JP2014201544A - Long-lasting aromatic agent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To solve the problem of a mixed oil conventionally used in an aroma therapy in which: according to a therapeutic purpose, usually several types of essential oils are blended to maximize the therapeutic effect by a complex/synergetic effect of each type of aroma, however, volatilization rates range from high to low depending on the type, therefore, with the mixed oil, due to the difference in the volatilization rate, the aroma changes significantly in a short time from an early stage of a therapy, lowering the effect of the therapy.SOLUTION: Essential oil is confined and adsorbed in particles of a porous inorganic oxide whose main component is silica having continuous pores in nanoscale in a high volume ratio. Thus, long-lasting effect of generation of aroma is improved. Furthermore, according to the volatilization rate, a particle size of the porous inorganic oxide is adjusted to improve the long-lasting effect and stability of strength of aroma to be generated for the various mixed essential oils.

Description

  The present invention is a fragrance material comprising a group of fragrance particles excellent in sustainability and stability of perfume intensity as compared to an essential oil composed of a conventional volatile liquid, and in addition, handling property, storage property, portability and safety. The present invention relates to an aroma therapy in which the quality of perfume, durability of strength, and stability are improved by blending at least one of them.

  In today's stressful society, there is a growing interest in healing the mind and body. Under such circumstances, natural essential oils (essential oils) extracted from plant leaves, roots, flowers, fruits, sap, xylem, etc. are used, and this ingredient is incorporated into the body in various ways to be used for mental and physical health and beauty. Aromatherapy, a plant therapy, is attracting attention, especially among younger generations and women.

  So-called aromatherapy attempts to balance the mind and body and bring out the natural healing power by acting on the olfaction known as the most instinctive sense among visual, auditory, tactile, and taste. Usually, in order to form a fragrance according to the purpose, several kinds of essential oils (essential oils) are blended to adjust the fragrance balance, and the mixture is used for aromatherapy.

The aromatherapy environment blends various essential oils according to the pathology of the subject, and continuously maintains the aroma environment according to the purpose for a predetermined time while maintaining its fragrance balance (aroma quality) and air concentration. This is very important. Since blended oils of several types have different volatilization rates for each essential oil, the fragrance of the essential oil that tends to volatilize is too strong at the beginning, and the essential oil that tends to volatilize over time is consumed quickly and the remaining amount decreases from the initial amount. Therefore, there is a problem that the fragrance becomes weak.
In addition, since essential oil is a volatile liquid and easily decomposes, there are problems in handling, storage, portability, and safety during use.

This is a major factor that complicates aroma treatment or prevents the spread of aroma in a wide range of environments and applications.
Provided is a non-woven absorbent desorbing / releasing sheet having a function of absorbing and absorbing moisture including plant-derived essential oils and a function of gradually releasing and releasing them.
It can be applied only to essential oils that dissolve in water but do not decompose. However, it is difficult to maintain the fragrance of essential oils that are partly decomposed and change the quality of essential oils, and that have a higher volatilization rate than water ( Patent Document 1).

In addition, a uniform jelly-like composition prepared by mixing an essential oil with a composition produced by blending a softening agent and / or a plasticizer with a styrenic thermoplastic elastomer is used. By using it by the method of use, the duration of fragrance can be significantly extended compared to the case of single use.
⇒ Odor changes due to reaction of elastomer and essential oil. Since this phenomenon is accelerated by heating and plasticizing the elastomer, it is difficult to apply to highly reactive essential oils (see Patent Document 2).

Moreover, the fiber material for cotton is characterized in that microcapsules enclosing plant-derived essential oil are fixed to the fibers via a binder resin.
The present invention is characterized in that a continuous fragrance is produced by randomly destroying the microcapsules in the batting with an accidental mechanical stress over time.
That is, it does not scent stably and continuously when left naturally (see Patent Document 3).

JP 2008-155566 A JP 2003-190267 A JP 2004-244756 A

In aromatherapy, essential oil (essential oil) is used as a fragrance.
Usually, several kinds of essential oils are blended according to the purpose of aroma treatment, and the purpose is to heal with the combined and synergistic effects, and to maximize the aromatherapy effects such as sleep, sedation, relaxation, relaxation, and refreshment.
However, there are various types of essential oils, from those with a large volatilization rate to those with a small volatilization rate. In mixed oils with adjusted fragrance balance, there is a problem that the aroma changes greatly in the short time from the beginning due to the difference in volatilization rate of the fragrance oil. . As a result, there is a problem that the quality and strength of the aroma change remarkably with the passage of time in aroma therapy, and the aromatherapy effect decreases.

  The essential oil is confined and adsorbed on porous inorganic oxide particles mainly composed of silica having nanoscale continuous pores at a high volume ratio. By optimizing the material and structure of the inorganic particles to be adsorbed and the confinement conditions according to the volatility characteristics of the essential oil, the intensity of the fragrance can be maintained stably for a long time. In addition, the essential oil having a high volatilization rate increases the particle size of the porous inorganic oxide, and the slow oil decreases the particle size, thereby improving the fragrance strength and the sustainability and stability of various mixed essential oils.

By blending several essential oil-encapsulated aroma materials with improved aroma intensity, durability and stability, depending on the purpose of aroma therapy, the target fragrance quality can be maintained stably for a long time. Aroma therapy can be realized.
Further, as a secondary effect, a solidification (particulate) from a liquid improves handling, storage, portability, and safety, so it is possible to realize aromatherapy in a wide range of uses and places.

Hereinafter, the present invention will be described in detail.
In the present invention, the plant-derived essential oil refers to a natural essential oil extracted by various methods from leaves, roots, flowers, fruits, sap, xylem, etc. of plants, specifically, red pine, ylang-ylang, Vetiver, Orange, Camomil, Camphor, Clarisage, Globras, Grapefruit, Kouyamaki, Cypress, Sawara, Sandalwood, Cedarwood, Jasmine, Juniper, Sugi, Geranium, Thyme, Dalasfer, Bamboo, Tea Tree, Todomatsu, Niauri, Niohiba, Nezuco , Neroli, pine, basil, patchouli, rose, palmarosa, cypress, hiba, petit gren, frankincense, cedar, peppermint, bergamot, marjoram, myrtle, melissa, fir, eucalyptus, lime, radiata, la Nsara, say lavender, linden, lemon, lemon grass, lemon balm, lemon verbena, rose absolute, rosewood, rose otto, those extracted from plants such as rosemary.

  The porous inorganic oxide mainly composed of silica is prepared by a sol-gel method in which tetraethoxysilane (TEOS) is formed by hydrolysis / condensation reaction. In the sol-gel method, a silanol group is formed by hydrolyzing TEOS in an acidic region. Furthermore, a silica network is formed by polycondensation of these. As the condensation rate is increased by adjusting the hydrogen ion concentration, the silica network formation rate is accelerated, and a porous inorganic oxide having a structure in which the pore size distribution is wide and the pore volume is large including a large number of pores can be obtained. In addition, when the network formation rate is slowed, a porous inorganic oxide having a narrow pore size distribution and slightly few pores can be obtained.

Thus, by using silica as the main component, the physical properties of the specific surface area due to the pores of the porous inorganic oxide particles can be adjusted in the range of the specific surface area of 300 to 1500 m 2 / g and the average pore diameter of 1.0 to 10 nm. it can. Moreover, it seems that the wettability of many essential oils can be improved by making silica a main component, and it has contributed to the stabilization of a fragrance characteristic. Further, the porous inorganic oxide particles have an average particle size adjusted in accordance with the target aroma characteristics, and the particle diameter is optimized in accordance with the aroma characteristics of the essential oil in the range of 0.5 to 5000 μm.
Regardless of the particle diameter, the amount of the essential oil contained in the porous inorganic oxide particles is preferably 5 to 300 wt%.

  In order to enclose the essential oil in the porous inorganic oxide particles mainly composed of silica, the oil is injected and filled into the pores by any of the following methods according to the kind and amount of the essential oil to be included. One is an immersion method.

  In this method, the inorganic oxide particles are immersed in the essential oil or a diluted solution thereof, the container is hermetically heated and the pressure is increased, and the essential oil is adsorbed and encapsulated in the pores. This method is desirable for an essential oil having a high affinity with silica and a relatively low molecular weight. The second is the vapor pressure method. After a required amount of inorganic oxide particles are sealed in a stainless steel sealable container, the pressure is reduced. Thereafter, the essential oil is poured into the container, an appropriate temperature is selected according to the vapor pressure of the essential oil, and the container is held and contained in a warm bath.

  The third is a supercritical method. Add essential oil to liquefied carbon dioxide in a closed container, mix with inorganic oxide particles, and dissolve the essential oil in supercritical carbon dioxide in the supercritical state of carbon dioxide (temperature: 31 ° C, pressure: 7.38MPA). At the same time, it is a method in which sensual oil is encapsulated in the pores with the excellent diffusivity of supercritical carbon dioxide. In this case, only the essential oil contained in the pores remaining in the pores is obtained by gasifying and discharging the supercritical carbon dioxide gas. It is desirable to select and optimize the inclusion means according to the type of essential oil, the targeted fragrance characteristics, and the duration.

  Since the inclusion means are all different in stability against degradation for each essential oil, physical adsorption to silica pores, chemical adsorption characteristics, boiling point, and vapor pressure, the optimum means is selected and optimized while confirming the change in fragrance through trial and error. There is a need. In general, in order to ensure sustainability, it is necessary to encapsulate the particles at a high concentration up to the deep part. In this case, it is desirable to set appropriate conditions by the vaporization press-fitting method for increasing the permeation power of the essential oil, and further by the supercritical method.

  The porous inorganic oxide particles mainly composed of silica preferably have an average particle size of 5 to 5000 μm. It is preferable to select the small particle size side for base note-based essential oils with a low volatilization rate, and the large particle size side for top notes with a high volatilization rate. The amount of fragrance tends to change. Further, in the process of pelletizing the particles using a binder resin, the fragrance intensity and fragrance time can be further finely adjusted by adjusting the resin ratio, pellet size, and shape.

A specific surface area of 300 to 1500 m <2> / g is preferred. Less than 300 m2 / g, the amount of inclusion is not sufficient and the durability is poor, and more than 1500 m2 / g, the particles are fragile and fragile. Prone. A more preferable range is 500 to 900 m <2> / g.
An average pore diameter of 1.0 to 200 nm is preferable. When the thickness is 1.0 nm or less, penetration is difficult by the dipping method, and even if press-fitting or supercritical is used, it is difficult to permeate the pores to the inside. When it is 200 nm or more, the fragrance persistence is lowered. The pore volume of the porous inorganic oxide is preferably 0.2 to 1.5 cm 3 / g. At 0.2 cm 3 / g or less, the amount of inclusion is small and the sustainability is low, while at 1.5 cm 3 / g or more, the particles are fragile and easily broken, and the stability of light emission cannot be expected.

  A ratio of 5 to 300 wt% of the inclusion amount of the essential oil is appropriate. If it is less than 5 wt%, the sustainability is low, and if it exceeds 300 wt%, it cannot be encapsulated and precipitates on the surface, so the perfume rate becomes unstable.

EXAMPLES Hereinafter, although this invention is demonstrated further in detail based on an Example, this invention is not limited to these Examples. The performance evaluation in the examples was sustained stability, and the sustainability was evaluated by changes in “scent strength” and “scent quality” with time.
<Strength of fragrance>
Inspect the scent of the sample from a total of 10 men and women in their 20's, 30's, 40's, 50's and 60's. Evaluation was made by a five-point scoring method. In other words, 0 for "moderate fragrance", +1 for "slightly strong", +2 for "too strong", -1 for "slightly weak", -2 for "too weak" The average value of 10 people was used as the evaluation score. In Table 1, when the evaluation score is −0.5 point or more and +0.5 point or less, “◯”, when it is −1.0 point or more and less than −0.5 point, or exceeds +0.5 point and +1.0 point The following cases are indicated as “Δ”, and cases where the value is less than −1.0 point or exceeds +1.0 point is also indicated as “x”.

<Aroma quality>
A sample of 10 men and women in their 20's, 30's, 40's, 50's, and 60's, who have a total of 10 scents. Rated by stage. That is, 5 for a “very favorable scent”, 4 for a “preferable scent”, 3 for a “cannot say”, 2 for a “unpleasant scent”, and “a very unsavory scent” ”Was 1, and the average value of 10 people was taken as the evaluation value. In Table 1, the case where the evaluation value is 3.5 or more is indicated as “◯”, the case where it is less than 3.5 and 2.5 or more is indicated as “Δ”, and the case where it is less than 2.5 is indicated as “×”.
Such fragrance evaluation was performed initially, 6 hours later, 12 hours later and 24 hours later.

Example 1
1.0 g of orange sweet which is an essential oil having a high volatilization rate was encapsulated in 1.0 g of porous silica having a pore diameter peak of 1.7 nm, a specific surface area of 970 m 2 / g and a pore volume of 0.5 m 3 / g by a supercritical method.
Strength: XXX Quality: XXX
Example 2
Except that grapefruit was used instead of orange in Example 1, all the items were as good as orange in the same manner as Example 1.
Example 3
1.0 g of orange sweet, which is an essential oil, was encapsulated in 1.0 g of porous silica having a pore diameter peak of 1.7 nm, a specific surface area of 470 m 2 / g, and a pore volume of 0.35 m 3 / g by a supercritical method.
Strength: XXX Quality: XXX

Example 4
1.0 g of orange sweet, which is an essential oil, was encapsulated in 1.0 g of porous silica having a pore diameter peak of 1.7 nm, a specific surface area of 270 m 2 / g, and a pore volume of 0.25 m 3 / g by a supercritical method.
Strength: ○○ △△ Quality: ○○○○
Example 5
1.0 g of sandalwood, which is an essential oil having a low volatilization rate, was encapsulated in 1.0 g of porous silica having a pore diameter peak of 5.0 nm, a specific surface area of 400 m2 / g, and a pore volume of 0.4 m3 / g by a supercritical method.
Strength: XXX Quality: XXX
Example 6
Even in the same manner as in Example 5 except that bachelors were used in place of sandalwood in Example 5, good results were obtained in all items.

Example 7
As a result of mixing 0.3g each of the fragrance material of Example 1.3.5 and evaluating the fragrance characteristics, the results were satisfactory in all items.
Example 8
As a result of mixing 0.3 g of the fragrance material of Example 2.5.6 and evaluating the fragrance characteristics, the results were satisfactory in all items.
Example 9
As a result of mixing 0.3g of each of the fragrance materials of Example 1.6 and evaluating the fragrance characteristics, all the items were satisfactory.

Comparative Example 1
As an essential oil, 0.15 g of each of orange sweet, ylang ylang and sandalwood was mixed for evaluation. As is clear from the evaluation results, good results were not obtained in both odor intensity and quality. Strength: ○ ××× Quality: ○ ×××.
Comparative Example 2
Ylang ylang and sandalwood 0.15 g each were mixed as an essential oil and mixed with the orange sweet of Example 1 for evaluation. As is clear from the evaluation results, good results were not obtained in both odor intensity and quality. Strength: ○ △△ × Quality: ○ △△ ×.
Comparative Example 3
As an essential oil, 0.15 g of sandalwood was mixed, and the orange sweet of Example 4 was mixed for evaluation. As apparent from the evaluation results, both the strength and quality of the odor were improved with respect to Comparative Example 1, but sufficiently good results were not obtained. Strength: ○○ △ × Quality: ○○ △ ×.

As is apparent from the above, the fragrance of the present invention is excellent in handleability, and also has excellent scent of mixed fragrance, scent strength and quality change over time and long-lasting durability. It has the characteristics. As described above, the present invention exhibits an aromatherapy effect such as healing, resting, sedation, relaxation, relaxation, refreshing, etc., which has never been achieved by the present invention.

Claims (4)

A long-lasting fragrance comprising a plant-derived essential oil encapsulated in porous inorganic oxide particles having a specific surface area of 400 to 1000 m 2 / g mainly composed of silica having continuous pores in the nanometer region. The long-lasting fragrance according to claim 1, wherein the means for embedding the essential oil in the porous inorganic oxide particles is any one of a liquid immersion method, a vaporization press-in method, and a supercritical method. A method for producing a long-lasting fragrance, characterized by optimizing perfume strength sustainability by adjusting the particle size and inclusion means of a porous inorganic oxide according to essential oil. In an aroma therapy characterized by blending two or more kinds of essential oils, at least one kind is a blended persistent fragrance characterized by blending a fragrance containing essential oil in a porous inorganic oxide.