WO2007093334A1

WO2007093334A1 - Cosmetic comprising coloured effect pigments and method of producing it

Info

Publication number: WO2007093334A1
Application number: PCT/EP2007/001150
Authority: WO
Inventors: Michael Gruener; Günter KAUPP
Original assignee: Eckart Gmbh
Priority date: 2006-02-13
Filing date: 2007-02-10
Publication date: 2007-08-23
Also published as: DE102006006716A1; EP1986595A1

Abstract

The invention relates to a cosmetic comprising one or more coloured effect pigments, the cosmetic comprising (a) an effect pigment A having an aluminium-containing core, with a colouring, enveloping layer of aluminium oxide, aluminium hydroxide and/or aluminium oxide hydrate, produced on the surface by wet-chemical oxidation of the aluminium-containing core, and/or (b) an effect pigment B having a core enveloped by at least one metal oxide layer, the at least one metal oxide layer comprising at least one colour pigment. The invention further relates to the production of a cosmetic of this kind.

Description

Cosmetic containing colored effect pigments and method for its

manufacturing

The present invention relates to a cosmetic containing colored effect pigments and a process for producing the same.

Cosmetics protect skin, hair, fingernails and toenails, eyes and lips from mechanical damage, dehydration and infections. Often, however, in addition to the caring and protective aspect, a certain optical effect should also be achieved, for example by adding colorants and / or effecting agents. These coloring and effecting agents may be dyes, laked organic dyes, inorganic or organic pigments and / or effect pigments.

Effect pigments are understood as meaning pigments which have a directional reflection on predominantly flat, oriented metallic or strongly refractive particles (DIN 55944). They are always platelet-shaped and have very large particle diameter compared to color pigments. Their optical properties are determined by reflection and interference. The most commonly used effect pigments are platelet-like aluminum pigments, also referred to as aluminum flakes, and coated mica platelets, the platelet-like aluminum pigments exhibiting typical metallic luster and coated mica platelets having typical pearlescence.

In recent years, the demand for colored effect pigments in a wide variety of fields has increased sharply. For example, oxide-coated copper and brass plates, transition metal oxide-coated substrates such as muscovite, phlogopite or glass, guanine single crystals (fish silver), BiOCl single crystals, platelet-shaped hematite single crystals, platelet-shaped phthalocyanines or comminuted thin multi-layer films having Fabry-Perrot structure are used as effect pigments ,

US-4,328,042 and EP-A-0033457 describe the preparation of gold-colored Pigments by deposition of iron oxide on aluminum, wherein iron pentacarbonyl is oxidized in a fluidized bed of aluminum flakes produced by fluidization with inert gas with oxygen.

US Pat. No. 5,037,475 describes the preparation of aluminum pigments colored by fixing color pigments on the metal surface. The fixing of the color pigments via carboxyl-containing polymers. To improve the adhesion, a protective layer can be applied by polymerization. However, the pigments thus produced have only a low color intensity.

WO 91/04293 (PCT / US90 / 05236) describes the coloring of aluminum pigments by fixing polymer-coated color pigments from aqueous solvents via electrostatic forces on the metal surfaces. The coating result depends in a complex manner on the type of aluminum pigment, the type of polymer coating of the color pigments, the solvent composition and the pH.

EP-A-0 328 906 discloses titanium dioxide-coated metal pigments, including aluminum pigments whose preparation is obtained by hydrolysis of an organic titanate ester compound, e.g. As tetraisopropoxytitanium, in the presence of suspended in an organic medium metal plate at pH 4 to 8 takes place. Different shades can be achieved with this method by varying the thickness of the titanium dioxide layer. Compliance with specific conditions is crucial for the production of the coated pigments. The pH must be in the range of 4 to 8, and the dropping rate in the addition of the titanate ester must be in the range of 1, 0 × 10 -7 to 1, 0 × 10 -4 mole per minute and m ^{2 of} metal surface. Therefore, this method is not industrially applicable. In addition, the coated pigments must be calcined after drying in order to achieve color effects, as only by removing the water from the metal oxide layer, a suitable layer structure is formed. However, because of the low melting point of aluminum, calcination of coated aluminum pigments is very poorly possible. US Pat. No. 4,978,394 describes the production of titanium dioxide-coated aluminum pigments by chemical vapor deposition (CVD), in which titanium tetrachloride is reacted at low concentration with steam in a fluidized fluidized bed in the presence of hot aluminum particles.

U.S. 4,158,074 discloses the preparation of colored aluminum pigments by coating with a film of hydrated alumina and hydrated metal oxide. The film is produced by treating fine aluminum flakes in alkaline solution of an iron-nickel, cobalt, zinc or copper salt at elevated temperature at pH 8 to 12, i. H. by an electrochemical reaction of the metal salts. For example, gold-colored pigments and black-brown and greyish-white pigments can be produced by the addition of chelating agents.

DE-PS 25 57 796 discloses colored metal pigments coated with a metal oxide layer containing carbon black as a color pigment. The disclosed pigments are either deep black pigments or colored pigments with special color effects.

DE-OS 36 17 430 describes platelet-shaped colored pigments in which a platelet-shaped substrate is covered with an iron oxide-containing glossy layer.

DE-OS 42 23 383 relates to luster pigments with metallallsulfidhaltiger coating based on coated platelet-shaped silicate or metallic substrates. As metallic substrates, all platelet-form metals known for metallic effect pigments are disclosed, in particular copper and its alloys, such as brass or bronzes, and above all aluminum and its alloys, such as aluminum bronzes. For the production of colored pigments exhibiting interference colors, the substrate particles may already be coated with a layer of high refractive index metal oxide on which the metal sulfide-containing layer is preferably applied to the substrate via the gas phase.

DE-OS 42 23 384 discloses luster pigments based on metal oxide coated Aluminum platelets with a total carbon content of <0.1% by weight. Titanium, zirconium, tin and chromium oxide are mentioned as preferred oxides of the metal oxide layer, as well as iron oxide.

JP-1-110568 discloses a colored aluminum powder pigment obtained by hydrolyzing a metallic alkoxide such as tetraethyl titanate, coating the surface of an aluminum powder with the resulting hydrolysis product and further heating the obtained powder to a temperature of> 200 ^° C and below the ignition point of the aluminum powder becomes.

US Pat. No. 5,261,955 describes a sol-gel process for producing colored metallic pigments wherein the metal platelets are dispersed in a sol of an inorganic salt, e.g. An aqueous alkaline zirconia sol, which is coated with the sol-coated platelets after filtration in a solution of an inorganic compound, e.g. As cobalt nitrate, are dispersed in an organic solvent, and formed by heating a sol-gel layer on the platelets. Due to the large number of individual steps, a high outlay on equipment is also required in this method.

JP-A-61-1 30375 discloses a gold-colored aluminum pigment prepared by treating aluminum powder with dichromate, sodium fluoride and surfactants in acidic solution, drying and then treating with a fatty acid derivative. Colors other than gold can not be achieved with this method.

US 3,067,052 discloses colored aluminum pigments which are prepared by oxidation of aluminum powder with KMnO-i solution, optionally with the addition of a reducing agent. The hue of these pigments is golden, optionally also depending on the reducing agent used with greenish or reddish clay.

DE 103 61 436 describes colored platelet-shaped metal pigments which on a base pigment of metal, a layer of silicon dioxide and subsequently a or more layers containing coloring materials. A disadvantage of the pigments obtainable according to this application is their low abrasion resistance which renders them useless for certain applications. According to the present process, one process step is less to carry out, and the incorporation of the color pigments into the metal oxide layer achieves better adhesion of the layer and increased shear stability of the pigments.

DE 41 40 295 finally describes pigments consisting of a platelet-shaped carrier material which is coated by an inorganic matrix in which metal oxide or dye particles are contained in the sub-micron range.

The object of the present invention is to find further uses for colored effect pigments, in particular to provide a cosmetic with new coloristic properties.

Another object of the invention is to provide a cosmetic in which there is no bleeding effects and no bleeding effects even after prolonged storage.

The object underlying the invention is achieved by providing a cosmetic containing one or more colored effect pigments, wherein the cosmetic

(A) an effect pigment A having an aluminum-containing core with a by wet-chemical oxidation of the aluminum-containing core surface produced coloring enveloping layer of alumina, aluminum hydroxide and / or alumina hydrate and / or

(b) an effect pigment B having a core coated with at least one metal oxide layer, wherein at least one color pigment is contained in the at least one metal oxide layer.

The inventors have surprisingly found that the effect pigments A and the effect pigments B are particularly suitable for use in cosmetics. Especially A combination of effect pigments A and effect pigments B can produce extraordinarily interesting and attractive color effects. This applies in particular when, in addition to the effect pigment A _1, which is an aluminum effect pigment, pearlescent pigments are used as effect pigment B. The bright colored mirror gloss of the colored aluminum effect pigments and the pearlescent effect produced by pearlescent pigments produce unusual color effects in cosmetics.

It has surprisingly been found that, in particular in the case of the mixtures of effect pigment A and effect pigment B, no aggregation and / or segregation phenomena occur. Rather, a very important for the visual impression homogeneous distribution of effect pigment A and effect pigment B is obtained.

Furthermore, the cosmetics according to the invention have a very high stability. The color pigments are reliably embedded in the metal oxide layers, so that there is no separation of the color pigment and the effect pigment even after prolonged storage at elevated temperatures, which may, for example, lead to an undesirable streaking or color change of the cosmetic.

Pigments usable in the present invention are exemplified by

Patent DE 195 20 312, which is hereby incorporated by reference.

From DE 195 01 307 basically colored aluminum pigments are known, in which case industrial color pigments without express permission to cosmetics

Coloring be used.

Preferred developments of the cosmetic according to the invention are specified in the subclaims 2 to 14.

The object underlying the invention is further achieved by a method for producing a cosmetic according to claim 15, wherein the effect pigment A and / or effect pigment B is incorporated in a suitable manner in a carrier system of a cosmetic.

Preferred developments of the method according to the invention are specified in the subclaims 16 to 28.

The formulation of the cosmetics is carried out using methods and measures familiar to the person skilled in the art.

The cosmetics according to the invention are in particular in the form of a cream, lotion, eye shadow, nail polish, lipstick, lip gloss, a mascara, a gel, a make-up formulation, a self-tanning cream or a self-tanning lotion.

According to the invention, "effect pigment" is understood to mean both an effect pigment and several effect pigments.

The core of effect pigment B is preferably platelet-shaped metal pigments selected from the group consisting of aluminum, copper, zinc, silver, gold, iron, titanium, brass, bronze, and alloys of these materials. Furthermore, the core may consist of pearlescent pigments or glass-based pearlescent pigments or mixtures thereof.

Pearlescent pigments are to be understood as meaning those pigments which have a high-indexing coating, for example of titanium dioxide or iron oxide, on a carrier material which may be, for example, mica, SiO ₂ , aluminum oxide or glass. Furthermore, this coating may contain tin oxide or chromium oxide. Of course, it is also possible to apply several layers with different metal oxides and / or metal hydroxides and / or metal oxide hydrates.

The carrier material used is preferably mica, which is coated with titanium dioxide. The use of glass-based metallic effect pigments as a core is also possible. These pigments consist of platelet-shaped glass which is provided with a metal layer, preferably a semitransparent metal layer, for example of silver, gold, aluminum or iron.

Preferably metallic effect pigments are used for the core, since these have better coverage compared to pearlescent pigments.

These metallic effect pigments preferably have a metallic core of aluminum with a particle size of 100% <75 μm and of 95% <45 μm. The content of mercury is usually 1 ppm or less, arsenic is 3 ppm or less, lead is 20 ppm or less, and the aluminum content is usually 99% by weight or more.

The metallic core of a bronze pigment preferably has a copper content of 70 to 95% by weight, a zinc content of 30% by weight or less, and an aluminum and tin content of 0.5% by weight or less.

For a copper pigment, the metallic core usually has a copper content of 95% by weight or more.

In general, it is advantageous that the degree of purity of the metals used in each case at least 99.0 wt .-%, preferably at least 99.5 wt .-%, more preferably at least 99.7 wt .-%, particularly preferably at least 99.9 wt. -%, in each case based on the total weight of metal.

The core of the colored effect pigment A or B to be used according to the invention is preferably a metallic effect pigment which preferably has a thickness of from 10 nm to 2 μm, more preferably from 40 nm to 500 nm. Furthermore, it is preferable that the thickness is in a range of 60 to 250 nm.

The aluminum core of the effect pigment A or B used in the cosmetic according to the invention particularly preferably has an average thickness of 10 to 225 nm, preferably 15 to 200 nm, preferably 20 to 150 nm and furthermore preferably from 25 to 100 nm. These may be PVD pigments or extremely thin pigments produced by milling, as described, for example, in DE 103 15 775 A1. This document is hereby incorporated by reference.

The aluminum-containing core of the effect pigment A preferably also has a thickness of from 10 nm to 2 μm, more preferably from 40 nm to 500 nm, prior to the oxidation. Furthermore, it is preferable that the thickness is in a range of 60 to 250 nm.

In the case of the effect pigment A, the aluminum-containing core or aluminum core is oxidized by wet-chemical means, so that a coloring layer of aluminum oxide, aluminum hydroxide and / or aluminum oxide hydrate surrounding the core is formed. This alumina and / or aluminum hydroxide and / or alumina hydrate layer grows into the aluminum-containing or aluminum core and therefore adheres very firmly to the core. Depending on the extent of the oxidation, different colors can be produced. The aluminum or aluminum alloy pigments obtainable by wet-chemical oxidation are described in DE 195 20 312 A1, which is hereby incorporated by reference.

Preferably, the effect pigment A used in the cosmetic according to the invention has an aluminum core with an average thickness of 10 to 225 nm after the oxidation and an optically non-homogeneous, firmly adhering, with the aluminum core intimately connected alumina / hydroxide / oxide hydrate- layer, which is produced by wet-chemical oxidation of the aluminum core by water in predominantly alcoholic medium. This oxide / hydroxide / oxide hydrate layer has a porosity which manifests itself, for example, in an increase in the specific surface area of at least 2.5 times that of the unoxidized aluminum pigment.

The layer thickness of the layer of aluminum oxide, hydroxide and / or oxide hydrate depends on the degree of oxidation of the aluminum and on the layer thickness of the aluminum pigment used. It is preferably 20 to 500 nm, preferably 35 to 300 nm, more preferably 50 to 200 nm and most particularly preferably 60 to 150 nm. The color of this pigment is in the yellowish to brown color range.

The effect pigment B according to claim 1 consists of a core coated with at least one metal oxide layer, wherein at least one color pigment is contained in the at least one metal oxide layer.

The metal oxide coated on the core preferably consists essentially of alumina, aluminum hydroxide, alumina hydrate, silica or mixtures thereof.

The metal oxide layer of the effect pigment comprises one or more color pigments. Optionally, another layer is disposed on the color pigment-containing layer. This further layer may be formed as a protective layer to protect the color pigment-containing layer and / or to stabilize. This further layer may consist of one or more metal oxide (s). Preferably, the further layer contains silicon oxide or consists of silicon oxide.

Preferably, the color pigments used are cosmetics-compliant, d. H. they comply with important regulations on the authorization of cosmetic ingredients.

The cosmetic color pigments may be FD & C Red No. 3, D & C Red no. 6, D & C Red No. 6 Ba Lake, D & C Red no. 7 Ca Lake, D & C Red No. 9 Ba Lake, D & C Red 17, D & C Red No. 19 AI Lake, D & C Red no. 21, D & C Red no. 22, D & C Red No. 27, D & C Red no. 27 AI Lake, D & C Red no. 28 AI Lake, D & C Red no. 30 Lake, D & C Red no. 33 Zr Lake, D & C Red no. 33 AI Lake, D & C Red 34 Ca Lake, D & C Red no. 36, FD & C Red no. 40 AI Lake, D & C Red no. 40, D & C Orange No. 11, D & C Green 6, D & C Green 5, D & C Green 3, 5 AI Lake, FD & C Yellow no. 5 AI Lake, FD & C Yellow No. 6 AI Lake, D & C Yellow no. 10 AI Lake, FD & C Blue No. 1 AI Lake, Pigment Blue 28, D & C Brown 1, D & C Orange 5, D & C Red 4, D & C Red 6, D & C Yellow 7, D & C Yellow 11, Acid Blue 9; Pigment Blue 29, Pigment Blue 27, Pigment Blue 29, Pigment White 27, White Pigment 1, Pigment White 29, White Pigment 4, Pigment White 31, Pigment White 6, White 4, D & C Brown 1, Iron Oxide Yellow, Brown, Orange, Red, Black, Manganese Violet, D & C Violet 2, Cl 77007, Chrome Oxide Green, Cl 77289, Cl 77891, D & C Blue No. 4, Ultramarine Blue, Carmine, 7 Vat Red 1, Red 101 act. The amount of color pigment is preferably 5 to 40 wt .-%, the amount of metal oxide 3 to 95 wt .-%, each based on the weight of the aluminum substrate.

In a particular embodiment of the invention, colored pigments are prepared as effect pigments A by suspending a suitable cosmetic-conforming aluminum pigment in an organic solvent and bringing it to reaction temperature and oxidizing it by adding water and preferably a catalyst. The achievable colors are in the yellowish to brown color range.

The colored effect pigments B used in the cosmetic according to the invention are prepared, for example, by suitable base pigments, for example metallic effect pigments or pearlescent pigments, by controlled hydrolysis of metal acid esters in the presence of color pigments in a, preferably organic, solvent by means of a sol-gel process carried out in one step be coated. The solvent may contain, for example, 80 to 99% by volume of organic solvent and 20 to 1% by volume of water.

In this production process, the color pigments are incorporated during the sol-gel process in the forming metal oxide and fixed reliably. When using these colored effect pigments in cosmetics, it is therefore extremely advantageous not to separate the color pigment from the effect pigment.

The effect pigments used in the present invention show a wide variety of shades, such as blue, red, violet or gold, depending on the color pigment (s) applied and contained in the metal oxide layer. In addition, the visual impression is characterized by the metallic luster or pearlescence of the base pigment used.

In a particular embodiment of the invention, the effect pigments B used are colored aluminum pigments obtainable by a) rubbing one or more types of color pigments in organic solvents, b) mixing the trituration with aluminum pigments and one or more organic solvents, c) adding one or more metal acid esters, d) adding 1 to 5 times the amount of water which is stoichiometrically necessary for the complete hydrolysis of the metal acid esters, e) the volatile constituents after the end of the reaction removed from the mixture in the usual way and f) preferably the resulting pigments are dried.

In a further embodiment, a customary additive which improves the color pigment dispersion is added in step a).

In a further embodiment, the reaction mixture obtained in step d) is heated to a temperature between 40 ^° C. and the boiling point of the solvent (s) added in step b), and preferably a basic catalyst is added.

The drying in step f) is preferably carried out at less than 200 ⁰ C, more preferably at less than 150 ⁰ C and most preferably at less than 100 ⁰ C in vacuo or under reduced pressure, for. B. at 90 ⁰ C in a vacuum oven.

The color pigments are preferably taken from the group consisting of azo dyes, xanthene dyes, triphenylmethane dyes, anthraquinone dyes, vat dyes, metal oxides, in particular TiO 2, iron oxides, chromium III oxide (s), metal sulfides, metal salts, metal complexes, carmine red, Berlin blue and mixtures thereof.

The rubbing of the color pigments is carried out in the usual manner by roughening the color pigments, for. B. in a bead mill or in a grinding media mill, for. B. with zirconia spheres. The trituration can be carried out in a conventional solvent, for. B. white spirit, or more solvents. It is favorable to add an additive for improving the pigment dispersibility with, for. B. Antiterra U80 the company Byk-Chemie. Suitable aluminum pigments in stage c) are all customary aluminum pigments which can be used for cosmetic applications. Preferably, round aluminum flakes are used, so-called silver dollars. These silver dollars allow particularly brilliant colorations due to their low Streuanteils.

Suitable solvents in stage b) are in particular organic solvents, preferably water-miscible solvents. Particularly preferred are alcohols such as methanol, ethanol, n-propanol, i-propanol, n-butanol, i-butanol and t-butanol, particularly preferred is i-propanol.

It is also possible to add an additional amount of the solvent used in stage b), depending on the need for stage d) of the process before the end of the reaction. The total amount of the solvent added is preferably 150 to 300 ml based on 100 g of aluminum substrate.

Suitable metal acid esters are preferably selected from the group consisting of alkyl and aryl alcoholates, carboxylates, alkyl radicals substituted with carboxyl radicals and / or alkyl and / or aryl radicals, and / or carboxylates of titanium, zirconium, silicon, aluminum and boron. Particular preference is given to alkyl and aryl alcoholates, in particular C 1 -C 6 -alkyl alcoholates, such as methanolates, ethanolates, n-propanolates, i-propanolates, n-butanolates, i-butanolates and t-butanolates of the metals mentioned. These compounds have the general formula M (OR) _y , where M is titanium, zirconium, vanadium, silicon, aluminum or boron, R is a C1-C6 alkyl, phenyl, xylene, ToIyI or cresyl group and y stands for 3 or 4. This type of compound may also be used as an ester of the metal acids, e.g. As ortho-silica, boric acid, aluminum hydroxide, titanic acid or zirconium acid can be construed. Preference is given to using aluminum triisopropylate (triisopropylaluminate), titanium tetraisopropylate (tetraisopropyl titanate), o-silicic acid tetraethyl ester (tetraethyl orthosilicate) and triethyl borate (triethyl borate). Mixed alkoxides are also possible in which not all the radicals OR are the same but different from one another. The cosmetic according to the invention preferably contains from 2 to 40% by weight, more preferably from 5 to 20% by weight, of colored effect pigment (s), based on the weight of the cosmetic.

The cosmetic according to the invention is preferably in the form of a cream, a lotion, an eyeshadow, a nail polish, a lipstick, a Np gloss, a mascara, a gel, a make-up formulation or a self-tanning cream or self-tanning lotion.

The preparation of the cosmetic is carried out by the colored effect pigment A and / or effect pigment B is incorporated in a suitable manner in the carrier system of the cosmetic. Preferably, the effect pigments are incorporated into the carrier system with gentle dispersion.

Examples

Example 1 (Preparation of paint rubbing):

60.0 g D & C Red 34 Ca Lake

0.9 g Disperbyk 240.0 g isopropanol 200.0 g ZrO ₂ balls, ball diameter 0.8-1.0 mm

The ingredients are placed in a 500 ml wide-mouth PE bottle and the bottle capped. The bottle is then clamped in a shaking unit of the type: WX4 from Winter (Finland) and shaken for 1 h. The sap is then separated from the balls by sieving.

Example 2 (Preparation of paint rubbing):

60.0 g of Pigment Blue 27 C index: 77510 0.9 g of Disperbyk 240.0 g of isopropanol

200.0 g ZrO ₂ balls, ball diameter 0.8 - 1, 0 mm

The ingredients are placed in a 500 ml wide-mouth PE bottle and the bottle capped. This is then clamped in a shaking unit of the type: WX4 from Winter (Finland) and shaken for 1 h. The sap is then separated from the balls by sieving.

Example 3:

100 g of pearlescent pigment of the type Prestige Silver Star from Eckart GmbH & Co. KG, Fürth, Germany are added with 400 ml of isopropanol to a 1000 ml flat-section reaction vessel and dispersed. After 5 minutes, 10 g of tetraethoxysilane are added and the mixture is then heated to 80 ^° C. After reaching this temperature, a mixture of 1 g of triethanolamine and 30 g of demineralized water are added. 50 min. later, a mixture of 0.8 g of triethanolamine and 20 g of isopropanol (hereinafter referred to as "base mixture") is added. 40 min. later, a mixture of 20 g of pigment pigment (Example 1) and 47 g of tetraethoxysilane are then metered in. 20 min. later, the base mixture is added a second time and then left stirring for 1 h, before adding 9 g of tetraethoxysilane and 0.1 g of triethanolamine and 4 g of deionized water. 60 minutes later, a mixture of 0.3 g of triethanolamine and 8 g of isopropanol is added. The mixture is allowed to react for 3 hours while stirring and then switches off the heating. The suspension is stirred for a further 18 h, filtered, then washed with isopropanol-water mixture and dried.

Example 4:

100 g of pearlescent pigment of the type Prestige Silver Star from Eckart GmbH & Co. KG are added with 400 ml of isopropanol to a 1000 ml flat-section reaction vessel and dispersed. After 5 minutes, 10 g of tetraethoxysilane are added and the mixture is subsequently heated to 80 ^° C. After reaching this temperature, the mixture is introduced Mixture of 1 g of triethanolamine and 30 g of demineralized water added. 50 min. later, a mixture of 0.8 g of triethanolamine and 20 g of isopropanol (hereinafter referred to as "base mixture") is added. Again 10 min. later, the mixture is then metered into a mixture of 20 g of pigment pigment (Example 2) and 47 g of tetraethoxysilane. 20 min. later, the base mixture is added a further time and then stirred for 1 h, before adding 9 g of tetramethoxysilane and 0.1 g of triethanolamine and 4 g of deionized water. 60 minutes later, a mixture of 0.3 g of triethanolamine and 8 g of isopropanol is added. The mixture is allowed to react for 3 hours while stirring and then switches off the heating. The suspension is stirred for a further 18 h, filtered, then washed with isopropanol-water mixture and dried.

Example 5a:

141 g of cosmetic-conformal aluminum pigment (d 50: 35 μm) (Lsm content 29% by weight) are introduced into a 1000 ml flat-section reaction vessel with 250 ml of isopropanol and dispersed. After 5 minutes, 17 g of tetraethoxysilane are added and the mixture is then heated to 65 ^° C. After reaching this temperature, a mixture of 2 g of triethanolamine (TEA) and 50 g of demineralized water are added. 50 min. later, a mixture of 0.8 g of triethanolamine and 20 g of isopropanol (hereinafter referred to as "base mixture") is added. Again 10 minutes later, a mixture of 20 g of pigment pigment (Example 1) and 47 g of tetraethoxysilane are then metered in. 20 min. later, add the base mixture once again and then stir for 3 hours before switching off the heating. The suspension is stirred for a further 18 h, filtered, then washed and dried.

Example 5b (comparative example)

200 g of Visionaire Bright Silver Sea (Eckart GmbH & Co. KG) are charged with 1100 g deionized water into a 3000 ml flat-section reaction vessel and dispersed. After 5 minutes, the pH is adjusted to 5.5 with HCl and then heated to 75 ° C. When the temperature has been reached, a 7.2% by weight AICb is metered in. Hexahydrate soln. within 20 minutes too. The pH is kept constant by means of a 5 wt .-% sodium hydroxide solution. Then 800 g of a 1.7% by weight carmine lacquer solution (addition rate: 8 ml / min.) Are added. The pH is kept constant at 5.5 by means of a dilute HCl solution. The resulting pigment is filtered, washed and dried in a drying oven.

The pigments obtained according to Example 5a and Comparative Example 5b are each coated with 4% by weight of colored pigment.

The abrasion resistance was evaluated in a rapid test by applying the wet filter cake to filter paper and rubbing with a spatula. The appearance of silvery metallic luster here is an indicator of poor adhesion of the color pigments on the base pigment. It turns out that the pigments of the invention (Example 5a) have better adhesion of the color pigments than the pigments obtained according to Comparative Example (Example 5b).

For testing, the pigments are incorporated into a nail varnish according to the following recipe:

4.0 parts effect pigment

96.0 parts Nailpolish TFF from the company International Lacquers

The pigment is initially charged, about 10 parts of lacquer added and well dispersed with a bristle brush. Subsequently, the remaining paint is added and homogenized.

The optical test is performed by a squeegee on a cover card of the Byk Gardner Byko-Chart 2853 with 50 microns wet film thickness.

The color measurement was carried out with a goniospektral photometer from Optronic, Multiflash, Berlin, Germany, according to the manufacturer's instructions and gave the values listed in Table 1. These make it clear that in the nail varnish according to the invention, the pigment of Example 5a a significantly higher Color strength than the pigment according to Example 5b in an otherwise identical nail varnish (comparative example).

Table 1 :

Example 6:

157 g of cosmetically compatible aluminum pigment (Lsm content 36.0% by weight) are charged with 300 ml of isopropanol into a 1000 ml flat-section reaction vessel and dispersed. After 5 minutes, 10 g of tetraethoxysilane are added and the mixture is then heated to 80 ^° C. After reaching this temperature, a mixture of 1 g of ethylenediamine (EDA) and 30 g of demineralized water are added. 50 min. later, a mixture of 1 g of EDA and 20 g of isopropanol (hereinafter referred to as base mixture) is then added. Again 10 min. later, a mixture of 50 g of pigment pigment (Example 2) and 47 g of tetraethoxysilane are then metered in. 30 min. later you add the base mix one more time. After another 30 min. in turn, a base mixture of 1.6 g of EDA and 20 g of isopropanol is added. The mixture is stirred for 1 h, before adding 9 g of tetraethoxysilane and 0.1 g of EDA and 4 g of deionized water. 60 minutes later, a mixture of 0.2 g of EDA and 4 g of isopropanol is added. The mixture is allowed to react for 3 h while stirring and then switches off the heating. The suspension is stirred for a further 18 h, filtered, then washed and dried.

Example 7:

Oxidation:

40 g of pigment pigment (Example 1) and 240 g of isopropanol are introduced into a 1 l flat-section reaction vessel and the mixture is stirred for 10 min. dispersed. Then 141.2 g of a cosmetically compatible aluminum pigment paste (Lsm content 29.2% by weight) are added and again for 20 minutes. later a mixture of 50 g of deionized water and 2.3 g of ethylenediamine in the reactor and the suspension starts to heat to 80 ⁰ C. After a heating time of 7 hours, 15 g of tetraethoxysilane are added and the mixture is heated for a further 2 hours before the suspension is allowed to cool. 16 hours later, the mixture is filtered off with suction and dried the filter cake.

Example 8 (moisturizer):

The components of phases 1 and 2 are each added to a glass flask and subsequently heated to 78 ° C. with stirring or shaking. After complete homogenization, phase 2 is added to phase 1 with stirring or shaking to obtain a homogeneous mixture. The homogeneous mixture is then cooled in a paddle mixer with stirring to room temperature. The resulting cream shows a hitherto unknown blue-shimmering effect.

Phase 1

Cyclomethicone 72 parts by weight

Dimethicone 20 parts by weight

C12-C15 alkyl benzoate 40 parts by weight (and) stearalkonium bentonite (and) propylene carbonate)

Cetyl Dimethicone Copolyol 4.8 parts by weight

Blue pearlescent pigment (Example 4) 2 parts by weight

Phase 2

Distilled water 252.5 parts by weight

Sodium chloride 1.5 parts by weight

Preservative 1.2 parts by weight

(Phenoxyethanol (and) Methylparaben ₁ _C N

(and) butylparaben (and) propylparaben)

Example 9 (lipstick):

Name Product name% W / W Manufacturer

Phase 1

Carnauba wax Carnauba # 1 Flake 3.0 Ray & Pitsch

Beeswax Yellow Beeswax 2.5 Ray & Pitsch

Candelilla Wax SP-75 5 Strahl & Pitsch

Ozokerit Ozokerite 170 2 Koster Keunen

PTFE Microslip 519 Micro Powders

Castor oil Castor OiI USP 17.82 Süd-Chemie Rheologicals

Polyisobutene Permethyl 104A 7 Presperse

Isostearyl Isostearate Isostearated'lsostearyle 5 Gattefosse

Isononyl Isononanoate Dermol 99 18 Alzo

Capryl Triglyceride Liponate GC 10 Lipo Phase 2

D & C Red 27 Aluminum Varnish, 33% dispersion in Castor OiI 10 Sun Chemical FD & C Blue # 1 A1 Varnish, 50% dispersion in Castor OiI 0.03 Sun Chemical

Phase 3

Propylparaben 0.10

BHT 0.05 Eastman

Red aluminum pigment 15 Eckart

(Example 5)

Boron Nitride Soft Touch CC5102 2.5 Advanced Ceramics

Production method:

1. Mix phase 1 with a low shear mixer.

2. Heat to 80 ° C to 84 ° C.

3. Addition of phase 2 and mixing until homogenization.

4. Addition of phase 3.

5. Pour into a lipstick mold at 70 ° C.

The lipstick shows after applying a dependent on the viewing angle multicolored iridescent effect.

Example 10 (eye shadow):

Name Product name% W / W Manufacturer

Phase 1

Mica Azco Mica BC 1020wg 34.9 Presperse

Titanium Dioxide Tronox CR-837 5.5 Kerr McGee

Chromium oxide Green Chromium Oxide Green 2.8 LCW

Iron Oxide Yellow Iron Oxide Yellow 1.8 Sun Chemical

Zinc Stearate Zinc Stearate SAK 25p 5.5 USP Blachford

Boron nitride Soft touch CCS 102 1.8 Advanced Ceramic

Phase 2

Red pearlescent pigment

(Example 3) 36.7 Eckart

Phase 3

Dimethicon Dow 200 5.5 Dow Corning

Capryl Triglyceride Liponate GC 5.5 Lipo

Manufacturing process (all components are mixed together at room temperature):

1. Mix Phase 1 in a blender to homogeneity.

2. Check the pigment dispersion.

3. Add phase 2 and mix to homogeneity.

4. Spray phase 3 and mix until homogeneous.

The eye shadow shows after application a fantastic gloss effect The examples show that cosmetics with colored effect pigments produce surprisingly brilliant and visually extremely interesting color effects.

In addition, it has surprisingly been found that the effect pigments used in the cosmetic according to the invention are extremely stable. In particular, there is no release or detachment of the color pigments from the effect pigments, since the color pigments are contained in the metal oxide layer. The pigments are therefore enclosed by metal oxides and reliably applied to the effect pigments, so that the color pigments in the respective carrier system of the cosmetic even after prolonged storage of the cosmetics at summer temperatures of up to 30 to 4O ⁰ C to no "bleeding" or leaking can.

Claims

claims

1. Cosmetic containing one or more colored effect pigments, characterized in that the cosmetic

2. Cosmetic according to claim 1, characterized in that the core of the effect pigment B consists of platelet-shaped metal pigments selected from the group consisting of aluminum, copper, zinc, silver, gold, iron, titanium, brass, bronze and alloys of these substances exists, be selected.

3. Cosmetic according to claim 1, characterized in that the core of the effect pigment B consists of pearlescent pigments or of glass-based pearlescent pigments or mixtures thereof.

4. Cosmetic according to claim 3, characterized in that the core is a pearlescent pigment on the basis of at least one high refractive index metal oxide, preferably TiO ₂ and / or Fe ₂ O ₃ , coated mica and / or coated glass flakes.

5. Cosmetic according to claim 1 or 2, characterized in that the core of the effect pigment A or B is a metal pigment and has a thickness of 10 nm to 2 microns, preferably 40 nm to 500 nm.

6. Cosmetic according to one of claims 1 to 5, characterized in that the metal oxide of the effect pigment B is selected from the group consisting of alumina, aluminum hydroxide, alumina hydrate, silica and mixtures thereof.

7. Cosmetic according to one of claims 1 to 6, characterized in that the metal oxide layer of the effect pigment B contains a plurality of color pigments.

8. Cosmetic according to one of claims 1 to 7, characterized in that at least one further layer on the color pigment-containing layer of the effect pigment B is arranged.

9. Cosmetic according to claim 8, characterized in that the at least one further layer comprises or consists of metal oxide.

10. Cosmetic according to claim 9, characterized in that the metal oxide is or contains silicon oxide.

11. Cosmetic according to one of claims 1 to 10, characterized in that the color pigment or the color pigments is or are cosmetic compliant.

12.Cosmetic according to one of claims 1 to 11, characterized in that the at least one color pigment from the group consisting of azo dyes, xanthene dyes, triphenylmethane dyes, anthraquinone dyes, vat dyes, metal oxides, in particular TiO ₂ , iron oxides, chromium-l-oxide (en ), Metal sulfides, metal salts, metal complexes, carmine red, Berlin blue, and mixtures thereof.

13. Cosmetic according to one of the preceding claims, characterized in that the cosmetic contains 1 to 40 wt .-% effect pigment A and / or effect pigment B.

14. Cosmetic according to one of the preceding claims, characterized in that the cosmetic in the form of a cream, a lotion, an eyeshadow, a nail polish, a lipstick, a Hp gloss, a mascara, a gel, a make-up formulation or a self-tanning cream or lotion is present.

1 S.Verfahren for the production of a cosmetic, characterized in that (a) an effect pigment A with an aluminum-containing core with a surface generated by wet-chemical oxidation of the aluminum-containing core surface-generating coloring layer of alumina,

Aluminum hydroxide and / or alumina hydrate and / or

(B) an effect pigment B having a core coated with at least one metal oxide layer, wherein at least one color pigment is contained in the at least one metal oxide layer, is incorporated in a suitable manner into a carrier system of a cosmetic.

16. The method according to claim 15, characterized in that the core of the effect pigment B consists of platelet-shaped metal pigments selected from the group consisting of aluminum, copper, zinc, silver, gold, iron, titanium, brass, bronze and alloys of these substances exists, be selected.

17. The method according to claim 15, characterized in that the core of the effect pigment B consists of pearlescent pigments or of glass-based pearlescent pigments or mixtures thereof.

18. The method according to claim 17, characterized in that the core is a pearlescent pigment on the basis of at least one high refractive index metal oxide, preferably TiO ₂ and / or Fe ₂ O ₃ , coated mica and / or coated glass flakes.

19. The method according to claim 15 or 16, characterized in that the core of the effect pigment B is a metal pigment and has a thickness of 10 nm to 2 microns, preferably 40 nm to 500 nm.

20. The method according to any one of claims 15 to 19, characterized in that the metal oxide of the effect pigment B is selected from the group consisting of alumina, aluminum hydroxide, alumina hydrate, silica and mixtures thereof.

21. The method according to any one of claims 15 to 20, characterized in that the metal oxide layer of the effect pigment B contains a plurality of color pigments.

22. The method according to any one of claims 15 to 21, characterized in that at least one further layer on the color pigment-containing layer of the effect pigment B is arranged.

23. The method according to claim 22, characterized in that the at least one further layer comprises or consists of metal oxide.

24. The method according to claim 23, characterized in that the metal oxide is or contains silicon oxide.

25. The method according to any one of claims 15 to 24, characterized in that the color pigment or the color pigments is or are cosmetic compliant.

26. The method according to any one of claims 15 to 25, characterized in that the at least one color pigment from the group consisting of azo dyes, xanthene dyes, triphenylmethane dyes, anthraquinone dyes, vat dyes, metal oxides, in particular TiO ₂ , iron oxides, chromium-l-oxide (en ), Metal sulfides, metal salts, metal complexes, carmine red, Berlin blue, and mixtures thereof.

27. The method according to any one of claims 15 to 26, characterized in that the cosmetic contains 1 to 40 wt .-% effect pigment A and / or effect pigment B.

28.The method according to any one of claims 15 to 27, characterized in that the cosmetic in the form of a cream, a lotion, an eyeshadow, a nail polish, a lipstick, a lip gloss, a mascara, a gel, a make-up formulation or a self-tanning cream or lotion.