JPS5834141B2 - fragrance composition - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a fragrance composition in which activated alumina or alumina-silica spheres having a diameter of 1 square meter or more are impregnated with a liquid fragrance.

The purpose of the present invention is to increase the fragrance content in activated aluminum or alumina-silica spheres as much as possible, so that the duration of fragrance generation is significantly longer than that of conventional products of this kind, and, moreover, the fragrance generated is The object of the present invention is to provide a fragrance composition that approximates the fragrance of a desired liquid fragrance.

As a conventionally known fragrance of this kind, there is a powder fragrance (Japanese Patent Publication No. 1989-1999), which is made by adsorbing fragrance vapor to synthetic magnesium silicate powder.
No. 1334), a powder or gel fragrance obtained by adding and solidifying an aerogel of silicic anhydride of 500 A or less to a liquid fragrance (Japanese Patent Publication No. 315100), and a composition in which a fragrance is adsorbed on a crystalline zeolite molecular sieve. (Japanese Patent Publication No. 35-11817).

Each of these broadcasting products has its own unique characteristics and is useful, but they require a step-by-step improvement in terms of ease of portability and handling, economy, and sustainability of dialing. Hope 1
It was

Furthermore, attempts have recently been made to impregnate activated alumina spheres (' = ! or activated aluminum/silica spheres, hereinafter the same) with liquid fragrance to make fragrance-impregnated alumina spheres, but the following problems arise. Due to unresolved issues, it is difficult to commercialize the product in practical terms, and it is unlikely that it will become widespread beyond the sample level.

The unresolved problem is that although it shows a favorable number when used as a liquid fragrance, when activated alumina spheres are impregnated with this fragrance, the fragrance emitted from the sphere is the same as that of the original liquid fragrance. The fact is that it has a completely different aroma, and moreover, it has a slightly irritating effect, and the mild aroma characteristic of perfumes is lost.

According to experiments conducted by the present inventors, this phenomenon tends to become stronger as the diameter of the activated alumina sphere increases and as the amount of fragrance impregnated into the sphere increases; .5
If it is less than a millimeter, this phenomenon will hardly be a problem.
However, this tendency gradually becomes stronger when the ball diameter increases from 0.5 to 1 mm, and when the ball diameter exceeds 1 mm, this phenomenon cannot be avoided unless the amount of perfume impregnated is less than 10 weight φ of the ball. It was obvious.

Therefore, if an attempt was made to prolong the persistence of fragrance by impregnating activated alumina spheres with a diameter of 1 mm or more with the perfume up to 10% by weight, it was necessary to solve this problem.

Another problem is that when an activated alumina sphere is impregnated with a liquid fragrance upstream by 10 weight, a large amount of adsorption heat is generated compared to when the amount of fragrance is less than 10 weight. A phenomenon is observed in which the spherical structure is destroyed, or even if the casing is destroyed, the structure becomes brittle and the particle strength and wear resistance deteriorate.

Because these two problems have not been resolved, this type of fragrance composition, which is currently available as a sample or as a part of the product, is
Either the sphere diameter is small, or even if the sphere diameter is large, the amount of perfume impregnated is limited to a small amount, and as a result, these conventional products have the disadvantage of a short duration of fragrance production.

As a result of intensive research aimed at solving the above problems, the present inventors have solved these problems and completed an inventive product that is not found in conventional products. is fragrance-impregnated aluminum with a diameter of 1 mm or more
When preparing spheres, the composition ratio of alumina to silica is 1.
Activated alumina or activated alumina/silica spheres with a ratio of 0:0 to 10:90 are used, and the perfume to be impregnated into the spheres uses the perfume composition when used as a perfume in liquid form. This fragrance is characterized by making a certain range of formulation corrections and then impregnating the activated alumina spheres or activated alumina or silica spheres in an amount of 10 to 30 of the weight of the perfume.

Hereinafter, to describe the fragrance composition of the present invention in more detail, the activated alumina or activated alumina/silica spheres used in the present invention have a composition ratio of alumina to silica of 100 to O.
The liquid fragrance ranges from 10 to 90, with 10 to 30
As long as it has the ability to adsorb heavy weight, it doesn't really matter how it is manufactured.

Normally, a mixture of silica sol and basic aluminum sol is passed through an immiscible solvent, and when it becomes spherical due to surface tension, it is heated to form a spherical hydrogel, which is then washed with water, dried, and calcined. It will be done.

The present inventors conducted repeated experiments in which activated alumina spheres were made to adsorb liquid fragrance of 10 mm or more, and found that the amount of impregnated fragrance was 2.
When the weight reaches 0 to 30 φ, the particles will break due to the heat of adsorption, or even if they do not break, the strength of the particles will decrease.This tendency is due to the silica ratio in the balls. We found that the higher the value, the greater the value.

Additionally, it has been surprisingly discovered that the time required to impregnate the bulb with perfume increases in proportion to the silica ratio in the bulb.

In the present invention, based on the above-mentioned findings, the activated alumina-silica spheres to be used are limited to a composition ratio of alumina to silica in the range of 100:0 to 10:90.

For the purpose of the present invention, prior to impregnating the activated alumina spheres with perfume, suitable pre-treatments such as calcination, alkali treatment, etc., may be carried out in order to improve or modify the adsorption properties of the activated alumina spheres. There is no problem if there is only one line.

Next, regarding the fact that the fragrance generated by the fragrance-impregnated alumina bulb gives a completely different fragrance from the fragrance of the fragrance before impregnation, in the present invention, the boiling point component of the liquid fragrance below 250 ° C. 3 to 30% by weight of the total amount of fragrance or /button and other single fragrances that have a boiling point close to the high boiling point components of the fragrance above 270°C and have the effect of masking the high boiling point components and making the fragrance milder. The solution is to add 1 to 10% of the total amount of fragrance.

Here, the amount of the low-boiling point component below 250°C of the fragrance to be added and the amount of the high-boiling point single fragrance for masking are determined by the type and amount of the fragrance to be impregnated, and the activated alumina bulb used. It should be selected appropriately depending on the diameter.

Also, add both low-boiling point ingredients and high-boiling point single fragrances, or
As for whether only one is enough, the type of fragrance to be impregnated,
It should be determined individually depending on the sphere diameter of the activated alumina sphere.

The lower limit of the low boiling point component button and the amount of high boiling point single fragrance that should be added,
In other words, if the desired effect is less than 30% by weight or 1% by weight each, it will be excluded, and if it exceeds the upper limit, 30% by weight or 10% by weight or more, the unique scent of these added ingredients will be added. I don't like it because it's too noticeable.

In accordance with the present invention, by blending as described above,
Although the theoretical basis for being able to solve the conventional problems has not been completely established, it can be inferred as follows.

In other words, when impregnating activated alumina spheres with a liquid fragrance, as long as the fragrance is a single substance, differences in the chemical structure or physical properties of the component substances that make up the fragrance may cause
It is thought that the rate of adsorption into the interior of the sphere and the mode of adsorption will naturally change depending on the degree of adsorption.

At this time, among the constituent substances of fragrances, components with simple chemical structures and small molecular weights are easily absorbed and absorbed into the interior near the center of the sphere. The hypothesis that the components penetrate into the interior of the sphere in a smaller amount than the former and is more likely to be adsorbed near the surface of the sphere is considered to be reasonable, but in fact, there are contradictions in explaining various phenomena observed in experiments. .

According to this hypothesis, components of fragrance components with relatively simple molecular structures, low molecular weights, and therefore low boiling points are mainly adsorbed near the center of the alumina sphere, while components with bulky molecular structures are adsorbed near the outside of the sphere. This is due to the structure in which high-boiling components with relatively large molecular weights are mainly adsorbed, and a concentration gradient of fragrance components occurs within the sphere due to the difference in boiling points.

Moreover, it is thought that this tendency is promoted as the sphere diameter becomes larger.

If these fragrance-impregnated alumina spheres are left in the environment,
It is predicted that the aroma generated from this bulb will mainly be the aroma of the high boiling point components located near the surface layer of the bulb and less of the low boiling point components, and this is actually the case.

That is, even taking into consideration the fact that high boiling point components are less volatile than low boiling point components, relatively high boiling point components are superior.

This is thought to be the reason why the fragrance from the fragrance-impregnated alumina bulb is different from the fragrance from the undiluted liquid fragrance. The reason for this is the following.

That is, when adsorbing the amount of fragrance under a 10 weight plate onto activated alumina spheres, the difference in fragrance from the original liquid fragrance does not become a problem as described above, and therefore, the technical idea of the present invention is achieved. In addition, if you try to adsorb a fragrance that exceeds the upper limit of 30% by weight to activated alumina spheres, as mentioned above, it will take a long time to adsorb, which is difficult from an economic point of view and due to the heat of adsorption. It is excluded because it is unfavorable in terms of decreasing the strength of the ball and risk of crushing it.

In the present invention, there is no particular restriction on the type of fragrance with which the activated alumina spheres are impregnated, and it may be any of animal fragrances, vegetable fragrances, and natural or synthetic fragrances.

For the present invention, the method of impregnating the activated alumina spheres with the fragrance is determined by the optimum method depending on the amount of fragrance and the type and diameter of the activated alumina spheres, but usually liquid fragrance is impregnated into the activated alumina spheres. A method of sprinkling and drying, a method of immersing activated alumina spheres in a liquid fragrance, and then drying are used.

In addition, if necessary, an adhesion promoter such as a suitable surfactant may be added, and any means capable of impregnating the activated alumina spheres with a fragrance can be used to achieve the technical idea of the present invention. It does not deviate from this.

Furthermore, in order to color the activated alumina spheres, coloring agents such as dyes and pigments are adsorbed together with fragrances, and volatilization retention agents,
There is no problem in adsorbing additives such as antioxidants to the spheres.

The most distinctive feature of the present invention is that even though the desired fragrance is produced as a liquid fragrance, when activated alumina spheres are impregnated with this liquid fragrance, the volatile fragrance from the spheres is
By solving the conventional problem of giving an unpleasant scent that is completely different from the original liquid fragrance, we have made it possible to provide alumina bulbs that generate the same fragrance as the original liquid fragrance.

This has made it possible to use activated alumina spheres with a large diameter, and also made it possible to use aluminum spheres impregnated with fragrance with 30 parts by weight of the spheres as a fragrance composition. As a result, it is of great significance that a fragrance composition has been developed that significantly extends the duration of the fragrance produced by alumina bulbs.

The fragrance composition of the present invention is provided as a pressure-resistant dry bulb containing up to 30% by weight of original fragrance, and the release of the fragrance occurs gradually and in gaseous form, leaving behind a stain of fragrance at the point of use. It is possible to enjoy the fragrance for a long time without worrying.

In addition, since the fragrance gas generated is more controlled than only fragrance ingredients, it is possible to use pure fragrance only, which is not possible with conventional products of this type, such as solid fragrances or spray set fragrances, which are more sensitive to other sublimable substances and fragrances. Another advantage is that you can enjoy the aroma.

In addition, conventional fragrances, including liquid fragrances and perfumes, have a strong tendency to volatilize a large amount of fragrance, which reduces the pleasantness of the fragrance, but the composition of the present invention allows the fragrance to be released very gradually. One of the benefits is that this point has been improved because of the divergence.

Due to the above-mentioned characteristics, the product of the present invention can be used for a wide range of purposes as a fragrance source that is extremely easy to carry and handle, and has extremely high practical utility value.

EXAMPLES Hereinafter, Examples will be shown to more specifically explain the present invention, but these Examples are not intended to limit the present invention in any way.

All parts are by weight.

Example 1 The diameter is 3 mm and the composition ratio of alumina to silica is 9.
Lemon essential oil (
(manufactured by Sunkist, USA) and dried.

The scent emanating from these bulbs is a rather pungent scent, and unlike the scent of raw lemon essential oil, it is difficult to feel the pleasant fragrance of so-called fragrances.

Next, to 100 parts of this lemon essential oil, 10 parts of limonene, which is a low-boiling point component of essential oil, and 5 parts of soot to mask the sesquiterpenes, which are high-boiling point components of essential oil, were mixed, and the same process was carried out. When the spheres were impregnated with 30 weight coefficients, the aroma from the spheres gave an aroma similar to that of raw lemon essential oil.

Example 2 Activated alumina spheres similar to those in Example 1 having a diameter of about 2 mm were impregnated with 10 weight φ of the fragrance of the following composition, and the spheres produced a desirable fragrance.

Example 3 Activated alumina/silica spheres with a diameter of 1 mm and a composition ratio of alumina to silica of 10:90 were mixed with fragrance and coloring agents (manufactured by Daiwa Kasei Co., Ltd., 60% Food Yellow No. 4 and Food Blue No. 1) with the following composition. A 40% mixture (1 ql) solution of diethylene glycol monoethyl ether) was adsorbed in 10 weight cups and dried, resulting in a green drying method, and no peculiar odor of sesquiterpenes was observed in its aroma.

Example 4 When 30 weight φ of the oriental type fragrance shown in the formulation A below was impregnated into activated alumina/silica spheres with a diameter of 2 to 3 mm and an alumina to silica composition ratio of 70:30, the fragrance obtained by the impregnation method was Since the fragrance is different, when I modified it to blend B and impregnated it, it had the same scent as the fragrance of blend A.

The bulb had a fragrance duration of approximately 2 months indoors at 20-25°C.

Example 5 A fragrance corrected to the D formulation to bring out the fragrance of the C formulation fragrance was pre-calcined at 200 to 300°C for 10 minutes.
~5 mm diameter activated alumina spheres pre-soaked at 30 weight and dried produced a scent similar to that of the fragrance containing C for about 3 months.

Claims (1)

[Claims] 1 Activated alumina casing or alumina to be used by impregnating an activated alumina or alumina/silica sphere with a diameter of 1 square meter or more with a liquid fragrance.7. The anti-silica sphere has a composition of alumina to silica ranging from 100 to 10 to 90, and the amount of liquid fragrance impregnated into the sphere is 10 to 30 parts by weight of the activated alumina or alumina-silica sphere. ,
And, in this liquid fragrance composition, the low boiling point component of 250°C or less of the fragrance has a boiling point similar to 3 to 30 weight sweets and/or the high boiling point component of 270°C or more, and the high boiling point component is masked. A fragrance composition characterized in that 1 to 10 weight parts of an effective fragrance are added.