JPS607964B2 - Manufacturing method for solid powder cosmetics - Google Patents

Description

[Detailed description of the invention] The present invention relates to a method for manufacturing powder solid cosmetics.

Specifically, it is a method for producing powder solid cosmetics using calcium silicate powder or silica powder having a specific shape as a solidification aid. Conventionally, powdered solid cosmetics, such as solid powder seals, cake-shaped foundations, cake-shaped eyeliners, cake-shaped eye shadows, and solid blushers, have been made using raw ingredients such as talc, kaolin, magnesium carbonate, mica, titanium oxide, and pigments. It is manufactured by mixing ingredients, fragrances, and other additives, and solidifying the mixture with a solidifying agent. As a solidifying agent, a liquid binder is generally used in which a liquid hydrocarbon such as liquid paraffin, squalane, ester, isopropyl myristate, octyl palmitate, etc., singly or in a mixture, and lanolin or a lanolin derivative added thereto is used. .

These liquid binders are usually added in an amount of 3 to 15% by weight based on the powder raw material component, but uniform mixing is difficult because the ratio of liquid to the volume of the powder raw material component is low.

On the other hand, if the amount of liquid binder added is too large, it will become oily and the characteristics of powdered cosmetics will be diminished. In addition, in the case of powders with poor compression moldability, such as mica, it is necessary to increase the molding pressure. It has the disadvantage of being bad (called ``sexuality''). The inventors,
As a result of various studies, we found that by using calcium silicate powder or silica powder with a specific shape as a molding aid, the liquid binder could be uniformly dispersed, compression molding could be performed at low pressure, and the resulting solid shape could be improved. It was discovered that cosmetics had good powder releasability, and this led to the completion of the present invention.

The present invention has an average longitudinal diameter of 0.1 to 30 mm and a thickness of 0.
．． A powder solid form characterized by using calcium silicate powder formed of an aggregate of flakes of 0.005 to 0.1 F, or silica powder formed of an aggregate having a similar shape as a solidification aid. This is a method for manufacturing cosmetics.

A typical manufacturing method for the above-mentioned specific calcium silicate or silica powder used in the present invention is disclosed in, for example, JP-A-54-9
As shown in No. 3698, when gypsum and a water-soluble silicate such as sodium silicate or potassium silicate are used as raw materials, the silicate is generally added gradually to a stone pipe suspension and reacted. The reaction system was used as it was, or after separating the reactants from the reaction system and making the spiked product into a suspension again,
It can be obtained by hydrothermal treatment at a temperature of 0.000°C. In these typical manufacturing methods, the size of the flakes obtained differs depending on the mixing ratio of raw materials, reaction conditions, etc.

Generally, the most suitable calcium silicate can be obtained by mixing the raw materials so that the Si02/Ca0 molar ratio of the obtained calcium silicate is 1.6 to 4.2. The calcium silicate obtained above is formed of an aggregate of flakes and has a gyrolite crystal structure.

The collection of flakes can be confirmed by taking microscopic photographs (eg, 500 sounds). Generally, the flakes have an average diameter in the longitudinal direction of 0.1 to 30 mm and a thickness of 0.005 to 0.
．． Normally, it is in the range of 1 Buddha, and in industry, the average diameter in the longitudinal direction is 0.5 to 15 Buddha, and the thickness is 0.005 to 0.
One Buddha level is the easiest to obtain.

From the above-mentioned microscopic photograph of calcium silicate, it can be observed that the aggregated state of the flakes resembles the shape of a flower with aggregated petals, especially the petals of a rose. Therefore, it is sometimes abbreviated as petal calcium silicate. Hereinafter, in the present invention, calcium silicate having the above-mentioned properties will be abbreviated as petal-like calcium silicate (petal-like silica).
This petal-shaped silica is a crystalline substance having a gyrolite type crystal structure, as shown in JP-A No. 54-93698, but it "often contains amorphous Si02 depending on the mixing ratio of raw materials. For Si02, grain boundaries cannot be confirmed even if a micrograph of a petal-shaped silica thin section is taken at a magnification of 100,000 times or more, and chemical analysis such as Na
Confirmed by extraction with OH. Of course, gyrolite-type calcium silicate is expressed as a○・$i02・2day20, so by chemically analyzing the petal-shaped silica and calculating the Si02/Ca○ molar ratio, the content of amorphous moxibustion i02 can be determined. You can also get .

As mentioned above, the petal-shaped silica that is most easily obtained industrially has an average longitudinal diameter of 0.1 to 15 mm and a thickness of 0.0 mm.
Generally, such petal-shaped silica has a molar ratio of Sj○ to Ca○ in the range of 1.6 to 42.

Although the manufacturing method and shape of the typical petal-shaped silica of the present invention have been described, the present invention is not limited thereto, and any petal-shaped silica having the above-mentioned shape can be used without particular limitation.

Further, the silicate used in the present invention is made of an aggregate of flakes having an average diameter in the longitudinal direction of 0.1 to 30 mm and a thickness of 0.005 to 0.1 mm.

In general, the above-mentioned aggregates of silica can be confirmed by taking microscopic photographs, and the shape is the same as, or almost the same as, petal-shaped silica, and in particular, it resembles an aggregate of rose petals, so petals are It is called silica. Hereinafter, in the present invention, it will be abbreviated using the term petal-shaped silica. The method for producing this petal-shaped silica is not particularly limited, and any method may be employed.

A typical method is disclosed in Japanese Patent Application Laid-Open No. 11839/1983.

As disclosed in JP-A-54-118399, petal-shaped silica is special compared to generally known silica such as white carbon and silica gel, and its properties are completely different. In particular, water lagoon silicate and water bath calcium compounds such as calcium chloride, gypsum, etc. are mixed, and if necessary, the reaction products produced during the mixing are concentrated and reslurred, or the mixture is mixed. A product obtained by directly subjecting it to a hydrothermal treatment at a temperature of 150 to 25,000 °C and further contacting it with, for example, a key acid to decalcify it, is excellent as the solidification aid of the present invention. The petal-shaped silica obtained by the above reaction may be dried or, if necessary, pulverized before use. The above-mentioned petal-shaped silica and petal-shaped silica are blended together with a liquid binder (solidifying agent) into the raw material components as a solidification aid.

The raw material components and liquid binder used as described above are used as they are. The amount of liquid binder added is generally 3 to 15% by weight based on the total components. Further, the amount of the solidification aid added is 2 to 15% by weight, preferably 3 to i weight%.
It is. If the amount of the solidification aid added is less than 2% by weight, the solidification effect will be small, and if it is more than 15% by weight, the powder solid cosmetic will become oily, which is not preferable.
Regarding the relationship between the solidification aid and the liquid binder, 1 to 1. It is better to use fang volume. There are no particular limitations on the method for producing the powdered solid cosmetic in the present invention. For example, powder raw materials such as talc and kaolin, solidification aids, coloring pigments, etc. are added in advance.
Mix with a blender, etc. Add a liquid binder to this, mix evenly, and adjust the color. If necessary, crush these with a crusher, sieve, fill in a metal plate, and compression mold. Another method is to mix a liquid binder such as liquid paraffin or isopropyl myristate with a solidification aid in a blender, and then mix this with powder raw materials, coloring pigments, etc. There is a molding method similar to the above method.The latter method is particularly preferred because the blending operation is simple, the binder can be uniformly dispersed, and molding can be performed at low molding pressure.

The first reason is that the amount of liquid absorbed by the petal-shaped silica and petal-shaped silica used as solidification aids is extremely large.

That is, the liquid binder is first mixed with petal-shaped silica and petal-shaped silica, but since these powders have a large amount of liquid absorption, the blend is in a powder state, and is used as a powder raw material and coloring pigment in the next process. Blending with other materials can be done extremely easily and uniformly. Incidentally, the liquid absorption amount of the petal-shaped silica and petal-shaped silica used in the present invention is generally 4 to 8 '/h. The second reason seems to be that the petal-like silica and petal silica are formed by an aggregate of flakes.

The liquid binder and the raw material powder are firmly inserted into the spaces between the petal-shaped aggregates of bonded flakes.
In the present invention, which is presumed to exhibit bonding strength, the advantages of using petal-shaped silica and petal-shaped silica formed from aggregates of flakes as solidification aids are as described above. It has the advantage that it has become possible to use high melting point waxes that were conventionally considered difficult to use, such as carnauba wax and candelilla wax. When high melting point wax is used, it feels good on the skin when dry and has a remarkable effect as a binder, but it is difficult to uniformly mix high melting point wax into powder due to its high melting point, and fine powder Its use was shunned because it was difficult to imitate. However, by mixing the high melting point wax with the solidification aid of the present invention in advance and keeping the mixing temperature of the blender above the high melting point wax involved, mixing becomes possible and the above drawbacks are overcome. It is.

As described above, by using the solidification aid of the present invention, powder raw materials, coloring pigments, etc. can be uniformly dispersed, and molding can be performed with low molding pressure. Moreover, the obtained powder solid cosmetic has the advantage of good powder releasability. The present invention will be explained below with reference to Examples, but the present invention is not limited thereto.

The petal-shaped silica and petal-shaped silica used in the examples were manufactured under the following conditions.

``Petal-shaped Kal'' 880 yen 20 minutes of water gypsum was put into the water and the flies were worshiped well. Next, while pouring this slurry, 0.243 mol of sodium silicate (Si○2 to Na20 molar ratio 2.5) was added for 20 minutes at 2500℃ under atmospheric pressure.
The mixture was added at a corresponding speed over 40 minutes. In this case, the molar ratio of CaS○4 to Na20/Si02 is 1.05.
Met. The obtained slurry was taken out into a Nutsche covered with a cloth and subjected to a reduced pressure (40 Hg), and washed with water for 30 minutes.The obtained cake was transferred to a waste tank and soaked in high temperature water
80-900C) was added and mixed uniformly to form a slurry. The slurry was autoclaved (inner volume: 5
0 pm) and subjected to hydrothermal treatment at 20,000 ℃ for 5 hours.
After the reaction was completed, the product slurry was taken out into a filter covered with heat-resistant paper cloth and filtered under reduced pressure (400 Yanagi Hg). The product after the above separation was dried at 12,000 for 16 hours. The weight of this dry product was 1084 kg. High specific volume is 17.8
cc′ evening, the volume of the pongee hole with a pore radius of 0.5 French or less is 6.3 c
It was c-nota. As a result of X-ray diffraction analysis of the dried product, it showed a pattern of gyrolite type calcium silicate. The results of chemical analysis are Ca024.9%, Si02
The weight loss on burning was 9.3%.

When this calcium silicate was photographed using an electron microscope and magnified twice, it was confirmed that the calcium silicate was composed of an aggregate of flakes with an average longitudinal diameter of 2 mm and a thickness of 0.1 mm or less.

"Petal-shaped silica" The dried material obtained in the above-mentioned method for producing petal-shaped silica was dried for 100 minutes, and then added with 100 g of isohydrochloric acid.
After adding 0 cc, the reaction was carried out at 70°C under atmospheric pressure for 1 hour. The reaction product was filtered and purified twice with 1,000 cc of ion-exchanged water, and then dried at 10,000 ml for 8 hours. The weight of this dry product was 73.2 kg. Further, the high specific volume of the dried product was 11.8 cc/night, and the volume of the string hole with a pongee hole radius of 0.5 French or less was 3.52 cc/night. As a result of chemical analysis, the dried material was found to be silicon dioxide. It also contained 8.4% by weight of water. When this silicon dioxide was photographed using an electron microscope and magnified twice, it was found that it was composed of an aggregate of flakes with an average longitudinal diameter of 2r and a thickness of less than 0.1 French.

Next, an example of a powder solid cosmetic product incorporating petal-shaped silica and petal-shaped silica into the formulation will be shown.

(Solid powder) (W Tsutomu) A 1 2 3 4 Talc 45.0 45.0 45.0 4
3.0 43.0 Power Orin 20.0 20.0
20.0 20.0 20.0 Zinc oxide 15.0
13.0 13.0 10.0 10.0 Minor incident.

7-.

707070 Su No. Tauru Ajimu 3-0 3-o 3-o 3-〇3-
〇Rice starch 20 20 20 20
20 Color pigment Appropriate amount Appropriate amount Appropriate amount Appropriate amount Fluorite S-7 - 5.0 10.0
- Fluorite R 5.0 -
10.0 Liquid paraffin 3.5 3.5 3.
5 3.5 3.5 myristic acid 1.5
1.5 1.5 1.5 Isopropyl 1.5 Preservatives Appropriate amount Appropriate amount Appropriate amount Appropriate amount Flavor Appropriate amount Appropriate amount Appropriate amount Appropriate amount (Fluorite S-700
is the petal-shaped silica of Eizan Soda ①, and the same R is the petal-shaped silica.

) The manufacturing method of A is to mix talc or other powder raw materials and coloring pigments in a blender, add a binder to this, and further mix uniformly to adjust the color. This is crushed in a crusher, passed through a sieve, then filled into a metal plate and compression molded. 1, 2, 3
In the case of , 4, the same manufacturing method as A is carried out, or as a different manufacturing method, petal-shaped silica and petal-shaped silica are mixed in advance with liquid paraffin and isopropyl myristate in a blender, and this is mixed in the same way as in A. The method of processing is sharp.

The product inspection results are as follows. A 1 2 3
4 Molding pressure 18* 14 wins 14* 10* 10
*Good moldability Good Good Good Good Powder release property Bad Good
Good Good Good In addition, the same results as 1, 2, 3, and 4 were obtained when petal-shaped silica or petal-shaped silica was premixed.

In other words, even if the molding pressure was lowered, by increasing the mixing ratio of petal-shaped silica and the same silica, powder release properties could be maintained without deteriorating moldability. Cake type ainyad (W multi) B 1 2 3 4 talc 48.0 44.0 Treatment. 0 44.0 44
．． 0 power Orin 15.0 14.0 14.0
13.0 13.0 Magnesium carbonate 1.0
1.0 1.0 1.0 1.0 Zinc stearate 10.0 10.0 10.0 8.0 8.
0 Titanium oxide 5.0 4.0 4.0 3.
0 3.0 Fluorite S-700-6.0
100 Fluorite R
6.0 - 10.0 Colored pigment 15.0 15.
0 15.0 15.0 15.0 Soba winding L 1.0
1.01・〇1・〇1・〇Liquid paraffin 4.0
4.0 4.0 4.0 4.0 Lanolin alcohol 1.0 1.0 1.0 1.0 1.
0 Preservatives Appropriate amount Appropriate amount Appropriate amount Appropriate amount Appropriate amount The manufacturing method is the same as the above-mentioned solid seal.

B 1 2 3 4 Molding pressure 2.8* 24* 24* 20* 20*
Moldability Fairly good Good Good Good Powder release property Bad Good Good Good Good Pre-mixed products obtained similar results and confirmed the same effect as the solid stamp.

Both solid eyeshadows and cake-shaped eyeshadows can be molded at a lower compression pressure than conventional formulas because they use petal-shaped silica or petal-shaped silica, and are easier to powder when used. In addition, even when the finished product was handled roughly, it did not lose its shape and was in good condition. Similar results were obtained for cake-shaped foundation, cake-shaped eyeliner, and solid blusher.

Similar results were also obtained with foundation and eyeliner containing a large amount of mica.・By using the petal-shaped silica or petal-shaped silica of the present invention, high-melting-point waxes that were conventionally considered difficult to use, such as carnauba wax and candelaya wax, can be premixed with the petal-shaped silica or petal-shaped silica. Depending on the situation, it can be used in powdered cosmetics.

Claims (1)

[Claims] 1. Average diameter in the longitudinal direction: 0.1 to 30μ, thickness: 0.00
A powder solid cosmetic product characterized in that calcium silicate powder formed of an aggregate of flakes having a size of 5 to 0.1μ or silica powder formed of an aggregate having a similar shape is used as a solidification aid. manufacturing method. 2. The manufacturing method according to claim 1, wherein the calcium silicate has a diairolite crystal structure and the SiO_2/CaO molar ratio is 1.6 or more.