Process for preparing a solid cosmetic composition with stirring, and associated composition
The process for preparing solid cosmetic compositions using a mixing device with a specific agitator design addresses the issues of non-Newtonian behavior and dead zones, achieving homogeneous agitation and a stable composition.
Patent Information
- Application Number
- FR2023014298
- Authority / Receiving Office
- FR · FR
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-12-15
- Publication Date
- 2025-06-20
AI Technical Summary
Existing methods for preparing solid cosmetic compositions often result in non-Newtonian behavior during stirring, leading to the formation of zones without flow and non-uniform temperature distribution.
A process involving a specific mixing device with a tank and an agitator, where the agitator has a base and blades with a radial edge, allowing for consistent radial distance from the side wall and blade height greater than 80% of the tank height, to enhance homogeneous agitation and prevent dead zones.
The process effectively limits the appearance of dead zones and ensures homogeneous agitation, resulting in a more uniformly mixed and stable solid cosmetic composition.
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Abstract
Description
Title of the invention: Process for preparing a solid cosmetic composition with stirring, and associated composition
[0001] The present invention relates to a process for preparing a solid cosmetic composition.
[0002] Cosmetic compositions intended for care and / or makeup and / or hair care, in particular for the lips, have been known for a very long time and come in increasingly varied forms, ranging from viscous fluid type formulas such as glosses, to solid compositions in the form of a stick, supported or not, compositions in the form of a pencil, or even compositions stored in pots.
[0003] The preparation method comprises, for example, at least one step of mixing several components together or of stirring a cosmetic mixture.
[0004] However, if, during stirring, the mixture exhibits non-Newtonian behavior, modifying the stirring parameters is not always sufficient to obtain satisfactory homogenization of the mixture.
[0005] Zones of no flow are likely to occur, and the temperature is likely to be non-uniform within the composition.
[0006] The aim of the invention is then to propose a process for preparing a solid cosmetic composition with stirring in which the appearance of non-flowing zones is limited.
[0007] For this purpose, the subject of the invention is a method for preparing a solid cosmetic composition, comprising a step of stirring a cosmetic mixture in a mixing device, the mixing device comprising a tank and an agitator, the tank defining a volume and having a central axis, the agitator having an axis of rotation and being capable of rotating about the axis of rotation in the tank about the central axis, the tank comprising a bottom and at least one side wall, the agitator comprising a base and at least one blade, the base extending opposite the bottom of the tank, the at least one blade having a radial edge extending opposite the side wall, the radial distance between the radial edge and the side wall being constant and non-zero over the entire length of the radial edge during the stirring step,at least one blade having a height measured parallel to the axis of rotation greater than or equal to 80% of the height of the tank measured along the central axis.
[0008] The base allows agitation with respect to the bottom and thus limits the appearance of a dead zone, i.e. without flow, at the bottom of the tank, while the height of the at least one blade allows agitation over the height of the tank and therefore limits the appearance of a dead zone at the top of the tank. In addition, the constant radial distance between the radial edge and the side wall allows for homogeneous agitation of the cosmetic mixture.
[0009] According to other advantageous aspects of the invention, the method comprises one or more of the following characteristics, taken in isolation or in all technically possible combinations:
[0010] - the radial distance between the radial edge and the side wall is less than or equal to 3 cm, preferably less than or equal to 2 cm, preferably less than or equal to 1 cm;
[0011] the relatively small radial distance between the radial edge and the side wall makes it possible to limit the risk of a dead zone appearing on the edges of the tank,
[0012] - the or each blade has a helix shape, the helix having a helix angle measured relative to the direction of the axis of rotation, the helix angle preferably being between 20° and 60°, more particularly between 20° and 30°;
[0013] such a helix angle is particularly advantageous for agitating the cosmetic mixture, in particular for applying a desired shear to the cosmetic mixture, and for improving the efficiency of the agitator,
[0014] - the or each blade has a width measured in the radial direction relative to at the axis of rotation between 10% and 20% of the width of the tank measured perpendicular to the central axis;
[0015] such a blade width allows the rotation of the blade to cause a force on an increased portion of the interior volume of the tank, without preventing the movement of the cosmetic mixture in the tank,
[0016] - the base and the bottom are spaced, at any point of the base, by a smaller dimension or equal to 40mm, and preferably between 5mm and 15mm;
[0017] a small distance between the base and the bottom makes it possible to limit the risk of a dead zone appearing at the bottom,
[0018] - the base comprises a plurality of radial arms, each radial arm having a radial scraping surface;
[0019] the radial scraping surface makes it possible in particular to avoid the deposit of cosmetic mixture on the bottom of the tank,
[0020] - each radial arm has a height measured parallel to the axis of rotation greater than or equal to 10% of the height of the tank measured along the central axis;
[0021] such a height limits the stagnation of the cosmetic mixture with respect to the bottom, and therefore the appearance of a dead zone in a lower part of the tank,
[0022] - each radial arm has a height measured parallel to the axis of rotation greater than twice its thickness measured perpendicular to the radial scraping surface;
[0023] the orientation of each radial arm so that its height is greater than twice its thickness prevents stagnation of the cosmetic mixture at the bottom, without weighing down the agitator,
[0024] - the method comprises a step of heating the cosmetic mixture before the step stirring, and / or a packaging step in which the stirred cosmetic mixture is inserted into a container;
[0025] the heating step makes it possible, for example, to make the cosmetic mixture more fluid, and the conditioning step then allows the storage and distribution of the cosmetic mixture;
[0026] - the mixing device comprises a temperature probe adapted to measure the temperature at at least one point in the volume defined by the tank, preferably in a lower part of the volume defined by the tank;
[0027] the temperature probe makes it possible to check the temperature of the cosmetic mixture, in particular in relation to a set or desired temperature,
[0028] - the cosmetic mixture comprises a fatty phase comprising at least 0.1% in weight, preferably at least 0.5% by weight, preferably at least 1% by weight, preferably at least 2% by weight, preferably at least 5% by weight, preferably at least 6% by weight, preferably at least 7% by weight relative to the total weight of the composition of at least one wax, preferably whose melting point is greater than or equal to 45°C, preferably greater than or equal to 70°C;
[0029] - the wax with a melting point greater than or equal to 70°C is chosen from waxes of pa raffines, ozokerite, polymethylene waxes and polyethylene waxes; preferably the wax with a melting point greater than or equal to 70°C is an apolar hydrocarbon wax, preferably a polyethylene wax, and said apolar hydrocarbon wax represents at least 50% by weight relative to the total weight of wax(es) of the fatty phase;
[0030] - the cosmetic mixture comprises a fatty phase further comprising at least a hydrophobic film-forming hydrocarbon resin, and / or at least one silicone resin and / or at least one polar or non-polar oil;
[0031] - the cosmetic mixture comprises an aqueous phase dispersed in the phase fat;
[0032] - the cosmetic mixture comprises at least one coloring matter and / or at least one active, preferably the coloring matter is chosen from water-soluble or fat-soluble dyes, pigments, pearlescent agents and their mixtures; and / or
[0033] - the mixing device comprises a cover, the cover being movable between a tank closed position, in which the volume defined by the tank is closed, and a tank open position, in which the volume defined by the tank is accessible, the agitator extending projecting from the cover and being able to rotate relative to the cover.
[0034] The invention also relates to a cosmetic composition obtained directly by a preparation process as defined above.
[0035] The invention will appear more clearly on reading the description which follows, given solely by way of non-limiting example, and made with reference to the drawings in which:
[0036] [Fig-1] [Fig.l] is a three-dimensional view of an example of a device for mixture of a method according to one embodiment of the invention.
[0037] The invention relates to a method for preparing a solid cosmetic composition, comprising a step of stirring a cosmetic mixture in a mixing device.
[0038] By "solid" is meant that the composition does not flow under its own weight. Preferably, the cosmetic composition is a makeup or care composition, or a hair composition, for example a shampoo or a conditioner. Preferably, the cosmetic composition is a makeup composition, preferably a lip makeup composition, preferably a lipstick.
[0039] The cosmetic composition comprises, for example, a continuous fatty phase.
[0040] The invention also relates to a cosmetic composition obtained directly by a preparation process according to the invention.
[0041] The stirring step allows, for example, the application of shear to the mixture being stirred, said shear being, for example, carried out at a shear rate ranging from 10 to 600 s1, preferably ranging from 50 to 300 s1. Depending on the size and geometry of the tank used, the shear rate is likely to vary.
[0042] During the stirring step, the cosmetic mixture has, for example, a viscosity greater than or equal to 0.1 Pa.s, in particular in the absence of shear.
[0043] The cosmetic mixture exhibits, for example, non-Newtonian behavior during stirring.
[0044] An example of a mixing device 10 used in the method of the invention is shown in [Fig.l].
[0045] The mixing device 10 comprises a tank 12 and an agitator 14.
[0046] The tank defines a volume 16 and has a central axis X.
[0047] Volume 16 is intended to receive the cosmetic mixture to be stirred.
[0048] The tank 12 comprises, more particularly, a bottom 18 and at least one side wall 20.
[0049] In the present example, the side wall 20 is a cylindrical wall with rotational symmetry around the central axis D.
[0050] The bottom 18 also has rotational symmetry around the central axis D.
[0051] The agitator 14 has an axis of rotation and is capable of rotating around the axis of rotation in the tank 12. During the rotation of the agitator 14 in the tank 12, the axis of rotation here coincides with the central axis X.
[0052] The agitator 14 comprises a base 22 and at least one blade 24.
[0053] The base 22 extends opposite the bottom 18 of the tank 12.
[0054] The base 22 and the bottom are, for example, spaced apart, at any point of the base 22, by a distance d less than or equal to 40 mm, and preferably between 5 mm and 15 mm.
[0055] The base 22 comprises, in the example shown, a plurality of radial arms 26, each radial arm 26 having a radial scraping surface 28.
[0056] Each radial arm 26 extends mainly in a direction perpendicular to the axis of rotation.
[0057] Each radial arm 26 here has a straight lower edge 30.
[0058] The lower edge 30 extends in a direction perpendicular to the axis of rotation.
[0059] The radial scraping surface 28 is here flat and extends in a perpendicular direction dicular to the axis of rotation and a direction parallel to the axis of rotation.
[0060] Each radial arm 26 has, for example, a height hb measured parallel to the axis of rotation greater than or equal to 10% of the height H of the tank 12 measured along the central axis.
[0061] Each radial arm 26 has, for example, a height hb measured parallel to the axis of rotation greater than twice its thickness measured perpendicular to the radial scraping surface 28.
[0062] The height hb is constant here.
[0063] Each radial arm and the bottom are spaced, at any point from the lower edge 30, by a dimension less than or equal to 40 mm, and preferably between 5 mm and 15 mm.
[0064] When the agitator 14 rotates in the tank 12, the radial arms 26 scrape the bottom 18 with a clearance, so as not to hinder the rotation by any possible friction between the bottom and the radial arms.
[0065] The radial arms are, for example, distributed regularly over the angular extent around the axis of rotation.
[0066] The base 22 is here connected to a central rod 31.
[0067] The central rod 31 extends along the axis of rotation.
[0068] The central rod 31 is, for example, included in the agitator.
[0069] Alternatively, the central rod 31 is fixed, the at least one blade 24 and the base 22 rotating around the central rod 31.
[0070] The central rod 31 extends here between a lower end and an upper end.
[0071] The base 22 is here connected to the lower end of the central rod 31.
[0072] The upper end of the central rod 31 is here connected to a motor (not shown) capable of driving the agitator in rotation.
[0073] In the example shown, the base comprises two radial arms 26.
[0074] The two radial arms 26 form an angle of 180° between them.
[0075] The at least one blade 24 has a radial edge 32 extending opposite the side wall 20.
[0076] The radial distance dr between the radial edge 32 and the side wall 20 is constant and non-zero over the entire length of the radial edge 32 when the agitator 14 is in the tank 12.
[0077] The radial distance dr is measured perpendicular to the central axis X, coincident with the axis of rotation.
[0078] The clearance between the radial edge 32 and the side wall 20 makes it possible not to hinder rotation by possible friction between the blade and the side wall.
[0079] The radial distance between the radial edge 32 and the side wall 20 is, for example, less than or equal to 3 cm, preferably less than or equal to 2 cm, preferably less than or equal to 1 cm.
[0080] In the example shown, the or each blade 24 has, for example, a propeller shape.
[0081] The propeller has a helix angle measured relative to the direction of the axis of rotation, the helix angle preferably being between 20° and 60°, more particularly between 20° and 30°.
[0082] The or each blade 24 extends here between a lower end 34 and an upper end 36.
[0083] The or each blade 24 has a height hp measured parallel to the axis of rotation greater than or equal to 80% of the height H of the tank 12 measured along the central axis.
[0084] The height hp of the or each blade 24 is equal to the distance in the direction parallel to the axis of rotation between the lower end 34 and the upper end 36.
[0085] The or each blade 24 has, for example, a width 1 measured in the radial direction relative to the axis of rotation comprised between 10% and 20% of the width L of the tank 12 measured perpendicular to the central axis X.
[0086] The width 1 is constant over the entire extent of the radial edge 32.
[0087] If the width is not constant over the entire extent of the radial edge 32, then the width considered is the average width of the blade.
[0088] The or each blade has an agitation surface 38.
[0089] The stirring surface 38 forms the upper surface of the blade.
[0090] The stirring surface 38 forms, at any point on the stirring surface, an angle with the direction of the axis of rotation equal to the helix angle.
[0091] The or each blade 24 has a thickness measured perpendicular to the stirring surface, the thickness of the or each blade 24 being less than half of the width 1 of said blade.
[0092] Each blade here comprises a lower portion, comprising the lower end 34, and an upper portion, comprising the upper end 36.
[0093] The lower portion is here connected to the central rod 31 by a radial element 40.
[0094] The upper portion is here connected to one of the radial arms 26 by a support element 42, here vertical.
[0095] There are, for example, as many blades as there are radial arms, the radial arms being arranged alternately with the lower ends of the blades.
[0096] In the example shown, the mixing device 10 comprises a plurality of, here two, blades 24.
[0097] The blades are distributed regularly over the angular extent around the axis of rotation.
[0098] The radial segment connecting the lower end 34 and the axis of rotation forms, for example, an angle with any radial arm 26 an angle between 80° and 100°.
[0099] Each radial element 40 forms with any radial arm 36 an angle between 80° and 100°, more particularly equal to 90°.
[0100] This allows for continuous homogenization during rotation of the agitator.
[0101] The agitator 14 is capable of rotating around the axis of rotation in a direction such that the upper end 36 of the or each moves towards the rest of said blade.
[0102] The agitator 14 is capable of rotating around the axis of rotation in a direction such that any radial surface which is not, initially, in contact with the or one of the blades comes into contact with the lower end 34 of said blade, then with the upper end of said blade.
[0103] In an advantageous embodiment, the mixing device 10 comprises a temperature probe 44 adapted to measure the temperature at at least one point of the volume defined by the tank 12, preferably in a lower part of the volume defined by the tank.
[0104] The lower part corresponds, for example, to the lower third of the volume of the tank from the bottom.
[0105] The mixing device 10 further comprises, for example, a cover 46.
[0106] The cover 46 is movable between a position for closing the tank 12 (visible in [Fig.l]), in which the volume defined by the tank is closed, and a position for opening the tank, in which the volume defined by the tank is accessible.
[0107] The cover 46 is, for example, also heated.
[0108] In the closed position of the tank 12, the agitator 14 extends into the closed volume of the tank.
[0109] In the closed position of the tank 12, the axis of rotation and the central axis X are merged.
[0110] The agitator 14 projects from the cover 46 and is capable of rotating relative to the cover 46, more particularly around the axis of rotation.
[0111] The agitator 14 is integral with the cover 46 for any movement other than rotation around the axis of rotation.
[0112] The agitator 14 moves with the cover 46 between the open position and the closed position.
[0113] In the open position, the agitator 14 extends at least partially outside the tank 12.
[0114] The agitator 14, more particularly the upper end of the central rod 31, is, for example, connected to the cover 46 by means of bearings.
[0115] The stirring step allows homogenization of the mixture, in particular by limiting the appearance of zones without flow, in particular of the temperature of the mixture within the tank.
[0116] The preparation method further comprises, for example, a step of heating the cosmetic mixture before the stirring step, and / or a packaging step in which the stirred cosmetic mixture is inserted into a container.
[0117] The heating step is, for example, carried out in a container different from the mixing device.
[0118] After heating, the cosmetic mixture is introduced into the tank 12 for the stirring step.
[0119] At the end of the stirring step, the tank is emptied of all of the cosmetic mixture, for example using a drain, which is then packaged in containers, in particular packaging devices.
[0120] The temperature at the temperature probe 44 is, for example, monitored while the tank is being emptied.
[0121] In a particular embodiment, the preparation method comprises the following steps:
[0122] a) a step of introducing into a tank a fatty phase comprising at least one fatty substance, at least partly solid at 25°C, chosen from waxes, pasties, and their mixtures,
[0123] b) a step of heating the fatty phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fatty substance(s),
[0124] c) optionally, a step of adding an aqueous phase to the fatty phase of step a) or to the heated fatty phase of step b), to obtain a composition cosmetic in the form of an emulsion, it being understood that when step c) is present, then step b) is carried out on the fatty phase obtained in a) or on the composition obtained in c),
[0125] d) a step of cooling the heated fatty phase obtained in b) or the composition obtained in c),
[0126] e) optionally, a step of remelting the cooled fatty phase obtained in d) or the cooled composition obtained in d),
[0127] wherein stirring is applied either during the cooling step d) or at the end of the remelting step e), said stirring being carried out until a target temperature is obtained within the fatty phase or the composition, said target temperature being less than 90% of the value of the melting point of the fatty substance having the highest melting point, and
[0128] f) a step of pouring the stirred fatty phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one container corresponding here to the packaging step.
[0129] Preferably, the method comprises the following steps:
[0130] a) a step of introducing into a tank a fatty phase comprising at least one fatty substance, at least partly solid at 25°C, chosen from waxes, pasties, and their mixtures,
[0131] b) a step of heating the fatty phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fatty substance(s),
[0132] c) optionally, a step of adding an aqueous phase to the heated fatty phase of step b), to obtain a cosmetic composition in the form of an emulsion,
[0133] d) a step of cooling the heated fatty phase obtained in b) or the composition obtained in c),
[0134] e) optionally, a step of remelting the cooled fatty phase obtained in d) or the cooled composition obtained in d),
[0135] wherein stirring is applied either during the cooling step d) or at the end of the remelting step e), said stirring being carried out until a target temperature is obtained within the fatty phase or the composition, said target temperature being less than 90% of the value of the melting point of the fatty substance having the highest melting point, and
[0136] f) a step of pouring the stirred fatty phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one container, corresponding here to the packaging step.
[0137] Alternatively, the cosmetic mixture is obtained by any other step of preparing a cosmetic mixture.
[0138] The steps of the particular embodiment will now be described in more detail. Step a)
[0139] The composition according to the invention comprises at least one fatty phase.
[0140] The fatty phase of the composition prepared in the particular embodiment comprises at least two fatty substances chosen from waxes and pastes and their mixtures.
[0141] The fatty substance considered is thus a fatty substance which is solid at an ambient temperature of 25°C.
[0142] The fatty phase according to the invention preferably comprises at least one wax or a mixture of waxes. Preferably, the fatty phase according to the invention comprises at least two waxes.
[0143] Preferably, the fatty phase of the composition prepared according to the invention comprises at least two fatty substances chosen from waxes, pasties and their mixtures.
[0144] According to a particular embodiment, a composition according to the invention comprises at least one wax and at least one pasty.
[0145] The first step of the process according to the invention, i.e. step a), is a step of introducing into a tank at least one, preferably at least two, fatty substances chosen from waxes, pasties and their mixtures.
[0146] Preferably, step a) is a step of introducing into a tank at least two fatty substances chosen from waxes. Preferably, step a) is a step of introducing into a tank at least two waxes having different melting points (Tm). Wax(s)
[0147] The wax(es) is (are) generally a lipophilic compound, solid at room temperature (25°C), with a reversible solid / liquid state change, having a melting point greater than or equal to 30°C and which can go up to 200°C and in particular up to 120°C.
[0148] Here, the melting temperature corresponds to the temperature of the most endothermic peak observed in thermal analysis (DSC) as described in the ISO 11357-3; 1999 standard. The melting point of the wax can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the name "DSC Q2000" by the company TA Instruments.
[0149] The measurement protocol is as follows:
[0150] A 5 mg sample of wax placed in a crucible is subjected to a first temperature rise ranging from -20°C to 120°C, at the heating rate of 10°C / minute, then is cooled from 120°C to -20°C at a cooling rate of 10°C / minute and finally subjected to a second temperature increase from -20°C to 120°C at a heating rate of 5°C / minute. During the second temperature increase, the following parameters are measured:
[0151] - the melting point (Tf) of the wax, as previously mentioned, corresponding to the temperature of the most endothermic peak of the observed melting curve, representing the variation of the difference in absorbed power as a function of temperature,
[0152] - AHf: the enthalpy of fusion of the wax corresponding to the integral of the whole of the melting curve obtained. This enthalpy of fusion of the wax is the amount of energy required to change the compound from the solid state to the liquid state. It is expressed in J / g.
[0153] The wax(es) may be hydrocarbon-based, fluorinated and / or silicone-based and be of plant, mineral, animal and / or synthetic origin.
[0154] A composition in accordance with the particular embodiment may comprise at least one wax selected from the group consisting of polar waxes, apolar waxes and their mixture.
[0155] Waxes are in particular those described in the document Ullmann's Encyclopedia of Industrial Chemistry 2015, Wiley-VCH Verlag GmbH & Co. KGaA,
[0156] Such waxes can in particular be natural but also synthetic.
[0157] By “natural” wax is meant any wax pre-existing in nature or capable of being transformed, extracted or purified from natural compounds existing in nature.
[0158] By “synthetic” wax is meant waxes whose synthesis requires one or more chemical reactions carried out by man.
[0159] Among the natural waxes, we can notably cite so-called fossil waxes including those of petroleum origin such as ozocerite, pyropissite, macrocrystalline waxes also called paraffins - including raw waxes or slack wax, slack wax raffinates, deoiled slack wax, soft waxes, semi-refined waxes, filtered waxes, refined waxes - and microcrystalline waxes called microwaxes including slack wax from "bright stock". Fossil waxes still contain lignite also called montan wax, or peat wax.
[0160] As natural waxes other than fossil waxes, we can cite animal and vegetable waxes.
[0161] Examples of vegetable waxes include carnauba wax, candelilla wax, ouricuri wax, sugarcane wax, jojoba wax, Trithrinax campestris wax, raffia wax, alfalfa wax, wax extracted from Douglas fir, sisal wax, flax wax, cotton wax, Batavia dammar wax, cereal wax, tea wax, coffee wax, rice wax, palm tree wax, Japanese wax and mixtures thereof.
[0162] Examples of animal waxes include beeswax, Ghedda wax, shellac, Chinese wax, lanolin also known as wool wax, their mixtures and their derivatives.
[0163] Mention may also be made of ester waxes such as waxes of formula RiCOOR2 in which Ri and R2 represent linear, branched or cyclic aliphatic chains whose number of atoms varies from 10 to 50, which may contain a heteroatom, in particular oxygen, and whose melting point temperature varies from 30 to 120°C, preferably from 30 to 100°C. In particular, a C2o-C4o alkyl (hydroxystearyloxy)stearate (the alkyl group comprising from 20 to 40 carbon atoms), alone or as a mixture, or a C2o-C4O alkyl stearate, may be used as ester wax. Such waxes are sold under the names "Kester Wax K 82 P", "Hydroxypolyester K 82 P", "Kester Wax K 80 P", or "KESTER WAX K82H" by the company KOSTER KEUNEN. Mixtures of C14-C18 carboxylic acid esters and alcohols can also be used, such as the products "Cetyl Ester Wax" from the company KOSTER KEUNEN, "SP Crodamol MS MB AL","Crodamol MS" from CRODA, "Miraceti" from LASERSON. It is also possible to use a glycol and butylene glycol montanate (octacosanoate) such as LICOWAX KPS FLAKES wax (INCI name: glycol montanate) marketed by Clariant. It is also possible to cite hydrocarbon waxes, polyoxyalkylenated or polyglycerolated, natural or synthetic, of animal or vegetable origin; the number of oxyalkylenated units (in C2-C4) can vary from 2 to 100, the number of glycerolated units can vary from 1 to 20. Examples include polyoxyethylenated beeswax, such as PEG-6 beeswax, PEG-8 beeswax; polyoxyethylenated carnauba waxes, such as PEG-12 carnauba; lanolin waxes, hydrogenated or not, polyoxyethenate or polyoxypropylene, such as PEG-30 lanolin, PEG-75 lanolin; PPG-5 lanolin wax glyceride; polyglycerolated beeswax,in particular polyglyceryl-3 Beewax; esters derived from waxes resulting from the reaction between vegetable waxes and a polyglycerol, preferably esters derived from the reaction between a mixture of jojoba, mimosa (Acacia Decurrens) and sunflower waxes and polyglycerol-3, for example the mixture Acacia Decurrens (Mimosa) / Jojoba / Sunflower Seed Wax Polyglyceryl-3 Esters sold under the name Hydracire S by the company Gattefossé, or the mixture Acacia Decurrens Flower Wax, Jojoba esters, Sunflower Seed Wax and Polyglycerin-3 sold in particular under the name Acticire MB by the company Gattefossé, and mixtures thereof.
[0164] Waxes that may also be mentioned are fatty alcohols that are solid at room temperature and that comprise from 14 to 22 carbon atoms, and more preferably from 16 to 18 carbon atoms. As particular examples of fatty alcohols that can be used, mention may in particular be made of stearyl alcohol, cetyl alcohol, myristyl alcohol and their mixtures. Preferably, cetostearyl alcohol (or cetearyl alcohol) can be used, which is a mixture of stearyl and cetyl alcohols.
[0165] Preferably, the composition comprises at least one apolar hydrocarbon wax.
[0166] By "apolar hydrocarbon wax" here, we mean a wax comprising only carbon or hydrogen atoms in its structure. In other words, such a wax is free of other atoms, in particular heteroatoms such as for example nitrogen, oxygen, silicon.
[0167] As an illustration of apolar waxes, mention may in particular be made of hydrocarbon waxes such as microcrystalline waxes, paraffin waxes, ozokerite, polymethylene waxes, polyethylene waxes, waxes obtained by Fischer-Tropsch synthesis, microwaxes, in particular polyethylene.
[0168] Preferably, the fatty phase of step a) comprises at least one wax having a melting point greater than or equal to 45°C. Preferably, the wax having a melting point greater than or equal to 45°C comprises at least one fatty alcohol.
[0169] Preferably, the lipophilic mixture of step a) comprises at least one wax having a melting point greater than or equal to 70°C. Preferably, the wax having a melting point greater than or equal to 70°C is chosen from paraffin waxes, ozokerite, polymethylene waxes and polyethylene waxes.
[0170] Preferably, the fatty phase of step a) comprises at least 0.1% by weight, preferably at least 0.5% by weight, preferably at least 1% by weight, preferably at least 2% by weight, preferably at least 5% by weight, preferably at least 6% by weight, preferably at least 7% by weight relative to the total weight of the mixture of at least one wax, preferably whose melting point is greater than or equal to 45°C, preferably greater than or equal to 70°C.
[0171] Preferably, the wax with a melting point greater than or equal to 70°C is an apolar hydrocarbon wax, preferably a polyethylene wax, and said apolar hydrocarbon wax represents at least 50% by weight relative to the total weight of wax(es) in the mixture. Pasty (or pasty fatty body)
[0172] By "pasty fatty body", here, is meant a lipophilic fatty compound with reversible solid / liquid state change, having in the solid state an anisotropic crystalline organization, and comprising at a temperature of 23°C a liquid fraction and a solid fraction.
[0173] In other words, the starting melting temperature of the pasty compound may be less than 23°C. The liquid fraction of the pasty compound measured at 23°C may represent 9 to 97% by weight of the compound. This liquid fraction at 23°C preferably represents between 15 and 85%, more preferably between 40 and 85% by weight.
[0174] The melting point of a solid fatty body can be measured using a calorimeter at differential scanning calorimeter (DSC), for example the calorimeter sold under the name “DSC Q100” by the company TA Instruments with the software “TA Universal Analysis”, according to the protocol defined previously.
[0175] The liquid fraction by weight of the pasty compound at 23°C is more particularly equal to the ratio of the enthalpy of fusion consumed at 23°C to the enthalpy of fusion of the pasty compound.
[0176] The enthalpy of fusion of the pasty compound is the enthalpy consumed by the compound to pass from the solid state to the liquid state. The pasty compound is said to be in the solid state when its entire mass is in crystalline solid form. The pasty compound is said to be in the liquid state when its entire mass is in liquid form.
[0177] The enthalpy of fusion of the pasty compound is in particular equal to the value under the curve of the thermogram obtained using a differential scanning calorimeter. The enthalpy of fusion of the pasty compound is the quantity of energy required to change the compound from the solid state to the liquid state. It is expressed in J / g.
[0178] The enthalpy of fusion consumed at 23°C is the quantity of energy absorbed by the sample to pass from the solid state to the state it presents at 23°C consisting of a liquid fraction and a solid fraction.
[0179] The pasty compound(s) may in particular be chosen from synthetic pasty compounds and fatty substances of plant origin. The pasty compound(s) may be hydrocarbon-based or silicone-based.
[0180] The pasty compound(s) may in particular be chosen from: - lanolin and its derivatives, such as lanolin alcohol, oxyethylenated lanolins, acetylated lanolin, lanolin esters such as isopropyl lanolate, oxypropylenated lanolins; - petroleum jelly (also called petrolatum), - polyol ethers chosen from pentaerythritol and C2-C4 polyalkylene glycol ethers, fatty alcohol and sugar ethers, and mixtures thereof. For example, mention may be made of pentaerythritol and polyethylene glycol ether comprising 5 oxyethylenated units (5 EO) (CTFA name: PEG-5 Pentaerythrityl Ether), pentaerythritol and polypropylene glycol ether comprising 5 oxypropylenated units (5 OP) (CTFA name: PPG-5 Pentaerythrityl Ether), and mixtures thereof, and more specifically the mixture of PEG-5 Pentaerythrityl Ether, PPG-5 Pentaerythrityl Ether and soybean oil, marketed under the name “Lanolide” by the company VEVY, a mixture in which the constituents are in a weight ratio of 46 / 46 / 8: 46% PEG-5 Pentaerythrityl Ether, 46% PPG-5 Pentaerythrityl Ether and 8% soybean oil, - polymeric or non-polymeric silicone compounds, polymeric or non-polymer fluorinated compounds, vinyl polymers, in particular: • homopolymers and copolymers of olefins, • homopolymers and copolymers of hydrogenated dienes, • linear or branched oligomers, homo or copolymers of alkyl (meth)acrylates preferably having a C8-C30 alkyl group, • homopolymer and copolymer oligomers of vinyl esters having C8-C30 alkyl groups, and • homopolymer and copolymer oligomers of vinyl ethers having C8-C30 alkyl groups, Liposoluble polyethers resulting from the polyetherification between one or more C2-C100, preferably C2-C50, diols. Among the liposoluble polyethers, particularly suitable are copolymers of ethylene oxide and / or propylene oxide with long-chain C6-C30 alkylene oxides, more preferably such that the weight ratio of ethylene oxide and / or propylene oxide with alkylene oxides in the copolymer is from 5:95 to 70:30. In this family, we will notably cite copolymers such as long-chain alkylene oxides arranged in blocks having an average molecular weight of 1000 to 10000, for example a block copolymer of polyoxyethylene / polydodecyl glycol such as the ethers of dodecanediol (22 mol) and polyethylene glycol (45 EO) marketed under the brand name ELFACOS ST9 by AKZO NOBEL. esters and polyesters. Among the esters, we consider in particular: • esters of a glycerol oligomer, in particular diglycerol esters, with optionally hydroxylated, linear or branched, saturated or unsaturated, preferably saturated, C6-C20 monocarboxylic acids, and / or linear or branched, saturated or unsaturated, preferably saturated, C6-C10 dicarboxylic acids, in particular condensates of adipic acid and diglycerol, for which a portion of the hydroxyl groups of the glycerols have reacted with a mixture of fatty acids such as stearic acid, capric acid, stearic acid, isostearic acid and 12-hydroxystearic acid, such as, for example, bis-diglyceryl polyacyladipate-2 marketed under the reference SOFTISAN® 649 by the company Sasol, • vinyl ester homopolymers having C8-C30 alkyl groups, such as polyvinyl laurate (notably sold under the reference Mexomère PP by the company Chimex), • arachidyl propionate marketed under the brand name Waxenol 801 by ALZO, • phytosterol esters, • fatty acid triglycerides and their derivatives, in particular fatty acid triglycerides, saturated or not, linear or branched, possibly mono or polyhydroxylated, in C6-C30, more particularly C8-C18, possibly hydrogenated (totally or partially); for example with Softisan 100® marketed by the company Sasol, • pentaerythritol esters, • aliphatic esters resulting from the esterification of an aliphatic hydroxycarboxylic acid ester with an aliphatic carboxylic acid. More particularly, the aliphatic carboxylic acid is C4-C30, preferably C8-C30. It is preferably chosen from hexanoic, heptanoic, octanoic, 2-ethylhexanoic, nonanoic, decanoic, undecanoic, dodecanoic, tridecanoic, tetradecanoic, pentadecanoic, hexadecanoic, hexyldecanoic, heptadecanoic, octadecanoic, isostearic, nonadecanoic, eicosanoic, isoarachidic, octyldodecanoic, heneicosanoic and docosanoic acids, and mixtures thereof. The aliphatic carboxylic acid is preferably branched.The hydroxycarboxylic acid ester is advantageously derived from a C2-C40, preferably C10-C34, and even more preferably C12-C28 hydroxylated carboxylic acid; the number of hydroxylated groups being between 1 and 20, more particularly between 1 and 10, preferably between 1 and 6.
[0181] Said hydroxycarboxylic acid esters are preferably chosen from:
[0182] a) total or partial esters of saturated, linear and monohydroxylated aliphatic monocarboxylic acids;
[0183] b) total or partial esters of saturated, monohydroxylated, monocarboxylic aliphatic acids;
[0184] c) total or partial esters of saturated, monohydroxylated polycarboxylic aliphatic acids;
[0185] d) total or partial esters of polyhydroxylated saturated aliphatic polycarboxylic acids;
[0186] e) partial or total esters of esters of C2-Ci6 aliphatic polyols with a mono or polyhydroxylated aliphatic acid
[0187] f) their mixtures. • dimer diol and dimer diacid esters, where appropriate, esterified on their free alcohol or acid function(s) by acid or alcohol radicals, in particular dimer dilinoleate esters; such esters may in particular be chosen from the esters with the following INCI nomenclature: bis-behenyl / isostearyl / phytosteryl dimer dilinoleyl dimer dilinoleate (Plandool G), phytosteryl / isosteryl / cetyl / stearyl / behenyl dimer dilinoleate (Plandool H or Plandool S) and mixtures thereof, • hydrogenated rosin esters (Lusplan DD-DHR or DD-DHR from Nippon Fine Chemical) • butters of vegetable origin such as mango butter, such as that marketed under the reference Lipex 203 by the company AARHUS-KARLSHAMN, shea butter, in particular that whose INCI name is Butyrospermum Parkii Butter, such as that marketed under the reference Sheasoft® by the company AARHUSKARLSHAMN, cupuacu butter (Rain forest RF3410 from the company Beraca Sabara), murumuru butter (RAIN FOREST RF3710 from the company Beraca Sabara), cocoa butter, babassu butter such as that marketed under the name Cropure Babassu SS-(LK) by Croda, as well as orange wax such as, for example, that marketed under the reference Orange Peel Wax by the company Koster Keunen, • fully or partially hydrogenated vegetable oils, such as hydrogenated soybean oil, hydrogenated coconut oil, hydrogenated rapeseed oil, mixtures of hydrogenated vegetable oils such as the mixture of hydrogenated vegetable oil of soybean, coconut, palm and rapeseed, for example the mixture marketed under the reference Akogel® by the company AARHUSKARLSHAMN (INCI name Hydrogenated Vegetable Oil), partially hydrogenated trans isomerized jojoba oil manufactured or marketed by the company Desert Whale under the commercial reference Iso-Jojoba-50®, partially hydrogenated olive oil such as, for example, the compound marketed under the reference Beurrolive by the company Soliance, • hydrogenated castor oil esters, such as hydrogenated castor oil dimer dilinoleate, for example RISOCAST-DA-L sold by KOKYU ALCOHOL KOGYO, hydrogenated castor oil isostearate, for example SALACOS HCIS (VL) sold by NISSHIN OIL, • and their mixtures.
[0188] Preferably, the pasty compound(s) are chosen from:
[0189] - petroleum jelly;
[0190] - pentaerythritol and C2-C4 polyalkylene glycol ethers;
[0191] - fatty alcohol and sugar ethers;
[0192] - copolymers of ethylene oxide and / or propylene oxide with alkylenes- long-chain C6-C30 oxides;
[0193] - esters of a glycerol oligomer, in particular diglycerol esters, with monocarboxylic acids, optionally hydroxylated, linear or branched, saturated or unsaturated, preferably saturated, in C6-C20, and / or dicarboxylic acids, linear or branched, saturated or unsaturated, preferably saturated, in C6-C10; in particular BIS-DIGLYCERYL POLYACYLADIPATE-2 (INCI name),
[0194] - vinyl ester homopolymers having C8-C30 alkyl groups;
[0195] - arachidyl propionate;
[0196] - triglycerides of fatty acids, saturated or not, linear or branched, optionally mono or poly hydroxylated, C6-C30, more particularly C8-C18, possibly hydrogenated;
[0197] - pentaerythritol esters;
[0198] - non-crosslinked esters obtained by condensation of a di- or poly- acid linear or branched C4-C50 carboxylic acid and a C2-C50 diol or polyol, aliphatic esters obtained by reaction of an ester of a hydroxycarboxylic acid and an aliphatic carboxylic acid; advantageously the carboxylic acid is C4-C30,
[0199] - esters of dimer diol and dimer diacid, such as dimer dilinoleate esters;
[0200] - butters of vegetable origin,
[0201] - partially hydrogenated vegetable oils,
[0202] - and their mixtures.
[0203] According to one embodiment, the composition comprises from 1 to 20% by weight of pasty fatty substance, relative to the total weight of the composition, preferably from 5 to 15% by weight, preferably from 10 to 15% by weight. Other ingredient(s) in the fat phase
[0204] The continuous fatty phase of the composition prepared according to the particular embodiment may also comprise at least one additional fatty substance chosen from at least one hydrophobic film-forming hydrocarbon resin, at least one silicone resin, at least one non-volatile hydrocarbon oil (polar or apolar), and mixtures thereof.
[0205] Preferably, the lipophilic mixture of step a) comprises, in addition to at least two fatty substances chosen from waxes and pasties, at least one hydrophobic film-forming hydrocarbon resin, at least one silicone resin and at least one non-volatile polar or apolar hydrocarbon oil.
[0206] Hydrophobic film-forming hydrocarbon resin
[0207] The hydrophobic film-forming hydrocarbon resin is preferably an indene resin. By the term "resin" is meant a compound whose structure is three-dimensional- sional.
[0208] The composition may comprise one or more indenic hydrocarbon resins in a total content preferably ranging from 0.1 to 20% by weight, better still from 0.5 to 15% by weight, preferentially from 1 to 10% by weight, even better still from 1.5 to 8% by weight, relative to the total weight of the composition.
[0209] The indene hydrocarbon resin(s) are preferably chosen from resins resulting from the polymerization in a majority proportion of indene monomer and in a minority proportion of monomer chosen from styrene, methylindene, methylstyrene and their mixtures; these resins may optionally be hydrogenated. These resins may have a molecular weight ranging from 290 to 1150 g / mol.
[0210] Examples of indene resins include those marketed under the reference ESCOREZ 7105 by the company Exxon Chem., NEVCHEM 100 and NEVEX 100 by the company Neville Chem., NORSOLENE S105 by the company Sartomer, PICCO 6100 by the company Hercules and RESINALL by the company Resinall Corp., or the indene / methylstyrene / hydrogenated styrene copolymers marketed under the name “REGALITE” by the company Eastman Chemical, in particular REGALITE R 1100, REGALITE R 1090, REGALITE R-7100, REGALITE R1010 HYDROCARBON RESIN, REGALITE RI 125 HYDROCARBON RESIN.
[0211] Preferably, the composition comprises at least one hydrocarbon resin which is solid at room temperature (20°C).
[0212] Preferably, the composition comprises one or more resins chosen from indene / methylstyrene / hydrogenated styrene copolymers. In particular, it is possible to use the indene / methylstyrene / hydrogenated styrene copolymers marketed under the name “REGALITE” by the company Eastman Chemical, such as REGALITE R 1100 CG HYDROCARBON RESIN, REGALITE R 1100, REGALITE R 1090, REGALITE R-7100, REGALITE R1010 HYDROCARBON RESIN, REGALITE RI 125 HYDROCARBON RESIN.
[0213] Silicone resin
[0214] The composition according to the particular embodiment may comprise at least one silicone resin. By the term "resin" is meant a compound whose structure is three-dimensional. Thus, here, a polydimethylsiloxane is not a silicone resin.
[0215] The nomenclature of silicone resins (also called siloxane resins or silicone resins) is known as "MDTQ", the resin being described according to the different siloxane monomeric units that it comprises, each of the letters "MDTQ" characterizing a type of unit.
[0216] The letter “M” represents the Monofunctional unit of formula RlR2R3SiOi / 2, the silicon atom being linked to a single oxygen atom in the polymer comprising this unit.
[0217] The letter "D" signifies a Difunctional unit RlR2SiO2 / 2 in which the silicon atom is linked to two oxygen atoms.
[0218] The letter “T” represents a Trifunctional unit of formula RlSiO3 / 2.
[0219] Such resins are described for example in “Encyclopedia of Polymer Science and Engineering, vol. 15, John and Wiley and Sons, New York, (1989), p. 265-270, and US 2,676,182, US 3,627,851, US 3,772,247, US 5,248,739 or even US 5,082,706, US 5,319,040, US 5,302, 685 and US 4,935,484.
[0220] In the M, D, T units defined above, Ri, namely RI, R2 and R3, identical or different, represent a hydrocarbon radical (in particular alkyl) having from 1 to 10 carbon atoms, a phenyl group, a phenylalkyl group or even a hydroxyl group.
[0221] Finally, the letter "Q" signifies a Tetrafunctional SiO4 / 2 unit in which the silicon atom is linked to four oxygen atoms themselves linked to the rest of the polymer.
[0222] Various silicone resins with different properties can be obtained from these different units, the properties of these polymers varying according to the type of monomers (or units), the nature and number of the radical(s) Ri, the length of the polymer chain, the degree of branching and the size of the pendant chains.
[0223] As silicone resins which can be used in the compositions according to the particular embodiment, it is possible to use, for example, silicone resins of type MQ, type T or type MQT.
[0224] MQ resins:
[0225] As an example of silicone resins of MQ type, mention may be made of alkylsiloxy-silicates of formula [(Rl)3SiOi / 2]x(SiO4 / 2)y (MQ units) in which x and y are integers ranging from 50 to 80, and such that the group RI represents a radical as defined previously, and preferably is an alkyl group having from 1 to 8 carbon atoms, or a hydroxyl group, preferably a methyl group,
[0226] Examples of solid silicone resins of the MQ type of trimethylsiloxy-silicate type include those marketed under the reference SR1000 by the company General Electric, under the reference TMS 803 by the company Wacker, under the name "KF-7312J" by the company Shin-Etsu, "DC 749", "DC 593" by the company Dow Corning.
[0227] As silicone resins comprising MQ siloxysilicate units, mention may also be made of phenylalkylsiloxysilicate resins, such as phenylpropyldimethylsiloxysilicate (Silshine 151 marketed by the company General Electric). The preparation of such resins is described in particular in patent US5817302. T resins:
[0228] Examples of T-type silicone resins include polysilses- quioxanes of formula (RSiO3 / 2)x (T units) in which x is greater than 100 and such that the R group is an alkyl group having from 1 to 10 carbon atoms, said polysilsesquioxanes being able to further comprise Si-OH terminal groups.
[0229] Mention may also be made of polymethylsilsesquioxanes which are polysilsesquioxanes in which none of the methyl radicals is substituted by another group. Such polymethylsilsesquioxanes are described for example in document US 5,246,694.
[0230] Preferably, polymethylsilsesquioxane resins in which R represents a methyl group can be used, such as, for example, those marketed: - by the company Wacker under the reference Resin MK such as Belsil PMS MK: polymer comprising repeating units CH3SiO3 / 2 (T units), which may also comprise up to 1% by weight of (CH3)2SiO2 / 2 units (D units) and having an average molecular weight of approximately 10,000 g / mol, or - by the company SHIN-ETSU under the references KR-220L which are composed of T units of formula CH3SiO3 / 2 and have Si-OH (silanol) end groups, under the reference KR-242A which comprise 98% of T units and 2% of dimethyl D units and have Si-OH end groups or under the reference KR-251 comprising 88% of T units and 12% of dimethyl D units and have Si-OH end groups.
[0231] MQT Resins:
[0232] As a resin comprising MQT units, those cited in document US 5,110,890 are known in particular.
[0233] A preferred form of MQT-type resins are MQT-propyl resins (also called MQTPr). Such resins usable herein include those described and prepared in application WO 2005 / 075542, the content of which is incorporated herein by reference.
[0234] The MQ-T-propyl resin preferably comprises the units: (i) (Rl3SiO1 / 2)a (ii) (R22SiO2 / 2)b (iii) (R3SiO3 / 2)c and (iv) (SiO4 / 2)d
[0235] with RI, R2 and R3 independently representing a hydrocarbon radical (in particular alkyl) having from 1 to 10 carbon atoms, a phenyl group, a phenylalkyl group or even a hydroxyl group and preferably an alkyl radical having from 1 to 8 carbon atoms or a phenyl group, a, b, c and d being molar fractions, a being between 0.05 and 0.5, b being between zero and 0.3, c being greater than zero, d being between 0.05 and 0.6, a + b + c + d=l, provided that more than 40 mol% of the R3 groups of the siloxane resin are propyl groups.
[0236] Preferably, the siloxane resin comprises the units: (i) (Rl3SiO1 / 2)a (iii) (R3SiO3 / 2)c and (iv) (SiO4 / 2)d
[0237] with RI and R3 independently representing an alkyl group having from 1 to 8 carbon atoms, RI preferably being a methyl group and R3 preferably being a propyl group, a being between 0.05 and 0.5, preferably between 0.15 and 0.4, c being greater than zero, preferably between 0.15 and 0.4, d being between 0.05 and 0.6, preferably between 0.2 and 0.6, or between 0.2 and 0.55, a + b + c + d = 1, eta, b, cetd being molar fractions, provided that more than 40 mol% of the R3 groups of the siloxane resin are propyl groups.
[0238] The siloxane resins usable in the particular embodiment can be obtained by a process comprising the reaction of:
[0239] A) an MQ resin comprising at least 80 mol% of (Rl3SiOi / 2)a and (SiO 4 / 2)d RI representing an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group, a and d being greater than zero, the a / d ratio being between 0.5 and 1.5;
[0240] and of
[0241] B) a propyl resin T comprising at least 80 mol% of (R3SiO3 / 2)c units, R3 representing an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group, c being greater than zero, provided that at least 40 mol% of the R3 groups are propyl groups, where the mass ratio A / B is between 95:5 and 15:85, preferably the mass ratio A / B is 30:70.
[0242] Advantageously, the mass ratio A / B is between 95:5 and 15:85. Preferably, the ratio A / B is less than or equal to 70:30. These preferred ratios have proven to allow comfortable deposits.
[0243] Preferably, the composition according to the particular embodiment comprises, as silicone resin, at least one MQ type resin as described previously.
[0244] In particular, the silicone resin is a siloxysilicate resin, preferably a trimethylsiloxysilicate resin.
[0245] Advantageously, the silicone resin is present in a content of at least 5% by weight, preferably in a content ranging from 5 to 15% by weight relative to the total weight of the composition, or better still from 6 to 9% by weight, relative to the total weight of the composition.
[0246] Polar or non-polar oil
[0247] By “oil” is meant a non-aqueous compound, liquid at 25°C and atmospheric pressure (1,013.105 Pa), immiscible with water.
[0248] By "immiscible" is meant that the mixture of the same quantity of water and oil, after stirring, does not lead to a stable solution comprising only one phase, under the aforementioned temperature and pressure conditions. The observation is made by eye or by means of a phase contrast microscope if necessary, on 100g of mixture obtained after Rayneri stirring sufficient to cause a vortex to appear within the mixture (for information 200 to 1000 rpm); the resulting mixture being left to stand, in a closed bottle, for 24 hours at room temperature before observation.
[0249] By "non-volatile oil" is meant an oil whose vapor pressure at 25°C and atmospheric pressure is non-zero and less than 2.66 Pa, more particularly less than or equal to 0.13 Pa. For example, the vapor pressure can be measured using the static method or by the isothermal thermogravimetry effusion method, according to the vapor pressure (OECD standard 104).
[0250] By "hydrocarbon oil" is meant an oil formed essentially, or even consisting of, carbon and hydrogen atoms, and possibly oxygen and nitrogen atoms, and not containing any silicon or fluorine atoms. Hydrocarbon oil is therefore distinct from a silicone oil and a fluorinated oil.
[0251] It may contain alcohol, ester, ether, carboxylic acid, amine and / or amide groups.
[0252] Preferably, the oil is hydrocarbon, i.e. it is free of heteroatoms such as nitrogen, sulfur and phosphorus.
[0253] When the hydrocarbon oil is non-volatile and polar, it comprises at least one oxygen atom. In particular, this non-volatile polar hydrocarbon oil comprises at least one alcohol function (in which case it is an “alcohol oil”) or at least one ester function (in which case it is an “ester oil”). The ester oils that can be used in the compositions can in particular be hydroxylated. The composition can comprise one or more non-volatile hydrocarbon oils, in particular chosen from C10-C26 alcohols, preferably monoalcohols; monoesters, diesters, triesters, optionally hydroxylated, of a C2-C8 mono- or polycarboxylic acid and of a C2-C8 alcohol; esters of a C2-C8 polyol and of one or more C2-C8 carboxylic acids, the ester oils, in particular having between 17 and 70 carbon atoms; vinylpyrrolidone / 1-hexadecene copolymers; dialkyl carbonates and mixtures thereof.Preferably, the polar non-volatile hydrocarbon oil(s) are chosen from C10-C26 monoalcohols, ester oils, and in particular monoesters comprising at least 17 carbon atoms in total, diesters, hydroxylated or not, comprising at least 18 carbon atoms in total, triesters, in particular having at least 35 carbon atoms, tetraesters, in particular having at least 35 carbon atoms, as well as mixtures thereof.
[0254] When the hydrocarbon oil is non-volatile and apolar, it is chosen from compounds comprising only carbon and hydrogen atoms. Said oils, linear or branched, may be of mineral or synthetic origin such as for example:
[0255] - paraffin oil,
[0256] - squalane, in particular of plant origin,
[0257] - isoeicosane,
[0258] - mixtures of linear, saturated hydrocarbons, more particularly mixtures whose INCI names are for example the following: Cl8-21 Alkane, C21-28 Alkane, such as for example the products Gemseal 60, Gemseal 120 marketed by Total,
[0259] - polybutenes, hydrogenated polybutenes, such as for example products of the Indopol range marketed by the company Ineos Oligomers,
[0260] - polyisobutenes, hydrogenated polyisobutenes such as for example Parléam ® marketed by the company NIPPON OIL FATS, PANALANE H-300 E marketed by the company INEOS OLIGOMERS, REWOPAL PIB 1000 marketed by the company EVONIK,
[0261] - decene / butene copolymers, polybutene / polyisobutene copolymers including the Indopol L-14,
[0262] - polydecenes and hydrogenated polydecenes such as, for example, PURESYN 10, PURESYN 150 or PURESYN 6 marketed by EXXONMOBIL CHEMICAL), Silkflo 366, Silkflo 364 marketed by the company INEOS OLIGOMERS, Dekanex 2008 by the company IMCD,
[0263] - and their mixtures.
[0264] Advantageously, the oil is present in a content of at least 5% by weight, preferably in a content ranging from 5 to 30% by weight relative to the total weight of the composition, or better still from 10 to 25% by weight, relative to the total weight of the composition.
[0265] At the end of step a), a lipophilic mixture is obtained comprising at least two fatty substances chosen from waxes, pasties and their mixtures, in a tank. Step b)
[0266] According to step b), the fatty phase obtained in a) is heated to a temperature above the melting point(s) of the fatty substance(s) (chosen from waxes, pasties and their mixtures).
[0267] This step b) allows the said fatty substance(s) to be completely melted.
[0268] In the case where steps a) and c) are simultaneous, an aqueous phase and a phase fat comprising at least one fatty substance at least partly solid at a temperature of 25°C chosen from waxes, pasties and their mixtures, are mixed (steps a and c)) prior to the heating step b). This step b) allows the said fatty substance(s) to be completely melted in the mixture.
[0269] Typically, this step b) is carried out with stirring.
[0270] At the end of step b), a homogeneous liquid lipophilic mixture is obtained. Step c)
[0271] Step c) is optional for this particular embodiment: in fact, it is possible to add an aqueous phase to the heated mixture of step b), to obtain a cosmetic composition in the form of an emulsion. The added aqueous phase is a dispersed aqueous phase. Such an emulsion is then an inverse emulsion (water-in-oil or W / O). The added aqueous phase may be a continuous aqueous phase; such an emulsion is then a direct emulsion (oil-in-water or O / W).
[0272] If this step c) is not present, then the composition obtained is anhydrous (consists of the continuous fatty phase).
[0273] The aqueous phase may consist essentially of water; it may also comprise a mixture of water and water-miscible solvent (miscibility in water greater than 50% by weight at 25°C) such as lower monoalcohols having from 1 to 5 carbon atoms such as ethanol, isopropanol, glycols having from 2 to 8 carbon atoms such as propylene glycol, ethylene glycol, 1,3-butylene glycol, di-propylene glycol and mixtures thereof.
[0274] The composition preferably comprises a water content representing at least 7% by weight, preferably a content ranging from 7% to 40% by weight, relative to the total weight of the composition. Advantageously, the water of the aqueous phase is present in an amount of between 7 and 30% by weight, preferably between 10 and 30% by weight, of preferably between 15 and 30% by weight, relative to the total weight of the composition.
[0275] The composition according to the particular embodiment may comprise, in addition to the compounds described above, water-in-oil surfactants, volatile oils, aqueous phase thickeners or one of their mixtures. It is understood that the quantity of these additional compounds may be adjusted by a person skilled in the art so as not to harm the desired final texture.
[0276] The compositions of the particular embodiment may comprise water-in-oil surfactants. Preferably, the surfactant has an HLB (hydrophilic / lipophilic balance) of less than or equal to 8, more particularly less than or equal to 7, preferably between 1 and 6. Preferably, it is non-ionic. The HLB value according to GRIFFIN is defined in J. Soc. Cosm. Chem. 1954 (volume 5), pages 249-256.
[0277] Preferably, the surfactant(s) are chosen from silicone nonionic surfactants, from hydrocarbon nonionic surfactants, or from mixtures thereof.
[0278] As regards silicone surfactants, mention may be made of alkyl or alkoxy dimethicone copolyols with a pendant alkyl or alkoxy chain or at the end of the silicone skeleton having, for example, from 6 to 22 carbon atoms; dimethicone copolyols, which are more particularly oxypropylenated and / or oxyethylene polydimethyl methyl siloxanes, as well as crosslinked solid elastomeric organopolysiloxanes comprising at least one oxyalkylenated group, and mixtures thereof.Among the particularly preferred silicone surfactants, mention may be made of dimethicone copolyols such as, for example, those sold under the names KF-6015 (PEG-3 dimethicone), KF-6016 (PEG-9 methyl ether dimethicone), KF-6017 (PEG-10 dimethicone), KF-6028 (PEG-9 poly-dimethylsiloxyethyl dimethicone), KF-6050 L (PEG / PPG 18 / 18 dimethicone in cyclopentasiloxane), by the company Shin-Etsu; dimethicone copolyols marketed under the names Dow Corning 3225C (PEG / PPG-18 / 18 Dimethicone in a mixture of cyclotetrasiloxane and cyclopentasiloxane), DC 5225 C Formulation Aid (PEG / PPG-18 / 18 Dimethicone in cyclopentasiloxane); or the product marketed under the name SF 1528 GE (mixture of PEG / PPG-20 / 15 Dimethicone and cyclopentasiloxane) by Momentive Performance Materials.Alkyl dimethicone copolyols such as Lauryl PEG / PPG-18 / 18 Methicone (which is more particularly an alkoxylated derivative of Lauryl Methicone containing on average 18 moles of ethylene oxide and 18 moles of propylene oxide, sold under the name "Dow Corning 5200 Formulation Aid" by the company Dow Corning) may also be used; Cetyl PEG / PPG-10 / 1 Dimethicone (which is more particularly a copolymer of Cetyl Dimethicone and an alkoxylated derivative of dimethicone containing on average 10 moles of ethylene oxide and 1 mole of propylene oxide) such as the product . sold under the name Abil EM 90 by the company Evonik Goldschmidt as well as the mixture of cetyl PEG / PPG-10 / 1 Dimethicone, polyglycerol isostearate (4 moles) and hexyl laurate sold under the name ABIL WE 09 by the company Evonik Goldschmidt.
[0279] Preferably, the composition comprises, as silicone surfactant(s), C8-C22 alkyl dimethicone copolyol such as cetyl dimethicone copolyol, in particular the INCI name of which is CETYL PEG / PPG-10 / 1 DIMETHICONE, dimethicone copolyols such as, for example, PEG-10 dimethicone, PEG / PPG 18 / 18 dimethicone, and mixtures thereof. It is also possible to use a mixture of cetyl dimethicone copolyol with polyglyceryl-4-isostearate and hexylaurate, such as the product marketed under the name Abil WE-09 by the company Evonik Goldschmidt (the INCI name is polyglyceryl-4-isostearate (and) hexylaurate (and) cetyl PEG / PPG-10 / 1 dimethicone).
[0280] The non-ionic surfactants may also be chosen in particular from polyoxyethylenated C8-C30 alcohols, (poly)oxyethylenated and / or (poly)oxypropylenated alkyl(C8-C30)- and polyalkyl(C8-C3o)-esters; polyoxyethylenated fatty acid polyesters, preferably polyhydroxylated, C12-C2o, having from 4 to 50 moles of ethylene oxide; sorbitan alkyl- and polyalkyl-esters; (poly)glycerol alkyl- and polyalkyl-esters and mixtures thereof. As alkyl(C8-C30)- and polyalkyl(C8-C30)-esters of (poly)glycerol, those having a number of glycerol units ranging from 1 to 4 are preferably used. Examples include polyglyceryl-4 isostearate (Isolan GI 34 marketed by the company Evonik Goldschmidt); polyglyceryl-3 dii-sostearate (Lameform TGI marketed by the company Cognis), glyceryl stearate, glyceryl laurate, alone or in mixtures.
[0281] According to a particularly preferred embodiment, the composition comprises at least one silicone non-ionic surfactant. Advantageously, the silicone surfactant(s) are chosen from dimethicone copolyols, the alkyl dimethicone copolyols previously described, in particular the C8-C22 alkyl dimethicone copolyols in particular of formula (I), alone or in mixtures. The composition comprises, for example, also at least one hydrocarbon non-ionic surfactant, very particularly the alkyl- and polyalkyl- esters of (poly)glycerol and / or sorbitan, and preferably polyglyceryl-3 diisostearate, polyglyceryl-4 isostearate, sorbitan isostearate or sorbitan and glycerol isostearate.
[0282] The surfactant(s) may be present in the composition in a content ranging from 0.1 to 20% by weight, and preferably ranging from 0.5 to 15% by weight, preferably from 1 to 10% by weight, relative to the total weight of the composition.
[0283] The aqueous phase may also comprise at least one hydrophilic thickening polymer (also called aqueous phase thickening polymer).
[0284] Typically, step c), like step b), is carried out with stirring. Coloring matters
[0285] Preferably, the cosmetic mixture obtained in step b) or c) comprises at least one coloring material and / or at least one active ingredient.
[0286] The coloring matter is typically chosen from water-soluble or liposoluble dyes, pigments, nacres and mixtures thereof.
[0287] The coloring materials may be present in the composition in a content ranging from 0.01% to 25% by weight, relative to the weight of the composition, preferably from 0.01% to 20% by weight.
[0288] By “colorants” we mean generally organic compounds soluble in fatty substances such as oils or in an aqueous or hydroalcoholic phase.
[0289] The water-soluble coloring materials used here are more particularly water-soluble dyes. By "water-soluble dye" is meant here any generally organic, natural or synthetic compound, soluble in an aqueous phase or water-miscible solvents and capable of coloring. In particular, the term "water-soluble" is intended to characterize the ability of a compound to dissolve in water, measured at 25°C, at a concentration of at least 0.1 g / l (obtaining a macroscopically isotropic and transparent solution, colored or not). This solubility is in particular greater than or equal to 1 g / l.Water-soluble dyes suitable herein may in particular be mentioned synthetic or natural water-soluble dyes such as, for example, DC Red 6 (Lithol Rubine Na; CI: 15850), DC Red 22 (CI: 45380), DC Red 28 (CI: 45410, Na salt), DC Red 30 (CI: 73360), DC Red 33 (CI: 17200), DC Red 40 (CI: 16035), FDC Yellow 5 (CI: 19140), FDC Yellow 6 (CI: 15985), DC Yellow 8 (CI: 45350 Na salt), FDC Green 3 (CI: 42053), DC Green 5 (CI: 61570), FDC Blue 1 (CI: 42090). By way of illustration and not limitation of sources of water-soluble coloring matter(s) likely to be used here, we can notably cite those of natural origin, such as extracts of carmine, cochineal, beetroot, grape, carrot, tomato, annatto, paprika, henna, caramel and curcumin.Thus, water-soluble coloring matters suitable here include carminic acid, betanin, anthocyanins, enocyanins, lycopene, bixin, norbixin, capsanthyn, cap-sorubin, flovoxanthin, lutein, cryptoxanthin, rubixanthin, violaxanthin, riboflavin, roudoxanthin, cantaxanthin, chlorophyll, and mixtures thereof. They may also include copper sulfate, iron sulfate, water-soluble sulfopolyesters, rhodamine, betaine, methylene blue, tartrazine disodium salt and fuchsia disodium salt. Some of these water-soluble coloring matters are approved for food use. As a representative of these dyes, we can particularly cite dyes from the caro- family. tenoids, referenced under food codes E120, E162, E163, E160a-g, E150a, E101, E100, E140 and E141. According to a particularly preferred embodiment, the water-soluble coloring matter(s) are chosen from the sodium salts of Yellow 6, Yellow 5, Red 6, Red 33, Red 40.
[0290] By "liposoluble colorant", here, is meant any generally organic compound, natural or synthetic, soluble in an oily phase or solvents miscible with the oily phase and capable of coloring. As liposoluble colorants suitable here, mention may in particular be made of liposoluble colorants such as, for example, DC Red 17, DC Red 21, DC Red 27, DC Green 6, DC Yellow 11, DC Violet 2, DC Orange 5, Sudan red, Sudan brown. As an illustration of natural liposoluble colorants, mention may particularly be made of carotenes such as [3-carotene, α-carotene, lycopene; quinoline yellow; xanthophylls such as astaxanthin, antheraxanthin, citranaxanthin, cryptoxanthin, canthaxanthin, diato-moxanthin, flavoxanthin, fucoxanthin, lutein, rhodoxanthin, ru-bixanthin, siphonaxanthin, violaxanthin, zeaxanthin; annatto; curcumin; quinizarin (Ceres Green BB, D&C Green No.6, CI 61565, 1,4-Di-p-Toluidinoanthraquinone, Green No. 202, Quinzaine Green SS) and chlorophylls. .
[0291] By pigments is meant white or colored particles, mineral or organic, insoluble in an aqueous solution, intended to color and / or opacify the resulting deposit. The pigments may be present in an amount of 0.01 to 25% by weight, in particular 0.01 to 20% by weight, relative to the total weight of the cosmetic composition. The pigments may be chosen from mineral pigments, organic pigments, and composite pigments (i.e. pigments based on mineral and / or organic materials). The pigments may be chosen from monochrome pigments, lakes, nacres, pigments with an optical effect, such as reflective pigments and goniochromatic pigments.
[0292] The pigments used here are, for example, chosen from mineral pigments.
[0293] By “mineral pigment” is meant any pigment which meets the definition of Ullmann's encyclopedia in the inorganic pigment chapter. Mineral pigments useful here include zirconium or cerium oxides, as well as zinc, iron (black, yellow or red) or chromium oxides, manganese violet, ultramarine blue, chromium hydrate and ferric blue, titanium dioxide, metal powders such as aluminum powder and copper powder. The following mineral pigments can also be used: Ta2O5, Ti3O5, Ti2O3, TiO, ZrO2 mixed with TiO2, ZrO2, Nb2O5, CeO2, ZnS.
[0294] The size of the pigment useful here is generally greater than 100 nm and can range up to 10 qm, preferably from 200 nm to 5 qm, and more preferably from 300 nm to 1 qm. The pigments have, for example, a size characterized by a D
[50] greater than 100 nm and up to 10 qm, preferably from 200 nm to 5 qm, and more preferably from 300 nm to 1 pm. The sizes are measured by laser diffraction using a commercial granulometer of the MasterSizer 3000® type from Malvern, making it possible to understand the particle size distribution of all the particles over a wide range from 0.01 pm to 1000 pm. The data are processed on the basis of the classical Mie scattering theory. This theory is the most suitable for size distributions ranging from submicron to multi-micron, it makes it possible to determine an “effective” particle diameter. This theory is notably described in the work of Van de Hulst, HC, "Light Scattering by Small Particles", Chapters 9 and 10, Wiley, New York, 1957. D
[50] represents the maximum size that 50% by volume of the particles presents.
[0295] The mineral pigments are, for example, more particularly iron oxide and / or titanium dioxide. By way of example, mention may be made more particularly of titanium dioxides and iron oxides, coated with aluminum stearoyl glutamate, for example marketed under the reference NAI® by the company MIYOSHI KASEI.
[0296] As mineral pigments which can be used here, mention may also be made of nacres. By "mother-of-pearl" is meant colored particles of any shape, iridescent or not, in particular, produced by certain molluscs in their shell or synthesized and which present a color effect by optical interference. The mother-of-pearls can be chosen from pearlescent pigments, such as titanium mica coated with iron oxide, titanium mica coated with bismuth oxychloride, titanium mica coated with chromium oxide, titanium mica coated with an organic colorant, as well as pearlescent pigments based on bismuth oxychloride. It can also be mica particles on the surface of which are superimposed at least two successive layers of metal oxides and / or organic coloring materials.
[0297] Examples of mother-of-pearls that may also be mentioned include natural mica coated with titanium oxide, iron oxide, natural pigment or bismuth oxychloride.
[0298] The mother-of-pearls can more particularly have a yellow, pink, red, bronze, orange, brown, gold and / or coppery color or reflection.
[0299] Among the pigments that can be used here, mention may also be made of those with an optical effect different from a simple conventional tint effect, that is to say unified and stabilized as produced by conventional coloring materials, such as, for example, monochromatic pigments. Here, "stabilized" means devoid of the effect of color variability with the viewing angle or in response to a change in temperature. For example, this material can be chosen from metallic sheen particles, goniochromatic coloring agents, diffracting pigments, thermochromic agents, optical brightening agents, as well as fibers, in particular, interference fibers. Of course, these different materials can be combined in such a way as to provide the simultaneous manifestation of two effects, or even a new effect.
[0300] According to a particular embodiment, the composition comprises, for example, at least one uncoated pigment.
[0301] According to another particular embodiment, the composition comprises, for example, at least one pigment coated with at least one lipophilic or hydrophobic compound. This type of pigment is particularly advantageous. To the extent that they are treated with a hydrophobic compound, they exhibit a predominant affinity for an oily phase which can then transport them. The coating may also comprise at least one additional non-lipophilic compound.
[0302] Here, “coating” a pigment generally designates the total or partial surface treatment of the pigment with a surfactant, absorbed, adsorbed or grafted onto said pigment.
[0303] The surface-treated pigments may be prepared according to surface treatment techniques of a chemical, electronic, mechanochemical or mechanical nature well known to those skilled in the art. Commercial products may also be used.
[0304] The surfactant may be absorbed, adsorbed or grafted onto the pigments by solvent evaporation, chemical reaction and creation of a covalent bond. According to one variant, the surface treatment consists of coating the pigments. The coating may represent from 0.1% to 20% by weight, and in particular from 0.5% to 5% by weight, of the total weight of the coated pigment.
[0305] The coating can be carried out for example by adsorption of a liquid surface agent on the surface of the solid particles by simple mixing with stirring of the particles and said surface agent, optionally hot, prior to the incorporation of the particles into the other ingredients of the makeup or care composition.
[0306] The coating can be carried out for example by chemical reaction of a surfactant with the surface of the solid pigment particles and creation of a covalent bond between the surfactant and the particles. This method is notably described in US patent 4,578,266.
[0307] The chemical surface treatment may consist of diluting the surfactant in a volatile solvent, dispersing the pigments in this mixture, and then slowly evaporating the volatile solvent, so that the surfactant is deposited on the surface of the pigments.
[0308] The pigments may, for example, be coated with at least one compound chosen from silicone surfactants; fluorinated surfactants; fluorosilicone surfaces; metallic soaps; N-acylated amino acids or their salts; lecithin and its derivatives; isopropyl trisostearyl titanate; isostearyl sebacate; natural vegetable or animal waxes; polar synthetic waxes; fatty esters; phospholipids; and mixtures thereof.
[0309] According to a particular embodiment, the coloring matter is an organic, synthetic, natural or naturally occurring pigment.
[0310] By "organic pigment" is meant any pigment which meets the definition of the Ullmann encyclopedia in the organic pigment chapter. The organic pigment may in particular be chosen from nitroso, nitro, azo, xanthene, quinoline, anthraquinone, phthalocyanine, metal complex type, isoindolinone, isoindoline, quinacridone, perinone, perylene, diketopyrrolopyrrole, thioindigo, dioxazine, triphenylmethane, quinophthalone compounds.
[0311] The organic pigment(s) may be chosen, for example, from carmine, carbon black, aniline black, melanin, azo yellow, quinacridone, phthalocyanine blue, sorghum red, the blue pigments codified in the Color Index under the references CI 42090, 69800, 69825, 73000, 74100, 74160, the yellow pigments codified in the Color Index under the references CI 11680, 11710, 15985, 19140, 20040, 21100, 21108, 47000, 47005, the green pigments codified in the Color Index under the references CI 61565, 61570, 74260, the orange pigments codified in the Color Index under the references CI 11725, 15510, 45370, 71105, the red pigments codified in the Color Index under the references CI 12085, 12120, 12370, 12420, 12490, 14700, 15525, 15580, 15620, 15630, 15800, 15850, 15865, 15880, 17200, 26100, 45380, 45410, 58000, 73360, 73915, 75470, and the pigments obtained by oxidative polymerization of indole derivatives,phenolics as described in patent FR 2 679 771.,
[0312] The pigments may also be in the form of composite pigments as described in patent EP 1 184 426. These composite pigments may be composed in particular of particles comprising an inorganic core covered at least partially with an organic pigment and at least one binder ensuring the fixing of the organic pigments on the core.
[0313] The pigment may also be a lake. By lake is meant insolubilized dyes adsorbed on insoluble particles, the whole thus obtained remaining insoluble during use.
[0314] The inorganic substrates on which the dyes are adsorbed are, for example, alumina, silica, calcium and sodium borosilicate or calcium and aluminum borosilicate, and aluminum.
[0315] Among the organic dyes, we can cite cochineal carmine. We can also cite the products known under the following names: D&C Red 21 (CI 45 380), D&C Orange 5 (CI 45 370), D&C Red 27 (CI 45 410), D&C Orange 10 (CI 45 425), D&C Red 3 (CI 45 430), D&C Red 4 (CI 15 510), D&C Red 33 (CI 17 200), D&C Yellow 5 (CI 19 140), D&C Yellow 6 (CI 15 985), D&C Green (CI 61 570), D&C Yellow 1 O (CI 77 002), D&C Green 3 (CI 42 053), D&C Bine 1 (CI 42 090). Examples of lakes include the product known as D&C Red 7 (CI 15 850:1).
[0316] Preferably, the cosmetic mixture obtained in step b) or c) comprises at least one active ingredient.
[0317] By active, we mean any active agent usable for topical application to the skin and / or hair.
[0318] The active agent, in particular for topical application to the skin, may in particular be chosen from emollients, deodorant actives, antiperspirant actives, moisturizers, anti-seborrheic agents, anti-acne agents, agents promoting hair regrowth, keratolytic and / or desquamating agents, anti-wrinkle agents, tightening agents, anti-irritant and / or soothing agents, vitamins, UV filters, depigmenters, odor absorbers and mixtures thereof.
[0319] The active agent, in particular for topical application to the hair, may in particular be chosen from coloring agents, conditioners, agents giving volume and / or shine to the hair, and mixtures thereof.
[0320] The active ingredient may be present in the composition in a content ranging from 0.001% to 25% by weight, relative to the weight of the composition, preferably from 0.01% to 20% by weight.
[0321] Preferably, the cosmetic composition obtained by the process according to the invention comprises at least one coloring material and / or at least one active ingredient. Step d)
[0322] Step d) is a cooling step
[0323] of the heated fatty phase obtained in b) or of the composition obtained in c).
[0324] When the composition that one wishes to obtain is anhydrous, then the heated fatty phase obtained in b) is cooled.
[0325] When the composition that one wishes to obtain is an emulsion, then the composition obtained in c) is cooled. Step e)
[0326] Step e) is optional for the particular embodiment: it comprises remelting the cooled fatty phase obtained in d) or the cooled composition obtained in d). This remelting typically comprises heating the cooled fatty phase obtained in d) or the cooled composition obtained in d) to a temperature above the melting point of the fatty phase or the composition.
[0327] Preferably, this remelting comprises heating the cooled fatty phase obtained in d) or the cooled composition obtained in d) to a temperature above the highest melting point of the fatty body of the fatty phase or of the composition.
[0328] Typically, the remelting comprises heating the cooled fatty phase obtained in d) or the cooled composition obtained in d) to a temperature greater than or equal to 85°C Step f)
[0329] Step f) comprises pouring the stirred fatty phase obtained at the end of step d) (after cooling) or e) (after remelting) or the stirred composition obtained at the end of step d) or e) into at least one container. In all cases, the stirred fatty phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) is stirred before being poured into the container.
[0330] The container may be in any suitable form. It may in particular be in the form of a pot, a case, a box, or a housing. Preferably, the container is leakproof.
[0331] Preferably, the container delimits a compartment containing the mixture, and it is closed by a closing element. The closing element may be in the form of a removable cap, a lid, in particular of the type comprising a body fixed to the container and a cap hinged on the body.
[0332] As indicated previously, the stirring step is carried out either during the cooling step d), or at the end of the remelting step e). In all cases, preferably, it is stopped before reaching the solidification point of the mixture of step d) or e) (according to a first embodiment); or it is carried out at a temperature 5°C or less lower than the solidification point of the fatty substances (according to a second embodiment); or it is carried out at a temperature more than 5°C lower than the solidification point of the fatty substances (according to a third embodiment).
[0333] Preferably, according to a first embodiment, the stirring step is stopped before reaching the solidification point of the mixture of step d) or e).
[0334] The solidification point of the mixture of step d) or e) is different from the melting point of the wax(es) and / or paste(s) used to make the fatty phase of step a). This solidification point can be determined using a differential scanning calorimeter (DSC), for example the calorimeter sold under the name "DSC Q2000" by the company TA Instruments:
[0335] The solidification point of the mixture of step d) is determined as follows: a sample of mixture obtained in b) or c) is cooled in step d), and during the cooling of this sample, the crystallization temperature range is measured, i.e. said range being defined by a crystal onset temperature Tl lization and by a temperature T2 of end of crystallization, with T1>T2. The solidification point of the fatty phase or of the composition of step d) is included in the interval [T2; Tl], and it is generally close to the value of Tl.
[0336] The solidification point of the mixture of step e) is determined as follows: a sample of fatty phase or composition remelted in step e) is cooled, and during this cooling, the crystallization temperature range is measured, i.e. said range being defined by a temperature T' 1 at the start of crystallization and by a temperature T' 2 at the end of crystallization, with T' 1 > T' 2. The solidification point of the fatty phase or composition of step e) is included in the range [T' 2 ; T' 1], and it is generally close to the value of T' 1.
[0337] The target temperature, which is less than 90% of the melting point value of the fatty substance having the highest melting point, is preferably included in the interval [T2; Tl] or [T'2; T' 1]. Indeed, over this range, the fatty phase or the composition of step d) or of step e) is homogeneous at this temperature.
[0338] To take the example cited above, if the cosmetic composition comprises at least one polyethylene wax with a melting point of around 85°C, and this wax is the fatty substance with the highest melting point in the composition, then the target temperature is less than 76.5°C, and preferably the target temperature is between 70 and 75°C (i.e. interval [T2; T1] or [T'2; T'1]).
[0339] Thus, according to a first embodiment, the stirring step is stopped before reaching the solidification point T2 of the mixture of step d) or T'2 of the mixture of step e).
[0340] Preferably, according to a second embodiment, the stirring step is carried out at a temperature 5°C or less, preferably 4°C or less, preferably 3°C or less, preferably 2°C or less, below the solidification point of the fatty substances. Preferably, the stirring step is carried out at a temperature 2°C to 3°C below the solidification point of the fatty substances.
[0341] The solidification point of the fatty substances corresponds to the fatty substance(s) used to make the fatty phase of step a) solidify(s)
[0342] Preferably, according to a third embodiment, the stirring step is carried out at a temperature more than 5°C lower than the solidification point of the fatty substances.
[0343] The solidification point of the fatty substances corresponds to the melting point of the mixture of fatty substances used to make the lipophilic mixture of step a).
[0344] Preferably, according to this third embodiment, the stirring step is carried out at room temperature (20-25°C).
[0345] As described above, the stirring step allows, for example, the application of shear to the mixture being stirred, said shear being, for example example, carried out at a shear rate ranging from 10 to 600 s1, preferably ranging from 50 to 300 s1.
[0346] Depending on the size and geometry of the tank used, the shear rate is likely to vary.
[0347] Indeed, before casting (step f), if the temperature of the cosmetic composition, preferably lipstick, in bulk decreases to a value close to the solidification point of the mixture of step d) or e) or the solidification point of the fatty substances, the start of crystal formation occurs. The shear applied by the stirring step during the formation of the crystalline structure breaks the network being formed. It is preferable to interrupt the shearing just before the solidification point, otherwise a paste may form instead of a solid network.
[0348] The resulting cosmetic composition, preferably lipstick, thus has a lower hardness due to the hindrance to the formation of the crystalline structure up to the casting temperature. Once the cosmetic composition, preferably lipstick, has been cast, waxes having a solidification point lower than the casting temperature can function properly and a cosmetic composition, preferably lipstick, is obtained that is solid and flexible.
[0349] In particular, the application of a controlled stirring step, here resulting in shearing, during cooling d) or at the end of remelting step e), and before casting f), makes it possible to obtain more supple and more melting lipsticks, having a moisturizing effect and better comfort when applied to the lips.
[0350] Without wishing to be bound by any theory, the texture and appearance of a loose lipstick evolves when constant shear is applied during cooling below the solidification point (e.g. below 70°C). When controlled shear is applied below the solidification point, a paste can be obtained (from 70 to 50°C), then the consistency decreases sharply until a liquid texture is obtained (constant shear applied up to 40 at 10°C). Applying controlled shear while cooling the loose lipstick allows a wide range of textures to be obtained:
[0351] 1. of the solid state (when a constant shear is stopped before reaching the point solidification, which allows the waxes to evaporate, giving a solid lipstick appearance): first preferred embodiment;
[0352] 2. in paste (when constant shear is applied just below the breaking point) solidification, which allows some remaining crystals to crystallize, which gives an appearance of intermediate firmness and a matte appearance): second preferred embodiment;
[0353] 3. to a liquid / fluid appearance (when constant shear is applied well en- below the solidification point, completely preventing crystallization of the solid, giving a fluid appearance with very low firmness and a shiny appearance): third preferred embodiment.
[0354] The invention also relates to a cosmetic composition obtained directly by a preparation process according to the invention.
[0355] The following examples are given for illustrative and non-limiting purposes of the present invention. The percentages are percentages by weight relative to the weight of composition, unless otherwise stated (% w / w). Example 1 of lipstick according to the invention
[0356] The solid inverse emulsion composition of example 1 according to the invention is obtained according to the following protocol: 1. Preparation of the hot fatty phase (90°C): the phases Al, A2, B, the hydrogenated polyisobutene and the silica are mixed. Then the Regalite, the silicone resin and the isohexadecane are added (steps a) and b) of the process according to the invention), and the mixture is left to cool to 85°C, 2. Preparation of the hot aqueous phase (85°C): phases F and Fl are mixed, 3. Emulsification (suction of the aqueous phase into the fatty phase) at 85°C for 20 minutes (step c) of the process), 4. Introduction of part of the pigments (phase Dl), homogenization, then addition of the other pigments and fillers, 5. Introduction of isododecane, 6. Homogenization for 5 min, then unloading into buckets and cooling (solidification to room temperature; step d) of the process):
[0357] Steps 1 to 6 above for manufacturing a composition in accordance with the invention are carried out in a KRIEGER MMD 30L TANK, equipped with a blade (rotating at 50 rpm), a scraper (rotating at 35 rpm) and a turbine, but also with a double jacket for thermoregulation and vacuum and pressure management, then the composition is discharged into buckets or tanks for cooling to room temperature.
[0358] The contents of these buckets are transferred into a tank equipped with an agitator according to the invention (the tank contains neither a turbine nor a scraper). 1. Recasting and casting (mold packaging):
[0359] In this tank equipped with an agitator according to the invention, the composition is heated to a temperature greater than or equal to the highest melting temperature of the waxes (in this case 85°C due to the presence of polyethylene wax) (remelting step e) of the process), then, to pre-crystallize the waxes, it is reduced to a target temperature of 70-75°C, thus creating a higher viscosity of the mixture which is agitated by the agitator according to the invention (agitation applied according to the invention at the end of the remelting step e)).
[0360] Once the temperature of the composition in the tank is stable, the composition is poured into molds (step f) of the process) to form the lipsticks, which have the characteristic of being softer and more melting than if the latter had been poured as usual at 85°C (without this cooling step); everything is left to cool to room temperature.
[0361] The solidification point for this composition (solidification point of the mixture obtained in d) or e)) is around 68°C.
[0362] Stirring is stopped at around 70-75°C.
[0363] [Tables 1] Compound (INCI name) Example 1 (% w / w) Phase Glycerin 4.75 Fl Sodium carbomer 0.2 Fl Isohexadecane 6.65 E1 / E2 Isododecane 7.1 G CETYL PEG / PPG-10 / 1 DIMETHICONE (Abil EM-90 from Evonik Goldschmidt) 2.85 B PEG / PPG-18 / 18 dimethicone in dimethicone (X-22-6711D, from Shin Etsu; in dimethicone;25% active ingredient) 0.95 B Polyglycerol-4 Isostearate (Isolan GI 34 from Goldschmidt) 0.95 B Glyceryl Stearate 0.2 Al Trimethylsiloxysilicate (SR1000 from Momentive Performance Materials) 6.5 E2 Hydrogenated Styrene / Methylstyrene / Indene Copolymer (Regalite RI 100 from Eastman) 1.9 El Hydrogenated Polyisobutene 11.5 A / E2 Coco-caprylate / caprate 3.8 A2 Colouring Matter (Pigments, Lakes and / or Titanium Oxide) 8.6 DI Dimethicone (100cSt) (KF 96 A - 100 CS from Shin Etsu) 0.48 A2 Acacia Decurrens / Jojoba / Sunflower Seed Wax / Polyglyceryl-3 Esters (Acticire de Gattefosse) 4.3 Al Mixture of paraffin, microcrystalline and synthetic waxes (PARACERA 30540 from Paramelt) 2.7 Al Polyethylene wax (Performalene 500-L from Nucera Solutions) 10 Al Silica 0.95 D2 Lauroyl lysine 1.4 D2; Additives: sodium hyaluronate, NaCl, preservatives, pentylene glycol, pentaerythrityl tetra dibutyl hydroxy-cinnamate Qs Fl Water Qsp 100 F
[0364] When agitation, and thus in this case shearing, are applied down to a low temperature (shearing carried out at a temperature more than 5°C lower than the solidification point of the fatty substances, i.e. third preferred embodiment), the crystal lattice cannot be established properly. In this case, the hardness obtained is a function of the waxes that can still crystallize below the casting temperature. In the specific case of the above formula, polyethylene wax has the highest dropping point (83-92°C). It may therefore be that this wax cannot completely crystallize when shearing is applied down to a casting temperature below 80°C, which results in a weaker formation of the crystal lattice and therefore of the hardness.
[0365] In an alternative embodiment, the shear applied during the stirring step is not an important parameter of the stirring.
[0366] Stirring then allows, for example, only a homogenization of the temperature or a homogenization of the components of the mixture.
[0367] The stirring step according to the invention limits the appearance of zones without flow, which allows more homogeneous stirring within the tank.
Claims
Claims
1. A method for preparing a solid cosmetic composition, comprising a step of stirring a cosmetic mixture in a mixing device (10), the mixing device (10) comprising a tank (12) and an agitator (14), the tank (12) defining a volume (16) and having a central axis (X), the agitator (14) having an axis of rotation and being capable of rotating about the axis of rotation in the tank (12) about the central axis (X), the tank (12) comprising a bottom (18) and at least one side wall (20), the agitator (14) comprising a base (22) and at least one blade (24), the base (22) extending opposite the bottom (18) of the tank (12), the at least one blade (24) having a radial edge (32) extending opposite the side wall (20), the radial distance between the radial edge (32) and the side wall (20) being constant and non-zero over the entire length of the radial edge (32) during the stirring step,the at least one blade (24) having a height (hp) measured parallel to the axis of rotation greater than or equal to 80% of the height (H) of the tank (12) measured along the central axis (X).,
2. Preparation method according to claim 1, wherein the radial distance between the radial edge (32) and the side wall (20) is less than or equal to 3 cm, preferably less than or equal to 2 cm, preferably less than or equal to 1 cm.
3. Preparation method according to claim 1 or 2, in which the or each blade (24) has a helix shape, the helix having a helix angle measured relative to the direction of the axis of rotation, the helix angle preferably being between 20° and 60°, more particularly between 20° and 30°.
4. Preparation method according to any one of claims 1 to 3, in which the or each blade (24) has a width (1) measured in the radial direction relative to the axis of rotation of between 10% and 20% of the width (L) of the tank (12) measured perpendicular to the central axis (X).
5. Preparation method according to any one of claims 1 to 4, in which the base (22) and the bottom (18) are spaced, at any point of the base (22), by a dimension less than or equal to 40 mm, and preferably between 5 mm and 15 mm.
6. Preparation process according to any one of claims 1 to 5, wherein the base (22) comprises a plurality of radial arms (26), each radial arm (26) having a radial scraping surface (28).
7. Preparation method according to claim 6, in which each radial arm (26) has a height (hb) measured parallel to the axis of rotation greater than or equal to 10% of the height (H) of the tank (12) measured along the central axis (X).
8. Preparation method according to claim 6 or 7, in which each radial arm (26) has a height (hb) measured parallel to the axis of rotation greater than twice its thickness measured perpendicular to the radial scraping surface (28).
9. A preparation method according to any one of claims 1 to 8, comprising a step of heating the cosmetic mixture before the stirring step, and / or a packaging step in which the stirred cosmetic mixture is inserted into a container.
10. Preparation method according to any one of claims 1 to 9, in which the mixing device (10) comprises a temperature probe (44) adapted to measure the temperature at at least one point of the volume (16) defined by the tank (12), preferably in a lower part of the volume (16) defined by the tank (12).
11. Preparation process according to any one of claims 1 to 10, wherein the cosmetic mixture comprises a fatty phase comprising at least 0.1% by weight, preferably at least 0.5% by weight, preferably at least 1% by weight, preferably at least 2% by weight, preferably at least 5% by weight, preferably at least 6% by weight, preferably at least 7% by weight relative to the total weight of the composition of at least one wax, preferably whose melting point is greater than or equal to 45°C, preferably greater than or equal to 70°C.
12. Preparation process according to claim 11, in which the wax with a melting point greater than or equal to 70°C is chosen from paraffin waxes, ozokerite, polymethylene waxes and polyethylene waxes; preferably the wax with a melting point greater than or equal to 70°C is an apolar hydrocarbon wax, preferably a polyethylene wax, and said apolar hydrocarbon wax represents at least 50% by weight relative to the total weight of wax(es) of the fatty phase.
13. Preparation process according to claim 11 or 12, wherein the cosmetic mixture comprises a fatty phase further comprising at least one hydrophobic film-forming hydrocarbon resin, and / or at least a silicone resin and / or at least one polar or non-polar oil.
14. Preparation process according to one of claims 11 to 13, in which the cosmetic mixture comprises an aqueous phase dispersed in the fatty phase.
15. Preparation process according to any one of claims 1 to 14, in which the cosmetic mixture comprises at least one coloring matter and / or at least one active ingredient, preferably the coloring matter is chosen from water-soluble or fat-soluble dyes, pigments, pearlescent agents and mixtures thereof.
16. Cosmetic composition obtained directly by a preparation process according to any one of claims 1 to 15.
Citation Information
Patent Citations
Composite particles, process for producing the same, and pigment, paint and resin composition using the same
EP1184426A2
Use of an insoluble pigment obtained by oxidative polymerisation of indole derivatives for the temporary dyeing of keratinous fibres
FR2679771A1
Copolymeric siloxanes and methods of preparing them
US2676182A
Flexible coating composition
US3627851A
siloxanes
US3772247A