EP4181865A1 - Capsules comprising a perfume composition for single-dose fragrancing - Google Patents
Capsules comprising a perfume composition for single-dose fragrancingInfo
- Publication number
- EP4181865A1 EP4181865A1 EP21755529.1A EP21755529A EP4181865A1 EP 4181865 A1 EP4181865 A1 EP 4181865A1 EP 21755529 A EP21755529 A EP 21755529A EP 4181865 A1 EP4181865 A1 EP 4181865A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- capsule
- perfume
- weight
- solvent
- shell
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
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- 231100000027 toxicology Toxicity 0.000 description 1
- 229960002622 triacetin Drugs 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Classifications
-
- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
-
- 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
-
- 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
-
- 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
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q13/00—Formulations or additives for perfume preparations
Definitions
- the present invention relates to a dry and breakable capsule comprising a liquid heart of perfume, said capsule being intended for perfuming, that is to say for the diffusion of odorous molecules. Said capsule, after breaking, allows the user to perfume themselves in a nomadic and unconventional way or to apply odorous molecules without a greasy feeling when using it.
- encapsulation consists of enclosing a liquid substance in a capsule. Encapsulation makes it possible, on the one hand, to protect the substance contained in the capsule against interactions with the external environment and, on the other hand, to transport the substance of interest to the place where it will be released, at the desired time.
- patent application FR3042690 describes a device for encapsulating perfume samples, as well as a method of manufacturing such devices.
- Said device for encapsulating perfume samples comprises an outer casing made of flexible and leaktight material, comprising a cavity in which is housed a “capsule”, typically composed of a tubular body closed by leaktight means.
- the tubular body is thus made of glass, closed by a tight stopper, and contains a perfume sample.
- the tubular body of the capsule can alternatively be composed of PMMA (for polymethyl methacrylate), closed by an ABS film (for Acrylonitrile Butadiene Styrene).
- Patent application WO2012/089819 describes a perfume capsule comprising:
- a gelled external phase comprising at least one polyelectrolyte in the gelled state, completely encapsulating said internal phase at its periphery.
- the external phase also comprises surfactants which make it possible to improve the formation and the gelation of the multiple drops during the encapsulation process.
- surfactants which make it possible to improve the formation and the gelation of the multiple drops during the encapsulation process.
- the capsules according to this patent application WO2012/089819 are in fact capsules encapsulating oil-in-water emulsion droplets.
- the presence of surfactants can be irritating to the skin when applying said capsules.
- the capsules obtained according to this document are intended to be integrated into a cosmetic composition in the presence of a dermatologically acceptable vehicle, and are therefore not intended to be used as such by a user.
- the devices such as those described above relate to capsules or microcapsules, either integrated into a bottle because they must be kept in a humid environment, or integrated into a cosmetic composition, or do not allow you to actually perfume yourself. because they are integrated into a cardboard or pouch type support to smell and evaluate the perfumes before buying a spray form.
- the present invention relates to a dry, seamless, breakable capsule comprising a shell enclosing a liquid perfume core, said capsule being intended to diffuse odorous molecules making it possible to perfume oneself on the skin in particular.
- the first object of the present invention relates to a seamless capsule of the heart-shell type for perfuming a user
- the shell is comprised of at least one hydrocolloid
- the core comprises at least one perfuming agent and at least one lipophilic solvent; characterized in that said shell is breakable, and in that the heart comprises from 15 to 40% of perfuming agents by weight relative to the total weight of the heart and from 60 to 85% by weight relative to the total weight of the heart a non-glyceride lipophilic solvent, said solvent being miscible with ethanol and having:
- the second object of the present application relates to a method of manufacturing a breakable capsule comprising a shell and a core, comprising the steps of:
- the third object of the present application relates to the use of a capsule according to the invention to perfume a user.
- the fourth object of the present application relates to a method for perfuming a user using the capsule according to the invention, characterized in that it comprises the following steps:
- FIG. 1 describes the rheological profile at 25°C of pure oils compared to that of ethanol.
- FIG. 2 describes the rheological profile at 25° C. of the 15/85 weight/weight perfume+oil mixtures compared to that with ethanol.
- FIG. 3 [0021] [Fig. 3] describes the comparison of viscosities at 25°C for a stress of 10 s- 1 .
- FIG. 4 describes the evolution of the spreading value as a function of viscosity (measured at 25°C) for all families of lipophilic solvents (a) esters, (b) silicones, (c) mineral oils and (d) vegetal oils.
- FIG. 5 describes the evaporation profile of standard 15% alcoholic perfumes in ethanol.
- Fig. 6 describes the evaporation profile of standard 15% alcoholic perfumes in ethanol.
- FIG. 6 describes the evaporation profile of pure oils and pure perfumes.
- FIG. 8 describes the evaporation profile of perfume A at 15% and 40% in different oils, compared to that with ethanol.
- FIG. 9 describes the evaporation profile of perfume A at 15% or 40% in different oils, compared to that with ethanol with a zoom on the small values.
- FIG. 10 describes the evaporation profile of perfume A at 15% in different oils, compared to that with ethanol.
- Fig. 11 [0029] [Fig. 11] describes the evaporation profile of perfume A at 15% in different oils, compared to that with ethanol with a zoom on the small values.
- FIG. 12 describes the evaporation profile of perfume B at 15% in different oils, compared to that with ethanol.
- FIG. 13 describes the evaporation profile of perfume B at 15% in different oils, compared to that with ethanol with a zoom on small values.
- FIG. 14 describes the evaporation profile of perfume C at 15% in different oils, compared to that with ethanol.
- FIG. 15 describes the evaporation profile of perfume C at 15% in different oils, compared to that with ethanol with a zoom on small values.
- FIG. 16 describes the evaporation profile of perfume D at 15% in different oils, compared to that with ethanol.
- FIG. 17 describes the evaporation profile of perfume D at 15% in different oils, compared to that with ethanol with a zoom on small values.
- the capsule is seamless, of the heart-shell type and intended to be perfumed:
- the shell comprises at least one hydrocolloid
- the core comprises at least one perfuming agent and at least one lipophilic solvent; characterized in that said shell is breakable, and in that the heart comprises from 15 to 40% of perfuming agents by weight relative to the total weight of the heart and from 60 to 85% by weight relative to the total weight of the core of a lipophilic non-glyceride solvent, said solvent being miscible with ethanol and having:
- the present invention has the advantage of having a means of perfuming oneself in a nomadic, new and unconventional way.
- the user can, for example, at any time extract from a pillbox comprising a set of capsules according to the present invention, a capsule and break it between his fingers. After breaking, the lipophilic core comprising the perfume composition is released and can be advantageously applied to the skin.
- the residual shell can be reincorporated into the pillbox or thrown directly into the trash.
- the capsule can be made entirely of food materials, natural or biosourced polymers, it has the advantage of being completely biodegradable or compostable.
- An important technical advantage of the present invention is that it allows the encapsulation of a perfume composition using a judiciously chosen lipophilic (that is to say oily) solvent which makes it possible to on the one hand, to obtain breakable and stable core-shell capsules and, on the other hand, very good evaporation of the perfume and very good persistence.
- a judiciously chosen lipophilic that is to say oily
- TCM greasy stains
- the non-glyceride lipophilic solvents as defined according to the present invention have the following advantages: good evaporation of the perfume composition, the absence of persistence of sensation or of a greasy film during application to the skin, and obtaining a stable core-shell capsule.
- the solvents according to the invention must imperatively be miscible with ethanol as well as with the perfume raw materials, and must not present any smell which would interfere with the smell of the perfume composition.
- miscible is meant that the solvent according to the invention can be mixed with perfume materials and with ethanol, forming a homogeneous mixture.
- the solvent according to the invention must be miscible with ethanol for interface facilitation issues during the co-extrusion process allowing the formation of the capsule. It may be necessary to use 0 to 10% ethanol to obtain a capsule, ethanol which will evaporate during the drying of the capsules.
- lipophilic and ethanol-miscible solvents as defined according to the present invention which make it possible to solve the technical problems raised are on the one hand non-glyceridic and, on the other hand, have:
- a solvent meeting the above parameters advantageously makes it possible to implement the capsule according to the present invention.
- the viscosity and spreading values as defined above allow optimum spreading of the lipophilic perfume composition on the skin, with virtually no appearance of a film or greasy feeling, while ensuring good evaporation of the perfume.
- the range of density values allows the co-extrusion process to be carried out optimally.
- the core of the capsule comprises a main quantity of a lipophilic non-glyceride solvent.
- a solvent of the glyceride type leads to the formation of a persistent greasy film on the skin which can be unpleasant for the user, which is not desired.
- said core contains less than 5% by weight of a glyceride solvent. Even more preferably, the core is essentially devoid of glyceride solvent.
- the non-glyceride lipophilic solvent represents between 70 and 80% by weight relative to the weight of the core of the capsule.
- the non-glyceride solvents according to the invention are chosen from esters, silicones, vegetable and mineral oils.
- vegetable oils will be used in order to obtain the most biosourced capsule possible and therefore preferentially biodegradable.
- the lipophilic solvent is chosen from isoadipate, cococaprylate, isopropyl myristate and dimethicone 1cSt.
- the density of the non-glyceride lipophilic solvent is between 0.82 and 0.89.
- the density at 20°C corresponds to the ratio of the density of said composition or solvent at 20°C to the density of water at 4°C.
- the density of the total composition of the core (that is to say of the ethanol, of the perfuming agent(s) and of the lipophilic solvent(s)) is between 0.82 and 0.99.
- the non-glyceride solvent according to the invention must have a spreading value greater than 850 mm 2 /10 min.
- the spreading value of a substance is defined as the capacity of said substance to cover a surface in 10 min. This parameter makes it possible to characterize a perfume/lipophilic solvent composition so that it is the least greasy possible and that it leaves the least trace of greasy on the skin after application.
- the spreading value of a lipophilic solvent can be calculated using equations given in the literature such as in the publication by M. Douguet et al. .
- esters (MIP, isoadipate and cococaprylate in our study):
- the total quantity of the mixture of perfuming agents is between 15 and 40% by weight relative to the total weight of the core of the capsule.
- the perfuming agents which can be encapsulated in the capsule according to the present invention can be natural products such as extracts, "jungle essence” extracts, essential oils, absolutes, resinoids, resins, concretes, etc. , but also synthetic products also called captives such as hydrocarbons, alcohols, aldehydes, ketones, ethers, acids, esters, acetals, nitriles etc., in particular saturated or unsaturated, aliphatic, heterocyclic or carbon cyclic compounds.
- Such odorous substances are mentioned, for example, in S. Arctander, “Perfume and Flavor Chemicals” (Montclair, N.J., 1969), or even in “Common Fragrance and Flavor Materials”, Wiley-VCH, Weinheim, 2006.
- the core of the capsule can advantageously comprise fixing agents.
- fixing agent is meant an ingredient which may or may not be perfumed, which makes it possible to prolong the retention of a perfume on the skin.
- a fixer is a compound that can equalize the vapor pressures (hence the volatilities) of raw materials in a perfume oil, to increase its tenacity.
- the fixing agents which can be encapsulated with the perfuming agents and the solvent according to the present invention can be chosen from the following non-exhaustive list: absolutes, concretes, resins and oleoresins, waxes, derivatives of glucose, of sucrose, sorbitol, citric acid and salicylic acid, celluloses (in particular ethylcellulose), seaweed extracts, triglycerides, oils such as castor oil and its derivatives, emollients such as certain esters such as ethylhexylglycerin, polymers and their mixtures, polyurethanes, polyamides, certain silicones, liquid paraffin, glycol, fumed silica and quaternary ammonium salts.
- capsule designates a membrane encapsulation system of a composition, said capsule having a core-shell structure, the encapsulated composition making up the "core” which is enclosed in a shell (or envelope) consisting of a coating material.
- the capsule according to the invention differs from a matrix system where the composition is dispersed in a continuous matrix of a material and which is generally designated by the term “microsphere”.
- the capsule is seamless makes it possible to avoid the presence of a breaking point located at the level of the sealing of the two half-shells forming the capsule, as is the case with so-called “softgel” capsules.
- the seamless capsule has the advantage of avoiding leaks linked to a rupture of the weld.
- breakable capsule refers to a capsule as defined above, in which the shell can be broken by means of pressure applied to the outer surface of the capsule when the latter is caught between the fingers or pressed against the skin to release the heart contained in the shell.
- the capsule according to the invention preferably has a hardness of between 0.5 and 2.5 kg.
- the breaking capacity (or hardness) is measured by the crushing force to be exerted to break the capsule and by the deformation (and therefore the elasticity) of the capsule when the pressure is applied. More preferably, the capsule has a hardness of between 0.8 and 2 kg.
- the hardness of the capsules is measured by a TAXT+ texturometer on 20 capsules with a PO piston, 5 at a speed of 0.50 mm/s; the hardness is expressed in kg and the elasticity in percentage (%) of strain at break.
- the core of the breakable capsule according to the invention represents by weight 50 to 95% of said capsule, preferably 80 to 92%, more preferably 85 to 92%.
- the thickness of the capsule shell is 10 to 500 microns, preferably 30 to 150 microns, more preferably 50 to 80 microns; the outer diameter of the capsule is between 2 and 10 mm, preferably 3 to 5 mm, more preferably 3.4 to 4.8 mm, and even more preferably 3.5 to 4.5 mm; the capsule diameter/shell thickness ratio is in the range of 10 to 100, preferably 50 to 70.
- the envelope of the capsule according to the invention advantageously comprises at least one hydrocolloid.
- the hydrocolloid according to the present invention is a biobased polymer.
- biobased polymer is meant a synthetic polymer partially (generally > 20%) or totally obtained from derivatives derived from biomass.
- the bio-based nature of a polymer can be determined in particular from its C14 content, according to the ASTM D6866 standard.
- the hydrocolloid constituting the envelope of the capsule is chosen from gellan gum, gelatin (of animal origin or of biotechnological origin), collagen, alginates, carrageenans, agar-agar, chitosan and its derivatives, pectins, gum arabic, ghatti gum, pullulan gum, mannan gum, starches and starch derivatives, vegetable proteins or modified cellulose, used alone or as a mixture.
- the quantity of said hydrocolloid(s) present in the envelope is from 1.5 to 95% by weight, preferably from 4% to 75% by weight, and even more preferably from 20% to 50% by weight relative to the dry weight total envelope.
- the selected hydrocolloid is gellan gum used alone or in combination with gelatin.
- the hydrocolloid is selected from carrageenans.
- the dry weight of the envelope is between 8-50%, preferably 8-20%, more preferably 8-15% by weight relative to the total dry weight of the capsule.
- the capsule in another embodiment, includes a moisture barrier coating.
- the capsule shell is coated with at least one moisture barrier layer comprising at least one moisture barrier agent dispersed in an organic solvent or in an aqueous solution or suspension.
- the shell may consist of any hydrocolloid used alone or in a mixture, with or without gelatin. The gelatin can also constitute the only gelling agent of the shell.
- the shell also comprises an amount of gellan gum, or agar, or carrageenans or alginates, or gum arabic, or pectins, or pullulan gum or gum mannan sufficient to provide some resistance to humidity; in this case, the shell may comprise from 1.5 to 95% by weight, preferably 4% to 75% by weight, and even more preferably from 20% to 50% by weight relative to the total dry weight of the shell of at least one hydrocolloid selected from the group consisting of gellan gum, agar, carrageenans and pullulan gum.
- the envelope of the coated capsule comprises gellan gum, or arabic gum, or pectins, or agar, or alginates, or carrageenans or gum ghatti, or pullulan gum or mannan gum or a mixture thereof, but does not include gelatin.
- the capsule shell can be covered with at least one moisture barrier agent which is at least one hydrophobic agent chosen from those suitable for pharmaceutical or cosmetic products, preferably chosen from the group consisting of waxes, including carnauba wax, candelilla wax or beeswax, poultry wax, shellac (in alcoholic or aqueous solution), ethyl cellulose, hydroxypropyl methylcellulose, hydroxypropyl cellulose, latex composition, polyvinyl alcohol or a combination of these. More preferably, the at least one barrier agent to moisture is ethyl cellulose or a mixture of ethyl cellulose and shellac.
- the at least one barrier agent to moisture is ethyl cellulose or a mixture of ethyl cellulose and shellac.
- the hydrophobic moisture barrier agent can be a combination of hydroxypropyl methylcellulose, plasticizer, cellulose and microcrystalline color.
- the moisture-barrier hydrophobic agent is a film-forming gelling agent, preferably gellan gum itself.
- the casing may also comprise at least one plasticizer, which may be glycerol, sorbitol, maltitol, triacetin or polyethylene glycol, or another polyalcohol with plasticizing properties, and optionally an acid of the monoacid type. , diacid or triacid, in particular citric acid, fumaric acid, malic acid and the like.
- the amount of plasticizer ranges from 1% to 30% by weight, preferably from 2% to 15% by weight, and even more preferably from 3 to 10% by weight of the total dry weight of the envelope.
- the envelope can advantageously comprise a colorant which can make the capsule comprising the perfumed composition more attractive.
- the coloring agent is preferably chosen from dyes and pigments of food or cosmetic origin.
- the coloring can be in the mass of the casing or applied by an additional coating process.
- Bulking agents can also be included in the composition of the envelope; bulking agent means any suitable material that can increase the percentage of dry matter in the external liquid phase and therefore after co-extrusion in the capsule shell obtained.
- the increase in the quantity of dry matter in the shell of the capsule has the result of solidifying said shell and making it physically more resistant.
- the bulking agent is chosen from the group comprising starch derivatives such as dextrin, maltodextrin, cyclodextrin (alpha, beta or gamma), or cellulose derivatives such as hydroxypropyl methylcellulose (HPMC), hydroxypropylcellulose (HPC), methylcellulose (MC), carboxymethylcellulose (CMC), polyvinyl alcohol, polyols or mixtures thereof.
- Dextrin is the preferred bulking agent.
- the amount of bulking agent in the envelope is at most 98.5%, preferably 25 to 95% more preferably 40 to 80% and even more preferably from 50 to 60% by weight on the total dry weight of the envelope.
- the capsule according to the invention when it is broken and the perfumed composition applied to the skin, does not leave a greasy feeling on the skin.
- the second object of the present invention relates to a method of manufacturing a breakable capsule comprising a shell and a core, to perfume a user, comprising the steps of:
- the external liquid phase comprising from 4 to 95% by weight relative to the dry weight of said external phase of a hydrocolloid
- the internal liquid phase comprising from 15 to 40% by weight of perfuming agents relative to the total weight of the heart, from 0 to 10% by weight of ethanol relative to the total weight of the heart and from 60 to 85% by weight relative to the total weight of the core of a non-glyceride lipophilic solvent, said solvent being miscible with ethanol and having:
- the co-extrusion process is a synchronous extrusion of two liquids: the external and hydrophilic liquid phase, and the internal and lipophilic liquid phase.
- the co-extrusion process consists of three main steps: the formation of drops, the solidification of the shell and the collection of capsules.
- the capsules of the invention can be produced by any co- suitable extrusion.
- the capsules are produced by an apparatus and process as described in EP 513603.
- the solidification step is carried out by keeping the capsules cold in order to ensure good gelation of the shell, for example by placing them in contact with a cold bath.
- the cold bath is preferably cold oil.
- cold within the meaning of the present invention, is meant a temperature between 1 and 20°C, preferably 2 and 10°C, more preferably between 4 and 6°C.
- the capsules can then be centrifuged to remove excess oil, optionally washed with an organic solvent - also to remove excess oil - and dried.
- the capsules are centrifuged.
- the capsules are co-extruded, centrifuged and possibly immersed in a solution or an emulsion containing an agent making it possible to harden the shell of the capsules, or a hardening agent.
- the hardening agent can also be ethanol or any other anhydrous organic solvent, maintained at a temperature between 0 and 25°C, more particularly between 10 and 20°C.
- the hardening agent can also be a calcium ion bath, for example calcium chloride, dicalcium phosphate or calcium sulphate or an acid bath containing calcium ions with a pH of less than 5, preferably from 3 to 4.
- acids can be adipic acid, fumaric acid, gluconic acid or glucono-delta-lactone.
- the calcium ion or acid bath is preferably at a temperature of 0 to 25°C, preferably 10 to 20°C.
- the immersion step has the effect of washing the oil remaining at the periphery of the capsule, and of gradually reinforcing the envelope, in particular by dehydration and osmotic balance.
- the capsules are dried in a stream or air at controlled temperature and humidity.
- the relative humidity of the drying air is 20% to 60%, preferably 30 to 50%; the drying air temperature is 15 to 60°C, preferably 35 to 45°C.
- the surface oil can be eliminated using an adsorbent such as starch added during drying, between 0.1 and 5%, preferably between 0.1 and 2%.
- the method according to the invention further comprises a coating step during which the outer moisture barrier layer is applied to the capsules.
- said coating step is carried out by immersing the capsules in a coating solution, or by spraying a coating solution on the capsules.
- Said coating step is preferably carried out after the drying step.
- the capsules manufactured by means of the process of the invention are essentially or perfectly spherical and of very homogeneous size.
- a third object of the present application relates to the use of a capsule according to the present invention to perfume a user. Once the capsule is broken, the perfume composition does not leave a greasy feeling on the skin after application to the skin.
- a fourth and final object of the present application relates to a method for perfuming a user, characterized in that it comprises the following steps:
- - MCT medium-chain triglyceride oil of the C8-C10 type (with a molar mass equal to 387.5 g/mol);
- Isopropyl myristate Isopropyl myristate, synthetic oil (ester of myristic acid and isopropanol);
- - Cococaprylate emollient of natural origin
- - Isoadipate diester of isopropyl alcohol and adipic acid produced by synthesis
- Perfume A 4 different perfumes are tested, hereinafter called Perfume A, Perfume B, Perfume C and Perfume D. These perfumes are composed for an application in fine perfumery.
- FIG. 3 presents the viscosity values at 25° C. for a stress of 10 s ⁇ 1 , with the assessments of oiliness on the skin (the perfume alone was not tested for toxicological reasons).
- TCM viscosity of TCM
- grapeseed oil 21.4 and 45.0 mPa.s respectively, compared to that of other oils or ethanol.
- the threshold of 10 mPa.s separates oils that are too greasy from those appreciated for their pleasant, even dry finish.
- MCT like grapeseed oil, is not suitable.
- the spreading data are calculated (see FIG. 4) using logarithmic regression formulas given in the literature such as in the publication by M. Douguet et al. (Spreading properties of cosmetic emollients: Use of synthetic skin surface to elucidate structural effects - Colloids and Surfaces B: Biointerfaces 154 (2017) 307-314).
- 53 emollients (among esters, silicones, vegetable and mineral oils) were characterized and the impact of three physicochemical parameters (viscosity, surface tension and density) on the spreading value was studied.
- esters [0103] for esters (MIP, isoadipate and cococaprylate in our study):
- 1 g of sample is deposited drop by drop on a paper filter in an aluminum dish.
- the analysis is carried out at 70°C.
- the first analyzes are carried out for 2 hours with the aim of determining the “plateau” region of evaporation, that is to say the time necessary to reach the maximum evaporation.
- Standard perfume/ethanol mixture The test results show that at least 85% of the evaporation of the standard perfume/ethanol mixtures (according to a mass ratio of 15/85) is obtained after 210 seconds, i.e. 3.5 minutes ( see Figure 5), 86.5%; 87.6%; 87.2% and 85.8% respectively for flavors A, B, C and D. Consequently, the following analyzes by heat treatment will be carried out thereafter only for 30 min (and not 2 hours).
- the analysis results at 210 seconds show that the TMC does not allow evaporation greater than 2% and this for any of the perfumes A, B, C or D. Grape seed oil does not allow more than 2% evaporation for C or D perfumes. On the other hand, the other oils all allow evaporation of more than 2% whatever the perfume (see figures 10 to 17).
- the oil/perfume/ethanol mixtures all have a density allowing co-extrusion, but the mixtures made with polydimethylsiloxane (dimethicone 10 cSt) are not homogeneous. This 10 cSt dimethicone is therefore not indicated as a solvent for the present invention since it is not miscible with the ethanol/perfume mixture.
- the rheological profiles at 25° C. (at a stress of 10 s ⁇ 1 ) of the oils tested show a population separation for a viscosity of 10 mPa.s.
- the MCT and grapeseed oil in the study have a viscosity above this limit.
- MCT and grapeseed oil have spread values in the “medium” range, which explains their oiliness on the skin.
- these two oils show the lowest evaporations at 70°C at 210 seconds.
- esters such as MIP, cococaprylate, isoadipate and low viscosity dimethicones such as octamethyltrisiloxane. It is these esters that are tested below in co-extrusion with different fragrances. Tests with various perfume concentrations are also carried out.
- the capsules are manufactured by a co-extrusion operation, as described in patent EP513603.
- the general procedure for preparing capsules is described below.
- the outer water phase of the gelable mixture and the inner oil phase of the core are individually pumped through an array of submerged coaxial nozzles to form a concentric composite stream which separates into discrete concentric drops under the effect of the applied vibrational energy to this one.
- the exhaust from the coaxial nozzle assembly is immersed in a carrier fluid (eg, TCM), which is at a temperature below the gel temperature of the gellable mixture.
- TCM carrier fluid
- the gellable mixture is thus cooled and forms the hydrated shell part of the capsule.
- the capsules thus formed are then collected and centrifuged to eliminate a majority of the residual TCM.
- the centrifuged capsules and a possible part of the drying agent are mixed, then dried in a turbine with air at 40°C.
- the dried capsules are collected and sieved.
- Dried breakable capsules, prepared according to embodiments of the present invention have a homogeneous and smooth appearance, and are spherical or substantially spherical (as measured by the average ratio of the width to the length of the microcapsules).
- the dried breakable capsules also have a texture profile which makes it possible to break these capsules between two fingers.
- composition of the capsule shell (mass percentages
- the composition of the lipophilic core (in mass percentages) in different lipophilic mixtures for each capsule sample is detailed in Table 6.
- the oils tested with flavor A at 20% are TCM, MIP, isoadipate and cococaprylate. Extrusion with fragrance A at higher concentration (40%) is tested with cococaprylate. Finally, the extrusion with perfume B at 20% is carried out with cococaprylate. [0126] All the capsules were able to be produced. The size (mm), hardness (kg) and elasticity (%) values of the associated capsules are also presented in Table 6.
- composition of the lipophilic mixtures introduced during the co-extrusion Composition of the lipophilic mixtures introduced during the co-extrusion
- an oil miscible with a mixture of fine perfumery perfume and ethanol having a density of between 0.82 and 0.99 makes it possible to produce perfumed capsules whose size is between 3.5 and 4, 5mm; whose hardness is between 0.5 and 2.5 kg; and whose elasticity (expressed as a percentage of strain at break) is between 30 and 50%.
- esters such as MIP, isoadipate and cococaprylate
- silicones such as octamethyltrisiloxane
- Table 7 below makes it possible to compare the volumes of perfume (plus solvent) delivered by a capsule when the latter is broken. Knowing that on average a pschitt of classic alcoholic perfume delivers between 50 and 120 pl, it is shown below that a single 5 mm capsule loaded at 90% can deliver 60 pl of perfume, which is advantageous.
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- Cosmetics (AREA)
- Fats And Perfumes (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR2007630A FR3112476B1 (en) | 2020-07-20 | 2020-07-20 | CAPSULES COMPRISING A PERFUME COMPOSITION FOR SINGLE-DOSE FRAGRANCE |
PCT/FR2021/051346 WO2022018372A1 (en) | 2020-07-20 | 2021-07-19 | Capsules comprising a perfume composition for single-dose fragrancing |
Publications (1)
Publication Number | Publication Date |
---|---|
EP4181865A1 true EP4181865A1 (en) | 2023-05-24 |
Family
ID=74125271
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP21755529.1A Pending EP4181865A1 (en) | 2020-07-20 | 2021-07-19 | Capsules comprising a perfume composition for single-dose fragrancing |
Country Status (12)
Country | Link |
---|---|
US (1) | US20240082120A1 (en) |
EP (1) | EP4181865A1 (en) |
JP (1) | JP2023542461A (en) |
KR (1) | KR20230049647A (en) |
CN (1) | CN116113395A (en) |
BR (1) | BR112023001031A2 (en) |
CA (1) | CA3185655A1 (en) |
CL (1) | CL2023000192A1 (en) |
FR (1) | FR3112476B1 (en) |
MX (1) | MX2023000915A (en) |
WO (1) | WO2022018372A1 (en) |
ZA (1) | ZA202301705B (en) |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3091254B2 (en) | 1991-05-14 | 2000-09-25 | フロイント産業株式会社 | Seamless capsule manufacturing equipment |
WO2006136196A1 (en) * | 2005-06-21 | 2006-12-28 | V. Mane Fils | Gellan seamless breakable capsule and process for manufacturing thereof |
ES2610627T3 (en) * | 2008-10-27 | 2017-04-28 | Unilever N.V. | Antiperspirant or deodorant compositions |
FR2969920B1 (en) | 2010-12-31 | 2013-05-10 | Capsum | PERFUMING CAPSULE WITHOUT ALCOHOL |
JP6256905B2 (en) * | 2013-06-07 | 2018-01-10 | 株式会社 資生堂 | Fragrance-encapsulating capsule and cosmetics containing the same |
ES2451291B1 (en) * | 2014-01-10 | 2014-09-29 | José María RODRÍGUEZ TEJERO | Breakable capsule and its use. |
FR3042690B1 (en) | 2015-10-27 | 2019-04-05 | Saabelis | DEVICE AND METHOD FOR ENCAPSULATION OF FRAGRANCE SAMPLES OR OTHER LIQUIDS |
-
2020
- 2020-07-20 FR FR2007630A patent/FR3112476B1/en active Active
-
2021
- 2021-07-19 CA CA3185655A patent/CA3185655A1/en active Pending
- 2021-07-19 JP JP2023504204A patent/JP2023542461A/en active Pending
- 2021-07-19 EP EP21755529.1A patent/EP4181865A1/en active Pending
- 2021-07-19 BR BR112023001031A patent/BR112023001031A2/en unknown
- 2021-07-19 MX MX2023000915A patent/MX2023000915A/en unknown
- 2021-07-19 CN CN202180063048.5A patent/CN116113395A/en active Pending
- 2021-07-19 KR KR1020237005886A patent/KR20230049647A/en unknown
- 2021-07-19 US US18/016,697 patent/US20240082120A1/en active Pending
- 2021-07-19 WO PCT/FR2021/051346 patent/WO2022018372A1/en unknown
-
2023
- 2023-01-19 CL CL2023000192A patent/CL2023000192A1/en unknown
- 2023-02-10 ZA ZA2023/01705A patent/ZA202301705B/en unknown
Also Published As
Publication number | Publication date |
---|---|
CN116113395A (en) | 2023-05-12 |
JP2023542461A (en) | 2023-10-10 |
ZA202301705B (en) | 2023-09-27 |
CL2023000192A1 (en) | 2023-07-28 |
KR20230049647A (en) | 2023-04-13 |
BR112023001031A2 (en) | 2023-03-28 |
FR3112476A1 (en) | 2022-01-21 |
MX2023000915A (en) | 2023-04-26 |
CA3185655A1 (en) | 2022-01-27 |
WO2022018372A1 (en) | 2022-01-27 |
FR3112476B1 (en) | 2022-07-01 |
US20240082120A1 (en) | 2024-03-14 |
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