actifs ou des agents colorants présents dans les différentes compositions huileuses. Selon un autre mode de réalisation, l'émulsion de la phase interne est constituée d'une seule goutte de phase huileuse dispersée dans la phase aqueuse continue. According to one variant, within the same capsule, there are different drops, whether in size or in composition, for example depending on the nature of the perfuming agents, active ingredients or coloring agents present in the various oily compositions. According to another embodiment, the emulsion of the internal phase consists of a single drop of oily phase dispersed in the continuous aqueous phase.
Quel que soit le mode de réalisation, la phase huileuse dispersée est maintenue hors de contact de la phase externe gélifiée par la phase aqueuse continue. Whatever the embodiment, the dispersed oily phase is kept out of contact with the gelled external phase by the continuous aqueous phase.
La phase huileuse est dispersée sous forme d'au moins une goutte ou de gouttes distinctes, de taille macroscopique visible à l'œil nu. The oily phase is dispersed in the form of at least one drop or distinct drops, of macroscopic size visible to the naked eye.
De préférence, la ou les gouttes constituant la phase huileuse dispersée des capsules selon l'invention possèdent un diamètre compris entre 0,025 et 4 mm, de préférence entre 0,2 et 2 mm. De préférence, le volume total de la phase huileuse dispersée des capsules représente moins de 60%, de préférence entre 2,5 et 30%, et avantageusement entre 10 et 20% du volume global de ladite capsule. Preferably, the drop or drops constituting the dispersed oily phase of the capsules according to the invention have a diameter of between 0.025 and 4 mm, preferably between 0.2 and 2 mm. Preferably, the total volume of the dispersed oily phase of the capsules represents less than 60%, preferably between 2.5 and 30%, and advantageously between 10 and 20% of the overall volume of said capsule.
L'invention concerne également l'utilisation de capsules parfumantes telles que décrites précédemment pour la préparation d'une composition cosmétique parfumante. The invention also relates to the use of perfume capsules as described above for the preparation of a perfuming cosmetic composition.
Les capsules selon l'invention stockent de manière étanche le ou les agents parfumant contenus dans la phase huileuse dispersée. The capsules according to the invention store in a sealed manner the perfume agent (s) contained in the dispersed oily phase.
L'invention concerne également une composition cosmétique parfumante, sans alcool, comprenant des capsules selon l'invention, identiques ou différentes, et un véhicule cosmétiquement acceptable. Le véhicule cosmétiquement acceptable est généralement à base d'une phase majoritairement aqueuse ou au contraire d'une phase majoritairement huileuse. The invention also relates to a perfume cosmetic composition, without alcohol, comprising capsules according to the invention, identical or different, and a cosmetically acceptable vehicle. The cosmetically acceptable vehicle is generally based on a predominantly aqueous phase or on the contrary a predominantly oily phase.
Le véhicule cosmétiquement acceptable contient éventuellement des principes actifs hydrophiles ou lipophiles. The cosmetically acceptable vehicle optionally contains hydrophilic or lipophilic active ingredients.
De préférence, le volume global des capsules parfumantes représente plus de 5% et moins de 80% du volume global de la composition cosmétique parfumante, avantageusement plus de 33%. Preferably, the overall volume of the perfume capsules represents more than 5% and less than 80% of the overall volume of the perfuming cosmetic composition, advantageously more than 33%.
Lors de l'utilisation des compositions cosmétiques parfumantes selon l'invention, typiquement par application sur la peau, l'agent parfumant est relargué lors de la rupture de la phase externe gélifiée des capsules. When using the cosmetic perfume compositions according to the invention, typically by application to the skin, the perfuming agent is released during the rupture of the gelled outer phase of the capsules.
Les compositions parfumantes selon l'invention sont typiquement appliquées selon une méthode de rupture de type mécanique. The perfume compositions according to the invention are typically applied according to a mechanical type of breaking method.
La composition cosmétique parfumante est appliquée par compression et cisaillement direct sur la peau d'au moins une capsule parfumante, ou à l'aide d'un flacon pompe qui rompt au moins une capsule parfumante et mixe les différentes phases, ou à l'aide d'un flacon spray qui rompt au moins une capsule, mixe les différentes phases et vaporise le mélange sous forme de gouttelettes. The perfuming cosmetic composition is applied by compression and direct shearing on the skin of at least one perfume capsule, or by means of a pump bottle which breaks at least one perfume capsule and mixes the different phases, or using a spray bottle that breaks at least one capsule, mixes the different phases and vaporizes the mixture in the form of droplets.
L'invention sera mieux comprise à la lecture qui va suivre, donnée uniquement à titre d'exemple, et faite en se référant au dessin annexé, sur lequel la Figure 1 est une vue à grande échelle, en coupe suivant un plan vertical médian d'une capsule parfumante selon l'invention. The invention will be better understood on reading which will be given solely by way of example and with reference to the appended drawing, in which FIG. large-scale view, in section along a median vertical plane of a perfume capsule according to the invention.
Une capsule parfumante 10 selon l'invention comprend une phase interne 15, constituée de gouttes 20 formant une phase huileuse 25 dispersée dans une phase aqueuse continue 30, et une phase externe gélifiée 40 encapsulant la totalité de la surface extérieure de la phase interne 15 pour retenir la phase interne 15. A perfume capsule 10 according to the invention comprises an internal phase 15 consisting of drops 20 forming an oily phase 25 dispersed in a continuous aqueous phase 30, and a gelled external phase 40 encapsulating the entire external surface of the internal phase 15 to retain the internal phase 15.
Une capsule alimentaire 10 selon l'invention est de forme sphérique et présente avantageusement un diamètre extérieur inférieur à 6 mm et compris de 2 mm à 5 mm. A food capsule 10 according to the invention is spherical in shape and advantageously has an outside diameter of less than 6 mm and of 2 mm to 5 mm.
EXEMPLE EXAMPLE
Dispositif expérimental Experimental apparatus
Le procédé de fabrication de capsules est basé sur la co-extrusion concentrique de solutions pour former des gouttes multi-composante. The capsule manufacturing process is based on the concentric coextrusion of solutions to form multi-component drops.
Une composition huileuse est injectée dans un courant d'une première composition aqueuse circulant dans un premier compartiment d'une double enveloppe. L'ensemble des gouttes de la composition huileuse dispersées dans la première composition aqueuse continue constitue le premier flux. An oily composition is injected into a stream of a first aqueous composition circulating in a first compartment of a double jacket. The set of drops of the oily composition dispersed in the first continuous aqueous composition constitutes the first flow.
Une deuxième composition aqueuse circulant dans le second compartiment de la double enveloppe constitue le deuxième flux. A second aqueous composition circulating in the second compartment of the jacket constitutes the second flow.
A la sortie de la double enveloppe, se forme alors une goutte multi-composante, le premier flux constituant la phase interne et le deuxième flux constituant la phase externe liquide de la goutte multi-composante. At the exit of the double envelope, a multi-component drop is formed, the first stream constituting the internal phase and the second stream constituting the liquid external phase of the multi-component drop.
Chaque goutte multi-composante se détache de la double enveloppe et chute dans un volume d'air, avant d'être immergée dans une solution gélifiante de lactate de calcium. Each multi-component drop is detached from the jacket and falls into a volume of air, before being immersed in a gelling solution of calcium lactate.
Les capsules formées sont rincées dans une solution de rinçage à base d'eau et sont stockées dans de l'eau. The formed capsules are rinsed in a water-based rinse solution and stored in water.
La taille de la phase interne, le nombre de gouttes de la phase huileuse dispersée et l'épaisseur de la phase externe des capsules formées sont contrôlées par l'utilisation de plusieurs pousse-seringues indépendants, réglant les débits d'injection des différentes compositions huileuse et aqueuses. Méthodologie The size of the internal phase, the number of drops of the oily phase dispersed and the thickness of the external phase of the capsules formed are controlled by the use of several independent syringe pumps, regulating the injection rates of the various oily compositions. and aqueous. Methodology
La composition huileuse, constituant la phase huileuse dispersée de la phase interne des capsules, est un agent parfumant tel que décrit dans la description. The oily composition constituting the dispersed oily phase of the inner phase of the capsules is a perfuming agent as described in the description.
La première composition aqueuse, constituant la phase aqueuse continue de la phase interne des capsules, est une solution aqueuse de hyaluronate de sodium à 1 ,0% en masse. The first aqueous composition constituting the continuous aqueous phase of the inner phase of the capsules is an aqueous solution of sodium hyaluronate at 1.0% by weight.
La deuxième composition aqueuse, constituant la phase aqueuse externe gélifiée des capsules, est une solution aqueuse possédant un pourcentage massique d'alginate de sodium de 2,0% et un pourcentage massique de dodécylsulfate de sodium (SDS) de 0,1 %. The second aqueous composition constituting the gelled outer aqueous phase of the capsules, is an aqueous solution having a weight percentage of sodium alginate of 2.0% and a weight percentage of sodium dodecyl sulphate (SDS) of 0.1%.
Le débit de la composition huileuse est réglé à 2 mL/h. The flow rate of the oily composition is set at 2 ml / h.
Le débit de la première composition aqueuse est réglé à 16,75 mL/h. Le débit de la première composition aqueuse est réglé à 2 mL/h. The flow rate of the first aqueous composition is set at 16.75 ml / h. The flow rate of the first aqueous composition is set at 2 mL / h.
Résultats Results
On obtient des capsules parfumantes dont le pourcentage massique de chaqu constituant est donné par rapport à la masse totale d'une capsule. Fragrance capsules are obtained, the mass percentage of each component being given relative to the total mass of a capsule.
%massique wt%
Agent parfumant 9,64% Fragrance agent 9.64%
Eau (phase interne) 79,92% Water (internal phase) 79.92%
Hyaluronate de sodium 0,81 % Sodium hyaluronate 0.81%
Eau (phase externe) 9,43% Water (external phase) 9.43%
Alginate de sodium 0,19% Sodium alginate 0.19%
SDS (avant l'étape de SDS (before the step of
0,01 % 0.01%
rinçage) rinsing)
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1061403 | 2010-12-31 | ||
| FR1061403A FR2969920B1 (en) | 2010-12-31 | 2010-12-31 | PERFUMING CAPSULE WITHOUT ALCOHOL |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2012089819A1 true WO2012089819A1 (en) | 2012-07-05 |
Family
ID=44541506
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP2011/074253 Ceased WO2012089819A1 (en) | 2010-12-31 | 2011-12-29 | Alcohol-free fragrancing capsule |
Country Status (2)
| Country | Link |
|---|---|
| FR (1) | FR2969920B1 (en) |
| WO (1) | WO2012089819A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013132082A1 (en) * | 2012-03-08 | 2013-09-12 | Capsum | Kit containing two separate compositions, in particular for cosmetic application |
| FR2996768A1 (en) * | 2012-10-15 | 2014-04-18 | Laboheme | Preparing cosmetic ball that is applied to e.g. skin of human body, comprises preparing basic solution using first polymer, mixing cosmetic active agent with basic solution, and performing spherification process |
| FR3029785A1 (en) * | 2014-12-16 | 2016-06-17 | Capsum | STABLE DISPERSIONS INCLUDING PERFUMING AGENT DROPS |
| WO2019077052A1 (en) | 2017-10-19 | 2019-04-25 | Firmenich Sa | Hydrogel beads |
| FR3112476A1 (en) | 2020-07-20 | 2022-01-21 | V. Mane Fils | CAPSULES COMPRISING A PERFUME COMPOSITION FOR SINGLE-DOSE FRAGRANCE |
| RU2846923C1 (en) * | 2020-07-20 | 2025-09-19 | В. Ман Фис | Capsules containing perfume composition for single aromatization |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013132082A1 (en) * | 2012-03-08 | 2013-09-12 | Capsum | Kit containing two separate compositions, in particular for cosmetic application |
| FR2987741A1 (en) * | 2012-03-08 | 2013-09-13 | Capsum | KIT COMPRISING TWO SEPARATE COMPOSITIONS, IN PARTICULAR FOR A COSMETIC APPLICATION |
| FR2996768A1 (en) * | 2012-10-15 | 2014-04-18 | Laboheme | Preparing cosmetic ball that is applied to e.g. skin of human body, comprises preparing basic solution using first polymer, mixing cosmetic active agent with basic solution, and performing spherification process |
| FR2996752A1 (en) * | 2012-10-15 | 2014-04-18 | Valerie Deniau | USE OF COSMETIC BALLS, PACKAGING AND ASSOCIATED COSMETIC BALLS. |
| FR3029785A1 (en) * | 2014-12-16 | 2016-06-17 | Capsum | STABLE DISPERSIONS INCLUDING PERFUMING AGENT DROPS |
| WO2016096995A1 (en) * | 2014-12-16 | 2016-06-23 | Capsum | Stable dispersions containing drops of perfuming agent |
| CN107106466A (en) * | 2014-12-16 | 2017-08-29 | 卡普苏姆公司 | Include the stabilising dispersions of aromatic drop |
| WO2019077052A1 (en) | 2017-10-19 | 2019-04-25 | Firmenich Sa | Hydrogel beads |
| US11331639B2 (en) | 2017-10-19 | 2022-05-17 | Firmenich Sa | Hydrogel beads |
| FR3112476A1 (en) | 2020-07-20 | 2022-01-21 | V. Mane Fils | CAPSULES COMPRISING A PERFUME COMPOSITION FOR SINGLE-DOSE FRAGRANCE |
| WO2022018372A1 (en) | 2020-07-20 | 2022-01-27 | V. Mane Fils | Capsules comprising a perfume composition for single-dose fragrancing |
| RU2846923C1 (en) * | 2020-07-20 | 2025-09-19 | В. Ман Фис | Capsules containing perfume composition for single aromatization |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2969920B1 (en) | 2013-05-10 |
| FR2969920A1 (en) | 2012-07-06 |
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