JPS584006B2 - Fun matsuyokuyouzainoseizouhouhou - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a process for producing a powder bath agent containing fluorescein salts which emits green fluorescence upon use.

Conventionally, powdered bath preparations containing fluorescein salts, mainly sodium fluorescein (uranine pigment),
Disperse and dissolve uranine pigment in a solvent such as alcohol,
It is manufactured by blending the uranine pigment into a powdered bath agent using a so-called spray method.

However, the bath additives obtained by this method may discolor or fade due to contact with air and the influence of humidity, etc., and the powders can easily stick to each other due to humidity, and the entire bath additive may change from rough to solid. It becomes easier to exhibit such phenomena.

In addition, since it uses a single spray method, it is difficult to mix the uranine pigment uniformly throughout the bath agent, which tends to result in uneven coloring.

Furthermore, the color interference effect of the uranine dye itself is too strong, and the desired color cannot be obtained even if other colorants are added.Therefore, bath preparations using only uranine dye as the formulation color cannot be considered beautiful, and the product value is low. It had the disadvantage of causing a decrease in

The present invention eliminates the above-mentioned drawbacks, and the salts of fluorescein are dissolved in water-containing lower monohydric alcohol, mixed with a small amount of acid and a porous adsorbent material selected from silicon dioxide and alumina powder. Powder baths that can be colored into a desired color by mixing with bath agent raw materials, and that the added colorant is uniformly dispersed and does not become wet, and therefore do not solidify easily, have good storage stability, and have high commercial value. The present invention provides a method for producing an agent.

The method for producing the powder bath preparation according to the present invention will be explained in detail below.

First, fluorescein salts are dissolved in a water-containing lower monohydric alcohol, and a small amount of acid and a porous adsorbent material selected from silicon dioxide and alumina powder are mixed with this alcoholic solution of fluorescein salts.

As fluorescein salts, sodium fluorescein (uranine dye) is mainly used because it is inexpensive, but potassium salts, aluminum salts, etc. are also used.

The alcohol may be any water-containing lower monohydric alcohol such as methyl alcohol, ethyl alcohol, isopropyl alcohol, or n-propyl alcohol with a concentration of about 95%, but 95% ethyl alcohol is preferable because it has excellent solubility of dyes. is suitable.

A crystalline acid such as tartaric anhydride, citric acid anhydride, etc. is used as the acid.

The purpose of blending the acid is to convert some of the fluorescein salts into an acid type or an acid anhydride type, and to cause the dye to be adsorbed onto a porous substance such as silicon dioxide.

As the porous material, silicon dioxide or alumina or a mixture thereof is used.

These porous adsorbent substances do not dissolve in water, but the amount incorporated into bath additives is small, and the amount used in bath additives is approximately 10 g/180 liters, so they do not become cloudy when added to bath water. It does not impair transparency.

As mentioned above, fluorescein salts, mainly uranine dye (sodium fluorescein), are evenly dissolved in alcohol, and by reacting this alcoholic solution of uranine dye with acid, some of the uranine dye can be converted into acid form or acid anhydride form. fluorescein, which allows the uranine dye to be adsorbed onto the porous adsorbent material.

Therefore, the uranine dye is well and evenly adsorbed and blended into the porous adsorbent material, and the interference effect of the uranine dye on other dyes is weakened, so that other dyes can be added to create desired preparations such as green, red, orange, etc. It is possible to obtain color.

In other words, when silicon dioxide is used as a porous adsorbent material and only uranine dye is used, a vivid yellow formulation color can be obtained, and by adding other dyes such as red and blue together with uranine dye, various colors can be obtained. A color of the formulation can be obtained.

In this way, various desired formulation colors can be obtained depending on the type, amount, surface area, and particle size of the porous adsorbent, as well as the type and amount of the dye added.

Pigments such as red and blue used to obtain the desired formulation color for bath agents are dissolved in water-containing lower monohydric alcohol together with uranine dye, and the alcohol solution of these dyes is mixed with acid and porous adsorbent material. After that, it is mixed with other bath agent raw materials to obtain a predetermined formulation color.

Furthermore, if a water-soluble polymeric substance such as methyl cellulose is added to the mixture of the above-mentioned alcoholic dye solution/acid and porous adsorbent material, the storage stability will be further increased.

For example, products containing water-soluble polymeric substances such as methylcellulose can be used at a temperature of 40°C and relative humidity of 85%.
Almost no moisture, discoloration, or odor was observed even after 4 hours of exposure.

A mixture of the above-mentioned alcohol solution/acid of the dye and a porous adsorbent substance, or a mixture of water-soluble polymer substances added to this mixture, is then used as a base material for other bath agents such as sodium sulfate and sodium bicarbonate. agent).

Therefore, the porous adsorbent is uniformly mixed with other bath agent raw materials, and the uranine pigment adsorbed by the porous adsorbent is also uniformly dispersed and blended into the powdered bath agent, resulting in color unevenness. A uniformly colored powder bath agent with no color is obtained.

As other bath agent raw materials, most of the conventionally used raw materials can be used, and suitable materials can be selected and used in combination depending on the purpose.

The mixture of dye/acid and porous adsorbent material with other bath agent raw materials is usually dried at a temperature of 80-90° C. to better remove alcohol and eliminate moisture.

However, since the above-mentioned mixture itself has no moisture and is smooth, the drying step can be omitted.

After drying or without drying, the above mixture is blended with perfume and other necessary ingredients, and finally sieved to make the mesh uniform.

If necessary, the obtained powder bath preparation can be granulated.

As mentioned above, the manufactured powder bath agent has a color that is compatible with the added fragrance or the taste of the consumer, and at the same time, when used in a bath, the amount of other pigments added together with the uranine pigment. Because of the low amount of uranine, the color dissolved in hot water is the same as the color when only uranine pigment is dissolved, giving off a green fluorescent color that gives bathers a sense of comfort.

According to the present invention, as described above, by mixing a small amount of acid and a porous adsorbent material with the uranine dye, the uranine dye is evenly and well adsorbed on the porous adsorbent material, and a bright yellow color can be obtained using only the uranine dye. It was possible to obtain a range of formulation colors, and since the interference effect of uranine dyes on other pigments was weakened, a pigment compatible with the fragrance was added together with uranine dyes to create a powder with the desired formulation color such as green, red, orange, etc. In addition to making it easier to manufacture bath additives, the porous adsorbent material that adsorbs pigments is evenly dispersed in the bath additive base, making it possible to manufacture powdered bath additives with a uniform color without uneven color. did.

Therefore, it is possible to easily produce a powdered bath agent with high commercial value that meets the preferences of beauty users.

Furthermore, according to the present invention, it is possible to obtain a smooth product that has good storage stability, is free of moisture that prevents the entire product from solidifying due to the powders sticking together, and is therefore easy to weigh at the time of use. There is no need to worry about weighing the product, and the powder bath preparation according to the invention is both easy to use and economical.

Furthermore, a powdered bath agent with good fragrance persistence, no odor, and no discoloration or fading, that is, no change in quality over time, can be obtained.

Below are examples of the invention.

Example 1 and Comparative Examples Powdered bathing agents according to the present invention and powdered bathing agents according to the conventional method were manufactured by the following methods, and these bathing agents were examined for solidification, color unevenness, wettability, and storage stability.

Product of the present invention: 0.3 parts by weight of uranine dye is uniformly dissolved in 3.6 parts by weight of ethyl alcohol (95%), and 1 part by weight of anhydrous citric acid and 1.8 parts by weight of silicon dioxide are added thereto.
Furthermore, 0.3 parts by weight of propylcellulose is added and mixed.

Next, 2 parts by weight of borax, 14.5 parts by weight of sodium bicarbonate, and finally 75 parts by weight of dry sodium sulfate are added and mixed well, and then dried at 80 to 90°C for 10 minutes and cooled.

Once cooled to near room temperature, 1.5 parts by weight of lemon flavor was added and mixed well.Finally, sieving was performed to align the mesh to obtain bath agent A with a uniform bright yellow color.

Further, a bath agent B was obtained in exactly the same manner except that silicon dioxide was replaced with alumina powder.

Conventional product: 0.3 parts by weight of uranine dye is uniformly dissolved in 3.6 parts by weight of ethyl alcohol (95%).

Furthermore, 0.3 parts by weight of probilcellulose is added and mixed.

Next, this was sprayed onto a mixture of 2 parts by weight of borax, 17.3 parts by weight of sodium hydrogen carbonate, and 75 parts by weight of dry sodium sulfate, mixed thoroughly, dried for 10 minutes at a temperature of 80 to 90°C, and then cooled. do.

When cooled to near room temperature, 1.5 parts by weight of lemon flavor was added and mixed well.Finally, sieving was performed to align the meshes to obtain a dark orange bath agent C.

Evaluation method: ■ Solidifying commercially available bath agent containers (carton cans with a diameter of 7 cm with a 4 x 2 cm opening formed on the top plate) are filled with a certain amount of the above bath agent, and the container is turned upside down to drain the contents. The solidification properties were evaluated according to the following criteria.

○: Almost no content remains in the container △: Approximately half of the content remains in the container ×: Most of the content remains in the container■ Pour 102 of the above bath agent into an unevenly colored Petri dish (diameter 9.5 cm) and spread evenly. The expanded surface condition was observed, and color unevenness was evaluated according to the following criteria.

○: The degree of coloration is uniform △: The degree of coloration is slightly uneven ×: The degree of coloration is quite uneven■ 7 cm, depth 1.3 cm), 10 g of the above bath agent was taken, and evaluated by the state of adhesion to the measuring pig when the bath agent was turned upside down.

○: Smooth and hardly adheres to the lid △: Slightly moist and slightly adheres to the lid ×: Moist and adheres to the lid considerably ■ Storage stability A commercially available bath agent container was filled with 400 g of the above bath agent. After covering with a lid, it was stored in a constant temperature and humidity room at 35° C. and 85% RH for 7 days, and the above-mentioned (1) solidification property and (2) color unevenness were evaluated.

The results are shown in the table below.

As is clear from the table, the bath agent according to the present invention has solidifying properties,
It can be seen that the color unevenness, moisture, and storage stability are superior to those made using conventional methods.

Example 2 Dye Blue No. 1 was dissolved in ethyl alcohol together with uranine dye.

The product obtained above was uniformly bright green, had no moisture, and had the same effect as the product obtained in Example 1.

The product obtained above had a uniformly beautiful orange color and no moisture, and the same effect as the product obtained in Example 1 was observed.

Example 4 The product obtained above was uniformly red in color and had no moisture, and the same effect as the product obtained in Example 1 was observed.

Claims (1)

[Claims] 1 Dissolve fluorescein salts in water-containing lower monohydric alcohol, mix with the acid and a porous adsorbent selected from silicon dioxide and alumina powder, and then mix this mixture with other powder compositions for bath agents. A method for producing a powder bath agent, which comprises blending the following.