MACROSCOPIC SOLAR DISPERSION WITHOUT SHELL

Abstract

A dispersion comprising a dispersed phase comprising drops and a continuous aqueous phase, preferably in gel form, wherein the drops comprise a fatty phase comprising at least one lipophilic gelling agent and at least one UV filter, wherein: the fatty phase has a melting point between 50° C. and 100° C., preferably between 60° C. and 90° C., and, at room temperature and atmospheric pressure, meets the following physical/chemical criteria—a hardness (x) of between 2 and 14 N, preferably between 2.5 and 12 N, more preferably between 3 and 9 N, and most preferably between 4 and 6 N; and an adhesiveness (y) greater than or equal to −2 N, and better still, greater than or equal to −1 N, and in particular greater than or equal to −0.6 N; and the dispersion does not comprise amodimethicone.

Claims

1. A dispersion comprising a fatty phase, in the form of drops, dispersed in a continuous aqueous phase, preferably in the form of a gel, the dispersed phase and the continuous phase being immiscible with each other at room temperature and atmospheric pressure, wherein the fatty phase comprises at least one lipophilic gelling agent, and at least one UV filter, wherein: the fatty phase has a melting point between 50° C. and 100° C., preferably between 60° C. and 90° C., and, at room temperature and atmospheric pressure, meets the following physical/chemical criteria: a hardness (x) of between 2 and 14 N, preferably between 2.5 and 12 N, more preferably between 3 and 9 N, and most preferably between 4 and 6 N; and an adhesiveness (y) greater than or equal to −2 N, or better still, greater than or equal to −1 N, and in particular greater than or equal to −0.6 N; and the dispersion does not comprise amodimethicone.

2. The dispersion according to claim 1, wherein the fatty phase has a cohesiveness (z) of less than or equal to 40, preferably less than or equal to 35, and better still, greater than or equal to 30.

3. The dispersion according to claim 1, wherein the fatty phase comprises between 1% and 60%, preferably between 5% and 50%, in particular between 10% and 40%, more preferably between 15% and 35%, and in particular between 20% and 25%, by weight of UV filter(s) based on the total weight of the fatty phase.

4. The dispersion according to claim 1, wherein the dispersion does not comprise a shell, in particular a shell formed by a coacervate layer interposed between the dispersed fatty phase and the continuous aqueous phase.

5. The dispersion according to claim 1, wherein the drops having a diameter greater than or equal to 100 μm represent a volume greater than or equal to 60%, or even greater than or equal to 70%, preferably greater than or equal to 80%, and better still, greater than or equal to 90% of the total volume of the dispersed phase and/or at least 60%, or even at least 70%, preferably at least 80%, and better at least 90%, of the drops have an average diameter greater than or equal to 100 μm.

6. The dispersion according to claim 1, the lipophilic gelling agent is selected from organic or inorganic, polymeric or molecular lipophilic gelling agents; solid fats at ambient temperature and pressure; and mixtures thereof.

7. The dispersion according to claim 1, comprising from 0.5% to 30%, preferably from 1% to 25%, in particular from 1.5% to 20%, better still from 2% to 15%, and most particularly from 5% to 12%, by weight of lipophilic gelling agent(s) relative to the total weight of the fatty phase.

8. The dispersion according to claim 1, wherein the continuous aqueous phase comprises at least one hydrophilic gelling agent, preferably selected from the group consisting of natural gelling agents; semi-synthetic gelling agents; synthetic gelling agents; and mixtures thereof, and preferably is selected from Carbomer, alkasealan (INCI: Alcaligenes Polysaccharides), and their mixture.

9. The dispersion according to claim 1, wherein from 0.0001% to 20%, preferably from 0.001% to 15%, in particular from 0.01% to 10%, and more preferably from 0.1% to 5%, by weight of hydrophilic gelling agent(s) based on the total weight of the continuous aqueous phase.

10. The dispersion according to claim 1, comprising from 1% to 60%, in particular from 5% to 50%, preferably from 10% to 40%, and more preferably from 15% to 30%, by weight of dispersed fatty phase relative to the total weight of the dispersion.

11. The dispersion according to claim 1, wherein the core is single-phase or comprises an intermediate drop of an intermediate phase and at least one, preferably a single, inner drop of an inner phase disposed in the intermediate drop, the intermediate phase and the inner phase being immiscible with each other at room temperature and atmospheric pressure, the UV filter(s) being present in the intermediate and/or internal phase.

12. The dispersion according to claim 1, wherein the dispersion does not comprise surfactants.

13. The dispersion according to claim 1, wherein the dispersion does not comprise: dextrin ester and fatty acid(s), in particular dextrin palmitate(s), and/or optionally hydrophobically treated silica, e.g. fumed silica, and/or Acrylates/C10-30 Alkyl Acrylate Crosspolymer, and/or Cetyl Ethylhexanoate.

14. A method of preparation a dispersion according to claim 1, comprising at least the following steps: a) heating an oily fluid FI to a temperature from 50° C. to 150° C.; b) heating an aqueous fluid FE to a temperature from 50° C. to 150° C.; c) bringing the aqueous fluid FE and the oily fluid FI into contact; and d) forming drops of fatty phase, consisting of the oily fluid FI, dispersed in a continuous aqueous phase, consisting of aqueous fluid FE, wherein: the oily fluid FI comprises at least one lipophilic gelling agent, at least one UV filter, and optionally at least one oil and has a melting point between 50° C. and 100° C., preferably between 60° C. and 90° C., and, at room temperature and atmospheric pressure, meets the following physical/chemical criteria: a hardness (x) of between 2 and 14 N, preferably between 2.5 and 12 N, more preferably between 3 and 9 N, and most preferably between 4 and 6 N; and an adhesiveness (y) greater than or equal to −2 N, better still, greater than or equal to −1 N, and in particular greater than or equal to −0.6 N; the oil fluid FI further being free of amodimethicone; and the aqueous fluid FE comprises at least water and, optionally, at least one hydrophilic gelling agent.

15. The method according to claim 1, wherein the drop formation step comprises forming drops of oily fluid FI at the outlet of a first conduit opening into the aqueous fluid FE.

16. The method according to claim 15, wherein the aqueous fluid FE is circulated in a second conduit, the outlet of the first conduit opening into the second conduit, advantageously coaxially with the local axis of the second conduit.

17. A dispersion obtained by a method according to claim 14.

18. A composition, in particular a cosmetic composition, comprising at least one dispersion according to claim 1, optionally in association with at least one physiologically acceptable medium.

19. The composition according to claim 18, said composition being a make-up composition, in particular a foundation composition.

20. A non-therapeutic method for the cosmetic treatment, in particular make-up and/or care, preferably make-up, of a keratinous material, in particular the skin, lips, or hair, comprising at least one step of applying to the said keratinous material at least one dispersion according to claim or at least one composition according to claim 18.

21. Use of a dispersion according to claim 1, for improving the properties of a cosmetic composition, in particular a make-up composition and more particularly a foundation composition, in terms of: hue intensity; progressive make-up results; coolness and/or moisturisation; kinetic stability; durability of the make-up effect, in particular the coverage; and cover for colour and/or relief imperfections without marking them, combined with a sensation of lightness, coolness and moisturisation on application without feeling greasy and/or sticky or slowing down application.

Description

[0345] The corresponding measurements are shown in FIGS. 1 to 7.

[0346] FIG. 1 is a graph representing the hardness criterion (x) of the anhydrous gels in Table 1.

[0347] FIG. 2 is a graph representing the adhesiveness criterion (y) of the anhydrous gels in Table 1.

[0348] FIG. 3 is an enlargement of FIG. 2 of the adhesiveness values (y) of the anhydrous gels 2A, 2B, 2C, 3A, 3B, 3C, 5 and 6.

[0349] FIG. 4 is a graph showing the cohesiveness criterion (z) of the anhydrous gels 1 B, 1 D, 2B, 3B, 5 and 6 from Table 1.

[0350] FIG. 5 FIG. 6 FIG. 7 Finally, FIGS. 5 to 7 are graphs representing the texturometry curves of the anhydrous gels in Table 1. These FIGS. 5 to 7 show the force (in N) of the gels in Table 1 as a function of the time (in seconds) during which the gels are subjected to (1) a first compression step (0 to 5 s) and then (2) a second relaxation step where the mobile rises (5 to 10 s). The previous steps (1) and (2) are repeated. These FIGS. 5 to 7 therefore provide information on the physical/chemical properties of the gels in Table 1, particularly in terms of hardness, adhesiveness and cohesiveness.

RESULTS

[0351] Hardness (x): as shown in FIG. 1, with the same percentage of lipophilic gelling agent and oil solvent (e.g. 1B vs 2B vs 3B), the differences in the hardness profiles of the different anhydrous gels tested are not significant. Furthermore, from tests 1C and 1D, it can be seen that the hardness is impacted by the nature of the solvent.

[0352] Adhesiveness (y): As shown in FIGS. 2 and 3, with the same percentage of lipophilic gelling agent and oil solvent:

[0353] gels 2 (A, B, C), 3 (A, B, C), 5 and 6 have similar adhesiveness profiles, and

[0354] gels 1 (B, C) and 4 show significantly better adhesiveness than gels 2 (A, B, C) and 3 (A, B, C).

[0355] Furthermore, from tests 1C and 1 D, it is observed that the nature of the solvent has an impact on the tackiness.

[0356] Cohesiveness (z): As shown in FIG. 4, gels 2B, 3B, 5 and 6 show similar physical/chemical properties in terms of cohesiveness, which are significantly lower than those of gels 1B and 1 D.

Example 2: Preparation of Macroscopic Sunscreen Dispersions

[0357] In this example 2, ten dispersions are prepared comprising a continuous aqueous phase and a dispersed phase in the form of drops, each represented by one of the anhydrous gels of example 1. These dispersions are obtained by means of a microfluidic manufacturing method as described in WO2019145424, namely where the formation of the drops is carried out by means of a nozzle suitable for conveying a fluid jet formed by a second fluid concentrically surrounding a first fluid and a device for mechanically fragmenting said fluid jet disposed in the vicinity of the nozzle outlet. According to this embodiment, the drops obtained by this microfluidic method ave a uniform size distribution with a high production efficiency.

[0358] The compositions of the phases (fluids) for the preparation of the dispersions are described in Table 3 below.

TABLE-US-00003 TABLE 3 % w/w % w/w Fluid Name INCI Phases final IF Anhydrous gel according to example 1 — 20 (gelled fatty phase) OF Osmosis water Aqua Qsf* Qsf* (continuous Microcare PE Phenoxyethanol, aqua 0.99 0.80 aqueous Microcare emollient PTG Pentylene glycol, aqua 2.47 2.00 phase) Glycerine codex Glycerin, aqua 9.88 8.00 Zemea Propanediol Propanediol, aqua 8.64 7.00 Butylene Glycol 1.3 Butylene glycol, aqua 6.17 5.00 Edeta BD Disodium EDTA 0.05 0.04 Carbopol ETD 2050 polymer Carbomer 0.33 0.27 Carbopol Ultrez 10 polymer Carbomer 0.10 0.08 Blanose CMC 7HF Cellulose, aqua 0.04 0.03 Sodium hydroxide pellets PRS codex Sodium hydroxide 0.01 0.01 Total 100 71 BF Osmosis water Aqua Qsf Qsf (base) Sodium hydroxide pellets PRS codex Sodium hydroxide 0.64 0.06 Total 100 9 QSF: quantity sufficient for

[0359] Preparation Protocol:

[0360] For the OF:

[0361] Mixture A: while stirring in a deflocculator, Phenoxyethanol, Pentylene glycol and EDTA are incorporated into water and the resulting mixture is stirred for 5 min.

[0362] Mixture B: Carbopol Ultrez 10 polymer carbomer is then sprinkled onto mixture A until hydrated, then stirred for 30 minutes with a paddle.

[0363] Mixture C: Carbopol ETD 2050 polymer is then dispersed in mixture B while stirring for 30 minutes using a paddle.

[0364] Mixture D: while stirring in a deflocculator, humectants (i.e. glycerine, zemea propanediol and butylene glycol 1.3) are added to mixture C. The resulting mixture D is kept stirring for 10 min.

[0365] Mixture E: the blanose, previously predispersed at 1% in water under magnetic stirring at 80° C., after returning to room temperature, is added to mixture D while stirring in a deflocculator.

[0366] Mixture F: soda is added to mixture E which is stirred for 10 minutes to obtain the OF solution.

[0367] The OF solution is then connected to a pump pOF connected to a heater to keep the OF hot (80° C.).

[0368] For IFs: see protocol described in example 1.

[0369] Each of the ten heated IF solutions is then connected to a pump pIF connected to a heater to keep the IF hot (80° C.). To reduce heat loss, the microfluidic system was installed directly at the outlet of pumps pIF and OF and is itself maintained at 80° C.

[0370] For BF: soda and water are mixed with the aid of a magnetic bar for 5 min. The BF solution is then introduced into an sBF syringe.

[0371] Using the pIF and pOF pumps and the sBF syringe and associated syringe plungers, the IF and OF are injected into the microfluidic system and the BF is injected into the dispersion at the outlet of the microfluidic system, at the flow rates described in Table 4 below.

TABLE-US-00004 TABLE 4 Flow rate per nozzle Phase (in mL/hr) OF 360 IF 40 BF 92.9

[0372] Depending on the configuration of the microfluidic system and the flow rates, the dispersions obtained may comprise drops with a satisfactory monodispersity and with an average diameter between 100 μm and 1,500 μm, in particular between 700 and 1,300 μm.

[0373] Results on the Manufacture of Dispersions:

[0374] It was possible to make dispersions from the ten anhydrous gels according to example 1.

Stability Test

[0375] Each of the ten dispersions is then packed into three 30 mL polypropylene (PP) containers, each half filled. After 1 day at room temperature, each test undergoes one of the following three transport tests (one receptacle per test):

[0376] roller test (i.e. horizontal circular motion): Wheaton reference, for 1 hour

[0377] vibration table (i.e. vertical circular motion): reference Heidolph Unimax 1,010, for 1 hour; and

[0378] 3D mixer (i.e. random movements): for 6 minutes.

[0379] At the end of these stability tests, the following are evaluated: (i) the integrity of the drops, in particular their fragmentation and (ii) the turbidity of the gel, generally linked to a transfer of the fatty phase into the continuous aqueous phase.

Scoring Criteria:

[0380]

TABLE-US-00005 TABLE 5 SCORING CRITERIA 0 1 2 3 BUBBLE FRAGMENTATION No fragmentation Slight fragmentation Average fragmentation High fragmentation GEL TURBIDITY Clear gel Slightly cloudy gel Medium cloudy gel Cloudy gel

Results:

[0381]

TABLE-US-00006 TABLE 6 Dispersion* D1A D1B D1C D1D D2A D2B D2C D3A D3B D3C 4 5 6 Bubble 3 1 0 1 3 1 0 2 1 0 0 2 2 fragmentation Gel turbidity 3 1 0 1 3 1 0 2 1 0 0 2 2 Conclusion KO OK OK OK KO OK OK OK OK OK OK OK OK D1A = dispersion according to example 2 using the anhydrous gel 1A of example 1 as the dispersed fatty phase.

[0382] The dispersions D1A and D2A show unsatisfactory stability results. The corresponding fatty phases are therefore excluded from the rest of the study. The D3A dispersion shows average stability results but is considered satisfactory enough to be retained for further study. The other dispersions tested showed satisfactory stability results. These results show that a fatty phase must have properties in terms of hardness greater than 2 N, preferably greater than or equal to 2.5 N, in particular greater than or equal to 3 N, and better still, greater than or equal to 4 N.

[0383] Sensory Testing

[0384] Then, based on the above eight dispersions with satisfactory stability, visual, sensory, and coverage tests were carried out on a cohort of 24 women aged between 22 and 45. Each woman blindly tested the eight dispersions that were satisfactory in terms of kinetic stability. The criteria evaluated are (i) the adhesion of the dispersed fatty phase drops onto the packaging wall, (ii) the aggregation of the dispersed phase drops with each other, (iii) the ease (or comfort) of application, and in particular the ease of crushing and spreading the dispersed phase drops, and (iv) coverage.

Scoring Criteria:

[0385]

TABLE-US-00007 TABLE 7 SCORING CRITERIA 0 1 2 3 ADHESION = Lack of adhesion Slight adhesion Average adhesion Strong adhesion adhesiveness (y) AGGREGATION = Lack of aggregation Slight aggregation Average aggregation Strong aggregation cohesiveness (z) COVERAGE Very satisfactory coverage Satisfactory coverage Moderately satisfactory Unsatisfactory coverage coverage EASE OF Very satisfactory application. Satisfactory application. Moderately satisfactory Unsatisfactory application. APPLICATION The drops are not (or only The drops are not or only application. The drops are felt and slightly) felt and the slightly felt and the The drops are felt and their crushing on the skin mixing between the aqueous mixing between the their crushing on the skin generates lumps that are and fatty phases is easy. aqueous and fatty generates lumps. The difficult to remove by phases is easy. application of dispersion spreading on the skin. The remains possible. hardness of the drops is too high.

Results:

[0386]

TABLE-US-00008 TABLE 8 Dispersion* D1B D1C D1D D2B D2C D3A D3B D3C 4 5 6 Adhesion = adhesiveness (y) 3 3 3 0 1 0 1 1 3 0 0 Aggregation = cohesiveness (z) 2 NR** 2 1 NR** NR** 1 NR** 2 1 1 Ease of application 1 2 1 1 2 0 1 2 3 1 1 D1A = dispersion according to example 2 implementing the anhydrous gel 1A of example 1 as the dispersed fatty phase. **NR: No information.

CONCLUSION

[0387] From the above results, it can be seen that a fatty phase:

[0388] in view of the above results in terms of “ease of application” and FIG. 1, must have a hardness (x) of 14 N or less, preferably 12 N or less, and preferably 9 N or less,

[0389] in view of the above results in terms of “adhesion” and of FIGS. 2 and 3, that the fatty phase must have a adhesiveness (y) greater than or equal to −2 N, and better still, greater than or equal to −1 N, or even greater than or equal to −0.6 N, and

[0390] in view of the above results in terms of “aggregation” and FIG. 4, that the fatty phase must have a cohesiveness (z) of less than or equal to 40, preferably less than or equal to 35, and better still, less than or equal to 30.

[0391] In conclusion, a dispersion comprising a dispersed phase comprising drops and a continuous aqueous phase, when the stability of this dispersion is not ensured by the presence of a shell at the “continuous aqueous phase/dispersed fatty phase” interface or of surfactant, can nevertheless and unexpectedly present satisfactory properties in terms of kinetic stability and sensory quality, in particular in terms of comfort, ease of application, coolness, and moisturisation, on the condition that the gelled fatty phase has:

[0392] a melting point between 50° C. and 100° C., preferably between 60° C. and 90° C., and,

[0393] (ii) at room temperature and atmospheric pressure:

[0394] a hardness (x) of between 2 and 14 N, in particular between 2.5 and 12 N, preferably between 3 and 9 N, and more preferably between 4 and 6 N;

[0395] an adhesiveness (y) greater than or equal to −2 N, and better still, greater than or equal to −1 N, and in particular greater than or equal to −0.6 N; and

[0396] optionally, a cohesiveness (z) of less than or equal to 40, preferably less than or equal to 35, and better still, less than or equal to 30.

[0397] Even more unexpectedly, these results are observed and applicable with a dispersion with dispersed fatty phase drops of macroscopic size.

[0398] Moreover, these dispersions have an SPF measured in vitro of between 20 and 30 They therefore provide appealing sun protection. The SPF can be evaluated by any means known to the skilled person.

[0399] It should also be noted that spreading them on the skin, especially wet skin, does not induce a whitening effect, which is very pleasant for the consumer.

[0400] Finally, these observations are all the more unexpected as they are obtained even in the presence of (i) high UV filter contents in relation to the weight of the dispersed fatty phase and (ii) a high proportion of dispersed fatty phase.

[0401] In addition to a particularly good SPF result, the dispersion provides satisfactory sensory properties when applied to the skin, particularly in terms of coolness and moisturisation.