PIGMENT MIXTURE

Abstract

The present invention relates to a pigment mixture based on at least two components A and B, where component A is a mixture of flake-form and spherical substrates which is covered with one or more inorganic layers and/or organic layers, and component B comprises crystalline or amorphous particles selected from the group of the metal oxides, metal hydroxides, metal oxy-halides, Prussian Blue or mixtures thereof,

and to the use thereof in paints, coatings, printing inks, security printing inks, plastics, ceramic materials, glasses, in cosmetic formulations, as tracer, as filler and for the preparation of pigment preparations and dry preparations.

Claims

1. A pigment mixture comprising at least two components A and B, where component A is a mixture of flake-form and spherical substrates which is covered with one or more inorganic layers and/or organic layers, and component B comprises crystalline or amorphous particles selected from the group of the metal oxides, metal hydroxides, metal oxyhalides, Prussian Blue or mixtures thereof.

2. The pigment mixture according to claim 1, wherein said flake-form substrates are natural mica, synthetic mica, talc, kaolin, glass flakes, SiO.sub.2 flakes, Al.sub.2O .sub.3 flakes, graphite flakes, Fe.sub.2O.sub.3 flakes, BiOCl, TiO.sub.2 flakes, nitride flakes, oxynitride flakes, BN flakes, pearl essence or mixtures thereof.

3. The pigment mixture according to claim 1 or 2, wherein said spherical substrates are magnesium silicate, aluminum silicate, alkali metal aluminum silicate, alkaline-earth metal aluminum silicate and combinations thereof, SiO.sub.2 spheres, glass spheres, hollow glass spheres, aluminum oxide, ceramic spheres and polymeric spheres comprising ethylene-acrylic acid copolymers, ethylene-methacrylate copolymers, HDI-trimethylolhexyl lactone copolymers, nylon, polyacrylates, polymethyl methacrylate copolymers, polyethylene, polymethylsilsesquioxanes or combinations thereof.

4. The pigment mixture according to one or more of claims 1 to 3, wherein component B consists of crystalline or amorphous particles of Fe.sub.2O.sub.3, TiO.sub.2, Prussian Blue, Cr.sub.2O.sub.3, Fe.sub.3O.sub.4, FeOOH, BiOCl, titanium suboxides or mixtures thereof.

5. The pigment mixture according to one or more of claims 1 to 4, wherein said flake-form substrates of component A are natural or synthetic mica flakes.

6. The pigment mixture according to one or more of claims 1 to 5, wherein said spherical substrate of component A comprises SiO.sub.2 spheres, glass spheres or hollow glass spheres.

7. The pigment mixture according to one or more of claims 1 to 6, wherein the substrate mixture of component A is covered with one or two metal oxide layers or mixtures of metal oxides.

8. The pigment mixture according to one or more of claims 1 to 7, wherein the inorganic layer of component A is TiO.sub.2, Fe.sub.2O.sub.3, Fe.sub.3O.sub.4, FeOOH, Cr.sub.2O.sub.3, Prussian Blue, Carmine Red, titanium suboxide, SnO.sub.2, ZnO, Al.sub.2O.sub.3, SiO.sub.2 or mixtures thereof.

9. The pigment mixture according to one or more of claims 1 to 8, wherein component A has one of the following compositions: substrate mixture+Fe.sub.2O.sub.3 (1st layer)+SnO.sub.2 (2nd layer) substrate mixture+Fe.sub.2O.sub.3 (1st layer)+SiO.sub.2 (2nd layer) substrate mixture+Fe.sub.3O.sub.4 (1st layer)+TiO.sub.2 (2nd layer) substrate mixture+Fe.sub.3O.sub.4 (1st layer)+SnO.sub.2 (2nd layer) substrate mixture+Fe.sub.3O.sub.4 (1st layer)+SiO.sub.2 (2nd layer) substrate mixture+Cr.sub.2O.sub.3 (1st layer)+TiO.sub.2 (2nd layer) substrate mixture+Cr.sub.2O.sub.3 (1st layer)+SnO.sub.2 (2nd layer) substrate mixture+Cr.sub.2O.sub.3 (1st layer)+SiO.sub.2 (2nd layer) substrate mixture+TiO.sub.2 (1st layer)+Prussian Blue (2nd layer) substrate mixture+TiO.sub.2 (1st layer)+Carmine Red (2nd layer) substrate mixture+SnO.sub.2 (1st layer)+TiO.sub.2 (2nd layer) substrate mixture+TiO.sub.2 (1st layer) substrate mixture+Fe.sub.2O.sub.3 (1st layer) substrate mixture+FeOOH (1st layer) substrate mixture+TiO.sub.2 (1st layer)+Fe.sub.2O.sub.3 (2nd layer) substrate mixture+Prussian Blue (1st layer) substrate mixture+Cr.sub.2O.sub.3 (1st layer) substrate mixture+Fe.sub.2O.sub.3 (1st layer)+TiO.sub.2 (2nd layer)+SiO.sub.2 (3rd layer) or substrate mixture+TiO.sub.2 (1st layer)+SiO.sub.2 (2nd layer)+TiO.sub.2 (3rd layer).

10. The pigment mixture according to at least one of claims 1 to 9, wherein components A and B are mixed in the weight ratio (parts by weight) of 99:1 to 1:99.

11. The pigment mixture according to one or more of claims 1 to 10, wherein component A and/or component B additionally has an outer protective layer in order to increase the light, temperature and weather stability.

12. A process for the preparation of the pigment mixture according to one or more of claims 1 to 11, comprising: covering the flake-form and spherical substrates of component A with one or more inorganic layers by wet-chemical coating or by the CVD or PVD process, and subsequently mixing component A and component B with one another and subsequently drying and optionally jointly calcining.

13. The process according to claim 12, wherein the flake-form and spherical substrates of component A are mixed and covered with one or more absorbent or non-absorbent layers by wet-chemical methods, and the coated substrate/sphere mixture (component A) is mixed with the crystalline or amorphous particles (component B), and the mixture of components A and B is worked up jointly, and the final mixture is calcined at temperatures of 150-1000° C., where the calcination is optionally carried out under reducing gas.

14. The process according to claim 12 or 13, wherein, in the case of wet-chemical coating, the aqueous suspension of component B is added to the aqueous suspension of component A and the suspension comprising components A and B is worked up, or in that, after the wet-chemical covering of the substrate mixture of component A, the product is separated off and worked up and the dried product of component A is subsequently mixed with the suspension of component B and the suspension is then worked up, or in that the substrate mixture of component A is added to the suspension of component B and the mixture of component B and substrate mixture of component A is jointly covered with one or more inorganic layers by wet-chemical methods and then worked up.

15. Use of the pigment mixture according to one or more of claims 1 to 11 in paints, coatings, printing inks, security printing inks, plastics, ceramic materials, glazes, glasses, in cosmetic formulations, as tracer, as filler and for the preparation of pigment preparations and dry preparations.

16. A formulation comprising a pigment mixture according to one or more of claims 1 to 11.

17. The formulation according to claim 16, wherein, besides the pigment mixture, said formulation comprises at least one constituent selected from absorbents, astringents, antimicrobial substances, antioxidants, antiperspirants, antifoaming agents, antidandruff active compounds, antistatics, binders, biological additives, bleaches, chelating agents, deodorizers, emollients, emulsifiers, emulsion stabilizers, dyes, humectants, film formers, fillers, fragrances, flavors, insect repellents, preservatives, anticorrosion agents, cosmetic oils, solvents, oxidants, vegetable constituents, buffer substances, reducing agents, surfactants, propellant gases, opacifiers, UV filters and UV absorbers, denaturing agents, aloe vera, avocado oil, coenzyme Q10, green tea extract, viscosity regulators, perfume and vitamins.

Description

EXAMPLES

Example 1

Pigment Mixture Having a Blue Mass Tone

Batch 1A:

[0141] 8 g of natural mica flakes from Merck KGaA (particle size<15 μm) together with 80 g of silicon dioxide spheres from ABC Nanotech (diameter: 2-4 μm) are stirred into 800 ml of deionized water.

[0142] This suspension is heated to the reaction temperature of 75° C. with stirring. The pH is adjusted to 2.1 by means of 10% sulfuric acid, and 2200 g of a 25% titanium tetrachloride solution are then metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then adjusted to 4.3 using 10% sulfuric acid. Two solutions 1 and 2 are subsequently added simultaneously, while the pH is kept constant using a 10% ammonium carbonate solution. Solution 1 is prepared from 60 g of potassium hexacyanoferrate (III) and 1300 g of deionized water. Solution 2 consists of 76 g of iron sulfate heptahydrate and 1250 g of deionized water. When the addition is complete, the mixture is stirred for a further 15 min, and the pH is then set to pH 6 using 20% sodium hydroxide solution.

Batch 1B:

[0143] 900 ml of deionized water are heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 4.3 using 10% sulfuric acid. Two solutions 1 and 2 are subsequently added simultaneously, while the pH is kept constant using a 10% ammonium carbonate solution. Solution 1 is prepared from 165 g of potassium hexacyanoferrate (Ill) and 2100 g of deionized water. Solution 2 consists of 209 g of iron sulfate heptahydrate and 1950 g of deionized water. The pH is then set to pH 6 using 20% sodium hydroxide solution.

[0144] When both batches are complete, the suspensions of batches 1A and 1B are mixed, filtered off, washed and dried at 150° C. and then sieved through a sieve having a mesh width of 24 μm, giving a pigment mixture having a blue mass tone and a soft skin feel and matt texture which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 1A/1B mixing ratio.

Example 1a

[0145] If the 1A:1B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 1b

[0146] If the 1A:1B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and medium hiding power are obtained.

Example 1c

[0147] If the 1A:1B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 2

Pigment Mixture Having a Red Mass Tone

Batch 2A:

[0148] 8 g of synthetic mica flakes from Merck KGaA (particle size<15 μm) together with 80 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 800 ml of deionized water.

[0149] This suspension is heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 3.3 using 10% hydrochloric acid. 923 g of 10% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 2.1 using 10% HCl, and 310 g of 25% titanium tetrachloride solution are subsequently metered in. During this, the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 min.

Batch 2B:

[0150] 1.7 l of deionized water are heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 3.3 using 10% hydrochloric acid. 1000 g of 10% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 7 using 20% sodium hydroxide solution.

[0151] When both batches are complete, the suspensions of batches 2A and 2B are mixed, filtered off, washed and dried at 150° C. The pigment mixture is subsequently calcined at 780° C. and then passed through a sieve having a mesh width of 24 μm.

[0152] A pigment mixture having a burgundy mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 2A/2B mixing ratio.

Example 2a

[0153] If the 2A:2B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 2b

[0154] If the 2A:2B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 2c

[0155] If the 2A:2B ratio is 2:8, highly chromatic pigment mixtures having a very good hiding power and a good skin feel are obtained.

Example 3

Pigment Mixture Having a White Mass Tone

[0156] 1.2 l of deionized water are heated to the reaction temperature of 75° C. with stirring, and the pH is then adjusted to pH 1.8 using 10% hydrochloric acid. 20 ml of a titanium tetrachloride solution (400 g/l) are subsequently metered in over the course of 25 minutes, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 20 minutes, and 600 ml of a suspension of 20 g of natural mica flakes from Merck KGaA (particle size<15 μm) and 60 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) in water are metered in over the course of 30 minutes, during which the pH is kept constant using hydrochloric acid. 200 ml of a titanium tetrachloride solution (400 g/l) are subsequently metered in over the course of 2.5 hours, during which the pH is kept at 1.8 using sodium hydroxide solution. After a subsequent stirring time, the pH is set to 5 using sodium hydroxide solution, and the mixture is stirred for a further 15 minutes.

[0157] The batch is filtered off, and the filter residue containing the product is washed with water and dried at 150° C. The powder is subsequently calcined at 800° C. for 45 minutes and then sieved through a sieve having a mesh width of 24 μm.

[0158] A pigment mixture having a white mass tone, a soft skin feel, a matt texture and an elegant shimmer is obtained which can be incorporated extremely well into cosmetic formulations without further effort, such as, for example, grinding or forced dispersion.

Example 4

Pigment Mixture Having a Red Mass Tone

Batch 4A:

[0159] 15 g of natural mica flakes from Merck KGaA (particle size<15 μm) together with 85 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 1500 ml of deionized water. This suspension is heated to the reaction temperature of 75° C. with stirring. The pH is then set to pH 10 using 10% sodium hydroxide solution, kept there for 5 minutes and finally adjusted to the covering pH of 3.1 using 10% hydrochloric acid.

[0160] 838 g of 14% iron chloride solution (170 g of Fe.sub.2O.sub.3/l) are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 15 minutes. The pH is then set to pH 1.8 using 10% HCl, and 956 g of titanium tetrachloride solution (400 g/l, which corresponds to 133 g of TiO.sub.2) are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH=5 using 10% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes.

[0161] When this batch is complete, the suspension is filtered off, washed with deionized water, dried at 110° C. for 10 h and calcined at 800° C. for 30 min.

[0162] This precursor has a composition of 42% of Fe.sub.2O.sub.3, 33% of TiO.sub.2, 21% of SiO.sub.2 and 4% of mica.

Batch 4B:

[0163] 2 l of deionized water are heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 2.8 using 10% hydrochloric acid. 295 g of iron chloride solution (w(Fe)=14%) are subsequently metered in (corresponds to 60 g of Fe.sub.2O.sub.3), during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The batch is not filtered off directly with suction.

[0164] 60 g of the calcined material from batch 4A are subsequently added, and the pH is then set to pH=5 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes. Finally, the suspension is filtered off, washed with 10 l of deionized water and dried at 110° C. for 10 h. Finally, the powder obtained is calcined at 800° C. for 30 min and sieved using a 24 μm sieve.

[0165] The final product has the following composition: 71% of Fe2O3, 16% of TiO2, 11% of SiO.sub.2 and 2% of mica.

[0166] A pigment mixture having a burgundy mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 4A/4B mixing ratio.

Example 4a

[0167] If the 4A:4B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 4b

[0168] If the 4A:4B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 4c

[0169] If the 4A:4B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 5

Pigment Mixture Having a Champagne-Colored Mass Tone

Batch 5A:

[0170] 8 g of aluminum oxide flakes from Merck KGaA (5-40 μm) together with 80 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 800 ml of deionized water. This suspension is heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 2.1 using 10% hydrochloric acid. 2200 g of a 25% titanium tetrachloride solution are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 3.3 using 20% sodium hydroxide solution, and the mixture is stirred for a further 5 minutes. 356 g of a 7% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition of the solution is complete, the mixture is stirred for a further minutes, and the pH is then set to pH 6 using 20% sodium hydroxide solution.

Batch 5B:

[0171] 1.7 l of deionized water are heated to the reaction temperature of 70° C. with stirring, and the pH is then adjusted to 2.1 using 10% hydrochloric acid. 1350 g of a 25% titanium tetrachloride solution are then metered in. The pH is kept constant using 20% sodium hydroxide solution. The pH is then adjusted to pH 3.3 using 20% sodium hydroxide solution, and the mixture is stirred for a further 5 minutes. The pH is subsequently set to 1.9, and 356 g of a 7% iron chloride solution are metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 6 using 20% sodium hydroxide solution.

[0172] When both batches are complete, the suspensions of batches 5A and 5B are mixed, filtered off, washed and dried at 150° C. The pigment mixture is subsequently calcined at 780° C. and then passed through a sieve having a mesh width of 24 μm.

[0173] A champagne- to skin-colored pigment mixture having a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 5A/5B mixing ratio.

Example 5a

[0174] If the 5A:5B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 5b

[0175] If the 5A:5B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 5c

[0176] If the 5A:5B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 6

Pigment Mixture Having a Champagne-Colored Mass Tone

Batch 6A:

[0177] 12 g of natural mica flakes from Merck KGaA (<15 μm) together with 100 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 800 ml of deionized water. This suspension is heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 2.1 using 10% hydrochloric acid. 1856 g of a 25% titanium tetrachloride solution are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 3.3 using 20% sodium hydroxide solution, and the mixture is stirred for a further 5 minutes. 3289 g of a 7% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition of the solution is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 6 using 20% sodium hydroxide solution. The suspension is filtered, washed until salt-free and dried. The dried pigment mixture is calcined at 700° C. under air in a muffle furnace.

Batch 6B:

[0178] 1.7 l of deionized water are heated to the reaction temperature of 65° C. with stirring, and the pH is then adjusted to 2.1 using 10% hydrochloric acid. 1265 g of a 25% titanium tetrachloride solution are then metered in. The pH is kept constant using 20% sodium hydroxide solution. The pH is then adjusted to pH 3.1 using 20% sodium hydroxide solution, and the mixture is stirred for a further 5 minutes. The pH is subsequently set to 2.1, and 564 g of a 7% iron chloride solution are metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 6 using 20% sodium hydroxide solution.

[0179] When both batches are complete, the calcined powder from batch 6A is added to the suspension of batch 6B. The suspension is filtered, washed and dried at 150° C. The powder is subsequently calcined at 780° C. and then passed through a sieve having a mesh width of 24 μm.

[0180] A champagne- to skin-colored pigment mixture having a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 6A/6B mixing ratio.

Example 6a

[0181] If the 6A:6B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 6b

[0182] If the 6A:6B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 6c

[0183] If the 6A:6B ratio is 2:8, highly chromatic pigment mixtures having a very good hiding power and a good skin feel are obtained.

Example 7

Pigment Mixture Having a Champagne-Colored Mass Tone

Batch 7A:

[0184] 15 g of aluminum oxide flakes from Merck KGaA (<20 μm) together with 85 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 800 ml of deionized water.

[0185] This suspension is heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 3.1 using 10% hydrochloric acid. 356 g of a 7% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 2.1 using 20% hydrochloric acid, and the mixture is stirred for a further 5 minutes. 1689 g of a 25% titanium tetrachloride solution are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition of the solution is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 6 using 20% sodium hydroxide solution. The suspension is filtered, washed until salt-free and dried at 140° C.

Batch 7B:

[0186] 1.7 l of deionized water are heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 3.1 using 10% hydrochloric acid. 685 g of a 7% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 2.1 using 10% hydrochloric acid, and 941 g of a 25% titanium tetrachloride solution are metered in. The pH is kept constant using 20% sodium hydroxide solution. The mixture is then stirred for a further 5 minutes, and the pH is adjusted to pH 5 using 20% sodium hydroxide solution.

[0187] When both batches are complete, the calcined powder from batch A is added to the suspension of batch B. The suspension is filtered, washed and dried at 150° C. The powder is subsequently calcined at 550° C. and then passed through a sieve having a mesh width of 24 μm.

[0188] A champagne- to skin-colored pigment mixture having a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 7A/7B mixing ratio.

Example 7a

[0189] If the 7A:7B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 7b

[0190] If the 7A:7B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 7c

[0191] If the 7A:7B ratio is 2:8, highly chromatic pigment having a very high hiding power and a good skin feel are obtained.

Example 8

Pigment Mixture Having a Black Mass Tone

Batch 8A:

[0192] 8 g of synthetic silicon dioxide flakes from Merck KGaA (5-50 μm) together with 80 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm are stirred into 800 ml of deionized water.

[0193] This suspension is heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 3.3 using 10% hydrochloric acid. 923 g of 10% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 2.1 using 10% HCl, and 310 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. During this, the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes.

Batch 8B:

[0194] 1.7 l of deionized water are heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 3.3 using 10% hydrochloric acid. 1000 g of 10% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 7 using 20% sodium hydroxide solution.

[0195] When both batches are complete, the suspensions of batches 8A and 8B are mixed, filtered off, washed and dried at 150° C. The powder is subsequently calcined at 650° C. under forming gas (N.sub.2:H.sub.2 ratio 95:5) and then passed through a sieve having a mesh width of 24 μm.

[0196] An effect pigment having a black mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 8A/8B mixing ratio.

Example 8a

[0197] If the 8A:8B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 8b

[0198] If the 8A:8B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 8c

[0199] If the 8A:8B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 9

Pigment Mixture Having a Black Mass Tone

Batch 9A:

[0200] 15 g of natural mica flakes from Merck KGaA (<15 μm) together with 85 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0201] This suspension is heated to the reaction temperature of 80° C. with stirring, and the pH is then adjusted to 3.1 using 10% hydrochloric acid. 886 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 32% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 2.1 using 10% HCl, and 1240 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes. The suspension is filtered, washed until salt-free and dried. The dried powder is calcined at 800° C. under air in a muffle furnace.

Batch 9B:

[0202] 1.7 l of deionized water are heated to the reaction temperature of 82° C. with stirring, and the pH is then adjusted to 3.2 using 10% hydrochloric acid. 495 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 5 using 20% sodium hydroxide solution.

[0203] When both batches are complete, the calcined powder from batch A is added to the suspension of batch B. The suspension is filtered, washed and dried at 150° C. The combined powder is subsequently calcined at 500° C. under forming gas (N.sub.2:H.sub.2 ratio=92:8) and then passed through a sieve having a mesh width of 24 μm.

[0204] An effect pigment having a black mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 9A/9B mixing ratio.

Example 9a

[0205] If the 9A:9B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 9b

[0206] If the 9A:9B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 9c

[0207] If the 9A:9B ratio is 2:8, highly chromatic pigment mixtures having a very good hiding power and a good skin feel are obtained.

Example 10

Pigment Mixture Having a Black Mass Tone

Batch 10A:

[0208] 10 g of natural mica flakes from Merck KGaA (10-60 μm) together with 85 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0209] This suspension is heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 2.9 using 10% hydrochloric acid. 925 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 32% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 2.1 using 10% HCl, and 1015 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. During this, the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes. The suspension is filtered, washed until salt-free and dried.

Batch 10B:

[0210] 1.7 l of deionized water are heated to the reaction temperature of 70° C. with stirring, and the pH is then adjusted to 3.2 using 10% hydrochloric acid. 750 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 5 using 20% sodium hydroxide solution.

[0211] When both batches are complete, the dried powder from batch A is added to the suspension of batch B. The suspension is filtered, washed and dried at 150° C. The combined powder is subsequently calcined at 760° C. under forming gas (N.sub.2:H.sub.2 ratio=92:8) and passed through a sieve having a mesh width of 24 μm.

[0212] An effect pigment having a black mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 10A/10B mixing ratio.

Example 10a

[0213] If the 10A:10B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 10b

[0214] If the 10A:10B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 10c

[0215] If the 10A:10B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 11

Pigment Mixture Having a Red Mass Tone

Batch 11A:

[0216] 15 g of natural mica flakes from Merck KGaA (5-35 μm) together with 85 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0217] This suspension is heated to the reaction temperature of 80° C. with stirring, and the pH is then adjusted to 3.1 using 10% hydrochloric acid. 886 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 32% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to 2.1 using 10% HCl, and 1240 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. During this, the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes. The suspension is filtered off, washed until salt-free and dried. The dried powder is calcined at 800° C. in a muffle furnace for 30 minutes.

Batch 11B:

[0218] 1.7 l of deionized water are heated to the reaction temperature of 82° C. with stirring, and the pH is then adjusted to 3.2 using 10% hydrochloric acid. 495 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then adjusted to pH 5 using 20% sodium hydroxide solution.

[0219] When both batches are complete, the calcined powder from batch 11A is added to the suspension of batch 11B. The suspension is filtered, washed and dried at 150° C. The combined powder is subsequently calcined at 780° C. and then passed through a sieve having a mesh width of 24 μm.

[0220] An effect pigment having a burgundy mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 11A:11B mixing ratio.

Example 11a

[0221] If the 11A:11B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 11b

[0222] If the 11A:11B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 11c

[0223] If the 11A:11B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 12

Pigment Mixture Having a Red Mass Tone

Batch 12A:

[0224] 10 g of synthetic mica flakes from Merck KGaA (<15 μm) together with 85 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0225] This suspension is heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 2.9 using 10% hydrochloric acid. 925 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 32% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 2.1 using 10% HCl, and 1015 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. During this, the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then adjusted to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 minutes. The suspension is filtered off, washed until salt-free and dried.

Batch 12B:

[0226] 1.7 l of deionized water are heated to the reaction temperature of 70° C. with stirring, and the pH is then adjusted to 3.2 using 10% hydrochloric acid. 750 g of 14% iron chloride solution are subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution.

[0227] When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 5 using 20% sodium hydroxide solution.

[0228] When both batches are complete, the dried powder from batch 12A is added to the suspension of batch 12B. The suspension is filtered, washed and dried at 150° C. The combined powder is subsequently calcined at 780° C. and passed through a sieve having a mesh width of 24 μm.

[0229] A pigment mixture having a burgundy mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 12A/12B mixing ratio.

Example 12a

[0230] If the 12A:12B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 12b

[0231] If the 12A:12B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 12c

[0232] If the 12A:12B ratio is 2:8, highly chromatic pigment mixtures having a very good hiding power and a good skin feel are obtained.

Example 13

Pigment Mixture Having a Yellow Mass Tone

Batch 13A:

[0233] 8 g of synthetic mica flakes from Merck KGaA (10-40 μm) together with 80 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 800 ml of deionized water.

[0234] This suspension is heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 3.5 using 10% sulfuric acid. A solution consisting of 101 g of iron(III) sulfate, 130 g of iron(II) sulfate heptahydrate and 480 g of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 8 using 20% sodium hydroxide solution, after which 150 g of a sodium water-glass solution (w SiO.sub.2=14%) is metered in. During this, the pH is kept constant using 20% sulfuric acid. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 5 using 10% sulfuric acid, and the mixture is stirred for a further 15 min.

Batch 13B:

[0235] 1.7 l of deionized water are heated to the reaction temperature of 87° C. with stirring, and the pH is then adjusted to 3.7 using 10% hydrochloric acid. A solution consisting of 190 g of iron(III) sulfate, 210 g of iron(II) sulfate heptahydrate and 600 g of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then adjusted to pH 7 using 20% sodium hydroxide solution, after which 90 g of a sodium water-glass solution (w SiO.sub.2=14%) is metered in. During this, the pH is kept constant using 20% sulfuric acid. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 5 using 10% sulfuric acid, and the mixture is stirred for a further 15 min.

[0236] When both batches are complete, the suspensions of batches 13A and 13B are mixed, filtered off, washed and dried at 150° C. and passed through a sieve having a mesh width of 24 μm.

[0237] A pigment mixture having a yellow mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 13A/13B mixing ratio.

Example 13a

[0238] If the 13A:13B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 13b

[0239] If the 13A:13B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 13c

[0240] If the 13A:13B ratio is 2:8, highly chromatic pigment mixtures having a very good hiding power and a good skin feel are obtained.

Example 14

Pigment Mixture Having a Yellow Mass Tone

Batch 14A:

[0241] 15 g of synthetic mica flakes Merck KGaA (5-40 μm) together with 85 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0242] This suspension is heated to the reaction temperature of 90° C. with stirring, and the pH is then adjusted to 3.5 using 10% sulfuric acid. A solution consisting of 200 g of iron(III) sulfate, 210 g of iron(II) sulfate heptahydrate and 700 g of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 8 using 20% sodium hydroxide solution, after which 290 g of a sodium water-glass solution (w SiO.sub.2=14%) is metered in. During this, the pH is kept constant using 20% sulfuric acid. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 5 using 10% sulfuric acid, and the mixture is stirred for a further 15 min. The suspension is filtered, washed until salt-free and dried.

Batch 14B:

[0243] 1.2 l of deionized water are heated to the reaction temperature of 75° C. with stirring, and the pH is then adjusted to 3.9 using 10% hydrochloric acid. A solution consisting of 120 g of iron(III) sulfate, 163 g of iron(II) sulfate heptahydrate and 500 g of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then adjusted to pH 7 using 20% sodium hydroxide solution, after which 65 g of a sodium water-glass solution (w SiO.sub.2=14%) is metered in. During this, the pH is kept constant using 20% sulfuric acid. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 6 using 10% sulfuric acid, and the mixture is stirred for a further 15 min.

[0244] When both batches are complete, the dried powder from batch 14A is added to the suspension of batch 14B. The suspension is filtered, washed and dried at 170° C. and passed through a sieve having a mesh width of 24 μm.

[0245] A pigment mixture having a yellow mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 14A/14B mixing ratio.

Example 14a

[0246] If the 14A:14B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 14b

[0247] If the 14A:14B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 14c

[0248] If the 14A:14B ratio is 2:8, highly chromatic pigment mixtures having a very good hiding power and a good skin feel are obtained.

Example 15

Pigment Mixture Having a Green Mass Tone

Batch 15A:

[0249] 8 g of natural mica flakes from Merck KGaA (particle size 10-100 μm) together with 80 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0250] This suspension is heated to the reaction temperature of 70° C. with stirring, and the pH is then adjusted to 5.5 using 10% hydrochloric acid. A solution of 309 g of chromium(III) chloride hexahydrate and 800 ml of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 min.

Batch 15B:

[0251] 2.1 l of deionized water are heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 6.0 using 10% hydrochloric acid. A solution of 556 g of chromium(III) chloride hexahydrate and 1250 ml of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 7 using 20% sodium hydroxide solution.

[0252] When both batches are complete, the suspensions of batches 15A and 15B are mixed, filtered off, washed and dried at 150° C. The powder is subsequently calcined at 800° C. under air and then sieved through a sieve having a mesh width of 24 μm.

[0253] A pigment mixture having a green mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 15A/15B mixing ratio.

Example 15a

[0254] If the 15A:15B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 15b

[0255] If the 15A:15B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 15c

[0256] If the 15A:15B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 16

Pigment Mixture Having a Green Mass Tone

Batch 16A:

[0257] 15 g of natural mica flakes from Merck KGaA (particle size 5-25 μm) together with 85 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 1800 ml of deionized water.

[0258] This suspension is heated to the reaction temperature of 80° C. with stirring, and the pH is then adjusted to 1.8 using 10% hydrochloric acid. 350 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 7 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 min. A solution of 516 g of chromium(III) chloride hexahydrate and 1010 ml of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The suspension is filtered, washed until salt-free and dried. The dried powder is calcined at 800° C. under air in a muffle furnace.

Batch 16B:

[0259] 1.9 l of deionized water are heated to the reaction temperature of 80° C. with stirring, and the pH is then adjusted to 6.0 using 10% hydrochloric acid. A solution of 706 g of chromium(III) chloride hexahydrate and 1200 ml of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 7 using 20% sodium hydroxide solution.

[0260] When both batches are complete, the calcined powder from batch A is added to the suspension of batch B. The suspension is filtered, washed and dried at 150° C. The combined powder is subsequently calcined at 750° C. under air and passed through a sieve having a mesh width of 24 μm.

[0261] A pigment mixture having a green mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 16A/16B mixing ratio.

Example 16a

[0262] If the 16A:16B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 16b

[0263] If the 16A:16B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 16c

[0264] If the 16A:16B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 17

Pigment Mixture Having a Green Mass Tone

Batch 17A:

[0265] 10 g of natural mica flakes from Merck KGaA (particle size <15 μm) together with 100 g of silicon dioxide spheres from ABC Nanotech (diameter 2-4 μm)) are stirred into 1800 ml of deionized water.

[0266] This suspension is heated to the reaction temperature of 80° C. with stirring, and the pH is then adjusted to 2.1 using 10% hydrochloric acid. 200 g of titanium tetrachloride solution (400 g/l) are subsequently metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 7.5 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 min. A solution of 480 g of chromium(III) chloride hexahydrate and 900 ml of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The suspension is filtered, washed until salt-free and dried.

Batch 17B:

[0267] 1.9 l of deionized water are heated to the reaction temperature of 85° C. with stirring, and the pH is then adjusted to 6.5 using 10% hydrochloric acid. A solution of 706 g of chromium(III) chloride hexahydrate and 950 ml of deionized water is subsequently metered in, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then adjusted to pH 7 using 20% sodium hydroxide solution.

[0268] When both batches are complete, the dried powder from batch 17A is added to the suspension of batch 17B. The suspension is filtered, washed and dried at 150° C. The combined powder is subsequently calcined at 850° C. under air and passed through a sieve having a mesh width of 24 μm.

[0269] A pigment mixture having a green mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 17A/17B mixing ratio.

Example 17a

[0270] If the 17A:17B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 17b

[0271] If the 17A:17B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 17c

[0272] If the 17A:17B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 18

Pigment Mixture Having a White Mass Tone

Batch 18A:

[0273] 20 g of natural mica flakes from Merck KGaA (particle size 10-60 μm) together with 65 g of silicon dioxide spheres from Sinoenergy (diameter 2-4 μm) are stirred into 1200 ml of deionized water.

[0274] This suspension is heated to the reaction temperature of 75° C. with stirring, and the pH is then adjusted to 2.0 using 10% hydrochloric acid. 150 g of 10% tin(IV) chloride solution are subsequently metered in over the course of 45 min, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. 1300 g of 12% titanium tetrachloride solution are then metered in over the course of 6 hours. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes. The pH is then set to pH 6 using 20% sodium hydroxide solution, and the mixture is stirred for a further 15 min.

Batch 18B:

[0275] 1.5 l of deionized water are heated to the reaction temperature of 75° C. with stirring, and the pH is then adjusted to pH 3.0 using 10% hydrochloric acid. 1900 g of 14% titanium tetrachloride solution are subsequently metered in over the course of 4 hours, during which the pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then set to pH 7 using 20% sodium hydroxide solution.

[0276] When both batches are complete, the suspensions of batches 18A and 18B are mixed, filtered off, washed with water and dried at 150° C. The powder is subsequently calcined at 800° C. for 45 min and then passed through a sieve having a mesh width of 100 μm.

[0277] A pigment mixture having a white mass tone, a soft skin feel, a matt texture and an elegant shimmer is obtained which can be incorporated extremely well into cosmetic formulations without further effort, such as, for example, grinding or forced dispersion. The hiding power, skin feel and luminance (shimmer) can be adjusted as desired through the 18A/18B mixing ratio.

Example 18a

[0278] If the 18A:18B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 18b

[0279] If the 18A:18B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 18c

[0280] If the 18A:18B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 19

Pigment Mixture Having a Blue Mass Tone

Batch 19A:

[0281] 8 g of glass flakes from Merck KGaA (particle size 10-100 μm together with 80 g of silicon dioxide spheres from ABC Nanotech (diameter: 2-4 μm)) are stirred into 800 ml of deionized water.

[0282] This suspension is heated to the reaction temperature of 75° C. with stirring. The pH is adjusted to 2.1 by means of 10% sulfuric acid, and 2200 g of a 25% titanium tetrachloride solution are then metered in. The pH is kept constant using 20% sodium hydroxide solution. When the addition is complete, the mixture is stirred for a further 5 minutes, and the pH is then adjusted to 4.3 using 10% sulfuric acid. Two solutions 1 and 2 are subsequently added simultaneously, while the pH is kept constant using a 10% ammonium carbonate solution. Solution 1 is prepared from 60 g of potassium hexacyanoferrate(III) and 1300 g of deionized water. Solution 2 consists of 76 g of iron sulfate heptahydrate and 1250 g of deionized water. When the addition is complete, the mixture is stirred for a further 15 min, and the pH is then set to pH 6 using 20% sodium hydroxide solution.

Batch 19B:

[0283] 900 ml of deionized water are heated to the reaction temperature of 73° C. with stirring, and the pH is then adjusted to 4.3 using 10% sulfuric acid. Two solutions 1 and 2 are subsequently added simultaneously, while the pH is kept constant using a 10% ammonium carbonate solution. Solution 1 is prepared from 165 g of potassium hexacyanoferrate(III) and 2100 g of deionized water. Solution 2 consists of 209 g of iron sulfate heptahydrate and 1950 g of deionized water. The pH is then set to pH 6 using 20% sodium hydroxide solution.

[0284] When both batches are complete, the suspensions of batches 1A and 1B are mixed, filtered off, washed and dried at 150° C. and then passed through a sieve having a mesh width of 24 μm.

[0285] A pigment mixture having a blue mass tone and a soft skin feel and matt texture is obtained which has a high chroma and can be incorporated extremely well into cosmetic formulations without further effort. The hiding power, skin feel and chroma can be adjusted as desired through the 19A/19B mixing ratio.

Example 19a

[0286] If the 19A:19B ratio is 8:2, particularly highly chromatic pigment mixtures having an extraordinarily good skin feel and a moderate hiding power are obtained.

Example 19b

[0287] If the 19A:19B ratio is 1:1, particularly highly chromatic pigment mixtures having a very good skin feel and a medium hiding power are obtained.

Example 19c

[0288] If the 19A:19B ratio is 2:8, highly chromatic pigment mixtures having a very high hiding power and a good skin feel are obtained.

Example 20

Pigment Mixture Having a White Mass Tone

[0289] 1500 ml of deionized water are initially introduced in a heatable reaction vessel and heated to 75° C., and 376 g of TiOCl.sub.2 solution (400 g of TiCl.sub.4/liter) are metered in at this temperature at a metering rate of 5 ml/min. with vigorous stirring. The pH drops in the process and is kept constant at 2.0 by controlled addition of 32% sodium hydroxide solution. When the addition of TiOCl.sub.2 is complete, the mixture is stirred at pH 2.0 for 15 min. A homogeneous suspension of 75 g of mica flakes (particle size 1-15 μm) and 25 g of SiO.sub.2 spheres (D.sub.50=2-4 μm; SILNOS 130 from ABC Nanotech Co., Ltd.) in 250 ml of deionized water is subsequently added, and, when 75° C. is re-attained, the pH is lowered to 2.2 using hydrochloric acid (18% HCl). While keeping the temperature and pH constant using 32% sodium hydroxide solution, a homogeneous solution of 8.64 g of SnOCl.sub.2 solution (50% SnCl.sub.4), 22.8 g of hydrochloric acid (37% HCl) and 167 g of deionized water is metered in at a uniform rate over the course of 30 min. After a subsequent stirring time of 15 min., 740 g of TiOCl.sub.2 solution (400 g of TiCl.sub.4/liter) are added at a metering rate of 5 ml/min. During this, the pH is kept constant at 2.2 using 32% sodium hydroxide solution. When the addition of the TiOCl.sub.2 solution is complete, the mixture is stirred for a further 15 min., the pH is then adjusted to pH 5.0 using 32% sodium hydroxide solution, and the mixture is stirred for a further 15 min.

[0290] The solid obtained is filtered off, washed with 15 l of deionized water and dried at 110° C. for 16 hours. The product is subsequently calcined at 850° C. for 30 min. and sieved through a sieve having a mesh width of 100 μm.

[0291] A white powder having a very soft skin feel is obtained which exhibits a slight bluish luster when spread on the skin.

Use Examples

Example A1

Eye Shadow Gel

[0292]

TABLE-US-00001 Raw material INCI [%] Phase A Timiron ® Super (1) MICA FLAKES FROM MERCK 15.00 Gold KGAA, CI 77891 (TITANIUM DIOXIDE) Pigment mixture 7.00 from Example 1 Carbopol Ultrez (2) ACRYLATES/C10-30 ALKYL 0.30 21 ACRYLATE CROSSPOLYMER Aloe vera powder (3) ALOE BARBADENSIS 0.05 regular 200x Citric acid (1) CITRIC ACID 0.00 monohydrate Water, AQUA (WATER) 55.87 demineralized Phase B Triethanolamine (4) TRIETHANOLAMINE, AQUA 0.78 90% Care (WATER) Germaben II (5) PROPYLENE GLYCOL, 1.00 DIAZOLIDINYL UREA, METHYLPARABEN, PROPYLPARABEN Glycerin, (1) GLYCERIN 2.00 anhydrous Water, AQUA (WATER) 13.00 demineralized Phase C Lubrajel DV (6) PROPYLENE GLYCOL, 5.00 POLYGLYCERYL METHACRYLATE

Preparation:

[0293] Dissolve the aloe vera powder in the water of phase A, then add all pigments and the pigment mixture and the remaining ingredients apart from the Carbopol and disperse. Acidify using a few drops of citric acid in order to reduce the viscosity, then scatter in the Carbopol with stirring. When completely dissolved, slowly stir in the pre-dissolved phase B (do not homogenize), and subsequently add phase C. If necessary, adjust the pH to between 7.0-7.5 using citric acid solution.

[0294] A water-based eye shadow gel formulation containing aloe vera is obtained (extremely fast-drying and easy to apply using the fingers).

Sources of Supply:

[0295] (1) Merck KGaA/Rona®

[0296] (2) Noveon

[0297] (3) Terry Laboratoires, Inc.

[0298] (4) BASF AG

[0299] (5) ISP Global Technologies

[0300] (6) Guardian

Example A2

Creamy Eye Shadow

[0301]

TABLE-US-00002 Raw material INCI [%] Phase A Colorona ® Light (1) MICA FLAKES FROM 10.00 Blue MERCK KGAA, CI 77891 (TITANIUM DIOXIDE) CI 77510 (FERRIC FERROCYANIDE) Pigment mixture 15.00 from Example 1 Talc (1) TALC 12.00 Phase B Crodamol PMP (2) PPG-2 MYRISTYL ETHER 32.80 PROPIONATE Miglyol 812 N (3) CAPRYLIC/CAPRIC 12.00 TRIGLYCERIDE Syncrowax HGLC (2) C18-36 ACID 10.00 TRIGLYCERIDE Syncrowax HRC (2) TRIBEHENIN 3.00 Parteck ® LUB STA (1) STEARIC ACID 3.00 Antaron V-216 (4) PVP/HEXADECENE 2.00 COPOLYMER Oxynex ® K liquid (1) PEG-8, TOCOPHEROL, 0.10 ASCORBYL PALMITATE, ASCORBIC ACID, CITRIC ACID Propyl 4-hydroxy- (1) PROPYLPARABEN 0.10 benzoate

Preparation:

[0302] Heat phase B to about 80° C. until everything has melted and cool to 65° C. with stirring. Then add the ingredients of phase A with stirring, and pour the composition into the packaging provided at 65° C. Allow to cool to room temperature.

Sources of Supply:

[0303] (1) Merck KGaA/Rona®

[0304] (2) Croda GmbH

[0305] (3) Sasol Germany GmbH

[0306] (4) ISP Global Technologies

Example A3

Face Powder

[0307]

TABLE-US-00003 Raw material INCI [%] Phase A Pigment mixture 20.00 from Example 5 Unipure Yellow LC (1) CI 77492 (IRON OXIDES) 1.20 182 Unipure Red LC (1) CI 77491 (IRON OXIDES) 0.20 381 Unipure Brown LC (1) CI 77491 (IRON OXIDES) 0.30 889 CI 77499 (IRON OXIDES) Magnesium (2) MAGNESIUM STEARATE 2.00 stearate Talc (2) TALC 71.90 Phase B RonaCare ® (2) TOCOPHERYL ACETATE 0.30 all-rac-alpha- tocopheryl acetate Perfume oil 200 (3) PERFUME 0.30 529 Eutanol G (4) OCTYLDODECANOL 3.70 Propyl 4-hydroxy- (2) PROPYLPARABEN 0.10 benzoate

Preparation:

[0308] Add the constituents of phase A to the mixer (for example La Moulinette from Moulinex) and mix for 2×10 seconds. Transfer the mixture into a beaker, add phase B, and stir in advance using the spatula. Again add the mixture of phase A and phase B to the mixer and process for 3×10 seconds to give a homogeneous phase.

[0309] The pressing pressure for a powder tray having a diameter of 36 mm is about 25 bar.

Sources of Supply:

[0310] (1) Les Colorants Wackherr

[0311] (2) Merck KGaA/Rona®

[0312] (3) Fragrance Resources

[0313] (4) Cognis GmbH

Example A4

Mattifying Foundation

[0314]

TABLE-US-00004 Raw material INCI [%] Phase A Water, AQUA (WATER) 57.89 demineralized Pigment mixture 6.00 from Example 13 Glycerin (87% (1) GLYCERIN, AQUA (WATER) 5.00 extra pure) RonaCare ® ectoin (1) ECTOIN 0.30 Keltrol CG-SFT (2) XANTHAN GUM 0.15 Triethanolamine (3) TRIETHANOLAMINE, AQUA 0.13 90% Care (WATER) Phase B Kronos 1001 (4) CI 77891 (TITANIUM 4.92 DIOXIDE) Unipure Yellow (5) CI 77492 (IRON OXIDES) 1.60 LC 182 Unipure Red LC (5) CI 77491 (IRON OXIDES) 0.20 381 Unipure Brown (5) CI 77491 (IRON OXIDES) 0.20 LC 889 CI 77499 (IRON OXIDES) Unipure Blue LC (5) CI 77007 (ULTRAMARINE 0.08 686 BLUE) Phase C Miglyol 812N (6) CAPRYLIC/CAPRIC 7.00 TRIGLYCERIDE Eutanol G (7) OCTYLDODECANOL 4.00 Montanov 202 (8) ARACHIDYL ALCOHOL, 4.00 BEHENYL ALCOHOL, ARACHIDYLGLUCOSIDE Avocado oil (9) PERSEA GRATISSIMA 2.00 (AVOCADO OIL) Eusolex ® 9020 (1) BUTYL 1.50 METHOXYDIBENZOYL- METHANE Hydrolite-5 (10)  PENTYLENE GLYCOL 1.20 Bentone gel (11)  STEARALKONIUM 1.00 GTCC V HECTORITE, PROPYLENE CARBONATE, CAPRYLIC/CAPRIC TRIGLYCERIDE RonaCare ® (2) TOCOPHERYL ACETATE 0.50 all-rac-alpha- tocopheryl acetate Phenonip (12)  PHENOXYETHANOL, 0.40 BUTYLPARABEN, ETHYLPARABEN, PROPYLPARABEN, METHYLPARABEN Oxynex ® K liquid (1) PEG-8, TOCOPHEROL, 0.03 ASCORBYL PALMITATE, ASCORBIC ACID, CITRIC ACID Phase D Simulgel EG (8) SODIUM ACRYLATE/ 0.60 SODIUM ACRYLOYL- DIMETHYLTAURATE COPOLYMER, ISOHEXADECANE, POLYSORBATE 80 Phase E Water, AQUA (WATER) 1.00 demineralized

Preparation:

[0315] Add the Keltrol slowly to the water of phase A and disperse. Scatter in the remaining constituents of phase A with stirring. Add the constituents of phase B to phase A and homogenize using the Ultra-Turrax T25 (red-blue setting, 13500-20500 rpm) for 3 min and check for agglomerates. Heat phase A/B and phase C separately to 75° C. Add phase C to phase A/B with stirring and homogenize for 2 min using the Ultra-Turrax T25 (yellow-green setting, 8000-9500 rpm). Add phase D at between 55 and 60° C., add phase E at 40° C., and cool to room temperature with further stirring; adjust the pH to 7.0 using 30% citric acid. Then transfer into suitable containers. A light, slightly opaque foundation is obtained which is suitable for all skin types. Avocado oil, vitamin E acetate and cell-protecting RonaCare® ectoin support the skin-care action.

Sources of Supply:

[0316] (1) Merck KGaA/Rona®

[0317] (2) C.P. Kelco

[0318] (3) BASF AG

[0319] (4) Kronos International Inc.

[0320] (5) Les Colorants Wackherr

[0321] (6) Sasol Germany GmbH

[0322] (7) Cognis GmbH

[0323] (8) Seppic

[0324] (9) Gustav Heess GmbH

[0325] (10) Symrise

[0326] (11) Elementis Specialities

[0327] (12) Clariant GmbH

Example A5

Body Lotion

[0328]

TABLE-US-00005 Raw material INCI [%] Phase A Aloe vera gel 10x (1) ALOE BARBADENSIS 2.00 decolorized D-Panthenol (2) PANTHENOL 0.40 Pigment mixture 6.00 from Example 3 RonaCare ® (3) ALLANTOIN 0.20 allantoin Glycerin, (3) GLYCERIN 4.00 anhydrous Water, AQUA (WATER) 67.57 demineralized Phase B Protelan AGL (4) SODIUM COCOYL 6.00 95/C GLUTAMATE Cosmacol EMI (5) DI-C12-13 ALKYL MALATE 3.00 Eutanol G (6) OCTYLDODECANOL 3.00 Jojoba oil (7) SIMMONDSIA CHINENSIS 1.50 (JOJOBA OIL) Tegosoft TN (8) C12-15 ALKYL BENZOATE 1.50 Carbopol ETD (9) ACRYLATES/C10-30 ALKYL 0.60 2020 ACRYLATE CROSSPOLYMER Phenonip (10)  PHENOXYETHANOL, 0.60 BUTYLPARABEN, ETHYLPARABEN, PROPYLPARABEN, METHYLPARABEN RonaCare ® (3) BISABOLOL 0.50 bisabolol RonaCare ® all- (3) TOCOPHERYLACETATE 0.50 rac-alpha- tocopheryl acetate Oxynex ® ST liquid (3) DIETHYLHEXYL 0.50 SYRINGYLIDENEMALONATE, CAPRYLIC/CAPRIC TRIGLYCERIDE Cremophor RH (11)  PEG-40 HYDROGENATED 0.30 410 CASTOR OIL Oxynex ® K liquid PEG-8, TOCOPHEROL, 0.03 ASCORBYL PALMITATE, ASCORBIC ACID, CITRIC ACID Phase C Lifetime (12)  PERFUME 0.50 DH10255/1 perfume oil Phase D Water, AQUA (WATER) 1.00 demineralized Germal 115 (13)  IMIDAZOLIDINYL UREA 0.30

Preparation:

[0329] Pre-dissolve the aloe vera and RonaCare® allantoin in the water of phase A with stirring, then add the other constituents of phase A and heat to 60° C. Introduce the jojoba oil, Oxynex K liquid, Cosmacol EMI, Eutanol G and Tegosoft TN into a stirred vessel, then incorporate the Carbopol homogeneously using the disperser disc (about 700 rpm, 20 min). Then add the remaining constituents of phase B, and stir everything to give a homogeneous mixture, only adding the Protelan AGL 95/C right at the end of phase B in order to prevent excessive incorporation of air. Slowly emulsify phase A into phase B (RT) at 60° C. with the aid of the disperser disc. Add phases C and D, then homogenize for 4 min using the Ultra-Turrax T50, speed 4. Cool to room temperature.

[0330] pH (23° C.) =5.5-6.0

[0331] Viscosity: Brookfield DV II+Helipath, spindle C, 5 rpm, 24° C.=11200 mPa.Math.s

Sources of Supply:

[0332] (1) Terry Laboratoires

[0333] (2) Alfa Aesar GmbH & Co. KG

[0334] (3) Merck KGaA/Rona®

[0335] (4) Zschimmer & Schwarz GmbH & Co.

[0336] (5) Nordmann, Rassmann GmbH & Co.

[0337] (6) Cognis GmbH

[0338] (7) Gustav Heess GmbH

[0339] (8) Evonik Goldschmidt GmbH

[0340] (9) Noveon

[0341] (10) Clariant GmbH

[0342] (11) BASF AG

[0343] (12) Parfex

[0344] (13) ISP Global Technologies

Example A6

Nail Varnish

[0345]

TABLE-US-00006 Raw material INCI [%] Pigment mixture (1) 2.00 from Example 8 Thixotropic nail (2) ETHYL ACETATE, BUTYL 98.00 varnish base 12897 ACETATE, NITROCELLULOSE, PHTHALIC ANHYDRIDE/TRIMETLLITIC ANHYDRIDE/GLYCOLS COPOLYMER, ACETYL TRIBUTYL CITRATE, ISOPROPYL ALCOHOL, STEARALKONIUM HECTORITE, ADIPIC ACID/NEOPENTYL GLYCOL/TRIMELLITIC ANYHDRIDE COPLYMER

Preparation:

[0346] The pigment mixture from Example 1 is weighed out together with the varnish base, mixed well and subsequently stirred at 1000 rpm for 10 minutes.

Sources of Supply:

[0347] (1) Merck KGaA

[0348] (2) International Lacquers S.A.

Example A7

Lipstick

[0349]

TABLE-US-00007 Raw material INCI [%] Phase A Pigment mixture (1) 15.00 from Example 4 Phase B Oxynex ® K liquid (1) PEG-8, TOCOPHEROL, 0.05 ASCORBYL PALMITATE, ASCORBIC ACID, CITRIC ACID Sensiva ® PA 20 (2) PHENETHYL ALCOHOL, 1.00 ETHYLHEXYL GLYCERIN Viscous paraffin (1) PARAFFINUM LIQUIDUM 2.10 Adeps lanae (3) LANOLIN 3.50 Paracera C 44 (4) COPERNICIA CERIFERA, 5.25 CERESIN Isopropyl myristate (5) ISOPROPYL MYRISTATE 5.60 White wax (1) CERA ALBA 8.75 Castor oil (3) RICINUS COMMUNIS 58.75 (CASTOR) SEED OIL

Preparation:

[0350] Heat the constituents of phase B to about 75° C. until everything has melted Add phase A and stir well. Cool the lipstick composition to 65° C. and stir until the phase is free from air bubbles. Pour the homogeneous melt into the casting molds preheated to 55° C. Subsequently cool the molds and remove the cold castings. Warm the lipsticks to room temperature and then briefly flame-treat the lipsticks.

Sources of Supply:

[0351] (1) Merck KGaA

[0352] (2) Schülke & Mayr GmbH

[0353] (3) Henry Lamotte Oils GmbHSasol Germany GmbH

[0354] (4) Azelis Germany GmbH

[0355] (5) BASF AG

[0356] The entire disclosures of all applications, patents and publications, cited herein and of corresponding European Application No. DE 102016004164.1, filed Apr. 11, 2016 are incorporated by reference herein.

[0357] Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent. The preceding preferred specific embodiments are, therefore, to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.

[0358] The preceding examples can be repeated with similar success by substituting the generically or specifically described reactants and/or operating conditions of this invention for those used in the preceding examples.

[0359] From the foregoing description, one skilled in the art can easily ascertain the essential characteristics of this invention and, without departing from the spirit and scope thereof, can make various changes and modifications of the invention to adapt it to various usages and conditions.