JP5670660B2 - Bath agent composition - Google Patents

Description

  The present invention relates to an effervescent tablet-type bath composition having a moderate fragrance and excellent high-temperature stability.

  It has been known that a bath preparation containing a carbon dioxide gas generator in which a carbonate and an acid are combined has an excellent blood circulation promoting effect and enhances a feeling of relaxation and refreshment (see, for example, 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, since the perfume contains highly volatile components, the perfume volatilizes during storage of the bath preparation, and the scent may change or a strange odor may be generated. Then, the technique which stabilizes the fragrance during preservation | save by granulating a fragrance | flavor with water-soluble polymer is reported (refer patent document 2).

  Moreover, in the bath agent which mix | blended the carbon dioxide generator, since a fragrance | flavor tends to volatilize simultaneously with foaming, there exists a problem that it is difficult to maintain a stable fragrance for a long time during bathing.

JP 59-70609 JP 2000-229843 A

  A bath agent made by compressing perfume particles granulated with a water-soluble polymer together with a carbon dioxide gas generator that combines carbonate and acid has a low perfume rate (ratio of perfume ingredients in the bath agent). There is no particular problem with storage stability. However, when the aromatization rate is 1% by mass or more, when the bath agent is placed in a high temperature environment of about 50 ° C., the dissolution of the perfume particles causes the dissolved water-soluble polymer or the perfume to dissolve the carbonate. The reaction of the acid proceeds to generate carbon dioxide, and phenomena such as swelling of the packaging material and reduced tablet solubility are observed. In addition, when a fragrance particle composed of a water-soluble polymer and a fragrance is perfumed into a bath agent so that the perfume rate is 1% by mass or more, the perfume component floats on the surface of the bath water, resulting in excessive fragrance. May also occur.

  Accordingly, an object of the present invention is to provide an effervescent tablet-type bath agent having an appropriate scent, excellent scent stability, and good storage stability even at a high temperature of 50 ° C.

  Therefore, as a result of various investigations aimed at achieving an appropriate fragrance in the foamable tablet-type bath agent and the storage stability of the fragrance particles at 50 ° C., the present inventors have found that the fragrance component contains a terpene or sesquiterpene hydrocarbon. By adding water-soluble polymer and nonionic surfactant to granulate perfume particles and formulating it with a carbon dioxide gas generator, the stability of the aroma is good, and the quality and strength of the aroma inherent in the perfume ingredients. It was also found that a tablet-type bath preparation having excellent stability at a high temperature of 50 ° C. can be obtained even when the perfume is 1% by mass or more.

That is, the present invention is an effervescent tablet containing the following components (A) to (C), and the total content of the components (a1) and (a2) in the bath preparation composition is 1 to 3% by mass. A bath agent composition is provided.
(A) Fragrance particles containing components (a1) to (a4) 10 to 30% by mass in bath agent composition
(a1) Fragrance ingredient (excluding ingredient (a2)) 7-25% by mass in the fragrance particles
(a2) Terpene hydrocarbon or sesquiterpene hydrocarbon 0.5 to 1.9% by mass in perfume particles
(a3) Nonionic surfactant 0.5 to 1% by mass in perfume particles
(a4) Water-soluble polymer having a weight average molecular weight of 2000 or more 67 to 92% by mass in perfume particles
(B) Sodium bicarbonate and / or sodium carbonate
(C) Organic acid

  The bath agent composition of the present invention provides a fragrance with an appropriate fragrance strength while maintaining the quality of the scent inherent in the fragrance component, is excellent in scent stability, and is excellent in storage stability even at 50 ° C. Furthermore, since the bath agent composition of the present invention can prevent oil from being floated by the fragrance on the surface of the bath water during use by adding a nonionic surfactant to the fragrance particles, the appearance during use is also good.

[(A): Fragrance particles]
The bath agent composition of the present invention contains perfume particles containing the components (a1), (a2), (a3) and (a4) as the component (A). Ingredients (a1), (a2), (a3), and (a4) are not simply blended into the bath preparation, but are blended into the fragrance particles so that the fragrance and fragrance when flavoring the fragrance at a high concentration It is important to ensure the stability of the material and the high temperature stability at 50 ℃.

Ingredient (a1): Perfume ingredients other than ingredient (a2) As perfume ingredients of ingredient (a1), for example, “Synthetic perfume chemistry and product knowledge” (Motoichi Indo, Kagaku Kogyo Nippo, revised edition 2005) ), Other than terpene hydrocarbons and sesquiterpene hydrocarbons corresponding to component (a2), that is, alcohols, aldehydes, ketones, ethers, oxides, esters, lactones A fragrance | flavor etc. can be used. The fragrance component of component (a1) can be blended into the fragrance particles as various blended fragrances according to the desired fragrance such as citrus, green, floral, herb and the like.

  The component (a1) is contained in the fragrance particles of the component (A) in an amount of 7 to 25% by mass, preferably 10 to 25% by mass, whereby a rich and mellow fragrance and scent persistence are obtained, It can also give a fresh feeling to the top note and is effective in enhancing the sustainability of the scent on the skin after bathing.

Component (a2): terpene hydrocarbon, sesquiterpene hydrocarbon The terpene hydrocarbon or sesquiterpene hydrocarbon of component (a2) has a role of increasing the storage stability of the tablet bath at high temperatures. By containing the terpene hydrocarbon or sesquiterpene hydrocarbon in the fragrance particles of the component (A), the storage stability at a high temperature of 50 ° C. can be ensured even if the fragrance rate is 1% by mass or more. it can.

  Specific examples of the terpene hydrocarbon and sesquiterpene hydrocarbon of the component (a2) include myrcene, ocimene, camphene, tarpinolene, alpha-terpinene, ferrandlene, alphaferrandlene, paracymene, farnesene, cedrene, longiforene, copaene, Examples include Guayen, Patchoulen, and Gurjunen. From the viewpoint of conspicuous fragrance quality inherent in the fragrance component of the component (a1), when the fragrance component of the component (a1) is a citrus fragrance, myrcene, alphaferrandylene, and terpinolene are preferable, and the component (a1) When the fragrance component is a green scent, paracymene or osymene is preferable.When the fragrance component of the component (a1) is a floral scent, myrcene, osimene or farnesene is preferable, and the fragrance component of the component (a1) is In the case of herbal scents, camphene, myrcene and alphaterpinene are preferred. Of these, myrcene, ocimene, farnesene, and paracymene are also frequently used fragrances and are particularly preferable.

  These component (a2) terpene or sesquiterpene hydrocarbons can be used alone or in combination of two or more. The content of the component (a2) in the fragrance particles of the component (A) is 0.5 to 1.9 mass from the viewpoint of maintaining the original fragrance that the component (a1) originally has and the stability of the bathing agent at high temperature. %, Preferably 0.8 to 1.7% by mass, and more preferably 1.0 to 1.5% by mass.

  In the bath preparation composition of the present invention, the total content of the fragrance component of component (a1) and the terpene hydrocarbons and sesquiterpene hydrocarbons of component (a2) is fragrant, long lasting, to the skin From the viewpoint of sustainability of the scent, it is 1 to 3% by mass, preferably 1.2 to 3% by mass, and more preferably 1.5 to 3% by mass.

  In addition, the blending ratio (mass ratio) of the fragrance component of component (a1) and the terpene hydrocarbon and sesquiterpene hydrocarbon of component (a2) is determined in addition to the storage stability of the bath agent composition, From the viewpoint of maintaining strength, (a1) :( a2) = 30: 1 to 5: 1 is preferable, 20: 1 to 5: 1 is more preferable, and 12: 1 to 5: 1 is particularly preferable.

・ Ingredient (a3): Nonionic surfactant By blending the nonionic surfactant of ingredient (a3), the use of the bath agent prevents the fragrance ingredient from floating on the surface of the bath water and causing excessive fragrance. Furthermore, the appearance at the time of use becomes comfortable. Moreover, even if the perfume rate is 1% by mass or more, the storage stability is excellent at a high temperature of 50 ° C.

  Examples of the nonionic surfactant of component (a3) include polyoxyalkylene alkyl ethers, polyoxyalkylene alkenyl ethers, and sucrose fatty acid esters.

  As the polyoxyalkylene alkyl ether, those having 2 to 3 carbon atoms of alkylene, 7 to 14 carbon atoms of oxyalkylene, and 14 to 20 carbon atoms of alkyl are preferable. Specific examples include polyoxyethylene (EO = 7) cetyl ether, polyoxyethylene (EO = 10) cetyl ether, polyoxyethylene (EO = 12) cetyl ether, polyoxyethylene (EO = 13) cetyl ether, poly Examples thereof include oxyethylene (EO = 8) stearyl ether, polyoxyethylene (EO = 9) stearyl ether, polyoxyethylene (EO = 13) stearyl ether and the like.

  As the polyoxyalkylene alkenyl ether, those having 2 to 3 carbon atoms of alkylene, 7 to 14 carbon atoms of oxyalkylene, and 14 to 20 carbon atoms of alkenyl are preferable. Specific examples include polyoxyethylene (EO = 8) oleyl ether and polyoxyethylene (EO = 9) oleyl ether.

  Of these, polyoxyethylene (EO = 7) cetyl ether, polyoxyethylene (EO = 13) cetyl ether, polyoxyethylene (EO = 9) Oleyl ether is particularly preferred.

  In addition, the sucrose fatty acid ester is preferably one having an HLB of 16 or less, more preferably 15 or less, from the viewpoint of dispersion of the fragrance component of the component (a1) in the bath water and fragrance. Examples include sucrose behenic acid ester, sucrose stearic acid ester, sucrose palmitic acid ester, sucrose myristic acid ester, sucrose lauric acid ester, sucrose oleic acid ester and the like.

  The nonionic surfactant of component (a3) is a combination of polyoxyalkylene alkyl or polyoxyalkenyl ether and sucrose fatty acid ester from the viewpoint of dispersion and flavoring of the fragrance component of component (a1) in bath water. From the viewpoint of fragrance, the compounding ratio (mass ratio) of polyoxyalkylene alkyl ether or polyoxyalkylene alkenyl ether and sucrose fatty acid ester is preferably 2: 1 to 5: 1. Further, 3: 1 to 5: 1 is particularly preferable.

  The content of the component (a3) in the fragrance particles of the component (A) is particularly preferable from the viewpoint of dispersion of the fragrance component of the component (a1) in the bath water and appropriate scenting at the time of dissolution in the bath water. It is 0.5 to 1.0% by mass, and preferably 0.6 to 1.0% by mass in terms of maintaining the fragrance quality and strength inherent in a1).

  The ratio of the total content of components (a1) and (a2) to the content of component (a3) is 10: 1 to 40: 1 from the viewpoint of dispersion in the fragrance components in the bath water and fragrance. Is more preferable, and 15: 1 to 25: 1 is more preferable.

・ Component (a4): Water-soluble polymer having a weight average molecular weight of 2000 or more Component (a4) is a water-soluble polymer having a weight average molecular weight of 2000 or more, and is an important component from the viewpoint of stabilizing perfume and producing a fragrance. .

  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, for example, 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. Natural 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, and cationic starch; Synthetic water-soluble polymers such as polyacrylic acid soda, polyethyleneimine, polyvinyl alcohol, polyethylene glycol, and polyvinylpyrrolidone Gerare can use one or more. Among these, polyethylene glycol, particularly polyethylene glycol having a weight average molecular weight of 2000 to 20000 is preferable.

  These water-soluble polymers of component (a4) can be used alone or in combination of two or more, and the content of component (a4) in the fragrance particles of component (A) From the standpoint of sustainability and storage stability of the bath agent composition at high temperatures, it is 67 to 92% by mass, preferably 70 to 90% by mass, and more preferably 73 to 90% by mass.

  The perfume particles of the component (A) can be produced, for example, by a rolling granulation method, a spray drying granulation method, a centrifugal granulation method, a stirring granulation method, a drop-on-plate granulation method or the like. In particular, a method capable of producing particles having a small particle diameter from a lump or liquid is preferable. For example, the perfume particles of the present invention are obtained by heating and melting the components (a1) to (a4) and mixing them uniformly, then dropping a predetermined amount onto a flat plate, solidifying, granulating, and granulating It is preferable to obtain a shaped particle (drop-on-plate granulation method). The heating and melting temperature is preferably a temperature at which the water-soluble polymer of the component (a4) to be used melts.

  The perfume particles of component (A) preferably have a particle size of 100 to 2000 μm, particularly 500 to 1500 μm, from the standpoint of fragrance, scent freshness, and scent persistence. The particle size is selected and measured by a sieve method using a sieve with openings defined in JIS Z 8801.

  Although the fragrance | flavor particle | grains of a component (A) contain 10-30 mass% in the bath agent composition of this invention, it contains 10-25 mass%, Furthermore, 12-25 mass% contained in the bath water. It is preferable from the standpoint of fragrance and sustainability.

[(B) + (C): Carbon dioxide generator]
The bath agent composition of the present invention contains sodium hydrogen carbonate 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 and fumaric acid are particularly preferable.

  Sodium bicarbonate and / or sodium carbonate is contained in a total amount of 10 to 60% by mass, particularly 10 to 50% by mass, in the bath agent composition of the present invention, so that sufficient carbon dioxide gas can be dissolved in the bath water. Therefore, it is preferable. In addition, since the organic acid is contained in the total amount of the organic acid in the bath agent composition of the present invention in an amount of 20 to 60% by mass, particularly 30 to 60% by mass, sufficient carbon dioxide gas can be dissolved in the bath water. preferable. Furthermore, the total content of sodium bicarbonate and / or sodium carbonate and the organic acid is preferably 40 to 85% by mass, particularly preferably 50 to 85% by mass.

The bath agent composition of the present invention may further contain components usually used in bath agents, such as inorganic salts, inorganic acids, crude drugs, fats and oils, alcohols, medicinal agents, pigments, vitamins and the like.
The bath agent composition 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 composition 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.

Production Example 1 (Production of perfume particles)
87.4 parts by mass of polyethylene glycol 6000 (weight average molecular weight 7500) was melted at about 60 ° C., and 11 parts by mass of the fragrance component of component (a1), 0.5 parts by mass of myrcene, 0.5 parts by mass of osimene, and component (a3) of component (a2) And 0.5 part by mass of polyoxyethylene cetyl ether and 0.1 part by mass of sucrose fatty acid ester were added and dissolved. After this was uniformly mixed, it was dropped on a flat plate at 20 ° C. and granulated into particles having a diameter of 100 to 2000 μm (measured with a sieve: major axis) to obtain perfume particles 1.
Fragrance particles 2 to 15 shown in Tables 1 and 2 were produced in the same manner.

Examples 1-8, Comparative Examples 1-8
Using the fragrance particles shown in Tables 1 and 2 obtained in Production Example 1, uniformly blended with the compositions shown in Tables 3 and 4, and tableting 100 g with a hydraulic tableting machine, bath composition The following [Evaluation of stability], [Evaluation of oil floating on the water surface] and [Evaluation of fragrance and sustainability] were performed. Moreover, [Evaluation of fragrance quality] was performed using the fragrance particles themselves.
Of the bath agent compositions shown in Table 3, Examples 5 and 8 are reference examples and are not included in the scope of the claims.

[Stability evaluation at 50 ℃]
After packing 100 g of a bath preparation composition tableted and molded with an aluminum pillow, place it in a thermostatic bath at 50 ° C., and the state of the aluminum pillow after 30 days will be visually checked by five professional panelists according to the following evaluation criteria. Evaluated. Evaluation was determined by consultation. The results are shown in Tables 3 and 4.

(Stability evaluation criteria)
1: No change in the appearance of the aluminum pillow is observed 2: Slight swelling is observed in the appearance of the aluminum pillow 3: Slight swelling is observed in the aluminum pillow 4: Swelling is recognized in the aluminum pillow

[Evaluation of oil floating on the water surface after dissolution]
In a 250 liter bath, put 40 ℃, 150 liter of hot water, dissolve 100 g of the tablet that was molded into a tablet, and five expert panelists evaluated the following conditions of oil floating on the water surface after dissolution. Visual evaluation was performed according to the standard. Evaluation was determined by consultation. The results are shown in Tables 3 and 4.

(Evaluation criteria for oil float on the water surface)
1: Does not allow oil float 2: Accepts oil float slightly 3: Accepts oil float

[Evaluation of fragrance and sustainability]
Into a 250 liter bath, put 150 liters of hot water at 40 ° C. Dissolve 100 g of a tablet that was molded into a tablet. Five professional panelists will give you a fragrance immediately after dissolution and 1 hour after dissolution. Evaluated according to the following evaluation criteria. Evaluation was determined by consultation. The results are shown in Tables 3 and 4.
Furthermore, the difference between “scenting immediately after dissolution” and “scenting 1 hour after dissolution” was calculated and used as [evaluation of sustainability]. The difference between (fragrance immediately after dissolution) and (fragrance after 1 hour after dissolution) is preferably within one. The results are shown in Tables 3 and 4.

(Evaluation criteria for fragrance)
1: Odorless 2: Slightly scented 3: Slightly scented 4: Scented well (setting range)
5: Scented clearly (setting range)
6: Strongly scented 7: Slightly scented

[Evaluation of fragrance quality]
Since the terpene or sesquiterpene hydrocarbon of component (a2) has a fragrance, adding component (a2) to the fragrance component of component (a1) may change the inherent fragrance of component (a1) . Therefore, evaluation was performed to confirm whether or not the fragrance was originally possessed by the component (a1).
That is, in the formulation of fragrance particles shown in Tables 1 and 2, fragrance particles not containing the component (a2) were prepared, and the fragrance quality of the fragrance particles shown in Tables 1 and 2 and the fragrance not containing the above component (a2) The quality of the scent of the particles was compared and evaluated.
20 g of each fragrance particle was dissolved in 150 liters of hot water at 40 ° C., and the fragrance immediately after dissolution of the whole amount was subjected to sensory evaluation by five panelists. Evaluation was determined by consultation. The results are shown in Tables 3 and 4 together.

(Evaluation criteria for fragrance quality)
1: It has the original fragrance of the fragrance component of component (a1) 2: It is almost the same as the original fragrance of the fragrance component of component (a1) 3: Slightly different from the original fragrance of the fragrance component of component (a1) 4: Component Different from the original fragrance of the fragrance component (a1)

〔Comprehensive evaluation〕
The overall evaluation is based on the following criteria in consideration of [stability evaluation], [evaluation of oil floating on the water surface], [evaluation of fragrance quality], and [evaluation of fragrance standing and sustainability]. Judgment.
(Evaluation criteria)
1: As a result of comprehensive evaluation of each evaluation, the effect is extremely excellent 2: As a result of comprehensive evaluation of each evaluation, the effect is excellent 3: As a result of comprehensive evaluation of each evaluation, the effect is sufficient 4: As a result of comprehensive evaluation of each evaluation, the effect is slightly insufficient 5: As a result of comprehensive evaluation of each evaluation, the effect is insufficient

Claims (4)

A effervescent tablets containing the following ingredients (A) ~ (C), Ri total content 1-3% by mass in the bath preparation composition components (a1) and (a2), and perfume the total content and ratio of content of the component (a3) is 10 components in the particles (a1) and (a2): 1~40: 1 der Ru bath composition.
(A) Fragrance particles containing components (a1) to (a4) 10 to 30% by mass in bath agent composition
(a1) Fragrance ingredient (excluding ingredient (a2)) 7-25% by mass in the fragrance particles
(a2) Terpene hydrocarbon or sesquiterpene hydrocarbon 0.8 to 1.7 % by mass in perfume particles
(a3) Nonionic surfactant 0.5 to 1% by mass in perfume particles
(a4) Water-soluble polymer having a weight average molecular weight of 2000 or more 67 to 92% by mass in perfume particles
(B) Sodium bicarbonate and / or sodium carbonate
(C) Organic acid   The bath agent composition according to claim 1, wherein (a3) the nonionic surfactant is at least one selected from polyoxyalkylene alkyl ethers, polyoxyalkylene alkenyl ethers and sucrose fatty acid esters.   (a4) The bath composition according to claim 1 or 2, wherein the water-soluble polymer is polyethylene glycol. The bath agent composition according to any one of claims 1 to 3 , wherein the particle diameter of the perfume particles of the component (A) is 100 to 2000 µm.