JP2018090532A - Production method of granules for skin detergent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide production methods of granules for skin detergents, the granules being able to enhance the functionality of a comprised functionalizing agent, to provide production methods of a skin detergent containing granules for skin detergents obtained by the production methods, and to provide methods of washing the skin using the same.SOLUTION: A production method of granules for skin detergents comprises: mixing a compatible liquid obtained by mixing a functionalizing agent having the compatibility between (a component a), a fatty acid having 10 or more to 22 or less carbon atoms and (a component b), a functionalizing agent compatible with the component a at a temperature not less than the melting point of the component a, with (a component c), a water-soluble inorganic salt powder using a stirring mixer at a temperature not less than the melting point of the component a; and granulating granules with an average grain diameter of 50 μm or more to 1000 μm or less, the mass ratio of the component a to the component b (the component a/the component b) being 2 or more to 50 or less.SELECTED DRAWING: None

Description

  The present invention relates to a method for producing granules for skin cleanser.

In recent years, imparting functionality such as a refreshing feeling to various skin cleansing materials has been performed. In addition, in order to obtain a physical cleaning effect and a massage effect, inclusion of granules and the like is performed.
Patent Document 1 discloses (a) polyoxyalkylene fatty acid alkanolamide, (b) cooling sensation for the purpose of providing a cleaning composition having excellent stability over time and further excellent cooling sensation and cooling sensation sustaining effect. And (c) a detergent composition containing a polyhydric alcohol having an IOB value (ratio of inorganic value and organic value (Inorganic Organic Balance) determined based on an organic conceptual diagram) of 1.5 to 3 ing.
Patent Document 2 discloses (1) 5% by weight sodium chloride aqueous solution for the purpose of providing a cleaning composition that is low-stimulation and low-damage to the skin while maintaining a feeling of massage and cleaning power. Particles having an average particle diameter of 5 to 500 μm and an elastic modulus in the aqueous solution exceeding 5 × 10 ⁵ dyne / cm ² , (2) an elastic modulus in a 5 wt% sodium chloride aqueous solution of 1 X10 ^{3 to} 5 × 10 ⁵ dyne / cm ² , and the weight ratio of (1) and (2) is 1: 100 to 10: 1, (1) And (2) have an average particle size ratio of 1:10 to 1: 1.

Japanese Patent Laying-Open No. 2015-182967 JP 09-031492 A

  However, there has been a demand for a detergent composition having a higher cooling sensation and a cooling sensation sustaining effect. The present invention provides a method for producing a granule for skin cleanser capable of enhancing the functionality of the functionalizing agent contained therein, and a method for producing a skin cleanser comprising the granule for skin cleanser obtained by the production method, Another object of the present invention is to provide a method for cleaning the skin using the same.

The present inventors have found that the above problem can be solved by a method for producing a granule for skin cleanser having a specific process.
That is, the present invention provides (a component) a fatty acid having 10 to 22 carbon atoms and (b component) a functionalizing agent that is compatible with the a component at a temperature equal to or higher than the melting point of the a component. The phase solution obtained by mixing at the above temperature and the (c component) water-soluble inorganic salt powder are mixed using a stirring mixer to obtain granules having an average particle diameter of 50 μm or more and 1,000 μm or less. The manufacturing method of the granule for skin washing | cleaning materials which has a process and whose mass ratio (a component / b component) of a component with respect to b component is 2-50.

  According to the present invention, a method for producing a granule for skin cleanser capable of enhancing the functionality of a functionalizing agent contained therein, and a production of a skin cleanser comprising granules for skin cleanser obtained by the above production method Methods and methods for cleaning skin using the same are provided.

The method for producing a granule for skin cleanser of the present invention comprises (a component) a fatty acid having 10 to 22 carbon atoms and (b component) a functionalizing agent that is compatible with the a component at a temperature equal to or higher than the melting point of the a component. And a phase solution obtained by mixing at a temperature equal to or higher than the melting point of component a and (component c) water-soluble inorganic salt powder using an agitating mixer, the average particle size is 50 μm or more, And having a step of forming granules that are 000 μm or less, and the mass ratio of the a component to the b component (a component / b component) is 2 or more and 50 or less.
The method for producing a granule for skin cleanser of the present invention has the following step 1 and step 2, and performs step 2 after step 1, and the mass ratio of component a to component b in step 1 (a component / b component) Is preferably 2 or more and 50 or less.
Step 1: (a component) a fatty acid having 10 to 22 carbon atoms and (b component) a functionalizing agent that is compatible with the a component at a temperature equal to or higher than the melting point of the a component; Step 2: Mixing the phase solution obtained in Step 1 with the phase solution obtained in Step 1 and the component (c) water-soluble inorganic salt powder using a stirring mixer, and the average particle size is 50 μm or more 1 Process to make granules less than 1,000 μm

In the present invention, granules are prepared by mixing a phase solution in which a component and b component are mixed with c component, and in this case, the mass ratio of a component to b component is set within a certain range. . It has been found that a skin cleanser with improved functionality of the functionalizing agent can be obtained by the granules produced by the above method.
Although the detailed mechanism for obtaining the above effect is unknown, a phase solution in which a functionalizing agent and a fatty acid are previously mixed is mixed with a water-soluble inorganic salt powder to obtain granules having a specific average particle size. Thus, when the skin is washed with the skin cleansing material containing the granules, the granules are appropriately disintegrated during the washing, so that the functional agent is released and the function of the functional agent is exhibited. The agent is locally present at a high concentration, and it is estimated that the functionality of the functionalizing agent is improved. In addition, at least a part of the granule for skin cleanser of the present invention disintegrates during washing.

Hereinafter, the manufacturing method of the granule for skin washing | cleaning materials of this invention is explained in full detail. In addition, in the following description, although it demonstrates centering on the manufacturing method which has said process 1 and process 2 which is a preferable aspect of this invention, this invention is not limited to such a manufacturing method, For example, In addition, a mode in which a phase solution of the component a and the component b is obtained and the step 2 is performed is included.
[Step 1]
Step 1 includes (a component) a fatty acid having 10 to 22 carbon atoms and (b component) a functionalizing agent that is compatible with the a component at a temperature equal to or higher than the melting point of the a component. This is a step of obtaining a phase solution by mixing at a temperature. In addition, mass ratio (a component / b component) of a component with respect to b component in the process 1 is 2-50.
The components a and b used in step 1 will be described below.

<(A component) Fatty acid having 10 to 22 carbon atoms>
In the present invention, (a component) the fatty acid having 10 to 22 carbon atoms is preferably dry-neutralized at least partially by contacting with (c component) the water-soluble inorganic powder. In addition, dry neutralization means neutralizing by contacting the melt | dissolved a component and c component, without using a solvent essentially.
(A component) Fatty acids having 10 to 22 carbon atoms are those having 10 or more carbon atoms from the viewpoint of stabilizing the (b component) functionalizing agent in the neutralized product with the (c component) water-soluble inorganic powder. The fatty acid is preferably 12 or more, more preferably 14 or more, and is a fatty acid having 22 or less carbon atoms, and preferably 18 or less, from the viewpoint of handling properties during production and production cost. The component a may be either a saturated or unsaturated fatty acid, but is preferably a saturated fatty acid from the viewpoint of suppressing odor derived from the fatty acid. The component a may be either linear or branched, but is preferably a linear fatty acid from the viewpoint of stabilization in a neutralized product with a water-soluble inorganic powder. Specifically, stearic acid, palmitic acid, and myristic acid are preferable, and palmitic acid is most preferable.
A component may be used individually by 1 type and may use 2 or more types together. Moreover, unless the effect of this invention is impaired, you may use together fatty acids other than a component.

<(Component b) functionalizing agent>
In the present invention, the (b component) functionalizing agent is compatible with the a component at a temperature equal to or higher than the melting point of the a component. The melting point of the component b is preferably lower than the melting point of the component a, but may be higher than the melting point of the component a. In that case, the phase solution is preferably used at a temperature equal to or higher than the melting point of the component b.
Here, “compatible” refers to a phenomenon in which two or more liquid components dissolve in each other in a fluid containing two or more liquid components. On the other hand, phase separation refers to a phenomenon in which in a fluid containing two or more liquid components, one or more of these liquid components do not mix with other liquid components and are separated. Whether the fluid containing two or more liquid components is in a compatible state is whether it is separated into multiple phases when mixed and allowed to stand, or phase separation when mixed and stirred Thus, it can be confirmed whether or not white turbidity occurs. In the present invention, the melting point of the component b is equal to or higher than the melting point of the component a, and at a temperature equal to or higher than the melting point of the component a, the solid component b is dissolved in the component a to obtain a uniform liquid. In some cases, it is also assumed that the solution is a phase solution.

  The “functionalizing agent” means an active ingredient for imparting some functionality to the skin cleansing agent, and examples thereof include sensates, moisturizers, bactericides, and fragrances. From the viewpoint of stabilizing the functionalizing agent in the dry neutralized product, the solubility parameter (Fedors method) of the functionalizing agent is preferably 7.5 or more, more preferably 8 or more, and more preferably 8.5. More preferably, it is 9 or more, preferably 15 or less, more preferably 14.5 or less, more preferably 14 or less, still more preferably 13.5 or less. As a sensation agent, l-menthol (solubility parameter = 10.1), l-mentholone (solubility parameter = 9.2), moisturizing agent sphingolipid E (solubility parameter = 10.0), sterilization Ingredients isopropylmethylphenol (solubility parameter = 12.4), triclosan (solubility parameter = 13.2), perfume ingredient 4,7-dimethyloctane-3-o (Solubility parameter = 9.7), phenylethyl alcohol (solubility parameter = 12.1), and the like. When the functionalizing agent is composed of a plurality of compounds, the solubility parameter can be obtained by weighted averaging the parameters of each compound.

Among these, as the functionalizing agent, a refreshing agent is preferable among sensory agents, l-menthol and l-mentholone are preferable, and l-menthol is more preferable.
A functionalizing agent may be used individually by 1 type, and may use 2 or more types together.

  In the present invention, the mass ratio of the a component to the b component in step 1 (a component / b component) is 2 or more from the viewpoint of supporting the b component in the granule for skin cleanser, and the b component is locally high. From the viewpoint of existence at a concentration, it is 50 or less. The mass ratio of the a component to the b component is preferably 2.5 or more, more preferably 3 or more. Moreover, Preferably it is 30 or less, More preferably, it is 20 or less, More preferably, it is 10 or less.

<Step of obtaining a phase solution>
Step 1 is a step of obtaining a phase solution by mixing the a component and the b component at a temperature equal to or higher than the melting point of the a component.
The mixing temperature is preferably the melting point of the a component + 3 ° C. or higher, more preferably the melting point of the a component + 5 ° C. or higher, more preferably the melting point of the a component + 10 ° C. or higher, from the viewpoint of increasing the compatibility between the a component and the b component. More preferably, the melting point of the component a is + 15 ° C. or higher, and from the viewpoint of suppressing the production cost and alteration and volatilization of the components a and b, the melting point of the component a is preferably + 50 ° C. or less, more preferably a The melting point of the component + 40 ° C. or lower, more preferably the melting point of the component a + 30 ° C. or lower.
When palmitic acid (melting point 63 ° C.) is used as component a, the mixing temperature is preferably 63 ° C. or higher, more preferably 68 ° C. or higher, and still more preferably 70 ° C. or higher. From the viewpoint of suppressing deterioration and volatilization of the component b, it is preferably 113 ° C. or lower, more preferably 98 ° C. or lower, and still more preferably 88 ° C. or lower.
When the melting point of the component b is higher than the melting point of the component a, the melting point of the component b is preferably + 3 ° C. or higher, more preferably the melting point of the component b + 5 ° C. or higher, from the viewpoint of increasing the compatibility between the components a and b. More preferably, it is melting | fusing point +10 degreeC or more of b component, More preferably, it is melting | fusing point +15 degreeC or more of a component, and it is preferable from a viewpoint of suppressing manufacturing cost, and a modification and volatilization of a component and b component, The melting point of the component + 50 ° C. or lower, more preferably the melting point of the component b + 40 ° C. or lower, more preferably the melting point of the component b + 30 ° C. or lower.

In Step 1, the apparatus for obtaining the phase solution of the component a and the component b, the power required for stirring, and the like are not particularly limited, and may be appropriately selected from known methods.
Further, the mixing time is not particularly limited, but from the viewpoint of productivity, it is preferably 120 minutes or less, more preferably 90 minutes or less, still more preferably 60 minutes or less, and from the viewpoint of sufficiently mixing to obtain a phase solution, Preferably it is 30 seconds or more, More preferably, it is 1 minute or more, More preferably, it is 5 minutes or more.

[Step 2]
In step 2, the phase solution obtained in step 1 and (c component) water-soluble inorganic salt powder are mixed using a stirring mixer to obtain granules having an average particle size of 50 μm or more and 1,000 μm or less. It is a process.

<(C component) Water-soluble inorganic salt powder>
In step 2, the phase solution obtained in step 1 and (component c) water-soluble inorganic powder are mixed to form granules.
Here, “water-soluble” means that the solubility in water at 20 ° C. is 5 g / L or more, and preferably 10 g / L or more.
The component c is preferably an alkali metal inorganic acid salt because of its high reactivity with fatty acids. The alkali metal sulfite, hydrogen sulfite, carbonate, bicarbonate, silicate, phosphate, boron Examples include acid salts and the like. c component may be used individually by 1 type, and may use 2 or more types together.
Among these, the component c is preferably at least one selected from the group consisting of alkali metal carbonates and alkali metal hydrogen carbonates, more preferably sodium carbonate and carbonic acid, because of its high reactivity with fatty acids. At least one selected from the group consisting of sodium hydrogenate, more preferably sodium carbonate and sodium bicarbonate are used in combination.

  When sodium carbonate and sodium bicarbonate are used in combination as component c, the mass ratio of sodium carbonate content to sodium bicarbonate content (sodium carbonate / sodium bicarbonate) is highly reactive with fatty acids. From the viewpoint of lowering the pH of the granule, it is preferably 0.01 or less, more preferably 0.02 or more, further preferably 0.02 or more, and more preferably 0.03 or more. Preferably it is 0.4 or less, More preferably, it is 0.3 or less.

  The component c is preferably in a powder form, and is preferably pulverized or pulverized in advance until a suitable particle size is obtained. Examples of the pulverizer that can be used for pulverization or crushing include impact crushers such as hammer crushers, impact crushers such as atomizers and pin mills, and shear crushers such as flash mills. These may be a single stage operation, or may be a multistage operation of the same kind or different kind of pulverizer.

  The average particle size of the component c is preferably 500 μm or less, more preferably 300 μm or less, still more preferably 150 μm or less, still more preferably 100 μm or less, still more preferably 50 μm or less, and even more preferably from the viewpoint of neutralization efficiency. 30 μm or less. Moreover, from the viewpoint of imparting appropriate disintegration of granules when blended in the skin cleansing agent and from the viewpoint of production, it is preferably 5 μm or more, more preferably 10 μm or more, and further preferably 15 μm or more.

  In step 2, the mass ratio of the a component to the c component (a component / c component) improves the feeling of washing with the dry neutralization viewpoint and the particle size of the resulting granule for skin cleansing within the desired range. In addition, from the viewpoint of setting the disintegration property of the granules within an appropriate range, it is preferably 0.3 or more, more preferably 0.33 or more, still more preferably 0.35 or more, and preferably 1.0 or less. Preferably it is 0.7 or less, More preferably, it is 0.5 or less.

  In step 2, the mass ratio of the b component to the c component (b component / c component) is preferably 0.01 or more, more preferably from the viewpoint of setting the particle size of the resulting granule for skin cleansing to a desired range. It is 0.03 or more, more preferably 0.05 or more, and preferably 0.18 or less, more preferably 0.16 or less, and further preferably 0.14 or less.

In step 2, the phase solution of component a and component b obtained in step 1 is mixed with component c. In step 2, as described above, dry neutralization is preferably performed with the melted component a and component c.
In the mixing in the step 2, it is preferable to add a phase solution of the component a and the component b obtained in the step 1 to the component c from the viewpoint of mixing properties. In the following description, the phase solution of component a and component b obtained in step 1 is also referred to as phase solution A. The amount of phase solution A added to 100 parts by mass of component c is preferably 5 parts by mass or more, more preferably 10 parts by mass or more, still more preferably 20 parts by mass or more, and more preferably, from the viewpoint of stabilizing the component b into granules. The amount is preferably 40 parts by mass or more, and preferably 500 parts by mass or less, more preferably 350 parts by mass or less, still more preferably 100 parts by mass or less, and still more preferably 60 parts by mass or less.

The addition rate of the phase solution A depends on the mixing device, but from the viewpoint of dry neutralization, it is preferably 5 minutes or more, more preferably 10 minutes or more, and further preferably 30 minutes or more, per 1 kg of the phase solution A. More preferably, it is 1 hour or more, and from the viewpoint of shortening the production time, it is preferably 4 hours or less, more preferably 3 hours or less, and even more preferably 2 hours or less per 1 kg of the phase solution A.
As a mixer of the phase solution A and the c component, any apparatus capable of uniformly mixing may be used. Specifically, high-speed mixer (manufactured by Earth Technica Co., Ltd.), Redige mixer (manufactured by Matsubo Co., Ltd.), proshear mixer (manufactured by Taiheiyo Kiko Co., Ltd.), ribbon blender (manufactured by Hosokawa Micron Co., Ltd.) Various mixers such as Hosokawa Micron Co., Ltd., and SV mixer (Shinko Bantech Co., Ltd.) can be used.

The temperature of component c in step 2 is preferably 50 ° C. or higher, more preferably 60 ° C. or higher, and still more preferably, from the viewpoint of maintaining a compatible state of the phase solution to obtain uniform granules and dry neutralization. From the viewpoint of suppressing volatilization and modification of the a component and the b component, it is preferably 120 ° C. or less, more preferably 110 ° C. or less, still more preferably 100 ° C. or less, and still more preferably 90 ° C. or less. is there.
The mixer may be one without a heat retaining mechanism, but the temperature of the jacket water of the mixer is preferably adjusted to the temperature of the component c from the viewpoint of dry neutralization.
The mixing time in step 2 depends on the production amount, but from the viewpoint of sufficiently mixing the phase solution A and the component c and forming granules, it is preferably 1 minute or more, more preferably 2 minutes or more, From the viewpoint of shortening the production time, it is preferably 3 hours or less, more preferably 1 hour or less, and even more preferably 30 minutes or less.
In the case of dry neutralization, the end point of mixing is the point at which dry neutralization is substantially completed, and it can be visually confirmed that the liquid fatty acid has become a solid soap.

The average particle size of the granules for skin cleanser obtained in step 2 is 50 μm or more and 1,000 μm or less. It is preferable for the skin cleansing granules to have an average particle size of 50 μm or more because the feeling of cleaning the skin is improved. In addition, when the average particle size of the granule for skin cleanser is 1,000 μm or less, the feeling of use is excellent, and the granule is appropriately disintegrated during washing.
In view of the above, the average particle diameter is preferably 100 μm or more, more preferably 150 μm or more, further preferably 200 μm or more, and preferably 900 μm or less, more preferably 800 μm or less, still more preferably 700 μm or less, and even more preferably. Preferably, it is 650 μm. In addition, you may adjust to the said particle size range by pulverizing, grind | pulverizing, or classifying the granule for skin washing materials obtained at the process 2. FIG.
The average particle size of the skin cleansing granules is measured by the method described in Examples.

In the present invention, in step 1 and / or step 2, components other than the a component, b component and c component described above may be added.
About process 1, adding fatty acid other than a component is illustrated.
In step 2, an oil-absorbing powder may be used in addition to the component c. The oil-absorbing powder may be added to promote granulation and produce granules having a desired particle size.
Examples of the oil-absorbing powder include amorphous silica, dextrin, soda ash, bow show, bentonite, zeolite and the like.

  The average particle diameter of the oil-absorbing powder is preferably 0.5 μm or more, more preferably 1.0 μm or more, still more preferably 3.0 μm or more, and still more preferably 5.0 μm or more from the viewpoint of exerting oil absorption. From the viewpoint of obtaining a skin cleansing granule having a desired particle size, it is preferably 100 μm or less, more preferably 50 μm or less, still more preferably 40 μm or less, and even more preferably 30 μm or less. The average particle diameter of the oil-absorbing powder can be measured by a laser diffraction / scattering method. The shape of the oil-absorbing powder is preferably spherical from the viewpoint of usability.

The oil-absorbing powder may be used alone or in combination of two or more.
The addition amount of the oil-absorbing powder is preferably 0.5 parts by mass or more, more preferably 100 parts by mass with respect to 100 parts by mass of the phase solution of component a and component b obtained in step 1 from the viewpoint of obtaining a desired particle size. Is not less than 1 part by mass, more preferably not less than 2 parts by mass, and from the same viewpoint, it is preferably not more than 10 parts by mass with respect to 100 parts by mass of the phase solution of component a and component b obtained in step 1. Preferably it is 8 mass parts or less, More preferably, it is 5 mass parts or less.

[Skin cleaning material and method for producing the same]
The granule for skin cleanser of the present invention is blended in the skin cleanser.
The skin cleanser can be in any form such as liquid, cream (O / W emulsified type, W / O emulsified type), paste, gel, solid, powder, etc. From the viewpoint of stably holding the granule for the material and imparting an excellent feeling of washing, it is preferably a paste.

  The content of the granule for skin cleanser in the skin cleanser depends on the dosage form, but when it is in the form of a paste, it is preferably 1% by mass or more, more preferably 2 from the viewpoint of obtaining an excellent feeling of cleansing. From the same viewpoint, it is preferably 40% by mass or less, more preferably 30% by mass or less, and still more preferably 20% by mass or less.

It is preferable that the skin cleanser is manufactured by a manufacturing method including the following step 3.
Step 3: Step of mixing the granule obtained in Step 2 above and (d component) surfactant The mixture of the skin cleansing granule and the surfactant is a skin cleanser containing a surfactant in advance. It is preferable to prepare a base and add and mix the skin cleansing granules obtained in step 2 to the base.
Examples of surfactants include anionic surfactants, cationic surfactants, nonionic surfactants, and amphoteric surfactants. Among these surfactants, the inclusion of an anionic surfactant can improve cleaning feeling. It is preferable from an excellent viewpoint.
The anionic surfactant is not limited as long as it is used in an ordinary detergent composition. For example, fatty acid salts, alkyl sulfates, polyoxyalkylene alkyl ether sulfates, polyoxyalkylene alkenyl ether sulfates, Sulfosuccinic acid alkyl ester salt, polyoxyalkylene sulfosuccinic acid alkyl ester salt, α-olefin sulfonate, alkyl ether carboxylate, polyoxyalkylene alkyl ether carboxylate, N-acyl amino acid salt, N-acyl alkyl taurine salt, etc. From the viewpoint of improving detergency against pores, foaming, and rinsing properties, at least one selected from sulfate ester salts, sulfonate salts, and carboxylate salts is preferable, and selected from sulfate ester salts and carboxylate salts. At least one Still more preferably, more than at least one selected from carboxylic acid salt is more preferable.

Surfactant may be used individually by 1 type and may use 2 or more types together.
The content of the surfactant is preferably 5% by mass or more, more preferably 6% by mass or more, still more preferably 7% by mass or more, and still more preferably from the viewpoint of obtaining a sufficient cleansing property. Is 8% by mass or more, and from the viewpoint of maintaining the content of other components, it is preferably 90% by mass or less, more preferably 50% by mass or less, and still more preferably 20% by mass or less.

In addition to the above ingredients, other ingredients may be added to the skin cleanser, such as gum, oil, other polymer compounds, higher alcohols, powders, preservatives, chelating agents, antioxidants Examples include agents, pH adjusters, pigments, fragrances, enzymes, scrubs, thickeners, foaming agents, humectants, solvents and the like.
In the present invention, the skin cleanser can be applied to facial cleansers, hand soaps, body shampoos, etc., and is particularly preferably used as a facial cleanser.

In the following examples and comparative examples, “%” means “mass%” unless otherwise specified.
[material]
Each component used in Examples and Comparative Examples is shown below.
<a component>
Palmitic acid: LUNAC P-95 (manufactured by Kao Corporation)
<Component b>
L-Menthol: Menthol JP (TAB) COS (manufactured by Takasago International Corporation)
<Component c>
・ Sodium carbonate: Soda ash (light) (Central Glass Co., Ltd., average particle size 100 μm)
-Sodium bicarbonate: baking soda-T (manufactured by Tosoh Corporation, average particle size 250 μm)
<Oil-absorbing powder>
Bentonite: Odosolv K-400 (Kurosaki Shirato Kogyo Co., Ltd., average particle size 7 μm)
<D component and its precursor>
・ Lauric acid: LUNAC L-98 (manufactured by Kao Corporation)
・ Myristic acid: LUNAC MY-98 (manufactured by Kao Corporation)
-Palmitic acid: LUNAC P-95 (manufactured by Kao Corporation)
・ Polyoxyethylene lauryl ether acetic acid: Kao Akipo RLM-45 (manufactured by Kao Corporation)
<Others>
・ Lauryl hydroxysulfobetaine solution: Amhitoal 20HD (Foaming agent, manufactured by Kao Corporation)
・ Glycerin mono-2-ethylhexyl ether solution (90%): Penetol GE-EH (foam increaser, manufactured by Kao Corporation)
・ Acrylic acid / alkyl methacrylate copolymer: Carbopol ETD2020 (Thickener, Lubrizol)
・ Potassium hydroxide solution: Liquid caustic potash (48%)
・ Sorbit liquid: Sorbitol # 650 (humectant, manufactured by Kao Corporation)
・ Phenoxyethanol: Hisolv EPH (preservative, manufactured by Toho Chemical Co., Ltd.)
・ Edetate disodium: Crewat N (preservative, manufactured by Nagase ChemteX Corporation)
-Fragrance: 4,7-dimethyloctane-3-ol (manufactured by Kao Corporation)

[Measuring method]
<Measurement of average particle size of water-soluble inorganic salt powder and granule for skin cleanser>
JIS Z8801-1: 2006 standard sieve (12-stage sieve and saucer with openings of 45 μm, 63 μm, 90 μm, 125 μm, 180 μm, 250 μm, 355 μm, 500 μm, 710 μm, 1,000 μm, 1,400 μm, 2,000 μm) The median diameter was calculated from the mass fraction depending on the mesh size. More specifically, using a 12-stage sieve and a saucer, stack the sieves in order from a sieve with a small mesh size, add 100 g of particles from the top of the top 2,000 μm sieve, and cover. Attached to a low-tap type sieve shaker (manufactured by HEIKO Mfg. Co., Ltd., tapping 156 times / minute, rolling: 290 times / minute), after vibrating for 5 minutes, the mass of the particles remaining on each sieve and the saucer is measured. The mass ratio (%) of the particle group on each sieve was calculated. The mass ratios of the particle groups on the sieve having a small mesh size were accumulated in order from the saucer, and the particle size at which the total amount was 50% was defined as the average particle size.

<Measurement of average particle diameter of oil-absorbing powder and ground water-soluble inorganic salt powder>
Using a laser diffraction / scattering particle size distribution measuring apparatus LA-920 (manufactured by Horiba, Ltd.), the median diameter measured by dispersing the particles in a solvent that does not dissolve was used as the average particle diameter. In addition, ion-exchange water was used as a solvent for measuring the average particle size of bentonite used in the examples, and acetone was used for measuring the average particle size of pulverized sodium carbonate and sodium bicarbonate.

[Example 1]
<Preparation of water-soluble inorganic salt powder>
Sodium carbonate and sodium hydrogen carbonate were pulverized with an atomizer (Dalton Co., Ltd .: AIIW, throughput 70 kg / min, hammer rotation speed 8,000 rpm, screen diameter 0.7 mm), and water-soluble with average particle sizes of 20 μm and 26 μm, respectively. An inorganic salt powder was obtained.

<Steps 1 and 2>
Granules for skin cleanser were prepared by the following method.
[Step 1]
Palmitic acid: 176 g and l-menthol: 24 g were mixed at 80 ° C. to obtain a phase solution.
[Step 2]
A 2 L high speed mixer (manufactured by Earth Technica: LFS-2, agitator rotation speed 850 rpm, chopper rotation speed 1,500 rpm, jacket hot water temperature 80 ° C.) was charged with 80 g of sodium carbonate and 320 g of sodium hydrogen carbonate. After mixing for 1 minute, the phase solution (80 ° C.) of palmitic acid obtained in Step 1: 176 g and 1-menthol: 24 g was added over 21 minutes, mixed for 3 minutes, and skin washed with an average particle size of 234 μm A raw granule was obtained.

[Example 2]
<Steps 1 and 2>
Granules for skin cleanser were prepared by the following method.
[Step 1]
Palmitic acid: 152 g and l-menthol: 48 g were mixed at 80 ° C. to obtain a phase solution.
[Step 2]
Sodium carbonate prepared in the same manner as in Example 1 in a 2 L high speed mixer (manufactured by Earth Technica: LFS-2, agitator rotation speed 850 rpm, chopper rotation speed 1500 rpm, jacket hot water temperature 80 ° C.): 80 g, sodium hydrogen carbonate: After adding 320 g and bentonite: 5.2 g and mixing for 1 minute, a phase solution (80 ° C.) of palmitic acid: 152 g and 1-menthol: 48 g obtained in Step 1 was added over 21 minutes. Mixing for 5 minutes gave granules for skin cleanser having an average particle size of 477 μm.

[Example 3]
A granule for skin cleanser having an average particle size of 639 μm was obtained in the same manner as in Example 1 except that 152 g of palmitic acid and 48 g of 1-menthol were used.

[Comparative Example 1]
A skin cleansing granule having an average particle size of 1,000 μm or more was obtained in the same manner as in Example 1 except that 74 g of sodium carbonate, 298 g of sodium hydrogen carbonate, 128 g of palmitic acid, and 72 g of 1-menthol were used. . In addition, there were many granules remaining on the sieve having an opening of 2,000 μm, and it was difficult to measure the average particle size.
The results are shown in Table 1 below.

[Preparation of granule 5]
The granule 1 obtained in Example 1 was dried under reduced pressure for 1 week in a vacuum dryer (manufactured by AS ONE Co., Ltd .: AVO-250NB, drying temperature 50 ° C., 0.02 MPa pressure) to volatilize l-menthol in the granule. Granule 5 was prepared.

[Example 4 and Comparative Examples 2 and 3]
Using the resulting granules for skin cleanser, the skin cleanser shown in Table 3 was prepared. First, a paste-like skin cleanser base was separately prepared using the ingredients from Table 2 Lunac L-98 to purified water, and the skin cleanser granules and paste-like skin cleanser base were placed in a beaker. The face wash, which is a skin cleanser, was prepared by manually stirring the mixture with the tube and filling the tube. Moreover, the evaluation mentioned later was performed 1 hour after preparation.

  Table 1 below shows the obtained face wash, the l-menthol content in the granules, and the blending amount of the granules. In addition, although the granule 1 was used for Example 4, as a result of the measurement, 1-menthol content in the granule was 3.28 mass%. Although the comparative example 2 uses the granule 5, the menthol content in a granule was 0 mass% as a result of the measurement.

[Sensory evaluation of cool feeling]
The following sensory tests were performed on three evaluation testers.
First, the face was lightly wetted with hot water, and the prepared paste-like face wash (1 g) was taken in both hands and whipped. Next, the face was massaged with foamed foam for 30 seconds, and the cool feeling during the massage was sensory evaluated.
After the massage, it was rinsed with hot water, and the cool feeling at the time of rinsing was sensory evaluated.
Furthermore, water was wiped off with a towel, and the cool feeling after towel drying was sensory evaluated.
The evaluation criteria for sensory evaluation are as follows. The average value of the three people is shown in Table 4 below.
4: A feeling of cooling is strongly felt 3: A feeling of cooling is felt 2: A feeling of cooling is slightly felt 1: A feeling of cooling is not felt The results are shown in Table 4 below.

In Example 4, a cool feeling was felt on the entire face after towel drying.
From the above results, it was found that in Examples 1 to 3, granules having a size suitable for use in a skin cleanser were obtained.
On the other hand, in Comparative Example 1, it was found that when the mixing ratio of the fatty acid and the functionalizing agent does not satisfy the provisions of the present invention, a granule that is too large to be used for a skin cleanser is obtained.
Furthermore, regarding the skin cleansing composition containing the above-mentioned granule for skin cleansing, in Example 4, compared with Comparative Examples 2 and 3, l-menthol (functional agent) as a whole face wash (skin cleansing) Although the content of is the same, it was found that a cool feeling was felt from the beginning of the face wash, and the cool feeling persisted for a long time after towel drying, and the functionality of the functionalizing agent was improved.

  According to the manufacturing method of the granule for skin cleansing agents of this invention, the functionality of the functionalizing agent contained can be improved. The skin cleanser containing the skin cleanser granules obtained by the present invention is suitably used for facial cleansers, hand soaps, body shampoos and the like.

Claims (9)

  (A component) A fatty acid having 10 to 22 carbon atoms and (b component) a functionalizing agent compatible with the a component at a temperature equal to or higher than the melting point of the a component are mixed at a temperature equal to or higher than the melting point of the a component. A phase solution obtained by mixing the water-soluble inorganic salt powder (component c) with a stirring mixer to obtain granules having an average particle diameter of 50 μm or more and 1,000 μm or less, b The manufacturing method of the granule for skin cleaning materials whose mass ratio (a component / b component) of a component with respect to a component is 2-50. The manufacturing method of the granule for skin washing materials of Claim 1 which has the following process 1 and the process 2, and performs the process 2 after the process 1.
Step 1: (a component) a fatty acid having 10 to 22 carbon atoms and (b component) a functionalizing agent that is compatible with the a component at a temperature equal to or higher than the melting point of the a component; Step 2: Mixing the phase solution obtained in Step 1 with the phase solution obtained in Step 1 and the component (c) water-soluble inorganic salt powder using a stirring mixer, and the average particle size is 50 μm or more 1 Process to make granules less than 1,000 μm   The manufacturing method of the granule for skin washing | cleaning of Claim 1 or 2 whose said c component is an inorganic acid salt of an alkali metal.   The manufacturing method of the granule for skin washing | cleaning in any one of Claims 1-3 whose said c component is an alkali metal carbonate or hydrogencarbonate.   The manufacturing method of the granule for skin cleansing materials in any one of Claims 1-4 whose mass ratio (a component / c component) of a component with respect to c component is 0.3 or more and 1 or less.   The manufacturing method of the granule for skin cleansing agents in any one of Claims 1-5 whose mass ratio (b component / c component) of b component with respect to c component is 0.01 or more and 0.18 or less.   The method for producing granules for skin cleanser according to any one of claims 1 to 6, wherein the component b contains at least one compound selected from the group consisting of l-menthol and l-mentholone.   A method for producing a skin cleanser, comprising a step of mixing the granule for skin cleanser obtained by the production method according to claim 1 and (d component) a surfactant.   A method for cleaning the skin using the skin cleansing material manufactured by the manufacturing method according to claim 8.