DE4336407A1 - Waterproof cosmetics - Google Patents

Description

The invention relates to a cosmetic composition, a aqueous composition containing this composition, a ver drive to their manufacture and their use as / in Kosme tikprodukt / s or for the production of cosmetic products.

Common methods of making small, discrete, one-core containing particles of hydrophobic polymer material the process step of polymerizing the monomer so as to to form the encapsulating polymer shell.

For example, Solc nee Hajna in US-A-4,421,660 describes such as particles of inorganic solid such as TiO₂ with colloidal Size in a hydrophobic addition polymer such as polystyrene in be encapsulated in a polymerization process, wherein a water-insoluble hydrophobic monomer in an aqueous, colloid dalen dispersion of the inorganic particles is dispersed and then this mixture was subjected to emulsion polymerization becomes. Another polymerization process is described by Bayley in the US-A-4,264,700. According to this patent, magneti toner particles made by a vinyl monomer  Polymerization initiator, magnetic particles and a solution means for the monomer as droplets in the form of a discontinuous animal phase in a continuous, aqueous phase sus are pending. Then the monomers in the discontinuous Lichen phase polymerized after removal of the solvent to form the polymer coated toner particles.

Another method comprising a polymerization is from Nguyen et al. in US-A-4,530,961. With this become soot particles in water with a water-soluble peroxide treated and then a water-soluble acrylic monomer is added puts. In the subsequent homogeneous free radical poly merization of the monomer occurs simultaneously grafting the mono on the soot particles.

All of these processes involve suspension polymerization of a monomer essential part of the encapsulation process. Those needed to polymerize a surrounding monomer However, conditions limit the range, for example usable concentration ratios of included Part of the component forming the shell, the physika properties of the included components and the possible choice of suitable auxiliaries such as surfactants. Furthermore, the Emulsion polymerization a complex reaction and for everyone desired combination of materials and resulting Concentration is the study of suitable polymerizations conditions required.

Micale describes in US-A-4 665 107 the manufacture of a Polymer shell that is tight around solid particles (pigment) with sub micrometer size (<1 µm) around, so a low viscosity To form writing fluid. This liquid is obtained by first placing the pigment submicron particles in be dispersed an intermediate solvent, which also containing the encapsulating, water-insoluble polymer, and then the mixture is dispersed in water and the intermediate solution  becomes medium. The polymeric material is not used in the wrapping changed significantly.

Another polymer dispersion is described by Ober et al. in US-A-4,692,188 described, according to which a polymer and an oil-soluble Dye in an water-immiscible organic solvent be solved. The mixture is then mixed with a Combined solution of water and surfactant, the combination emul and then evaporates the organic solvent, so the dye and the polymer in an aqueous phase to get suspended.

With the of Micale and Ober et al. described procedures and especially the use of an intermediate solvent however, there are two major disadvantages. The first The disadvantage is the economic outlay due to the additional step of removing the solvent and then cleaning the removed solvent to the how use or disposal is required. The second night Part is that typical intermediate solvents such as Methylene chloride tend to cause environmental problems and also the removal of trace amounts of the solvent from the End product is required to end consumer health to protect.

There are also methods of making capsules therein included active ingredients known in which the Capsule size in the micrometer and submicrometer range.

Miyano et al. describe a process in US-A-3 856 699 for the production of capsules with walls made of wax-like material al, in which a waxy material that ent a core material holds in a moving aqueous medium at a temperature dropwise above the melting point of the waxy material is dispersed and then the waxy material in an unbe away aqueous medium is transferred to a temperature  points that is lower than the melting temperature of the wax like material. The size of the droplets is determined by the stirring speed controlled and is a minimum of 20 to 500 µm.

Compositions are known in the field of cosmetics a more or less thick film after application the skin that contributes to the applied active ingredient for example, before the premature and unintentional washing up protected by water.

DE 37 10 292 A1 and DE 37 10 293 A1 specifically polymeric cellulose derivatives used to make waterproof suns to manufacture protective products that have waterproof films on the skin form.

EP-A-0 356 196 describes a cosmetic preparation with a stable oil-in-water emulsion on the skin a film is formed that is a thin flexible acrylate homo polymer layer and a sunscreen.

EP-A-0 265 228 describes a skin protection agent which an acrylic copolymer of ethyl acrylate and methacrylic acid.

In addition, in DE 25 44 180 is a cosmetic cosmetic Preparation described that certain UV absorbers and ointments Contains cream bases or solvents that are used to manufacture position liquid light protection and skin care products. They are made by the ingredients at temperatures at 75 ° C, for example, stirred and homogenized become.

However, the known compositions and preparations have the Disadvantage that they are not or only to a small extent or penetrate the skin superficially, so that some of the be written water resistance is not long lasting.

The present invention is therefore based on the object to create a cosmetic composition that as or for the manufacture of cosmetic products is suitable without using polyme risk assessment process and without the use of intermediary, later organic solvents to be removed can be produced, according to Applying a permanent waterproof order of active Ingredient yields and a variety of cosmetic effects Can contain components individually or in combination. Opp there may also be a delayed submission and therefore longer lasting cosmetic effect of the enclosed substance.

This task is accomplished through a cosmetic composition solves that

• a) a solid, particulate water-insoluble matrix of min at least a water-insoluble, non-polymeric, matrix forming material that is solid at room temperature, and
• b) a water-insoluble, kos enclosed in the matrix includes active ingredient having a metic effect,

the matrix particles having an average size of about 1 µm or less.

This cosmetic composition, which is also in the form of its aq dispersion can be obtained by a process adjustable, which is characterized in that

• 1) at least one water-insoluble, non-polymeric, matrix forming material that is solid at room temperature and a Water-insoluble active to be included in the matrix Ingredient to be heated together to a temperature that is sufficient to melt the matrix-forming material,
• 2) the hot melt formed from matrix-forming material and active ingredient added to water while moving is, optionally surfactant is present to a sta bile to produce aqueous emulsion, the matrix-forming Material with the active ingredient included in the form of droplets with an average size of comprises about 1 µm or less, and  
• 3) the stable, aqueous emulsion is cooled to room temperature is made up of an aqueous dispersion of solid particles Matrix-forming material with encapsulated active Obtain component, which then, if necessary, the water is withdrawn.

The composition or dispersion according to the invention and the The inventive method for their production is a signi fictional improvement over the previously known set tongues or procedures.

Advantageously in the production according to the invention Formation of an encapsulating matrix requires no polymerization derdlich since the active ingredient is not in a monomer or a monomer mixture is dispersed or dissolved. Especially there is no need to stop certain emulsifiers conditions that also allow polymerization of a monomer ben. The matrix-forming material according to the invention is used in the Production of the composition is not chemically modified, so that get the known chemical and physical properties stay. The use of a polymeric matrix material is even eliminated overall.

Since also the use of an intermediate solvent for a Monomer to be polymerized can advantageously be eliminated Costly process steps that involve removal processing and processing of this solvent are connected, and avoid possible environmental problems and health risks.

The rheological and physical properties of the inventions cosmetic composition or dispersion according to the invention by the mass properties, morphology and the surfaces properties of the matrix-forming material are determined and are thus on the nature or nature of the active be included partially independent.  

The matrix-forming material can be any material that in Water is essentially insoluble, preferably less than 5%, preferably less than 3% and especially less than 1% is soluble in water and in terms of active stock is partially inert. It should be stable during heating preferably a melting point below about 100 ° C point and form a melt that has a viscosity, which is less than about 600 mPa · s and preferably less than is about 500 mPa · s. The matrix-forming material can be a Solid, a liquid or a mixture of solids and be liquid that is usually solid at room temperature are.

Suitable matrix-forming materials are vegetable oils, in particular their hardened palm oil, hydrogenated triglycerides of coconut and the oil palm, cotton oil, castor oil and esters thereof, animal Waxes such as tallow, beeswax, whale wax or aqueous lanolin, Fatty acids such as stearic acid, lauric acid or myristic acid, Esters or amides of fatty acids such as ethylene glycol monostearate, Propylene glycol monostearate and glycerol monostearate, sorbitan fat acid esters such as sorbitan monopalmitate, sorbitan monostearate and Sorbitan tristearate, fatty alcohols such as cetyl alcohol, ethoxylated Fatty alcohols, triglycerides such as triglycerides of vegetable oils or modified vegetable oils, petroleum or mineral waxes such as paraffin, alkylene glycols, especially at room temperature solid ethylene glycols and propylene glycols. Ins are preferred special stearic acid esters such as ethylene glycol and propylene glycol colmonostearate and sorbitan tristearate, and hydrogenated triglyce ride the coconut and oil palm (e.g. Wecobee FS from Stepan).

The active ingredient in the matrix forming material too encapsulate or dissolve in it is extremely low Solubility in water and high solubility in hydro phobic liquids or solvents. If the active ingredient is a solid submicron particle like a Pigment, it should be in the melt of the matrix-forming mate  rials can be dispersed without significant agglomeration. If the active ingredient is a solid or a liquid, it is preferred in the melt of the matrix-forming material Wise soluble and gives a homogeneous mixture in the matrix educational material. Preferably the active ingredient is one lipophilic liquid.

The vapor pressure of the active ingredient is sometimes low or the active ingredient is sometimes solid at room temperature and not soluble in the matrix-forming material of choice. Of the active ingredient may also be in the form of particles which are too big to be encapsulated successfully. In such The active ingredient can first be mixed with water immiscible liquid that is able to with the melted matrix-forming component a homogeneous one To give mixture and then lead in the dispersion may. Suitable carrier liquids include solvents such as tributyl citrate, dioctyl phthalate, pine oil, etc.

The active Be encapsulated by the matrix-forming material is part

• a) a solid particle with a size smaller than 1 µm (sub micrometer particles),
• b) a solid or a liquid that is in the Production in the melt of the matrix-forming material solved, or
• c) a solid or a liquid which is used in the manufacture position in a water-immiscible carrier liquid has been solved.

For example, all are included as active ingredients coloring components, skin care or skin protecting Suitable components and fragrances. It is irrelevant here whether the respective active ingredient as such at room temperature is solid or liquid.  

These include in particular those approved for cosmetic products colorants, especially those for lipsticks. Example fat-soluble dyes such as fatty brown B (Cas sella), various food colors (e.g. as the naturid table-synthesized food coloring agent β-carotene oil-soluble, liquid (E160a) from Riedel-arom.), if necessary on a natural basis, Pigments and pigment preparations.

Also included are essential oils such as bergamot oil, cedarwood and -leaf oil, citronella oil, eucalyptus oil, spruce needle oil, camomile lenöl, camphor oil, pine needle oil, Krausminzöl, Latschenkie Fern oil, lavender oil, lemon balm oil, clove leaf and flower oil, Orange oil, pepper oil, peppermint oil, rose oil, cinnamon oil and lemon oil.

Furthermore, caring substances such as oil-soluble vitamins, Avoca dool, jojoba oil, aloe vera extract in oily preparation, pan thenol, walnut oil, tocopherol (vitamin E), tocopherol acetate, hydrogenated peanut oil, sweet almond oil, wheat germ oil, coconut oil, Soybean oil, calendula, evening primrose oil, various plant extracts based on soybean oil, castor oil, various perfume oils and biobranil (concentrated extract from wheat bran).

Active components such as are also used as sun protection components Butylmethoxydibenzoylmethane, benzophenone-3, menthylbenzylidene camphor, octyl methoxycinnamate, octyl dimethyl PABA (or 2-ethyl hexyl 4-dimethylaminobenzoate) and isoamyl p-methoxycinnamate suitable.

The active Be encapsulated by the matrix-forming material Component is preferably a UV absorbing material essential oil, an organic dye, an organic or inorganic pigment, a lubricating oil, a perfume or a Flavor and is especially selected from pine oil, pepper ferminzöl, substituted or unsubstituted cinnamic acids or substituted or unsubstituted cinnamic acid esters, triazole  compounds, organic dyes, inorganic pigments, Perfume oils, derivatives of γ-linolenic acid, vitamins such as vitamin E and A or skin softeners.

The active ingredient is therefore preferably, for example Colorants for a variety of dyeing or coating applications or a chemical that releases in a controlled manner should be set, such as to improve breathing or to keep the skin moist. Suitable active ingredients include UV absorbing materials such as substituted or unsubstituted cinnamic acids and their esters, formamidine compounds genes, triazole compounds and those compounds that can be used as optical brighteners, as well as organic and inorganic dyes, organic and inorganic pigments such as micronized titanium dioxide, micronized zinc oxide and Iron ferrocyanide, lubricating oils such as emollients for the Skin, fragrances and substances such as perfume oils (e.g. lavender, pini oil, clove oil, peppermint oil and the like.

The active ingredient can be found in widely varying concentrations be present, but preferably the ratio of acti vem component to encapsulate matrix material in the range of about 1:25 to 25: 1, preferably 1:10 to 10: 1. If a carrier is used to dissolve the active ingredient should the active ingredient preferably in the carrier in a conc tration of about 0.5 to 95 wt .-%, preferably 1 to 90 wt .-% and more preferably 2 to 85% by weight.

The active ingredient is typically insoluble in water, but is soluble in the matrix-forming material, so that it Formation of an aqueous emulsion or dispersion does not occur in the aqueous phase passes. The matrix-forming material used influences the emulsion and dispersion behavior in water and is used to clean up the active ingredient in an environment preserve, protect and transport in which it is otherwise  due to solubility, oxidation or other factors would not be stable or would only be stable to a limited extent.

An essential feature of the present invention is hence also in the fact that the active ingredient, when in the matrix-forming material is embedded or encapsulated, in an aqueous solution can be stable and not released, before the particle in a suitable, z. B. lipophilic, Surrounding area.

Depending on the chemical nature of the active stock partly due to physical forces involved in the Applying the composition to the desired substrate, e.g. B. the skin can be applied from the matrix-forming mate rial be released. Alternatively, the effective inventory partly after removal of the surrounding water by evaporation be delivered. Furthermore, it can be made from the matrix-forming material al after a change of chemical, biological or physical environmental conditions. The release mechanisms such as diffusion through the Matrix material and / or increased solubility of either the active Component or matrix material in the target environment grasp.

Suitable substrates on which the composition according to the invention tion or the dispersion of the invention are applied can, for example, close human skin, finger and Toenails or hair substrates. The cosmetics according to the invention compositions or dispersions can as such as Cosmetic preparations are used or for the production of such preparations be used.

According to the method according to the invention, particles in the submi micrometer range (size 1 µm), which is an active Contain ingredient that in this way in a hydrophilic, d. H. Environment containing water stored, stabilized or  can be transported and then through targeted environment change can be released.

Furthermore, the particles can be formulated to have the desired surface and physical properties zei gene, which in turn depends on the chemical or physical properties independent of the included active ingredient are. The active ingredient is preferably uniform in that Distributed matrix material or from the matrix material as a shell surround.

The rheology and the ability to control the dispersion stability with respect to both flake formation and Suspendability of the submicroscopic, dispersed particles is significantly improved overall. The stability and the rheological properties of an aqueous dispersion therefore largely predictable, relying on knowledge of the physi potash and chemical properties of the matrix-forming mate rials can be used with these properties by nature or the amount of active ingredient be significantly influenced.

For example, if the active ingredient is one through the skin feeding and skin moisturizing compound that is on the skin should be applied and then over a lipophilic Transmission system is mediated are larger concentrations possible at this connection as if water-based Transmission systems are used based on the solubility limits based in water. Another important aspect is there in that the particles can be formulated more easily that they show the desired properties, such as the particle sizes, film-forming properties or adhesive properties properties and properties such as gloss and abrasion resistance.

In contrast to the prior art, the present Er acceptable physical and chemical  Properties of the active ingredient, desirable ratio nisse from active ingredient to matrix forming material and the choice of suitable matrix-forming materials che. The present invention enables these advantages without the need for an intermediate solvent and the associated removal and disposal requirements.

Furthermore, matrix-forming materials are used according to the invention that can easily be formulated to include the Release rate of an included active ingredient can control them in a targeted manner. A possible explanation for this Phä nomen is that the diffusion rate of an active ingredient through the surrounding matrix primarily through the physi interaction of the active ingredient with the matrix material rial can be checked.

The matrix and active ingredient composition particles have a size smaller than 1 µm and preferably one Average size of 500 to 5 nm, in particular 200 to 5 nm or even less.

It is preferred that in each particle of the matrix forming Ma terials at least one particle of the active ingredient present that is, or that the active ingredient in the matrix-forming Material is loosened. The ratio of active ingredient to The matrix-forming material is preferably in the range of 0.04 to 25, more preferably 0.1 to 10, which is a ratio of 1:25 to 25: 1, more preferably 1:10 to 10: 1.

The solid particles of matrix material and enclosed therein Nem active ingredient can be dispersed in an aqueous medium be greeded and accordingly form an aqueous dispersion, used as or for the manufacture of cosmetic products can be.  

The aqueous dispersion then preferably comprises 1.0 to 50% by weight, in particular 10 to 40 and preferably 20 to 30% by weight the solid, particulate cosmetic according to the invention Composition as a discontinuous phase and also against also surfactant.

Suitable surfactant material which can be used according to the invention comprises anionic, cationic, amphoteric and non-ionic surfactants or mixtures thereof.

Examples of suitable surfactants include non-ionic surfactants such as polyethylene oxides, ethoxylated alkylphenols (e.g. nonylphe nolpolyoxyethylene), ethoxylated fatty acid esters, ethoxylated Fatty alcohols (e.g. cetyl, stearyl, lauryl or tridecyl alcohol hol), ethoxylated glyceride esters, sorbitan esters (e.g. sorbitan tristearate), long-chain fatty acid esters from polyethylene glycols, Diethanolamide, coconut fatty acid monoethanolamide, alkylaryl poly ether alcohols, etc. Close usable anionic surfactants Sodium lauryl sulfate, sulfosuccinic acid derivatives (e.g. Dinatri um-N-octadecylsulfosuccinate, disodium ethoxylated alcohol half ester of sulfosuccinic acid, disodium ethoxylated No nylphenol half ester of sulfosuccinic acid, diamine ester of Sodium sulfosuccinic acid), alkylarylsulfonates (e.g. sodium isopropylnaphthalenesulfonate), sulfated higher alcohol esters (e.g. ammonium salts of sulfated nonylphenoxy poly (ethylene oxy) ethanol), ammonium lignin sulfonate, lecithin and of course occurring mixtures of diglycerides of stearin, palmitin and Oleic acids ver with the quinoline ester of phosphonic acids are bound. Useful cationic surfactants include quaternary ones Ammonium salts, cetylpyridinium chloride, polyalkylamidoimidazoli nium sulfate and ethanolized alkylguanidine amine complexes. Usable amphoteric surfactants include complex fatty amidovers bonds, modified fatty amine condensates and sulfobetaine inverters bindings. Of these surfactants are non-ionic and anio niche surfactants preferred, especially those that are out are selected from ethoxylated alkylphenols, ethoxylated alcohols  get ethoxylated fatty esters, sulfosuccinic acid esters, Sorbitan esters, alkyl and aryl sulfonates, lecithin and mono- and Diglycerides of stearic, palmitic and oleic acids. Lecithin and the naturally occurring mixtures of diglycerides from Stearic, palmitic and oleic acids are particularly useful ten side.

The following is a manufacturing process for the Invention appropriate composition or the dispersion of the invention described, which contains this composition.

The first stage of the process involves heating together at least one water-insoluble, non-polymeric, matrix bil material that is solid at room temperature and one in water-insoluble, cosmetic, active ingredient. Heating continues until one Temperature is reached, which is sufficient, the matrix-forming mate rial to melt, but is preferably lower than about 100 ° C so as to form a hot melt which has a viscosity is less than about 500 mPa · s. Preferably the temperature is in a range from about 60 to about 85 ° C and again preferred is the mixture during heating zens stirred with a mechanical stirrer.

The matrix-forming material essentially determines the density the aqueous emulsion. It can easily be concentra tion ratios within a wide range in the aq emulsion by the ratios of the active ingredient corresponding to the matrix-forming material be changed. The ratio of active is preferably Part of the matrix-forming material in the range of about 0.1 to 10.0.

The density of the final composition particles is a function of this ratio and the density of the matrixbil material.  

During heating, the active ingredient becomes hot liquefied melt of the matrix-forming material dissolved and dispersed in it. Preferably or if necessary at least one surfactant is added to the hot melt before the Melt in stage 2) is added to water. The choice of the ten sids, if used, depends essentially on the chemistry and the surface properties of the active ingredient. It however, a wide variety of surfactants can be used as long as they have the ability to be the active ingredient in the hot melt to wet or the interfacial tension between to reduce hot melt and water in stage 2) gladly.

After heating in stage 1) the hot melt is in one Amount added to water that there is a concentration in the range from preferably 1 to 50% by weight, in particular 10 to 40% by weight and more preferably 20 to 30% by weight. The surfactant, the given is also present when the hot melt is in motion is added to water (level 2), can with the hot melt be combined, previously added to the water to which the hot melt is given, or both. Preferably at least one surfactant with the hot melt in stage 1) com and then another surfactant or an additional amount of the same surfactant added to the water to which the hot Melt is added. The aqueous phase should be added of the hot melt at the same temperature level, around one Avoid "temperature shock". If a surfactant to the water is given, either before or simultaneously with the Hot melt addition can be added. Definitely is the presence of a surfactant when added in step 2) advantageous adheres to the interfacial tension between the hot melt and the water to a value of less than about 10 dynes / cm, preferably lower than 5 dynes / cm, thereby reducing the Preparation of a stable aqueous emulsion additionally facilitate is tert.  

Although the relative concentrations of all components increase Lich can vary, suitable aqueous emulsions are typi produced when the relative concentrations in the following ranges fall, with the information on 100 g of the Particle emulsion based:

• - Matrix-forming material such as propylene glycol monostearate and sorbitan tristearate in total about 0.1 to about 50 g,
• - Active ingredient such as liquid pine oil or one in one suitable solvent total dissolved solid 0.1 to about 50 g,
• Surfactant such as sorbitan tristearate from about 0 to about 25 g and
• - Water, which may contain up to about 10% additional surfactant Disodium ethoxylated alcohol half ester from sulfobernstein contains acid, at least 40 g.

The sufficient movement of the hot melt in the water The emulsification in stage 2) can be achieved through a number of commercial processes currently available devices can be achieved such as wise ultrasound devices, especially ultrasound heads, high speed stirrers, mixers or suitable homogenizers.

Preferably, the movement is caused by ultrasound to obtain an aqueous emulsion with very small droplets. (Sound output power max. 350 W with adjustable power levy, e.g. B. 20 to 40% output, sonication duration 30 Seconds to 5 minutes with a 100 g batch). The droplets size in the aqueous emulsion obtained is average smaller than 1 µm, preferably is on average 500 to 5 nm, more preferably 200 to 5 nm or even less.  

The aqueous emulsion should remain after at least two hours be stable in their manufacture. If the emulsification in stage 2) has led to a sufficiently homogeneous mixture, the aqueous emulsion a stable discontinuous phase, the one has an average size of less than 1 µm, and a continuous aqueous phase (water).

The required to produce the desired droplet size Time varies with the type of device used, the amount the hot melt and the water used and the limit surface tension between hot melt and water. Generally will mean a time of at least two minutes, preferably takes about four minutes when ultrasound is applied an average drop size of <1 µm can be achieved and 100 g should be treated. In a preferred embodiment the drops have an effective average size of about 500 nm or less, more preferably about 200 nm or less and particularly preferably about 5 µm or less on what with electron microscope, laser diffraction or based on the determined ten zeta potential can be detected.

A subsequent lowering of the system temperature to at for example room temperature leads to solidification of the emulsion drop and to form spherical solid matrix particles, the contain the active ingredient. The cooling in stage 3) he preferably follows at a cooling rate of about 0.5 to 15 ° C, in particular 1 ° C to about 10 ° C and preferably 2 to 5 ° C per minute te. Cooling is achieved, for example, by the aqueous Simply let the emulsion cool to room temperature, is actively cooled from the outside or internally by adding zu additional water is cooled, this added water has a lower temperature than the emulsion.

The particles so formed are flake and Sedimentation stable, show good dispersibility and possess as before, the droplets an average particle  diameter of less than about 1 micron, preferably they are in the size range of about 5 to 500 nm, more preferably in the range from about 5 to 200 nm and are also small in some cases ner. Furthermore, at least one particle of the active ingredient 5 preferably present as the core in each matrix particle or he is dissolved in the matrix material.

All or each of levels 1), 2) and 3) can be controlled pressure conditions, if appropriate is what is the case when a volatile active ingredient is used. Similarly, all levels or each the steps under a suitable inert gas such as nitrogen, helicopter um or argon can be carried out when the active ingredient is sensitive to oxygen.

The exact formulation determines the release rate of the akti ven component in response to changes in the environment. Ins the diffusion rate is determined by the solubility of the active ingredient in the matrix-forming material, the Ver Ratio of matrix-forming material to active ingredient, the Solubility of active ingredient in a changed environment conditions and the degradation rate of the matrix. Further is the size of the particles directly with the total surface of the part Chen, which is available for release connected. The Particle size could be a function of the amount of surfactant used, that the interfacial tension between the hot melt and the water controls, and the amount of energy which is necessary to achieve a desired degree of emulsion To get melt in the water.

The active ingredient is believed to be controlled Way into a desired environment according to one or more of the following mechanisms can be released:

• (1) If the active ingredient has a sufficiently high vapor pressure, by diffusion through the matrix material wall, as  Function of the radius of curvature of the particle and the Vapor pressure of the active ingredient,
• (2) when the active ingredient is in a carrier liquid is solved within the particle structure, by diffusion through the matrix material as a function of the vapor pressure of the Carrier liquid, when the carrier evaporates,
• (3) when a new medium moves around the particles in the target environment there, by diffusion of the active ingredient through the Matrix material as a function of its solubility in the medium such as fat or the like lipophilic substrates, or
• (4) when physical influences such as pressure, heat, radiation chemical or biological conditions in the target environment exist by breaking down or breaking up the structure of the Matrix material.

The invention is further illustrated by the following examples clear.

First is an exemplary basic recipe for an invent Cosmetic dispersion according to the invention specified on the jewei League specific application can be adapted without the To leave the scope of the invention.

Manufacturing process for the basic dispersion

The matrix material is heated until all components have melted. The active ingredient is added and the Mix homogenized by stirring. The dispersion medium is preheated to 75 ° C, at this temperature the head of an ul ultrasonic homogenizer immersed in it and the mixture Matrix material and active ingredient slowly added. Wuh After the addition is done with ultrasound (350 W, 20-40% dispensing treated). Following the homogenization, no further ultrasound treatment and, if necessary, with light Stirring cooled to room temperature.

The specific embodiments given below include such an aqueous base dispersion.

example 1 (Facial moisturizer)

The following ingredients became a cosmetic disper sion processed.

The components of Part A with the exception of triethanolamine were mixed and dispersed. Then the tri ethanolamine added. For this purpose, part B given. Part C was then added and stirring continued until there was a homogeneous dispersion.  

part B

The components listed under 2) were heated together, until they were completely melted. Then that was under 1) mentioned mineral oil, which was preheated to 75 ° C, added ben and a homogenized mixture prepared with stirring. To the pre-heated mixture of the ingredients in 3) the mixture of 1) and 2) was slowly added, using an ultrasound head. Then 5 minutes long gently stirred and cooled to 35 ° C.

Example 2 (Liquid, tinted lotion (o / w emulsion for oily skin))

The following ingredients became a cosmetic disper sion processed.

The components of Part A were heated to 70 ° C mixed together. The deionized water from Part D was which is also heated to 70 ° C and added to part A. It was cooled, with homogenization by stirring. After that the mixed ingredients of Part B are added with stirring and when a temperature of 30 to 35 ° C was reached. The Dis Persion from part C was then added with stirring, so that a homogeneous formulation emerged. In the end, fragrance and Preservatives added.

Part C.

The ingredients of part 1) were heated together until they were completely melted. The components of part 2) were ground as necessary and using a Ultrasonic homogenizer dispersed in part 1). The stock Parts of part 3) were preheated together to 80 ° C and then slowly with the homogeneous mixture of part 1) and part 2) sets, with an immersed ultrasound head the desired Dispersion caused. Then the dispersion was added gentle stirring cooled to ambient temperature.

Example 3 (Sun protection lotion; o / w emulsion)

The following ingredients became a cosmetic disper sion processed.

The components of Part B were heated to 85 ° C, with was stirred with a planetary stirrer. Then Part C was added and with continued stirring a homogeneous mixture poses. Subsequently, the mixture was also heated to 75 ° C. Pre-warmed mixture of Part D ingredients added. It was then cooled to 40 ° C and part E and optionally  Water added to compensate for any loss of water. Wuh Part A became a while cooling to ambient temperature stirred, resulting in a homogeneous dispersion.

Part A

The ingredients of part 2) were heated until they were complete had melted. With stirring and homogenization Pre-heated mixture of the components of part 1) to 75 ° C set. This homogeneous mixture was pre-heated to 80 ° C warmed part 3), using an ultrasound head was dispersed. It was then opened with gentle stirring Ambient temperature cooled.

Example 4 (Perfume oils)

The following ingredients were weighed, warmed and mixed:

1. 11.0% by weight of propylene glycol monostearate,
2. 14.6% by weight of sorbitan tristearate,
3. 20.0% by weight of perfume oil
4. 52.9% by weight of demineralized water and
5. 1.5% by weight disodium ethoxylated alcohol half ester of sulfosuccinic acid.

The above mixture was placed in a closed container and warmed and stirred carefully, warming in one Water bath took place and was continued until all solids  had melted. Here, all were in a 1-phase approach Components weighed and then heated together or the com Components 1-3 and 4 + 5 were heated separately and then ge mixes.

Then the emulsion was made by adding the hot melt Water was given, being treated with an ultrasound has been. The temperature was kept between 60 and 75 ° C After a 4 minute ultrasound treatment, droplets with an average diameter of less than 500 nm found. The aqueous emulsion then slowly opened up Cooled to room temperature, causing the droplets to become solid parts froze.

The solid particle dispersion was applied to a substrate brings. Compared to ethanolic or isopropanolic The fragrance remained essential to preparations of the same perfume oil received longer.

Example 5 (UV absorber)

Following the procedure of the previous example, the fol mixed compounds:

8.2% by weight of a mixture of mono- and diglycerides of palmitic and stearic acids,
11.0% by weight of purified, hardened palm oil,
15.0% by weight of 2-ethylhexyl p-methoxycinnamate
64.6% by weight of demineralized water and
1.2% by weight disodium ethoxylated alcohol half ester of sulfosuccinic acid.

The heating and emulsification was carried out according to the described Ver driving done. The resulting dispersion of solid Particles provided excellent UV protection, and that over a long period of time.  

Example 6 (Essential oils)

Following the procedure of the previous examples, the mixed the following compounds:

12.0% by weight of ethylene glycol monostearate,
10.0% by weight of sorbitan tristeart,
12.0% by weight of a mixture of essential oils,
64.5% by weight of demineralized water and
1.5% by weight disodium ethoxylated alcohol half ester of sulfosuccinic acid.

The heating and emulsification were described according to the above procedure. When applied to a substrate the scent of the essential oil remained much longer than a standard oil-in-water emulsion Concentration.

Example 7 (Vitamin A)

Following the procedure of the previous examples, the mixed the following compounds:

6.0% by weight hydrogenated fatty acid from rapeseed oil,
19.6% by weight of sorbitan tristearate,
5.0% by weight of vitamin A,
67.9% by weight of demineralized water,
1.5% by weight disodium ethoxylated alcohol half ester of sulfosuccinic acid.

The heating and emulsification were carried out as before, with except that an inert gas atmosphere was used to To prevent oxidation. The resulting particle dispersion contained the vitamin in a stabilized form that was widely is less sensitive to oxidation than a non-encapsulated one Shape.  

Example 8 (Long-term fragrance dispenser (liquid, effective ingredient))

15 g of a solid, hydrogenated vegetable oil (commercially available Lich from Stepan Comp. under the trade name WECOBEE SS) and 5.0 g solid stearic acid (commercially available from Eastman Kodak Comp.) Were weighed into a vessel. For this, 10.0 g Lavender essence (commercially available from Reynaud Ltd. at the trade name R 152). The container was sealed closed so that no volatile component could escape. (This can be done, for example, by using a heat-resistant seal film happen). The sealed container was then put in a 70 ° C oven until all the ingredients had melted. 60.0 g were placed in a second container ionized water and 3.0 g of surfactant, namely the ammonium salt of sulfated nonylphenoxypoly (ethyleneoxy) ethanol (com available from GAF under the trade name Alipal EP 110) weighed, the container covered and in a 70 ° C warm oven given until the container reached this temperature. Then both containers were removed from the oven and those contained in them mixtures kept homogenized. Without cooling them down an ultrasonic homogenizer was placed in the water given and slowly the liquefied mixture of lavas Deloil / vegetable oil matrix added. Formed in the water an emulsion of the lavender / vegetable oil mixture. There was one Ultrasound sonication until a microscopic review revealed that the emulsion drop size was uniform and below was half 1 µm. The emulsion was then gently stirred until the Liquid reached room temperature, causing the lavender / vegetable oil Mix solidified and became a stable dispersion revealed.

The dispersion was useful for water-based cosmetics to manufacture. It provided a pleasant smell for a long time, this period was significantly longer than the one with an unencapsulated lavender oil.

Claims (29)

1. Cosmetic composition that

• a) a solid, particulate water-insoluble matrix of at least one water-insoluble, non-polymeric, matrix-forming material which is solid at room temperature, and
• b) comprises a water-insoluble, cosmetically active ingredient encased in the matrix,

where the matrix particles have an average size of have about 1 µm or less. 2. Composition according to claim 1, characterized in that the at least one matrix-forming material is selected from vegetable oils, especially hydrogenated palm oil Triglycerides of coconut and oil palm, cotton oil, kasto röl and esters of the same animal waxes such as tallow, beech nen wax, whale wax or aqueous lanolin, fatty acids such as Stearic acid, lauric acid or myristic acid, esters or Amides of fatty acids such as ethylene glycol monostearate, propy lenglycol monostearate and glycerol monostearate, sorbitan fat acid esters such as sorbitan monopalmitate, sorbitan monostearate and sorbitan tristearate, fatty alcohols such as cetyl alcohol, ethoxylated fatty alcohols, triglycerides such as triglycerides of vegetable oils or modified vegetable oils, petroleum or Mineral waxes like paraffin and alkylene glycols like at Room temperature solid ethylene glycols and propylene glycols. 3. Composition according to claim 1 or 2, characterized in that the active ingredient encapsulated by the matrix-forming material

• a) is a solid particle with a size smaller than 1 µm,
• b) is a solid or a liquid which has dissolved in the hot melt of the matrix-forming material during production, or
• c) is a solid or a liquid that was dissolved in a water-immiscible carrier liquid during manufacture.

4. Composition according to one of claims 1 to 3, characterized characterized in that of the matrix-forming material encapsulated active ingredient a UV absorbing mate rial, an essential oil, a vitamin, an organic color substance, an organic or inorganic pigment Lubricating oil, a fragrance or a flavoring agent and ins special is selected from pine oil, peppermint oil, sub substituted or unsubstituted cinnamic acids or substit ized or unsubstituted cinnamic acid esters, triazoles bonds, organic dyes, inorganic pigments, Perfume oils, derivatives of γ-linolenic acid, vitamins, ins special vitamins E and A, or skin softening agents. 5. Composition according to one of claims 1 to 4, characterized characterized in that the particles of matrix and active Be component an average size of 500 to 5, ins have particular 200 to 5 nm or less. 6. Composition according to one of claims 1 to 5, characterized characterized in that in each particle of the matrix-forming Material at least one particle of the active ingredient is available. 7. Composition according to one of claims 1 to 6, characterized characterized in that the ratio of active ingredient to the matrix-forming material in the range from 0.04 to 25, is in particular 1 to 10.   8. Aqueous dispersion containing a solid, particulate composition composition according to one of claims 1 to 7. 9. Aqueous dispersion according to claim 8, characterized in that that they 1.0 to 50.0 wt .-% of solid, particulate Zu composition as discontinuous phase and given if surfactant comprises. 10. Aqueous dispersion according to claim 8 or 9, characterized records that the surfactant is anionic, cationic, amphote res or nonionic surfactant or a mixture thereof includes and is particularly selected from ethoxylated Alcohols and ethoxylated alkylphenols, ethoxylated Fatty acid esters, sulfosuccinic acid esters, sorbitan esters, Alkyl and aryl sulfonates as well as mono- and diglycerides from Stearic, palmitic and oleic acids. 11. A method for producing a composition according to any one of claims 1 to 7 or an aqueous dispersion according to any one of claims 8 to 10, characterized in that

• 1) at least one water-insoluble, non-polymeric, matrix-forming material which is solid at room temperature and a water-insoluble active ingredient to be encapsulated in the matrix are heated together to a temperature which is sufficient to melt the matrix-forming material,
• 2) the hot melt formed from matrix-forming material and active ingredient is added to water with agitation, optionally with surfactant being present to produce a stable aqueous emulsion, the matrix-forming material with the active ingredient enclosed therein in the form of droplets of average size of about 1 µm or less, and
• 3) the stable, aqueous emulsion is cooled to room temperature in order to obtain an aqueous dispersion of solid particles of matrix-forming material with encapsulated active ingredient, which is then optionally removed from the water.

12. The method according to claim 11, characterized in that the at least one matrix-forming material is selected from Vegetable oils, especially hydrogenated palm oil, are hydrogenated Triglycerides of coconut and oil palm, cotton oil, kasto röl and esters of the same animal waxes such as tallow, beech nen wax, whale wax or aqueous lanolin, fatty acids such as Stearic acid, lauric acid or myristic acid, esters or Amides of fatty acids such as ethylene glycol monostearate, propy lenglycol monostearate and glycerol monostearate, sorbitan fat acid esters such as sorbitan monopalmitate, sorbitan monostearate and sorbitan tristearate, fatty alcohols such as cetyl alcohol, ethoxylated fatty alcohols, triglycerides such as triglycerides of vegetable oils or modified vegetable oils, petroleum or Mineral waxes like paraffin and alkylene glycols like at Room temperature solid ethylene glycols and propylene glycols. 13. The method according to claim 11 or 12, characterized in that the active ingredient to be encapsulated by the matrix-forming material

• a) is a solid particle with a size smaller than 1 µm,
• b) is a solid or a liquid which is soluble in the hot melt of the matrix-forming material during manufacture, or
• c) is a solid or a liquid which is dissolved in a water-immiscible carrier liquid.

14. The method according to any one of claims 11 to 13, characterized ge indicates that of the matrix-forming material encapsulating active ingredient a UV absorbing material al, an essential oil, a vitamin, an organic color  substance, an organic or inorganic pigment Lubricating oil, a fragrance or a flavoring agent and ins special is selected from pine oil, peppermint oil, sub substituted or unsubstituted cinnamic acids or substit ized or unsubstituted cinnamic acid esters, triazoles bonds, organic dyes, inorganic pigments, Perfume oils, derivatives of γ-linolenic acid, vitamins, ins special vitamins E and A, or skin softening agents. 15. The method according to any one of claims 11 to 14, characterized ge indicates that the hot melt has at least one surfactant is added before the melt in step 2) to the water is given and / or the water to which the hot melt is given in step 2), contains at least one surfactant. 16. The method according to any one of claims 11 to 15, characterized ge indicates that the surfactant is anionic, cationic, amphoteric or nonionic surfactant or a mixture the same includes and is particularly selected from ethoxy lated alcohols and ethoxylated alkylphenols, ethoxy gated fatty acid esters, sulfosuccinic acid esters, Sorbi Tan esters, alkyl and aryl sulfonates as well as mono- and digly cerides of stearic, palmitic and oleic acids. 17. The method according to any one of claims 11 to 16, characterized ge indicates that the hot melt in stage 1) at least a surfactant is added and then to the water to which the hot melt in stage 2) is added before or the same in time with the addition of the hot melt to the water either a different or the same surfactant is given. 18. The method according to any one of claims 11 to 17, characterized ge indicates that the movement in stage 2) through treatment is effected with ultrasound, this treatment ins particularly 0.1 to 30 minutes and preferably about 4 minutes long.   19. The method according to any one of claims 11 to 18, characterized ge indicates that the interfacial tension between the Droplets of matrix-forming material with inside chem active ingredient and the water less than about 10 dynes / cm is. 20. The method according to any one of claims 11 to 19, characterized ge indicates that the droplets of matrix and active Be component an average size of 500 to 5, ins particularly obtained from 200 to 5 nm or less. 21. The method according to any one of claims 11 to 20, characterized ge indicates that in each particle of the matrix-forming Ma terials at least one particle of the active ingredient is available. 22. The method according to any one of claims 11 to 21, characterized ge indicates that the ratio of active ingredient to Matrix-forming material in stage 1) in the range from 0.04 to 25 (= 1:25 to 25: 1). 23. The method according to any one of claims 11 to 22, characterized ge indicates that the cooling in stage 3) with an Ab cooling rate of 1 ° C to 10 ° C per minute. 24. The method according to any one of claims 11 to 23, characterized ge indicates that the cooling in stage 3) by adding additional water to the aqueous emulsion is reached, this additional water being a lower temperature than the emulsion. 25. The method according to any one of claims 11 to 24, characterized ge indicates that the matrix-forming material in stage 1) to a temperature below 100 ° C, in particular 60 to 85 ° C is heated, this temperature during the movement in Level 2) is maintained.   26. The method according to any one of claims 11 to 25, characterized ge indicates that it is carried out under inert gas. 27. The method according to any one of claims 11 to 26, characterized ge indicates that the hot melt has a viscosity points that is less than about 500 mPa · s. 28. Use of a composition according to any one of the claims 1 to 7 or a dispersion according to any one of claims 8 up to 10 as / in cosmetic product / s or for the production of Cosmetic products.