Near-complexion transparent matte sericite powder and preparation method thereof

Abstract

The invention relates to a preparation method of near-skin-color sericite powder, which comprises the following steps: (1) mixing 100 parts of sericite powder with deionized water to form a suspension with a solid-to-liquid ratio of 1: (5-15), uniformly stirring, heating the suspension to 65-85 DEG C, and adjusting the pH value of the suspension to 2.0-8.0 by using hydrochloric acid; (2) adding 1-10 parts of ferric salt, cerium salt and silicon salt solutions corresponding to ferric oxide, cerium oxide and silicon dioxide, keeping the pH value constant by using alkali liquor or dilute acid, and stirring for 15 minutes at a constant temperature after the charging is completed; and (3) filtering, washing and drying the suspension liquid formed in the step (2) to obtain the near-skin-color matte transparent sericite powder. The prepared near-skin-color sericite powder can be used as a filler in cosmetics, the skin color is natural and refreshing after the sericite powder is smeared, and the sericite powder has good concealing and sunscreen performance.

Description

Technical Field

[0001] The invention relates to a skin-colored transparent matte sericite powder and a preparation method thereof, and belongs to the field of color powder fillers or pigments for cosmetics. Background Art

[0002] As people's living standards improve, their pursuit of beauty and physical health continues to increase. The use of non-toxic nude makeup effects has become a focus of attention. In order to meet consumers' high requirements for colorants in cosmetics, research in the cosmetics industry is expanding day by day.

[0003] CN102753138A discloses a basic makeup cosmetic and a method for producing the same.

[0004] CN103788713A discloses a red iron oxide pigment containing sericite powder. The pigment is prepared from the following raw materials in parts by weight: 280-300 parts of red iron oxide, 2-3 parts of allyl polyethylene glycol, 2-3 parts of magnesium aluminosilicate, 6-8 parts of glass fiber, 20-25 parts of sericite powder, 1-2 parts of lanthanum oxide, 3-4 parts of zirconium dioxide, 2-3 parts of dimethyl silicone oil, and 4-5 parts of additives. The pigment utilizes raw materials such as allyl polyethylene glycol and dimethyl silicone oil to improve the dispersibility of the red iron oxide powder, and the raw materials such as glass fiber, sericite powder, and zirconium dioxide to improve the hardness and toughness of the red iron oxide pigment, and the red iron oxide pigment is wear-resistant and weather-resistant, and has a certain temperature resistance. The red iron oxide pigment prepared by the invention has a delicate appearance, is evenly dispersed in a matrix material, has a bright and lasting color, and has a long service life, and can be widely used in various fields.

[0005] CN115252443A discloses a sunscreen compound and a wet and dry sunscreen powder containing the sunscreen compound, which belongs to the field of assembly and compounding of micro-nano powders. The sunscreen compound comprises 55-90 parts of component A, 1-5 parts of component B, and at least one of modified nano-TiO sericite, talc, aluminum oxide and organic silicon powder by weight, and the particle size range is 5-15 μm; component B is selected from at least one of silane modifiers and silicone oil modifiers. The sunscreen compound of the present invention is used to improve the dispersibility of inorganic sunscreen in powder, so that the efficacy of the sunscreen can be more effectively exerted.

[0006] Natural sericite is superior to other fillers in terms of whiteness, purity, transparency and stability, and contains fewer impurities and heavy metal elements, so it has greater advantages in cosmetic applications.

[0007] However, since natural sericite itself is white or grayish white (grayish tone) with not too high whiteness, and is a low-refractive-index transparent substrate, it is difficult to obtain good angle-dependent color or colorful optical effects by coating it with a commonly used metal oxide layer. Therefore, technical personnel in this field believe that sericite has low application value in the field of pearlescent pigments for cosmetics and therefore do not pay attention to it. Summary of the invention

[0008] The purpose of the present application is to provide a transparent, nearly skin-colored matte sericite powder that can be used in cosmetics.

[0009] The inventor of the present application has found through a large number of experiments that by coating a layer of low-refractive-index metal oxides, i.e., oxides of iron, cerium, silicon, etc., on ultra-fine matte sericite (produced in Sichuan Saihe) powder, a (modified) matte sericite powder (composed of modified matte sericite particles) with a skin color close to that of the skin can be obtained. The sericite powder has matte transparency, good dispersibility and UV sunscreen function, and makes the skin naturally refreshing and transparent after application, and is a new cosmetic carrier. It has the smoothness and transparency of sericite powder itself, and its skin color close to that of the skin can be used in cosmetics to present a nude makeup effect, thereby completing the present invention.

[0010] According to the first embodiment of the present invention, there is provided a (modified) transparent matte sericite powder or particles close to the skin color, that is, a (modified) transparent matte sericite in powder or particle form close to the skin color, the transparent matte sericite particles or powder (referred to as matte sericite particles) comprising: 1) a granular or particulate matte sericite substrate (or substrate), and 2) a metal oxide coating (one or two layers) on the surface of the substrate; or 1) a granular or particulate matte sericite substrate (or substrate), 2) a metal oxide coating layer (one or two layers) on the surface of the substrate, and 3) a silicon oxide coating layer or a hydrated silicon oxide coating layer on the surface of the metal oxide coating layer (one or two layers); The (one or two) metal oxide coating layers are one or two (or one or two) selected from the group consisting of an iron oxide coating layer, a cerium oxide coating layer, and an iron oxide / cerium oxide mixed oxide coating layer. That is, the metal oxide coating layer is: an iron oxide coating layer, a cerium oxide coating layer, (in order from the inside to the outside) an iron oxide coating layer + a cerium oxide coating layer, or (in order from the inside to the outside) a cerium oxide coating layer + an iron oxide coating layer, or (single) an iron oxide / cerium oxide mixed oxide coating layer.

[0011] The order from inside to outside refers to from close to the substrate to the outer layer.

[0012] Preferably, the (average) particle size or (average) flake size of the matte sericite (e.g., produced by Sichuan Saihe New Material Technology Co., Ltd.) substrate (or base sheet) is 3-30 μm, more preferably 3.2-25 μm, more preferably 3.5-22 μm, more preferably 3.7-20 μm, more preferably 3.8-18 μm, more preferably 4-15 μm, for example 4.5, 5, 6, 7, 8, 9, 10, 11, 12, 13 or 14 μm.

[0013] Preferably, based on 100 parts by weight of matte sericite (produced by Sichuan Saihe New Materials Technology Co., Ltd.) substrate (or substrate), the weight of the metal oxide coating (e.g., iron oxide coating and / or cerium oxide coating) on ​​the surface of the substrate is 1-12 parts by weight, preferably 1.2-10 parts by weight, more preferably 1.5-8 parts by weight, more preferably 1.6-7 parts by weight, more preferably 1.8-6 parts by weight, and more preferably 2-5 parts by weight.

[0014] Preferably, based on 100 parts by weight of the matte sericite substrate (or substrate), the weight of the silicon oxide coating layer or the hydrated silicon oxide coating layer on the surface of the metal oxide coating layer is 2-10 parts by weight, preferably 2.5-9 parts by weight, more preferably 3-8 parts by weight, more preferably 3.5-7.5 parts by weight, more preferably 4-7 parts by weight, more preferably 4.5-6.5 parts by weight, for example 5-6 parts by weight.

[0015] Preferably, the thickness of the metal oxide coating layer 2) is 1-20 nm (nanometer), preferably 1.1-18 nm, preferably 1.2-15 nm, preferably 1.5-12 nm, preferably 1.8-10 nm, preferably 2-9 nm, preferably 2.2-8 nm, more preferably 2.5-7 nm, for example 3, 4, 5 or 6 nm.

[0016] The parameters (or color coordinates) of the (modified) matte sericite powder or particles close to skin color of the present invention in the CIE Lab system are as follows: L value is 56-62, preferably 57-61, more preferably 58-60.50; a value is 4.5-9, preferably 4.8-8.5, preferably 5-8, preferably 5.1-7.3; The b value is 10-14, preferably 10.5-13.5, preferably 11-13, preferably 11.50-12.50.

[0017] ΔEab is 0.4-2.2, preferably 0.45-2.1, preferably 0.48-2.0, preferably 0.5-1.9, preferably 0.52-1.85, preferably 0.55-1.75.

[0018] Among them, L represents brightness (white, black), a represents red and green, b represents yellow and blue, and ΔE represents color difference.

[0019] Skin-colored (modified) matte sericite powder has the same meaning as skin-colored transparent matte sericite powder or particles.

[0020] According to a second embodiment of the present invention, the present invention provides a method for preparing a skin-colored transparent matte sericite powder or particles, comprising the following steps: (1) 100 parts by weight of low-refractive-index transparent matte sericite (produced by Sichuan Saihe New Materials Technology Co., Ltd.) powder is mixed with deionized water to form a suspension with a solid-liquid ratio of 1: (5-15), preferably 1: (6-14), preferably 1: (7-13), preferably 1: (8-12), and stirred evenly. The suspension is heated to a temperature of, for example, 60-90° C., preferably 65-85° C., preferably 70-80° C., and the pH value of the suspension is adjusted to 2.0-8.0, preferably 2.2-7.0, preferably 2.3-6.8, preferably 2.5-6.5, for example, pH 3, 4, 5, 6, with hydrochloric acid; (2) adding 1 to 10 parts by weight, preferably 2 to 9 parts by weight, preferably 3 to 8 parts by weight of an aqueous solution of a water-soluble iron salt or a water-soluble cerium salt corresponding to iron oxide or cerium oxide (as the first metal salt) to the suspension obtained in step (1), wherein the molar concentration of the aqueous solution of the iron salt or the cerium salt is 0.15 to 2.5 mol / L, preferably 0.2 to 2.0 mol / L, preferably 0.25 to 1.8 mol / L, preferably 0.3 to 1.5 mol / L, for example 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.4 mol / L; using an alkali or an acid (for example, an aqueous sodium hydroxide solution with a concentration of 5 to 30 wt% or an ammonia solution with a concentration of 10 to 30 wt%, or an acid such as a hydrochloric acid solution with a concentration of 5 to 10 wt%) to keep the pH value of the mixture constant (for example, within an acidic pH range, for example, keeping the pH value within a range of 2.2 to 7.0, preferably 2.3 to 6.8, preferably 2.5 to 6.5, for example, pH values ​​of 3, 4, 5, or 6), and after the addition is completed, stirring at a constant temperature (for 5 to 50 minutes, for example, 15 to 30 minutes) to obtain a suspension; (3) Optionally, (substantially) repeating step (2), further adding 1 to 10 parts by weight, preferably 2 to 9 parts by weight, preferably 3 to 8 parts by weight of an aqueous solution of a metal salt (i.e., an iron salt or a cerium salt) different from the metal salt (i.e., a cerium salt or an iron salt) (i.e., a first metal salt) in step (2) to the suspension obtained in step (2), to obtain a suspension; (4) Optionally, 1 to 10 parts by weight, preferably 2 to 9 parts by weight, preferably 3 to 8 parts by weight of an aqueous solution of a water-soluble silicon salt corresponding to silicon oxide is further added to the suspension obtained in step (2) or step (3), wherein the molar concentration of the aqueous solution of the silicon salt is 0.15 to 2.5 mol / L, preferably 0.2 to 2.0 mol / L, preferably 0.25 to 1.8 mol / L, preferably 0.3 to 1.5 mol / L, for example 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.4 mol / L; using an alkali or an acid (for example, an aqueous sodium hydroxide solution with a concentration of 5 to 30 wt% or an ammonia solution with a concentration of 10 to 30 wt%, or an acid such as a hydrochloric acid solution with a concentration of 5 to 10 wt%) to keep the pH value of the mixture constant (for example, within an acidic pH range, for example, keeping the pH value within a range of 2.2 to 7.0, preferably 2.3 to 6.8, preferably 2.5 to 6.5, for example, pH values ​​of 3, 4, 5, or 6), and after the addition is completed, stirring at a constant temperature (for 5 to 50 minutes, for example, 15 to 30 minutes) to obtain a suspension; and (5) The suspension formed in the above steps (i.e., step 2, 3 or 4) is filtered, washed and dried to obtain a skin-colored, transparent, matte sericite powder or particles.

[0021] The metal salt in step (3) is different from the metal salt in step (2), which means: when an iron salt (as the first metal salt) is used in step (2), a cerium salt (as the second metal salt) is used in step (3); or, when a cerium salt (as the first metal salt) is used in step (2), an iron salt (as the second metal salt) is used in step (3). Or, when an aqueous solution of an iron salt (as the first metal salt) is used in step (2), an aqueous solution of a cerium salt (as the second metal salt) is used in step (3); or, when an aqueous solution of a cerium salt (as the first metal salt) is used in step (2), an aqueous solution of an iron salt (as the second metal salt) is used in step (3). The remaining conditions (such as process, concentration, temperature, etc.) in the two steps (2) and (3) are the same. When the first metal salt is a (water-soluble) iron salt, the second metal salt is a (water-soluble) cerium salt, and vice versa, when the first metal salt is a (water-soluble) cerium salt, the second metal salt is a (water-soluble) iron salt.

[0022] In the present application, "optionally" means to be performed or not to be performed, or to have or not to have.

[0023] In this application, close to skin color refers to skin color close to that of yellow people.

[0024] Among them, matte sericite (produced by Sichuan Saihe New Material Technology Co., Ltd.) is a low-refractive-index transparent substrate, and its refractive index is 1.52-1.64, more preferably 1.54-1.62, more preferably 1.56-1.60, for example 1.58.

[0025] Generally, the metal oxide is composed of iron oxide or cerium oxide, and the silicon oxide is composed of silicon dioxide or hydrated silicon oxide. The molar concentration of the iron salt or cerium salt is 0.2-2 mol / L, preferably 0.2-0.8 mol / L, and particularly preferably 0.2-0.5 mol / L.

[0026] In the transparent matte sericite powder close to the skin color, the coverage rate of the oxide is 1 to 10 wt %, preferably 1.5 to 8 wt %, preferably 2 to 5 wt %, based on the weight of the substrate.

[0027] The iron salt is selected from one or more of FeCl3, Fe2(SO)4 and Fe(NO3)3.

[0028] The cerium salt is selected from one or more of CeCl3, Ce(SO4)2·4H2O and Ce(NO3)4.

[0029] The silicon-containing salt is selected from sodium metasilicate (Na2SiO3) or sodium metasilicate hydrate.

[0030] The drying can be carried out at 80-150° C., preferably 100-120° C., for 10 to 60 minutes, preferably 20 to 30 minutes.

[0031] The present invention further relates to a skin-colored transparent matte sericite powder or microparticles prepared by the above method, whose parameters (or color coordinates) in the CIE Lab system are as described above.

[0032] The present invention further relates to the use of the skin-colored transparent matte sericite powder or microparticles in cosmetics, such as the use in preparing cosmetic pressed powder.

[0033] In order to obtain different skin-color-like tones, some post-processing is required to obtain the desired effect. Selecting different base tones, such as pink, pink orange or apricot, can make the nude makeup effect close to the skin color. In addition to titanium dioxide, iron oxide is the most widely used inorganic coloring pigment in cosmetics. Iron oxide has a bright and pure color, and its soft tones are pleasing to the eye and have a unique style. In terms of chemical stability, iron oxide has extremely strong isolation and extremely low water absorption against ultraviolet rays. Cerium oxide is slightly yellowish with a slight red color and can be used in cosmetics as an ultraviolet shielding agent. Therefore, iron oxide and cerium oxide are both ideal pigments for cosmetics. Combining the matte sericite (produced in Sichuan Saihe) substrate with oxides can better show the characteristics. Therefore, the present invention studies a matte sericite powder close to the skin color with good dispersibility and transparency, so that it can be used in cosmetics as a carrier of pressed powder, loose powder, honey powder, etc. After application, the skin color is naturally refreshing, making the skin smooth and transparent, close to the skin color of the yellow race, thereby presenting a nude makeup effect.

[0034] Compared with the prior art, the beneficial technical effects of the present invention are: This type of pigment is a matte sericite powder composed of low-refractive index oxides. The matte sericite powder has a matte transparency close to the skin color and has UV protection function, making the skin smooth and transparent. It is a new cosmetic color powder filler and can be widely used in various cosmetics. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 The following are color photographs of the pressed powders of Examples 1-4.

[0036] Figure 2 The following are color photographs of the pressed powders of Examples 5-7. DETAILED DESCRIPTION

[0037] The technical solution of the present invention is illustrated below by way of example, and the scope of protection requested by the present invention includes but is not limited to the following embodiments.

[0038] In the embodiment, matte sericite powder (produced from Sichuan Saihe New Material Technology Co., Ltd.) is used as the base material, and oxides of different components are coated. It is produced by grinding natural matte sericite minerals (such as Liangshan Prefecture, Sichuan Province). Example 1

[0039] (1) Weigh 100 g of matte sericite powder (produced by Sichuan Saihe New Materials Technology Co., Ltd., with a refractive index of 1.58) with an average particle size of 12 μm, put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) The suspension was heated in a constant temperature water bath and stabilized at 80°C, and the pH was adjusted to 3.0 with dilute hydrochloric acid; (3) According to the amount of iron oxide to be added, 10.14 g of FeCl3·6H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 3.0 with sodium hydroxide solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (5) The structure of the pigment obtained is as follows: 100 parts of matte sericite mica powder (Sichuan Saihe) is used as a base material, and 3 parts by weight of iron oxide with a thickness of about 2.5 nm is coated on the surface of the mica base material to obtain a matte transparent matte sericite mica powder close to the skin color (light orange).

[0040] 10 g of the sample from Example 1 was weighed and pressed into a cake under a pressure of 60 kg. Example 2

[0041] (1) Weigh 100 g of matte sericite powder (produced by Sichuan Saihe, refractive index 1.58) with an average particle size of 12 μm, put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) The suspension was heated in a constant temperature water bath and stabilized at 80°C, and the pH was adjusted to 3.0 with dilute hydrochloric acid; (3) According to the amount of iron oxide added, 6.76g FeCl3·6H2O was dissolved in 100ml water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5ml / min. At the same time, the pH was kept constant at 3.3 with sodium hydroxide solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) adjusting the temperature of the suspension to 83°C and adjusting the pH to 6.5 with liquid alkali; (5) According to the amount of hydrated silicon oxide to be added, 18.21 g of Na2SiO3·9H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, a dilute hydrochloric acid solution was used to keep the pH constant at 6.5. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (6) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (7) The structure of the pigment obtained is as follows: 100 parts of matte sericite mica (produced in Sichuan Saihe) powder is used as the base material, and 2 parts of iron oxide and 5 parts of hydrated silicon oxide are coated on the surface of the mica base material. The thickness of the mixed coating layer is about 6 nm, and a matte transparent matte sericite mica powder close to the skin color (pink orange) is obtained.

[0042] 10 g of the sample from Example 2 was weighed and pressed into a cake under a pressure of 60 kg. Example 3

[0043] (1) Weigh 100 g of matte sericite powder (produced in Sichuan Saihe, refractive index 1.59) with an average particle size of 7 μm, put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) Heat the suspension in a constant temperature water bath and stabilize it at 80°C, and adjust the pH to 6.5 with dilute hydrochloric acid or liquid alkali; (3) According to the amount of cerium oxide added, 10.10 g of Ce(NO3)3·6H2O was dissolved in 100 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 6.5 with an ammonia solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (5) The structure of the pigment obtained is as follows: 100 parts of matte sericite mica (produced in Sichuan Saihe) powder is used as the base material, and 4 parts of cerium oxide is coated on the surface of the mica base material. The coating layer has a thickness of about 3 nm, and a matte transparent matte sericite mica powder close to the skin color (light orange) is obtained.

[0044] 10 g of the sample from Example 3 was weighed and pressed into a cake under a pressure of 60 kg. Example 4

[0045] (1) Weigh 100 g of matte sericite powder (produced in Sichuan Saihe, refractive index 1.59) with an average particle size of 7 μm, put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) Heat the suspension in a constant temperature water bath and stabilize it at 80°C, and adjust the pH to 6.5 with dilute hydrochloric acid or liquid alkali; (3) According to the amount of cerium oxide added, 7.57g Ce(NO3)3·6H2O was dissolved in 100ml water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5ml / min. At the same time, the pH was kept constant at 6.5 with an ammonia solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) The suspension was adjusted to 83°C and the pH was maintained at 6.5 with aqueous ammonia. (5) According to the amount of hydrated silicon oxide to be added, 18.21 g of Na2SiO3·9H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, a dilute hydrochloric acid solution was used to keep the pH constant at 6.5. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (6) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (7) The structure of the pigment obtained is as follows: 100 parts of matte sericite mica (produced in Sichuan Saihe) powder is used as the base material, and 3 parts of cerium oxide and 5 parts of hydrated silicon oxide are coated on the surface of the mica base material. The thickness of the mixed coating layer is about 7 nm, and a matte transparent matte sericite mica powder close to the skin color (light orange) is obtained.

[0046] 10 g of the sample from Example 4 was weighed and pressed into a cake under a pressure of 60 kg. Example 5

[0047] (1) Weigh 100 g of matte sericite powder (produced by Sichuan Saihe New Materials Technology Co., Ltd., with a refractive index of 1.59) with an average particle size of 6 μm, put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) The suspension was heated in a constant temperature water bath and stabilized at 80°C, and the pH was adjusted to 3.0 with dilute hydrochloric acid; (3) According to the amount of iron oxide to be added, 10.14 g of FeCl3·6H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 3.0 with sodium hydroxide solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) Adjust the pH of the suspension to 6.5 with liquid alkali; (5) According to the amount of cerium oxide added, 10.10 g of Ce(NO3)3·6H2O was dissolved in 100 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 6.5 with an ammonia solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (6) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (7) The structure of the pigment obtained is as follows: 100 parts of matte sericite mica powder (Sichuan Saihe) is used as the base material, and 3 parts by weight of iron oxide and 4 parts by weight of cerium oxide are coated on the surface of the mica base material with a thickness of about 5 nm to obtain a matte transparent matte sericite mica powder close to the skin color (light orange).

[0048] 10 g of the sample from Example 5 was weighed and pressed into a cake under a pressure of 60 kg. Example 6

[0049] (1) Weigh 100 g of matte sericite powder with an average particle size of 5 μm (produced by Sichuan Saihe New Materials Technology Co., Ltd., with a refractive index of 1.59) and put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) The suspension was heated in a constant temperature water bath and stabilized at 80°C, and the pH was adjusted to 3.0 with dilute hydrochloric acid; (3) According to the amount of iron oxide to be added, 10.14 g of FeCl3·6H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 3.0 with sodium hydroxide solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) Adjust the pH of the suspension to 6.5 with liquid alkali; (5) According to the amount of cerium oxide added, 10.10 g of Ce(NO3)3·6H2O was dissolved in 100 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 6.5 with an ammonia solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (6) The suspension was adjusted to 82°C and the pH was maintained at 7 with aqueous ammonia. (7) According to the amount of hydrated silicon oxide to be added, 18.21 g of Na2SiO3·9H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 7 with dilute hydrochloric acid solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (8) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (9) The structure of the pigment obtained is as follows: 100 parts of matte sericite powder (Sichuan Saihe) is used as the base material, and 3 parts by weight of iron oxide, 4 parts by weight of cerium oxide and 5 parts of hydrated silicon oxide are coated on the surface of the mica base material to a thickness of about 6 nm to obtain a matte transparent matte sericite powder close to the skin color (light orange).

[0050] 10 g of the sample from Example 6 was weighed and pressed into a cake under a pressure of 60 kg. Example 7

[0051] (1) Weigh 100 g of matte sericite powder with an average particle size of 5 μm (produced by Sichuan Saihe New Materials Technology Co., Ltd., with a refractive index of 1.59) and put it into a 2 L reactor, add 1000 ml of deionized water, and stir to evenly disperse it into a suspension; (2) The suspension was heated in a constant temperature water bath and stabilized at 80°C, and the pH was adjusted to 6.0 with dilute hydrochloric acid; (3) According to the amount of iron oxide added, 10.14g FeCl3·6H2O and 10.10g Ce(NO3)3·6H2O were dissolved in 150ml water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5ml / min. At the same time, the pH was kept constant at 6.0 with sodium hydroxide solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (4) The suspension was adjusted to 82°C and the pH was maintained at 7 with aqueous ammonia. (5) According to the amount of hydrated silicon oxide to be added, 18.21 g of Na2SiO3·9H2O was dissolved in 150 ml of water to prepare a mixed solution, and the mixed solution was added dropwise at a rate of 0.5 ml / min. At the same time, the pH was kept constant at 7 with dilute hydrochloric acid solution. After the addition was completed, the mixture was stirred at a constant temperature for 15 minutes; (6) After the reaction is completed, the suspension is filtered, washed with deionized water, and dried at 105°C; (7) The structure of the pigment obtained is as follows: 100 parts of matte sericite powder (Sichuan Saihe) is used as the base material, and 7 parts by weight of a mixture of iron oxide and cerium oxide and 5 parts of hydrated silicon oxide are coated on the surface of the mica base material to a thickness of about 6 nm to obtain a matte transparent matte sericite powder close to the skin color (light orange).

[0052] 10 g of the sample from Example 7 was weighed and pressed into a cake under a pressure of 60 kg.

[0053] test: 10 grams of sample was weighed from the samples of Examples 1-7, and pressed into a cake under a pressure of 60 kg. The L, a, b values ​​and ΔE were measured using an X-rite colorimeter, as shown in Table 1. The color photographs of the powder cakes of Examples 1-4 are shown in the attached figure. Figure 1 As shown in the figure, the color photos of the pressed powders of Examples 5-7 are shown in the attached Figure 2 as shown in .

[0054] Weigh 0.5 g of sample from the samples of Examples 1-7, add 4.5 g of transparent polyester resin, drop a few drops of anhydrous ethanol, stir well, apply it on a transparent glass plate with a 20 μm coating rod, and measure the transmittance with a visible light transmittance meter, as shown in Table 1.

[0055] Table 1 - Effects Sample parameters Skin☆(Cheek) Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 L 59.47 60.50 58.44 59.10 59.3 60.68 61.01 59.87 a 6.01 5.11 7.11 6.42 6.22 7.30 7.21 7.04 b 12.01 11.50 12.85 12.43 12.5 11.2 12.20 11.98 ΔEab \ 1.46 1.72 0.69 0.56 1.77 1.96 1.10 Light transmittance (%) \ 81 83 85 86 76 78 79 Note: ☆ Excerpted from "Chinese Journal of Aesthetic Medicine" 2010 Issue 02, "Skin Color of Different Parts of Healthy Adults in Shanghai".

[0056] In the CIE Lab system, L represents brightness (white, black), a represents red and green, b represents yellow and blue, and ΔE represents color difference.

[0057] ΔE<1: The color difference cannot be distinguished by the naked eye.

[0058] 1<ΔE<2: The colors are very similar (slight color difference is visible to the naked eye).

[0059] 2<ΔE<3.5: Slightly clear color difference.

[0060] 3.5<ΔE<5: The color difference is obvious.

[0061] As can be seen from Table 1, the color difference is less than 2, and the samples of the embodiments are close to the skin color of the yellow race. In particular, the samples of Examples 3, 4 and 7 are closer to the skin color of the yellow race, and there is almost no difference in color from the skin color of the yellow race, among which the sample of Example 4 is closest to the skin color of the yellow race.

[0062] For this material, transmittance is proportional to transparency. When the transmittance is between 76-86, the transparency is good.

[0063] The results of the above examples show that by coating 2 to 10 parts of iron oxide or cerium oxide on the surface of matte sericite (produced in Sichuan Saihe), the thickness of the (metal oxide) coating layer is about 1.5 to 8 nm, and a transparent matte sericite powder close to skin color can be obtained. As a color powder filler, it can be used in cosmetics, such as pressed powder, loose powder, honey powder, etc. It is a transparent matte functional matte sericite powder close to skin color and good dispersibility, which can present a nude makeup effect when used on the skin.

Claims

1. A transparent matte sericite powder close to the skin color, the transparent matte sericite powder comprising: 1) a matte sericite substrate in particulate form, and 2) a metal oxide coating on the surface of the substrate; or 1) a matte sericite substrate in a particulate form, 2) a metal oxide coating layer on a surface of the substrate, and 3) a silicon oxide coating layer or a hydrated silicon oxide coating layer on a surface of the metal oxide coating layer; The metal oxide coating layer is one or two selected from an iron oxide coating layer, a cerium oxide coating layer and an iron oxide / cerium oxide mixed oxide coating layer; Preferably, the average particle size of the matte sericite substrate is 3-30 microns, more preferably 3.2-25 microns, more preferably 3.5-22 microns, more preferably 3.7-20 microns, more preferably 3.8-18 microns, more preferably 4-15 microns.

2. The skin-colored transparent matte sericite powder according to claim 1, wherein: Based on 100 parts by weight of the matte sericite substrate, the weight of the metal oxide coating on the surface of the substrate is 1-12 parts by weight, preferably 1.2-10 parts by weight, more preferably 1.5-8 parts by weight, more preferably 1.6-7 parts by weight, more preferably 1.8-6 parts by weight, and more preferably 2-5 parts by weight.

3. The skin-colored transparent matte sericite powder according to claim 2, wherein: Based on 100 parts by weight of the matte sericite substrate, the weight of the silicon oxide coating layer or the hydrated silicon oxide coating layer on the surface of the metal oxide coating layer is 2-10 parts by weight, preferably 2.5-9 parts by weight, more preferably 3-8 parts by weight, more preferably 3.5-7.5 parts by weight, more preferably 4-7 parts by weight, more preferably 4.5-6.5 parts by weight, for example 5-6 parts by weight.

4. The skin-colored transparent matte sericite powder according to any one of claims 1 to 3, wherein: The thickness of the metal oxide coating layer 2) is 1-20 nm, preferably 1.1-18 nm, preferably 1.2-15 nm, preferably 1.5-12 nm, preferably 1.8-10 nm, preferably 2-9 nm, preferably 2.2-8 nm, more preferably 2.5-7 nm; and / or The metal oxide coating layer is: an iron oxide coating layer; a cerium oxide coating layer; in order from the inside to the outside, an iron oxide coating layer + a cerium oxide coating layer; in order from the inside to the outside, a cerium oxide coating layer + an iron oxide coating layer; or a single iron oxide / cerium oxide mixed oxide coating layer.

5. The skin-colored transparent matte sericite powder according to any one of claims 1 to 4, wherein: The parameters of matte sericite powder close to skin color in CIE Lab system are as follows: L value is 56-62, preferably 57-61, more preferably 58-60.50; a value is 4.5-9, preferably 4.8-8.5, preferably 5-8, preferably 5.1-7.3; The b value is 10-14, preferably 10.5-13.5, preferably 11-13, preferably 11.50-12.50; ΔEab is 0.4-2.2, preferably 0.45-2.1, preferably 0.48-2.0, preferably 0.5-1.9, preferably 0.52-1.85, preferably 0.55-1.75; Where L represents black and white brightness, a represents red and green, b represents yellow and blue, and ΔE represents color difference.

6. A method for preparing a transparent matte sericite powder close to skin color, the method comprising the following steps: (1) 100 parts by weight of low-refractive index transparent matte sericite powder is mixed with deionized water to form a suspension with a solid-liquid ratio of 1:(5-15), preferably 1:(6-14), preferably 1:(7-13), preferably 1:(8-12), and the mixture is stirred uniformly. The resulting suspension is heated to a temperature of, for example, 60-90° C., preferably 65-85° C., preferably 70-80° C., and the pH value of the suspension is adjusted to 2.0-8.0, preferably 2.2-7.0, preferably 2.3-6.8, preferably 2.5-6.5 with hydrochloric acid; (2) adding 1 to 10 parts by weight, preferably 2 to 9 parts by weight, preferably 3 to 8 parts by weight of an aqueous solution of a water-soluble iron salt or a water-soluble cerium salt corresponding to iron oxide or cerium oxide to the suspension obtained in step (1), wherein the molar concentration of the aqueous solution of the iron salt or the cerium salt is 0.15 to 2.5 mol / L, preferably 0.2 to 2.0 mol / L, preferably 0.25 to 1.8 mol / L, preferably 0.3 to 1.5 mol / L, for example 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.4 mol / L; using an alkali or an acid (for example, an aqueous sodium hydroxide solution with a concentration of 5 to 30 wt% or an ammonia solution with a concentration of 10 to 30 wt%, or an acid such as a hydrochloric acid solution with a concentration of 5 to 10 wt%) to keep the pH value of the mixture constant (for example, within an acidic pH range, for example, keeping the pH value within a range of 2.2 to 7.0, preferably 2.3 to 6.8, preferably 2.5 to 6.5, for example, pH values ​​of 3, 4, 5, or 6), and after the addition is completed, stirring at a constant temperature (for 5 to 50 minutes, for example, 15 to 30 minutes) to obtain a suspension; (3) Optionally, repeating step (2), further adding 1 to 10 parts by weight, preferably 2 to 9 parts by weight, preferably 3 to 8 parts by weight of an aqueous solution of a metal salt different from the metal salt, i.e., cerium salt or iron salt, in step (2) to the suspension obtained in step (2) to obtain a suspension; (4) Optionally, 1 to 10 parts by weight, preferably 2 to 9 parts by weight, preferably 3 to 8 parts by weight of a water-soluble silicon salt aqueous solution corresponding to silicon oxide is further added to the suspension obtained in step (2) or step (3), wherein the molar concentration of the silicon salt aqueous solution is 0.15 to 2.5 mol / L, preferably 0.2 to 2.0 mol / L, preferably 0.25 to 1.8 mol / L, preferably 0.3 to 1.5 mol / L, for example 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.4 mol / L; using an alkali or an acid (for example, an aqueous sodium hydroxide solution with a concentration of 5 to 30 wt% or an ammonia solution with a concentration of 10 to 30 wt%, or an acid such as a hydrochloric acid solution with a concentration of 5 to 10 wt%) to keep the pH value of the mixture constant (for example, within an acidic pH range, for example, keeping the pH value within a range of 2.2 to 7.0, preferably 2.3 to 6.8, preferably 2.5 to 6.5, for example, pH values ​​of 3, 4, 5, or 6), and after the addition is completed, stirring at a constant temperature (for 5 to 50 minutes, for example, 15 to 30 minutes) to obtain a suspension; and (5) The suspension formed in step 2, 3 or 4 is filtered, washed and dried to obtain a transparent matte sericite powder close to the skin color.

7. The preparation method according to claim 6, wherein the molar concentration of the iron salt or cerium salt is 0.2-2 mol / L, preferably 0.2-0.8 mol / L, particularly preferably 0.2-0.5 mol / L.

8. The preparation method according to claim 6 or 7, wherein In the transparent matte sericite powder close to the skin color, the coverage of the oxide is 1 to 10 wt %, preferably 1.5 to 8 wt %, preferably 2 to 5 wt %, based on the weight of the substrate; and / or wherein the iron salt is selected from one or more of FeCl3, Fe2(SO)4 and Fe(NO3)3; and / or wherein the cerium salt is selected from one or more of CeCl3, Ce(SO4)2·4H2O and Ce(NO3)4; and / or The silicon-containing salt is selected from sodium metasilicate (Na2SiO3) or sodium metasilicate hydrate.

9. Skin-colored transparent matte sericite powder prepared by the preparation method according to any one of claims 6 to 8.

10. Use of the skin-colored transparent matte sericite powder according to any one of claims 1 to 5 or the skin-colored transparent matte sericite powder according to claim 9 in preparing cosmetics, such as for preparing cosmetic pressed powder.

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