JP2001206712A - Transparent powder - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide powder having high total transmissivity and low diffuse transmissivity even if the refraction factor of a vehicle takes any value. SOLUTION: Silicate powder is a silicate of a metal element containing silica and one or more kind of the metal oxide, in which the ratio of total moles of the metal oxide per silica of 1 is <=0.5 expressed in terms of oxide. When the powder is dispersed in the vehicle and following equation 1 and equation 2 are defined based on the spectroscopic measurement in a spectroscope with integrating sphere for measuring the transmissivity or the reflectance of light using a transmission cell or by film forming, T in equation 1 takes high value and Ts in equation 2 takes low value in the range of the refraction factor of the vehicle at the time of making the volume ratio of the powder to the vehicle constant and continuously changing the refraction factor of the vehicle. Equation 1: I=T+R+K Equation 2: T=Ts+Td In the equations, I: incident quantity of light, T: total transmissivity, R: total reflectance, K: total absorption, Ts: diffuse transmissivity, Td: straight transmissivity and Ts exhibits a value measured by canceling the straight transmissivity at the time of measuring in the spectroscope with integrating sphere.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a powder suitable as a raw material for paints and cosmetics, and to a composition containing such powders such as paints and cosmetics.

[0002]

2. Description of the Related Art Light is reflected, absorbed, and transmitted as it enters the other medium from the current medium. Generally, when the refractive index difference between the media is large, the refraction angle is large and the ratio of reflection is large, and when the difference is small, the refraction angle is small and the transmission ratio is large. In addition, when the surface of another medium is uneven and the angle of incidence of light is not constant, the reflection ratio is further increased. That is, in a dispersion of a vehicle and a solid, if the refractive indices of the vehicle and the solid are equal, the dispersion is transparent. On the other hand, human eyes perceive light reflected or transmitted from an object and perceive the shape and color of the object. Therefore, the shape and color of the light appear different depending on the progress of the light. Also,
Powders are rarely used alone in all industries, most often with vehicles.
For example, in the case of paints and inks,
In the case of cosmetics, it is kneaded with an oil or water, in the case of resin or fiber, it is kneaded with a base material, and in the case of pottery or glass, it is melted and used with a glaze. In such a case, the refractive index difference is a very important factor since the transparency of the finished product depends on the refractive index difference between the vehicle and the powder. To explain this situation in more detail, when a certain powder is dispersed in a vehicle to form a film, the light entering the vehicle hits the powder, and is partially reflected, partially transmitted, and partially absorbed. Is done. In the membrane,
The reflected or transmitted light repeats reflection, transmission and absorption again, and eventually goes out of the film. Accordingly, light transmitted through the film takes various directions, and is roughly classified into light transmitted straight through the film (straight transmission light) and light transmitted repeatedly while being reflected (diffuse transmission light). When these are represented by formulas, they are represented by formulas 1 and 2. Formula 1 I = T + R + K Formula 2 T = Ts + Td In this formula, I: incident light amount = 1 T: total transmittance R: total reflectance K: total absorption Ts: diffuse transmittance Td: straight transmission Ts indicates a value measured by canceling straight transmitted light at the time of measurement with a spectroscope equipped with an integrating sphere.

In a dispersion of a vehicle and a single compound powder alone, the refractive index of the vehicle is continuously changed so that the refractive index of the vehicle is equal to the refractive index of the powder in the middle. When the refractive index is equal, the dispersion becomes transparent when the refractive index is equal, but when the refractive index of the vehicle is higher or lower, the opacity increases in accordance with the refractive index difference. Normally, where T is transparent, the proportion of T in Equation 1 is large, and the proportion of T decreases as opacity increases.
On the other hand, Ts at this time shows the lowest value when the refractive indices are equal, increases according to the refractive index difference, and becomes T = Ts after a certain refractive index difference. This is the optical characteristic of a single compound dispersion. This feature is defined as T and Ts at specific wavelengths.
When a graph is plotted in relation to the refractive index of the vehicle, the typical pattern is as shown in FIG. This figure also shows that the maximum value of T is Tmax and the minimum value of Ts is Smin, Tmax and Sm.
The refractive index at which in appears is n, the refractive index range at which T = Ts at substantially equal intervals around n is N, and the values of Ts and T at which T = Ts are T ( N)
Parameter. In the dispersion, when the powder is merely a mixture of single compounds A and B having different refractive indices, even if the refractive indices of the vehicle and A are matched, they do not match those of B, and the dispersion is opaque. It is.
The converse is also opaque and does not provide the refractive index of a completely transparent vehicle.

[0004] A powder is mixed with a vehicle in a certain ratio to prepare a dispersion, and when the dispersion is formed into a film, if the film is transparent, the other side should be visible through the film.
If the membrane is completely opaque, the other side is not visible. At this time, if the refractive index difference between the powder and the vehicle is properly adjusted, the other side is clearly visible through the film,
Various films can be produced until they are completely invisible. The phenomenon of the film which is clearly visible is a case where the ratio of T is high in Expression 1 and the ratio of Ts is low in Expression 2. Usually, when the other side is not clearly seen, the ratio of T is low and the ratio of Ts is high. By the way, in the form of cosmetics, especially make-up cosmetics, it is common to use pigments and extender pigments with oils, waxes, vehicles such as organic polymers, etc., but most oils used in these forms, The refractive index of the wax or the organic polymer is in the range of 1.4 to 1.5. On the other hand, the refractive index of bengara or titanium oxide, which is often used as a pigment, is 2 or more, and the refractive index of clay mineral powder, such as talc or sericite, which is often used as an extender, is around 1.6. For this reason, pigments are used for correcting skin color and concealing spots and freckles, and have a higher transparency than pigments. It is often used for improving oil absorption and adjusting oil absorption and viscosity. However, although the refractive index of the extender is low, there is a considerable difference between the extender and the cosmetic vehicle.If too much extender is used in the dosage form, not only the transparency is impaired, but also the transparency is impaired. However, there is a disadvantage that the saturation of the pigment is reduced to make it a dull color. In particular, silica is frequently used as an extender when the transparency of the dosage form is desired. However, this is because silica has a refractive index of around 1.45, and is the only powder having a refractive index similar to that of a vehicle for cosmetics. That's why. That is, the ratio of T in the above equation 1 can be increased.

[0005] However, for example, when the refractive index of silica is 1.45, the refractive index of the vehicle differs depending on the vehicle composition and the size of silica.
T (N) = 0.8 at 0.005, and ± 0.0.
Within the range of 005, high transparency is exhibited, but otherwise, opacity increases according to the difference in refractive index. By the way, when commercializing cosmetics, various additives must be used because the basic qualities such as improvement of skin quality and texture, good feel, color tone, etc. must be satisfied. It is almost impossible to adjust within .445 to 1.455. Therefore, hitherto, when formulating cosmetics, attempts have been made to reduce the refractive index difference between the vehicle and the powder. That is, it is an attempt to minimize the difference in the refractive index as much as possible by using a mixture of silica and other substance powder in accordance with the vehicle to be used. However, in this case, since the refractive index of silica and the other extender is too different, when the refractive index of the vehicle is the same value as that of silica, the refractive index of the other powder does not match the refractive index of the other powder, and the other powders have different refractive indexes. When the refractive index is close to the refractive index of the body, it does not match the refractive index of silica and lowers the total transmittance. Therefore, development of powder with high transparency is desired regardless of the vehicle with any refractive index. I was That is, it has been desired to develop a powder having a high total transmittance and a low diffuse transmittance regardless of the value of the refractive index of the vehicle.

On the other hand, a silicate of a metal element containing silicon and at least one of the metal elements, wherein the ratio of the total mole number of the metal oxide to silica 1 in terms of moles of oxide is 0.5 No silicate powder is known at all, characterized by the following: Therefore, among such powders, the powder is dispersed in a vehicle and used in a transmission cell or formed into a film to form an optical filter. In the spectroscopic measurement using a spectroscope equipped with an integrating sphere, which measures the transmittance and reflectance of light, when the above formulas 1 and 2 are defined, the volume ratio between the powder and the vehicle is kept constant and the refractive index of the vehicle is continuously measured. When the refractive index of the vehicle is changed,
Is high and the Ts of the formula 2 is low, and the silicate powder has a high transparency regardless of the vehicle having any refractive index, that is, the refractive index of the vehicle is high. Regardless of the value, it has never been known that the powder has a high total transmittance and a low diffuse transmittance.

[0000]

SUMMARY OF THE INVENTION The present invention has been made under such circumstances, and powders having high transparency, that is, the refractive index of the vehicle, regardless of the vehicle having any refractive index. It is an object of the present invention to provide a powder having a high total transmittance and a low diffuse transmittance whatever the value.

[0008]

In view of such circumstances, the present inventors have developed a highly transparent powder, that is, what value the refractive index of the vehicle has, regardless of the vehicle having any refractive index. As a result of intensive research efforts to find a powder having a very high total transmittance and a low diffuse transmittance, it was found that silicon and metal elements 1
A silicate of a metal element containing at least one or more species, and in terms of moles of oxide, the ratio of the total moles of the metal oxide is 0.5 or less with respect to silica 1; When the following formulas 1 and 2 are defined in a spectrometer with an integrating sphere, in which a powder is dispersed in a vehicle and a transmittance cell or a film is measured using a transmission cell or formed into a film, and the light transmittance and the reflectance are measured. ,
When the volume ratio between the powder and the vehicle is kept constant and the refractive index of the vehicle is continuously changed, it is considered that T in Formula 1 is high and Ts in Formula 2 is low in the range of the refractive index of the vehicle. The inventors have found that the characteristic silicate powder is such a powder, and have completed the invention. That is, the present invention relates to the following technology. (1) A silicate of a metal element containing silicon and at least one metal element, wherein the ratio of the total mole number of the metal oxide to the silica 1 is 0.5 or less in terms of moles of oxide. In a certain silicate powder, the powder is dispersed in a vehicle, and the transmittance or the reflectance of light is measured using a transmission cell or formed into a film.
When Equation 2 is defined, when the refractive index of the vehicle is continuously changed while the volume ratio of the powder and the vehicle is kept constant, the T of Equation 1 is high in the range of the refractive index of the vehicle and the equation 2. A silicate powder characterized in that Ts of (2) is reduced. Formula 1 I = T + R + K Formula 2 T = Ts + Td In this formula, I: incident light amount = 1 T: total transmittance R: total reflectance K: total absorption Ts: diffuse transmittance Td: straight transmission Ts indicates a value measured by canceling straight transmitted light at the time of measurement with a spectroscope equipped with an integrating sphere. (2) The metal element is aluminum, zinc, magnesium,
Of calcium, barium, iron, cobalt and manganese
(1) a silicate powder having a spherical shape or a shape close to a spherical shape and an average diameter of 0.5 or more; The silicate powder according to (1) or (2), wherein the silicate powder has a thickness of from about 100 μm to about 100 μm. (4) The silicate powder according to any one of (1) to (3), wherein the vehicle is a solid or a liquid. (5) A silicate of a metal element containing silicon and one or more metal elements, and the metal element does not form an oxide, and is a total of metal oxides in terms of moles of oxide. An amorphous silicate powder, wherein the molar ratio is 0.5 or less with respect to 1 silica. (6) In a spectrometer using an integrating sphere, in which a powder is dispersed in a vehicle and a transmittance cell or a reflectance is measured using a transmission cell or formed into a film, the following formulas 1 and 2 are used. When defined, when the refractive index of the vehicle is continuously changed while the volume ratio of the powder and the vehicle is kept constant, T in Equation 1 is high and Ts in Equation 2 is high in the range of the refractive index of the vehicle. The silicate powder according to (5), wherein the silicate powder has a low content. Formula 1 I = T + R + K Formula 2 T = Ts + Td In this formula, I: incident light amount = 1 T: total transmittance R: total reflectance K: total absorption Ts: diffuse transmittance Td: straight transmission Ts indicates a value measured by canceling straight transmitted light at the time of measurement with a spectroscope equipped with an integrating sphere. (7) A water / glass emulsion and an oil agent are emulsified to form a W / O emulsion, an acid solution containing a metal element is added thereto, and firing is performed at a firing temperature of the crystallization temperature or lower. The silicate powder according to any one of (1) to (6). (8) A composition comprising the silicate powder according to any one of (1) to (7). (9) The composition according to (8), which is a cosmetic. Hereinafter, the present invention will be described in detail focusing on embodiments.

[0009]

DETAILED DESCRIPTION OF THE INVENTION The silicate powder of the present invention is a silicate of a metal element containing silicon and one or more metal elements,
In a silicate powder in which the ratio of the total mole number of the metal oxide is 0.5 or less with respect to silica 1 in terms of moles of oxide,
When the following formulas 1 and 2 are defined in a spectrometer with an integrating sphere, in which a powder is dispersed in a vehicle and a transmittance cell or a film is measured using a transmission cell or formed into a film, and the light transmittance and the reflectance are measured. When the refractive index of the vehicle is continuously changed while keeping the volume ratio between the powder and the vehicle constant, T in the formula 1 is high and Ts in the formula 2 is low in the range of the refractive index of the vehicle. Characterized by the following: Formula 1 I = T + R + K Formula 2 T = Ts + Td In this formula, I: incident light amount = 1 T: total transmittance R: total reflectance K: total absorption Ts: diffuse transmittance Td: straight transmission Ts indicates a value measured by canceling straight transmitted light at the time of measurement with a spectroscope equipped with an integrating sphere.

Here, the silicate is characterized by containing silicon and one or more metal elements. Since the refractive index of the metal element is higher than that of silica, the metal element is used to adjust the refractive index of silica to a higher value. Among them, aluminum, zinc, magnesium, calcium, barium, iron, cobalt, and manganese are selected as silicate-producing elements.
More than one species can be used in combination. The content of these metal elements in the silicate is preferably 0.5 mol or less per mol of silica in terms of moles of oxide,
In this case, the number of moles of oxide of the metal element is a value obtained by adding the number of moles of oxide of the metal element used. The value of the mole equivalent of the metal element in terms of oxide is a value within a range in which the metal element does not take the form of an oxide. It is not preferable because the refractive index rapidly approaches that of the oxide. The refractive index of the silicate can be adjusted such that the molar number in terms of oxide of the metal element used is 0.5 or less with respect to the silica 1 in terms of the molar amount of the metal element, and if it is large, it can be adjusted high. That is, the refractive index of the powder can be adjusted according to the range of the refractive index of the vehicle to be used, for example, lower for cosmetics, higher for paints and the like. Can be adjusted accordingly. When such a silicate is observed in a diffraction pattern with a powder X-ray diffractometer (XRD), there is no peak attributed to a metal oxide, and an amorphous or halo pattern derived from a silicate of a metal element exists. From these properties, it is clear that the metal atoms present in the silicate powder of the present invention do not take the form of an oxide, and the silicate is amorphous.

Looking at the optical behavior of a dispersion in which such a silicate powder is dispersed in a vehicle having a different refractive index, it is clearly different from a dispersion of a single compound or a dispersion of two single compounds. Behavior. For example, an example of the silicate powder of the present invention is a silicate of aluminum having an average diameter of 10 μm.
m, a silicate powder having a molar ratio of 0.4 of alumina oxide was taken, and this and the other powder were dispersed in vehicles having different refractive indexes so that the volume% of the powder became equal. The optical behavior of the dispersion at the time is as follows. First, a dispersion of single silica spheres having an average diameter of 10 μm has n = 1.45, Tmax = 1, Ts = 0.05, and N =
0.01, T (N) = 0.8, where the refractive index of the vehicle is 1.45 ± 0.01, T = 0.6, Ts =
0.6, and T = 0.6 or less at other refractive indices. Next, a mixture of 1% by weight of alumina powder having an average particle diameter of 0.05 μm mixed with a single silica sphere having an average diameter of 10 μm is used as a dispersion of T anywhere in the range of 1.4 to 1.5 of the vehicle refractive index. = 0.3 and Ts = 0.3. The silicate powder of the present invention exemplified for these has n = 1.4.
7, Tmax = 1, Smin = 0.01, N = 0.04, T
(N) = 0.8. As is apparent from this comparison, the silicate powder of the present invention has a high total transmittance and a low diffuse transmittance even if the refractive index of the vehicle changes greatly to N = 0.04. And can be kept. That is, a powder having high transparency regardless of the vehicle having any refractive index, that is, a powder having a high total transmittance and a low diffuse transmittance regardless of the value of the refractive index of the vehicle. This is because the metal element contained in the silicate powder of the present invention is so small that it cannot form oxide crystals or stoichiometric silicate crystals in a molar ratio with silicon, and becomes non-stoichiometric silicate. It is. That is, the silicate of the present invention is a single compound composed of silica and a metal element as a compound, but is an amorphous substance in which the metal element is dispersed in the silica skeleton and does not take a definite crystal form. When such a substance is viewed optically, it is a substance that exhibits a refractive index of a single compound but has a microscopically distributed refractive index. Therefore, even if the refractive index of the vehicle is different, it has high light transmittance. The total transmittance and the diffuse transmittance of the dispersion obtained by dispersing the powder in the vehicle take different values depending on the refractive index of the vehicle and the refractive index of the powder. The content of the metal element for achieving the rate and the diffuse transmittance is various, and is not limited to one. Further, the silicate powder of the present invention contains water or / and OH in its skeleton.
In some cases, a group or an alkali metal such as Na, K, or Li may be incorporated, but these elements are acceptable as long as they do not promote crystallization of the silicate.

The silicate powder of the present invention can have a spherical or spherical shape. Here, the sphere or the shape approximate to a sphere means that the average diameter is 0.5 to 100 μm.
In this case, the distortion from a true sphere or a sphere has a length, and has no corner having a radius of 20% or less. The range of the average diameter is generally at least half of the wavelength of light, and is preferably 100 μm or less for visually perceiving a graininess, that is, 0.5 to 100 μm, and more preferably 0.5 to 50 μm where almost no graininess is felt. It is. Further, the silicate powder is not crystalline but takes the form of silicate having an amorphous or broad halo pattern when viewed from a powder X-ray diffraction pattern. Of these, it is preferable to take an amorphous form.

The production of the silicate powder according to the present invention is performed by various methods. A method of reacting water glass with an acid containing a metal element to form a silicate containing a metal element, a method of hydrolyzing silicon and an alkoxide of a metal element to form a silicate containing a metal element, and the like. is there. In addition, as a method for producing a silicate sphere according to the present invention, a method of emulsifying a water glass and an oil agent to form a W / O emulsion, adding an acid solution containing a metal element thereto, silicon and metal There is a method of spraying an alkoxide of an element at a crystallization temperature or lower. In these methods, if manganese or iron is used as a metal element, coloring can be performed. Further, as described above, the silicate powder of the present invention is a powder having high transparency regardless of the vehicle having any refractive index. Therefore, the silicate powder may be used as a coating agent for a pigment or other extender. Can be done. That is, it is possible to smooth, stabilize, or deactivate the surface properties of the pigment or other extender without changing the optical properties of the pigment or the like. As a coating method, for example, a method of reacting water glass with an acid containing a metal element in the presence of a pigment or other extender to form a silicate of the metal element on the surface of the pigment or other extender or the like Etc. The temperature at which the material obtained by these methods is fired is 300 ° C. depending on the type of the metal element.
It may be performed at about 1000 ° C. The silicate powder of the present invention containing silicon and one or two or more metal elements thus obtained can be used as it is as a raw material for cosmetics or the like. Can also be used. Such surface treatments include phosphate coating such as sodium polyphosphate, baking of silicone such as dimethicone and hydrogen methylpolysiloxane, alkyl fluoride group introduction treatment, silane coupling agent treatment, and acylated amino acid salt. And the like, a coating treatment with a phospholipid such as lecithin, a polymer coating treatment and the like. These processes may be performed according to a conventional method.

The cosmetic of the present invention is characterized by containing the above-mentioned silicate powder of the present invention. As the cosmetic of the present invention, any cosmetic can be applied without particular limitation, for example, creams and emulsions, basic cosmetics such as sun care products, under makeup and foundation, cheek color, lip color, eye Examples include make-up cosmetics such as color, hair cosmetics such as hair color and hair cream, and cleansing cosmetics such as shampoo, rinse and soap, and among these, the touch is refreshed without impairing transparency. When it is desired to change the direction, it is preferably applied to a case where the amount of oil absorption is adjusted without impairing the finish feeling of the powder product and the finish feeling of the powder product,
It is preferably applied to basic cosmetics such as creams and emulsions, and make-up cosmetics such as lip colors and foundations. Further, since the silicate powder of the present invention can be colored, it is also preferable that the silicate powder is an under makeup cosmetic such as a makeup base. Because of the characteristics of the silicate powder of the present invention, which is a powder having a spherical shape or a shape close to a spherical shape, it is also suitable as a makeup agent for making up a card or paper. The preferred content of the silicate powder of the present invention in the cosmetic of the present invention is 1 to 100% by weight.
And more preferably 5 to 60% by weight. In the cosmetic of the present invention, in addition to the silicate powder of the present invention,
Optional components commonly used in cosmetics can be contained within a range that does not impair the effects of the present invention. Such optional components include, for example, hydrocarbons such as petrolatum and microcrystalline wax, esters such as jojoba oil and gay wax, triglycerides such as tallow, olive oil, higher alcohols such as cetanol and oleyl alcohol, and stearic acid. Fatty acids such as oleic acid, polyhydric alcohols such as glycerin and 1,3-butanediol, nonionic surfactants, anionic surfactants, cationic surfactants, amphoteric surfactants, ethanol, carbopol, etc. Preferred examples include a tackifier, a preservative, an ultraviolet absorber, an antioxidant, a pigment, and powders. The cosmetic of the present invention can be produced by treating these raw materials according to a conventional method. The cosmetics thus obtained can provide the same quality of transparency, regardless of the optional ingredients in any formulation.
The optical design is easy, and makeup collapse caused by a change in pigment wetting in an optical sense is extremely small.

[0015]

EXAMPLES The present invention will be described in more detail with reference to the following examples, but it goes without saying that the present invention is not limited to these examples.

Example 1 An aqueous phase A was prepared by dissolving 21 g of sodium orthosilicate in 400 ml of water in advance. Separately, 1.3 g of zinc chloride and 100 ml of 3N hydrochloric acid are dissolved and the aqueous phase B is dissolved.
And The aqueous phase B was added dropwise to the aqueous phase A under stirring at room temperature to form a precipitate, which was then aged at that temperature for 3 hours and further at 60 ° C. for 1 hour. The deposited precipitate was filtered, dried and calcined at 650 ° C. to obtain 7 g of the silicate powder 1 of the present invention. This powder was white and had an average particle size of 1 μm. The oxide-converted molar ratio was 0.1 (X-ray fluorescence analysis) in terms of ZnO, and the powder X-ray diffraction pattern was amorphous.

Example 2 5 g of a surfactant was added to 500 g of liquid paraffin to form an oil phase. Separately, 21 g of sodium metasilicate is dissolved in 120 ml of water to obtain an aqueous phase A.
Separately, 3.6 g of barium nitrate monohydrate and 1.6 g of ferric nitrate hexahydrate are dissolved in 100 ml of 2N hydrochloric acid to obtain an aqueous phase B. The water phase A is added to the oil phase to form a W / O emulsion, the temperature is maintained at 20 ° C., and the water phase B is added dropwise thereto.
After dropping, the mixture was aged at that temperature for 4 hours and further at 60 ° C. for 1 hour. The deposited precipitate was filtered, dried and calcined at 750 ° C. to obtain 7 g of the silicate powder 2 of the present invention. This powder had a fine flesh-colored sphere and an average particle diameter of 10 μm. The molar ratio in terms of oxide was 0.23 in terms of BaO + Fe2O3 (X-ray fluorescence analysis),
The powder X-ray diffraction pattern was a broad halo pattern. The molar ratio of BaO to Fe2O3 is
1: 0.15.

Example 3 11.8 g of tetraethoxysilane and 16 g of aluminum triisopropoxide were added to 400 ml of ethanol, and the mixture was refluxed overnight to obtain an alcohol phase. Separately, prepare 20 g of water. Water was added dropwise to the alcohol phase at room temperature with stirring. After dropping, the mixture was aged at that temperature for 2 hours. The deposited precipitate was filtered, dried, and then calcined at 850 ° C. to give the silicate powder 3 of the present invention at 8.5.
g obtained. This powder was white and had an average particle size of 0.2 μm.
The molar ratio in terms of oxide was 0.4 in terms of Al2O3 (X-ray fluorescence analysis), and the powder X-ray diffraction pattern was a broad halo pattern.

Example 4 11.8 g of tetraethoxysilane, 2.1 g of magnesium diisopropoxide and 1.95 g of calcium diethoxide were added to 200 ml of ethanol.
And refluxed overnight to make the alcohol phase. This alcohol phase was sprayed into a furnace at 800 ° C. to obtain 7.1 g of a silicate powder 4 of the present invention. This powder had a white spherical shape and an average particle size of 2 μm. The oxide equivalent molar ratio is MgO + Ca
0.3 in terms of O (X-ray fluorescence analysis), and the powder X-ray diffraction pattern was amorphous. Note that the molar ratio of MgO to CaO was 1: 1.

Example 5 The transmittance patterns of the silicate powders 1 to 4 of Examples 1 to 4 were examined. That is, 1-bromonaphthalene (refractive index = 1.66), squalene (refractive index = 1.496), glycerin tri-2-ethylhexanoate (refractive index = 1.44) and dimethyl silicone (refractive index = 1.4) Refractive index of 1.4 to 1.
In the range of 66, vehicles having different refractive indexes in 30 steps were prepared, and each vehicle and powder were mixed in a volume ratio of 4: 0.04.
, And after ultrasonic dispersion, the mixture was placed in a 10 mm × 10 mm cell, and the transmittance was measured with a spectrophotometer. Measurement wavelengths of 400, 560 and 800 nm were used. As the sample, in addition to the silicate powders 1 to 4 of the present invention, spherical silica powder having a purity of 98% and an average particle diameter of 10 μm (Comparative Powder 1) was used.
Table 1 shows the values of Tmax, Smin, n, and N for each sample for each wavelength. In addition, T (N) was about 0.8 in all samples. Thus, in the silicate powder of the present invention, as compared with the comparative powder 1, n is different, Tmax is almost the same, and N indicating a range where T is high and Ts is low is large. I understand. That is, it can be seen that the silicate powder of the present invention has higher transparency than the comparative powder 1 in a wide range of the refractive index of the vehicle.

[0021]

[Table 1]

Embodiment 6 Silicate Powder 1 of Embodiments 1-4
~ 4 were made into a film, and the visibility (resolution) of the shape under the film was examined. That is, heavy liquid isoparaffin (refractive index = 1.
5) Using methyl methacrylate (refractive index 1.48) and sucrose fatty acid ester (refractive index 1.46) as filming agents (vehicles) having different refractive indices, 30% by volume ethylene glycol monoethyl ether solutions were prepared. This solution and the powder were mixed at a volume ratio of 2: 0.1, ultrasonically dispersed, and this dispersion was formed on a slide glass using a 0.5 mil doctor blade. This film was vacuum-dried at room temperature or lower to evaporate ethylene glycol monoethyl ether to obtain a film for measurement. The resolution measurement is performed by preparing a test pattern in which lines are drawn on white paper with an equal difference of 0.1 mm from 0.1 to 1 mm and placing a film on this test pattern to determine the limit at which the intervals can be identified. went. The color of the test pattern line was black. The same sample as in Example 5 was used. The results of this measurement are shown in Table 2 as the resolution. The values in the table are the limit values at which the intervals between lines can be identified. The smaller the value, the higher the transparency. As is clear from the results, it can be seen that the resolution of the silicate powder of the present invention is much higher than that of the comparative powder 1. That is, it can be seen that the transparency is extremely high even in the films having different refractive indexes of the vehicles.

[0023]

[Table 2]

<Example 7> The above silicate powder 1, silicate powder 4 and comparative powder 1 were used as transparent powders instead of talc or sericite according to the following formulation.
Each created a foundation. That is, i, b, c,
Heat each component of D to 70 ° C, mix A and B, knead well, dilute by adding C, add E, disperse by disperser, gradually add D and emulsify Then, the mixture was stirred and cooled to obtain Foundation 1 (silicate powder 1), Foundation 2 (silicate powder 4), and Foundation 3 (Comparative powder 1). The emulsion prepared by removing the transparent powder, iron-doped titanium dioxide, red iron oxide and yellow iron oxide from this formulation was vacuum-dried at room temperature or lower, and the refractive index of the remaining component was 1.4831. A 70% maltose aqueous solution 5 parts by weight Glycerin 1 part by weight 1,3-butanediol 5 parts by weight Methylparaben 0.2 parts by weight b Triglycerin diisostearate 4 parts by weight Sorbitan sesquiolate 0.5 parts by weight C Liquid paraffin 10 parts by weight Parts Heavy liquid isoparaffin 7 parts by weight Isooctyl paradimethylaminobenzoate 3 parts by weight D Water 42.7 parts by weight Transparent powder 18 parts by weight Iron-doped titanium dioxide 1.3 parts by weight Bengala 0.8 parts by weight Yellow iron oxide 1.5 parts by weight

Example 8 The above silicate powder 1, silicate powder 4 and comparative powder 1 were used as transparent powders instead of talc and sericite, and foundations were respectively prepared according to the following formulation. Created. That is, each component of i, b, c, and d is heated to 70 ° C., and a and b are mixed,
Knead well, dilute this by adding c, add e, disperse with a disperser, gradually add and emulsify this, emulsify, stir and cool, foundation 4 (silicate powder 1), foundation 5 ( A silicate powder 4) and a foundation 6 (comparative powder 1) were obtained. The emulsion prepared by removing the transparent powder, iron-doped titanium dioxide, red iron oxide and yellow iron oxide from this formulation was vacuum-dried at room temperature or lower, and the refractive index of the remaining component was 1.423. A 70% maltose aqueous solution 5 parts by weight Glycerin 1 part by weight 1,3-butanediol 5 parts by weight Methylparaben 0.2 parts by weight b Triglycerin diisostearate 4 parts by weight Sorbitan sesquiolate 0.5 parts by weight Haskulan 4 parts by weight Glycerin tri-2-ethylhexanoate 8 parts by weight Polydimethylsilicone 20CS 5 parts by weight Isooctyl paradimethylaminobenzoate 3 parts by weight D Water 42.7 parts by weight E Transparent powder 18 parts by weight Iron-doped titanium dioxide 1.3 parts by weight Bengala 0.8 parts by weight Yellow iron oxide 1.5 parts by weight

<Example 9> Using foundations 1 to 6 of examples 7 and 8, the transparency of the foundation was examined. That is, one woman of the beauty staff was sequentially applied to makeup using foundations 1 to 6, and the cosmetic finish was sensory-evaluated for transparency by seven cosmetic technicians. The evaluation was performed on a 10-point scale, with 10: very transparent to 1: no transparency. The results are shown in Table 3 as average scores. Compared to the foundations 3 and 6 using the comparative powder 1, the foundation using the silicate powder of the present invention is superior in transparency in both the formulations having different vehicle compositions of the examples 7 and 8 I understand.

[0027]

[Table 3]

Example 10 According to the following formulation,
A night cream using the silicate powder 2 was prepared.
That is, each component of b, b, c, d is heated to 70 ° C, b and k are mixed, kneaded well, diluted with c, added with e, and dispersed with a disper. The mixture was gradually added and emulsified, stirred and cooled to obtain a cream. This cream was a night cream which had a refreshing feel without impairing the transparency as compared with a normal night cream, and had an effect of giving the skin a pale red color. A 70% maltose aqueous solution 5 parts by weight Glycerin 3 parts by weight 1,3-butanediol 5 parts by weight Methyl paraben 0.2 parts by weight b Triglycerin diisostearate 4 parts by weight Sorbitan sesquiolate 0.5 parts by weight C Light isoparaffin 10 parts by weight Part isooctyl paradimethylaminobenzoate 5 parts by weight D water 51.6 parts by weight Heparin-like substance 0.1 part by weight Bakugacon essence 0.1 part by weight Elhibin 0.1 part by weight Kouki extract BG 0.1 part by weight Placenta Extract 0.1 parts by weight Glycogen 0.1 parts by weight Silicate powder 25 parts by weight

Example 12 97 parts by weight of the above silicate powder 3 was coated with 3 parts by weight of hydrogen methylpolysiloxane, baked at 180 ° C. for 72 hours, and treated with silicone-treated silicate powder. Body 5 was obtained.

Example 13 According to the following formulation,
Pressed powder for makeup repair was created. That is, the component (a) was mixed with a Henschel mixer, crushed with a pulverizer equipped with a 0.9 mm round hole screen, and the component (b) was dropped and coated while mixing with a Henschel mixer. This was pulverized with a pulverizer equipped with a 1 mm herringbone screen, packed in a metal plate, and pressed to obtain a pressed powder. This product was excellent in the effect of maintaining the finish of the foundation for a long time. B Silicate powder 5 46.5 parts by weight Silicone-treated iron-doped titanium dioxide 3 parts by weight Silicone-treated mica 5 parts by weight Methysiloxane network polymer 5 parts by weight Nylon powder 10 parts by weight Silicone-treated yellow iron oxide 2 parts by weight Silicone-treated redwood 0.5 parts by weight Silicone treated sericite 3 parts by weight Silicone treated talc 5 parts by weight Lo octyldodecyl oleate 10 parts by weight High polymerization degree silicone 5 parts by weight Dimethicone 5 parts by weight

Example 14 1.2 g of tetraethoxysilane and 1.6 g of aluminum triisopropoxide were added to 400 ml of ethanol, and the mixture was refluxed overnight to obtain an alcohol phase. Separately, prepare 5 g of water. After adding yellow No. 4 aluminum lake powder to the alcohol phase and dispersing well, water was added dropwise at room temperature with stirring. After dropping, the mixture was aged at that temperature for 2 hours. The deposited precipitate was filtered and dried to obtain 9 g of a processed powder 1 obtained by coating a yellow No. 4 aluminum lake powder with the silicate powder of the present invention. The color tone of this powder was unchanged from that before the treatment, the coating amount of the coated silicate powder of the present invention was 10% by weight, and the molar ratio in terms of oxide was 0.4 in terms of Al2O3 (from X-ray fluorescence analysis). Calculation). The powder X-ray diffraction difference pattern was amorphous.

Example 15 The treated powder 1 of Example 14 and the untreated yellow No. 4 aluminum lake powder were each dispersed in 100 ml of water, stirred at 50 ° C. for 1 hour, and allowed to stand still. After the body sank, I checked whether the supernatant colored. As a result, the supernatant of the dispersion of Yellow No. 4 aluminum lake powder was colored yellow, but the supernatant of the treated powder 1 was not colored. As you can see from this result,
The organic pigment coated with the silicate powder of the present invention significantly improved the water resistance without changing the color tone.

[0033]

According to the present invention, a powder having high transparency regardless of the vehicle having any refractive index, that is, having a high total transmittance and diffusing regardless of the value of the refractive index of the vehicle, A powder having a low transmittance can be provided.

[Brief description of the drawings]

FIG. 1 is a diagram showing the relationship between the refractive index of a vehicle and the transmittance of a powder.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) C03B 8/02 C03B 8/02 B F term (Reference) 4C083 AA012 AA072 AA112 AB232 AB242 AB371 AB372 AB381 AB382 AB432 AC022 AC122 AC132 AC342 AC392 AC442 AC482 AC552 AD072 AD152 AD242 AD312 CC05 CC12 DD21 DD22 DD32 EE07 FF01 4G014 AH02 4G073 BA10 BA11 BA13 BA32 BA36 BA40 BA52 BA57 BD22 CB07 CB08 CB09 FB19 FC05 FC25 FC27 FD18 FD21 FD23 GA35 UB31

Claims (9)

[Claims] 1. A silicate of a metal element containing silicon and at least one metal element, wherein the ratio of the total mole number of the metal oxide to silica 1 is 0.5 to the mole number of the oxide. In the silicate powder, which is characterized in that the powder is dispersed in a vehicle, and a transmission cell is used or formed into a film to measure light transmittance and reflectance, and a spectroscope with an integrating sphere is used. When the following formulas 1 and 2 are defined in the spectroscopic measurement, when the volume ratio between the powder and the vehicle is constant and the refractive index of the vehicle is continuously changed, the variation in the refractive index of the vehicle is A silicate powder, wherein T in Formula 1 is high and Ts in Formula 2 is low. Formula 1 I = T + R + K Formula 2 T = Ts + Td In this formula, I: incident light amount = 1 T: total transmittance R: total reflectance K: total absorption Ts: diffuse transmittance Td: straight transmission Ts indicates a value measured by canceling straight transmitted light at the time of measurement with a spectroscope equipped with an integrating sphere. 2. The silicate powder according to claim 1, wherein the metal element is one or more of aluminum, zinc, magnesium, calcium, barium, iron, cobalt and manganese. 3. The silicate powder according to claim 1, wherein the powder has a spherical shape or a shape close to a spherical shape, and has an average diameter of 0.5 to 100 μm. 4. The silicate powder according to claim 1, wherein the vehicle is a solid or a liquid. 5. A silicate of a metal element containing silicon and at least one metal element, wherein the metal element does not form an oxide, and the metal oxide is a metal oxide in terms of moles of oxide. Characterized in that the ratio of the total number of moles is 0.5 or less with respect to 1 of silica. 6. A spectrometer with an integrating sphere, in which a powder is dispersed in a vehicle and a transmittance cell or a reflectance is measured using a transmission cell or formed into a film, and the following formula 1 is used.
When Equation 2 is defined, when the refractive index of the vehicle is continuously changed while the volume ratio of the powder and the vehicle is kept constant, the T of Equation 1 is high in the range of the refractive index of the vehicle and the equation 6. The silicate powder according to claim 5, wherein Ts of No. 2 is low. Formula 1 I = T + R + K Formula 2 T = Ts + Td In this formula, I: incident light amount = 1 T: total transmittance R: total reflectance K: total absorption Ts: diffuse transmittance Td: straight transmission Ts indicates a value measured by canceling straight transmitted light at the time of measurement with a spectroscope equipped with an integrating sphere. 7. A method for producing a silicate in which a water glass solution is reacted with an acid solution containing a metal element and then calcined, 1) the reaction between the water glass and the acid solution containing a metal element is carried out at room temperature or lower. And / or 2) a silicate powder according to any one of claims 1 to 6, wherein the silicate powder is produced by a production method that satisfies the condition that the calcination temperature is lower than the crystallization temperature. . A composition comprising the silicate powder according to any one of claims 1 to 7. 9. The composition according to claim 8, which is a cosmetic.