JPS597114A - Preparation of granular composition for emitting fragrance - Google Patents

Abstract

PURPOSE:To obtain the titled composition inexpensively without requiring a specific drying process, by dissolving liquid and/or solid perfume in a solvent having a specific boiling point, volatile at normal temperature, imgregnating a granular porous inorganic material with it, adsorbing it on the material. CONSTITUTION:Perfume liquid and/or solid at normal temperature is dissolved in a solvent (e.g., acetone, methyl alcohol, ethyl acetate, etc.) having 50-90 deg.C boiling point, volatile at normal temperature, the perfume solution is impregnated into a granular porous inorganic material (preferably about 1-10mm. particle diameter, <=10Angstrom pore diameter) such as zeolite, boiling bubble stone, etc., adsorbed on the material, allowed to stand at room temperature, and dried to give a granular composition which will not get greasy on the surface even if it is used as a liquid perfume. Dye and/or pigment is added to the perfume solution, to give a colored, beautiful, granular composition for emitting fragrance having more raised value of commodity.

Description

DETAILED DESCRIPTION OF THE INVENTION (Technical Field) The present invention relates to a method for producing a fragrant granular composition, and more particularly to a method for producing a numberable granular composition colored with a dye and/or a pigment.

(Prior Art) It has been known that porous substances adsorb fragrances (
Tokuko Sho 25-1334. Tokuko Sho 35-1181”7).

1-However, according to these proposals, methods for adsorbing gaseous or vaporous aroma components are described, but no methods for adsorbing liquid fragrances and/or solid fragrances are disclosed. .

Furthermore, no method has been clarified regarding the production of fragrance-producing granular compositions which have conventionally been colored with dyes and pigments and have high commercial value.

In general, when a liquid fragrance is simply impregnated into a granular porous inorganic material and adsorbed, or is sprayed and adsorbed, the liquid fragrance sticks to the surface of the obtained granular composition.
Drying required a lot of effort, such as blowing hot air or hot air and stirring.

Further, even if such a drying process is carried out, the drying is often insufficient, resulting in problems such as staining the storage container 2 and clothes.

In the case of solid fragrances, since they are solids, no attempt has been made to make them adsorbed onto granular porous inorganic materials, and a method for producing fragrant granular compositions has not been clarified. Furthermore, no method has been disclosed for producing a colored granular composition using a solid fragrance.

(Object of the invention) The object of the present invention is to produce a fragrant granular composition by:
To provide a manufacturing method that prevents the surface of a fragrant granular composition from becoming sticky with a liquid fragrance without using a special drying process.

Another object of the present invention is to develop a method for adsorbing solid perfumes onto particulate porous minerals.

A further object of the present invention is to provide a method for producing a fragrant granular composition colored with dyes and/or pigments and having excellent commercial value.

(Structure of the Invention) In order to solve the various problems as described above, the present inventors have conducted intensive research and found that liquid fragrance and/or solid fragrance are once dissolved in a room-temperature volatile solvent with a boiling point of 50°C to 90°C. By dissolving dyes and/or pigments in a perfume solvent bath solution obtained by mixing and dissolving them, the dyes and/or pigments are impregnated into a granular porous inorganic material and adsorbed thereon, thereby solving the above objects at once and completing the present invention. The dye and/or pigment may be mixed and dissolved in a liquid perfume or a volatile solvent at room temperature before use.

In one embodiment of the present invention, dyes and/or pigments are dissolved in a perfume solvent solution obtained by mixing and dissolving liquid perfume and/or solid perfume in a room temperature volatile solvent with a boiling point of 50°C to 90°C. , it is impregnated into a granular porous inorganic material, and allowed to stand overnight at room temperature (20° C.) to be adsorbed. Excess unadsorbed perfume solvent solution is then removed by a natural filtration operation.

The colored fragrant granular composition is kept at room temperature (20°C) for about 20 minutes on a laboratory scale, and for about 2 to 20 minutes at room temperature (20°C) even in large-scale production.
When left for 3 hours, drying is completed, and even when a liquid fragrance is used, a granular composition with high commercial value is obtained whose surface is not sticky due to the liquid fragrance.

A detailed explanation of the constituent elements of the present invention is as follows.

(Granular porous inorganic material) The granular porous inorganic material used in the present invention has a diameter of about 1
It is a porous inorganic material such as granular zeolite, boiling stone, etc. with a size of about mm to IQmm. When using synthetics that are relatively chemotactic in composition and particle size, fragrant particulate compositions that are beautiful and have higher commercial value are obtained. There are no particular limitations on the pore diameter, but pore diameters of 10 angstroms or less are usually used.

(Fragrance) The liquid fragrance and solid fragrance used in the present invention are fragrances that are not gaseous or vaporous but liquid or solid at room temperature, and include natural fragrances, synthetic fragrances, and mixed fragrances.

Examples of natural fragrances include orange oil, lemon oil,
Examples include penoq-mint oil, rose oil, and jasmine oil.

Examples of synthetic fragrances include hydrocarbons, alcohols, phenols, aldehydes, ketones, lactones, esters, oxides, and acids.

Among synthetic fragrances, examples of solid fragrances include menthol,
Vanillin, ethervanillin, coumarin, cinnamic acid, heliotropin, methylnaphthyl ketone, zerneol, nitro musks such as musk quidylol, musk ketone, musk en bread, indane musks such as fantolid, celethride, and tonalid. Tetralin-based musks can produce shimmering effects. Examples of blended fragrances include rose, jasmine, mugette, and other blended fragrances that can be commonly used in cosmetics, as well as strawberry, grapefruit, melon, chocolate, and cola nuts.

The weight of the fragrance to be used relative to the granular porous inorganic material can be arbitrarily selected depending on the desired odor intensity of the fragrant granular composition.

(Normal temperature volatile solvent) A room temperature volatile solvent has a boiling point in the range of 50°C to 90°C, and includes, for example, acetone, methyl alcohol, hexano,
Examples include ethyl acetate, ether alcohol, isopropyl alcohol, and diimpropyl ether.

It is not preferable to use a solvent with a boiling point that is too low because there is a risk of ignition when heat of adsorption is generated.

It is not preferable to use a solvent with a boiling point that is too high because it takes a long time to dry.

In order to achieve the purpose of the present invention, the boiling point is 50°C to 90°C.
range is most suitable.

(Fragrance Solvent Solution) It is preferable that the perfume solvent solution be mixed with the granular porous inorganic material so that the solution is still soaked when adsorption is completed.

The adsorption amount of the solution varies depending on the type of granular porous inorganic material, and in general, the larger the pore diameter, the greater the adsorption amount. There is also a difference depending on whether or not.

Therefore, the amount of perfume solvent solution to be used should be selected appropriately taking into consideration the properties of the granular porous inorganic material.

If the concentration of fragrance in the solvent is too high, it will be difficult to dry.
If it is too low, the resulting fragrant granular composition will have a weak odor, which is not preferable. Preferably about 20-8
0% by weight is adopted.

(Dye, Pigment) The dye and pigment used in the present invention are not particularly limited as long as they are soluble in the perfume solvent solution. Examples of highly safe and beautiful colors include Yellow No. 406 (Methanil Yellow) and Blue No. 1 (Brilliant Blue 1i' O).
F), red No. 106 (acid red), etc. can be used. Among pigments that are soluble in alcohol, there are Red No. 205 (Resol Red) and Red No. 219 (Brilliant Lake Red It). These colors can also be mixed arbitrarily with each other. There is no harm in using an antioxidant in combination to prevent discoloration. The antioxidant used is butylno-idroxytoluene? , can be given. The amount of dye and/or pigment used is 0.1% by weight based on the fragrance solvent solution.
The effect is fully demonstrated below.

It is sufficient that the amount of antioxidant used is less than one part per part of the perfume solvent solution.

(Effects of the Invention) According to the production method of the present invention, there is no need for any special drying process, so the cost is low, and the obtained fragrant granular composition has a liquid fragrance that is not sticky and is beautifully colored. It is of excellent quality and has a high commercial value.

(Examples) Next, the present invention will be explained in more detail by describing examples of the present invention, but the present invention is not limited in any way by the following examples.

Example 1 5 kg of Chassis No. 4 (manufactured by Kobayashi Perfume Co., Ltd.) was dissolved in 5 kg of 95% undenatured ethanol, and 10 kg of fragrance solvent solution was prepared.
Don't put a 9 on it. Furthermore, blue No. 1, 102ff: After dissolving it, add granular boiling stone (manufactured by Motoyama Pharmaceutical Co., Ltd.) 10
When the mixture was mixed into 1 kg, the internal temperature rose to 295°C.

After the mixture was left at room temperature (20° C.) overnight, excess perfume solvent solution was removed by gravity filtration. When the blue colored fragrant granular composition was left at room temperature (20°C) for 2 hours,
After drying, the yield was 11.8 kg (118% by weight based on the granular boiling stone used).

Example 2 Muguette 452 was dissolved in -N (manufactured by Kobayashi Perfume ■[)3f'e-R Isozolopyl Alcohol Shoten Co., Ltd.] 32 to prepare 6ft of a perfume solvent solution. Furthermore, yellow No. 406 0. After dissolving 0 0 6 f i, this was mixed into 9f of granular boiling stone (manufactured by Motoyama Yakuhin Kogyo ■), and the internal temperature rose to 29°C. The mixture was left to stand overnight at room temperature (20°C) and then filtered by gravity to remove excess perfume solvent solution.

The yellow colored fragrant granular composition was heated in a room @ (20℃) for 2 hours.
When left for 0 minutes, it dried and the yield was 10.5 F (
It was 117% by weight based on the granular boiling stone used.

Example 3 Melon Flavor FO (Kobayashi Perfume ■ff) was dissolved in 2 g of 8y gold-grade acetone (manufactured by Morizuihikotabe Shoten) to prepare a flavor solvent solution 10F. Furthermore, yellow No. 406 0. OO7g
After dissolving 0.0031/ml of Blue No. 1, this was mixed in 10 y of Zeorum A-4 (Toyo Soda Kogyo M), and the internal temperature rose to 355°C. After standing at room temperature overnight, excess perfume solvent solution was removed by natural pore filtration. When the green colored fragrant granular composition was left in a room @ (20°C), it dried in 15 minutes and the yield was 12. Of(
(120% by weight based on the Zeolum A-4 used).

Example 4 0-Z KT) B (manufactured by Kobayashi Perfume ■) 242 was grade 1 n
-Dissolve in 367 hexane (manufactured by Shuzuihikotabe Shoten) to prepare a fragrance solvent solution 67. Furthermore, red No. 106 0. O
After all O6y is dissolved, this is all the liquid) Igu-134
(manufactured by Kurita Kogyo ■) When mixed in 6 g, the temperature rose to 49°C. After the mixture was allowed to stand overnight at room temperature (20°C), excess perfume solvent bath 1 was removed by gravity filtration. The red colored fragrant granular composition was left at room temperature (20°C) and dried in 20 minutes, with a yield of 827% (137% by weight based on Illit K-154).

Example 5 Grapefruit HK 2167 (manufactured by Kobayashi Kogyo ■) 3
2 was dissolved in 7 grams of primary isopropyl ether (manufactured by Kanto Kagaku ■) to make a fragrance solvent solution 102, and then yellow 40
After No. 6 o and o i y were dissolved, this was mixed into Mizuriki Sheeps 4A (manufactured by Mizusawa Kagaku Kogyo ■) 81, and the internal temperature rose to 325°C. After standing at room temperature (20°C) overnight, excess perfume solvent solution was removed by gravity filtration.

The yellow colored fragrant granular composition was left at room temperature (20°C) for 30 minutes and then dried, with a yield of 1.0.2F.
(128% by weight based on the used Mizuriki Thieves 4A).

Example 6 Powdered solid fragrance 2y consisting of 50% by weight of borneol, 10% by weight of coumarin, and 40% by weight of vanillin was dissolved in 195% undenatured ethanol 82% to make 10g of fragrance solvent solution, and red No. 106 o, o i y After dissolving it, it is mixed with granular boiling stone (manufactured by Yoneyama Yakuhin Kogyo ■) 102
When mixed inside, the internal temperature rose to 29°C. After the mixture was left at room temperature (20° C.) overnight, excess perfume solvent solution was removed by gravity filtration. The red colored fragrant granular composition was allowed to stand at room temperature (20° C.) for 30 minutes and dried, with a yield of 1132 (113% by weight based on the granular zeolites used).

Example 7 Solid fragrance t-menthol 5 ii”t 95% undenatured ethanol 59 was dissolved to prepare a fragrance solvent solution 10y,
Furthermore, Blue No. 1 0.01fff: After being dissolved, this was mixed into granular boiling stone (manufactured by Yoneyama Yakuhin Kogyo ■) 102, and the internal temperature rose to 295°C. As it is\room temperature (2
0° C.), and then operated in the same manner as in Example 6. 1. 118 grams of a numberable granular composition colored blue (118% by weight based on the granular evolite used) was obtained.

Patent applicant: Kobayashi Fragrance Co., Ltd.

Claims (2)

[Claims] (1) A method of development characterized by impregnating and adsorbing a granular porous inorganic material with a perfume solvent solution obtained by mixing and dissolving a liquid perfume and/or a solid perfume in a volatile solvent at room temperature with a boiling point of 50°C to 90°C. A method for producing a fragrant granular composition. (2) The manufacturing method according to claim 1, wherein the perfume solvent solution is a solution colored with a dye and/or a pigment.