JPS623123B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention can be used as a powder or molded into a cake, has good adhesion to the skin without using water, and has excellent texture, moisturizing effect, and fragrance retention. This invention relates to a method for producing an oil-based powder makeup composition with excellent effects. Conventionally, the method for manufacturing oil-based powder makeup materials in which a powder base material for cosmetics is treated with an oil-based substance involves spraying a single oil-based substance onto a mixture of powder base materials and spraying it onto the surface of the powder base material. Coating methods are known, but while they are easy to manufacture, it is extremely difficult to obtain a product with uniform coating. Therefore, products form a non-uniform oily coating layer, and even if silk powder is added to the powder base material, it will give a dry feeling unique to fibers, and even if silk powder is not added, it will not adhere to the skin. It has poor properties, sticks unevenly, easily comes off, and is completely impossible to recoat. As a method for improving this, it is known to spray coat the surface of the powder base material with a solution of an oily substance in an organic solvent or a dispersion solution in which a small amount of water is mixed with this solution, but this method achieves highly uniform coating. However, the adhesion of the obtained oil-based powder make-up is also not sufficient, and the oil-based powder make-up formed into a cake shape tends to thin or crack during long-term storage, making it difficult to apply multiple coats. is also impossible. As a further improved method, after adding and mixing a powder base material to an aqueous emulsion of an oily substance, the powder surface is activated by mechanical polishing, and then left at 20 to 40°C for 5 to 7 days to dry and pulverize. A method for doing this is disclosed in Japanese Patent Publication No. 35-12800. However, this method requires a long production time of 5 to 7 days or more, and the obtained oil-based powder makeup has poor adhesion to the skin, poor affinity, spreadability, and is completely impossible to layer. . Furthermore, as a manufacturing method similar to the above method,
A method is known in which the powder base material is mixed and dispersed in an aqueous emulsion of an oily substance and then heated to a temperature of 80°C or higher and dried. Since it takes a long time for the oil-based substance to adhere, coalescence of the powder base material and the formation of coarse, hardened agglomerated particles take place during that time, making it virtually impossible to achieve a uniform surface coating. However, they have the disadvantage that they tend to produce oil-based powder makeup that gives a rough and uncomfortable feeling to the skin and does not spread easily. On the other hand, Patent No. 44304 discloses that inorganic pigments (talc and zinc white) are added and mixed with stirring into an emulsion made by mixing lanolin gum arabic and water, and the upper liquid becomes transparent. A method for producing white flour is disclosed, which comprises filtering, squeezing, dehydrating, and adding glycerin and a preservative to the lanolin-coated pigment thus obtained and kneading the mixture, with stirring stopped at that point. However, even with this method, uniform surface coating with the inorganic pigment lanolin is not possible. Therefore, even if the above-mentioned lanolin-coated pigment is dried and used as an oil-based white powder,
It has many drawbacks, such as insufficient adhesion, blending, and spreadability to the skin, and the complete inability to apply multiple coats to the skin. As described above, the conventional manufacturing method has many problems such as the long production time, and the resulting oil-based powder makeup has an uneven and unstable surface coating made of oil-based substances, so it is difficult to use silk. Even if powder is added, it does not adhere well to the skin, spreads well, or feels good when used. Furthermore, when formed into a cake shape, not only does it not hold well in the puff, but the cake tends to become thinner (volume reduction) and cracks (cracks) during storage. Furthermore, oil-based powder cosmetics obtained by conventional methods have many drawbacks, such as no moisturizing effect, and consumers have been demanding improvements in these problems. The present inventors have previously (Japanese Patent Application No. 52-40597, JP 53-127840) mixed an aqueous emulsion of an oil-based substance and an inorganic powder, and then dissolved it by adding a water-miscible organic liquid. In the case of emulsification, the inorganic powder becomes a coagulated substance uniformly coated with an oily substance, which settles when left to stand, and then the coagulated substance is separated from the liquid and dried. It has been found that an improved oily white powder can be obtained by the method. Subsequently, it was found that this oil-based white powder improved all the drawbacks of the prior art, but was found to be insufficient in heat retention and flavor retention. As a result of further research,
When silk powder, wool powder, inorganic powder, or even organic pigments are mixed with an aqueous emulsion of an oil-based substance, a water-miscible organic liquid is added thereto under stirring to demulsify the aqueous emulsion, as described above. All of the powder becomes a coagulate structure that is uniformly coated with an oily substance and settles when left to stand still. When drying the coagulated material (a mixture of powders coated with an oily substance) from the liquid component (a mixed solution consisting of water, a water-miscible organic liquid, and an emulsifier), each of the above-mentioned powders It was discovered that oil-based powder makeup can be obtained by quickly drying without causing agglomeration (secondary particle formation), omitting the pulverization process, and also has excellent moisturizing and fragrance-retaining properties. Completed the invention. The object of the present invention is to provide a method in which the coexisting silk powder, wool powder, inorganic powder, or even organic pigment is uniformly coated with an oily substance to form a powder or cake shape, and water is not used. It adheres easily even if you don't have it, takes it off to the puff, and spreads easily.
To provide a method for industrially easily and advantageously producing an oil-based powder makeup composition that can be easily applied in layers, gives a good feel and moisturizing effect to the skin, and has excellent fragrance retention during storage after application. There is a particular thing. That is, in the present invention, after mixing an aqueous emulsion of an oily substance, silk powder, wool powder, inorganic powder, or further an organic pigment, a water-miscible liquid is added thereto under stirring to form the aqueous emulsion. This is a method for producing an oil-based powder makeup composition, which is characterized by demulsifying, and then separating the coagulated product from the liquid and drying it. The above-mentioned coagulated substances are those that separate and precipitate from the liquid phase when left to stand after being demulsified, and include silk powder, wool powder, and inorganic powder coated with an oily substance. Furthermore, it is mainly a mixture consisting of an organic pigment. Further, the liquid component is a mixed solution consisting of water, a water-miscible organic liquid, and a small amount of an emulsifier. Furthermore, the powder makeup ingredients in oil-based powder makeup ingredients include face powder (white powder), pressed powder (solid white powder), stage color, blusher, powder eye shadow, powder foundation, and cake-like foundation. ,
Powder lipstick and cake-like mascara. The silk powder used in the present invention is, for example, pulverized raw silk, refined silk (fibroin), recycled silk thread, chemically treated silk thread, etc., or dyed, bleached, antistatically treated, insect repellent treated, etc. as necessary. However, the present invention is not limited to these. The particle size of the silk powder is such that it passes through a Tyler standard sieve of 60 mesh or more (preferably 100 mesh or more). The amount of silk powder used (mixed amount) is 1 to 30% by weight, preferably 5 to 30% by weight based on the weight of the inorganic powder.
It is 20% by weight. When it is less than 1% by weight,
Improving effects on moisturizing properties, fragrance retention, texture, etc. tend to decrease, and if the amount exceeds 30% by weight, the appearance and cosmetic effects of the product tend to deteriorate. The mixing ratio (use ratio) of silk powder and wool powder is 90:10 ~
10:90, preferably 70:30-30:70. Wool powder is made by grinding top-like or cotton-like wool (raw wool) such as merino, down, and Lincoln wool through normal washing and combing processes using a normal mechanical grinding method. It may be used, or it may be dyed, bleached, treated to prevent static electricity, insect repellent, etc., if necessary, but is not limited thereto. The particle size of the wool powder is such that it passes through a Tyler standard sieve of 60 mesh or more (preferably 100 mesh or more). The amount of wool powder used is within the range of 1 to 30% by weight, preferably 5 to 20% by weight based on the weight of the inorganic powder. If it is less than 1% by weight, the effect of improving moisturizing properties, fragrance retention, feel, etc. tends to decrease, and if it exceeds 30% by weight, the appearance of the product and the cosmetic effect tend to deteriorate. In the present invention, by using silk powder and wool powder together, it is possible to jointly develop the unique feel of both powders, giving the skin a moderately soft and extremely good feel. Furthermore, both are amphoteric compounds that are polypeptides, and have a similar structure to natural moisturizing factor (NMF), which is necessary to prevent skin dryness and roughness and maintain suppleness, and are also related to the specificity of their physical shapes. Since it has high water absorption, oil absorption, and affinity for fragrances, it has extremely good moisturizing and protective effects on the skin surface, and has very good fragrance retention in the product and after use. The water-miscible organic liquid used in the present invention is one that does not show acidity or alkalinity when mixed with water, and is one that does not exhibit acidity or alkalinity when mixed with water, and is one that does not exhibit acidity or alkalinity as proposed by Hildebrand ("coloring material").
Vol. 47, 1974, pp. 28-37) Solubility parameter formula; δ = (ΔE/V) 1/2 (ΔE is heat of vaporization, V is molecular volume, δ is solubility parameter) (δ) is 8.2 to 16.0 (preferably 9.5 to
15.0) is preferable. Examples include methanol, ethanol, isopropanol, n-butanol, cellosolve, butyl cellosolve, butyl carbinol, methyl ethyl ketone, methyl isopropyl ketone, acetone, ethyl acetate, cello acetate, butyl acetate, carbitol, and the like. These materials may be used alone or in combination. Particularly the most preferred water-miscible organic liquids are ethanol, isopropyl alcohol, n-
These are propanol, n-butanol, and acetone. The amount of water-miscible organic liquid added is the amount necessary to demulsify the aqueous emulsion, and is usually 20 to 130% by weight, preferably 30 to 100% by weight, based on the weight of the aqueous emulsion. By adding the above-mentioned water-miscible organic liquid to demulsify the aqueous emulsion of the oily substance, the oily substance dispersed in the system is coagulated and instantly dispersed into a powder (inorganic powder). , organic pigments, silk powder, and wool powder) to form a uniform coating layer (oil-based film), thereby making it possible to obtain a product with good adhesion properties to the skin. In particular, it is possible to incorporate a large amount of silk powder or wool powder, which was previously impossible, and the addition of these ingredients can provide a moisturizing effect and a fragrance-retaining effect. In addition, the use of water-miscible liquids (eg, alcohol, acetone, etc.) speeds up the drying of the coagulation and facilitates pulverization, and its effects are extremely specific. The aqueous emulsion of an oily substance as used herein refers to a conventional oil-in-water emulsion and a water-in-oil emulsion containing an oily substance for cosmetics as the oil component. The oily substances used in the emulsion are oily substances for cosmetics, such as ordinary fats and oils, waxes, hydrocarbon oils, higher fatty acids, higher alcohols, esterified oils, silicone oils, etc., and may include one or two types. The above are used in combination. Examples of the above-mentioned fats and oils include castor oil, avocado oil, and cacao butter; examples of the wax include beeswax, lanolin, and carnauba wax; and examples of the hydrocarbon oil include liquid paraffin, squalane, and the like.
pristane, hydrogenated polyisobutylene, etc.
Examples of the esterified oil include, but are not limited to, isopropyl myristate, isopropyl palmitate, 2-ethylhexyl succinate, isopropyl isostearate, and 2-ethylhexyl palmitate. Examples of emulsifiers contained in the emulsion include fatty acid soaps, anionic surfactants such as higher alcohol sulfate ester salts and higher alkylphenol sulfonates, fatty acid monoglycerides,
Examples include nonionic surfactants such as fatty acid esters of sugars, polyoxyethylene alkyl ethers, and polyoxyethyl higher alkyl phenol ethers. The content of oily substances in the aqueous emulsion is usually 5 to 60% by weight, preferably 10 to 50% by weight.
The amount of aqueous emulsion of oily substance used varies depending on the oil concentration and demulsification conditions, but is usually 20 to 200% by weight based on the total weight of the powdery substance.
(preferably 50 to 150% by weight). Examples of the inorganic powder used in the present invention include:
Examples include magnesium carbonate, titanium oxide, iron oxide, talc, kaolin, mica, titanium mica, calcium carbonate, magnesium silicate, bentonite, zinc oxide, and zinc stearate. Examples of the organic pigments include organic pigments Red No. 201, Red No. 202, Red No. 204, and Red No. 205.
No., Red No. 206, Red No. 207, Red No. 226, Yellow 4
Examples include aluminum lake No. 203, yellow No. 203, yellow No. 401, blue No. 1 aluminum lake, blue No. 404, and orange No. 203. The amount of organic pigment used is usually 5 to 10% by weight based on the weight of the inorganic powder. When mixing the above powders with an aqueous emulsion of an oily substance, they are stirred and mixed using a kneader or mixer until the powders are uniformly dispersed in the aqueous emulsion. Next, a water-miscible organic liquid is gradually added to this mixed dispersion system under stirring. The amount of oil in the vicinity of each powder particle can be adsorbed onto the particle surface of each powder to form an oily film. In this case, if the powder base material is immersed in the organic liquid in advance and then mixed and dispersed in the aqueous emulsion, a more uniform coating can be easily formed on the surface of the single powder particles. , it is possible to express better cosmetic effects. This is also one of the features of the present invention. From the demulsified product (consisting of a coagulated product consisting of a mixture of each powder coated with an oily substance and a liquid component of a mixed solution consisting of water, a water-miscible organic liquid, and an emulsifier), the above-mentioned As a method for separating the coagulated material from the liquid component, a gradient method, a filtration method, a centrifugation method, etc. are employed. When drying the coagulated product after separating and removing the liquid, the water-miscible organic liquid (e.g., alcohol, acetone, etc.) that remains together with the water allows for uniform drying in an extremely short period of time. Another feature is that it can prevent powder aggregation (secondary particle formation) that tends to occur during drying. The oil-based powder makeup powder obtained by drying is
There are very few fused and hardened parts between the particles and between the surfaces, so it can be made into single particles with a weak external force similar to wind pressure during fluidized fluid drying, and it is extremely easy to crush. Therefore, when the fluidized drying method is employed, a pulverization step is not particularly required. For drying, a known drying method such as a stationary hot air drying method or a fluidized drying method is applied. After drying, crush as necessary.
It is easy to crush, and even when sieved, it can be made into single particles to a large extent, and an oil-based powder make-up with uniform particle size can be obtained at a high yield. The oil-based powder make-up obtained by the method of the present invention is such that the silk powder, wool powder, inorganic powder, or organic pigment co-mixed therein is substantially uniformly coated with the oil-based substance, and The powder is in the form of a powder or cake, and when used, its adhesion to the skin, affinity (affinity), and feeling of use also depend on how easily the cake-shaped oil-based makeup powder can be applied to a puff or brush. Furthermore, it has a moisture-retaining ability (heat-retaining effect, moisturizing effect) that is completely impossible with conventional oil-based powder makeup products, and has a moist feel and long-lasting properties after application and during storage. It also makes it possible to impart a fragrance effect, and the specificity of its action and effect is extremely remarkable. The oil-based powder make-up composition of the present invention, in which silk powder, wool powder, inorganic powder, or further organic pigment (e.g., pigment) is substantially uniformly coated with an oil-based substance, is shown in FIGS. 1 and 2;
This can be clearly observed by comparing FIG. 3 and FIG. 4, and FIG. 5 and FIG. 6. That is, FIG. 1 (wool powder and pigment), FIG. 3 (silk powder and pigment), and FIG. Looking at Figure 5 (wool powder, silk powder, and pigment), Figure 1 clearly shows the scale characteristic of wool in wool powder and the sharp edges of the pigment, and Figure 3 clearly shows the characteristic scale of wool in wool powder and the sharp edges of the pigment. The thin filaments and sharp edges of the pigments are further added to the fifth layer.
In the image, the scale characteristic of wool and the sharp edges of the pigment can be clearly observed. However, Figure 2 (wool powder and pigment coated with an oil-based substance) and Figure 4 (silk powder and pigment coated with an oil-based substance) and Figure 4 (silk powder and pigment coated with an oil-based substance) show the state of the powder substance in the obtained powder foundation. Figure 6 (Wool powder, silk powder and pigment coated with oily substance)
In Figures 2 and 6, the scale peculiar to wool in wool powder is coated with an oily substance.
It is clear that the edges of the wool powder are rounded, and the sharp edges seen in Figures 1 and 5 have disappeared, and the edges and the whole have clearly become rounded. It is observed that the edges and the whole of the silk powder are rounded, and it is evident that the wool powder, silk powder and pigment are coated with an oily substance. As described above, the oil-based powder makeup composition of the present invention, in which a powder-like substance is coated with an oil-based substance, has excellent adhesion to the skin, affinity, and feeling of use, and can be easily layered. Since powder coexists, the feel when applying,
When molded into a cake shape, it is even easier to apply to a puff or brush, and it is possible to impart a moisturizing effect on the skin surface and a scent-retaining effect during storage after application. However, in the oil-based powder makeup compositions obtained by the conventional methods shown in Reference Examples 1 to 3,
As is clear from the comparison between Figure 8 (silk powder pigment before treatment) and Figure 8 (silk powder and pigment after treatment), the oily substance adheres unevenly to the powder base material and is not coated uniformly. Therefore, adhesion, affinity, feeling of use, moisturizing effect, etc. are significantly inferior. Examples will be described below. % shown in examples
means % by weight, and parts means parts by weight. Reference Example 1 (Coating with oil/fat alcohol solution) Stir a mixture of 21 parts of talc, 6 parts of kaolin, 4 parts of zinc stearate, 15 parts of titanium oxide, 10 parts of silk powder (passed through a 100 mesh sieve), and 3 parts of iron oxide. A solution of 3 parts of isopropyl myristate in 3 parts of ethanol was spray coated and then dried. Observation of the obtained powder foundation under an electron microscope revealed that the coating layer on the powder surface was non-uniform. Furthermore, when this powder foundation was molded into a cake shape using a conventional method and left for three months, cracks appeared and it also shrank slightly. The results of the usage test (panel test) are shown in Example 1 below.
It is also listed in Table 1. Reference Example 2 (Coating with oil and fat substance alone) Stir a mixture of 50 parts of talc, 16 parts of kaolin, 4 parts of zinc stearate, 15 parts of titanium oxide, 10 parts of silk powder (same as Reference Example 1), and 2 parts of iron oxide. Meanwhile, the particle surface was coated with 3 parts of liquid paraffin by spraying. Observation of the resulting powdery foundation using an electron microscope revealed that the coating layer on the powder surface was extremely non-uniform. The results of the usage test for this powder foundation are also listed in Table 1 of Example 1. Reference Example 3 (Method of attaching an emulsion of fat and oil substances and drying while aging) Sorbitan monostearate 1.4 parts, polyoxyethylene glycol distearate 5 parts, glycerin monostearate 4 parts, glycerin distearate 6 parts, 4 parts stearic acid, 8 parts squalane
130 parts of water (82-84°C) was mixed with stirring into a mixture (82-84°C) of 1.5 parts of talc, 8 parts of beeswax, and 4 parts of petrolatum to emulsify it, and after 50 minutes, 200 parts of talc and rutile titanium were added. A mixture with 12 parts of white was mixed in and heating was continued to complete lysis in 40 minutes. After leaving it to stand for an additional hour to complete the activation of the pigment, it was rolled for about an hour to polish the particles and impart uniform binding properties, and then aged at 35° C. for 7 days. Next, 330 parts of talc, 245 parts of magnesium carbonate, 125 parts of zinc white, and silk powder (same as Reference Example 1) were added to this aged product.
A mixture of 100 parts and 5 parts of bentonite (No. 7 on the drawing)
A mixture of silk powder and pigment (as shown in the figure) was mixed, ground in a ball mill, and sieved to obtain a product. The surface coating layer of the obtained powder foundation (the powder foundation shown in FIG. 8) made of an oily substance is the eighth layer.
As shown in the figure, it was non-uniform, had insufficient adhesion and affinity to the skin, had extremely poor spreadability, and was virtually impossible to recoat. The results of the usage test are also listed in Table 1 of Example 1. Example 1 (In the case of using an oil-in-water emulsion in the method of the present invention) Triethanol was added to a molten mixture (80°C) consisting of 3 parts of stearic acid, 6 parts of liquid paraffin, 1.5 parts of beeswax, and 3 parts of lanolin. 0.7 parts of amine and pure water
85.1 parts of an aqueous solution (80°C) was mixed in and emulsified for 5 minutes, and the mixture was cooled to 30°C to obtain an aqueous emulsion (oil-in-water emulsion) of an oily substance. Next, add 83 parts of talc, 10 parts of mica, 5 parts of titanium oxide, and silk powder (same as Reference Example 1) to this emulsion.
5 parts of wool powder (passed through a 100 mesh sieve), and a mixture of 2 parts of iron oxide;
The powder base material was uniformly dispersed by stirring for 10 minutes, and then 80 parts of ethanol was gradually added and mixed over 10 minutes while stirring to demulsify the emulsion.
The demulsified product is then subjected to a dehydrator to separate and remove the liquid component (mixed aqueous solution consisting of water, ethanol, and emulsifier), and the remaining coagulates (silk powder and wool powder whose main components are coated with an oily substance) are removed. A mixture of talc, mica, and titanium oxide (with a small amount of water, ethanol, and a trace amount of emulsifier) was dried with hot air at 80 to 90°C. The drying speed was extremely fast, and the dried material was dried uniformly to the extent that it could be easily pulverized by hand, and no agglomeration of powder, which tends to occur during drying, was observed. Thereafter, the dried product was subjected to a pulverizer (atomizer), and it was possible to easily pulverize it to a fairly uniform particle size.
Next, the pulverized product was sieved to obtain a powdered foundation of the present invention with extremely uniform particle size in a high yield. As a result of analysis of this powder foundation, the content of oily substances was 12.5%. As a result of observing this powder foundation with an electron microscope, it was found that
As shown in the figure, the wool powder is coated with an oily substance, and the scale peculiar to wool is no longer visible (the scale of the wool powder is clear in Figures 1 and 5). Also, the sharp edges of the pigment powders are rounded (the sharp edges of the pigments are observed in Figures 1 and 5), indicating that they are covered substantially uniformly by the oily substance. Admitted. The edges of the pigment powder are also rounded in FIGS. 4 and 6 (sharp edges of the pigment are observed in FIGS. 3 and 5). The silk powder also has a puffy feel (there is no puffy taste in Figure 3).
It was confirmed from the above that these were substantially uniformly coated with an oily substance. Next, a comparative practical test was conducted on each of the powder foundations of Example 1 (Invention 1) and Reference Examples 1 to 3.
Table 1 shows the results of the survey conducted by 30 female panelists aged 25 to 35.

【table】

[Table] As shown above, the powder foundation (not molded) of the present invention adheres well to the skin, blends well, spreads well, provides a powdery finish, and can be layered. It is clear that it is extremely superior. Next, the powdered foundation of the present invention is molded into a cake shape using a molding machine in a conventional manner,
A cake-like foundation of the invention was obtained. This cake-like foundation is heated from 45℃ to -15℃.
As a result of being left in a constant temperature room for one year where the temperature was changed back and forth within the temperature range, it remained stable without any abnormalities, such as cracking, shrinkage (thinning), or changes. Next, a practical test was conducted using this cake-like foundation (invention 1) and cake-like foundations obtained by molding each of the powder foundations of Reference Examples 1 to 3 in the same manner as described above. The results obtained by humans are shown in Table 2.

【table】

[Table] (Note) How to use each sample: After preparing the base,
Stroke the surface of the sample cake with a sponge and spread it out while pressing.
Comparing the results in Table 1 and Table 2 above, it is clear that the powder foundation of the present invention is substantially effective even when used as it is or when molded into a cake shape. It has the same excellent makeup effect, spreads well on the skin, adheres well to the skin, provides a powdery finish, and has a moisturizing feeling that was thought to be almost impossible. It is possible to impart and express a moist feeling,
The specificity of the effects of the present invention is remarkable. Example 2 (When water-in-oil emulsion is used in the method of the present invention) 5 parts of sorbitan sesquiolate, 5 parts of beeswax
A molten mixture (80°C) consisting of 22 parts of liquid paraffin, 5 parts of lanolin, 5 parts of lanolin alcohol, and 5 parts of petrolatum was emulsified by mixing it with an aqueous solution (80°C) of 0.5 parts of Boushia dissolved in 52.5 parts of water. A water-in-oil emulsion was prepared. The procedure of Example 1 was repeated except that 60 parts of this emulsion, 100 parts of the powder mixture of Example 1, and 60 parts of ethanol were used, and the obtained powder foundation of the present invention had an oil-based 17.6% substance;
It contained 2.1% emulsifier. In addition, the surfaces of the powder base material, silk powder, and wool powder are substantially uniformly coated with the oily substance, and the cosmetic effect is almost as good as when using the oil-in-water emulsion of the present invention 1. It was hot. The results are shown in Table 3. The effectiveness in this case was judged by three specialized inspectors, and very good was marked with ◎, good with ○, somewhat poor with △, and very poor with ×.

[Table] Next, the powder foundation of Invention 2 was compression molded into a cake shape in the same manner as Invention 1. This cake-like foundation was left in the constant temperature room for one year as in the case of Invention 1, but it was found to be extremely stable without any abnormalities. Next, as a result of comparing the cosmetic effects of the cake-like foundation of the present invention 2 and the cake-like foundation of the present invention 1, almost no difference was observed. The results are shown in Table 4.

[Table] Example 3 A powder foundation was produced in the same manner as in Invention 1 of Example 1, except that various organic liquids shown in Table 5 were used instead of ethanol, and its cosmetic effect etc. Examined. The results are shown in Table 5.

[Table] As is clear from this result, among the water-miscible organic liquids that can be used in the present invention, ethanol, n-propanol, isopropanol, acetone, n-
Butanol and cellosolve are preferred.

[Table] Even in the case of cake-like foundations, ethanol, n-propanol, n-butanol,
Most preferred are isopropanol, cellosolve and acetone. Example 5 (When the powder base material is used after being immersed in alcohol in advance) The powder base material of Example 1 (the present invention) was immersed in ethanol (30°C) for 1 hour, and then separated from the alcohol. I took it out. A powder foundation was produced in the same manner as in Example 1, except that this pretreated powder base material was used. The uniformity of the coating layer (oil-based substance) on the surface of the base material of the obtained powder foundation was even better than that of the powder foundation of Example 1. In addition, the content of oily substances is 10.7%, and the content of emulsifiers is 1.2%.
It was %. As Comparative Example 1, the powder base material of Reference Example 1 was pretreated with ethanol in the same manner as in the present invention, and then treated in the same manner as in Reference Example 1 to produce a powder foundation. The surface coating of the obtained powder foundation was extremely non-uniform; Reference Example 1
There was no significant difference between this powder and the powder foundation. As Comparison-2, the powder base material of Reference Example 2 was pretreated with ethanol in the same manner as in the present invention, and then treated in the same manner as in Reference Example 2 to produce a powder foundation. The surface coating of the obtained powder foundation was extremely non-uniform, and no significant difference from that of the powder foundation of Reference Example 2 was observed. Furthermore, as comparison-3, reference example 3
The powder base material was pretreated with ethanol in the same manner as in the present invention. A powder foundation was produced in the same manner as in Reference Example 3. The surface coating of the obtained oil-based white powder was extremely non-uniform, and no significant difference was observed from that of the powder foundation of Reference Example 3. Next, a comparative practical test was conducted in the same manner as in Example 1. The results are shown in Table 7.

[Table] In this way, even if the powder base material is pretreated with ethanol (immersion treatment) and then coated with an oily substance, the methods of Comparisons 1 to 3 do not work in Reference Examples 1 to 3.
Similar to 3, uniform coating cannot be achieved and the practical effect is also inferior. However, pretreatment according to the method of the present invention further improves the uniformity of the surface coating,
In addition, the cosmetic effect in the practical test was significantly superior, and was slightly improved compared to the case of Example 1 without pretreatment, and the difference was sufficiently recognized. Example 6 The same procedure as in Example 1 was carried out for the powder-like foundation and cake-like foundation of the present invention except that two parts of organic dye Red No. 226 were added, and powder-like almost red color and cake-like almost red color were obtained. produced red. The content of oily substance in both of the obtained blushes was 12.3% and the content of emulsifier was 1.8%. Next, we similarly examined the storage stability of the cake-like blush, and found that no change was observed even after it was left for one year. In addition, as a result of observation with an electron microscope,
Powder-like substances (wool powder, silk powder, pigments) were coated with oily substances. Their cosmetic effects were extremely good as shown in Tables 8 and 9. Example 7 The powder foundation and cake foundation of the present invention in Example 1 were used, except that 8 parts of iron oxide and 2 parts of organic dye Blue No. 1 aluminum lake were used instead of 2 parts of iron oxide. Powder-like eyelid dough and cake-like eyelid dough were produced in the same manner as in the case of silon. The content of oily substances in both of the obtained eyelids was 1.7%, and the content of emulsifiers was 1.7%. Furthermore, the silk powder, wool powder, and pigment were uniformly coated with the oily substance. Next, the storage stability of the cake-like eyelid dough was examined in the same way, and no change was observed even after it was left for one year.

【table】

[Table] Comparative Example 1 A powder foundation and a cake foundation were produced in the same manner as in Example 1 of the present invention except that silk powder and wool powder were not used. As a result of observing both of the obtained foundations, as shown in FIG. 10, the pigment of the powder base material was almost uniformly covered with the oily substance. Next, in order to compare the powder foundation and cake foundation of the present invention in Example 1, a test was conducted on 30 women between the ages of 20 and 36. The results of the practical test are shown in Tables 10 and 11.

【table】

[Table] In this way, even in the method of the present invention in which pigments are coated with an oily substance by demulsification, the method in which silk powder and wool powder are further blended (the present invention) is better than the method in which they are not blended (Comparative Example 1). than,
It has been recognized that it is superior in terms of moisturizing effect, scent retention effect, feel when applied, and ability to be applied to a puff. However, how do you compare these two samples with the commercially available product? In response to the question, 23 out of 30 people answered that the product of Comparative Example 1 was also better than the commercially available product. Reference Example 4 (Additional study of the example in Patent No. 44304) After mixing 21 g of lanolin, 8 g of gum arabic, and 306 c.c. of water with stirring, further add 2.7 g of water and stir to form an aqueous emulsion of lanolin. Prepared. Next, while stirring this emulsion 2.7, add 375 g of zinc oxide (zinc white) and 75 g of talc (talc), continue stirring vigorously, and stop stirring when the upper liquid becomes transparent. The mixture was filtered, pressed, dehydrated, dried with hot air at 80-90°C and ground to obtain a lanolin-coated pigment. When particles of this lanolin-coated pigment were observed under an electron microscope (magnification: 4,400 times), it was found that the coating state of lanolin on the surface of talc and the surface of zinc oxide was extremely non-uniform. Next, this lanolin-coated pigment was compression molded into a cake shape by a conventional method to obtain a cake-like oily white powder. A practical test of this cake-like oily white powder was conducted by three specialized inspectors. As a result, the removal of the cake from the puff (application tool), the finish of the makeup,
Adhesion to the skin, blendability to the skin, and spread on the skin were all somewhat poor (△), and it was impossible to apply over the skin, which was very poor (x). Reference Example 5 (When silk powder and wool powder are mixed and used in the example of Patent No. 44304) Furthermore, 22.5 g of silk powder and wool powder are used.
A mixture consisting of lanolin-coated pigment, lanolin-coated silk powder and lanolin-coated wool powder was obtained in the same manner as in Reference Example 4, except that 22.5 g of lanolin aqueous emulsion was added and mixed. When this mixture was observed under an electron microscope, it was found that the surfaces of the silk powder, wool powder, zinc oxide, and talc were coated with lanolin extremely nonuniformly. Next, the above lanolin-coated powder was formed into a cake shape by a conventional method to obtain a cake-like oily powder. A practical test of this cake-like oily white powder was conducted by three specialized inspectors. As a result, the removal of the cake from the puff, the finish of the makeup, the adhesion to the skin,
The adhesion to the skin, spreadability on the skin, and moisturizing properties (moisture feeling) were all somewhat poor (△), and very poor (x) as it was impossible to recoat the skin. Example 8 Aqueous emulsion of lanolin in Reference Example 4, zinc oxide, talc, and 22.5 g of silk powder
After adding and dispersing wool powder, ethyl alcohol 1 was gradually added and mixed over 10 minutes to demulsify the emulsion, and the following steps were carried out in the same manner as in Reference Example 4. hand,
An oily white powder of the present invention was obtained. When particles of this oily white powder were observed under an electron microscope (magnification: 4,400 times), it was found that the lanolin coating on each surface of silk powder, wool powder, zinc oxide, and talc was extremely uniform. Next, this oily white powder was compression molded into a cake shape by a conventional method to obtain a cake-like oily white powder. A practical test of this cake-like oily white powder was conducted by three specialized inspectors. As a result, the removal from the cake to the puff, makeup finish, adhesion to the skin, blending into the skin, spreadability on the skin, and moisturizing properties (moisture feeling) were all extremely good (◎).
It was possible to apply the product over the skin and the result was extremely good (◎).

[Brief explanation of the drawing]

1, 3, and 5 are electron micrographs showing the surface condition (500 times magnification) of the powdery substance mixture (before treatment) used in Example 1; Figure 3 shows the state of wool powder and pigment, Figure 3 shows the state of silk powder and pigment, and Figure 5 shows the state of wool powder, silk powder, and pigment. Figures 2, 4 and 6 are electron micrographs showing the surface condition (500x magnification) of the powder foundation obtained in Example 1, and Figure 2 shows the surface condition of the powder foundation obtained in Example 1. The state of coated wool powder and pigment, Figure 4 shows the state of wool powder and pigment coated with oily substance, Figure 6
The figure shows wool powder, silk powder, and pigment coated with an oily substance.
FIG. 7 is an electron micrograph showing the surface condition of the mixture of silk powder and pigment used in Reference Example 3 (magnified 500 times). Figure 8 shows the surface condition of the powder foundation obtained in Reference Example 3 (magnified 500 times), and shows an electron microscope showing that the oily substance is non-uniformly attached to the pigment and silk powder. It's a photo. Figure 9 shows the surface condition of the pigment used in Comparative Example 1 (enlarged 500 times).
This is an electron micrograph showing. FIG. 10 is an electron micrograph showing the surface state of the powder foundation obtained in Comparative Example 1 (magnified 500 times) and also showing the state of the pigment coated with the oily substance.

Claims (1)

[Claims] 1. After mixing an aqueous emulsion of an oily substance, silk powder, wool powder, inorganic powder, or even an organic pigment, a water-miscible organic liquid is added thereto under stirring to demulsify the aqueous emulsion, After that, the coagulates generated by demulsification are
A method for producing an oil-based powder makeup material, which is characterized in that it is separated from a liquid and then dried.