JP6886672B1 - Manufacturing method of effervescent cosmetics - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an effervescent cosmetic which is one agent excellent in transdermal absorption performance of carbon dioxide, moisture proofing property, water solubility and economy. SOLUTION: The thickness is 5 mm or less and the hardness is 4 containing at least one organic acid of citric acid, fumaric acid, malic acid and succinic acid, sodium hydrogen carbonate and polyethylene glycol having an average molecular weight of 2000 or more and 8000 or less. It is a molded product of .9N or more and 235.4N or less, and 0.7 parts by weight to 1.5 parts by weight of sodium hydrogen carbonate and 0.08 parts by weight to 0.20 parts by weight of polyethylene glycol with respect to 1 part by weight of organic acid. Effervescent cosmetics containing parts by weight were used. [Selection diagram] Fig. 1

Description

The present invention relates to a method for producing an effervescent cosmetic product having excellent percutaneous absorption performance of carbon dioxide.

Free carbon dioxide (HCO 3 _- in the state of ^the bicarbonate ion, carbon dioxide components dissolved in water) to bathe carbonated spring containing carbonate components in the carbonated spring acts on the capillaries under the skin It is widely known that by dilating the capillaries and improving blood circulation, the bathers can recover from fatigue and improve their health. In order to utilize this property, an attempt has been made to dissolve an organic acid and a bicarbonate ion-containing solid agent at the time of bathing and use it as an artificial carbonated spring developed for general household use (Non-Patent Document 1).

Cosmetics to which the above effects are applied include a first agent containing at least one of an organic acid and an inorganic acid and a second agent containing a carbonate, and the first agent and the second agent are mixed to form carbon dioxide. A cosmetic for scalp massage that generates carbon, at least one of the first agent and the second agent is an emulsion containing a higher alcohol having 10 to 30 carbon atoms and a nonionic surfactant, and is described above. There is a cosmetic for scalp massage having a pH of 4.0 to 8.0 and a viscosity of 3000 to 50000 mPa · s after mixing the first agent and the second agent (Patent Document 1).

Further, 1/50 to 1/5 of polyethylene glycol was added to bicarbonate (sodium hydrogen carbonate or potassium hydrogen carbonate), and organic acid and polyethylene were added to the granulated product A granulated by the fluidized layer granulator. There is a tablet characterized by having a tablet hardness of 15 kg (f) (147.1 N) or more in a tablet obtained by mixing and compression-molding a mixture B of glycol in an amount ratio of 1/20 to 1/3. (Patent Document 2).

Further, there is a briquette-shaped solid bath agent using organic acids and carbonates as raw materials for the purpose of similar effects to the above (Patent Document 3).

Japanese Unexamined Patent Publication No. 2017-14172 Japanese Unexamined Patent Publication No. 2013-245218 Japanese Unexamined Patent Publication No. 2007-51117

Man Hidenori et al., Research on artificial carbonated spring baths (1st report) On the effective carbonic acid concentration of carbonated springs, Journal of the Japanese Society of Hot Spring Climate Physics, Vol. 47, No. 3, 4, May 1984

However, in the technique of Patent Document 1, the viscosity of the mixture of the first agent and the second agent is as high as 3000 mPa · S to 5000 mPa · S, and the fluidity of the mixture is poor, so that the transdermal absorption efficiency of carbon dioxide gas is high. I had the problem of being bad.

Further, in the technique described in Patent Document 2, when an attempt is made to wash the face by dissolving it in a small amount of tap water before use, it is not completely dissolved in tap water at 35 ° C. or lower (body temperature or lower) and is an insoluble matter. Will remain. Therefore, there is a problem that the original purpose of removing stains on the face (especially old keratin) by washing the face while promoting blood circulation of the face and recovering the skin condition by promoting metabolism cannot be fully exerted. Had.

Further, in order to produce a briquette-shaped solid bath agent by using the technique described in Patent Document 3, it is necessary to pressurize a plurality of raw materials, and in that case, heat is generated due to pressure and friction of the mixed material. To do. On the other hand, raw materials (particularly water-soluble raw materials and substances having water of crystallization) contain some water, and therefore, when pressurized, a part of the solid raw material is liquefied by the water in the raw materials, and an organic acid is used. In some cases, a neutralization reaction with carbonate occurs and the quality of the briquette is deteriorated, or the shape of the briquette solid agent cannot be maintained and the briquette may collapse. Furthermore, at the time of use, when the water is dissolved, the balance between the organic acid and the carbonate is different, the amount of carbon dioxide dissolved in the aqueous solution is not stable, and a problem arises in terms of quality.

For the above reasons, it is difficult to form a molded product containing organic acids and carbonates as main components with one agent such as tablets. Therefore, in order to provide it easily, the two agents shown in Patent Document 1 are used. This had to be done, and there were problems such as complicated packaging and storage. Further, at the time of manufacturing, since the current amount of adhesion occurs, a special briquette device is required, which has a problem that the manufacturing cost becomes high.

The present invention has been made to solve the above problems, and provides a method for producing an effervescent cosmetic product, which is an agent and is excellent in transdermal absorption performance of carbon dioxide, moisture proofing property, water solubility and economy. The purpose is to do.

In order to achieve the above object, the present invention comprises at least one organic acid of citric acid, fumaric acid, malic acid and succinic acid, sodium hydrogen carbonate and an average molecular weight of 2000 or more and 8000 or less (preferably 4000 to 4000). A thickness of 5 mm or less, a hardness of 4.9 N (0.5 kgf) or more and 235.4 N (24.0 kgf) or less (preferably 9.8 N) containing polyethylene glycol of 6000) and sodium n-octansulphonate. It is a molded product of (1.0 kgf) or more and less than 147.1 N (15.0 kgf)), and 0.7 parts by weight to 1.5 parts by weight of the sodium hydrogen carbonate and 0.7 parts by weight of the sodium hydrogen carbonate with respect to 1 part by weight of the organic acid. polyethylene glycol with each containing 0.08 parts by weight to 0.20 parts by weight, foaming is coating of the polyethylene glycol is formed in the surface layer cosmetics (hereinafter sometimes referred to as "the foamable cosmetic" .) Ri manufacturing method der of the above organic acid, and sodium the bicarbonate, and the polyethylene glycol, the n- octane sulfonic von sodium were mixed and stirred, followed by the feature that formed as the shaped body It provides a method for producing effervescent cosmetics.

The effervescent cosmetics need to contain at least one organic acid of citric acid, fumaric acid, malic acid and succinic acid. In this case, citric acid is particularly preferable because it has a particularly high chelating effect in organic acids and has a remarkably good effect of dissolving old keratin of the skin when carbon dioxide gas is transdermally absorbed. ..

The hardness is a value measured by a method similar to the hardness test of tablets, and uses a specimen molded into a predetermined shape (diameter 5 mm × maximum thickness 4 mm) in the thickness direction (height direction of the specimen). ) Is applied with a compressive force in a uniaxial state, and is the value of the compressive force (compressive fracture strength) when the specimen is compressed and fractured (unit: N). Further, the hardness can be measured by a general hardness tester (for example, a hardness tester using an altimeter strain gauge type load cell used in the examples).

Further, the molded product may have a briquette shape, a tablet shape, or the like, regardless of its shape, but it is preferable to have a briquette shape from the viewpoint of hardness and productivity.

This effervescent cosmetic is formed by molding an organic acid, sodium hydrogen carbonate and an appropriate amount of polyethylene glycol in the above mixing ratio, so that when the raw material is pressed during molding, it is applied to the surface layer of the pressurized body. Polyethylene glycol oozes out and covers the surface layer portion. Therefore, heat generation can be prevented by solidifying while the surface temperature is lowered, and friction between the organic acid and the carbonate can be prevented, and the neutralization reaction between the two can be suppressed. Therefore, the moisture proof property can be improved, and a single effervescent cosmetic product having excellent storage stability can be obtained.

Further, by setting the blending ratio as described above, the action of the water-soluble polyethylene glycol makes it possible to easily obtain an aqueous solution having a concentration of 1000 ppm or more, which corresponds to a carbonated spring having a medical medical effect, even at a low temperature.

Further, in the present effervescent cosmetics, 0.1 parts by weight to 1.0 parts by weight (more preferably 0.3 parts by weight to 0. parts by weight) of the anti-adhesion agent with respect to 100 parts by weight of the total amount of the effervescent cosmetics. 6 parts by weight) It is preferable to contain it.

Among the surfactants, the above-mentioned adhesion inhibitor has ease of handling (easy to grind and can be made into fine particles), good mixing performance, low foamability, and safety. At least one of the compounds of sodium n-octanesulfonate, sodium n-hexanesulphonate, sodium tetradecensulfonate, and sucrose fatty acid ester is mixed alone or in combination. It is preferable to use it. In particular, it is preferable to use sodium n-octanesulfonate and sodium n-hexanesulfonate.

According to the present effervescent cosmetics, it is possible to prevent the composition from adhering to the molding apparatus at the time of molding by the action of the anti-adhesion agent, and it is possible to improve productivity and economy.

Further, by blending this effervescent cosmetic, it is possible to easily set the brightness (L *) to 80 or more and the saturation (C *) to 10.0 or less, and the surface layer portion is coated with polyethylene glycol. It is suitable because the aesthetic appearance can be easily improved because the molded product can be formed without any shape.

The lightness (L *) and saturation (C *) are values quantitatively specified as the coordinates of the L * a * b * color space chromaticity diagram defined in "JIS Z8781-4". ..
C * = √ {(a *) ² + (b *) ² }
a *: Saturation that is a component in the direction of magenta and blue-green b *: Saturation that is a component in the direction of yellow and blue

According to the present invention, it is possible to provide a method for producing an effervescent cosmetic product, which is an agent and has excellent percutaneous absorption performance of carbon dioxide, moisture resistance, water solubility and economy.

(A) is a drawing substitute photograph showing an example of a molded body of an effervescent cosmetic produced according to the present invention, and (b) is a drawing substitute photograph showing an example of a molded body of an effervescent cosmetic of a comparative example. ..

Hereinafter, a preferred embodiment of the present invention will be described in detail. However, the embodiments of the present invention are not limited to the illustrated embodiments.

[Basic concept of this effervescent cosmetics]
When free carbonic acid is dissolved in water, it has an equilibrium reaction shown in Reaction Scheme 1 below.
This equilibrium reaction will be affected by pH, but the more alkaline the aqueous solution, the more free carbonic acid can be retained in the aqueous solution. However, in the state of free carbonic acid, it is difficult to be absorbed transdermally, and it is difficult to obtain the same effect as natural carbonated spring.

[Reaction formula 1]

The mechanism of percutaneous absorption is that free carbon dioxide is converted to carbon dioxide in the vicinity of the barrier layer (hereinafter referred to as "skin barrier layer") in human skin, which is acidic (pH less than 7), and the carbon dioxide is absorbed. (The carbon dioxide that can be absorbed transdermally is the carbon dioxide generated by the change of free carbon dioxide in the vicinity of the skin barrier layer. This is present in the air. It can be understood empirically in view of the fact that carbon dioxide is difficult to be absorbed through the skin).

Under the above premise, the present inventor prepares a molded product by changing the blending ratio of the constituent materials, and repeats an experiment for confirming the change in the properties thereof, thereby appropriately deteriorating the molded product even when the molded product is formed. We have found a blending ratio that can prevent this, and have developed this effervescent cosmetics.

[Constituents of this effervescent cosmetics, etc.]
This effervescent cosmetics achieves the above object by containing an organic acid, sodium hydrogen carbonate, polyethylene glycol, and an adhesion inhibitor as main constituent materials (constituent substances). The constituent materials and the like will be described in detail below.

(1) Organic acid and sodium hydrogen carbonate Organic acid plays a role of neutralizing sodium hydrogen carbonate and effectively causing foaming of carbon dioxide, and when it is water-soluble, it has a cleaning effect on the skin and flexibility of the skin. It is a component for exerting a role of exerting an effect of retaining the above, and one or more kinds of substances of citric acid, fumaric acid, malic acid and succinic acid can be used.
Although the beauty effect and the like differ depending on the type of organic acid, citric acid is most suitable because it has remarkably large reactivity and high foaming performance as compared with other organic acids.

(2) Polyethylene glycol As is known, polyethylene glycol is a substance obtained by polymerizing ethylene oxide, and is a substance having water solubility, non-volatility and viscosity. The function of this substance in this effervescent cosmetics is to promote the dissolution of sodium hydrogen carbonate in water, as well as the binder that binds the constituent materials such as organic acid and sodium hydrogen carbonate, the coating of the surface layer of the molded product. It plays an important role such as the action of making it.

That is, polyethylene glycol is fine particles at the time of mixing, but when pressurized, a part of the polyethylene glycol becomes a liquid and exudes to the surface layer portion of the molded product to become an individual, and a coating film is formed on the surface layer portion to improve moisture resistance. Has an action.

Further, in the above process, depending on the pressing force and the blending amount, a part of the mixture moves inside the molded product and adheres to the surface layer of sodium hydrogen carbonate, so that the organic acid and sodium hydrogen carbonate come into direct contact with each other. Has the effect of preventing. At this time, the larger the amount of polyethylene glycol and the higher the adhesion to sodium hydrogen carbonate (the adhesion in both substances shifts from point adhesion to surface adhesion), due to the action of the water-soluble polyethylene glycol. , Sodium hydrogen carbonate becomes easily soluble in water.

The degree of action of the polyethylene glycol varies depending on the pressing force and the content. That is, when the content of the substance is small, the coating film cannot be sufficiently formed. However, when the content is excessive and the pressing force is large (when the hardness of the molded product exceeds 235.4 N (24.0 kgf)), the coating film becomes too thick, which hinders the solubility during use. , It becomes impossible to prepare an aqueous solution having the concentration required to achieve the expected effect.
Further, even when the content of polyethylene glycol is desired, when the pressing force is small (the hardness of the molded product is less than 4.9 N (0.5 kgf)), the alteration of polyethylene glycol is small, so that the polyethylene glycol flows. Will not.

In view of the above, in this effervescent cosmetics, in order to exert a predetermined effect, the blending ratio of polyethylene glycol is not excessive or insufficient, and the predetermined pressure (hardness of the molded product is 4.9 N (0.5 kgf) or more) at the time of molding. It is necessary to set it to 235.4 N (24.0 kgf or less) (preferably 9.8 N (1.0 kgf) or more and less than 147.1 N (15.0 kgf)).

Furthermore, polyethylene glycol has an average molecular weight of 2000 or more (particularly preferably 4000) in consideration of water solubility, functionality as a binder, ease of handling during molding, and adhesion to equipment (viscosity, etc.). It is preferable that the amount is 6000 or less.) It is preferable to use a substance of 8000 or less.

(3) Anti-adhesion agent The anti-adhesion agent is a material added to prevent the mixed material from adhering to the molding apparatus during molding. Compounds of sodium n-octanesulfonate, sodium n-hexanesulphonate, sodium tetradecencefurfonate and sucrose fatty acid ester, considering ease of handling, pulverizability, low foaming property, safety and economy. It is preferable to use at least one of them alone or in combination of two or more, and in particular, it is preferable to use sodium n-octanesulphonate and sodium n-hexanesulfonate.

(4) Other constituent materials Thickeners (hyaluronic acid, sodium hyaluronate, collagens, glycerin, etc.) and antioxidants (L) that are widely used in cosmetics as long as they do not interfere with the function of this effervescent cosmetics. -In addition to ascorbic acid, L-ascorbic acid salt, L-ascorbic acid derivative, erythorbic acid, erythorbic acid salt, L-isoascorbic acid and L-isoascorbic acid) and other various additives, fragrances, pigments, etc. are added. can do.

(5) Mixing ratio, etc. This effervescent cosmetic has a thickness of 5 mm or less and a hardness of 4.9 N (0.5 kgf) or more and 235.4 N (24.0 kgf) or less (preferably 9.8 N (1.)). It is necessary to form a molded product such as a briquette or tablet having a hardness of 0 kgf) or more and less than 147.1 N (15.0 kgf) (for hardness, refer to the description of means for solving the problem). This is due to the pressure at the time of molding acting on the molded product having a thickness of 5 mm or less, which is required to reduce the hardness of the molded product to 4.9 N (0.5 kgf) or more and 235.4 N (24.0 kgf) or less. As a result of verifying the optimum ratio between the amount of converted heat energy and the amount of polyethylene glycol that melts as described above, the following compounding ratio was successfully detected.

In order to obtain the effect of the effervescent cosmetics, 0.7 parts by weight to 1.5 parts by weight of the sodium hydrogen carbonate and 0.08 parts by weight to 0 parts by weight of the polyethylene glycol with respect to 1 part by weight of the organic acid. It is necessary to make the blending ratio so as to be 20 parts by weight.

In addition, 0.1 weight by weight of at least one of sodium n-octanesulphonate, sodium n-hexanesulphonate, sodium tetradecenesulfonate and sucrose fatty acid ester with respect to 100 parts by weight of the total amount of effervescent cosmetics. It is necessary to contain from 10 parts by weight to 1.0 part by weight.

When the above mixing ratio is used, the total amount of carbonic acid (total amount of hydrogen carbonate ion, carbonate ion and free carbon dioxide) can be set to a concentration of 1000 ppm or more, which corresponds to a carbonated spring having a medical effect.
In this effervescent cosmetic, a known pH adjuster or the like is used so that the pH becomes pH = 5.0 to pH = 6.8 (preferably pH = 5.5 to pH = 6.5) when in water. Although it is necessary to adjust by adding, it is preferable to use sodium carbonate (anhydrous sodium carbonate) as the pH adjuster.

(6) Brightness and Saturation In the case of the above blending ratio, the brightness index (L *) is 80 or more and 100 or less, the saturation index (C *) is 10.0 or less, and the color is not colored by another colorant or the like. Yellow and blue are the strongest shades (for lightness and saturation, see the description of the means for solving the problem).

FIG. 1 (a) shows a molded product of the present effervescent cosmetic (with respect to 1 part by weight of citric acid, 1.2 parts by weight of the above sodium hydrogen carbonate and 0.12 parts by weight of polyethylene glycol were contained, and the hardness was 63. It is a drawing substitute photograph showing an example of 7N (6.5 kgf)) (hereinafter, referred to as “target molded body”), and is a molded body (target molding) of a comparative example of foamable cosmetic shown in FIG. Compared with (the one in which only polyethylene glycol is removed from the composition of the body), the gloss of the surface layer portion can be visually recognized.
As described above, according to the present effervescent cosmetics, the surface layer portion is coated with polyethylene glycol to obtain a molded product having no unevenness.

[Manufacturing method of this effervescent cosmetics]
The present effervescent cosmetics can be produced by mixing the above-mentioned constituent materials and shaping them into a desired shape, thickness and the above-mentioned hardness by a known mixing device, a molding device (bricker device) or the like.

For example, a mixing device in which a rotatable plow-shaped excavator is arranged in a horizontal drum and a pair of roll mechanisms, each of which is rotatable, are provided, and a mixing device is provided between the roll mechanisms. By supplying the mixed material from the above, it is possible to use a molding device that pressurizes the mixed material and forms it into a briquette shape so as to have a predetermined shape.

Using this molding device, the total amount of sodium hydrogen carbonate and 30% by weight to 40% by weight of polyethylene glycol with respect to the total amount are put into the mixing portion, and the material is subjected to centrifugal diffusion and vortex action to cause a three-dimensional flow. Mix and stir well. Next, the total amount of the organic acid, the remaining amount of polyethylene glycol, and other raw materials excluding the adhesion inhibitor are added to the mixture, and the mixture is sufficiently mixed by the same method as described above. Finally, an anti-adhesion agent is added and mixed well.

Subsequently, the mixed material is sent to the roll mechanism of the molding apparatus to be molded into a desired shape. By adjusting at least one of the supply speed of the mixed material from the mixing device to the molding device (roll mechanism) and the rotation speed of the roll mechanism, a molded product having a desired thickness, shape and hardness can be formed.

[Action and effect of the present invention]
According to this effervescent cosmetics, when the constituent materials are pressurized during molding by adding the above-mentioned appropriate amount of polyethylene glycol to organic acid and sodium hydrogen carbonate, the polyethylene glycol melts due to heat generated by compression energy. Then, the polyethylene glycol exudes to the surface layer portion of the pressurized body, and the surface layer portion is coated (a coating film is formed). This makes it possible to prevent friction between the organic acid and sodium hydrogen carbonate, suppress the neutralization reaction between the two, and prevent heat generation by solidifying while lowering the surface temperature. Therefore, the moisture proof property can be improved, and a single agent can be used as an effervescent cosmetic product having excellent storage stability.

Further, according to this effervescent cosmetic, it is more effective to use it in hot water having a body temperature of 36 ° C. or higher, but by adding the above-mentioned appropriate amount of polyethylene glycol having water solubility, the water solubility at low temperature can be improved. Can be improved. Therefore, even at a low temperature, an aqueous solution having a concentration of 1000 ppm or more, which corresponds to a carbonated spring having a medical medical effect, can be obtained.

Further, the hardness of the effervescent cosmetic is 4.9 N (0.5 kgf) or more and 235.4 N (24.0 kgf) or less (preferably 9.8 N (1.0 kgf) or more and less than 147.1 N (15.0 kgf)). By setting the concentration to free carbon, the neutralization reaction rate of the organic acid and sodium hydrogen carbonate generated when the molded product is dissolved can be appropriately controlled, and the blood flow improving effect can be effectively exhibited. it can.

Further, since an adhesion inhibitor containing at least one compound of sodium n-octanesulfonate, sodium n-hexanesulfonate, sodium tetradecenesulfonate and sucrose fatty acid ester is mixed, the molding apparatus is used at the time of molding. It is possible to prevent the composition from adhering to the sodium, and it is possible to improve productivity and economic efficiency.

Further, by blending this effervescent cosmetic product, a molded product having a brightness index (L *) of 80 or more and a saturation index (C *) of 10.0 or less and having a surface layer portion coated with polyethylene glycol should be formed without unevenness. Therefore, the aesthetic feeling can be easily improved.

Although an example of a preferred embodiment of the present invention has been described above, the present invention is not limited to the embodiment, and the design can be appropriately changed without departing from the spirit of the present invention. It may contain various other additives widely used in cosmetics as long as the function is not impaired. In addition, there are no restrictions on the shape of the effervescent cosmetics. Further, the manufacturing method does not ask the type of the molding apparatus, and may include other appropriate steps.

Hereinafter, the effects of the effervescent cosmetics will be verified while further showing examples. In the following description, the same test piece will be given the same number and the same material will be given the same name, and duplicate explanations will be omitted.

<Preparation of test specimen (common to each example)>
Before the detailed explanation, the method of preparing the test piece used in each example will be described.

(1) Step 1
200 kg of sodium hydrogen carbonate and 12 kg of polyethylene glycol (average molecular weight 6000) are added to a mixing device (Ladyge Mixer Ladyge Mixer VT1200 type manufactured by Matsubo Co., Ltd.), and the mixture is stirred and mixed at a rotation speed of 115 rpm for 10 minutes.

(2) Step 2
After completion of step 1, 200 kg of anhydrous citric acid, 17 kg of anhydrous sodium carbonate and 11 kg of polyethylene glycol are added, and the mixture is stirred and mixed at a rotation speed of 115 rpm for 10 minutes.

(3) Step 3
After the completion of step 2, 2 kg of sodium n-octanesulfonate is added, and the mixture is stirred and mixed at 115 rpm for 2 minutes to prepare a mixed material.

(4) Step 4
The mixed material prepared in step 3 is supplied to a molding apparatus (Bricketta BSS-IH, a roll-type high-pressure granulator manufactured by Shinto Kogyo Co., Ltd.), and has a tablet shape having a diameter of 5 mm, a thickness of 4 mm, and a weight of 0.1 g. A briquette-shaped test piece having a predetermined hardness is formed (in the following description, for convenience, the units of hardness are N and kgf together (however, the values in the upper part of the table are N notation, and the values in parentheses). Is in kgf notation)).

The hardness of the standard test piece (No. 1-1 below and each test piece of Examples 2 to 7 below) in which the hardness was not a variable was set to 63.7 N (6.5 kgf).
The hardness was measured in the thickness direction of 10 test pieces using a hardness tester (DC-200 manufactured by Okada Seiko Co., Ltd.) in an environment of room temperature 23 ° C ± 3 ° C and relative humidity 40%. , The arithmetic mean of eight test specimens with the maximum and minimum values removed.

The pH of the aqueous solution in the following reference test body (No1-1) is 5.60 when 150 of them are dissolved in 1 liter of tap water (25 ° C.).

<First Example> [Dampproof performance confirmation test]
A moisture-proof performance confirmation test was conducted to confirm the moisture-proof performance, which is one of the effects of this effervescent cosmetic.
That is, test specimens having different amounts of sodium hydrogen carbonate, polyethylene glycol, and hardness with respect to citric acid were prepared, and 150 of each test specimen was placed in a commercially available aluminum bag and sealed. Then, it was placed in a constant temperature bath at 40 ° C., and the volume change rate of each test piece was measured immediately after sealing and one week after sealing. Further, the lightness (L *) and saturation (C *) of the test piece were measured with a colorimeter (M200QC manufactured by X-rite).

[Volume change rate]
Volume change rate (%) = (volume one week after sealing-volume immediately after sealing)
× 100 / Volume immediately after sealing

According to the results (Tables 1 and 2), the volume of the test specimens not covered by the effervescent cosmetics changed, but the test specimens having a blending ratio satisfying the effervescent cosmetics (hereinafter, "the effervescent cosmetics"). No volume change occurred (0%) in "Cosmetic test specimens" (indicated by "○" in the table). Since the volume change is caused by the neutralization reaction of citric acid and sodium hydrogen carbonate, it was confirmed that the test piece of this effervescent cosmetic had good storage performance without the neutralization reaction.

Further, the test body of this effervescent cosmetic is molded so that the hardness is 4.9 N (0.5 kgf) or more, so that the lightness (L *) is 80 or more and the saturation (C *) is 10 or less. became. During molding, due to the action of molding pressure, polyethylene glycol in the mixed material melts in the molded body, is discharged to the surface layer and solidifies, and a coating film is formed, thereby increasing the brightness and saturation. Along with the change, it was confirmed that the surface layer portion was coated with polyethylene glycol to form an outer shape without unevenness.

On the other hand, it was also clarified that when the ratio of citric acid and polyethylene glycol does not satisfy the formulation or hardness of the present effervescent cosmetics, the polyethylene glycol does not work effectively.

<Second Example> [Dissolution Performance Confirmation Test]
A dissolution performance confirmation test was conducted to confirm the dissolution performance, which is one of the effects of this effervescent cosmetic.
That is, the time required to prepare test specimens in which the amounts of sodium hydrogen carbonate and polyethylene glycol with respect to citric acid were changed, and to dissolve 150 of the prepared test specimens in 1 liter of tap water (water temperature 20 ° C.) (hereinafter referred to as). , "Dissolution time") was measured.

According to this result (Table 3), in the test specimen in which the compounding ratio of polyethylene glycol to the organic acid is not the subject of the present effervescent cosmetics invention, it takes a long time (283 seconds or more) to dissolve in tap water. In order to dissolve it in tap water quickly (within 180 seconds), it was confirmed that the mixing ratio of the organic acid and sodium hydrogen carbonate should be within the range of this effervescent cosmetic.
In particular, when the mixing ratio of polyethylene glycol to 1 part by weight of citric acid is as small as 0.8 or less, the absolute amount is insufficient, and when it exceeds 0,20, the coating film becomes thick. It was confirmed that both were dissolved in tap water for a long time.

<Third Example> [Blood circulation improvement effect confirmation test]
In order to confirm the effect of improving blood circulation, etc. by bathing, which is one of the effects of this effervescent cosmetic, a blood circulation improvement effect confirmation test was conducted.
That is, test specimens in which the amounts of sodium hydrogen carbonate and polyethylene glycol with respect to citric acid were changed were prepared, and the subjects were bathed in 160 liters of warm water (water temperature 40 ° C.) in which 450 of the prepared test specimens were dissolved, and carbon dioxide was added. The improvement status of blood circulation, etc. was measured.

In this study, 10 subjects (average age 40.5 years, women aged 25 to 60 years) were targeted at (1) immediately before bathing (TB), (2) immediately after bathing (TA), and (3) bathing 1 The epidermis temperature of the right instep after time (TA') was measured, and the amount of temperature change immediately after bathing and the amount of temperature change after 1 hour were calculated. Then, the average value of the temperature change amount immediately after bathing and the temperature change amount after 1 hour of the subject is calculated, and the evaluation index [temperature change value immediately after bathing (T1)] of the temperature change immediately after bathing and the temperature change after 1 hour have passed. [Temperature change value (T2) after 1 hour] was used as the evaluation index of.

The bathing time was 20 minutes, and the subjects spent a resting state in a room maintained at 25 ° C. after bathing. The epidermis temperature was measured using (Non-contact infrared thermometer T0-400 manufactured by Doritech Co., Ltd.).

[Temperature change value]
T1 = Σi {TA (i) -TB (i)} / 10
T2 = Σi {TA'(i) -TA (i)} / 10
T1: Temperature change value (° C) immediately after bathing
T2: Temperature change value (° C) after 1 hour
TB (i): Epidermis temperature (° C.) of the right instep immediately before bathing of subject i
TA (i): Epidermis temperature (° C.) of the right instep immediately after bathing of subject i
TA'(i): Epidermis temperature (° C.) of the right instep after 1 hour of bathing of subject i
Σi: Indicates that the arithmetic sum of 10 subjects (i = 1 to 10) is to be obtained.

According to this result (Table 4), the test body of this effervescent cosmetic (indicated by ○ in the table) has a body temperature increasing effect that the body temperature rises by 1.0 ° C or more after bathing, and also takes a bath. It is recognized that the heat retention effect that the decrease in body temperature is 0.3 ° C. or less is maintained even after 1 hour has passed. On the other hand, in the test specimens having a composition that does not satisfy this effervescent cosmetics, the increase in body temperature was as low as 0.7 ° C or less even after bathing, and a decrease in body temperature of 0.6 ° C or more was observed 1 hour after bathing. Be done. As described above, it was confirmed that this effervescent cosmetic has the effect of improving blood flow and increasing body temperature by transdermal absorption of carbon dioxide.

<Fourth Example> [Whitening effect confirmation test]
A whitening effect confirmation test was conducted to confirm the whitening effect, which is one of the effects of this effervescent cosmetic.
That is, 1 liter of tap water (water temperature 20 ° C.) in which 150 test specimens prepared by preparing test specimens in which the amounts of sodium hydrogen carbonate and polyethylene glycol with respect to citric acid were changed was prepared (hereinafter, "face wash water"). ) Was used to measure the skin condition when the subject was allowed to wash his face.

In this test, 10 subjects (average age 40.5 years old, women aged 25 to 60 years old), the same as in the third example, were asked to wash their face 20 times with both hands every morning using the above facial cleansing water. The skin condition was measured immediately after the final face wash.
For the skin condition, attach it to a smartphone and take a picture of the skin condition using a lens (manufactured by Maxell Smart Communications Co., Ltd., skin lens "Memore") that can take high-quality images of the texture and stains of the skin condition. The transparent skin area was measured by numerically analyzing the image, and the transparency (%) was calculated based on the following formula.
Transparency (%) = (transparent skin area without dullness / total skin area) x 100

Then, using the calculated transparency, the whitening degree (lowest evaluation 1 to highest evaluation 5) is defined based on the following five evaluation criteria (Table 5), and when the evaluation is 3 or more, the predetermined effect (whitening) is achieved. It was judged to have the effect).

According to this result (Table 6), the whitening effect (evaluation 3 or higher) was obtained by washing the face using face-washing water in which the test body of this effervescent cosmetic (indicated by ○ in the table) was dissolved. It became clear that there is. From this, it was confirmed that the carbon dioxide generated during the dissolution of the test body of this effervescent cosmetic was transdermally absorbed to improve the blood flow and promote the metabolism of the skin.

<Fifth Example>"Whitening effect confirmation test by different types of organic acids"
In order to demonstrate the whitening effect of this effervescent cosmetic by the difference in the type of organic acid, citric acid (No1-1), fumaric acid (No5-1), malic acid (No5-2), succinic acid as organic acids Four types of test specimens were prepared using (No. 5-3), respectively, and the same whitening effect confirmation test as in the fourth example was performed.

According to this result (Table 7), in the test body (No1-1) using citric acid as the fixed-term acid, the whitening degree was the highest evaluation 5, and fumaric acid (No5-1) and malic acid (No5-2). It was clarified that the effect was very high as compared with the evaluation 4 of No. 4 and the evaluation 3 of succinic acid (No5-3).
From this, it was demonstrated that citric acid has a high effect of dissolving and removing old keratin of the skin, and that more carbon dioxide is percutaneously absorbed, thereby having an effect of improving blood flow and an effect of maintaining heat retention.

<Sixth Example>"Effect Confirmation Test on Molding Rate by Anti-Adhesion Agent"
Sodium n-octanesulphonate (No. 1) was used as an anti-adhesion agent in order to demonstrate the effect of preventing the adhesion of the mixed material from adhering to the molding apparatus during molding due to the presence or absence of the anti-adhesion agent and the difference in the target substance of the anti-adhesion agent. -1), sodium n-hexanesulfonate (No6-1), sodium tetradecensulfonate (No6-2), sucrose fatty acid ester (No6-3), and no anti-adhesion agent added (No6-4) , And this confirmation test was conducted.

That is, when the molding apparatus (see step 4) was continuously operated for 24 hours to prepare each test piece, the total weight of the test piece with respect to the total weight of the supplied mixed material was calculated as the molding rate (molding). If the rate is low, it means that the amount of the mixed material adhered to the molding apparatus is large).
Molding rate (%) = total weight of test piece x 100 / total weight of supplied mixed material

According to this result (Table 8), each test body (No1-1, No6-1 to No6-3) to which the anti-adhesion agent was added had a molding rate of 97% or more, and the test body (No. 6) to which the anti-adhesion agent was not added. It was confirmed that the anti-adhesion effect was excellent as compared with the molding rate of -4) of 95% or more.
Although the data is not shown, when the same test was performed using test specimens to which kaolin and bentonite were added instead of the anti-adhesion agent, the amount of adhesion was about 90%, and the anti-adhesion agent was used. The result was that the amount of adhesion increased even when compared with the case where it was not added.

Further, among the adhesion inhibitors, the molding rate is 100% when sodium n-octanesulfonate is used, which exceeds the molding rate of 97% or more when the other three types of adhesion inhibitors are used. The result was. From this example, it was confirmed that the effect of preventing the adhesion of sodium n-octanesulfonate was excellent.

<7th Example>"Test for confirming whitening effect due to difference in pH of aqueous solution after dissolution"
In order to demonstrate the whitening effect of the effervescent cosmetics due to the difference in the pH of the aqueous solution after dissolution, the amounts of citric acid and anhydrous sodium carbonate (pH adjuster) were adjusted so as to satisfy the blending ratio of the effervescent cosmetics. , 7 types of test specimens were prepared (Table 9), and the same whitening effect confirmation test as in the 4th example was performed.

According to this result (Table 9), in the test specimens (No1-1, No7-2 to No7-5) having a pH of 5.0 to 6.8, the whitening degree was evaluated as 4th or higher, and the effect was effective. It turned out to be expensive. In particular, the test specimens having a pH of 5.5 to 6.5 (No1-1, No7-3, No7-4) received the highest evaluation of 5, and it was clarified that the effect was very high.

Claims (1)

It contains at least one organic acid of citric acid, fumaric acid, malic acid and succinic acid, sodium hydrogen carbonate and polyethylene glycol having an average molecular weight of 4000 or more and 6000 or less.
A molded product having a thickness of 5 mm or less, a hardness of 9.8 N or more and less than 147.1 N, a polyethylene glycol coating film formed on the surface layer portion, a brightness of 80 or more, and a saturation of 10.0 or less. ,
With respect to 1 part by weight of the organic acid, 0.7 parts by weight to 1.5 parts by weight of the sodium hydrogen carbonate and 0.08 parts by weight to 0.20 parts by weight of the polyethylene glycol are contained, respectively .
It is a method for producing an effervescent cosmetic containing 0.3 part by weight to 0.6 part by weight of sodium n-octanesulfonate with respect to 100 parts by weight of the total amount of the effervescent cosmetic.
The organic acid, the sodium hydrogen carbonate, the polyethylene glycol, and the sodium n-octanesulfonate are mixed and stirred.
Subsequently, a method for producing an effervescent cosmetic product, which comprises forming the molded product.

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