JPH11240714A - Synthetic mica, its production and cosmetic by using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To produce a synthetic mica having high whiteness not in a dried state but also in a wet state, and providing good touch and slipperiness to skin, and further to provide a method therefor and cosmetics obtained by using the mica. SOLUTION: This synthetic mica usable as a raw material for cosmetics has >=90 whiteness in a dried state and >=75 whiteness in a wet state, and is produced by (I) a method for press-compacting a mixture of talc, potassium silicofluoride, alumina and iron oxide, heat-treating the compacted mixture in a sealed state at 900-1,400 deg.C, and annealing the heat-treated compact at a temperature <=100 deg.C lower than the heat-treating temperature, or (II) a method for press-compacting a mixture of the talc and the potassium silicofluoride, heat-treating the compacted mixture at 600-1,000 deg.C in the sealed state, allowing the heat-treated compact to be swelled with water, and carrying out an ion exchange of the swelled compact in a solution acidified by sulfuric acid and containing aluminum sulfate and iron sulfate.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a synthetic mica suitable for use as a raw material for cosmetics, which has a soft touch, a high smoothness, and a high whiteness in both dry and wet states. The present invention relates to a production method and a cosmetic using the same.

[0002]

2. Description of the Related Art Powders of natural minerals such as talc, mica and sericite are used as extenders of conventional cosmetics. The mixing amount of these powders is appropriately adjusted in consideration of the spreading (extensibility), sticking (adhesiveness), covering power (hiding ability), moldability, and the like of the cosmetic. However, since talc is hard, there is a problem in that when it is added to cosmetics, the feel becomes poor. In addition, mica has a problem that the quality varies greatly, and when wet with water or oil, the whiteness decreases and the color becomes dull.

On the other hand, it has a soft touch and high slipperiness
Good quality with excellent whiteness
Serisite has a locality limited to Japan,
However, there are concerns about the future in terms of supply due to low reserves. So
To solve the above problem, various synthetic mica
Is being developed. Japanese Patent Publication No. 6-27002 discloses N
a_TwoSiF₆, Li_TwoSiF₆Or K _TwoSiF₆Indicated by
10 to 35% by weight of alkali fluorosilicate and talc
Obtained by heating a mixed fine powder with the formula:

[0004]

Embedded image

(Wherein M represents a sodium, lithium or potassium atom. Α, β, γ, a and b each represent a coefficient, α is 0.1 to 2, β is 2 to 3.5, γ Is 3 ~
4, a and b represent 0 to 1. However, a + b = 1. ), Or an alkali silicofluoride represented by the formula: M ₂ SiF ₆ (where M represents a sodium, lithium or potassium atom), or the alkali silicofluoride; A mixture obtained by heating a mixture of an alkali fluoride represented by NaF, LiF or KF (10 to 35% by weight), Al ₂ O ₃ (25% by weight or less), and talc, formula:

[0006]

Embedded image

(Where M, α, β, γ, a and b are
Same as above. δ represents a coefficient of 0 to 1. )
Synthetic mica is disclosed. Further, Japanese Patent No. 256
No. 7596 includes potassium phlogopite [KMg_Three(AlSi
_ThreeO_Ten)] Is converted to water of an acid such as citric acid.
A unique particle shape obtained by contact with a solution
Adult mica is disclosed.

[0008]

However, any of the synthetic mica disclosed in the above publication has a problem that a sufficient whiteness cannot be obtained when it is actually blended into a cosmetic.
Therefore, an object of the present invention is to solve the above problems, the softness of the skin, high slipperiness, and a synthetic mica that shows excellent whiteness when blended in cosmetics, a method for producing the same, and The purpose is to provide the cosmetics used.

[0009]

Means for Solving the Problems As the inventors of the present invention have been conducting studies to solve the above problems, the conventional synthetic mica has excellent whiteness in a dry state, but has a high wetness in a wet state. Was found to have low whiteness. Therefore, by including a small amount of iron atoms in natural sericite and mica in synthetic mica, it has excellent whiteness not only in the dry state but also in the wet state, and has properties closer to natural sericite. With the idea that synthetic mica having the same could be obtained, further studies were conducted. As a result, despite the fact that synthetic mica was considered to exhibit brown color and reduced whiteness when iron atoms were mixed therein, by synthesizing mica through a predetermined manufacturing method, the dry state and the wet state were obtained. In each case, the present inventors have found a new fact that synthetic mica having excellent whiteness, soft touch, and high slipperiness can be obtained, and the present invention has been completed.

The synthetic mica of the present invention has a whiteness of at least 90 in a dry state and a whiteness of 75 in a wet state.
It is characterized by the above. The synthetic mica of the present invention comprises (I) talc having an average particle size of 1 to 100 μm and an average particle size of 1
１００100 μm potassium fluorosilicate 60: 40-9
0.1 to 3 parts of alumina having an average particle size of 0.01 to 50 μm with respect to 100 parts by weight of the mixture contained at a weight ratio of 0:10.
0 parts by weight and iron oxide having an average particle size of 0.01 to 50 μm.
After mixing with 001 to 30 parts by weight, 20 to 1000 k
press molding at a pressure of g / cm ² , followed by heat treatment in a sealed state at a temperature of 900 to 1400 ° C., and annealing at a temperature lower by 100 ° C. or more than the temperature of the heat treatment, or (II) After press-molding a mixture containing talc having an average particle diameter of 1 to 100 μm and potassium silicofluoride having an average particle diameter of 1 to 100 μm in a weight ratio of 60:40 to 90:10 at a pressure of ²⁰ to 1000 kg / cm ² , Heat treatment at a temperature of 600 to 1000 ° C. in a sealed state, then disperse and swell in water, further add 0.001 to 40% by weight of aluminum sulfate and 0.04% by weight of iron sulfate.
The ion exchange reaction was carried out in a sulfuric acid solution containing 0.01 to 30% by weight.

The synthetic mica of the present invention preferably has a fluorine elution amount of 50 ppm or less from the viewpoint of enhancing the safety when used in cosmetics.
The first method for producing synthetic mica of the present invention is a method for producing synthetic mica having a whiteness of 90 or more in a dry state and a whiteness of 75 or more in a wet state. To 100 parts by weight of a mixture containing talc having an average particle size of 100 to 100 μm and potassium silicofluoride having an average particle size of 1 to 100 μm in a weight ratio of 60:40 to 90:10.
After mixing 0.1 to 30 parts by weight of alumina having a particle size of 0.01 to 50 μm and 0.001 to 30 parts by weight of iron oxide having an average particle size of 0.01 to 50 μm, the mixture is press-formed at a pressure of ^{20 to} 1000 kg / cm ^2. And then 900-140 under sealed condition
The heat treatment is performed at a temperature of 0 ° C., and the annealing is performed at a temperature lower by at least 100 ° C. than the temperature of the heat treatment.

The second method for producing synthetic mica of the present invention comprises:
A method for producing synthetic mica having a whiteness of 90 or more in a dry state and a whiteness of 75 or more in a wet state, comprising talc having an average particle size of 1 to 100 μm and an average particle size of 1 to 1
00 μm potassium fluorosilicate 60: 40-90:
A mixture containing a weight ratio of 10 to 20 to 1000 kg /
After press molding at a pressure of ² cm ² , 60
Heat treatment at a temperature of 0 to 1000 ° C., then swelling by dispersing in water, further adding aluminum sulfate 0.001 to
The ion exchange reaction is performed in a sulfuric acid solution containing 40% by weight of iron sulfate and 0.001 to 30% by weight of iron sulfate.

The synthetic mica obtained by the first and second production methods not only exhibits excellent whiteness in both a dry state and a wet state, but also has a soft touch and a high smoothness. In the method for producing synthetic mica of the present invention, it is preferable to further treat the obtained synthetic mica with a weakly acidic solution from the viewpoint of reducing the elution amount of fluorine from the synthetic mica.

The cosmetic of the present invention is characterized by containing the synthetic mica of the present invention.

[0015]

DESCRIPTION OF THE PREFERRED EMBODIMENTS First, the synthetic mica of the present invention will be described. The whiteness of the synthetic mica of the present invention is 90 or more in a dry state, preferably 92 or more, more preferably 94 or more.
It is at least 75, preferably at least 78, more preferably at least 80 in a wet state. When the whiteness falls below the above range, the synthetic mica takes on a yellow tint. as a result,
It is not preferable because hues other than white become remarkably visible.

The difference in whiteness between the dry state and the wet state is preferably 15 or less, more preferably 10 or less. If the difference in whiteness exceeds the above range, for example, when synthetic mica is actually blended into a cosmetic or the like, a desired whiteness may not be obtained. In addition, it is preferable that the synthetic mica of the present invention not only has high whiteness but also has low chromaticity other than whiteness such as yellowness (specifically, close to 0).

In the present invention, "whiteness" is defined by JIS
In accordance with the rules of K 7105, a sample area of 3
0 mmφ, sample container 30 mmφ × 13 mm, tristimulus value of standard version (X = 81.2, Y = 82.6, Z = 92.5)
Was measured under the following conditions. In the present invention, the “dry state” indicates that the synthetic mica has been dried at 120 ° C. for about 2 hours, and the “wet state”
This shows that synthetic mica was put into water about twice as heavy as that, stirred, and then settled.

[0018] The particle size of the synthetic mica of the present invention is not particularly limited.
Preferably, it does not contain particles of μm or more. The elution amount of fluorine of the synthetic mica of the present invention is not particularly limited.
pm or less is more preferable from the viewpoint of enhancing safety when used in a cosmetic. The fluorine elution amount is particularly preferably 20 ppm or less in the above range.

In the present invention, the "fluorine elution amount" is a value measured in accordance with the rule of "synthetic mica" in the standard of non-standard cosmetic raw materials. Next, the method for producing synthetic mica of the present invention will be described in detail. [First Manufacturing Method] The first manufacturing method will be described by dividing it into first to fourth steps.

In the first production method of the present invention, first, talc [Mg ₃ SiO ₁₀ (O
H) ₂ ] and potassium silicofluoride [K ₂ SiF ₆ ] having an average particle size of 1 to 100 μm, from 60:40 to 90:10.
Mix well by weight ratio. Next, with respect to 100 parts by weight of the mixture, 0.1 to 30 parts by weight of alumina [Al ₂ O ₃ ] having an average particle diameter of 0.01 to 50 μm, and iron oxide with an average particle diameter of 0.01 to 50 μm [ Fe ₂ O ₃ ] to 0.00
1 to 30 parts by weight are mixed [first step].

The average particle size of talc is particularly preferably from 1 to 50 μm, more preferably from 5 to 20 μm in the above range. The average particle size of potassium silicofluoride is particularly preferably 1 to 50 μm in the above range,
More preferably, it is 5 to 20 μm. When the average particle size of talc and potassium silicofluoride exceeds the above range, the reactivity is reduced. In addition, since the particle size of the generated mica becomes large, it is necessary to go through a pulverizing step to actually use the mica, which causes a problem that the number of steps increases. on the other hand,
If the particle size is less than the above range, the particle size of the produced mica becomes too small, making it unsuitable for use in cosmetics and the like. The talc and the potassium silicofluoride may be pulverized and mixed by a mixing pulverizer such as a ball mill.

When the mixing ratio of talc and potassium silicofluoride is out of the above range, the synthetic mica to be produced has a reduced touch and slipperiness, and a reduced whiteness in dry and wet states. The mixing ratio (weight ratio) of talc and potassium silicofluoride is particularly 70: 3 in the above range.
The ratio is more preferably 0 to 85:15. The average particle size of alumina is particularly preferably 0.01 to 30 μm, more preferably 0.01 to 20 μm in the above range. The average particle size of the iron oxide is particularly within the above range.
001 to 30 μm, preferably 0.001 to 2
More preferably, it is 0 μm. If the average particle size of alumina and iron oxide exceeds the above range, the reactivity decreases. Further, since the particle size of the generated mica increases, a pulverizing step is required. Alumina and iron oxide are each preferably fine, but those having an average particle size smaller than the above range are difficult to obtain.

If the amount of alumina and iron oxide is out of the above range, the resulting synthetic mica has a reduced touch and slipperiness, and a reduced whiteness in dry and wet states. The amount of alumina is particularly preferably 0.1 to 25 parts by weight in the above range, and 0.1 to 20 parts by weight.
More preferably, it is part by weight. On the other hand, the compounding amount of iron oxide is particularly preferably from 0.001 to 25 parts by weight, more preferably from 0.001 to 20 parts by weight in the above range.

The mixed powder obtained in the first step is weighed,
Press molding with a molding pressure of 0 to 1000 kg / cm ² [second step]. By pressing the mixed powder,
The distance between the particles in the molded article becomes shorter, and the reactivity becomes better. When the press forming pressure is lower than 20 kg / cm ² , the formed body is easily broken, so that it is difficult to handle.
On the other hand, if it exceeds 1000 kg / cm ² , cracks and peeling occur in the molded body, and the reactivity at the time of heat treatment or annealing described below decreases. The press molding pressure is preferably 20 to 500 kg / cm ² in the above range.

The press molding is performed by weighing the mixed powder obtained in the first step in a range of usually 1 to 1000 g, preferably 1 to 300 g. The amount of the mixed powder to be subjected to press molding is not particularly limited to the above range. The press molding method is not particularly limited, and may be performed by a conventionally known method. After the mixed powder pressed in the second step is sealed, 900-1400
Heat treatment at a temperature of ° C. [third step].

The heat treatment is performed under conditions that are sufficient to cause the mixed powder to undergo a solid-phase reaction to form mica and that the mixed powder does not sinter. In addition, the heat treatment
It is performed in a sealed state to avoid volatilization of the mixed powder. If the temperature of the heat treatment is lower than 900 ° C., the mica generation rate decreases. Conversely, when the temperature exceeds 1400 ° C., the mixed powder sinters, so that it is necessary to go through a pulverizing step to actually use the produced mica. The heating temperature is particularly preferably 1000 to 1300 ° C. in the above range.

The time of the heat treatment is set in the range of 30 to 300 minutes, preferably 60 to 180 minutes. If the heating time is shorter than 30 minutes, the mica generation rate may be reduced. Conversely, if it exceeds 300 minutes, the mixed powder may be sintered. The method of the heat treatment is not particularly limited, and examples thereof include a method in which a press-formed mixed powder is put in a crucible, covered with a lid, sealed, and then heated.

After performing the heat treatment in the third step, annealing (annealing) is performed at a temperature lower by at least 100 ° C. than the heating temperature in the third step (fourth step). Annealing is not necessarily performed in a sealed state, but may be performed in an open system. Annealing temperature is 500 ~ 1
The heating is performed at a temperature in the range of 000 ° C. and at least 100 ° C. lower than the heating temperature in the third step. Annealing temperature
When the temperature is not lower than the heating temperature in the third step by 100 ° C. or more, the effect of annealing becomes insufficient or sintering proceeds. On the other hand, when the annealing temperature is lower than 500 ° C., the reactivity becomes low, and the annealing takes a long time.
Conversely, when the temperature exceeds 1000 ° C., sintering proceeds.

The annealing time is set in the range of 30 to 300 minutes. If the annealing time is less than 30 minutes, there is almost no change in the state of the product before and after annealing, and the effect of annealing may not be obtained. Conversely, if it exceeds 300 minutes, sintering may proceed. In the first manufacturing method, the whiteness in the dry state is 90 by sequentially performing the first to fourth steps described in detail above.
As described above, synthetic mica having a whiteness of 75 or more in a wet state, a soft touch, and a high slip property can be obtained.

The mica obtained by the first production method is
It is simply an aggregate made of powder having a particle size of 100 μm or less. Therefore, there is no need to go through a pulverizing step when actually using it. In order to use such mica as a raw material for cosmetics, particles having a particle size of 40 μm or more may be removed by classification. Further, by further treating the mica obtained by the first production method with a weakly acidic solution, the amount of eluted fluorine can be reduced to 50 ppm or less. Synthetic mica with a reduced amount of fluorine elution is more suitable as a raw material for cosmetics from the viewpoint of safety, more specifically, from the viewpoint that it has little effect on the human body.

As an example of the treatment with a weakly acidic solution, first, the produced mica is placed in a 1 to 10% aqueous lactic acid solution and stirred for 15 to 180 minutes, preferably for 15 to 90 minutes.
Then, after washing with water, a method of drying at 50 to 250 ° C. may be mentioned. By subjecting the synthetic mica obtained by the above manufacturing method to the treatment, the amount of fluorine eluted from the synthetic mica can be reduced to 50 ppm or less. Such treatment may be performed before classification, and in this case, particles having a size of 40 μm or more may be removed by classification after treatment.

Examples of the weakly acidic solution used for treating mica include, in addition to the aforementioned lactic acid aqueous solution, a conventionally known weakly acidic aqueous solution. The weak acid may be either an inorganic acid or an organic acid. As inorganic acids, for example, hydrochloric acid, nitric acid,
Sulfuric acid, chloric acid, perchloric acid, periodic acid, bromic acid, phosphoric acid, boric acid, carbonic acid and the like. Examples of the organic acid include carboxylic acids such as formic acid, acetic acid, acrylic acid, benzoic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, and phthalic acid; lactic acid, malic acid, tartaric acid, and citric acid And oxycarboxylic acids such as glycine, alanine, valine, leucine, tyrosine, threonine, cystine, thyroxine, amino acids such as alparagine, glutamic acid, lysine, and arginine.

[Second Manufacturing Method]
The description will be made by dividing into the fifth step. In the second production method of the present invention, first, talc having an average particle size of 1 to 100 μm,
An average particle size of 1 to 100 μm potassium fluorosilicate,
Mix well at a weight ratio of 60:40 to 90:10 [first step].

The preferred range of the average particle size of talc and potassium silicofluoride used and the mixing ratio of both are the same as in the first production method. Next, the mixed powder obtained in the first step is weighed and press-formed [second step].
The preferred range of the press forming pressure, the amount of the mixed powder weighed during the press forming, and the press forming method are the same as those in the first manufacturing method.

The mixed powder pressed in the second step is
After sealing, heat treatment is performed at a temperature of 600 to 1000 ° C. [third step]. The heat treatment is performed under conditions that are sufficient to cause the mixed powder to undergo a solid-phase reaction to generate mica and that the mixed powder does not sinter. When the temperature of the heat treatment is lower than 600 ° C., the reactivity decreases. vice versa,
If the temperature exceeds 1000 ° C., sintering proceeds, so that it is necessary to go through a pulverizing step in order to actually use the produced mica. The heating temperature is particularly in the range of 700 to 900.
C. is preferred.

The heating time is set in the range of 60 to 300 minutes, preferably 120 to 180 minutes. If the heating time is less than 60 minutes, the reaction may be insufficient.
Conversely, if it exceeds 300 minutes, sintering may proceed. The method of the heat treatment is not particularly limited, and examples thereof include a method in which a press-formed mixed powder is put in a crucible, covered with a lid, sealed, and then heated.

After the heat treatment in the third step, the powdery product is dispersed in water and swelled (fourth step).
The time for dispersing and immersing the product in water is set to be 10 hours or more. If the immersion time is less than 10 hours, the product cannot be sufficiently swollen, so that the mica generation rate in the fifth step described below decreases.

Next, the powdery product obtained in the fourth step is placed in a sulfuric acid acidic solution, and aluminum sulfate is further added at a ratio of 0.001 to 40% by weight, and iron sulfate is added at 0.001% by weight. An ion exchange reaction is carried out by blending and stirring each so as to have a ratio of about 30% by weight [fifth step]. In the fifth step, 0.001 to 40% by weight of aluminum sulfate and 0.001% of iron sulfate
The powdery product obtained in the fourth step may be blended with a sulfuric acid acidic solution containing ３０30% by weight, followed by stirring to carry out an ion exchange reaction.

The concentration of sulfuric acid in the above sulfuric acid acidic solution is 1
It is adjusted so as to be -20%, preferably 2-10%. When the content of aluminum sulfate in the sulfuric acid acidic solution exceeds 40% by weight or the content of iron sulfate exceeds 30% by weight, the mica generation rate decreases. On the other hand, when the content of aluminum sulfate is less than 0.001% by weight or the content of iron sulfate is less than 0.001% by weight, the ion exchange reaction takes a long time or the ion exchange reaction proceeds sufficiently. No longer.

The conditions of stirring and dispersion at the time of ion exchange are not particularly limited, but at a temperature of 0 to 100 ° C. and 0.05 to 24.
What is necessary is just to stir and disperse for about an hour. In the second manufacturing method,
The powdery product obtained by sequentially passing through the first to fifth steps described in detail above is further filtered, washed and dried to have a whiteness of 90 or more in a dry state and a whiteness in a wet state. A synthetic mica having a degree of 75 or more, a soft touch and a high slip property can be obtained.

The mica obtained by the second production method is
As in the case of the first manufacturing method, it is a mere aggregate made of powder having a particle size of 100 μm or less. Therefore, there is no need to go through a pulverizing step when actually using it. In order to use such mica as a raw material for cosmetics, particles having a particle size of 40 μm or more may be removed by classification. Further, by further treating the mica obtained by the second production method with a weakly acidic solution, the amount of eluted fluorine can be reduced to 50 ppm or less. The treatment method with a weakly acidic solution is the same as in the case of the first production method.

Next, the cosmetic of the present invention will be described in detail. The cosmetic of the present invention contains the synthetic mica of the present invention. The compounding amount of the synthetic mica is about 0.1 to 99% by weight based on the total amount of the cosmetic. If the amount of the synthetic mica is less than 0.1% by weight, it is not possible to adjust the spread, stickiness, covering power, moldability, etc. of the cosmetic amount. In addition, the characteristics of the synthetic mica of the present invention, which has a soft touch and high slipperiness, cannot be applied to cosmetics.

In the cosmetic of the present invention, in addition to the synthetic mica of the present invention, other components which are usually compounded in cosmetics can be appropriately compounded as long as the effects of the present invention are not impaired. Such other components include, for example, talc, kaolin, sericite, natural mica, vermiculite, magnesium carbonate, calcium carbonate, diatomaceous earth, magnesium silicate,
Inorganic powders such as calcium silicate, aluminum silicate, barium silicate, strontium silicate, metal tungstate, silica, hydroxyapatite, barium sulfate, ceramic powder; nylon powder, polyethylene powder, benzoguanamine powder, ethylene tetrafluoride powder , Distyrylbenzene pinhole polymer powder, organic powders such as microcrystalline cellulose; inorganic white pigments such as titanium oxide and zinc oxide; inorganic red pigments such as iron oxide (iron oxide) and iron titanate; γ-iron oxide Inorganic yellow pigments such as iron oxide yellow, loess;
Inorganic black pigments such as black iron oxide and carbon black; inorganic purple pigments such as mango violet and cobalt violet; inorganic green pigments such as chromium oxide, chromium hydroxide and cobalt titanic acid; inorganic blue pigments such as ultramarine and navy blue Pigment; pearl pigments such as titanium oxide-coated mica, titanium oxide-coated bismuth oxychloride, bismuth oxychloride, titanium oxide-coated talc, fish scale foil, colored titanium oxide-coated mica; metal powder pigments such as aluminum powder and copper powder; red 10
No. 4, Yellow No. 4, Yellow No. 5, Green No. 3, Blue No. 1, Blue No. 2, Red No. 202, Red No. 226, Red No. 227, Red No. 230, Orange No. 206, Orange No. 207, Yellow No. 202
No., green No. 201, green No. 204, blue No. 201, green No. 205 and the like; carminic acid, raccaic acid,
Lakes of natural dyes such as calsamine, bradylin, crocin; squalane, liquid paraffin, petrolatum, microcrystalline wax, ozokerite, ceresin, myristic acid, palmitic acid, stearic acid,
Oleic isostearic acid, cetyl alcohol, hexadecyl alcohol, oleyl alcohol, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, 2-octyl dodecyl myristate, 2-octyl dodecyl gum ester, neopentyl glycol-2-
Ethyl hexanate, isooctylic acid triglyceride, 2-octyldodecyl oleate, isopropyl myristate, isostearic acid triglyceride, coconut oil fatty acid triglyceride, olive oil, avocado oil,
Various hydrocarbons such as beeswax, myristyl myristate, mink oil and lanolin; oils such as higher fatty acids, fats and oils, esters, higher alcohols and waxes; organic solvents such as acetone, toluene, butyl acetate and ethyl acetate; alkyd resins And urea resins; plasticizers such as camphor and acetyltributyl citrate; ultraviolet absorbers, antioxidants, preservatives, surfactants, humectants, fragrances, water, alcohols, thickeners and the like.

[0044]

The present invention will be described below with reference to Examples, Comparative Examples and Formulation Examples. Note that Examples 1 and 2 correspond to the first manufacturing method of the present invention, and Examples 3 and 4 correspond to the second manufacturing method. Comparative Examples 1 and 2
Correspond to Examples 3 and 11 disclosed in Japanese Patent Publication No. Hei 6-27002, and Comparative Example 3 corresponds to Patent No. 256
No. 7596 corresponds to Production Example 1.

[Production of Synthetic Mica] Example 1 Talc and potassium silicofluoride having an average particle size of 15 μm by pulverization were used. The alumina used had an average particle size of 1 μm by pulverization. The iron oxide used had an average particle size of 1 μm by pulverization.

The talc and the potassium fluorosilicate were mixed at a weight ratio of 80:20, and 2 parts by weight of the alumina and 0.5 part of the iron oxide were added to 100 parts by weight of the mixture.
Parts by weight. From the mixed powder thus obtained, 2
00 g was weighed and pressed with a pressing machine at a molding pressure of 200 kg / cm ² to obtain a molded body having a diameter of 100 mm and a thickness of 15 mm.

Next, the molded body was placed in an alumina crucible, covered, sealed, and then placed in an electric furnace for 1200 minutes.
Heat treatment was performed at 2 ° C. for 2 hours. After the heat treatment, open the crucible lid and perform annealing at 700 ° C. for 1 hour.
Synthetic mica was obtained. The obtained synthetic mica was an aggregate composed of powder having an average particle diameter of 100 μm or less. Therefore, only classification was performed without going through a pulverizing step, and the particle size was 40 μm.
The above particles were removed.

Example 2 100 g of the synthetic mica after classification in Example 1 was used.
After dispersing in 1 liter of a 5% lactic acid solution and stirring for 1 hour, the mixture was filtered, washed, and dried at 120 ° C. for 5 hours. The amount of fluorine eluted in the powdery synthetic mica thus obtained was measured by ion chromatography. The amount of fluorine eluted before treatment with the lactic acid solution was 70 ppm, which was reduced to 12 ppm.

After mixing talc and potassium fluorosilicate at a weight ratio of 80:20, 2 parts were obtained from the resulting mixture.
00g was weighed and pressed with a pressing machine at a molding pressure of 200 kg / cm ² to obtain a molded body having a diameter of 100 mm and a thickness of 15 mm. Next, the molded body was placed in an alumina crucible, covered, sealed, and then heat-treated at 900 ° C. for 3 hours in an electric furnace.

After the heat treatment, the obtained powdery product was
0 g was weighed, put in 1000 g of water, and stirred for 24 hours. Further, 20 g of the above powder, 0.4 g of aluminum sulfate, and 0.1 g of iron sulfate were added to 1000 g of a 5% sulfuric acid acidic solution (pH 2) and stirred for 1 hour. Next, the resultant was filtered, washed, and dried at 120 ° C. to obtain powdered synthetic mica.

Example 4 100 g of the powdery synthetic mica obtained in Example 3 was
% Lactic acid solution and stirred for 1 hour.
It was washed by filtration and dried at 120 ° C. for 5 hours. The amount of fluorine eluted in the powdery synthetic mica thus obtained was measured by ion chromatography. The amount of fluorine eluted before treatment with the lactic acid solution was 50 ppm.
It was reduced to 0 ppm.

Comparative Example 1 Talc and potassium silicofluoride having an average particle size of 2 μm by pulverization were used. The talc and potassium fluorosilicate are mixed at a weight ratio of 80:20,
This mixture is placed in an alumina crucible and placed in an electric furnace for 90 hours.
Heat treated at 0 ° C for 1 hour to produce synthetic mica (fluor mica)
I got

Comparative Example 2 The same talc and potassium silicofluoride as in Comparative Example 1 were used. Alumina has an average particle size of 2 μm by grinding.
Was used. The talc and the potassium silicofluoride were mixed at a weight ratio of 80:20.
0.01 parts by weight of the above alumina was mixed with 00 parts by weight.

Next, the mixed powder thus obtained was placed in an alumina crucible and heated at 900 ° C. for 1 hour in an electric furnace to obtain synthetic mica (fluoric mica). Comparative Example 3 40 parts by weight of silicic anhydride, 30 parts by weight of magnesium oxide,
After mixing 13 parts by weight of aluminum oxide and 17 parts by weight of potassium silicofluoride, the mixture was melted at 1400 to 1500 ° C and crystallized at 1300 to 1400 ° C to obtain a synthetic mica ore.

The obtained ore of synthetic mica was pulverized and classified to a powdery form, and further finely pulverized by a vibration mill.
The mixture was stirred in a 1 M aqueous citric acid solution for 5 hours. After stirring, the mixture was dried at 120 ° C. for 5 hours, and those having a particle size of 40 μm or more were removed by classification. [Evaluation of Synthetic Mica] (X-ray crystal analysis) The synthetic mica obtained in Examples 1 to 4 and Comparative Examples 1 to 3 was subjected to crystal analysis by powder X-ray diffraction. The measurement was performed in the range of 2θ = 2 to 70 degrees.

(001), (002),
As a result of obtaining the lattice constant of the (003) plane, the lattice constants in Examples 1 to 4 were 10.00.0Å, 5.0 in order.
Comparative Example 1 was 120 ° and 3.3360 °.
Then 10.0400Å, 5.010Å, 3.3330
Å, in Comparative Example 2, 10.0420Å, 5.0310Å,
3.3400 °, 10.0500 ° in Comparative Example 3,
0500 ° and 3.3500 °.

As is clear from the above results, Example 1
The synthetic mica of Nos. To 4 was (002) as compared with Comparative Examples 1 to 3.
The peak of the plane was shifted to the lower angle side. That is, the synthetic mica of Examples 1 to 4 had a different crystal structure from the mica of Comparative Examples 1 to 3. (Measurement of Average Particle Size) The average particle size of the synthetic mica obtained in Examples 1 to 4 and Comparative Examples 1 to 3 was measured with a laser diffraction particle size distribution meter (trade name “Rodos” manufactured by JEOL Ltd.). Measured. Table 1 shows the results.

[0058]

[Table 1]

As is apparent from Table 1, the average particle size of the synthetic mica of Examples 1 to 4 is about 12 to 13 μm, and even when used as a raw material for cosmetics, it is necessary to go through a pulverizing step. I knew it wasn't. (Evaluation of color) With respect to the synthetic mica obtained in Examples 1 to 4 and Comparative Examples 1 to 3, whiteness W and yellowness Y1 were measured in a dry state and a wet state.

The measurement was performed in accordance with the "reflection method" defined in JIS K 7105, and a color difference meter "ND-
1001DP ". The measurement conditions are as follows. Sample area: 30 mmφ Sample container: 30 mmφ × 13 mm Tristimulus value of standard plate: X = 81.2, Y = 82.6, Z =
92.5 Table 2 shows the measurement results.

[0061]

[Table 2]

As is clear from Table 2, the whiteness was extremely high in the dry state. On the other hand, in the wet state,
Examples 1 to 4 have high whiteness, but Comparative Examples 1 and 2
The whiteness was greatly reduced. In addition, although the synthetic mica of Examples 1-4 contained iron content, all were low in yellowness and did not have yellowishness.

[Production of Cosmetic] Formulation Example 1 A foundation was prepared using the synthetic mica of Examples 1 to 4 according to the formulation shown in Table 3.

[0064]

[Table 3]

Component A shown in Table 3 was treated with a 3% by weight aqueous solution of a perfluoroalkyl phosphate ester salt. Next, component A and component B are mixed, and component C is added thereto.
Was added and mixed. Further, the mixture was pulverized and stamped on a metal plate using a mold to form a foundation. All of the obtained foundations were excellent in feel (feel), spread (extensibility), sebum resistance (adhesion, adhesion), covering power (hiding ability) and moldability.

Formulation Example 2 Using the synthetic mica of Examples 1 to 4, a foundation was prepared according to the formulation shown in Table 4.

[0067]

[Table 4]

The inorganic powders shown in Table 4 were all treated with a 3% by weight aqueous solution of a perfluoroalkyl phosphate ester salt. Each of the obtained foundations was excellent in feel, spread (extensibility), sebum resistance (adhesion, adhesion), covering power (hiding ability), and moldability. Formulation Example 3 A foundation was prepared using the synthetic mica of Examples 1 to 4 according to the formulation shown in Table 5.

[0069]

[Table 5]

The obtained foundations were all excellent in feel, spread (extensibility), sebum resistance (adhesion, adhesion), covering power (hiding), and moldability.

[0071]

As described in detail above, the synthetic mica of the present invention exhibits excellent whiteness not only in a dry state but also in a wet state, and is therefore suitably used as a raw material for cosmetics and the like. ADVANTAGE OF THE INVENTION According to the manufacturing method of the synthetic mica of this invention, the synthetic mica which is soft, has high slipperiness, and has excellent whiteness not only in a dry state but also in a wet state can be obtained.

Further, since the cosmetic of the present invention contains the synthetic mica of the present invention, it is excellent in feel, spread, sticking, covering power, moldability and the like.

Claims (6)

[Claims] (1) a whiteness degree in a dry state of 90 or more,
A synthetic mica characterized in that the whiteness in a wet state is 75 or more. 2. The synthetic mica according to claim 1, wherein the elution amount of fluorine is 50 ppm or less. 3. The method for producing synthetic mica according to claim 1, wherein talc having an average particle size of 1 to 100 μm and potassium silicate fluoride having an average particle size of 1 to 100 μm are mixed in a ratio of 60:40 to
Alumina having an average particle diameter of 0.01 to 50 μm is used in an amount of 0.1 to 100 parts by weight of a mixture containing 90:10 by weight.
After mixing 30 parts by weight and 0.001 to 30 parts by weight of iron oxide having an average particle size of 0.01 to 50 μm,
Press molding at a pressure of 0 kg / cm ² , followed by heat treatment in a sealed state at a temperature of 900 to 1400 ° C., and annealing at a temperature lower by 100 ° C. or more than the temperature of the heat treatment. Mica production method. 4. The method for producing synthetic mica according to claim 1, wherein talc having an average particle size of 1 to 100 μm and potassium silicate fluoride having an average particle size of 1 to 100 μm are mixed in a ratio of 60:40 to
A mixture containing 90:10 by weight is used in an amount of 20 to 1000.
After press-molding at a pressure of kg / cm ² , heat treatment is performed at a temperature of 600 to 1000 ° C. in a sealed state, then dispersed and swelled in water, and further aluminum sulfate is added to a pressure of 0.02 kg / cm ^2.
01-40% by weight and iron sulfate 0.001-30% by weight
A method for producing synthetic mica, wherein an ion exchange reaction is carried out in a sulfuric acid solution containing at a ratio of: 5. A method for producing synthetic mica, wherein the synthetic mica obtained by the method according to claim 3 is further treated with a weakly acidic solution. 6. A cosmetic comprising the synthetic mica according to claim 1 or 2.