Patent Application
20170105915
The present invention relates to α-Al2O3 flakes and the use in variety of applications, especially in cosmetics. Preferably, the present invention relates to functional filler pigments for cosmetics.
Filler pigments for cosmetics have constantly been demanded to have a comfortable and favorable touch and good adherence to skin and last longer (Material Technology (Zairyo Gijutsu), 16 (2), 64 (1998)).
Filler pigments for cosmetics that have transparency serving as a factor of beautiful skin, improve skin tone, and accomplish more natural make-up have been demanded in order to produce healthy beauty (J. Soc. Cosmet. Chem. Jpn. 39 (3), 201-208, (2005)); (HIFU TO BIYO, 124 (4), 4080 (1992)); and (HYOMEN in Japanese), 30(9), 703 (1992)). As optical functions of filler pigments for cosmetics, there have been demanded properties that are capable of covering irregular skin color, and the like, with a thin film and giving a light and natural finish. Moreover, filler pigments for cosmetics are applied to skin and therefore, of course, require a good skin feeling.
Among filler pigments for cosmetics, filler pigments usually having white colors do not influence the final formulation color. The effect that white emulsions with these filler pigments look even whiter, supports positively the precious visual appearance. The filler pigment having white color should offer high chemical and physical stability and is light stable in cosmetic formulations.
The important factors of filler pigments are the particle size, thickness, aspect ratio, shape, surface property, refractive index and the like. The particle size greatly affects the coloration of the filler pigment because it is closely related with the wavelength of the light. That is, the smaller the particle size, the larger the surface area, thereby increasing the coloration and enhancing reflectivity, and offering a more vivid color.
Suitable filler pigments can be for example Al2O3 flakes. Al2O3 flakes are well known and can be used as substrate for effect pigments α-Al2O3 in the form of hexagonal flakes having a particle diameter which are greater than 10 μm and an aspect ratio (particle diameter/thickness) of 5-10 are known from Japanese Unexamined Patent Application Publication No. 1982-111239.
The Japanese Unexamined Patent Application Publication No. 1991-72572 discloses α-Al2O3 in the form of flakes having an average particle diameter of 0.5-3 μm.
The Japanese Unexamined Patent Application Publication No. 1992-39362 describes Al2O3 in the form of fine platy particles of a hexagonal crystal system with the plane perpendicular to the c axis grown into a plate.
Al2O3 flakes composed of aluminum oxide (as a major constituent) and of titanium dioxide (as a minor constituent) are disclosed in U.S. Pat. No. 5,702,519. The Al2O3 flakes are manufactured by using mineralizer which is sulfated alkali metal sulfate such as sodium sulfate or potassium sulfate.
WO 04/60804 A1 discloses Al2O3 flakes manufactured by using mineralizer such as metal fluoride. The preferred metal fluorides disclose are sodium fluoride, calcium fluoride, aluminum fluoride and sodium aluminum fluoride. The Al2O3 flakes have a particle diameter of 0.1-30 μm, and thickness of 50-200 nm.
On the other hand, the filler pigments for the cosmetics such as a foundation which is directly applied to the skin, those capable of providing a good feeling (skin feeling) are continuously desired (Material Technology (Zairyo Gijutsu), 16 (2), 64 (1998)). As the index to express this skin feeling, there is an average friction coefficient (MIU value) measured by the KES friction tester (KES-SE-DC-tester by KATO TECH. Co., Ltd.).
The average friction coefficient (MIU value) indicates slipperiness of sample, determined as average of μ (a friction coefficient) in a distance of 20 mm. μ (a friction coefficient) is measured to scan surface of the sample by friction block. μ (a friction coefficient) integrates and obtained value divided by 20 mm, and the average friction coefficient (MIU value) is obtained.
In case that the average friction coefficient (MIU value) is smaller, the skin feeling improves because friction becomes less against skin. A MIU value of less than 0.8 is preferred.
The Al2O3 flakes of the prior art have the disadvantages that the average friction coefficient (below, it may be abbreviated to MIU value) is relatively high, and the skin feeling is not good and sometimes cosmetic skin has irritation. Therefore, Al2O3 flakes are required which do not show the above mentioned advantages and at the same time decrease the MIU value.
In case that Al2O3 flakes manufactured by using mineralizer such as fluorine compound, Al2O3 flakes are doped by fluorine. But cosmetics including fluorine are not recommended to use in almost countries. Therefore, Al2O3 flakes are required which do not contain any fluorine.
The object of the present invention is to provide improved Al2O3 flakes having a good skin feeling which do not contain any fluorine or only very small amounts of fluorine and which can be easily prepared and show an excellent skin feeling.
Surprisingly, it has been found that functional filler pigments prepared according to Claim 1 have significantly increased properties with regard to the whiteness, color purity, natural appearance of the skin and the dispersibility into cosmetic formulations.
The Al2O3 flakes according to the invention are used, in particular, as filler pigments for cosmetics, especially for the use in decorative and personal care applications. However, they can also be employed in all formulations where alumina flakes are usually employed, such as, for example, in inks, coatings, preferably automotive coatings and plastics.
In a preferred embodiment of the present invention, the Al2O3 flakes are prepared starting from an aqueous aluminum salt solution by precipitation with a basic solution. Optionally, at least one alkali metal sulfate such as sodium or potassium sulfate and at least one dopant such as a titanium compound are added to the starting solution. The precipitation step is followed by drying (evaporation or dehydration by heating), and molten salt treatment including the following steps:
Examples for aluminum salts can be water-soluble or insoluble salt. Suitable aluminum salts are for example aluminum sulfate, aluminum chloride, aluminum nitrate, poly aluminum chloride, aluminum hydroxide, boehmite, basic aluminum sulfate or combinations thereof. From the view points of the ready availability and handling, aluminum sulfate, aluminum chloride, and aluminum nitrate are preferred.
Examples for a sulfate compound which acts as mineralizer, is for example a metal sulfate. Besides metal sulfates, alkali metal sulfate, alkali earth metal sulfate or combinations thereof are preferred. In particular, an alkali metal sulfate is preferred.
Examples for alkali metal sulfate are sodium sulfate, potassium sulfate, lithium sulfate or combinations thereof. From the view points of the ready availability and low price, sodium sulfate is preferred.
Examples for a suitable basic solution which acts as the pH controlling agent for the precipitation, ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or combinations thereof are preferred.
From the view points of the ready availability and low price, sodium carbonate and potassium carbonate are more preferable, and sodium carbonate is particularly preferable.
Suitable dopants which could be helpful as control agent for the particle size, thickness, optical properties and/or surface morphology, are preferably selected from the following group of compounds: TiO2, ZrO2, SiO2, In2O3, SnO2, ZnO or combinations thereof. The amount of the dopant is preferably 0.01-5 wt % based on the Al2O3 flake.
In a preferred embodiment the dopant is TiO2, SnO2 or ZnO. TiO2 is preferably considered to have a function to suppress the color in the produced Al2O3 flakes. ZnO and SnO2 are preferably considered to promote a decrease in thickness and a growth of the particles and prevent the agglomeration. TiO2, SnO2 or ZnO is preferably used in amounts of less than 0.05 wt % based on the Al2O3 flakes.
Example for suitable titanium salt for the formation of TiO2 is titanium tetra-chloride, titanium tri-chloride, titanium oxy sulfate, titanium sulfate or combinations thereof. From the view points of the ready availability and low price, titanium tetra-chloride and titanium sulfate are preferable.
Example for a suitable zinc salt for the formation of ZnO is an acid salt, a halide and an oxide of zinc, specifically zinc sulfate, zinc nitrate and zinc chloride. Example for suitable tin salt for the formation of SnO2 is an acid salt, a halide and an oxide of tin, specifically tin sulfate, tin nitrate and tin chloride. With regard to the chemical affinity with the aluminum sulfate and superiority in preventing the thickness decrease and agglomeration of flaky crystals, zinc sulfate and tin sulfate are preferred.
In a preferred embodiment the total molar ratio of the sulfate compound to Al2O3 is 1 to ≦3.5 after step (2).
When the total molar ratio of the sulfate compound to Al2O3 is 1 to ≦3.5 after step (2), it is considered that the MIU value to be at most 0.8. When the aluminum salt and basic solution undergo the neutralization reaction, molar ratio of the produced alkali metal sulfate to produced Al2O3 is 3.0. Therefore, optionally, molar ratio of the sulfate compound to the Al2O3 is able to desirably add at most 0.5.
In a preferred embodiment the calcination temperature is from 900 to 1400° C. Al2O3 is transformed from γ-Al2O3 to α-Al2O3 having a corundum structure by the calcination of at least 900° C. In case of calcination temperature over 1400° C., it is increased the probability of damage to equipment. Therefore, the calcination temperature is usually at least 900° C. and more desirably at least 1000° C., and it is usually at most 1400° C. and more desirably at most 1250° C.
In a preferred embodiment the Al2O3 flakes have a particle size distribution characterized by a Gaussian distribution in which the volume size fractions are distributed as follows:
In this patent application D50 and D80 of the alumina flakes are evaluated by using Malvern MS 2000.
The particle size distribution D50 is also known as the median diameter or the medium value of the particle size distribution, it is the value of the particle diameter at 50% in the cumulative distribution and is one of the important parameter characterizing the particle size of pigments.
Correspondingly, the D80 value indicates the maximum longitudinal dimensions of the Al2O3 flakes, as determined again by means of laser granulometry in the form of sphere equivalents, which 80% of the particles attain at maximum, or fall below, out of the entirety of all Al2O3 particles.
The average thickness is determined on the basis of a cured paint film in which the Al2O3 flakes are oriented substantially plane-parallel to the substrate. For this purpose a transverse section of the cured paint film is examined under a scanning electron microscope (SEM), the thickness of 100 Al2O3 flakes being ascertained and statistically averaged.
The desired size and thickness distribution can be obtained by suitable classification of the flakes, such as by classifying through selected screens and the like.
In a preferred embodiment the Al2O3 flakes have a thickness of ≦500 nm.
In a preferred embodiment the Al2O3 flakes are α-Al2O3 flakes.
In a preferred embodiment the Al2O3 flakes have a MIU value of less than 0.8.
The Al2O3 flakes according to the present invention are highly suitable as substrate in the preparation of effect pigments. To this end, they are preferably coated with at least one high refractive index layer, like at least one layer of a metal oxide, such as, for example, TiO2, ZrO2, SnO2, ZnO, Ce2O3, Fe2O3, Fe3O4, FeTiO5, Cr2O3, CoO, Co3O4, VO2, V2O3, NiO, furthermore of titanium suboxides (TiO2 partially reduced with oxidation states from <4 to 2, such as the lower oxides Ti3O5, Ti2O3, TiO), titanium oxynitrides, FeO(OH), thin semitransparent metal layer, for example comprising Al, Fe, Cr, Ag, Au, Pt or Pd, or combinations thereof. The TiO2 layer may be in the rutile or anatase modification. In general, the highest quality and gloss and at the same time the most stable effect pigments are obtained when the TiO2 is in the rutile modification. In order to obtain the rutile modification, an additive can be used which is able to direct the TiO2 into the rutile modification. Useful rutile directors such as tin dioxide are disclosed in the U.S. Pat. No. 4,038,099 and U.S. Pat. No. 5,433,779 and EP 0 271 767. Preferred effect pigments based on Al2O3 flakes are coated with one or more layers of metal oxides, preferably with one metal-oxide layer only, in particular with TiO2, Fe2O3, Fe3O4, SnO2, ZrO2 or Cr2O3. Especially preferred are Al2O3 flakes coated with TiO2 or Fe2O3.
The thickness of each high-refractive-index layer depends on the desired interference color. The thickness of each layers on the surface of the Al2O3 flakes is preferably 20-400 nm, preferably 30-300 nm, in particular 30-200 nm.
The number of layers on the surface of the Al2O3 flakes is preferably one or two, furthermore three, four, five, six or seven layers.
In particular, interference packages consisting of high- and low-refractive-index layers on the surface of the Al2O3 flakes result in effect pigments having increased gloss and a further increased interference color or color flop.
Suitable colorless low-refractive-index materials for coating are preferably metal oxides or the corresponding oxide hydrates, such as, for example, SiO2, Al2O3, AlO(OH), B2O3, compounds such as MgF2 or a mixture of the said metal oxides.
In case of multilayer applied on the surface of the Al2O3 flakes the interference system is, in particular, a TiO2—SiO2—TiO2 layer sequence.
Furthermore, the effect pigments according to the invention may also have a semitransparent metal layer as outer layer. Coatings of this type are known, for example, from DE 38 257 02 A1. The metal layers are preferably chromium or aluminum layers having layer thicknesses of 5-25 nm.
Al2O3 flakes can also be coated with one or more layers of a metal or metal alloy selected e.g. from chromium, nickel, silver, bismuth, copper, tin, or hastelloy. Al2O3 flakes coated with a metal sulfide are coated with sulfides e.g. of tungsten, molybdenum, cerium, lanthanum or rare earth elements.
Furthermore, the effect pigments based on Al2O3 flakes can be finally coated with an organic dye as a top coat, preferably with Prussian Blue or Carmine Red.
Particularly preferred effect pigments based on the Al2O3 flakes according to the invention have the following layer sequence(s):
Al2O3 flake+TiO2
Al2O3 flake+TiO2/Fe2O3
Al2O3 flake+Fe2O3
Al2O3 flake+TiO2+Fe2O3
Al2O3 flake+TiO2+Fe3O4
Al2O3 flake+TiO2+SiO2+TiO2
Al2O3 flake+Fe2O3+SiO2+TiO2
Al2O3 flake+TiO2/Fe2O3+SiO2+TiO2
Al2O3 flake+TiO2+SiO2+TiO2/Fe2O3
Al2O3 flake+TiO2+SiO2
Al2O3 flake+TiO2+SiO2/Al2O3
Al2O3 flake+TiO2+Al2O3
Al2O3 flake+SnO2
Al2O3 flake+SnO2+TiO2
Al2O3 flake+SnO2+Fe2O3
Al2O3 flake+SiO2
Al2O3 flake+SiO2+TiO2
Al2O3 flake+SiO2+TiO2/Fe2O3
Al2O3 flake+SiO2+Fe2O3
Al2O3 flake+SiO2+TiO2+Fe2O3
Al2O3 flake+SiO2+TiO2+Fe3O4
Al2O3 flake+SiO2+TiO2+SiO2+TiO2
Al2O3 flake+SiO2+Fe2O3+SiO2+TiO2
Al2O3 flake+SiO2+TiO2/Fe2O3+SiO2+TiO2
Al2O3 flake+SiO2+TiO2+SiO2+TiO2/Fe2O3
Al2O3 flake+SiO2+TiO2+SiO2
Al2O3 flake+SiO2+TiO2+SiO2/Al2O3
Al2O3 flake+SiO2+TiO2+Al2O3
Al2O3 flake+TiO2+Prussian Blue
Al2O3 flake+TiO2+Carmine Red
In this application, the term “coating” or “layer” is taken to mean the complete enveloping of the Al2O3 flakes according to the invention.
The effect pigments based on doped or undoped Al2O3 flakes preferably consist of 40-90 wt. % of Al2O3 flakes and 10-60 wt. % of the coating based on the total pigment.
The Al2O3 flakes can be coated by wet chemical coating, by CVD or PVD processes.
The coating of the α-Al2O3 flakes with one or more layers, preferably one or more metal oxide layers, is preferably carried out by wet-chemical methods, it being possible to use the wet-chemical coating methods developed for the preparation of pearlescent pigments. Methods of this type are described, for example, in DE 14 67 468, DE 19 59 988, DE 20 09 566, DE 22 14 545, DE 22 15 191, DE 22 44 298, DE 23 13 331, DE 15 22 572, DE 31 37 808, DE 31 37 809, DE 31 51 343, DE 31 51 354, DE 31 51 355, DE 32 11 602, DE 32 35 017 or also in further patent documents and other publications known to the person skilled in the art.
In the case of wet coating, the Al2O3 flakes are suspended in water, and one or more hydrolysable metal salts are added at a pH which is suitable for hydrolysis, which is selected in such a way that the metal oxides or metal-oxide hydrates are precipitated directly onto the flakes without secondary precipitations occurring. The pH is usually kept constant by simultaneous metered addition of a base and/or acid. The pigments are subsequently separated off, washed and dried at 50-150° C. for 6-18 h and calcined for 0.5-3 h, where the calcination temperature can be optimized with respect to the respective coating present. In general, the calcination temperatures are 500-1000° C., preferably 600-900° C. If desired, the pigments can be separated off after application of individual coatings, dried and optionally calcined and then re-suspended again for the application of the further layers.
The application of a SiO2 layer to the Al2O3 flake and/or to the already coated Al2O3 flake is generally carried out by addition of a potassium or sodium water-glass solution at a suitable pH.
Furthermore, the coating can also be carried out in a fluidized-bed reactor by gas-phase coating, it being possible to use, for example, the methods proposed in EP 0045851 and EP 0106235 for the preparation of pearlescent pigments correspondingly.
The hue and chroma of the effect pigment based on Al2O3 flakes according to the invention can be varied in very broad limits through the different choice of the coating amounts or the layer thicknesses resulting there from. Fine tuning for a certain hue and chroma can be achieved beyond the pure choice of amount by approaching the desired color under visual or measurement technology control.
In order to increase the light, water and weather stability, it is frequently advisable, depending on the area of application, to subject the metal oxide coated Al2O3 fillers to post-coating or post-treatment. Suitable post-coatings or post-treatments are, for example, the processes described in German Patent 2215191, DE-A 3151354, DE-A 3235017 or DE-A 3334598. This post-coating further increases the chemical and photochemical stability or simplifies the handling of the pigment, in particular the incorporation into various media. In order to improve the weatherability, dispersibility and/or compatibility with the user media, it is possible, for example, for functional coatings of Al2O3 or ZrO2 or mixtures thereof to be applied to the pigment surface. Furthermore, organic post-coatings are possible, for example with silanes, as described, for example, in EP 0090259, EP 0634459, WO 99/57204, WO 96/32446, U.S. Pat. No. 5,759,255, U.S. Pat. No. 5,571,851, WO 01/92425 or in J. J. Ponjeé, Philips Technical Review, Vol. 44, No. 3, 81 ff. and P. H. Harding J. C. Berg, J. Adhesion Sci. Technol. Vol. 11 No. 4, pp. 471-493.
In accordance with the present invention, an effect pigment based on Al2O3 flakes having the desired size distribution has been found useful in all types of compositions, including plastics, cosmetics, and, in particular in automotive paints.
The Al2O3 flakes and the effect pigments based on Al2O3 flakes according to the invention are compatible with a multiplicity of color systems, preferably from the area of paints, automotive coatings, industrial coatings, printing inks and cosmetic formulations. For the preparation of printing inks for, for example, gravure printing, flexographic printing, offset printing and offset over varnishing, a multiplicity of binders, in particular water-soluble grades, as sold, for example, by BASF, Marabu, Pröll, Sericol, Hartmann, Gebr. Schmidt, Sicpa, Aarberg, Siegberg, GSB-Wahl, Follmann, Ruco or Coates Screen INKS GmbH, is suitable. The printing inks can be water-based or solvent-based. The Al2O3 flakes and the effect pigments according to the invention are furthermore also suitable for the laser marking of paper and plastics and for applications in the agricultural sector, for example for greenhouse sheeting, and, for example, for the coloring of tent awnings.
It goes without saying that, for the various applications, the coated and uncoated Al2O3 flakes according to the present invention can also advantageously be used in blends with organic dyes, organic pigments or other pigments, such as, for example, transparent and opaque white, colored and black pigments, and with flake-form iron oxides, organic pigments, holographic pigments, LCPs (liquid crystal polymers) and conventional transparent, colored and black luster pigments based on metal oxide-coated mica and SiO2 flakes, etc. The pigments according to the invention can be mixed in any ratio with commercially available pigments and fillers.
Fillers which may be mentioned are, for example, natural and synthetic mica, nylon powder, pure or filled melamine resins, talc, SiO2, glasses, kaolin, oxides or hydroxides of aluminum, magnesium, calcium or zinc, BiOCl, barium sulfate, calcium sulfate, calcium carbonate, magnesium carbonate, carbon, and physical or chemical combinations of these substances. There are no restrictions regarding the particle shape of the filler. It can be, for example, flake-form, spherical or needle-shaped in accordance with requirements.
The Al2O3 flakes and the effect pigments based on Al2O3 flakes according to the invention are simple and easy to handle. The Al2O3 flakes and the effect pigments based on Al2O3 flakes can be incorporated into the system in which it is used by simple stirring. Laborious milling and dispersing of the Al2O3 flakes and the effect pigments is not necessary.
The Al2O3 flakes and the effect pigments based on Al2O3 flakes according to the invention can be used for pigmenting coating materials, printing inks, plastics, agricultural films, button pastes, for the coating of seed, for the coloring of food, coatings of medicaments or cosmetic formulations. The concentration of the Al2O3 flakes and the effect pigments in the system in which it is to be used for pigmenting is generally between 0.01 and 50% by weight, preferably between 0.1 and 20% by weight, based on the overall solids content of the system. This concentration is generally dependent on the specific application.
Plastics containing the Al2O3 flakes and the effect pigments based on Al2O3 flakes according to the invention in amounts of 0.1 to 50% by weight, in particular from 0.5 to 7% by weight, are frequently notable for a particular gloss and shimmer effect.
In the coating sector, especially in automotive coating and automotive finishing, the effect pigments based on Al2O3 flakes according to the invention are employed in amounts of 0.5-10% by weight.
In the coating material, the Al2O3 flakes and the effect pigments based on Al2O3 flakes according to the invention have the advantage that the desired color and gloss is obtained by a single-layer coating (one-coat systems or as a base coat in a two-coat system).
In the pigmentation of binder systems, for example for paints and printing inks for intaglio, offset or screen printing, the effect pigments based on Al2O3 flakes with Stapa®-aluminum and gold bronze pastes from Eckart GmbH have proven particularly suitable. The effect pigment is incorporated into the printing ink in amounts of 2-50% by weight, preferably 5-30% by weight and, in particular, 8-15% by weight. The printing inks containing the effect pigment according to the invention in combination with a metal effect pigment exhibits purer hues and is of improved printability owing to the good viscosity values.
The invention likewise provides pigment preparations containing coated or uncoated Al2O3 flakes according to the present invention and further effect pigments, binders and, if desired, additives, the said preparations being in the form of substantially solvent-free, free-flowing granules. Such granules contain up to 95% by weight of the Al2O3 flakes or the effect pigments according to the invention. A pigment preparation in which the effect pigment based on Al2O3 flakes of the invention is pasted up with a binder and with water and/or an organic solvent, with or without additives, and the paste is subsequently dried and brought into a compact particulate form, e.g. granules, pellets, briquettes, a master batch or tablets, is particularly suitable as a precursor for printing inks.
The invention thus also relates to the use of the coated (=effect pigments) or uncoated Al2O3 flakes in formulations from the areas of paints, coatings, automobile coatings, automotive finishing, industrial coatings, paints, powder coatings, printing inks, security printing inks, plastics, ceramic materials, cosmetics. The coated and uncoated Al2O3 flakes can furthermore be employed in glasses, in paper, in paper coating, in toners for electrophotographic printing processes, in seed, in greenhouse sheeting and tarpaulins, in thermally conductive, self-supporting, electrically insulating, flexible sheets for the insulation of machines or devices, as absorber in the laser marking of paper and plastics, as absorber in the laser welding of plastics, in pigment pastes with water, organic and/or aqueous solvents, in pigment preparations and dry preparations, such as, for example, granules, for example in clear coats in the industrial and automobile sectors, in sunscreens, as filler, in particular in automobile coatings and automotive finishing.
The invention thus also relates to formulations containing Al2O3 flakes and at least one component selected from the group of water, polyols, polar and non-polar oils, fats, waxes, film formers, polymers, copolymers, surfactants, free-radical scavengers, antioxidants, stabilisers, odour enhancers, silicone oils, emulsifiers, solvents, preservatives, thickeners, rheological additives, fragrances, colorants, effect pigments, UV absorbers, surface-active assistants and/or cosmetic active compounds, fillers, binders, pearlescent pigments, color pigments and organic dyes.
All percentage data in this application are percent by weight, unless indicated otherwise.
The following examples are intended to explain the invention in greater detail, but without restricting it.
In 450 ml of deionized water are dissolved 111.9 g of aluminum sulfate 18-hydrate by heating above 60° C. The resulting solution is designated as the aqueous solution (a).
In 150 ml of deionized water are dissolved 55.0 g of sodium carbonate. The resulting solution is designated as the aqueous solution (b).
The aqueous solution (b) is added with stirring to the aqueous solution (a) kept at about 60° C. Stirring is continued for 15 minutes. The resulting mixture of the two solutions is a gel. The gel is evaporated to dryness, and the dried product is heated at 1200° C. for 5 hours. Water is added to the heated product to dissolve free sulfate. Insoluble solids are filtered off, washed with water, and finally dried. The obtained alumina flake is examined by X-ray diffractometry. The diffraction pattern has only peaks attributed to corundum structure (α-alumina structure).
D50 is 11.3 μm and D80 is 16.2 μm. The MIU value is 0.55 measured by the KES friction tester.
3.6 g of sodium sulfate is added in the aqueous solution (a) of Example 1. The obtained alumina flake is examined by X-ray diffractometry. The diffraction pattern has only peaks attributed to corundum structure (α-alumina structure).
D50 is 12.3 μm and D80 is 17.0 μm. The MIU value is 0.59 measured by the KES friction tester.
11.9 g of sodium sulfate is added in the aqueous solution (a) of Example 1. The obtained alumina flake is examined by X-ray diffractometry. The diffraction pattern has only peaks attributed to corundum structure (α-alumina structure).
D50 is 12.9 μm and D80 is 17.8 μm. The MIU value is 0.70 measured by the KES friction tester.
0.50 g of 3.44% solution of titanyl sulfate is added in the aqueous solution (a) of Example 1.
The obtained alumina flake is examined by X-ray diffractometry. The diffraction pattern has only peaks attributed to corundum structure (α-alumina structure).
D50 is 11.5 μm and D80 is 15.8 μm measured by Malvern MS 2000. The MIU value is 0.56 measured by the KES friction tester.
In 300 ml of deionized water are dissolved 111.9 g of aluminum sulfate 18-hydrate, 57.3 g of anhydride sodium sulfate, and 46.9 g of potassium sulfate by heating above 60° C. To resulting solution is added 4.06 g of 35.0% solution of zinc sulfate. The resulting solution is designated as the aqueous solution (a).
In 150 ml of deionized water are dissolved 0.45 g of sodium tertiary phosphate 12-hydrate and 55.0 g of sodium carbonate. The resulting solution is designated as the aqueous solution (b).
The aqueous solution (b) is added with stirring to the aqueous solution (a) kept at about 60° C. Stirring is continued for 15 minutes. The resulting mixture of the two solutions is a gel. The gel is evaporated to dryness, and the dried product is heated at 1200° C. for 5 hours. Water is added to the heated product to dissolve free sulfate. Insoluble solids are filtered off, washed with water, and finally dried. The obtained alumina flake is examined by X-ray diffractometry. The diffraction pattern has only peaks attributed to corundum structure (α-alumina structure).
D50 is 22.3 μm and D80 is 35.0 μm. The MIU value is 1.00 measured by the KES friction tester.
Measurements
Evaluation for Particle Size D50 and D80
D50 and D80 of the alumina flakes according to the above given (comparative) examples are evaluated by using Malvern MS2000.
Evaluation for MIU Value
MIU value is evaluated by using KES friction tester (KES-SE-DC-tester by KATO TECH. Co., Ltd.).
Determination of the Thickness and Particle Size and the Thickness Distribution
0.01 g/l of the alumina flake slurry is prepared and 0.1 ml of this slurry is dropped onto a flat substrate like a silicon wafer. The substrate is dried and cut to adequate size. The substrate is set with almost vertically tilted angle on the base of SEM (Scanning electronic microscope) and the thickness of the alumina flake is determined.
The thickness of more than 100 alumina flakes is measured for the calculation of the thickness distribution. The standard deviation of the thickness is calculated with the Gaussian distribution equation.
Al2O3 flakes according to the above given examples are summarized in the following table:
Heat phase B to 85° C. and stir until all ingredients are melted. Cool down to 75° C. and add the ingredients of phase A and C while stirring. Fill into godets while compact is still liquid.
It is further possible to use it as creamy eye shadow, as blush for cheeks and color for lips. The filler pigment of Example 1 improves the homogeneous application, supports a smooth and good gliding skin feel and promotes the pearl luster effect.
Heat phase B to 85° C. and stir until all ingredients are melted. Cool down to 75° C. and add the ingredients of phase A and C while stirring. Fill into godets while compact is still liquid.
It is further possible to use it as creamy eye shadow, as blush for cheeks and color for lips. The filler pigment of Example 2 improves the homogeneous application, supports a smooth and good gliding skin feel and promotes the pearl luster effect.
Heat phase B to 85° C. and stir until all ingredients are melted. Cool down to 75° C. and add the ingredients of phase A and C while stirring. Fill into godets while compact is still liquid.
It is further possible to use it as creamy eye shadow, as blush for cheeks and color for lips. The filler pigment of Example 3 improves the homogeneous application, supports a smooth and good gliding skin feel and promotes the pearl luster effect.
Heat phase B to 85° C. and stir until all ingredients are melted. Cool down to 75° C. and add the ingredients of phase A and C while stirring. Fill into godets while compact is still liquid.
It is further possible to use it as creamy eye shadow, as blush for cheeks and color for lips. The filler pigment of Example 4 improves the homogeneous application, supports a smooth and good gliding skin feel and promotes the pearl luster effect.
ZEA MAYS
Mix the ingredients of phase B until the blend is uniform. Add the pigments of phase A. Then add the presolved phase C while stirring strongly. The powder is pressed between 30-40 bar.
The filler pigment of Example 1 is improving the structure of the powder and the pay-off significantly. Furthermore it reduces the forming of greasy spots on the surface of the powder—an effect frequently appearing when using an eye shadow often.
ZEA MAYS
Mix the ingredients of phase B until the blend is uniform. Add the pigments of phase A. Then add the presolved phase C while stirring strongly. The powder is pressed between 30-40 bar.
The filler pigment of Example 2 is improving the structure of the powder and the pay-off significantly. Furthermore it reduces the forming of greasy spots on the surface of the powder—an effect frequently appearing when using an eye shadow often.
ZEA MAYS
Mix the ingredients of phase B until the blend is uniform. Add the pigments of phase A. Then add the presolved phase C while stirring strongly. The powder is pressed between 30-40 bar.
The filler pigment of Example 3 is improving the structure of the powder and the pay-off significantly. Furthermore it reduces the forming of greasy spots on the surface of the powder—an effect frequently appearing when using an eye shadow often.
ZEA MAYS
Mix the ingredients of phase B until the blend is uniform. Add the pigments of phase A. Then add the presolved phase C while stirring strongly. The powder is pressed between 30-40 bar.
The filler pigment of Example 4 is improving the structure of the powder and the pay-off significantly. Furthermore it reduces the forming of greasy spots on the surface of the powder—an effect frequently appearing when using an eye shadow often.
Add phase A slowly with vigorous stirring to phase B. Homogenize. Afterwards add phase C.
The filler pigment of Example 1 adds body and a pleasant skin feeling to this white emulsion. After application it leaves a nice silver shimmer on the skin.
Add phase A slowly with vigorous stirring to phase B. Homogenize. Afterwards add phase C.
The filler pigment of Example 2 adds body and a pleasant skin feeling to this white emulsion. After application it leaves a nice silver shimmer on the skin.
Add phase A slowly with vigorous stirring to phase B. Homogenize. Afterwards add phase C.
The filler pigment of Example 3 adds body and a pleasant skin feeling to this white emulsion. After application it leaves a nice silver shimmer on the skin.
Add phase A slowly with vigorous stirring to phase B. Homogenize. Afterwards add phase C.
The filler pigment of Example 4 adds body and a pleasant skin feeling to this white emulsion. After application it leaves a nice silver shimmer on the skin.
Heat phase B to 85° C. and stir until all ingredients are melted. Cool down to 75° C. and add the ingredients of phase A and C while stirring. Fill into godets while the 3-in-1 Compact is still liquid.
Add phase A slowly with vigorous stirring to phase B. Homogenize. Afterwards add phase C.
ZEA MAYS
Mix the ingredients of phase B until the blend is uniform. Add the pigments of phase A. Then add the presolved phase C while stirring strongly. The powder is pressed between 30-40 bar.
OLEA EUROPAEA
Heat phase A and B separately to 75° C. Add phase C slowly to phase A while stirring until a homogeneous mixture is obtained. At 75° C. add phase B to phase A/C and homogenize for 1 min. (Ultra Turrax T25 at 8000 rpm). Cool down to 35° C. and add perfume. Cool down to room temperature while stirring. The pH value should be between 5-5.5.
Heat phase A and B separately to 80° C. Ad d phase B slowly to A while stirring. Homogenize. Add the ingredients of phase C to adjust the pH value.
Heat phase A and B separately to 80° C. Add phase B slowly to A while stirring. Homogenize it well. Add the ingredients of phase C at 35 degrees. Neutralize to adjust the pH.
Heat the ingredients of phase B to 85° C. Ad d phase A and stir until the melt is homogeneous. Cool down slowly to room temperature while stirring slowly and continuously without high shear forces to reach a smooth, homogeneous product.
Mix phase A and add this phase slowly with vigorous stirring to phase B. Homogenize. Finally add phase C under stirring.
Grind the ingredients of phase A until the blend is homogeneous. Then add the previously dissolved phase B and grind again until the whole phase A/B is homogeneous. Fill the bulk into pans and press with the desired pressure. The pressure for pans with 36 mm in diameter is approx. 25-35 bar.
Mix all ingredients by stirring at 1000 rpm for 10 min. Avoid introducing air.
COPERNICIA CERIFERA,
RICINUS COMMUNIS
Heat the ingredients of phase B to 75° C. Ad d phase A and stir until the melt is homogeneous. Transfer the mixture into a moulding machine, which is heated up to 65° C., add the perfume and stir about 15 minutes. Fill into a lipstick mould which has been preheated to about 55° C. Cool down the mould and transfer the cold bullets to mechanisms. A highly glossy appearance can be obtained by subsequent flaming if desired.
PRUNUS AMYGDALUS
DULCIS OIL
Disperse Carbopol ultrez 21 in the water. Add the xanthane gum premixed with glycerin. Add the active ingredients and the titriplex. Add the UV-pearls. Prepare phase B and heat A and B up 80° C. Emulsion B in A. Neutralise with C. At temperature <60° C. add D. At temperature <30° C. add E.
PERSEA GRATISSIMA OIL
Heat phase A and phase B separately to 75° C. Incorporate phase A into phase B while stirring and homogenize. Cool down to 30° C. while stirring and add ingredients of phase C.
Disperse all pigments and the filler in the water of phase A. Add some drops of citric acid solution to lower the viscosity if necessary, then add the Carbopol Ultrez 21 while stirring. Mix with high agitation until thoroughly dispersed. Mix the ingredients of phase B until a complete solution is obtained. Add phase B slowly to phase A while stirring (not homogenizing), then add phase C while stirring and adjust pH to 7.0-7.5 with citric acid solution, if necessary.
RICINUS COMMUNIS
COPERNICIA CERIFERA,
Heat the ingredients of phase B to 75° C. Ad d phase A and stir until the melt is homogeneous. Transfer the mixture into a moulding machine, which is heated up to 65° C., add the perfume and stir about 15 minutes. Fill into a lipstick mould which has been preheated to about 55° C. Cool down the mould and transfer the cold bullets to mechanisms. A highly glossy appearance can be obtained by subsequent flaming if desired.
Combine Phase A with gentle agitation. Spray Phase B onto batch while agitating bulk. Pass entire batch through a jump gap.
Heat phases A and B separately to 80° C. Add phase A and B while stirring. Homogenize. At 60° C. add the ingredients of phase C in the given order while strong mixing. Homogenize. Disperse RonaCare® Luremin™ in the water of phase D and add to the batch while stirring. Finally add preservative sand fragrance below 40° C. Check pH and adjust to 5-5.5 with citric acid solution if necessary. Cool down to room temperature.
| Number | Date | Country | Kind |
|---|---|---|---|
| 14001769.0 | May 2014 | EP | regional |
| Filing Document | Filing Date | Country | Kind |
|---|---|---|---|
| PCT/EP2015/000906 | 5/4/2015 | WO | 00 |
