JP5183984B2 - Bath preparation - Google Patents

Description

  The present invention relates to a foaming compression mold bath agent having good fragrance and excellent stability.

  It has been known that a bath preparation containing a carbon dioxide gas generator in which a carbonate and an acid are combined is excellent in blood circulation promoting effect and hardly causes hot water cooling (see Patent Document 1).

In addition, as important effects expected as a bath preparation, there are aromatherapy effects due to aroma, relaxation effects, and the like, and it is important to stabilize the fragrance blended in the bath preparation. However, in a bath preparation containing a carbon dioxide gas generation product, it is difficult to maintain a stable fragrance for a long time during bathing because the fragrance is likely to volatilize simultaneously with foaming. Then, the technique which mix | blends a fragrance | flavor in particle | grains and stabilizes the fragrance in storage and bathing is reported (patent document 2).
JP 59-70609 A JP 2000-229843 A

However, if a fragrance is blended in the particles and compression molding is performed together with a carbon dioxide gas product that is a combination of carbonate and acid, sticking occurs at the time of compression molding depending on the type of the fragrance. It has been found that a compression mold bath agent cannot be obtained.
Accordingly, an object of the present invention is to provide a foamable compression molding bath agent having good fragrance, excellent fragrance stability, and good moldability.

  Therefore, as a result of various investigations aimed at achieving compatibility between fragrance formation and fragrance stability and moldability, the present inventor has obtained a specific ClogP value in a fragrance particle containing an aryl alcohol or alcohol-based fragrance component and a water-soluble polymer. If it is granulated by blending a fatty acid ester having a carbon dioxide, and a carbon dioxide gas generator that is a combination of carbonate and acid, and then compression-molded, it has good foaming properties, fragrance standing, and scent stability It has been found that a compression mold bath agent excellent in moldability and excellent in moldability without causing sticking can be obtained.

That is, this invention provides the foaming compression mold type bath agent containing the fragrance | flavor particle | grains containing the following components (a1)-(a3), sodium hydrogencarbonate and / or sodium carbonate, and an organic acid.
(A1) A fragrance containing 5% by weight or more of an alcohol component having an aryl group or 30% by weight or more of an alcohol component having 6 to 15 carbon atoms 1 to 50% by weight
(A2) 0.1 wt% or more of fatty acid esters having a molecular weight of 100 or more and a ClogP value of 6-12, and (a3) a water-soluble polymer having an average molecular weight of 4000 or more, 45 to 95 wt%.

  According to the present invention, the scent is good, the scent is excellent and the sticking does not occur at the time of compression molding, so that not only the productivity but also the scent and foaming compatibility, the scent sustainability, etc., the quality is constant. A foamable compression mold bath agent can be provided.

  The bath agent of the present invention contains perfume particles containing the above (a1), (a2) and (a3). The components (a1), (a2), and (a3) are not simply blended in the bath agent, but may be blended in the fragrance particles to produce a fragrance, fragrance persistence, fragrance stability, and compression molding. This is important in preventing sticking.

  The component (a1) is a fragrance component containing 5% by weight or more of an alcohol component having an aryl group or 30% by weight or more of an alcohol component having 6 to 15 carbon atoms. When these fragrance ingredients are blended, the fragrance is good when the bath agent is dissolved. In particular, when creating a “flower fragrance”, the fragrance can be fresh. Furthermore, it is effective in increasing the sustainability of the fragrance to the skin after bathing. However, if a fragrance particle containing an alcohol-based fragrance component having an aryl group is used together with a carbon dioxide gas generation product, the problem of sticking will occur. In the present invention, sticking can be effectively prevented by blending the fatty acid ester of (a2) with a fragrance containing (a1) an alcohol component having an aryl group in the fragrance particles.

  Examples of the alcohol component having an aryl group include alcohols having 6 to 28 carbon atoms having an aryl group having 6 to 14 carbon atoms. Specific examples include benzyl alcohol, 4-methoxybenzyl alcohol (anis alcohol), 4- Isopropylbenzyl alcohol (cumin alcohol), 4-methyl-α-phenylethyl alcohol (p, α-dimethylbenzyl alcohol), β-phenylethyl alcohol, α-phenylethyl alcohol, 2-phenyl-propan-1-ol (hydra Tropa alcohol), ortho-, meta-, or para-methylbenzeneethanol (β- (methylphenyl) ethyl alcohol), phenoxyethyl alcohol, 2-methoxyphenylethyl alcohol, α, α-dimethylphenylethyl alcohol, α- Propylphenylethyl alcohol, p-methyldimethylbenzyl carbonate Rubinol, isobutylbenzyl carbinol, 3-phenylpropyl alcohol, 1,1-dimethyl-3-phenylpropanol (dimethylphenylethyl carbinol), 2,2-dimethyl-3-phenylpropanol, 3-methyl-1-phenyl- 3-Pentanol, 3-Phenyl-2-propan-1-ol (Cynamic Alcohol), 2-Benzylideneheptanol (Amyl Cynamic Alcohol), 3-Methyl-5-phenylpentanol-1, 4-hydroxy- Examples include 3-methoxybenzyl alcohol (vanillyl alcohol). In particular, an alcohol having 7 to 18 carbon atoms having an aryl group having 6 to 10 carbon atoms is more preferable. For example, p, α-dimethylbenzyl alcohol, β-phenylethyl alcohol, α-phenylethyl alcohol, hydratropa alcohol, β- (methylphenyl) ethyl alcohol and phenoxyethyl alcohol are preferred. These alcohols having an aryl group are contained alone or in combination of two or more, and are contained in an amount of 5% by weight or more in the total amount of the fragrance component, but particularly 5 to 50% by weight in terms of fragrance, scent freshness, and scent persistence. % Content is preferable.

  Examples of the alcohol component having 6 to 15 carbon atoms include linear, branched or cyclic saturated or unsaturated alcohols. Specifically, 3-methyl-1-pentanol, 1-heptanol, 2-heptanol, 3-heptanol, 1-octanol, 2-octanol, 3-octanol, 2-ethylhexanol, 2-nonanol, 1-nonanol Linear saturated alkyl alcohols such as 2-nonanol, 1-decanol, 1-undecanol, 2-undecanol, 1-dodecanol; 3,5,5-trimethyl-1-hexanol, 3,7-dimethyloctane-3- Branched saturated alkyl alcohols such as all (tetrahydrolinalol); 4-methyl-3-decen-5-ol (undecavertol), 3,7-dimethyl-6-octen-1-ol (citronellol), cis- 3,7-dimethyl-2,6-octadien-1-ol (nerol), 3,7-dimethyl-1,6-octadien-3-ol (linalool), 2,6-dimethyl-7-octene-2- All (dihydromyrcenol), 3,7-dimethyl-1,6-nonadiene-3 Branched-chain unsaturated alkyl alcohols such as -ol (ethyllinalool), 3,7,11-trimethyl-1,6,10-dodecatrien-3-ol (nerolidol); 5-methyl-2-isopropylcyclo And cyclic saturated alkyl alcohols such as hexanol (menthol); cyclic unsaturated alkyl alcohols such as 1-methyl-4-isopropyl-1-cyclohexen-8-ol (terpineol). Especially 3-methyl-1-pentanol, 1-heptanol, 2-heptanol, 3-heptanol, 1-octanol, 2-octanol, 3-octanol, 2-ethylhexanol, 2-nonanol, 1-nonanol, 2-nonanol 1-decanol, 1-undecanol, 2-undecanol and 1-dodecanol are preferred. These alcohols are contained alone or in combination of two or more, and are contained in an amount of 30% by weight or more in the total amount of the fragrance component, but are preferably contained in an amount of 30 to 80% by weight from the viewpoint of fragrance and scent sustainability.

The fragrance component of (a1) contains 1 to 50% by weight from the viewpoint of fragrance in the fragrance particles (A), fresh scent of fragrance, and sustainability of fragrance, but further 1 to 30% by weight, particularly 1 It is preferable to contain -15 weight%. In addition to the aryl alcohol and alcohol, various blended fragrances can be blended with the fragrance component (a1) according to the desired fragrance.

  The component (a2) is a fatty acid ester having a molecular weight of 100 or more and a ClogP value of 6 to 12, and is added to the fragrance particles to form the fragrance particles and a carbon dioxide generator such as carbonate. This prevents sticking at times and maintains the strength of the bath preparation. That is, the component (a2) is effective when blended in the fragrance particles to form a fragrance granule. The ClogP value was calculated by the method described in A. Leo Comprehensive Medicinal Chemistry, Vol. 4 C. Hansch, PG Sammens, JB Taylor and CA Ramsden, Eds., P. 295, Pergamon Press, 1990. (ClogP) ”, which is the ClogP value calculated by the program CLOGP v4.01.

  Preferred fatty acid esters include fatty acid esters having a total carbon number of 8 to 40, particularly esters having a fatty acid group having 6 to 20 carbon atoms and an alkyl group having 2 to 18 carbon atoms, preferably 6 to 20 carbon atoms. An ester having a fatty acid group and an alkyl group having 2 to 16 carbon atoms is more preferred. Specifically, cetyl octoate, cetyl isooctanoate, butyl laurate, isoamyl laurate, methyl myristate, ethyl myristate, isopropyl myristate, isopropyl palmitate, ethyl stearate, butyl stearate, isotridecyl isononanoate, isononanoic acid Examples include isononyl, isopropyl linoleate, isopropyl isostearate, methyl oleate, and ethyl oleate.

  These fatty acid esters are used singly or in combination of two or more, in the perfume particles, 0.1% by weight or more, more preferably 0.1 to 40% by weight, particularly 0.1% by weight from the viewpoint of anti-sticking effect and smell. It is preferable to contain ~ 20% by weight.

  Component (a3) is a water-soluble polymer having an average molecular weight of 4,000 or more, which is important from the viewpoint of stabilization of fragrance, fragrance formation, and fragrance persistence.

The water-soluble polymer used in the present invention is preferably a solid or paste at room temperature (25 ° C.). Here, the paste form is a semi-solid substance. Specifically, natural such as glue, gelatin, collagen protein, casein, sodium alginate, carrageenan, fur celerin, tamarind gum, pectin, gum arabic, guar gum, xanthan gum, tragacanth gum, locust bean gum, dextrin, dextran, agar, starch, etc. Water-soluble polymers; semi-synthetic water-soluble polymers such as carboxymethylcellulose, methylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, cellulose acetate phthalate, propylene glycol alginate, oxidized starch, esterified starch, etherified starch, cationic starch; poly Synthetic water-soluble polymers such as sodium acrylate, polyethyleneimine, polyvinyl alcohol, polyethylene glycol, and polyvinylpyrrolidone. Is, it is possible to use one or more.
Among these, polyethylene glycol, particularly polyethylene glycol having a molecular weight of 4000 to 20000 is preferable.

  The water-soluble polymer can be used alone or in combination of two or more thereof, and the content in the fragrance particles is 45 to 95% by weight, particularly 55 from the viewpoint of fragrance formation, fragrance persistence and fragrance stability. -95 mass%, Furthermore, 65-95 weight% is preferable.

Examples of the granulation method of the fragrance particles containing (a1), (a2) and (a3) are, for example, extrusion granulation tableting molding method, rolling granulation method, spray drying granulation method, centrifugal granulation method, It can be produced by a stirring granulation method, dropping granulation on a plate or the like. In particular, a method capable of producing particles having a small particle diameter from a lump or liquid is preferable. In the fragrance particles of the present invention, (a1) to (a3) are heated and melted and uniformly mixed, and then a predetermined amount is dropped on a flat plate, solidified and granulated, and 0.1 to 5 mm. It is preferable to obtain granular particles. The heating and melting temperature is preferably a temperature at which the (a3) water-soluble polymer used melts.
Further, the strength of the fragrance particles is preferably 0.3 kgf or more at the maximum stress when 1.0 mm is penetrated at a speed of 10 mm / min using a fudo rheometer equipped with a φ1 mm cylindrical probe, and it is difficult to cause sticking during molding. From this point of view, it is particularly preferably 0.4 kgf or more, more preferably 0.5 kgf or more. The strength was measured by melting 7 g of the obtained fragrance particles at 63 ° C. and casting it into an aluminum dish (diameter 25 mm, thickness 7 mm) immersed in a 20 ° C. water bath at 20 ° C. to form a cylinder. Molded into a sample.

  The particle diameter of the fragrance particles is preferably 100 to 5000 μm, particularly preferably 500 to 2000 μm from the standpoint of fragrance, fresh fragrance, and fragrance persistence. The particle size is selected and measured using a sieve.

  The perfume particles are contained in the bath preparation of the present invention in an amount of 0.1 to 50% by weight, particularly 0.5 to 30% by weight, and further 1 to 15% by weight. It is preferable in terms of sustainability.

The bath agent of the present invention contains sodium bicarbonate and / or sodium carbonate as a carbon dioxide gas generator and an organic acid. Examples of the organic acid include succinic acid, fumaric acid, malic acid, adipic acid, tartaric acid, citric acid, malonic acid, maleic acid and the like. Of these, succinic acid or fumaric acid is particularly preferred.
Sodium hydrogen carbonate and / or sodium carbonate is preferably contained in the bath agent of the present invention in an amount of 20 to 80% by weight, particularly 40 to 60% by weight, because sufficient carbon dioxide gas can be dissolved in the bath water. Further, the organic acid is preferably contained in the bath agent of the present invention in an amount of 20 to 80% by weight, particularly 40 to 60% by weight, because sufficient carbon dioxide gas can be dissolved in the bath water. Furthermore, the total content of sodium bicarbonate and / or sodium carbonate and the organic acid is preferably 60 to 98% by weight, particularly preferably 70 to 98% by weight.

  Moreover, in addition to the said component, in order to improve the dispersibility of a fragrance | flavor, the nonionic surfactant can be mix | blended with the bath agent of this invention. Nonionic surfactants include, for example, glycerin fatty acid ester, propylene glycol fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbit fatty acid ester, polyoxyethylene alkyl ether, polyoxypropylene alkyl ether, polyoxyethylene alkyl ether, Examples thereof include oxyethylene polyoxypropylene glycol, polyoxyethylene polyoxypropylene alkyl ether, polyethylene glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, polyglycerin fatty acid ester, and sucrose fatty acid ester. These surfactants may be contained in the perfume particles or may be contained separately from the perfume particles. The surfactant is preferably contained in the bath agent of the present invention in an amount of 0.01 to 30% by weight, particularly 1 to 20% by weight.

The bath agent of the present invention may further contain components usually used for bath agents, such as inorganic salts, inorganic acids, herbal medicines, fats and oils, alcohols, medicinal agents, pigments, vitamins and the like.
The bath preparation of the present invention can be formed into a compression-molded preparation, such as a tablet, by a compression molding method such as tableting.

  The bath agent of the present invention foams and generates carbon dioxide when dissolved in a bathtub. The carbon dioxide gas dissolves in bath water at a high concentration and exhibits a blood circulation promoting effect. On the other hand, the fragrance particles blended in the bath preparation of the present invention are released into the bath water simultaneously with foaming, and a good aroma persists during bathing, so that a good aromatherapy effect is obtained.

Example 1
83 parts by weight of polyethylene glycol 6000 (average molecular weight 7500) was melted at about 60 ° C. and dissolved by adding 13 parts by weight of a rose-based blended fragrance shown in Table 1, 1 part by weight of phenylethyl alcohol (fragrance), and 3 parts by weight of isopropyl myristate. did. After uniformly mixing this, it was dropped on a flat plate at 20 ° C. and granulated into granules having a diameter of about 0.3 to 5 mm to obtain perfume particles.
Examples 2 to 5 and Comparative Examples 1 to 7 were also manufactured in the same manner as in Table 1 to obtain fragrance particles.

[Strength of perfume particles]
7 g of the obtained fragrance particles of each Example and Comparative Example were melted at 63 ° C., and cast into an aluminum dish (diameter 25 mm, thickness 7 mm) immersed in a 20 ° C. water bath to form a cylindrical shape. , Measure the maximum stress (25 ° C) when penetrating 1.0 mm at a speed of 10 mm / min using a Fudoreometer (RT-2010D-D; Fudo Kogyo Co., Ltd.) equipped with a φ1 mm cylindrical probe. It was. The results are shown in Table 1.

[Sticking to the punch when tableting]
Using the fragrance particles shown in Examples 1 to 5 and Comparative Examples 1 to 7 in Table 1, uniformly mixed with the composition shown in Table 2, 100 tablets of 50 g are continuously compressed and evaluated for sticking. It was. As the compression molding machine, an eccentric tableting machine (Masina) was used. After compression molding, the presence or absence of powder that adhered firmly to the ridge was evaluated. The results are shown in Table 2.

[Evaluation criteria for sticking]
4: No sticking at all 3: Slight adhesion on the wrinkle surface but smooth tablet surface 2: Slight adhesion on the tablet surface 1: Remarkable adhesion on the tablet surface

[Rating evaluation]
The tablets containing the fragrance particles obtained in Examples 1 to 5 and Comparative Examples 1 to 7 in Table 1 were dissolved in 150 liters of hot water at 40 ° C., and the odor immediately after dissolution was evaluated. The results are shown in Table 2. Indicated.
[Evaluation criteria for fragrance]
○: It smells like rose.
X: Almost no rose-like odor.

  As is clear from Tables 1 and 2, the bath preparation containing the fragrance particles containing (a2) in addition to (a1) and (a3) did not cause sticking and the fragrance particles had good strength. In contrast, (a2) perfume particles not containing esters (Comparative Examples 1, 5, 6) and perfume particles (Comparative Examples 2, 3) containing a fatty acid ester having a ClogP value of 16.5 or 3.4 The strength was insufficient and sticking occurred. Further, when the component (a1) was less than 1% by weight (Comparative Example 4), the obtained bath agent did not give a good fragrance. Sticking also occurred when the fatty acid ester was blended in the tableting dough instead of the granulated product (Comparative Example 7).

Claims (10)

A foamable compression mold bath agent comprising perfume particles containing the following components (a1) to (a3), sodium bicarbonate and / or sodium carbonate, and an organic acid.
(A1) Perfume containing 5 % by weight or more of an alcohol component having an aryl group or 30% by weight or more of an alcohol component having 6 to 15 carbon atoms 1 to 5 % by weight
(A2) 3 to 20% by weight of a fatty acid ester having a molecular weight of 100 or more and a ClogP value of 6 to 12, and (a3) a water-soluble polymer having an average molecular weight of 4000 or more to 45 to 95% by weight. The bath agent according to claim 1, wherein the fragrance particles are granular particles having a diameter of 0.1 to 5 mm. The bath agent according to claim 1 or 2, comprising 20 to 80% by weight of sodium carbonate. The bath agent according to any one of claims 1 to 3, wherein the total content of sodium carbonate and organic acid is 60 to 98% by weight. The bath agent according to any one of claims 1 to 4, wherein the intensity of the fragrance particles is 0.4 kgf or more at 63 ° C. The bath agent according to any one of claims 1 to 5, comprising 0.1 to 50% by weight of fragrance particles. The bath agent according to any one of claims 1 to 6, wherein the fragrance particles are obtained by dripping after the components (a1) to (a3) are heated and melted and mixed. Furthermore, the bath agent of any one of Claims 1-7 containing a nonionic surfactant. The bath agent according to any one of claims 1 to 8 , wherein the fatty acid ester is a fatty acid ester having a total carbon number of 8 to 40. The bath agent according to any one of claims 1 to 9 , wherein the water-soluble polymer is polyethylene glycol.