SURFACE-REACTED CALCIUM CARBONATE FOR THE USE AS SKIN APPEARANCE MODIFIER

Abstract

The present invention refers to the use of a surface-reacted calcium carbonate having a volume median particle size d.sub.50 from 0.1 to 90 m as skin appearance modifier in a cosmetic and/or skin care composition.

Claims

1. A method for modifying skin appearance comprising applying to the skin a cosmetic and/or skin care composition comprising a surface-reacted calcium carbonate having a volume median particle size d.sub.50 from 0.1 to 90 m, wherein the surface-reacted calcium carbonate is a reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more H.sub.3O.sup.+ ion donors, wherein the carbon dioxide is formed in situ by the H.sub.3O.sup.+ ion donors treatment and/or is supplied from an external source.

2. The method of claim 1, wherein the surface-reacted calcium carbonate has a volume median particle size d.sub.50 from 0.5 to 50 m.

3. The method of claim 1, wherein the surface-reacted calcium carbonate has a specific surface area of from 15 m.sup.2/g to 200 m.sup.2/g, measured using nitrogen and the BET method.

4. The method according to claim 1, wherein the natural ground calcium carbonate is selected from the group consisting of marble, chalk, limestone, and mixtures thereof, or the precipitated calcium carbonate is selected from the group consisting of precipitated calcium carbonates having an aragonitic, vateritic or calcitic crystal form, and mixtures thereof.

5. The method according to claim 1, wherein the at least one H.sub.3O.sup.+ ion donor is selected from the group consisting of hydrochloric acid, sulphuric acid, sulphurous acid, phosphoric acid, citric acid, oxalic acid, an acidic salt, acetic acid, formic acid, and mixtures thereof.

6. The method according to claim 1, wherein the skin appearance modifier is a covering agent, a mattifying agent and/or a skin colour modifier.

7. The method according to claim 1, wherein the cosmetic and/or skin care composition has a pH value of 8.5.

8. The method according to claim 1, wherein the surface-reacted calcium carbonate is present in the cosmetic and/or skin care composition in an amount from 0.1 to 50 wt.-%, based on the total weight of the composition.

9. The method according to claim 1, wherein the cosmetic and/or skin care composition further comprises water and/or at least one oil.

10. The method according to claim 1, wherein the cosmetic and/or skin care composition comprises at least one active agent being adsorbed onto and/or absorbed into the surface of the surface-reacted calcium carbonate.

11. The method according to claim 10, wherein the at least one active agent is selected from pharmaceutically active agents, biologically active agents, vitamins, disinfecting agents, preservatives, flavouring agents, surfactants, oils, fragrances, essential oils, and mixtures thereof.

12. The method according to claim 1, wherein the composition further comprises at least one additive selected from the group consisting of bleaching agents, thickeners, stabilizers, chelating agents, preserving agents, wetting agents, emulsifiers, emollients, fragrances, colorants, skin tanning compounds, antioxidants, minerals, pigments, UV-A and/or UV-B filter, and mixtures thereof.

13. The method according to claim 1, wherein the cosmetic and/or skin care composition is selected from an eye make-up product, a facial make-up product, a lip care product, a hand care product, a skin care product, or a combination product thereof.

14. The method according to claim 1, wherein the cosmetic and/or skin care composition has a Brookfield viscosity in a range from 4,000 to 50,000 mPa.Math.s at 25 C.

15. The method according to claim 1, wherein the surface-reacted calcium carbonate further provides skin feel modification.

16. The method according to claim 1, wherein the at least one H.sub.3O.sup.+ ion donor is selected from the group consisting of hydrochloric acid, sulphuric acid, sulphurous acid, phosphoric acid, oxalic acid, H.sub.2PO.sub.4, being at least partially neutralised by a cation selected from Li.sup.+, Na.sup.+ and/or K.sup.+, HPO.sub.4.sup.2, being at least partially neutralised by a cation selected from Li.sup.+, Na.sup.+, K.sup.+, Mg.sup.2+, and/or Ca.sup.2+, and mixtures thereof.

17. The method according to claim 1, wherein the skin appearance modifier is a covering agent and/or a mattifying agent.

18. The method according to claim 1, wherein the cosmetic and/or skin care composition has a pH value of 8.0.

19. The method according to claim 1, wherein the surface-reacted calcium carbonate is present in the cosmetic and/or skin care composition in an amount from 0.5 to 20 wt.-%,-based on the total weight of the composition.

20. The method according to claim 1, wherein the cosmetic and/or skin care composition further comprises water, and/or at least one oil selected from the group consisting of vegetable oils and esters thereof, alkanecoconutester, plant extracts, animal fats, siloxanes, silicones, fatty acids and esters thereof, petrolatum, glycerides and pegylated derivatives thereof.

21. The method according to claim 1, wherein the cosmetic and/or skin care composition has a Brookfield viscosity in a range from 10,000 to 45,000 mPa.Math.s at 25 C.

Description

EXAMPLES

1. Measurement Methods

[0179] In the following, measurement methods implemented in the examples are described.

Particle Size Distribution

[0180] Volume determined median particle size d.sub.50 (vol) and the volume determined top cut particle size d.sub.98 (vol) was evaluated using a Malvern Mastersizer 2000 Laser Diffraction System (Malvern Instruments Plc., Great Britain). The d.sub.50 (vol) or d.sub.98 (vol) value indicates a diameter value such that 50% or 98% by volume, respectively, of the particles have a diameter of less than this value. The raw data obtained by the measurement was analyzed using the Mie theory, with a particle refractive index of 1.57 and an absorption index of 0.005. The methods and instruments are known to the skilled person and are commonly used to determine particle size distributions of fillers and pigments.

[0181] The weight determined median particle size d.sub.50 (wt) was measured by the sedimentation method, which is an analysis of sedimentation behaviour in a gravimetric field. The measurement was made with a Sedigraph 5120 of Micromeritics Instrument Corporation, USA. The method and the instrument are known to the skilled person and are commonly used to determine particle size distributions of fillers and pigments. The measurement was carried out in an aqueous solution of 0.1 wt.-% Na.sub.4P.sub.2O.sub.7. The samples were dispersed using a high speed stirrer and supersonicated.

Specific Surface Area (SSA)

[0182] The specific surface area was measured via the BET method according to ISO 9277 using nitrogen, following conditioning of the sample by heating at 250 C. for a period of 30 minutes. Prior to such measurements, the sample was filtered within a Buchner funnel, rinsed with deionised water and dried overnight at 90 to 100 C. in an oven. Subsequently, the dry cake was ground thoroughly in a mortar and the resulting powder was placed in a moisture balance at 130 C. until a constant weight was reached.

Intra-Particle Intruded Specific Pore Volume (in Cm.SUP.3./g)

[0183] The specific pore volume was measured using a mercury intrusion porosimetry measurement using a Micromeritics Autopore V 9620 mercury porosimeter having a maximum applied pressure of mercury 414 MPa (60 000 psi), equivalent to a Laplace throat diameter of 0.004 m (nm). The equilibration time used at each pressure step was 20 seconds. The sample material was sealed in a 5 cm.sup.3 chamber powder penetrometer for analysis. The data were corrected for mercury compression, penetrometer expansion and sample material compression using the software Pore-Comp (Gane, P. A. C., Kettle, J. P., Matthews, G. P. and Ridgway, C. J., Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations, Industrial and Engineering Chemistry Research, 35(5), 1996, p1753-1764.).

[0184] The total pore volume seen in the cumulative intrusion data can be separated into two regions with the intrusion data from 214 m down to about 1-4 m showing the coarse packing of the sample between any agglomerate structures contributing strongly. Below these diameters lies the fine inter-particle packing of the particles themselves. If they also have intra-particle pores, then this region appears bi-modal, and by taking the specific pore volume intruded by mercury into pores finer than the modal turning point, i.e. finer than the bi-modal point of inflection, the specific intra-particle pore volume is defined. The sum of these three regions gives the total overall pore volume of the powder, but depends strongly on the original sample compaction/settling of the powder at the coarse pore end of the distribution.

[0185] By taking the first derivative of the cumulative intrusion curve the pore size distributions based on equivalent Laplace diameter, inevitably including pore-shielding, are revealed. The differential curves clearly show the coarse agglomerate pore structure region, the inter-particle pore region and the intra-particle pore region, if present. Knowing the intra-particle pore diameter range it is possible to subtract the remainder inter-particle and inter-agglomerate pore volume from the total pore volume to deliver the desired pore volume of the internal pores alone in terms of the pore volume per unit mass (specific pore volume). The same principle of subtraction, of course, applies for isolating any of the other pore size regions of interest.

Oil Absorption

[0186] The oil absorption value was determined in according to ISO 787-5:1980.

Coating of Contrast Cards

[0187] Contrast cards were coated by using the respective coating compositions and applying them with a coater gap of 50 m on the surface of the contrast card. The contrast cards used are Leneta contrast cards, form 3-B-H, size 7-11- (194289 mm), sold by the company Leneta, and distributed by Novamart, Stafa, Switzerland.

Determination of Colour Values (Rx, Ry, Rz)

[0188] The colour values Rx, Ry, Rz are determined over the white and black fields of the Leneta contrast card, and are measured with a spectraflas SF 450 X spectrophotomer of the company Datacolor, Montreuil, France.

Contrast Ratio (Opacity) of the Surface of a Coated Contrast Card

[0189] Contrast ratio values are determined according to ISO 2814 at a spreading rate of approx. 20 m.sup.2/l.

[0190] The contrast ratio is calculated as described by the equation below:

[00002]$.Math.\mathrm{Contrast}.Math..Math.\mathrm{ratio}.Math.\left[\%\right]=\frac{{\mathrm{Ry}}_{\mathrm{black}}}{{\mathrm{Ry}.Math.}_{\mathrm{white}}.Math..Math.}100.Math..Math.\%.Math.$

with Ry.sub.black and Ry.sub.white being obtained by the measurement of the color values.

Measurements of Skin Glossiness and Mattifying Power

[0191] A Skin-Glossymeter GL200 probe (of the company Courage & Khazaka) was used for the determination of the mattifying power. Mode of operation: head parallel white light is sent in a 60-degree angle to the skin surface. Part of the light is directly reflected in the same angle (=angle of reflection) and part of the light is absorbed by the skin surface and then scattered and reflected diffusely. The Skin-Glossymeter GL200 measures both the portion of directly reflected light, mirrored from the surface, which is related to the gloss and the scattered portion from the surface.

2. Pigment Materials

Talc

[0192] Micro Talc FC CG AW was supplied by Mondo Minerals, and shows the characteristics listed in Table 1 below.

Boron Nitride

[0193] Boroneige SF-3 was supplied by Merck KGaA, and shows the characteristics listed in Table 1 below.

Titanium Dioxide

[0194] The titanium dioxide was supplied by Sigma-Aldrich, and shows the characteristics listed in Table 1 below.

Ground Calcium Carbonate (GCC)

[0195] GCC 1 is a high purity natural calcium carbonate obtained from marble, sold by Omya, and shows the characteristics listed in Table 1 below.

[0196] GCC 2 is a high purity natural calcium carbonate sold by Omya, and shows the characteristics listed in Table 1 below.

[0197] GCC 3 is a high purity natural calcium carbonate obtained from limestone, sold by Omya, and shows the characteristics listed in Table 1 below.

Surface-Reacted Calcium Carbonate

SRCC 1

[0198] SRCC 1 had a d.sub.50 (vol)=6.6 m, d.sub.98 (vol)=15.1 m, SSA=144 m.sup.2/g with an intra-particle intruded specific pore volume of 0.811 cm.sup.3/g (for the pore diameter range of 0.004 to 0.23 m).

[0199] SRCC 1 was obtained by preparing 450 litres of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground marble calcium carbonate from Hustadmarmor, Norway, having a mass based median particle size distribution of 90% less than 2 m, as determined by sedimentation, such that a solids content of 16 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0200] Whilst mixing the slurry, 47.1 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 15 minutes at a temperature of 70 C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying.

SRCC 2

[0201] SRCC 2 had a d.sub.50 (vol)=4.5 m, d.sub.98 (vol)=8.6 m, SSA=96.1 m.sup.2/g with an intra-particle intruded specific pore volume of 1.588 cm.sup.3/g (for the pore diameter range of 0.004 to 0.4 m).

[0202] In a mixing vessel, 10 liters of an aqueous suspension of ground limestone calcium carbonate was prepared by adjusting the solids of a ground limestone calcium carbonate having a particle size distribution of 90 wt.-% below 2 m, based on the total weight of the ground calcium carbonate, such that a solids content of 15 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0203] Whilst mixing the slurry, 2.8 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 10 minutes. Throughout the whole experiment the temperature of the suspension was maintained at 70 C. After the addition of the acid, the suspension was stirred for additional 5 minutes before removing it from the vessel and drying.

SRCC 3 SRCC 3 has a d.sub.50=6.6 m, a d.sub.98=13.7 m, a SSA=59.9 m.sup.2g.sup.1 and an intra-particle intruded specific pore volume of 0.939 cm.sup.3/g (for the pore diameter range of 0.004 to 0.51 m).

[0204] The SRCC 3 has been prepared as follows:

[0205] SRCC 3 was obtained by preparing 350 litres of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground limestone calcium carbonate from Omya SAS, Orgon having a mass based median particle size of 1.3 m, as determined by sedimentation, such that a solids content of 10 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0206] Whilst mixing the slurry at a speed of 6.2 m/s, 11.2 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 20 minutes at a temperature of 70 C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying using a jet-dryer.

SRCC 4

[0207] SRCC 4 has a d.sub.50=6.6 m, d.sub.98=16.8 m, a SSA=25.1 m.sup.2/g and an intra-particle intruded specific pore volume of 0.37 cm.sup.3/g (for the pore diameter range of 0.004 to 0.43 m).

[0208] SRCC 4 was obtained by preparing 330 liters of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground limestone calcium carbonate from Omya SAS, Orgon having a mass based median particle size of 3.0, as determined by sedimentation, such that a solids content of 14.5 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0209] Whilst mixing the slurry at a speed of 12.5 m/s, 7.9 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 10 minutes at a temperature of 70 C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying using a jet-dryer.

SRCC 5

[0210] SRCC 5 has a d.sub.50=1.6 m, d.sub.98=10.0 m, a SSA=31.4 m.sup.2/g and an intra-particle intruded specific pore volume of 0.837 cm.sup.3/g (for the pore diameter range of 0.004 to 0.59 m).

[0211] SRCC 5 was obtained by preparing 7 liters of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground marble calcium carbonate from Omya Madencilik A. S., Turkey, having a mass based median particle size of 0.4 m, as determined by sedimentation, such that a solids content of 15 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0212] Whilst mixing the slurry, 290 g phosphoric acid was added in form of an aqueous solution containing 10 wt.-% phosphoric acid to said suspension over a period of 100 minutes at a temperature of 70 C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel, filtering the product for removing excess water and then further drying in an oven.

SRCC 6

[0213] SRCC 6 has a d.sub.50=8.6 m, d.sub.98=22.0 m, a SSA=96.1 m.sup.2/g and an intra-particle intruded specific pore volume of 1.73 cm.sup.3/g (for the pore diameter range of 0.004 to 0.34 m).

[0214] SRCC 6 was obtained by preparing 1500 liters of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground limestone calcium carbonate from Omya SAS, Orgon, having a mass based median particle size of 0.6 m, as determined by sedimentation, such that a solids content of 10.0 wt.-%, based on the total weight of the aqueous suspension, is obtained. Whilst mixing the slurry rapidly, 80 kg phosphoric acid was added in form of an aqueous solution containing 20 wt.-% phosphoric acid to said suspension over a period of 60 minutes at a temperature of 62 C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying using a jet-dryer.

TABLE-US-00001 TABLE 1 Properties of used pigment materials Oil d.sub.50 d.sub.98 SSA Absorption R(y) Products (m) (m) (m.sup.2/g) (g/100 g) (%) SRCC 1 6.56 15.09 144 88 95.2 SRCC 2 4.54 8.56 96.1 105 93.0 SRCC 3 6.6 13.7 59.5 82 92.9 SRCC 4 6.6 16.8 25.1 35 92.9 SRCC 5 1.6 10.0 31.4 44 96.4 SRCC 6 8.6 22.0 96.1 67 91.7 GCC 1 2.35 10.0 3.0 14 96.4 GCC 2 2.85 13.0 2.6 10 91.7 GCC 3 0.85 5.0 9.7 18 91.7 Micro Talc 8.0 26.0 6.0 37 92.0 FC CG AW Boroneige 7.49 30.0 12.5 46 97.7 SF-3 Titanium 0.45 5.0 8.3 16 96.8 dioxide

3. Skin Appearance ModificationTest Results

3.1 Determination of the Covering Power of the Base Composition

[0215] In order to determine the covering power (coverage) of a pigment material, a base composition comprising different pigment concentrations of the pigment material, namely 5, 10 and 15 wt.-%, were prepared. The covering power of the respective base compositions was determined by measuring the colour values (Rx, Ry, Rz) and then calculation the contrast ratio, as described above.

[0216] Table 2 shows the ingredients that were used to prepare a base composition and table 3 shows the ingredients that were used to prepare a cosmetic and/or skin care composition.

[0217] In the following the INCI name of some ingredients will be used. INCI stands for International Nomenclature of Cosmetic Ingredients.

TABLE-US-00002 TABLE 2 Ingredients for base composition Ingredients/trade name Characterization Function Supplier Bermocoll EHM 200 Cellulose ether Thickener 1) Butyldiglycol acetate Ester Film forming 2) agent Byk 011 Polymer Defoamer 3) Byk 019 Polyether-modified Defoamer 3) polydimethylsiloxane Byk 349 Polyether-modified Surfactant 3) siloxane Calgon N new Sodium Dispersing 4) polyphosphate agent Coapur 2025 Polyurethane based Rheology 5) modifier Disperbyk-181 Alkylolammonium Wetting 3) salt of a agent polyfunctional polymer Dowanol DPnB Dipropylene glycol Open time 6) n-butyl ether Ecodis P 90 Ammonium Wetting and 5) neutralized dispersing polyacrylate agent Mergal 723 K Benzoisothiazolinone Preservative 7) Mowilith DM 2425, Aqueous copolymer Binding 8) 50% dispersion based on agent vinyl acetate Sodium hydroxide, Sodium hydroxide pH 2) 10% solution regulation Texanol Isobutyric acid, ester Film 9) with 2,2,4-trimethyl- forming agent 1,3-pentanediol 1) Akzo Nobel 2) Diverse (e.g. Sigma-Aldrich) 3) Byk (Altana Group) 4) BK Giulini 5) Coatex (Arkema Group) 6) Dow 7) Troy Chemical Company 8) Celanese 9) Eastman

TABLE-US-00003 TABLE 3 Ingredients for a cosmetic and/or skin care composition Ingredients INCI Nomenclature Supplier A) Aqua dem. Aqua (Water) A2 Vivapur COS 8 Microcrystalline Cellulose, 10) Cellulose A3 Xanthan Gum Xanthan Gum 11) B) Emulium Mellifera Polyglyceryl-6 Distearate (and) 12) Jojoba Esters (and) Polyglyceryl-3 Beeswax (and) Cetyl Alcohol Lanette O Cetearyl Alcohol 13) Imwitor 372 P Glyceryl Stearate Citrate 14) MOD Octyldodecyl Myristate 12) Miglyol 812 Caprylic/Capric Triglycerides 15) Jojoba Oil Simmondsia Chinensis (Jojoba) 15) Seed Oil Olive Oil Olea Europaea (Olive) Fruit Oil 15) Lipocire A SG C10-18 Triglycerides 12) Eutanol G Octyldodecanol 13) Phenonip Phenoxyethanol (and) 16) Methylparaben (and) Ethylparaben (and) Propylparaben (and) Butylparaben (and) Isobutylparaben C) Cocoate BG Butylene Glycol Cocoate 12) Titanium Dioxide CI 77891 17) Ferroxide 216 P CI 77491 18) Red Ferroxide 510 P CI 77492 18) Yellow Ferroxide 78 P CI 77499 18) Black D) Flavour Aroma 10) J. Rettenmaier & Soehne, Germany 11) Omya Hamburg GmbH, Germany 12) Gattefoss SAS, France 13) BASF Schweiz AG, Switzerland 14) Sasol GmbH, Germany 15) Haenseler AG, Switzerland 16) SLI Chemicals GmbH, Germany 17) Sigma Aldrich, Switzerland 18) Huntsman, Switzerland

[0218] The base composition contains the ingredients listed in Table 4.

TABLE-US-00004 TABLE 4 Ingredients and amounts of base composition Weight % (based on total Ingredients weight of base colour) Demineralised water 40.0 Calgon N new 0.2 Bermocoll EHM 200 1.0 Sodium hydroxide solution, 10% 0.6 Byk 011 2.0 Texanol 0.5 Butyldiglycol acetate 0.5 Dowanol DPnB 1.0 Byk 019 0.5 Coapur 2025 1.8 Mergal 723 K 0.2 Demineralized water 5.0 Ecodis P 90 0.6 Disperbyk-181 1.0 Byk 349 0.4 Demineralized water 14.7 Mowilith DM 2425, 50% 30.0 Total 100.0

[0219] The base composition was prepared as follows:

[0220] The demineralized water was added to a beaker, then, Calgon, Bermocoll and the sodium hydroxide solution were added under stirring with a lab dissolver until all ingredients were dissolved. Then the other ingredients listed in Table 2 up to Byk 349 were added while continuously stirring the mixture. Then the demineralized water was added and the resulting mixture was thoroughly mixed. Finally, the binding agent Mowilith was added during continuous stirring of the mixture at a speed of 100 rpm to obtain the final base colour.

[0221] This base composition was used for the preparation of formulations with different pigment concentrations according to the formulae listed in Table 5:

TABLE-US-00005 TABLE 5 Formulations with different pigment concentrations Amount of Amount of Powder with X % base colour pigment material pigment concentration [wt.-%] [wt.-%] Powder with 5% 95.0 5.0 pigment concentration Powder with 10% 90.0 10.0 pigment concentration Powder with 15% 85.0 15.0 pigment concentration

[0222] The formulations were prepared by weighing the respective pigment material in the required amount and adding the respective amount of the base composition. Then the resulting mixtures were homogenized for 1 minute by use of a speed mixer at a speed of 3000 rpm. Then the mixture was mixed using a spatula and subsequently the mixture was again homogenized for 1 minute by use of a speed mixer at a speed of 3000 rpm. The resulting mixture was then used for the measurement of the colour values (Rx, Ry, Rz) which in turn were used for the calculation of the contrast ratio. The contrast ratio (coverage) values for the used pigment materials at the different pigment concentrations are listed in Table 6.

TABLE-US-00006 TABLE 6 Coverage values for the different pigment materials and for different pigment concentrations in a base composition Coverage (%) Percentage of pigment material (%) Products 5 10 15 SRCC 1 6.6 21.3 44.6 SRCC 2 8.9 54.3 73.9 SRCC 3 6.7 24.6 53.8 GCC 1 3.1 4.8 5.8 GCC 2 3.1 4.8 5.8 Micro Talc FC CG AW 4.5 5.8 6.4 Boroneige SF-3 16.9 32.4 45.6 Titanium Dioxide 29.4 51.2 62.9

[0223] The above results clearly show that the inventive surface-reacted calcium carbonates SRCC 1, SRCC 2, and SRCC 3, at pigment concentrations of 10 or 15%, have comparable or even better coverage values when compared to Boroneige SF-3 that is used in prior art cosmetic formulations for this purpose. The best coverage shows SRCC 2. The coverage is even better than that of titanium dioxide.

3.2 Determination of the Covering Power in a 50/50 Mixture of Base Composition and Cosmetic and/or Skin Care Composition

[0224] In order to determine the covering power (coverage) of 50/50 mixture of a base composition and a cosmetic and/or skin care composition, cosmetic and/or skin care composition with different pigment material as well as with different pigment material concentrations were prepared. The specific amounts of ingredients of the different cosmetic and/or skin care compositions are shown in Table 7 (general formulation of the cosmetic and/or skin care composition) and Table 8 listing the different pigment materials as well as their concentrations in each cosmetic and/or skin care composition.

[0225] The cosmetic and/or skin care compositions were prepared according to the following scheme: [0226] Under rapid mixing (Eurostar 20 high speed control, IKA, 1 000 rpm) disperse A2 into the water (A1) for 10 minutes, then add A3 and disperse for another 10 minutes [0227] Pour all ingredients of phase B and heat phases A and B, separately, to a maximum temperature of 70 C. [0228] Mix phase C using a mixer or a three-roll mill (Ultra Turrax T25-D, IKA, 24 000 rpm). Add phase D to phase C when the oil absorption of the pigment material is below 50 g/100 g. If the oil absorption of the pigment material is above 50 g/100 g then it has to be added at later stage of the procedure, [0229] Under rapid mixing (Eurostar 20 high speed control, IKA, 3 000 rpm) add phase B to phase A [0230] Maintain the rapid mixing and add phase C at a temperature of 40 C., [0231] Add separately phase D (if not already added) and phase E at a temperature of 30 C., [0232] Allow the resulting mixture to cool to room temperature

TABLE-US-00007 TABLE 7 Foundation formulation with type and amount of ingredients Ingredients % w/w A1) Aqua dem. add. 100 (*) A2) Vivapur COS 8 1.20 A3) Xanthan Gum 0.20 B) Emulium Mellifera 4.00 Lanette O 1.00 Imwitor 372 P 0.10 MOD 2.00 Miglyol Oil 6.00 Jojoba Oil 2.00 Olive Oil 1.00 Lipocire A SG 3.00 Eutanol G 3.00 Phenonip 1.00 C) Cocoate BG 6.50 Titanium Dioxide 4.00 Ferroxide 216 P red 0.57 Ferroxide 510 P yellow 1.14 Ferroxide 78 P black 0.05 D) Pigment materials X.00 E) Flavor 0.30 Total 100.00 (*) The water is added in an amount so that the total sum of the weight of all ingredients in the respective foundation is equal to 100.00 wt.-%.

TABLE-US-00008 TABLE 8 Amount X.00 and nature of pigment material used in the respective cosmetic and/or skin care composition of Table 7 Pigment Material (nature and amount X.00 (w/w %)) Composition No. SRCC 1 SRCC 3 SRCC 2 GCC 1 GCC 2 Micro Talc Boroneige TiO.sub.2 1 A 5.0 2 A 5.0 3 A 5.0 4 A 5.0 5 A 10.0 6 A 15.0 7 A 5.0 8 A 10.0 9 A 15.0 10 A 5.0 11 A 10.0 12 A 5.0 13 A 4.0 14 A 3.0 15 A 3.0 5.0

[0233] 50 wt.-% of the respective cosmetic and/or skin care composition was then mixed with 50 wt.-% of the base composition shown in Table 4. (SpeedMixer DAC 150.1 FVZ, Hauschild Engineering, 3 000 rpm).

[0234] The covering power of the resulting 50/50 mixtures was determined by measuring the colour values (Rx, Ry, Rz) followed by calculation the contrast ratio, as described above. The results for the respective compositions are listed in Table 9.

TABLE-US-00009 TABLE 9 Covering power (%) and the R(y) value measured for the respective 50/50 mixtures of base composition and cosmetic and/or skin care composition 50/50 Mixture of base composition & cosmetic Covering and/or skin care composition power R(y) Mixture No. (%) (%) 1 B 42.5 19.4 2 B 43.0 19.2 3 B 52.7 22.4 4 B 26.1 13.3 5 B 33.5 16.1 6 B 38.1 17.6 7 B 31.9 13.9 8 B 39.8 17.8 9 B 34.1 16.4 10 B 37.7 18.2 11 B 40.8 17.1 12 B 39.8 19.8 13 B 27.5 13.4 14 B 29.3 15.4 15 B 34.2 17.2

[0235] The 50/50 mixtures including the inventive surface-reacted calcium carbonates (1B, 2B, 3B, 14B and 15B) all show a better coverage power when compared to 50/50 mixtures containing other pigment materials, such as ground calcium carbonate, Boroneige and Micro Talc, at the same pigment concentration.

3.3 Mattifying Power of the Cosmetic and/or Skin Care Composition

[0236] The formulations shown in Table 10 have been tested:

TABLE-US-00010 TABLE 10 Mattifying formulation with type and amount of ingredients Formula-No. Ingredients F01 F02 [Supplier] INCI Nomenclature % w/w % w/w A) Lanette O [8] Cetearyl Alcohol 2.00 2.00 Imwitor 372P [1] Glyceryl Stearate 5.00 5.00 Citrate Almond Oil [3] Prunus Amygdalus 2.00 2.00 Dulcis (Sweet Almond) Oil Apricot Oil [3] Prunus Armeniaca 3.00 3.00 Kernel Oil KCC SF1000N - Polydimethylsiloxane 2.00 2.00 100 cSt [2] KCC 4130P [2] Stearyl Dimethicone 2.00 2.00 Coconut Oil [7] Cocos nucifera Oil 3.00 3.00 B) Water dem. Aqua (water) add. 100 add. 100 1,2-Propanediol Propylene Glycol 4.00 4.00 Glycerin Glycerin 3.00 3.00 Xanthan Gum [5] Xanthan Gum 0.20 0.20 Potassium Sorbate Potassium Sorbate 1.00 1.00 [8] Sodium Chloride Sodium Chloride 1.00 1.00 C) GCC 3 5.00 SRCC 5 5.00 D) Phenonip Methylparaben (and) 1.00 1.00 Ethylparaben (and) Butylparaben (and) Propylparaben (and) Phenoxyethanol 100.00 100.00 [1] Sasol GmBH, Germany [2] KCC Silicone Corporation, Korea [3] Hnseler AG, Switzerland 4 Sigma Aldrich, Switzerland [5] Omya Hamburg GmbH, Germany 6 SLI Chemicals GmbH, Germany [7] Georges Walther AG, Switzerland [8] Cognis GmbH, Germany

Results of the Mattifying Test:

[0237] Results for formulation F01 based on GCC 3 are shown in Table 11.

TABLE-US-00011 TABLE 11 Results for formulation F01 based on GCC 3 Gloss rate Student t-test % of subjects with Kinetic (mean SEM) % on mean p Significance the expected effect D 28 0.7 0.3 8% 0.028 Yes 67

[0238] Under these study conditions, after 28 days of once daily use, the formulation F01 based on GCC 3 maintained the skin not shiny, characterized by a decrease of the gloss rate of 8% on average. Less shiny skin was observed in 67% of the subjects.

[0239] Results for formulation F02 based on SRCC 5 are shown in Table 12.

TABLE-US-00012 TABLE 12 Results for formulation F02 based on SRCC 5 Gloss rate Student t-test % of subjects with Kinetic (mean SEM) % on mean p Significance the expected effect D 28 1.1 0.2 12% <0.001 Yes 91

[0240] Under these study conditions, after 28 days of once daily use, the formulation F02 containing SRCC 5 maintained the skin not shiny, characterized by a significant decrease of the gloss rate of 12% on average. Less shiny skin was observed in 91% of the subjects. Thus, it can be gathered from the results presented in Tables 11 and 12 that the formulation based on surface-reacted calcium carbonate provides a better mattifying effect than the formulation based on ground calcium carbonate.

3.4 Skin Feel ModificationCosmetic and/or Skin Care Composition Comprising Mint Oil
Cosmetic and/or Skin Care Composition Containing Mint Oil

[0241] Mint oil was loaded onto the surface of GCC 1 and SRCC 3 using a Ldige mixer. Depending on the weight percentage of the mint oil, both calcium carbonates were used in an oil in water emulsion. High quantity of mint oil, exactly 83.2 wt.-%, based on the weight of the surface-reacted calcium carbonate, was loaded on SRCC 3. 1 and 2 wt.-% of the loaded SRCC 3, based on the weight of the skin care composition, was used for formulating the compositions. Given that GCC 1 contains the lower weight percentage of mint oil with 22.6 wt.-%, the weight percentage of the loaded GCC 1 was adjusted to 2 wt.-%, based on the weight of the skin care composition. To compare the skin feel modification between all samples, mint oil alone, i.e. not loaded to a calcium carbonate carrier, was added at a concentration of 0.45 wt.-% to another emulsion, in order to get the same final concentration of mint oil in all compositions. Additionally, skin feel modification of a composition comprising SRCC 4 having a lower surface compared to SRCC 3 was evaluated using the primary test. The primary test included the direct application of the loaded SRCCs on the skin, followed by a movement of spreading and circling the material on the skin. All cosmetic and/or skin care compositions were prepared as oil-in-water emulsions.

3.4.1 Sensory Evaluation

[0242] Sensory evaluation of the skin care and/or cosmetic composition is a specific method for applying a composition to the skin, in order to analyze the modification of the skin feel upon and after application. To guarantee comparability, the method follows a strict and identical procedure for each step of the test. For carrying out the test, a quantity of composition, approx. 0.075 mL, is applied on the hand or the finger by using a small spoon. Compositions were marked with a rating from 0 to 10, see also explanation of sensory properties in Tables 13 to 17.

Sensory Properties

[0243]

TABLE-US-00013 TABLE 13 Aspect Descriptor Description Separation It is a visible separation between the both phases. No separation No separation is sensed between the both phases. Opaque Under a standard lamp the product does not let light. No opaque The product is completely transparent under a standard lamp. Transparent means that the light passes through the product. White Under a standard lamp the product appears white. No white The product appears as dark brown or it is transparent. Shiny The product reflects the light under a standard lamp. No shiny The product is mat and reflects no light under a standard lamp.

TABLE-US-00014 TABLE 14 Hand movement Descriptor Description Fluid When the product is placed between the thumb and index fingers and that a pressure is applying, there is no holding, flows of the fingers and moves away from the pressure zone. No resistance is felt. No fluid When the product is placed between the thumb and index fingers and that a pressure is applying, there is no flow between the both fingers and it moves not away from the pressure zone. A resistance is felling. Stringy When the product is placed between the thumb and index fingers and that a distance is slowly applied between the both fingers, it is a continuous string. It breaks when the distance between the fingers becomes too large. No stringy When the product is placed between the thumb and index fingers and that a distance is slowly applied between the both fingers, there is no string/elongated filament formed. Slippery When the product is placed between the thumb and index fingers and that a movement of friction is made, there is no resistance. The product makes the movement easier. No slippery When the product is placed between the thumb and index fingers and that a movement of friction is made, there is a resistance. The product restricts the movement.

TABLE-US-00015 TABLE 15 Spread Descriptor Description Fresh At the first rotation on the hand a fresh sensation is felt comparable to cold water. No fresh At the first rotation on the hand there is no modification of temperature on the hand. Bleaching Between 2 and 3 rotations the product makes the skin white. No bleaching Between 2 and 3 rotations there is no whitening on the hand. Spread Between 5 and 10 turns on the hand there is a good distribution of product. No spread Between 5 and 10 turns on the hand there is no repartition of product.

TABLE-US-00016 TABLE 16 After one minute Descriptor Description Greasy When the product is placed between the thumb and index fingers and that a movement of friction is applied, there is no resistance. The products have an oily aspect. No greasy When the product is placed between the thumb and index finger and that a movement of friction is applied, there is a resistance and no oily aspect. Sticky By performing a pressure with index finger on the hand, there is an adhesion. No sticky By performing a pressure with index finger on the hand, there is no adhesion. Soft Dry and sliding touch is felt by perform of a slippery on the skin. No soft No dry and sliding touch is felt by perform of a slippery on the skin.

TABLE-US-00017 TABLE 17 After two minutes Descriptor Description Penetrating The product is disappearing and no residue is detected when touching skin after two minutes. No penetrating There can still a residue be detected when touching skin after two minutes.

[0244] The following compositions were used:

[0245] Composition 1: 0.45% mint oil

[0246] Composition 2: 2% SRCC 3 loaded with 83.2 wt.-% mint oil

[0247] Composition 3: 1% SRCC 3 loaded with 83.2 wt.-% mint oil

[0248] Composition 4: 2% GCC 1 loaded with 22.6 wt.-% mint oil

[0249] Composition 5: 1% SRCC 4 loaded with 58.0 wt.-% mint oil

[0250] The results of the sensory evaluation for the storage at room temperature are shown in Table 18.

TABLE-US-00018 TABLE 18 Results of the sensory evaluation for the storage at room temperature Composition No. 1 2 3 4 5 ASPECT Opacity 6 9 8 9 9 Whiteness 4 6 6 9 9 Brightness 7 7 7 6 7 HAND MOVEMENT Fluidity 6 6 5 7 6 Stringiness 2 1 1 1 1 Slipperiness 7 6 8 8 8 SPREAD Freshness 7 10 9 7 10 Bleaching 5 6 7 5 6 Spreadability 7 8 8 7 7 AFTER ONE MINUTE Greasiness 4 2 3 3 3 Stickiness 4 2 1 1 1 Softness 1 2 3 6 3 AFTER TWO MINUTES Penetrating 5 5 5 5 5 Lasting 4 8 7 5 9 OTHERS Odor Ok (but mint oil Ok (odor of raw Ok (odor of raw OK (odor of raw Ok (odor of raw does not cover materials is materials is materials is materials is the odor of raw covered after covered after covered after covered after materials) opening the opening the opening the opening the beaker and beaker and beaker and beaker and application application) application) application on skin) on the skin) Viscosity in 32 200 32 800 39 940 21 640 34 550 Cps at 25 C., after 30 s

Interpretation of Results

[0251] Mint oil is currently used in cosmetic compositions as a fragrance component. The concentration used in prior art compositions usually ranges from 0.25 to 1 wt.-% of mint oil, for example, in refreshing creams and lotions. This is comparable to composition 1. As can be gathered from the results of the sensory evaluation, a composition comprising a small quantity of loaded SRCC 3 (1 or 2 wt.-%; see compositions 2 and 3) improves many parameters. For example, opacity and whiteness of compositions comprising SRCC 3 are increased. Compositions comprising SRCC 3 show the best results of freshness during the first application. Furthermore, the compositions based on SRCC 3 are non-greasy and sticky during and/or after application. The skin feel modification is long lasting, i.e. for two to five minutes, when the composition comprises SRCC 3. SRCC 3 is able to deliver a cooling effect during a long time and to feel a pleasant sensation after application. The SRCC 3 has the capacity to conceal the odor of raw ingredients. It has the advantage to take out the fragrance at the end after formulating.

[0252] Results show that the freshness sensation was higher when the composition comprises SRCC 3, which indicates that the low proportion of SRCC 3 might have enhanced mint oil liberation and penetration into the skin, increasing freshness perception. No significant differences in freshness intensity after 2 minutes of application were found between compositions containing only mint oil or loaded GCC 1. Loaded SRCC 3 contributes to the immediate perception of freshness and it is not only a skin feel modifier, but a carrier for oils too.

[0253] It has been shown that SRCC 3 acts on several different skin feel parameters. The compositions comprising SRCC 3 are easy to spread and show a pleasant feeling during and/or after application. Compositions comprising SRCC 3 reduce dryness, improve mattifying effect, and show the ability to smooth out lines and wrinkles, i.e. the skin appears without blemishes.

[0254] SRCC 4 was loaded with 58 wt.-% of mint oil, based on the total weight of the SRCC. To compare its performance, the same quantity, i.e. 58 wt.-% of mint oil, was loaded on SRCC 3. SRCC 4 has a lower surface. It was selected to evaluate the skin feel characteristics and to determine how much oil can be loaded onto the surface-reacted calcium carbonate. The above-described primary test was carried out. Freshness feeling was further intensified for the loaded SRCC 4 compared to loaded SRCC 3. This might be due to the lower surface area and/or lower surface porosity of the SRCC 4. This might in turn result in a smaller quantity of mint oil being adsorbed and/or absorbed onto SRCC 4. The mint oil would be more exposed to the skin surface, and that might be reason why the freshness evaluation is rated as higher. Use of loaded SRCC 4 assures a long lasting skin feel modification, i.e. for two to five minutes. Loaded SRCC 3 also offers a good freshness lasting over a long period of time, but the time period is shorter than with loaded SRCC 4. Slipperiness, softness and spreadability are slightly better for SRCC 4. SRCC 4 is easier to spread and soft to the skin.

[0255] Mint oil loading onto the surface of SRCC 4 demonstrated that skin feeling, especially freshness sensation, can be improved and intensified using a SRCC having a lower surface area.

3.5 Skin Feel ModificationSkin Care and/or Cosmetic Composition in Form of a Lipstick

[0256] The performance of ground calcium carbonate (GCC) and surface-reacted calcium carbonate (SRCC) has been compared. Lipsticks were prepared with the ingredients shown in Table 19. The amount of GCC or SRCC, respectively, is indicated below.

TABLE-US-00019 TABLE 19 Lipstick formulation with type and amount of ingredients Ingredients [Supplier] INCI Nomenclature % w/w A) Beeswax [3] Cera Flava (Beeswax) 7.00 Carnauba wax [3] Copernicia Cerifera 5.00 (Carnauba) Wax Candelilla wax [3] Euphorbia Cerifera 8.00 (Candelilla) Wax Jojoba oil [4] Simmondsia Chinensis 5.00 (Jojoba) Seed Oil Apricot kernel oil Prunus Armeniaca 5.00 [2] (Apricot) Kernel Oil Ricin Oil [3] Ricinus Communis 28.40 (Castor) Seed Oil Almond Oil [4] Prunus Amygdalus 10.00 to 19.00.sup.1 Dulcis (Sweet Almond) Oil Coconut Oil [6] Cocos Nucifera Oil 15.00 Submica M [1] Mica 2.00 GCC or SRCC 1.00 to 10.00.sup.1 Carmine Lake 50% C.I. 75470 6.00 B) DL--tocopheryl Tocopheryl Acetate 0.30 acetate [5] Flavor Aroma q.s 100.00 .sup.1The amount of almond oil was adapted based on the used amount of GCC or SRCC to a combined amount of almond oil and GCC or SRCC of 20 wt. %, based on the total weight of the composition. [1] Omya Hamburg GmbH; Germany [2] Gustav Heess; Germany [3] Georges Walther AG; Switzerland [4] Hnseler AG; Switzerland [5] Sigma Aldrich; Switzerland [6] Mimox AG; Switzerland [0257] Phase A is heated to 80 C. in a glass beaker until homogeneous. [0258] Add phase B components to phase A while stirring gently. Homogenize the mixture (Ultra Turrax T25-D, IKA, 24 000 rpm) [0259] Then pour the liquid mixture into the appropriate molds and place the molds in the refrigerator overnights. [0260] Place the molds at room temperature and wait 1 hour. Remove the lipstick from the molds.

[0261] The following amounts of GCC 2 or SRCC 2 were used for the compositions as described in Table 19:

[0262] Composition 1: 2 wt. % SRCC 2

[0263] Composition 2: 5 wt. % GCC 2

[0264] Composition 3: 10 wt. % GCC 2

[0265] Composition 4: w/o filler (i.e. 20 wt.-% almond oil)

[0266] Composition 5: 1 wt. % SRCC 2

[0267] Sensory evaluation was carried out according to the criteria shown in tables 20 to 22.

TABLE-US-00020 TABLE 20 Aspect Descriptor Description Defect on the If there are exudation, blooming or bubbles lipstick on the surface of the lipstick No homogeneous The lipstick shows some irregularities Homogeneous The surface of the lipstick is even No shiny The lipstick looks matt Shiny The appearance of the lipstick is shiny No smooth The surface of the lipstick appears irregular Smooth The surface of the lipstick looks smooth, without any irregularities

TABLE-US-00021 TABLE 21 Hand movement (on the hand) Descriptor Description No hard Breaking easily, bend or crumble during application Hard The stick has a good rigidity/strength No homogeneous The film is not homogeneous and does not cover the skin Homogeneous An uniform film is gotten during application Slippery When the lipstick is applied on the hand, it makes the movement easier No slippery When the lipstick is applied on the hand, it restricts the movement Coverage (only The lipstick covers the skin. visual) Color strength Only visual determination

TABLE-US-00022 TABLE 22 Spread (on lip) Descriptor Description No smooth The film is not homogeneous and rough Smooth No grainy feeling Not messy Pigments are not smeary on lip Messy Pigments leave some marks on lip No spread It is difficult to apply the lipstick, it is not uniform et doesn't remain on lips spread Pigment spread easily, evenly and stick on the lip once applied No shiny It has glossy effect on lip Shiny It looks shiny on lip No greasy No oily feeling after application Greasy Feel oily on lip after use

[0268] Results of the sensory evaluation are shown in Table 23. Table 24 shows the results of the color evaluation.

TABLE-US-00023 TABLE 23 Results of the sensory evaluation Composition-No. 1 2 3 4 5 ASPECT Defect on the lipstick *2 Homogeneity 8 7 7 6 6 Brightness 5 3 2 6 5 Smoothness 6 8 8 8 8 HAND MOVEMENT (ON THE HAND) Hardness 8 7 8 5 7 Homogeneity 9 6 6 3 7 Slippery 5 7 7 5 7 Coverage (only visual) 9 7 8 4 7 Color strength 9 7 6 5 5 SPREAD (ON LIP) Smoothness 8 7 8 4 8 Messiness 1 1 1 3 1 Spreadability 7 7 8 3 8 Brightness 8 6 6 8 8 Greasiness 3 4 3 5 3 PERCENTAGE OF FILLER (%) SRCC 2 2 1 GCC 2 5 10

TABLE-US-00024 TABLE 24 Results of the color evaluation Composition No.. 1 2 3 4 5 COLOR MEASUREMENT R (y) 89.18 89.12 90.17 80.32 59.85 PERCENTAGE OF FILLER (%) SRCC 2 2 1 GCC 2 5 10

Interpretation of Results

[0269] When the concentration of powders is too high, e.g. above 10 wt. %, the lipstick shows some defects like bubbles, cracks or streaks. Evaluation of homogeneity seems to be better in presence of minerals but it depends on the concentration used. More precisely, the homogeneity is good for concentrations in the range of 2 to 10 wt. %. Hardness of the lipstick correlates with the weight percentage of calcium carbonate present in the lipstick composition. The higher the concentration of the calcium carbonate in the composition is, the higher is the hardness of the prepared lipstick. All lipsticks provide a better homogeneity during application compared to the reference, which does not contain GCC or SRCC. The best homogeneity is provided by composition 1 and 5 comprising SRCC 2. Furthermore, composition 5 comprising 1 wt. % SRCC 2 provides a good slippery. The addition of SRCC to a composition further allows for improving the coverage. SRCC 2 provides a darker color compared to the reference. Smoothness is increased for composition 1 and 5 comprising SRCC 2.