Shellless stable dispersions
By using an oil-in-water dispersion without amino-terminated polydimethylsiloxane, and employing a lipophilic gelling agent and an oil phase, the stability and comfort issues of existing technologies have been resolved, achieving droplet kinetic stability and aesthetics, and providing greater freedom in encapsulating active ingredients.
Patent Information
- Application Number
- CN202511390313.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2020-05-21
- Filing Date
- 2021-05-21
- Publication Date
- 2025-11-18
AI Technical Summary
Existing oil-in-water dispersions, when containing amino-terminated polydimethylsiloxane, suffer from poor dispersion stability, compatibility issues, droplet aggregation and adhesion, affecting aesthetics and user comfort, and are also environmentally unfriendly.
An oil-in-water dispersion without amino-terminated polydimethylsiloxane is used, employing lipophilic gelling agents and an oil phase to meet specific physicochemical standards, such as hardness, adhesion, and cohesion, ensuring the kinetic stability and aesthetics of the droplets.
It achieves kinetic stability and aesthetics over long periods of time, preventing droplets from agglomerating and adhering, providing a comfortable user experience, and allowing for greater freedom in encapsulating active ingredients.
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Abstract
Description
[0001] This application is a divisional application of the invention patent application with application number 202180036208.7.
[0002] The object of this invention is a stable oil-in-water dispersion comprising droplets, particularly macroscopic droplets, of a continuous aqueous phase and a dispersed fatty phase including at least one lipophilic gelling agent. The object also includes compositions containing said dispersion, particularly cosmetic compositions, and their use in the cosmetic field.
[0003] To date, dispersions in the form of direct emulsions exist, such as those described in US2004 / 137020 and EP2189081. However, the dispersed phase of these dispersions is not in the form of macro-droplets and is too stiff for satisfactory sensory and / or comfort upon application, especially in the presence of a macro-droplet dispersed phase.
[0004] Stable dispersions of aliphatic phase droplets also exist in a continuous aqueous phase, as described in WO2017046305. These dispersions are obtained using microfluidic methods and their kinetic stability is ensured by the presence of a shell from a complex interfacial condensation reaction, which in particular depends on a lipophilic organosilicon cationic polymer, amino-terminated polydimethylsiloxane. The dispersed aliphatic phase droplets in these dispersions are macroscopic, i.e., visible to the naked eye, and give the dispersions an attractive aesthetic appearance sought by consumers. This property is even more interesting because the droplet shells are very thin, and the user does not feel any resistance associated with shell breakage when applied to keratin materials, and the observed shells do not leave any residual deposits. This is called an evanescent shell.
[0005] Due to their environmental impact, their non-biodegradability, and / or their potential health hazards, consumers are increasingly demanding cosmetic compositions that do not contain silicone compounds.
[0006] Furthermore, the inventors have observed that the presence of amino-terminated polydimethylsiloxane can sometimes lead to compatibility issues with other raw materials and / or droplet aggregation, droplet adhesion to packaging, and / or droplet sphericity defects, which are undesirable for obvious reasons. In fact, such drawbacks can affect the stability of the dispersion and / or the uniformity of delivery of the different phases constituting the dispersion and / or the visual and aesthetic appearance of the dispersion, or even its sensory properties when applied to the skin, and these drawbacks are exacerbated with increasing droplet diameter. Without wishing to be bound by any theory, the applicant believes that the aforementioned droplet sphericity defects may be related to a reduction in the elasticity of the dispersed fatty phase due to the presence of amino-terminated polydimethylsiloxane.
[0007] Therefore, there is a need for new dispersions that include droplets of dispersed fatty phases in a continuous aqueous phase, particularly macroscopically sized droplets of dispersed fatty phases, and that maintain satisfactory kinetic stability, sensory properties, and application comfort despite the absence of amino-terminated polydimethylsiloxane and therefore no shell.
[0008] Therefore, the present invention relates to an oil-in-water dispersion comprising or even containing a dispersed phase comprising droplets and a continuous aqueous phase, preferably in gel form, wherein the droplets comprise a fatty phase containing at least one lipophilic gelling agent and preferably at least one oil, wherein:
[0009] - The melting point of the aliphatic phase is 50-100℃, preferably 60-90℃, and it meets the following physicochemical standards at room temperature and atmospheric pressure:
[0010] - The hardness (x) is 2-14 N, preferably 2.5-12 N, more preferably 3-9 N, and most preferably 4-6 N; and
[0011] - Adhesion (y) greater than or equal to -2N, better to be greater than or equal to -1N, and especially greater than or equal to -0.6N; and
[0012] - The dispersion does not include amino-terminated polydimethylsiloxane.
[0013] Preferably, the cohesiveness (z) of the fatty phase of the dispersion according to the invention is less than or equal to 40, preferably less than or equal to 35, and more preferably greater than or equal to 30.
[0014] As can be seen and surprisingly from the examples below, the use of a dispersed fatty phase having the above-described physicochemical properties makes it possible to obtain dispersions, particularly macroscopic dispersions, which, despite the absence of amino-terminated polydimethylsiloxane and therefore no shell, exhibit satisfactory or even improved performance in terms of kinetic stability, and thus have a visual and aesthetic appearance, ease of application to the skin, and comfort.
[0015] In particular, the inventors have observed that the dispersion according to the invention exhibits satisfactory or even improved performance in terms of droplet non-aggregation, droplet non-adhesion to packaging, and comfort and ease of application to the skin.
[0016] Given the absence of amino-terminated polydimethylsiloxanes, the dispersions according to the present invention also allow for greater freedom regarding the encapsulated compounds and / or their contents, particularly the active ingredients.
[0017] Within the meaning of this invention, the terms "stable" and "kinetic stability" mean that, for the dispersion according to the invention, over a period of time greater than or equal to one month, preferably greater than or equal to three months, and more preferably greater than or equal to six months, at room temperature and atmospheric pressure, the droplets of the dispersed phase in the continuous phase do not exhibit emulsion stratification or sedimentation, the continuous aqueous phase is not opaque, the droplets do not aggregate with each other, particularly there is no agglomeration or Ostwald ripening between them, the droplets do not adhere to the packaging, and the material does not leak from the dispersed phase into the continuous phase, and vice versa.
[0018] Within the meaning of this invention, "gelling agent" refers to a reagent capable of increasing the viscosity of a phase without said gelling agent, and preferably achieving a final viscosity of the phase such that it is gelled to be greater than 20,000 mPa·s, more preferably greater than 50,000 mPa·s, more preferably greater than 100,000 mPa·s, and very particularly greater than 200,000 mPa·s.
[0019] In the context of this invention, "macroscopic" or "macroscopic droplets" or "macroscopic dispersion" refers to droplets of a dispersed fatty phase that are visible to the naked eye, as opposed to microscopic droplets that are invisible to the naked eye. Therefore, preferably, in the dispersion according to the invention:
[0020] - The volume of the droplets having a diameter greater than or equal to 100 μm, or even greater than or equal to 200 μm, or better, greater than or equal to 300 μm, particularly greater than or equal to 400 μm, preferably greater than or equal to 500 μm, or even greater than or equal to 1,000 μm, or even between 100 μm and 3,000 μm, better between 200 μm and 2,000 μm, particularly between 300 μm and 1,000 μm, or better between 500 μm and 3,000 μm, preferably between 1,000 μm and 2,000 μm, particularly between 800 μm and 1,500 μm is greater than or equal to 60%, or greater than or equal to 70%, preferably greater than or equal to 80%, and more preferably greater than or equal to 90%, and / or;
[0021] - At least 60%, or even at least 70%, preferably at least 80%, and more preferably at least 90% of the said droplets have an average diameter greater than or equal to 100 μm, or even greater than or equal to 200 μm, and more preferably greater than or equal to 300 μm, particularly greater than or equal to 400 μm, preferably greater than or equal to 500 μm, or even greater than or equal to 1,000 μm, or even between 100 μm and 3,000 μm, and more preferably between 200 μm and 2,000 μm, particularly between 300 μm and 1,000 μm, more preferably between 500 μm and 3,000 μm, preferably between 1,000 μm and 2,000 μm, and particularly between 800 μm and 1,500 μm.
[0022] Determining the volume of a droplet with a specific diameter relative to the total volume of the dispersed phase is common knowledge to those skilled in the art, particularly regarding the diameter measurement methods described below.
[0023] The dispersion according to the invention can be described as a macroscopically heterogeneous mixture of two immiscible phases, particularly when the droplets are macroscopic. In other words, in the dispersion according to the invention, each phase can be distinguished individually, especially by the naked eye.
[0024] In the context of this invention, the above-described dispersion may be referred to as an "emulsion". Regarding the properties of the phases, the emulsion according to the invention is an oil-in-water emulsion (or a direct emulsion), wherein the dispersed fatty phase and the continuous aqueous phase are immiscible with each other at room temperature and atmospheric pressure. Therefore, the solubility of the dispersed fatty phase in the continuous aqueous phase is advantageously less than 5 wt%, and vice versa.
[0025] According to another embodiment, the dispersion according to the invention is a simple emulsion, i.e., containing only a continuous aqueous phase and a dispersed fatty phase. In other words, the dispersion according to the invention is not a multiple emulsion, especially a dual emulsion, such as an oil-in-water emulsion.
[0026] According to another embodiment, the dispersion according to the invention does not include a surfactant.
[0027] According to one embodiment, the dispersion according to the invention does not include tricaprylic acid glyceride, tricaprylic acid / capric acid glyceride, or a mixture thereof.
[0028] According to one embodiment, the dispersion according to the present invention does not include:
[0029] - Dextrin esters and fatty acids, especially dextrin palmitate, and / or optionally hydrophobically treated silica, such as fumed silica, and / or
[0030] - Acrylic ester / C10-30 alkyl acrylate crosspolymers, particularly Pemulen from Lubrizol.TM EZ-4U polymer emulsifier; and / or
[0031] - Cetyl ethylhexanoate.
[0032] Preferably, the droplets exhibit significant monodispersity (i.e., they are perceived by the eye as spheres of the same diameter).
[0033] The droplets are advantageously substantially spherical.
[0034] The droplets of the dispersion according to the invention do not contain a shell or membrane, particularly a polymer membrane or a membrane formed by interfacial polymerization. Specifically, the droplets of the dispersion according to the invention are not stabilized by a coagulated layer membrane (anionic polymer (carbomer) / cationic polymer (amino-terminated polydimethylsiloxane) type). In other words, the contact between the continuous aqueous phase and the dispersed fatty phase is direct.
[0035] Therefore, according to one embodiment, the dispersion according to the invention does not include a shell, particularly a shell formed by a coagulated layer inserted between the dispersed fatty phase and the continuous aqueous phase.
[0036] In particular, the dispersions according to the present invention do not include (are free from) lipophilic cationic polymers of the following formula:
[0037] in:
[0038] -R1, R2, and R3 independently represent OH or CH3;
[0039] -R4 represents a -CH2- group or a -X-NH- group, where X is a divalent C3 or C4 alkylene group;
[0040] -x is an integer from 10 to 5,000, preferably from 30 to 1,000, and more preferably from 80 to 300;
[0041] -y is an integer from 1 to 1000, particularly from 2 to 1000, preferably from 4 to 100, and more preferably from 5 to 20; and
[0042] -z is an integer from 0 to 10, preferably 0 to 1, and more preferably equal to 1.
[0043] The droplet is different from a solid capsule, i.e. a capsule with a solid shell (or “membrane”), such as the capsule described in WO2010 / 063937, and a capsule with an evanescent shell, such as the capsule described in WO2012120043.
[0044] According to the present invention, the pH of the dispersion is typically 4.0-8.0, particularly 5.0-7.0.
[0045] Temperature and pressure
[0046] Unless otherwise stated, all the following are assumed to be at room temperature (e.g., T = 25℃ ± 2℃) and atmospheric pressure (760 mm Hg, i.e., 1.013 × 10⁻⁶). 5 Pa or 10 13 (mbar) below.
[0047] Viscosity
[0048] The viscosity of the dispersion or at least one phase thereof according to the invention can vary significantly, which allows for the acquisition of various textures. Viscosity was measured at room temperature and room pressure according to the method described in WO2017046305.
[0049] According to one embodiment, the viscosity of the dispersion according to the invention is from 1 mPa·s to 500,000 mPa·s, preferably from 10 mPa·s to 300,000 mPa·s, more preferably from 400 mPa·s to 100,000 mPa·s, and particularly from 1,000 mPa·s to 30,000 mPa·s, as measured at 25°C according to the method described above.
[0050] Continuous aqueous phase
[0051] As described above, the dispersion according to the invention comprises a continuous aqueous phase, preferably in gel form, particularly a gel with a viscosity suitable for suspending droplets and thus contributing to the kinetic stability and visual appeal of the dispersion according to the invention.
[0052] Advantageously, the continuous aqueous phase is not a solid at room temperature and room pressure, i.e., it is able to flow under its own weight.
[0053] According to one embodiment, the viscosity of the aqueous phase is from 400 mPa·s to 100,000 mPa·s, preferably from 800 mPa·s to 30,000 mPa·s, as measured at 25°C by the method described above.
[0054] The continuous phase of the dispersion according to the invention comprises water.
[0055] In addition to distilled or deionized water, the water suitable for use in this invention can also be natural spring water or flower water.
[0056] According to one embodiment, the weight percentage of water in the continuous aqueous phase is at least 30%, preferably at least 40%, particularly at least 50%, and more preferably at least 60%, particularly 70-98%, and preferably 75-95%, relative to the total weight of the continuous phase.
[0057] The continuous aqueous phase of the dispersion according to the invention may further comprise at least one base. It may comprise a single base or a mixture of several different bases. The presence of at least one base in the continuous aqueous phase is particularly beneficial for increasing the viscosity of the latter.
[0058] In one embodiment, the base present in the aqueous phase is an inorganic base.
[0059] According to one embodiment, the inorganic base is selected from alkali metal hydroxides and alkaline earth metal hydroxides.
[0060] Preferably, the inorganic base is an alkali metal hydroxide, especially NaOH.
[0061] In one embodiment, the base present in the aqueous phase is an organic base. Examples of such organic bases are ammonia, pyridine, triethanolamine, aminomethylpropanol, or triethylamine.
[0062] The dispersion according to the invention may include 0.01-10 wt%, preferably 0.01-5 wt%, and more preferably 0.02-1 wt%, of an alkali, preferably an inorganic alkali, and particularly NaOH, relative to the total weight of the dispersion.
[0063] Fat phase
[0064] The melting point of the dispersed fatty phase in the dispersion according to the present invention is 50-100°C, preferably 60-90°C.
[0065] The melting point of the adipose phase can be measured using a differential scanning calorimeter (DSC), such as the calorimeter sold by TA Instruments as “DSCQ2000”. The sample preparation and measurement protocol is as follows: A 5 mg test sample, preheated to 80 °C and removed with a heated scraper under magnetic stirring, is placed in a hermetically sealed aluminum capsule or crucible. Two tests are performed to ensure reproducibility of the results. Measurements are performed on the aforementioned calorimeter. The furnace is purged with nitrogen. Cooling is provided by an RCS 90 heat exchanger. The sample is then subjected to the following protocol: first, heating to 20 °C, followed by a first heating rate of 5 °C / min from 20 °C to 130 °C, then cooling at a rate of 5 °C / min from 130 °C to -80 °C, and finally a second heating rate of 5 °C / min from -80 °C to 130 °C. During the second heating, the power difference absorbed by the empty crucible and the crucible containing the sample is measured as a function of temperature. The melting point of a compound is the temperature value corresponding to the peak of the curve representing the power input difference as a function of temperature. The melting point is the temperature at which 95% of the sample melts.
[0066] The dispersed fatty phase of the dispersion according to the present invention must meet at least two of the following physicochemical standards regarding hardness and adhesion:
[0067] The hardness (x) is 2-14 N, preferably 2.5-12 N, particularly 3-9 N, and more preferably 4-6 N. Hardness (or firmness) corresponds to the maximum compressive force measured in Newtons. Regarding the dispersion according to the invention, hardness (x) is an indicator of the sensory feel of the dispersion when applied to keratin materials, particularly the skin. On the one hand, the hardness must not be too low to ensure that the dispersed fatty phase droplets have sufficient mechanical resistance, particularly to shear and / or mechanical stresses associated with, for example, the manufacture and packaging and / or transport of the dispersion, and thus ensure satisfactory kinetic stability of the dispersion, especially in the presence of non-aerobic packaging. On the other hand, the hardness should not be too high to avoid reducing sensory qualities, particularly comfort and ease of application when applied to the skin. The larger the diameter of the dispersed fatty phase droplets in the dispersion, the more pronounced the above situation becomes.
[0068] - Adhesion (y) is greater than or equal to -2N, more preferably greater than or equal to -1N, and particularly greater than or equal to -0.6N. Adhesion represents the work required to overcome the attraction between the product surface and the material in contact with it (e.g., the total force required to separate a measuring tool from a sample). Regarding the dispersion according to the invention, the adhesion criterion (y) is an indicator of the kinetic stability of the dispersion with respect to the phenomenon of droplets adhering to the packaging wall.
[0069] The cohesiveness (z) of the dispersed fatty phase in the dispersion according to the invention is advantageously less than or equal to 40, preferably less than or equal to 35, and more preferably greater than or equal to 30. Preferably, the cohesiveness (z) of the dispersed fatty phase in the dispersion according to the invention is advantageously greater than or equal to 15, preferably greater than or equal to 20, and more preferably greater than or equal to 25. Advantageously, the cohesiveness (z) of the dispersed fatty phase in the dispersion according to the invention is 15-40, preferably 20-35, and more preferably 20-30. Cohesiveness refers to the ability of a tested product to resist a second deformation relative to its behavior during the first deformation. Cohesiveness corresponds to the area of the second curve (area 2) on the surface of the first curve (area 1) (i.e., area 2 / area 1). In other words, cohesiveness represents the strength within the tested sample. Therefore, strong bonding within the gel will allow for fully reversible deformation during the first compression, which will cause a force A2 equal to force A1, and thus 100% cohesiveness. Therefore, the stronger the cohesiveness, the more easily the gel deforms. The lower the cohesiveness, the more brittle the gel (weak binding, no stress resistance). Regarding the dispersions according to the invention, the cohesiveness criterion (z) is an indicator of the kinetic stability of the dispersion with respect to the aggregation or even coalescence of the dispersed phase droplets between them. Cohesiveness is a property of droplet self-adhesion. Therefore, a minimum cohesiveness is required to ensure the "gelling" properties of the droplets, but not too much to prevent gelled droplets from sticking together.
[0070] Hardness, adhesion, and cohesiveness measurements were obtained using the Shimadzu EZ-X texture analyzer and the following texture analyzer protocol:
[0071] - Place the test sample in a mold with a diameter of 40 mm and fill it to 75% of its height.
[0072] - The moving body used is a cylindrical acrylic moving body with a diameter of 12.7 mm. The movement of the moving body includes 4 steps:
[0073] 1) In the first step after automatic sample surface detection, the moving body moves at a measuring speed of 1 mm / s and penetrates the sample to a penetration depth of 5 mm, and the software records the value of the maximum force reached.
[0074] 2) The second step of the retraction is called retraction at a speed of 1 mm / s, wherein the moving body returns to its initial position and rises 5 mm, and the retraction energy (negative force) of the probe is recorded.
[0075] 3) Repeat step 3 of the same action 1) above, and
[0076] 4) Repeat step 4 of the same action 2) above.
[0077] This combination of physicochemical standards constitutes a non-obvious compromise, characterized by a brittle but not very adhesive and not very elastic anhydrous gel. As can be seen from the examples below, this combination of physicochemical standards enables the production of dispersions, particularly macroscopic dispersions, which, despite the absence of amino-terminated polydimethylsiloxane and therefore no shell, exhibit satisfactory or even improved performance in terms of kinetic stability, thus possessing visual and aesthetic appeal, as well as sensory qualities, particularly comfort and ease of application to the skin.
[0078] Regarding hardness, the hardness value in N obtained by the above measurement method can be easily converted to Pa, for example, for the surface of the above 12.7mm cylindrical acrylic moving body.
[0079] Typically, 1 MPa is equivalent to 1 N / mm². 2 Furthermore, to convert the measured hardness values according to the invention into N, it is sufficient to divide them by the surface area of the probe. For example, using a probe with a diameter of 12.7 mm as described above, its surface area is equal to S = π × (12.7 / 2). 2 =126.68mm 2 To obtain the hardness value in MPa, the value measured with this probe should be divided by 126.68.
[0080] For the above measurements, the Shimadzu EZ-X texture analyzer was used in combination with the TRAPEZIUM X software.
[0081] The dispersed fatty phase droplets of the dispersion according to the invention are preferably based on a viscoelastic gel with an elastic modulus greater than its viscous modulus. The droplets do not flow under their own weight but can be easily deformed by pressure (e.g., with a finger). Therefore, they have a consistency similar to butter, exhibiting stretchable and graspable properties. The droplets can be easily spread by hand, particularly on keratinous materials, especially on the skin.
[0082] The dispersed fatty phase of the dispersion according to the invention comprises at least one lipophilic gelling agent. Essentially, the combination of at least one lipophilic gelling agent and at least one oily solvent enables the dispersed fatty phase of the dispersion according to the invention to satisfy the aforementioned physicochemical standards x and y, or even z.
[0083] Lipophilic gelling agents
[0084] Advantageously, the lipophilic gelling agent is a heat-sensitive gelling agent, i.e., a gelling agent that reacts with heat, and particularly a gelling agent that is solid at room temperature and liquid at temperatures above 50°C, preferably above 60°C, and more preferably above 70°C. Preferably, the melting point of the lipophilic heat-sensitive gelling agent according to the invention is 50-130°C, more preferably 60-120°C.
[0085] The lipophilic gelling agent according to the present invention may be selected from organic or inorganic, polymeric or molecular lipophilic gelling agents; fats that are solid at ambient temperature and pressure; and mixtures thereof.
[0086] Organic or inorganic, polymeric or molecularly lipophilic gelling agents
[0087] As a lipophilic mineral binder, one could mention modifiable clays, such as those using C... 10 -C 22 Ammonium chloride-modified lithium montmorillonite, such as lithium montmorillonite modified with distearate dimethyl ammonium chloride, for example, by Hymens under the name Bentone. Other examples include distearate-dimethylammonium chloride modified lithium montmorillonite, also known as quaternary ammonium-18 bentonite, such as products sold or manufactured by Veles under the trade name Bentone 34; Claytone XL, Claytone 34, and Claytone 40 sold or manufactured by Southern Clay Company; modified clays known as benzoyl ammonium and quaternary ammonium-18 bentonite sold or manufactured by Southern Clay Company under the trade names Claytone HT, Claytone GR, and Claytone PS; stearyl dimethylbenzoyl ammonium chloride modified clay, known as stearyl chloride bentonite, such as products sold or manufactured by Southern Clay Company under the trade names Claytone APA and Claytone AF; and Baragel 24 sold or manufactured by Veles.
[0088] Another example is fumed silica, which can be treated with hydrophobic surface treatment to achieve a particle size of less than 1 μm. Indeed, the surface of silica can be chemically modified through chemical reactions to reduce the number of silanol groups present on the silica surface. In particular, silanol groups can be replaced with hydrophobic groups to obtain hydrophobic silica.
[0089] The hydrophobic group can be:
[0090] -Trimethylsilyloxy, which is obtained, in particular, by treating fumed silica in the presence of hexamethyldisilazane. According to CTFA (8th edition, 2000), silica treated in this manner is referred to as "silylated silica". They are sold, for example, by Degussa under the designation Aerosil R812, and by Cabot under the designation CAB-O-SIL TS-530; or
[0091] -Dimethylsiloxy or polydimethylsiloxane groups, which are obtained, in particular, by treating fumed silica in the presence of polydimethylsiloxane or dimethyldichlorosilane. According to CTFA (8th edition, 2000), silica treated in this manner is referred to as "dimethylsilylated silica". These are sold, for example, by Degussa under the numbers Aerosil R972 and Aerosil R974, and by Cabot under the numbers CAB-O-SIL TS-610 and CAB-O-SIL TS-720.
[0092] In particular, the particle size of hydrophobic fumed silica can be from nanometers to micrometers, for example, about 5-200 nm.
[0093] Polymer organic lipophilic gelling agents include, for example, partially or fully crosslinked elastomeric organopolysiloxanes with a three-dimensional structure, such as those marketed by Shin-Etsu Chemical Co. under the names KSG6, KSG16 and KSG18; by Dow Corning Co. under the names Trefil E-505C and Trefil E-506C; by Grant Chemical Co. under the names SR-CYC, SR DMF 10, SR-DC556, SR 5CYC gel, SR DMF 10 gel and SR DC 556 gel; and by General Electric Co. under the names SF 1204 and JK 113; ethyl cellulose, for example, marketed by Dow Chemical Co. under the name Ethocel; galactomannan containing 1-6, particularly 2-4 hydroxyl groups / sugars, substituted with saturated or unsaturated alkyl chains, such as guar gum alkylated with C1-C6, particularly C1-C3 alkyl chains, and mixtures thereof. Block copolymers of the "diblock," "triblock," or "radial" type, such as polystyrene / polyisoprene and polystyrene / polybutadiene, such as those marketed by BASF under the name Luvitol. Block copolymers of the polystyrene / copolymer (ethylene-propylene) type sold, such as those marketed by Shell Chemical Company under the name... Block copolymers of polystyrene / copolymer (ethylene-butene) type mixtures, such as those sold by PENRECO under the name of triblock and radial (star-shaped) copolymers in isododecane. Products for sale include mixtures of triblock butene / ethylene / styrene copolymers and ethylene / propylene / styrene star copolymers in isododecane (Versagel M 5960).
[0094] According to one embodiment, the gelling agent that can be used according to the invention may be selected from polyacrylates; sugars / polysaccharides and fatty acid esters, especially dextrins and fatty acid esters, glycerols and fatty acid esters or inulin and fatty acid esters; polyamides and mixtures thereof.
[0095] As a lipophilic gelling agent, polymers with a weight average molecular weight of less than 100,000 may also be mentioned, comprising a) a polymer backbone having a hydrocarbon repeating unit containing at least one heteroatom, and optionally b) at least one side aliphatic chain and / or at least one optionally functionalized terminal aliphatic chain having 6 to 120 carbon atoms and bonded to these hydrocarbon units, as described in applications WO02 / 056847 and WO02 / 47619, particularly polyamide resins (particularly including alkyl groups having 12 to 22 carbon atoms), such as those described in US5783657.
[0096] An example of a polyamide resin that can be used according to the present invention is UNICLEAR 100, sold by Arizona Chemical Company.
[0097] Alternatively, organosilicon polyamides of the polyorganosiloxane type, such as those described in US5874069, US5919441, US6051216 and US5981680, may be used.
[0098] These organosilicon polymers can belong to the following two families:
[0099] - A polyorganosiloxane having at least two groups capable of establishing hydrogen interactions, these two groups being located in the polymer chain, and / or
[0100] - A polyorganosiloxane containing at least two groups capable of establishing hydrogen interactions, wherein these two groups are located on a graft or branch.
[0101] Lipophilic gelling agents that can be used in this invention include fatty acid dextrin esters, such as dextrin palmitate. According to one embodiment, the esters of dextrin and fatty acids according to this invention are monoesters or polyesters of dextrin and at least one fatty acid corresponding to the following formula:
[0102]
[0103] in:
[0104] n is an integer between 2 and 200, preferably between 20 and 150, and especially between 25 and 50.
[0105] Groups R4, R5, and R6 may be the same or different, and are selected from hydrogen or acyl-CORa, wherein group Ra represents a straight-chain or branched saturated or unsaturated hydrocarbon group having 5 to 50, preferably 5 to 25 carbon atoms.
[0106] The condition is that at least one of the R4, R5, or R6 groups is not hydrogen.
[0107] Examples of dextrin fatty acid esters are dextrin palmitate, dextrin myristate, dextrin palmitate / ethylhexanoate, and mixtures thereof. Examples include those produced by Sanhao Europe under the name... KL2 or D2 (INCI name: dextrin palmitate), TT2 (INCI name: dextrin palmitate / ethylhexanoate) and MKL2 (INCI name: dextrin myristate) is a fatty acid dextrin ester. Among the lipophilic gelling agents that can be used in this invention, reference may also be made to the product manufactured by Miyoshi Europe under the name... ISK2 or ISL2 (INCI name: Stearoyl Inulin) sells inulin and fatty acid esters.
[0108] Among the lipophilic gelling agents that can be used in this invention, reference may also be made to acrylic acid C. 10 -C30 Alkyl ester, preferably acrylic acid C 14 -C 24 Alkyl esters, or even more preferably acrylic C 18 -C 22 Polyacrylates are produced by the polymerization of alkyl esters. According to one embodiment, the polyacrylate is a polymer of acrylic acid esterified with a fatty alcohol or a mixture of said fatty alcohols whose saturated carbon chain contains 10 to 30 carbon atoms, preferably 14 to 24 carbon atoms. Preferably, the fatty alcohol contains 18 or 22 carbon atoms. Polyacrylates particularly include stearyl polyacrylate and behenyl polyacrylate. Preferably, the gelling agent is stearyl polyacrylate or behenyl polyacrylate. Examples include those produced by Air Products under the name... Polyacrylates sold (INCI name: C10-C30 alkyl polyacrylate), including 13.1 and 13.6.
[0109] In the lipophilic gelling agents that can be used in this invention, esters of glycerol and fatty acids, particularly monoesters, diesters, or triesters of glycerol and fatty acids, may also be mentioned. Typically, the esters of glycerol and fatty acids can be used alone or in mixtures. According to the invention, this can be an ester of glycerol and fatty acids or an ester of a mixture of glycerol and fatty acids. According to one embodiment, the fatty acids are selected from behenic acid, isooctadecanoic acid, stearic acid, eicosanoic acid, and mixtures thereof.
[0110] In one embodiment, the glycerol fatty acid ester has the following formula (III):
[0111]
[0112] Wherein, R1, R2, and R3 are independently selected from H and saturated alkyl chains containing 4 to 30 carbon atoms, and at least one of R1, R2, and R3 is different from H. According to one embodiment, R1, R2, and R3 are different. Examples include fatty acid glycerides sold by Nissin Oriyo Group under the names Nomcort HK-G (INCI name: glyceryl behenate / eicosanoate) and Nomcort SG (INCI name: glyceryl tri(behenate / isostearate / eicosanoate)).
[0113] solid fats
[0114] Solid fats at room temperature and pressure are specifically selected from waxes, pasty fats, butter, and mixtures thereof.
[0115] wax
[0116] Within the meaning of this invention, "wax" is a lipophilic compound that is solid at room temperature (25°C), has a reversible solid / liquid phase change, and has a melting point greater than or equal to 50°C and at most 120°C.
[0117] The method for measuring this melting point is as described above.
[0118] The waxes that can be used in the dispersions according to the invention may be selected from solid waxes (deformable or non-deformable at room temperature) and mixtures thereof from animal, plant, mineral, or synthetic sources. Hydrocarbon waxes such as beeswax, lanolin wax, and Chinese insect wax are used; rice bran wax, carnauba wax, candelilla wax, calomel wax, alpha wax, cork fiber wax, sugarcane wax, Japanese wax, and sumac wax are used; lignite wax, microcrystalline wax, paraffin wax, and ceresin wax; polyethylene wax, waxes obtained through Fischer-Tropsch synthesis, and waxy copolymers and their esters are also used. Examples include those produced by Kahl Wachsraffinerie under the name... 2039 (INCI name: Candelilla wax) and 6607 (INCI name: sunflower seed wax), produced by SACI CFPA under the name Casid HSA (INCI name: hydroxystearic acid), produced by New Phase under the name... 260 (INCI name: synthetic wax) and 103 (INCI name: Synthetic Wax) and waxes sold by Kokyu Alcohol Kogyo under the name AJK-CE2046 (INCI name: Cetearyl Alcohol, Dibutyllauroyl Glutamine, Dibutylethylhexanoyl Glutamine). Also mentioned are waxes obtained by catalytic hydrogenation of animal or vegetable oils having straight or branched C8-C32 fatty chains. These include hydrogenated jojoba oil, hydrogenated sunflower oil, hydrogenated castor oil, hydrogenated coconut oil, and hydrogenated lanolin oil; di-(1,1,1-trimethylolpropane)tetrastearate sold by HETERENE under the name "HEST 2T-4S"; and di-(1,1,1-trimethylolpropane)tetrabenzoate sold by HETERENE under the name HEST 2T-4B.
[0119] Waxes obtained through transesterification and hydrogenation of vegetable oils (such as castor oil or olive oil), for example, those produced by SOPHIM under the name Phytowax Castor, can also be used. and 22L The wax sold by Phytowax Olive 18L57. Such waxes are described in application FR2792190.
[0120] Silicone waxes can also be used, which can be advantageously substituted polysiloxanes, preferably having a low melting point.
[0121] This type of commercially available silicone wax includes silicone waxes sold under the names Abilwax 9800, 9801 or 9810 (GOLDSCHMIDT), KF910 and KF7002 (Shin-Etsu Chemical, Japan), or 176-1118-3 and 176-11481 (General Electric).
[0122] The silicone waxes that can be used are also alkyl or alkoxy polydimethylsiloxanes, such as the following products: Abilwax 2428, 2434 and 2440 (GOLDSCHMIDT), or VP 1622 and VP 1621 (WACKER, Germany), and (C20-C60) alkyl polydimethylsiloxanes, especially (C30-C45) alkyl polydimethylsiloxanes, such as the silicone wax sold by GE Bayer Silicones under the name SF-1642.
[0123] Hydrocarbon waxes modified with silicone or fluorine groups can also be used, such as silicone-based candelilla wax, silicone-based beeswax, and fluorinated beeswax from Koster Keunen.
[0124] Wax can also be selected from fluorinated wax.
[0125] Butter or paste fat
[0126] In the context of this invention, "butter" (also known as "paste fat") refers to a lipophilic fatty compound having a reversible solid / liquid phase change and comprising both liquid and solid portions at 25°C and atmospheric pressure (760 mm Hg). In other words, the initial melting temperature of the paste compound can be below 25°C. The liquid fraction of the paste compound, measured at 25°C, can be 9-97 wt% of the compound. This liquid fraction is preferably 15-85 wt% at 25°C, more preferably 40-85 wt%. Preferably, the final melting temperature of the butter is below 60°C. Preferably, the hardness of the butter is less than or equal to 6 MPa.
[0127] Preferably, the butter or paste fat has an anisotropic crystalline structure in the solid state, which can be observed by X-ray.
[0128] For the purposes of this invention, the melting point is the temperature of the most endothermic peak observed in thermal analysis (DSC) as described in ISO 11357-3:1999. The melting point of a paste-like compound or wax can be measured using a differential scanning calorimeter (DSC), such as the calorimeter sold by TA Instruments as “DSC Q2000”.
[0129] To measure the melting point and determine the melting endpoint temperature, the sample preparation and measurement protocol is as described in WO2017046305.
[0130] The liquid fraction of butter (or paste fat) at 25°C, by weight, is equal to the ratio of the enthalpy of melting consumed at 25°C to the enthalpy of melting of the butter. The enthalpy of melting of butter or paste compound is the enthalpy consumed when the compound changes from a solid to a liquid state.
[0131] Butter is considered solid when its entire substance is in a solid crystalline form. It is considered liquid when its entire substance is in a liquid form. The enthalpy of fusion of butter is equal to the integral of the entire melting curve obtained according to ISO 11357-3:1999 using the calorimeter mentioned above at a temperature rise of 5°C or 10°C / min. The enthalpy of fusion of butter is the amount of energy required to change the compound from a solid to a liquid state. It is expressed in J / g.
[0132] The enthalpy of fusion consumed at 25°C is the amount of energy absorbed by the sample as it changes from a solid state to its state at 25°C, consisting of both liquid and solid components. The liquidus fraction of the butter measured at 32°C is preferably 30-100 wt%, more preferably 50-100 wt%, and even more preferably 60-100 wt% of the compound. When the liquidus fraction of the butter measured at 32°C is equal to 100%, the melting point of the paste-like compound is at a temperature less than or equal to 32°C. The liquidus fraction of the butter measured at 32°C is equal to the ratio of the enthalpy of fusion consumed at 32°C to the enthalpy of fusion of the butter. The enthalpy of fusion consumed at 32°C is calculated in the same manner as that consumed at 23°C.
[0133] For hardness measurement, sample preparation and measurement procedures are as described in WO2017046305.
[0134] Pasty fats or butter can be selected from synthetic compounds and plant-derived compounds. Pasty fats can be obtained by synthesis from plant-derived starting materials.
[0135] Pasty fatty substances are preferably selected from:
[0136] - Lanolin and its derivatives such as lanolin alcohol, oxyethylene lanolin, acetylated lanolin, and lanolin esters such as isopropyl lanolinate and oxypropylene lanolin.
[0137] - Polymer or non-polymeric organosilicon compounds, such as high molecular weight polydimethylsiloxanes, polydimethylsiloxanes with alkyl or alkoxy side chains having 8-24 carbon atoms, especially stearyl polydimethylsiloxanes.
[0138] - Polymer or non-polymeric fluorinated compounds,
[0139] - Vinyl polymers, especially
[0140] - Homopolymers of olefins
[0141] -Olefin copolymer,
[0142] -Homopolymers and copolymers of hydrogenated dienes,
[0143] Linear or branched oligomers, homopolymers, or copolymers of alkyl (meth)acrylates, preferably having C8-C30 alkyl groups.
[0144] - Homopolymers and copolymer oligomers of vinyl esters containing C8-C30 alkyl groups,
[0145] - Homopolymers and copolymer oligomers of vinyl ethers containing C8-C30 alkyl groups,
[0146] - A fat-soluble polyether produced by polyetherification of one or more C2-C100, preferably C2-C50 diols.
[0147] -Esters and polyesters, and
[0148] - Its mixture.
[0149] According to a preferred embodiment of the invention, the specific butter is of plant origin, as described in the Ullman Encyclopedia of Industrial Chemistry (“Fats and Fatty Oils”, Alfred Thomas, published June 15, 2000, DO1:10.1002 / 14356007.a10_173, 13.2.2.2. Shea Butter, Borneo Fat and Related Fats (Vegetable Butter)).
[0150] Of particular note are C10-C18 triglycerides (INCI name: C10-18 triglycerides), which, at 25°C and atmospheric pressure (760 mm Hg), include liquid and solid fractions, shea butter, East African shea butter (from the avocado tree), shea butter, Borneo butter or fat or salsa butter (narrow-winged salsa), salsa resin, *Cercis chinensis* oil, *Cercis chinensis* or *Cercis chinensis* longleaf valerian butter, *Madhuca latifolia* oil, *Madhucamottleyana* oil, *M. butyracea* oil, mango butter (mango (Mangifera indica)), *Astrocatyum murumuru* oil, *Garcinia indica* oil, and *Virola chinensis* oil. (Sebifera), Brazil palm oil, Painya (golden shea butter), coffee oil (Coffea Arabica), almond oil (Prunus armeniaca), macadamia oil (Macadamia temifolia), grape seed oil (Vitis vinifera), avocado oil (Perseagratissima), olive oil (Olea europaea), sweet almond butter (Prunus amygdalusdulcis), cocoa butter (Theobroma cacao), and sunflower butter, butter with INCI name of muruman palm seed oil, butter with INCI name of kupuasau butter, butter with INCI name of wild mango kernel oil, jojoba ester (a mixture of wax and hydrogenated jojoba oil) (INCI name: jojoba ester), and shea butter ethyl ester (INCI name: shea butter ethyl ester), and mixtures thereof.
[0151] According to a particularly preferred embodiment, the lipophilic gelling agent is selected from castor oil / IPDI copolymer (and) caprylic / capric triglyceride, particularly sold by PolymerExpert under the name Estogel M, caprylic / capric triglyceride (and) polyurethane-79, particularly sold by Lubrizol under the name OILKEMIA. TM 5S polymer sales, trihydroxystearin, especially by Haimings Specialty Chemicals Co., Ltd. R is sold, as well as mixtures thereof, and better yet, castor oil / IPDI copolymer (and) caprylic / capric triglycerides.
[0152] According to specific embodiments, the dispersions according to the invention, particularly the fatty phase, do not include elastomeric gels containing at least one polydimethylsiloxane, especially those produced by Norsil Corporation under the name CareSil. TM CXG-1104 (INCI: polydimethylsiloxane (and) polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer) is sold.
[0153] Preferably, at 25°C, the viscosity of the aliphatic phase of the dispersion droplets according to the invention is between 20,000 and 100,000,000 mPa·s, more preferably between 50,000 and 1,000,000 mPa·s, and even more preferably between 100,000 and 500,000 mPa·s.
[0154] Those skilled in the art will be mindful of selecting lipophilic gelling agents and / or their amounts to satisfy the aforementioned melting point and physicochemical properties x and y, or even z, of the aliphatic phase. In particular, the properties and / or amount of the lipophilic gelling agent must take into account the method used to produce the dispersion according to the invention (especially “non-microfluidic” or “microfluidic” types). These adjustments are within the capabilities of those skilled in the art in relation to the teachings of this specification.
[0155] In particular, the dispersion according to the invention may comprise 0.5-30 wt%, preferably 1-25 wt%, especially 1.5-20 wt%, more preferably 2-15 wt%, and most particularly 5-12 wt% of a lipophilic gelling agent relative to the total weight of the fatty phase.
[0156] Preferably, the content of the lipophilic gelling agent is greater than or equal to 2 wt% relative to the total weight of the fatty phase, more preferably greater than or equal to 5 wt%, and even more preferably greater than or equal to 8 wt%.
[0157] These percentages refer to lipophilic gelling agents present only in the dispersed fatty phase.
[0158] Oil
[0159] In one embodiment, the dispersed fatty phase may include at least one oil.
[0160] "Oil" refers to fatty substances that are liquid at room temperature and atmospheric pressure.
[0161] Examples of oils according to the present invention include:
[0162] - Hydrocarbon oils of plant origin, as described below;
[0163] - Hydrocarbon oils of animal origin, such as perhydrosqualene and squalane;
[0164] - Synthetic esters and ethers, especially synthetic esters and ethers of fatty acids, such as oils of formula R1COOR2 and R1OR2, where R1 represents C8 to C9. 29 The fatty acid residues, and R2 represents the branched or unbranched C3 to C4. 30 Hydrocarbon chains, such as duck tail gland oil, isononyl isononanoate, isodecanyl neopentanoate, isostearyl neopentanoate, isopropyl myristate, octyl-dodecyl myristate, ethyl-2-hexyl palmitate, octyl-2-dodecyl stearate, octyl-2-dodecyl erucate, isostearyl hydroxy esters of isostearate, such as isostearyl lactate, octyl hydroxystearate, octyl dodecyl hydroxystearate, diisostearyl malate, triisoceryl citrate, heptanoate, octanoate, decanoate of fatty alcohols; polyol esters, such as propylene glycol dioctanoate, neopentyl glycol diheptanoate and diethylene glycol diisononanoate; and pentaerythritol esters, such as pentaerythritol tetrabenzoate (DUB PTB) or pentaerythritol tetraisostearate (Prisorin 3631);
[0165] - Straight-chain or branched hydrocarbons of mineral or synthetic origin, such as paraffin oils (whether volatile or not) and their derivatives, petrolatum, polydecene, hydrogenated polyisobutylene such as Parleam oil;
[0166] -Silicone oils, such as volatile or non-volatile polymethylsiloxanes (PDMS) having straight or cyclic siloxane chains, which are liquid or paste at room temperature, particularly cyclic polydimethylsiloxanes (cyclomethylsilicones), such as cyclohexylsiloxane and cyclopentylsiloxane polydimethylsiloxane (or polydimethylsiloxane), which contain alkyl, alkoxy, or phenyl groups having 2 to 24 carbon atoms during or at the end of the siloxane chain; phenylened polysiloxanes, such as phenyl polytrimethylsiloxane, phenyl polydimethylsiloxane, phenyltrimethylsiloxydiphenylsiloxane, diphenyl polydimethylsiloxane, diphenylmethyldiphenyltrisiloxane, 2-phenylethyltrimethylsiloxysilicate, and polymethylphenylsiloxane;
[0167] - Fatty alcohols having 8 to 26 carbon atoms, such as cetyl alcohol, stearyl alcohol and mixtures thereof (cetylstearyl alcohol) or octyldodecanool;
[0168] - Certain hydrocarbons and / or silicone fluorinated oils, as described in JP-A-2-295912;
[0169] - and its mixtures.
[0170] Preferably, the fatty phase of the dispersion according to the invention comprises at least one vegetable oil.
[0171] Plant-derived hydrocarbon oils include triglycerides of caprylic and capric acids, triglycerides of caprylic, capric, and capric acids (also known as "MCT oil"), triglycerides of myristic and stearic acids (INCI name: caprylic / capric / myristic / stearic acid triglycerides), triethylhexanoate, meadowfoam seed oil (INCI name: meadowfoam (Limnanthes Alba) seed oil), macadamia nut oil (INCI name: macadamia nut seed oil), rosehip oil (INCI name: rosehip oil), soybean oil (INCI name: wild soybean (soybean) oil), sunflower seed oil (INCI name: sunflower (Helianthus Annuus) seed oil), tri-mountain yam extract (INCI name: tri-mountain yam extract), triisostearin (INCI name: triisostearin), and almond oil (INCI name: almond (Prunus)). Armeniaca (almond) kernel oil, rice bran oil (INCI name: rice bran oil), argan oil (INCI name: Argania spinosa kernel oil), avocado oil (INCI name: Persea Gratissima oil), evening primrose oil (INCI name: Oenothera Biennis oil), rice germ oil (INCI name: rice germ oil), hydrogenated coconut oil (INCI name: hydrogenated coconut oil), sweet almond oil (INCI name: Prunus Amygdalus Dulcis oil), sesame seed oil (INCI name: Sesamum Indicum seed oil), hydrogenated rapeseed oil (INCI name: hydrogenated rapeseed oil), safflower seed oil (INCI name: Carthamus Tinctorius seed oil), Queensland nut oil, macadamia nut oil (INCI name: macadamia nut seed oil), caprylic acid glycerides (or triacylglycerols), wheat germ oil (INCI name: wheat Triticum... Vulgare wheat germ oil, borage seed oil (INCI name: Borago Officinalis seed oil), shea butter oil (INCI name: Butyrospermum Parkii oil), hydrogenated castor oil (INCI name: hydrogenated castor oil), Chinese rapeseed oil (INCI name: Brassica Campestris seed oil), camellia oil.In particular, Japanese camellia seed oil (INCI name: Camellia Japonica seed oil), green tea seed oil (INCI name: Camellia Sinensis seed oil), sea buckthorn oil (INCI name: Hippophae Rhamnoides oil), camellia seed oil (INCI name: Camellia oleifera seed oil), moringa seed oil (INCI name: Moringa Pterygosperma seed oil), rapeseed oil (INCI name: rapeseed oil), tea seed oil (INCI name: Camellia Oleifera seed oil), and carrot seed oil (INCI name: Daucus carotenoides seed oil). Carota Sativa seed oil, triheptanoic acid glycerides (INCI name: triheptanoic acid glycerides), vanilla oil (INCI name: vanilla (Planifolia) fruit oil), rapeseed oil glycerides and phytosterols (INCI name: phytosterol low erucic acid rapeseed oil glycerides), blackcurrant seed oil (INCI name: blackcurrant (Ribes Nigrum) seed oil), Pongamia glabra seed oil (INCI name: Indian Pongamia glabra seed oil), Bixaorella oil (INCI name: Bixaorella (annatto) oil), and mixtures thereof.
[0172] Preferably, the oil is selected from vegetable oils rich in polyunsaturated fatty acids. For the purposes of this invention, "unsaturated fatty acid" means a fatty acid comprising at least one double bond. According to a preferred embodiment, unsaturated fatty acids having 18 to 22 carbon atoms, particularly polyunsaturated fatty acids, especially ω-3 and ω-6 fatty acids, are used as the oil.
[0173] Advantageously, the adipose phase comprises at least one oil with a refractive index close to that of the continuous aqueous phase, i.e., an oil with a refractive index preferably 1.2-1.6, more preferably 1.25-1.5, and particularly 1.3-1.4 at room temperature and atmospheric pressure. This method is advantageous because it improves the transparency of the adipose phase and thus improves the transparency of the dispersion according to the invention. Transparency can be defined according to the method described in WO2018 / 167309. Advantageously, the oil with a refractive index of 1.2-1.6 is a silicone oil, particularly a phenylenedilicate silicone oil.
[0174] Advantageously, the fatty phase of the dispersion according to the invention comprises at least one or even at least two oils, said oils preferably selected from plant-derived hydrocarbon oils, and more preferably selected from meadowfoam (Limnanthes Alba) seed oil (INCI name: Meadowfoam (Limnanthes alba) seed oil), caprylic triglyceride, caprylic triglyceride, and mixtures thereof.
[0175] Preferably, the oil present in the fatty phase of the dispersion according to the invention is not silicone oil or fluorinated oil. Preferably, the dispersion according to the invention, particularly the dispersion of the fatty phase, does not contain polydimethylsiloxane (PDMS or polydimethylsiloxane) or its derivatives, and preferably does not contain silicone oil, particularly octamethylcyclotetrasiloxane (or cyclotetrasiloxane or D4), decamethylcyclopentasiloxane (or cyclopentasiloxane or D5), and cyclohexasiloxane (or D6).
[0176] Those skilled in the art will take note of selecting oils and / or their amounts to satisfy the aforementioned melting point and physicochemical properties x and y, or even z, of the aliphatic phase. These adjustments are within the capabilities of those skilled in the art in relation to the teachings of this specification.
[0177] Based on the total weight of the fatty phase, the dispersion according to the invention may comprise 10-99.5 wt%, preferably 20-90 wt%, more preferably 30-85 wt%, and particularly 50-80 wt% oil.
[0178] The dispersion according to the invention may comprise 1-50 wt%, preferably 5-40 wt%, and advantageously 10-25 wt% oil relative to the total weight of the dispersion.
[0179] The dispersion according to the invention is also advantageous because its kinetic stability allows for a high percentage of dispersed fatty phase. Therefore, relative to the total weight of the dispersion, the dispersion according to the invention may comprise 1-60 wt%, particularly 5-50 wt%, preferably 10-40 wt%, more preferably 15-30 wt% of dispersed fatty phase.
[0180] Other compounds
[0181] The dispersions according to the invention, particularly the continuous aqueous phase and / or dispersed fatty phase, may also include at least one additional compound different from the lipophilic gelling agent and the oils described above.
[0182] As additional compounds, the dispersions according to the invention, particularly the continuous aqueous phase and / or dispersed fatty phase, may also include powders; fillers; flakes; colorants, particularly selected from water-soluble or insoluble, fat-soluble or insoluble, organic or inorganic colorants, optical effect materials, liquid crystals and mixtures thereof; granules insoluble in the fatty phase; preservatives; humectants; fragrances, particularly as defined in WO2019002308; stabilizers; chelating agents; emollients; modifiers selected from gelling / texturing agents, viscosity modifiers different from the above-mentioned lipophilic gelling agents, pH, penetration strength and / or refractive index modifiers, etc., or any commonly used cosmetic additives; and mixtures thereof.
[0183] Within the meaning of this invention, "filler" refers to colorless or white solid particles of any shape, in an insoluble form and dispersed in the medium of the composition. For both inorganic and organic properties, they enable the imparting of bulk or rigidity and / or softness and uniformity to the deposit, particularly in cosmetic environments, and improved stability regarding exudation and non-migration properties upon application and / or matting and / or covering.
[0184] For the purposes of this invention, "particulates insoluble in the fatty phase" refers to the group consisting of pigments, ceramics, polymers, particularly acrylic polymers, and mixtures thereof.
[0185] As an additional compound, the dispersions according to the invention, particularly the continuous aqueous phase and / or dispersed fatty phase, may also include at least one bioactive / cosmetic ingredient, particularly selected from moisturizers, healing agents, decolorizing agents, UV filters, peeling agents, antioxidants, active ingredients that stimulate the synthesis of macromolecules in the dermis and / or epidermis, skin astringents, antiperspirants, soothing agents and / or anti-aging agents, and mixtures thereof. Such advantages are particularly described in FR1558849.
[0186] hydrophilic gelling agent
[0187] Advantageously, the aqueous phase may also include at least one hydrophilic gelling agent, i.e., one that is soluble or dispersible in water. In the context of this invention, the term "hydrophilic gelling agent" may be used interchangeably with "hydrophilic texturer." Hydrophilic gelling agents allow for the adjustment of the flowability of the dispersion, thereby modulating the desired sensory and / or Galenic properties, and / or contributing to further improvement of the kinetic stability of the dispersion.
[0188] Hydrophilic gelling agents include:
[0189] - Natural gelling agents, particularly those selected from algae extracts, plant exudates, seed extracts, and microbial exudates, such as alkasealan (INCI: Alcaligenes polysaccharide) sold by Hakuto, and other natural agents, especially hyaluronic acid.
[0190] - Semi-synthetic gelling agents, particularly those selected from cellulose derivatives and modified starches,
[0191] - Synthetic gelling agents, particularly selected from homopolymers of (meth)acrylic acid or its esters, copolymers of (meth)acrylic acid or its esters, copolymers of AMPS (2-acrylamido-2-methylpropanesulfonic acid), and associative polymers.
[0192] - Other gelling agents, especially those selected from polyethylene glycol (sold under the name Carbowax), clay, silica, etc., such as those listed under the name... Glycerin sold in 90 / 130 / 150 / 200 / 300 / 380 quantities, and
[0193] - Its mixture.
[0194] Within the meaning of this invention, "associative polymer" refers to any amphiphilic polymer whose structure includes at least one aliphatic chain and at least one hydrophilic moiety; the associative polymers according to the invention can be anionic, cationic, nonionic, or amphoteric; these are particularly those described in FR2999921. Preferably, these are amphiphilic and anionic associative polymers, as well as amphiphilic and nonionic associative polymers, as described below.
[0195] These hydrophilic gelling agents are described in more detail in FR3041251.
[0196] According to one embodiment, the dispersion according to the invention comprises 0.0001-20 wt%, preferably 0.001-15 wt%, particularly 0.01-10 wt%, and more preferably 0.1-5 wt% of a hydrophilic gelling agent relative to the continuous aqueous phase. These percentages refer to the hydrophilic gelling agent present only in the continuous aqueous phase.
[0197] In one embodiment, the dispersion according to the invention comprises 0.0001-20 wt%, preferably 0.001-15 wt%, and more preferably 0.01-10 wt% of another compound relative to the total weight of the dispersion.
[0198] Of course, those skilled in the art will take note of selecting possible additional compounds and / or their amounts such that the advantageous properties of the dispersion according to the invention, particularly its kinetic stability, and with respect to the dispersed aliphatic phase, its melting point and its aforementioned physicochemical properties x and y, or even z, are not, or substantially not, altered by the planned addition. In particular, the properties and / or amounts of the additional compounds depend on the aqueous or aliphatic nature of the phase under consideration in the dispersion according to the invention and / or must take into account the method employed to produce the dispersion according to the invention (particularly of “non-microfluidic” or “microfluidic” types). These selections and modifications are within the capabilities of those skilled in the art.
[0199] Preparation method
[0200] The dispersion according to the present invention can be prepared by different methods.
[0201] Therefore, the dispersion according to the invention has the following advantages: it can be prepared by a simple “non-microfluidic” method, i.e. by simple emulsification, especially by means of a Rayneri-type stirring device or a paddle stirrer.
[0202] In conventional emulsions, aqueous and fat solutions are prepared separately. A direct emulsion is produced by adding the fat phase to the aqueous phase under stirring.
[0203] The viscosity of the aqueous phase can be controlled, in particular, by adjusting the amount of hydrophilic gelling agent and / or the pH of the solution. Typically, the pH of the aqueous phase is below 4.5, which may require the addition of a third sodium bicarbonate solution (BF) as a final step to achieve a pH of 5.5 to 6.5.
[0204] The viscosity of the aqueous phase and the shear force applied to the mixture are two main parameters affecting the droplet size and monodispersity in an emulsion.
[0205] Those skilled in the art will know how to adjust the parameters of non-microfluidic methods to achieve the dispersion according to the invention, particularly to meet the required droplet diameter criteria.
[0206] The dispersion according to the invention can also be prepared by microfluidic methods, particularly as described in applications WO2012 / 120043 or WO2019 / 145424. According to this embodiment, the implemented microfluidic nozzle can have a configuration based on a T-shaped, co-current flow, or flow-focusing geometry.
[0207] According to this embodiment, the droplets obtained by this microfluidic method advantageously have a uniform size distribution.
[0208] Preferably, the dispersion of the present invention consists of a group of monodisperse droplets, particularly such that their average diameter... The range is 100-3,000 μm, especially 500-3,000 μm, and the coefficient of variation Cv is less than 10%, or even less than 3%.
[0209] In the context of this specification, "monodispersive droplet" refers to a group of droplets of the dispersion according to the invention having a uniform size distribution. Monodisperse droplets have good monodispersity. Conversely, droplets with poor monodispersity are referred to as "polydisperse".
[0210] One method involves measuring the average diameter D of a batch of N droplets by analyzing photographs of the droplets using image processing software (Image J). Typically, in this method, the diameter is measured in pixels and then reported in μm, depending on the size of the container containing the dispersed droplets.
[0211] Preferably, the value of N is chosen to be greater than or equal to 30, such that the analysis reflects the droplet diameter distribution of the emulsion in a statistically significant manner. N is advantageously greater than or equal to 100, especially when the dispersion is polydisperse.
[0212] The diameter Di of each droplet is measured, and the average diameter is obtained by calculating the arithmetic mean of these values.
[0213]
[0214] From these Di values, the standard deviation σ of the droplet diameter of the dispersion can also be obtained:
[0215]
[0216] The standard deviation σ of a dispersion reflects the droplet diameter Di within the dispersion relative to the average diameter. The surrounding distribution.
[0217] The average diameter of the dispersion is known. And the standard deviation σ can determine the diameter range 95.4% of the droplet population was found within this range, and within this range The study found that 68.2% of the population was affected.
[0218] To characterize the monodispersity of the dispersion according to this invention, the coefficient of variation is:
[0219]
[0220] This parameter reflects the distribution of droplet diameter relative to the average droplet diameter.
[0221] According to this mode of the invention, the coefficient of variation Cv of the droplet diameter is less than 10%, preferably less than 5%, or even less than 3%.
[0222] Alternatively, monodispersity can be demonstrated by placing a sample of the dispersion in a vial with a constant circular cross-section. Gentle stirring is performed by rotating the vial about a quarter turn for half a second, followed by the remaining half second, and then repeating this process four times in the opposite direction.
[0223] When monodispersed, the droplets of the dispersed phase are organized in a crystalline form. Therefore, they stack in a pattern that repeats itself in three dimensions. Regular stacking (indicating good monodispersity) and irregular stacking (indicating polydispersity of the dispersion) can then be observed.
[0224] To obtain monodisperse droplets, microfluidics can also be used (Utada et al., Materials Research Society Bulletin 32, 702-708 (2007); Cramer et al., Chemical Engineering Science 59, 15, 3045-3058 (2004)), and more specifically, co-current (fluids travel in the same direction) or flow-focused (fluids travel in different directions and usually in opposite directions) microfluidic systems.
[0225] The presence of lipophilic gelling agents in the dispersed fatty phase, or even in the continuous aqueous phase, may necessitate adjustments to the method used to prepare the dispersion according to the invention. Specifically, the method for preparing such a dispersion according to the invention comprises the step of heating the fatty phase (50°C to 150°C, particularly 60°C to 90°C) at least before mixing / contacting the fatty phase with the aqueous phase, and, if necessary, (i) maintaining this heating during stirring in the case of a “non-microfluidic” method, or (ii) maintaining this heating at the level of a microfluidic system in the case of a “microfluidic” method, until the desired dispersion is obtained.
[0226] The method for preparing the dispersion of the present invention includes at least the following steps:
[0227] a) Heating the oil fluid FI to 50-150°C, preferably 60-120°C, more preferably 70-100°C;
[0228] b) Optionally, the aqueous fluid FE is heated to 50-150°C, preferably 60-120°C, more preferably 70-100°C;
[0229] c) Contacting the aqueous fluid FE and the oily fluid FI; and
[0230] d) Forming droplets of an oily phase composed of the aqueous phase FE dispersed in a continuous aqueous phase.
[0231] in:
[0232] - The oily fluid FI comprises at least one lipophilic gelling agent and optionally at least one oil, and has a melting point of 50-100°C, preferably 60-90°C, and meets the following physicochemical criteria at room temperature and atmospheric pressure:
[0233] - The hardness (x) is 2-14 N, preferably 2.5-12 N, more preferably 3-9 N, and most preferably 4-6 N; and
[0234] - Adhesion (y) is greater than or equal to -2N, or better, greater than or equal to -1N, and particularly greater than or equal to -0.6N;
[0235] The oily fluid FI also does not contain amino-terminated polydimethylsiloxane, and optionally further includes at least one additional compound as described above; and
[0236] The aqueous fluid FE comprises at least water and optionally at least one other compound as described above, and preferably at least one hydrophilic gelling agent.
[0237] Steps (c) and (d) are carried out at a temperature equal to or higher than the melting point of the gelling agent used. In other words, steps (c) and (d) are carried out with an oily fluid FI that can be emulsified with the aqueous fluid FE and thus ensures the formation of droplets, particularly with an oily fluid FI in liquid form.
[0238] According to one embodiment, the fluid FI is initially prepared by mixing a fatty phase intended to form droplet cores, the fatty phase comprising at least one lipophilic gelling agent and optionally at least one oil and also optionally at least one other compound as described above.
[0239] According to one embodiment, the fluid FE is initially prepared by mixing an aqueous phase intended to form the dispersion with optionally at least one alkali, at least one other compound, a preservative and / or other water-soluble product such as glycerol, and most particularly at least one hydrophilic gelling agent.
[0240] In one embodiment, the continuous aqueous phase of the formed dispersion comprises or is represented by an aqueous fluid FE.
[0241] According to one embodiment, the method for preparing the dispersion according to the invention may further include the step e) of injecting a thickening solution of the continuous aqueous phase of the FE fluid, for example as described in WO2015 / 055748. Preferably, the thickening solution is aqueous. Typically, the thickening solution is injected into the aqueous fluid FE after the dispersion according to the invention has been formed, and therefore after the droplets have been formed.
[0242] According to one embodiment, the thickening solution comprises an alkali, particularly an alkali metal hydroxide, such as sodium hydroxide.
[0243] In the case of the “non-microfluidic” method described above, step c) is represented by stirring, during which heating can be maintained to obtain the desired dispersion.
[0244] In the case of the “microfluidic” method described above, the microfluidic system itself can be adapted to be maintained at a temperature of 50°C to 150°C, preferably 80°C to 90°C.
[0245] In the case of the "microfluidic" method, droplet formation step d) may include forming a droplet of the oily fluid FI at the outlet of a first conduit leading to the aqueous fluid FE. Preferably, the aqueous fluid FE circulates in a second conduit, the outlet of the first conduit leading to the second conduit, advantageously coaxial with a local axis of the second conduit.
[0246] Advantageously, the method of the present invention may include a cooling step f) after step d) but before step e) to accelerate the cooling kinetics of the formed dispersion and thus prevent the risk of subsequent droplet aggregation and fragmentation (10°C to 30°C).
[0247] The present invention also relates to dispersions that can be obtained by, for example, the methods described above.
[0248] use
[0249] Preferably, the dispersion according to the invention can be used directly as a composition, particularly a cosmetic composition, after the above-described preparation method. When prepared by the microfluidic method as described above, the dispersion according to the invention can also be used as a composition, particularly a cosmetic composition, after droplet separation and subsequent redispersion in a suitable second phase.
[0250] The present invention also relates to the use of the dispersion according to the invention in the preparation of compositions, particularly cosmetic, pharmaceutical, nutritional or agro-food compositions, preferably cosmetic compositions, particularly compositions for care and / or cosmetic keratin materials, especially for the skin.
[0251] Therefore, the present invention also relates to a composition, particularly a cosmetic composition, particularly for the care and / or makeup of keratin materials, especially for skin and / or hair, more particularly for skin, comprising at least one dispersion according to the invention, optionally in combination with at least one physiologically acceptable medium.
[0252] Therefore, the dispersions or compositions according to the present invention can be used particularly in the cosmetics field.
[0253] In addition to the aforementioned components or compounds, they may also include at least one physiologically acceptable medium.
[0254] The physiologically acceptable medium is generally suitable for the properties of the matrix to which the composition is to be applied, and for the appearance of the composition to be packaged.
[0255] In one embodiment, the physiologically acceptable medium is directly represented by a continuous aqueous phase as described above.
[0256] In the context of this invention, unless otherwise stated, "physiologically acceptable medium" means a medium suitable for cosmetic applications, particularly suitable for applying the compositions of this invention to keratin materials, especially skin and / or hair, and more particularly skin.
[0257] The cosmetic compositions of this invention can be, for example, creams, lotions, serums and gels, foundations (liquids, pastes) for skin (hands, face, feet, etc.), bath and shower preparations (salts, foams, oils, gels, etc.), hair care products (hair dyes and bleaches), cleansing products (lotions, powders, shampoos), hair cleaning products (lotions, creams, oils), hair styling products (lotions, hairsprays, shine agents, etc.), shaving products (soaps, foams, lotions, etc.), products applied to the lips, sunscreen products, and tanning products that do not require sun exposure. Skin whitening products and anti-wrinkle products are also possible. In particular, the cosmetic compositions of this invention can be anti-aging serums, youth serums, moisturizing serums, or perfumes.
[0258] Therefore, in view of the foregoing, the dispersion or composition according to the present invention is for oral or topical use, preferably topical, more preferably topical on keratinous materials, particularly on the skin, and more preferably on facial skin.
[0259] The present invention also relates to a non-therapeutic method for cosmetic treatment of keratin materials, particularly skin and / or hair, more particularly skin, comprising the step of applying at least one of the above-described dispersions or at least one of the above-described cosmetic compositions to the keratin material.
[0260] The present invention also relates to the use of dispersions or compositions according to the invention for improving the surface appearance of skin, particularly for moisturizing skin and / or reducing fine lines and wrinkles.
[0261] Throughout this specification, unless otherwise stated, the phrase "comprising one" should be understood as synonymous with "comprising at least one". Unless otherwise stated, the terms "between... and...", "from... to...", and "ranging from... to..." should be understood to include both low and high numbers. Unless otherwise stated, the amounts of ingredients in the examples are expressed as weight percentages relative to the total weight of the composition.
[0262] The following examples illustrate the invention but do not limit its scope. Example
[0263] Example 1: Physicochemical study of an aliphatic phase including at least one lipophilic gelling agent
[0264] This embodiment includes the preparation of 13 anhydrous gels of dispersed fatty phases capable of forming the dispersions of the present invention, and the evaluation of their physicochemical properties based on hardness (or firmness) (x), adhesiveness (y), and cohesiveness (z). These anhydrous gels are essentially in oil solvents and / or lipophilic gelling agents (e.g., Rheopearl D2 (equivalent to Rheopearl KL2), Estogel M, or OILKEMIA). TMThe properties of the 5S polymers and their concentrations (e.g., 5%, 10%, and 15%) differ. In the case of RheopearlD2, the difference between Test 1D and Test 1C lies in the nature of the solvent. Table 1 below shows the composition of these different anhydrous gels.
[0265] Table 1
[0266]
[0267] *QSF: Sufficient quantity
[0268] **EMC30 is a premix of Estogel M (INCI: castor oil / IPDI copolymer (and) caprylic / capric triglyceride) in caprylic / capric triglyceride oil at a ratio of 30 / 70; therefore, based on the total weight of the anhydrous gel, the corresponding concentrations of the lipophilic gelling agent (i.e., Estogel M) are 5% / 10% / 15%.
[0269] The preparation method for these anhydrous gels is as follows.
[0270] - Mixture A: The dye (if present) is pre-dispersed in a portion of Labrafac CC or DUB Inin. Heat the mixture to 50°C and mix with a magnetic stirrer.
[0271] -Mixture B: Stir the remaining solvent (Labrafac CC or DUB Inin) and heat to 80°C / 90°C, depending on the gelling agent to be dispersed; add the lipophilic gelling agent (e.g., Estogel M, Rheopearl D2, or OILKEMIA) at 80°C / 90°C with magnetic stirring. TM 5S polymer), until a homogeneous solution is obtained, thereby ensuring good dispersion of the polymer.
[0272] -Mixture C: Add meadowfoam oil or Lipex 205 or coconut oil to mixture B while stirring hot (80℃ / 90℃).
[0273] - Final mixture: Add mixture A to mixture C while hot-stirring (80°C / 90°C).
[0274] The melting point of the anhydrous gel was measured as described above, and the results are shown in Table 2 below.
[0275] Table 2
[0276]
[0277] The physicochemical standards x, y, and z of the anhydrous gel were then measured using the texture analyzer protocol described above. It should be noted that the hardness of the fatty phase could not be measured in Example 18 of US2004 / 137020 and Example 31 of EP2189081. These fatty phases are too hard for the Shimadzu EZ-X texture analyzer, with a maximum hardness of 50 N.
[0278] The corresponding measurements are as follows Figures 1 to 7 As shown.
[0279] Figure 1 This is a graph representing the hardness standard (x) of the anhydrous gel in Table 1.
[0280] Figure 2 This is a graph representing the adhesion standard (y) of hydrogel-free products in Table 1. Figure 3 The adhesiveness values (y) of the anhydrous gels 2A, 2B, 2C, 3A, 3B, 3C, 5, and 6 are... Figure 2 Enlarged image.
[0281] Figure 4 This is a graph showing the cohesiveness criteria (z) of the anhydrous gels 1B, 1D, 2B, 3B, 5 and 6 from Table 1.
[0282] at last, Figures 5 to 7 This is a graph representing the texture determination curves of the hydrogel-free gels in Table 1. These... Figures 5 to 7 The table shows the change in force (in N) of the gels in Table 1 over time (in seconds), during which the gels undergo (1) a first compression step (0 to 5 s) followed by (2) a second relaxation step, during which the moving body rises (5 to 10 s). Steps (1) and (2) are repeated. Therefore, these... Figures 5 to 7 Information on the physicochemical properties of the gels in Table 1 is provided, particularly regarding hardness, adhesion, and cohesion.
[0283] result:
[0284] Hardness (x): such as Figure 1 As shown, when the percentages of lipophilic gelling agent and oil solvent are the same (e.g., 1B vs. 2B vs. 3B), the differences in the hardness curves of the different anhydrous gels tested are not significant. Furthermore, tests 1C and 1D show that hardness is affected by the properties of the solvent.
[0285] Adhesion (y): such as Figure 2 and 3 As shown, when the percentages of lipophilic gelling agent and oil solvent are the same:
[0286] Gels 2 (A, B, C), 3 (A, B, C), 5, and 6 have similar adhesive properties, and
[0287] Gels 1 (B, C) and 4 showed significantly better adhesion than gels 2 (A, B, C) and 3 (A, B, C).
[0288] Furthermore, tests 1C and 1D showed that the properties of the solvent affect the viscosity.
[0289] Cohesion (z): such as Figure 4 As shown, gels 2B, 3B, 5, and 6 exhibit similar physicochemical properties in terms of cohesion, which are significantly lower than those of gels 1B and 1D.
[0290] Example 2: Preparation of macroscopic dispersion
[0291] In this Example 2, ten dispersions were prepared, comprising a continuous aqueous phase and a droplet-like dispersed phase, each represented by one of the anhydrous gels of Example 1. These dispersions were obtained using a microfluidic manufacturing method as described in WO2015 / 055748. The microfluidic system used consisted of two parts: a first part in which a fatty phase (also known as IF or FI) and an aqueous phase (also known as OF or FE) were contacted at a high temperature (70°C to 90°C) to form a dispersion; and a second part which ensured rapid cooling of the formed dispersion to accelerate the kinetics of droplet gelation, thereby preventing the risk of droplet aggregation and fragmentation after formation (10°C to 30°C).
[0292] The composition of the phase (fluid) used to prepare the dispersion is shown in Table 3 below.
[0293] Table 3
[0294]
[0295] *QSF: Sufficient quantity
[0296] Preparation method:
[0297] For OF:
[0298] -Mixture A: While stirring in a deflocculation centrifuge, phenoxyethanol, pentylene glycol and EDTA are added to water, and the resulting mixture is stirred for 5 minutes.
[0299] -Mixture B: Then spray Carbopol Ultrez 10 polymer carbomer onto Mixture A until hydrated, and then stir with a paddle for 30 minutes.
[0300] -Mixture C: Then disperse the Carbopol ETD 2050 polymer in Mixture B while stirring with a paddle for 30 minutes.
[0301] -Mixture D: While stirring in a deflocculation centrifuge, add the wetting agent (i.e., glycerol, zemea propylene glycol, and butylene glycol 1.3) to mixture C. Keep the resulting mixture D stirring for 10 minutes.
[0302] -Mixture E: After returning to room temperature, add 1% pre-dispersed blanose in water at 80°C with magnetic stirring to mixture D, while stirring in a deflocculation centrifuge.
[0303] -Mixture F: Add baking soda to mixture E and stir for 10 minutes to obtain OF solution.
[0304] The OF solution is then passed into the sOF injector connected to the heater to maintain OF heat (80°C).
[0305] For IFs: see the scheme described in Example 1.
[0306] Each of the ten heated IF solutions was then passed into an sIF injector connected to a heater to maintain the IF temperature (80°C). To minimize heat loss, the microfluidic system was mounted directly at the outlets of the sIF and sOF injectors and was itself maintained at 80°C.
[0307] For BF: Mix baking soda and water for 5 minutes with the help of a magnetic rod, then pass the BF solution into the sBF syringe.
[0308] Using sIF, sOF, and SBF syringes and associated syringe plungers, IF and OF are injected into the microfluidic system at the flow rates described in Table 4 below, and BF is injected into the dispersion at the outlet of the microfluidic system.
[0309] Table 4
[0310]
[0311] Depending on the microfluidic system's construction and flow rate, the resulting dispersion can include droplets with satisfactory monodispersity and an average diameter between 100 μm and 1500 μm, particularly between 700 μm and 1300 μm.
[0312] Results of dispersion preparation:
[0313] Dispersions can be prepared from the ten anhydrous gels according to Example 1.
[0314] Stability test
[0315] Each of the ten dispersions was then filled into three 30 mL polypropylene (PP) containers, each half-filled. After one day at room temperature, each test underwent one of the following three transport tests (one container per test):
[0316] - Roller test (i.e., horizontal circular motion): Wheaton reference, lasting 1 hour.
[0317] - Vibration table (i.e., vertical circular motion): Referencing the Haidorf Unimax 1010, continuous for 1 hour; and
[0318] -3D Mixer (i.e., random movement): lasts 6 minutes.
[0319] At the end of these stability tests, assess: (i) the integrity of the droplets, especially their fragmentation, and (ii) the turbidity of the gel, which is generally associated with the transfer of the fatty phase into the continuous aqueous phase.
[0320] Scoring criteria:
[0321] Table 5
[0322]
[0323]
[0324] result:
[0325] Table 6
[0326] Dispersion* D1A D1B D1C D1D D2A D2B D2C D3A D3B D3C 4 5 6 Bubble breaking 3 1 0 1 3 1 0 2 1 0 0 2 2 Gel turbidity 3 1 0 1 3 1 0 2 1 0 0 2 2 in conclusion KO OK KO OK KO OK OK OK OK OK OK OK OK
[0327] *D1A = Dispersion according to Example 2 using anhydrous gel 1A from Example 1 as the dispersion of the fatty phase.
[0328] Dispersions D1A and D2A showed unsatisfactory stability results. Therefore, the corresponding aliphatic phases were excluded from the remainder of the study. Dispersion D3A showed average stability results but was considered sufficiently satisfactory to be retained for further research. The other dispersions tested showed satisfactory stability results. These results indicate that the aliphatic phase must possess a hardness greater than 2 N, preferably greater than or equal to 2.5 N, particularly greater than or equal to 3 N, and more preferably greater than or equal to 4 N.
[0329] Sensory test
[0330] Then, based on the above eight dispersions exhibiting satisfactory stability, visual and sensory tests were conducted on 24 women aged 22 to 45 years. Each woman was blind-tested on the eight dispersions that demonstrated satisfactory kinetic stability. The evaluation criteria were: (i) adhesion of the dispersed fatty phase droplets to the packaging wall, and (ii) ease (or comfort) of the dispersed phase droplets aggregating and being applied, particularly the ease of droplet breakage and spreading.
[0331] Scoring criteria:
[0332] Table 7
[0333] result:
[0334] Table 8
[0335]
[0336] *D1A = Anhydrous gel 1A of Example 1 is implemented as a dispersion of the fatty phase according to Example 2.
[0337] **NR: No information.
[0338] Adipose phase was observed:
[0339] -In view of the ease of application and Figure 1 For the above results, the hardness (x) must be 14 N or less, preferably 12 N or less, and more preferably 9 N or less.
[0340] - In view of the "adhesion" aspect and Figure 2 and Figure 3 For the above results to be valid, the adhesion (y) of the adipose phase must be greater than or equal to -2N, and more preferably greater than or equal to -1N, or even greater than or equal to -0.6N.
[0341] - In view of the "gathering" aspect and Figure 4 Based on the above results, the cohesiveness (z) of the adipose phase must be less than or equal to 40, preferably less than or equal to 35, and more preferably less than or equal to 30.
[0342] in conclusion
[0343] In view of the above results,
[0344] It was observed that when the presence of a shell or surfactant at the "continuous aqueous phase / dispersed fatty phase" interface fails to ensure the stability of the dispersion, dispersions comprising both the droplet-containing dispersed phase and the continuous aqueous phase can still, and unexpectedly, exhibit satisfactory properties in terms of kinetic stability and sensory characteristics, particularly in terms of ease and comfort of application, provided that the gelling fatty phase has:
[0345] (i) a melting point of 50-100℃, preferably 60-90℃, and
[0346] (ii) At room temperature and atmospheric pressure:
[0347] -2-14N, particularly 2.5-12N, preferably 3-9N, more preferably 4-6N hardness (x);
[0348] - Greater than or equal to -2N, better yet greater than or equal to -1N, especially for adhesion (y) greater than or equal to -0.6N; and
[0349] - Optionally, cohesion (z) is less than or equal to 40, preferably less than or equal to 35, and more preferably less than or equal to 30.
[0350] Even more surprisingly, these results were observed and applied to dispersions of macroscopically dispersed fatty phase droplets.
Claims
1. A dispersion comprising a dispersed phase containing droplets and a continuous aqueous phase, wherein, The droplets comprise a fatty phase containing at least one lipophilic gelling agent, wherein: - The melting point of the aliphatic phase is 50-100℃, and it meets the following physicochemical standards at room temperature and atmospheric pressure: - Hardness (x) is 2-14 N; and - Adhesion (y) is greater than or equal to -2N; - The dispersion does not include amino-terminated polydimethylsiloxane; and The characteristic feature is that the dispersion does not contain a shell formed by a coagulated layer between the dispersed fatty phase and the continuous aqueous phase.
2. The dispersion according to claim 1, characterized in that, The cohesiveness (z) of the adipose phase is less than or equal to 40.
3. The dispersion according to claim 1, wherein, The volume of the droplets with a diameter greater than or equal to 100 μm is greater than or equal to 60% of the total volume of the dispersed phase, and / or at least 60% of the droplets have an average diameter greater than or equal to 100 μm.
4. The dispersion according to claim 1, characterized in that, The lipophilic gelling agent is selected from organic or inorganic, polymeric or molecular lipophilic gelling agents; solid fats under ambient temperature and pressure; and mixtures thereof.
5. The dispersion according to any one of the preceding claims, comprising 0.5-30 wt% of a lipophilic gelling agent relative to the total weight of the fatty phase.
6. The dispersion according to claim 1, characterized in that, The continuous aqueous phase includes at least one hydrophilic gelling agent.
7. The dispersion according to claim 6, comprising 0.0001-20 wt% of a hydrophilic gelling agent based on the total weight of the continuous aqueous phase.
8. The dispersion according to claim 1, comprising 1-60 wt% of a dispersed fatty phase relative to the total weight of the dispersion.
9. The dispersion according to claim 1, characterized in that, The dispersion does not contain surfactants.
10. The dispersion according to claim 1, characterized in that, The dispersion does not include: - Dextrin esters and fatty acids, and / or optionally hydrophobically treated silica, and / or - Acrylic ester / C10-30 alkyl acrylate crosspolymer, and / or - Cetyl ethylhexanoate.
11. A method for preparing the dispersion as described in claim 1, comprising at least the following steps: a) Heat the oily fluid FI to 50-150℃; b) Optionally, the aqueous fluid FE is heated to 50-150°C; c) Contact the aqueous fluid FE and the oily fluid FI; as well as d) Forming droplets of an oily phase composed of the aqueous phase FE dispersed in a continuous aqueous phase. in: - The oily fluid FI comprises at least one lipophilic gelling agent and optionally at least one oil, and has a melting point of 50-100°C, and meets the following physicochemical criteria at room temperature and atmospheric pressure: - Hardness (x) is 2-14 N; and - Adhesion (y) is greater than or equal to -2N; The oily fluid FI also does not contain amino-terminated polydimethylsiloxane; and The aqueous fluid FE comprises at least water and optionally at least one hydrophilic gelling agent.
12. The method according to claim 11, characterized in that, The droplet formation step includes forming a droplet of the oily fluid FI at the outlet of a first conduit leading to the aqueous fluid FE.
13. The method according to claim 12, characterized in that, The aqueous fluid FE circulates in the second conduit, and the outlet of the first conduit leads to the second conduit.
14. The dispersion obtained by the method of claim 11.
15. A composition comprising at least one dispersion as claimed in claim 1, optionally in combination with at least one physiologically acceptable medium.
16. A non-therapeutic method for cosmetic treatment of keratin materials, comprising the step of applying at least one dispersion as claimed in claim 1 or a composition as claimed in claim 15 to said keratin material.
Citation Information
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