JPS63185810A - Synthetic mica powder, its production and cosmetic compounded therewith - Google Patents

Abstract

PURPOSE:To suppress surface activity of a synthetic mica, to prevent the dissolution of fluorine ion from the mica and to enable the use of the synthetic mica as a compounding raw material for safe and high-quality cosmetics, by adjusting the molar number of fluorine in a synthetic mica composition at a specific level below the stoichiometric composition of synthetic mica. CONSTITUTION:The molar number of fluorine in the objective synthetic mica powder is 75-99% of the stoichiometric level of synthetic mica. The synthetic mica powder can be produced by heat-treating a synthetic mica at 600-1,350 deg.C in an atmosphere properly selected from oxidizing atmosphere, reducing atmosphere, argon gas atmosphere, N2 gas atmosphere, ammonia gas atmosphere, vacuum, etc. The obtained synthetic mica is compounded to a cosmetic in an amount of about 1-100wt.% based on the whole cosmetic.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a synthetic mica powder, a method for producing the same, and a cosmetic containing the synthetic mica powder. Cosmetics containing the synthetic mica powder of the present invention have a colorful appearance, ease of use,
It is a cosmetic with an excellent finish, and is highly stable and safe.

[Prior Art] Various extender pigments are blended into cosmetics for the purpose of improving the spreadability, adhesion, hiding power, moldability, etc. of the product.

Extender pigments include inorganic powders such as talc, kaolin, and mica, and organic powders such as nylon powder, polyethylene powder, polystyrene powder, acrylic resin powder, and epoxy resin powder. Among these, mica has excellent transparency, luster, and extensibility when used.
There are many opportunities to use it. Recently, not only natural mica, but also
Synthetic micas have also been developed.

Synthetic mica is a phyllosilicate mineral obtained by a melting method, a hydrothermal method, or a solid-solid reaction method. Traditionally, high-quality crystalline synthetic mica powder contains potassium, sodium,
Compounds containing magnesium, aluminum, silicon, fluorine, etc. are mixed in a certain ratio, and this is melted, crystallized,
After cooling, it is obtained by mechanical pulverization. Examples of such things include the following:

KMg3 (AI St 30 trout) F2 Potassium phlogopite K Mg2 h (Si40wx) F2 Potassium tetrasilicon mica K Mg2 Li (Sin Otn) F
9-1Mg2'aLi% (
Sin OwJ) F2NaMg3 (AI Si
30! O) F2 Sodium Phlogopite NaMg2 Li
(Si4010) F2 Sodium Taeniolite NaM
g2 h (Si40w) F2 sodium tetrasilicon mica Na”ss Mgs+ %I Li% (St40
m) F disodium hectorite [Problem to be solved by the invention 1 As described above, although mica has excellent properties, natural mica is slightly colored because it contains a trace amount of metal. Therefore, when incorporated into cosmetics, there is a tendency to reduce the saturation of the cosmetic's appearance color. A common way to increase the saturation of the external color of cosmetics is to use organic pigments, but organic pigments have poor photostability and deteriorate due to light, causing discoloration and odor, which are undesirable for cosmetics. cause a phenomenon.

In addition, mica has a highly active powder surface and easily causes deterioration of oils, fragrances, etc.

In terms of extensibility when used, it is possible to substitute this with spherical resin powder to some extent, but if a large amount of spherical resin powder is blended, the adhesion of the cosmetic to the skin will be lowered, and the makeup will be more difficult to apply. Another problem arises in that the moldability of the material is deteriorated.

In terms of luster, it may be possible to incorporate a titanium-mica pearl pigment instead of mica, but this also leads to deterioration in the moldability of the cosmetic.

In other words, mica has excellent properties that cannot be substituted with other powders, but the problem of coloring due to trace amounts of metal and surface activity currently prevents it from being freely blended.

In order to solve these problems, the above-mentioned synthetic mica has been produced. Synthetic mica does not contain trace metals, so
Although the problem of lowering the saturation of the external color of cosmetics has been solved,
The surface activity of the powder is as strong as that of natural mica, and when incorporated into cosmetic preparations, fluorine ions (F-) are eluted, so safety issues remain unsolved.

Based on the above, the development of an excellent synthetic mica with suppressed surface activity and no elution of fluorine ions has been made.
It has been desired for the purpose of producing cosmetics, especially makeup cosmetics, which have excellent adhesion and moldability, give a highly saturated external color, and are highly stable and safe.

Therefore, the present inventors attempted to solve the above problems by reducing the number of moles of F in the synthetic mica. In such cases, the following methods can generally be considered.

(1) A method of dissolving F with a strong acid.

(2) A method of synthesizing by reducing the amount of F added during melting.

(3) A method of repeated washing with purified water, boiled water, etc.

However, in method (1), not only F but also Mg
.

K etc. may also be dissolved at the same time and the structure may be destroyed. (
In method 2), only the amount of mica crystals precipitated decreases, and the number of moles of F in the synthetic mica does not change.

Method (3) is hardly effective in reducing the number of moles of F.

[Means for Solving the Problems] In view of the above circumstances, the present inventors conducted further studies and succeeded in developing a new synthetic mica powder that exhibits extremely useful and interesting properties and a method for producing the same. However, the present invention was completed.

That is, the first invention is a synthetic mica powder characterized in that the number of moles of fluorine in the synthetic mica composition is 75 to 99% of the stoichiometric composition of the synthetic mica, and the second invention is a method for producing the synthetic mica powder by heat-treating synthetic mica at 600 to 1,350°C, and the third invention is a cosmetic characterized by blending the synthetic mica powder. .

The present invention will be explained in detail below.

In the synthetic mica powder of the present invention, the number of moles of fluorine in the synthetic mica is 75 to 2 moles, which is the stoichiometric composition of the synthetic mica.
It is characterized by being ~99%.

If the F mole number is less than 75% of the stoichiometric composition, the synthetic mica decomposes and forms forsterite (MgSiO+).
, leucite (KAISt20s), etc., which is not preferable. Also, when the number of moles of F exceeds 99%,
It is not preferable since there is no difference in characteristics from that of 2 moles.

The number of moles of F is 75 to 99% of the stoichiometric composition, preferably 80 to 97.5%, more preferably 90 to 95%.
%.

The general formula of the synthetic mica powder of the present invention is shown below.

X'h~IY2~3 (Z4010) FIs~vs(
In the formula, X is Na", K", Lt", Ca", Rb
2+, Sr2+, Y represents one or more ions selected from the group consisting of M g2+, pe2+, )H2+, M
represents one or more ions selected from the group consisting of n2+, A13+, p e3+, Ll'', Z is ^13+, S
Represents one or more ions selected from the group consisting of i4+, G e4+, Fe'', and B3+.) The method for producing synthetic mica powder of the present invention includes heat treating synthetic mica at 600 to 1.350°C. At temperatures below 600°C, it is not possible to reduce the number of moles of fluorine, and on the other hand, at temperatures above 1,350°C,
This is not preferable because synthetic mica melts. The heat treatment temperature is 6
00 to 1,350°C, preferably 700 to 1,350°C
1,200°C, more preferably 900-1.1
It is 00℃.

The heat treatment time ranges from several seconds to several days and can be appropriately selected depending on the treatment temperature. For example, when synthetic fluorine phlogopite is treated at 1.000°C, about 0.5 to 10 hours is preferable.

A general method for producing synthetic mica is, for example, in the case of synthetic fluorophlogopite, about 40 parts of silicic anhydride and about 30 parts of magnesium oxide.
After mixing about 13 parts of aluminum oxide, and about 17 parts of potassium silicofluoride, the mixture was melted at 1,400 to 1,500°C and further crystallized at 1,300 to 1,400°C to form synthetic fluorophlogopite (KMg (AI). St 30MI)
F2) is obtained. After obtaining synthetic mica in this manner, the obtained ore lump is crushed and, if necessary, classified to obtain synthetic mica powder.

When crushing an ore lump, it is common to first coarsely crush it and then finely crush it. The heat treatment may be performed either after coarsely pulverizing or finely pulverizing the ore lump, but in the present invention, it is preferable to perform the heat treatment after pulverizing and classifying, as this is superior in terms of time reduction and effectiveness.

As the equipment for heat-treating the synthetic mica, all known methods such as an external heating furnace, an internal heating furnace, and a rotary kiln can be used.

The heat treatment atmosphere may be an oxidizing atmosphere, a reducing atmosphere, an argon gas atmosphere, a N2 gas atmosphere, an ammonia gas atmosphere, a vacuum, or a combination thereof, and can be selected as appropriate depending on the purpose and function.

The particle size of the synthetic mica powder with a small number of F moles of the present invention is generally 0.05 to 2 μm in the thickness direction, although it depends on the application.
, the surface direction is 2 to 60μ.

The amount of the synthetic mica powder added to the cosmetic is 1 to 100% by weight based on the total amount of the cosmetic.

The cosmetics of the present invention include a wide range of cosmetics such as facial cosmetics, makeup cosmetics, hair cosmetics, etc.
It is particularly suitable for makeup cosmetics, such as foundation, powder, eye shadow, blusher, makeup base, nail enamel, eyeliner, mascara, lipstick, fancy powder, and the like.

The synthetic mica powder of the present invention may be subjected to silicone treatment, metal soap treatment, fatty acid treatment, surfactant treatment, or treatment with acids, alkalis, or inorganic salts, as necessary when incorporated into cosmetics. It may be blended after performing the composite treatment.

In addition to the synthetic mica powder described above, other components commonly used in cosmetics can be appropriately blended into the cosmetics of the present invention, if necessary. For example, talc, kaolin, sericite, muscovite, phlogopite, red mica, biotite, lithium mica, vermiculite, magnesium carbonate, calcium carbonate, diatomaceous earth, magnesium silicate, calcium silicate, aluminum silicate, barium silicate. Inorganic powders such as barium sulfate, stronium silicate, metal tungstate, silica, hydroxyapatite, zeolite, boron nitride, ceramic powder, nylon powder, polyethylene powder, polystyrene powder, benzoguanamine powder, polytetrafluoroethylene powder, Organic powders such as styrene benzene polymer powder, epoxy powder, acrylic powder, and microcrystalline cellulose; inorganic white pigments such as titanium oxide and zinc oxide; inorganic red pigments such as iron oxide (red iron oxide) and iron titanate; Inorganic brown pigments such as gamma iron oxide, inorganic yellow pigments such as iron yellow oxide and loess, inorganic black pigments such as scorched iron oxide and carbon blank, inorganic purple pigments such as mango violet and cobalt bioleft,
Inorganic green pigments such as chromium oxide, chromium hydroxide, cobalt titanate, inorganic blue pigments such as ultramarine blue and navy blue, mica coated with titanium oxide, bismuth oxychloride coated with titanium oxide, bismuth oxychloride, talc coated with titanium oxide, fish scale foil , Burl pigments such as colored titanium oxide coated mica, metal powder pigments such as aluminum powder, copper powder, etc., Red 201
No., Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 226, Red No. 228, Red No. 405, Orange No. 203, Orange No. 204, Yellow No. 205, Yellow 4
Organic pigments such as No. 01 and Blue No. 404, Red No. 3, Red No. 104, Red No. 106, Red No. 227, Red No. 230, Red No. 401, Red No. 505, Orange No. 205, Yellow 4
Organic pigments such as zirconium, barium or aluminum lake of No. 5, Yellow No. 202, Yellow No. 203, Green No. 3 and Blue No. 1, natural pigments such as chlorophyll and β-carotene, squalane, liquid paraffin, petrolatum,
Microcrystalline wax, osikelite, ceresin, myristic acid, palmitic acid, stearic acid, oleic acid, isostearic acid, cetyl alcohol, hexadecyl alcohol, oleyl alcohol, cetyl 2-ethylhexanoate, 2-ethylhexyl valmitate, 2-myristic acid. Octyldodecyl, neopentyl glycol di-2-ethylhexanoate, glycerol tri-2-ethylhexanoate, 2-octyldodecyl oleate,
Isopropyl myristate, glycerol triisostearate, tori palm oil fatty acid glycerol, Tori 2-
Various hydrocarbons such as glycerol ethylhexanoate, 2-octyldodecyl oleate, isopropyl myristate, glycerol triisostearate, tricoconium oil fatty acid glycerol, olive oil, avocado oil, beeswax, myristyl myristate, mink oil, lanolin, silicone oil, Higher fatty acids, esters of oils and fats, higher alcohols, oily components such as waxes, organic solvents such as acetone, toluene, butyl acetate, acetic esters, resins such as alkyd resins and urea resins, camphor, acedol tributyl citrate, etc. Plasticizers, ultraviolet absorbers, antioxidants, preservatives, surfactants, humectants, fragrances, water, alcohol, thickeners, etc.

The cosmetic according to the present invention can be in the form of powder, cake, pencil, stick, ointment, liquid, emulsion, cream, etc.

[Examples] Next, the present invention will be further explained with reference to Examples and Reference Examples, but the present invention is not limited to these Examples.

First, an example of manufacturing the synthetic mica powder according to the present invention will be described. Measurements of chemical bone d value, X-ray diffraction, etc. in the production examples were carried out by the following methods.

Chemical analysis Potassium and magnesium were analyzed by flame photometry, aluminum by atomic absorption spectrophotometry, silica by gravimetric analysis, and fluorine by spectrophotometry.

It is a measurement chart of 2θ=2° to 50° by X-ray diffraction method. The measurement was carried out at 30kV and 25mA, and the slit system was set at 0.5. -1°, S, S, -1°R,S, -0,2m
+w was used. Note that the measurement conditions were 25° C. and 65% RH.

Fluorine elution amount sample 20g/200nd? F concentration of filtrate after stirring with distilled water at room temperature for 30 minutes. F analysis was performed by spectrophotometry.

4. Potassium elution amount Sample 20g/200mff Concentration of filtrate after stirring at room temperature for 30 minutes with distilled water. K analysis was performed by flame photometry.

5. Surface activity 20 mg of the powder was fixed with quartz wool in a Pyrex glass tube with an inner diameter of 4 cm, and t-butanol was passed through the tube at 250°C to measure its decomposition rate.

t-Butanol injection amount: 0.3μl Carrier gas: Nitrogen flow rate: 50m12/win Analysis by Shimabara Seisakusho! ! ! Using GC-7A, column P
EG-20M, 0.31mm x 25m,
The column temperature was 80°C. The surface activity was evaluated by the residual rate of t-butanol.

6. Brightness Powder was packed into a quartz glass powder measurement cell, measured with Hitachi Color Analyzer 607, and H,
The V and C values were calculated, and the brightness was expressed as the V value.

<Production Example 1> After mixing 40 parts of silicic anhydride, 30 parts of magnesium oxide, 13 parts of aluminum oxide, and 17 parts of potassium fluorosilicate, synthetic fluorophlogopite was melted at 1.500°C and crystallized at 1,350°C. was crushed and classified to obtain 100 parts of a synthetic fluorine phlogopite powder having a particle size of 2.5 μm (spherical equivalent value as measured by Sedigraph Model 5000-01 manufactured by Micromeritic Co., Ltd.; the same applies hereinafter).

This powder was heat-treated at 1100° C. for 1 hour in an Elema type electric furnace to obtain a synthetic mica powder (particle size: 2.6 μm) of the present invention.

Production Example 2 After mixing 50 parts of silicic anhydride, 20 parts of magnesium oxide, 10 parts of lithium carbonate, and 22 parts of sodium silicofluoride, the synthetic sodium teniodine was dissolved at 1,500°C and crystallized at 1,350°C. Grind and classify light, particle size 6
．． 100 parts of 0μ sodium taeniolite powder was obtained.

This powder was heat-treated at 700° C. for 1 hour in an Elema type electric furnace to obtain a synthetic mica powder (particle size: 6.0 μm) of the present invention.

Production Example 3 After mixing 40 parts of silicic anhydride, 30 parts of magnesium oxide, 13 parts of aluminum oxide and 17 parts of sodium silicate, 1. synthesized sodium teniodine was dissolved at 500°C and crystallized at 350°C. Crush and classify light,
100 parts of synthetic fluorophlogopite powder with a particle size of 2.5 μm was obtained.

This powder was heat-treated at 1300°C for 10 minutes in an Elema type electric furnace to obtain the synthetic mica powder of the present invention (particle size 2.6.17).
I got it.

<Comparative Production Example 1> Synthetic fluorophlogopite was melt-synthesized in the same manner as in Production Example 1, crushed and classified in the same manner as in Example 1, and then heated at 500°C.
A synthetic mica powder was obtained by heat treatment in an Elema type electric furnace for 8 hours.

<Comparative Production Example 2> Synthetic sodium taeniolite was synthesized by melting in the same manner as in Production Example 2, pulverized and classified in the same manner as in Example 1, and then heat-treated at 500°C for 8 hours in an Elema type electric furnace. , synthetic mica powder was obtained.

<Production Example 4> After mixing 40 parts of silicic anhydride, 30 parts of magnesium oxide, 13 parts of aluminum oxide, and 17 parts of sodium fluorosilicide, the synthetic sodium was dissolved at 1,500°C and crystallized at 1,350'C. Teniolite was crushed and classified to obtain 100 parts of synthetic fluorophlogopite powder with a particle size of 2.5 μm.

This powder was heat-treated at 900° C. for 8 hours in an Elema type electric furnace to obtain a synthetic mica powder (particle size: 2.6 μm) of the present invention.

Comparative Production Example 3> Synthetic fluorophlogopite was melt-synthesized in the same manner as in Production Example 1, crushed and classified in the same manner as in Example 1, and then heated at 1400°C.
The mixture was heat-treated in an Elema type electric furnace for 1 hour to obtain a synthetic mica powder.

<Comparative Production Example 4> Synthetic sodium taeniolite was melt-synthesized in the same manner as in Production Example 2, crushed and classified in the same manner as in Example 1, and then heat-treated in an Elema type electric furnace at 1400°C for 1 hour. , synthetic mica powder was obtained.

(Margin below) Table 1 **; t-butanol residual rate *: Unable to measure as it melts and solidifies.

Next, examples of cosmetics containing synthetic mica powder will be shown.

The performance of the cosmetics was evaluated on a five-point sensory evaluation by a panel of 20 experts regarding the items listed in the table below.

(Hereinafter in the margin) Table 2 (Hereinafter in the margin) The evaluation results are shown by the following symbols based on the average value of 20 people.

◎ ・・・・・・・・・・・・ 4.5 or more up to 5.0 ○ ・・・・・・・・・・・・ 3.5 or more but less than 4.5 △ ・・・・・・・・・・・・・・・ 2.5 or more, less than 3.5 0 or more 1.5
Example 1: Powder Foundation Powder foundation X according to the present invention was prepared from the following ingredients.

(Weight%) ■ Titanium oxide 72 Talc
203 Muscovite
34 Synthetic mica powder of Production Example 1
555 Nylon powder 26 Red iron oxide 0.57 Yellow iron oxide
18 Black iron oxide
0.19 silicone oil
110 Palmitate 2-9 Ethylhexyl 11 Sorbitan sesquioleate 112
Preservative 0.313 Fragrance 0.1 Ingredients 1 to 8 are mixed in a Henschel mixer, and to this mixture, ingredients 9 to 8 are mixed.
After adding and mixing 13 by heating and melting, 5HP
The powder was pulverized with a Valverizer (Kokuyo Micron) and molded into a medium plate with a diameter of 5.31 mm under a pressure of 160 kg/- to obtain powder foundation X according to the present invention.

Comparative powder foundation Y was prepared in the same manner as above except that the same amount of sericite was used instead of the synthetic mica powder of component 4. The sensory evaluation results are shown in the table below.

(Hereafter, blank space) Table 3 (hereinafter, blank space) As shown in the table, it can be seen that Powder Foundation X of the present invention received higher evaluations. Further, the hardness of the foundation was 26 for the foundation X of the present invention and 46 for the comparative foundation Y, which indicates that the foundation X of the present invention has a better molding state.

Example 2: Blusher A Blusher X according to the present invention was prepared from the following components.

(Weight%) +11 Talc 12.6
(2) Sericite 8.1 (3)
Mica 5.0 (4) Production example 1
Synthetic mica powder 62.5 (5) Red No. 226
0.4 (6) Titanium mica
3.0(7) Squalane
3.0(8) Palmitic acid
5.0 Ethylhexyl (9) Preservative 0.301
Fragrance 0.2 ingredients + 11
+21 (3) (4) (5) are mixed in a Henschel mixer, and the ingredients (71 (81 (9)
1QOI was heated and mixed and sprayed, and after further mixing, it was pulverized with a 511P balberizer (Kokuyo Micron), and after adding and mixing component (6), 4×61
The brush was molded into a medium plate at a pressure of 120 kg/aJ to obtain the brusher X of the present invention.

-Y in a comparative brush was prepared in the same manner as described above, except that 62.5 it% of the synthetic mica powder of component (4) was replaced with 20% by weight of sericite and 42.5% by weight of mica. . The sensory evaluation results are shown in the table below.

(Hereinafter in the margin) Table 4 (hereinafter in the margin) As is clear from the table, it can be seen that the Blasocia X according to the present invention is excellent in all of the sensory evaluation items. Furthermore, the hardness of the foundation was 29 for the Blusher X of the present invention and 35 for the comparative Blusher Y, indicating that the Blusher X of the present invention has better moldability.

Furthermore, the exterior color of the molded product was measured using Hitachi Color Analyzer 607.
As a result of measurement, the color saturation of the Brasscher of the present invention was 11.8.
It was found that the comparison Blusher Y had a chroma of 10.5, and the Blusher-X of the present invention had a higher chroma and a brighter appearance color.

Example 3: Fancy Powder Fancy powder X of the present invention was prepared from the following ingredients.

(Weight%) (1) Synthetic mica powder of Production Example 2 95(2)
Talc 4 (3) Fragrance
1(4) Iron oxide pigment
After mixing components (1), (2), and (41), component (3) was added and mixed, and the mixture was filled into a container to obtain fancy powder X of the present invention.

Comparative Fancy Powder Y was prepared in the same manner as above except that the same amount of talc (therefore, 99% by weight in total) was used instead of 95% by weight of the synthetic mica powder in component (11).
was prepared. Each fancy powder X and Y at 37℃
The odor stability of the sample stored in a constant temperature bath for one month and each control (immediately after production of Fancy Powder X and Y produced using the same formulation) was compared in terms of odor stability through sensory evaluation. In the case of Fancy Powder X of the present invention, there was almost no difference between the sample and the control after storage for -month. On the other hand, in the case of Comparative Fancy Powder Y, the sample after being stored for -month had a considerably odor compared to the control.

[Effects of the invention] The synthetic mica powder of the present invention does not elute fluorine ions,
It also has less surface activity. Therefore, by incorporating it into cosmetics, it has excellent extensibility, gloss, adhesion, and moldability, and has a highly saturated external color, which was not possible with conventional powder raw materials such as talc, mica, and kaolin, and is also stable. Excellent cosmetics with high safety and performance can be obtained.

In other words, when the synthetic mica powder of the present invention is blended into foundations, eye shadows, blushers, etc., cosmetics with good spreadability, glossy coverage, and smooth usability can be obtained. Furthermore, by blending the synthetic mica powder of the present invention, a cosmetic with a highly saturated external color can be obtained, making it possible to reduce the amount of organic pigments that have poor photostability and are prone to discoloration and odor. . Furthermore, since the synthetic mica powder of the present invention has low catalytic activity, it is possible to obtain highly stable cosmetics without deterioration such as odor. In addition, the synthetic mica powder used in the present invention has a fluorine ion eluator that is one of the ordinary synthetic mica powders.
/100, it can be said that the cosmetic of the present invention is highly safe.

Claims (3)

[Claims] (1) A synthetic mica powder characterized in that the number of moles of fluorine in the synthetic mica composition is 75 to 99% of the stoichiometric composition of the synthetic mica. (2) A synthetic mica powder in which the number of moles of fluorine in the synthetic mica composition is 75 to 99% of the stoichiometric composition of the synthetic mica, which is characterized by heat-treating the synthetic mica at 600 to 1,350°C. Production method. (3) A cosmetic comprising a synthetic mica powder in which the number of moles of fluorine in the synthetic mica composition is 75 to 99% of the stoichiometric composition of the synthetic mica.