JP2000096079A - Method and composition for enhancement of substantivity of fragrance material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject composition capable of manifesting the substantivity of a fragrance material for a long period and enhancing the substantivity of the fragrance by mixing with a soap, a detergent, etc., by mixing the fragrance material of a specific composition with a specified tetrahydroxypropylethylenediamine. SOLUTION: This composition comprises a mixture of (A) a fragrane material selected from the group consisting of at least one aroma chemical and at least one perfume composition with (B) tetra(2-hydroxypropyl)ethylenediamine represented by the formula which is a hydrophilic surface treating agent and has a high substantivity of the fragrance. The composition is preferably composed of substantially eliptical hydrophobic particles having a continuous outer surface and a matrix volume in the interior and the particles are preferably a solid solution having the outer surface substantially covered with the surface treating agent. The component A preferably has 1-8 value of calculated log10P (P is the partition coefficient of the component A between n-octanol and water).

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a fragrance selected from the group consisting of at least one aroma compound and at least one perfume composition.
The present invention relates to a composition for enhancing the persistence of a fragrance substance by mixing with a substance, and a method for increasing the persistence of a fragrance substance.

[0002]

2. Description of the Related Art Conventionally, household products such as soap or personal use products such as cosmetics, health maintenance products such as cleaners, and fragrances used for imparting aroma or imparting medicinal effects to textiles, skin, hair and others. It has been known. US Pat. No. 4,152,272 relates to the flavoring agent and the like.
No. 5,188,837; U.S. Pat.
540,853; U.S. Patent No. 5,540,853;
U.S. Pat. No. 5,476,660, U.S. Pat.
No. 2,206, U.S. Pat. No. 4,919,841, Don
brow, Microcapsules and Nanoparticles in Medicine
and Pharmacy, Chapter 6, "NANOPARTICLES-PREPARATION
AND APPLICATIONS ", Jorg Kreuter (pages 126-14
8), CRC Press, 1992. and Adeyeye et al, "Developme
nt and Evaluation of Sustained-Release Ibuprofen
Wax Microspherers, I. Effect of Formulation Vari
ables on Physical Characteristics ", Pharm. Res. (1
991), volume 8, No. 11, pages 1377-1383.

[0003]

However, there has been no conventional flavoring agent that can maintain its effect for a long period of time or that can control the amount of generated fragrance. It is an object of the present invention to provide a composition for enhancing the persistence of a fragrance substance and a method for increasing the persistence of a fragrance substance over a long period of time.

Another object of the present invention is to provide a lotion such as soap, detergent, hair tonic, aftershave lotion, etc.
It is an object of the present invention to provide a composition and a method for enhancing the fragrance persistence by mixing with a refreshment enhancer for a vehicle interior, a dashboard deodorant and the like.

[0005]

SUMMARY OF THE INVENTION The present invention provides (a) at least one aroma compound and at least one perfume.
e) flavoring (fragra selected from the group consisting of the composition
a) substance and (b) tetra (2-hydroxypropyl) ethylenediamine having the following structural formula:

Embedded image Having a high fragrance persistence, consisting of a mixture with In order to increase the persistence of the fragrance material, it is preferable to mix the tetra (2-hydroxypropyl) ethylenediamine having the above structural formula so as to increase the amount and concentration. The present invention relates to skin,
A finely divided active and bioactive composition (perfuming composition) with controlled emission time for distribution to the surface of a specific location, such as hair, fabric, and even the closest environment.
composition)), where
Active and bioactive ingredients have a calculated log ₁₀ P between 1 and 8 (P represents n-octanol-water partition coefficient). Here, the activity and the biological activity include a medicinal composition, an insect repellent, an insecticide, a bactericide, or an animal pheromone and a flavoring agent, a flavoring agent, and the biological activity is an action on a plant or a mammal, A term that includes action.

[0006] The above composition is a surfactant (compatible sur
The active or bioactive ingredient present in a single-phase solid solution in a wax or polymatrix that is coated on the surface and / or contained therein.

[0007] In particular, the present invention provides a method for applying a bioactive or bioactive compound to a substantially solid surface comprising at least one substantially elliptical hydrophilic particle having a continuous outer surface and an inner matrix volume consisting essentially of: The present invention relates to a composition for effectively delivering an active substance to a specific site.

(1) At least a hydrophobic polymer and / or
Or a single-phase solid solution of a matrix material, which is either at least one hydrophobic wax, wherein each of the polymer and the wax is at about 35 ° C. to 120
It has a melting point in the range of ° C. and dissolves at least one hydrophobic active or physiologically active substance (for example, a flavoring substance), and the solid solution has a matrix volume on the outer surface and inside. (2) Tetra (2-hydroxypropyl) ethylenediamine whose outer surface has substantially the following structural formula

Embedded image Consisting essentially of a hydrophilic surface treatment agent (surfactant).

For example, active or physiologically active ingredients such as flavoring substances have log ₁₀ P calculated values (P
Represents the partition coefficient of n-octanol and water activity or biologically active ingredients) and has hydrophobic particles having an outer diameter of about 0.05 to 20 microns in width. The concentration of the active or bioactive substance in the polymer or wax is between 5% and 60% by weight of the particle weight.

The proportion by weight of the surfactant is from about 0.01% to 5% by weight of the particles.
Waxes, surface treatments and polymers do not react with biologically active or active ingredients.

The preferred compositions of the present invention have a rate of penetration of active or bioactive substances, such as flavoring substances, into waxes or polymers, which is measured by the IFF penetration test described in more detail in the detailed description of the drawings below. 10 ^-8 (m
g-mm) / (cm ² -min) to 8 × 10 ⁻³ (mg
−mm) / (cm ² −min). As mentioned above, otherwise, the entire outer surface of the substantially elliptical hydrophobic particles is substantially composed of a hydrophilic surface treatment agent. More specifically, there are the following three cases regarding the arrangement of the surface treatment agent.

(A) the substantially hydrophilic surface treatment agent is substantially completely applied to the entire outer surface of the single phase solid solution in the form of a continuous submicron thick layer of the surface treatment agent; It is coated and fixedly bonded to the entire outer surface of the single phase solid solution. (B) the substantially hydrophilic surface treatment agent is provided directly below the entire outer surface of the solid solution (proximate to and immedia
tely, substantially beneath of outer surface)
Substantially disposed within the volume of the inner matrix.

(C) The substantially hydrophilic surface treating agent tetra (2-hydroxypropyl) ethylenediamine comprises (a)
Substantially completely coated over the outer surface of the single phase solid solution in the form of a continuous submicron thick layer of the surface treatment agent;
Fixedly bonded and (b) substantially in the volume of the inner matrix, directly below the entire outer surface of the solid solution.

Regarding the surface treatment agent, if the surface treatment agent is a cationic surface treatment agent, the particles are positively charged. If the surface treatment agent is an anionic surface treatment agent,
The particles are negatively charged. If the surface treatment agent is a non-ionic surface treatment agent, the particles have a neutral charge. When the surface treatment agent has a varying charge, the surface treatment agent is an amphoteric surface treatment agent.

[0015] The at least one hydrophobic polymer and / or at least one hydrophobic wax useful in practicing the present invention are preferably at least one of the following materials. (A) polyamines having a molecular weight in the range of about 6,000 to about 12,000, such as MACROME manufactured by Henkel Agricultural Co. of Dusseldorf, Germany
LT6030 (another example is that of U.S. Pat. No. 4,184,099, Lindawer et al., Issued Jan. 15, 1980, the specification of which is incorporated herein by reference.
ERSALON-based polyamide polymer manufactured by Henkel Corporation of Minneapolis, Minnesota)

(B) synthetic and natural carnaub
a) waxes (c) synthetic and natural candelilla waxes (d) cetyl palmitite (eg CUTIN brand name)
(E) a mixture of cetyl palmitite and candelilla wax (f) ozokerite wax (g) ceresin wax (h) about 500 to about 6,000 Low density polyethylene wax with a range of molecular weights

It is desirable to use different flavoring compositions having different total log ₁₀ P calculations for different combinations of waxes and surface treatment agents for different applications, such as hair care and textile care.

The maximum vapor pressure for the active or physiologically active substance in the composition according to the invention is 4.1 mm / Hg at 30.degree. The active substance is a scented substance, the scented substance having a top note component, a middle note component and a bottom note component, and the vapor pressure of each of the three component groups. Desirably, the width is as follows.

(A) For the top note component, the vapor pressure at 25 ° C. is 0.0001 mm / Hg to 0.009 mm
/ Hg. (B) Regarding the middle note component, the middle note has a vapor pressure of 0.01 mm / Hg to 0.09 mm / H at 25 ° C.
g. (C) For the bottom note component, the vapor pressure of the bottom note should be from 0.1 mm / Hg to 2.0 mm / Hg at 25 ° C.

Examples of the above-mentioned fragrance are as follows.

[Table 1]

The particles of the composition of the present invention contain (1) a sufficient charge per molecule of the surface treatment agent and (2) a sufficient concentration of the surface treatment agent on each particle or are coated on the surface thereof. (Or both), the electrostatic charge density on the surface of each particle is sufficient to cause adhesion of the particle to a given surface, such as hair, mammalian skin or fabric.

A substance having the following structural formula, tetra (2-hydroxypropyl) ethylenediamine, is used as a surfactant.

Embedded image

Ratio of tetra (2-hydroxypropyl) ethylenediamine: about 2:15 to 4: 5 perfume
It has been found that, when used at the following ratios, this substance also has surprising utility as it increases the persistence as a flavoring and aroma chemical (aroma chemical).

Fragrance lasts about 50%
Examples of substances that increase above are as follows. (A) GALAXOLIDE, a mixture of compounds having the following structural formula:

[0025]

Embedded image

(B) Geraniol having the following structural formula

Embedded image

(C) β-pinene having the following structural formula

Embedded image

(D) n-octanol having the following structural formula

Embedded image

(E) dihydromycenol having the following structural formula

Embedded image

(F) KOAVONE having the following structural formula
(International in New York, NY
Flavor &Fragrance's trade name).

[0031]

Embedded image

(G) An eigenol (e) having the following structural formula
ugenol)

Embedded image

As described above, the activity of the solid solution containing particles of the present invention into a wax or a polymer and the permeation rate of a physiologically active substance are in the range of about 10 ^-8 (mg-mm / cm ² -m
in) to about 8 × 10 ⁻³ (mg-mm / cm ² -min). In particular, materials having log ₁₀ P calculations as shown in Table 2 below also have permeability through various waxes and polymers that are useful in the practice of the present invention.

[0034]

[Table 2]

The present invention relates to a perfumable substance as defined above, comprising at least one particle.
perfumable material having a substantially solid surface, such as, for example, hair, fabric and mammalian skin.
Includes the method of frgrancing. Here, the perfumable material is used to refresh the hair, fabric, mammalian skin, and other cosmetics such as soaps, detergents, hair tonics, and lotions, daily necessities, and the interior of automobiles. Examples include fresheners and deodorants for dashboards. When performing this method, the flavor (fr
grancing) The strength, ΔA, is determined by the following algorithm.

[0036]

(Equation 1) Here, α is a constant, and β _k is an individual threshold value or a complex threshold value of the Q component of the fragrance material (fragment material) in the fine particles to be released in a controlled manner. As well as flavoring substances (fragrance materia
Since the threshold value of each pair and the threshold value of each pair of l) are also measured, the number of threshold values is “P”. ), M _0j is the number of initial _gram moles of one of the Q flavor components, D _j is the dispersibility of each Q flavor component in the particles, and θ is the dispersive, controlled flavor of the particles. Where R _i is the radius of the n particles.
The aroma intensity generated from one particle is represented by the following equation.

[0037]

(Equation 2)

The aroma intensity of n particles having an average radius R is given by the following equation: Average radius

(Equation 3) Is given by the following equation:

(Equation 4)

The above equations are derived from partial differential equations.

(Equation 5) And

(Equation 6) It is. The rate of change, △ A, that varies with time of aromatization is expressed by the following equation:

(Equation 7)

The formula for the diffusion of an active or bioactive product from the particle composition of the present invention is Pe
ppas et al., 1996 Journal of Cont.
rolled Release No. 40 245-25
"Controlled Release of Flavor from Polymer I."
Thermodynamic analysis ", published by Marcel Decker in 1996,
A textbook edited by P. Neogi, "Polymer Dispersion (diffusi
on) ”, pages 165 to 169 (Duda & Zielin)
It can be derived from the suggestions of the ski chapter “Free Volume Theory” and the subchapter “Compound Component Diffusion”.

The present invention also includes a method for producing a composition comprising a hydrophobic active ingredient or a physiologically active ingredient as defined above, comprising the following steps. (1) at least one hydrophobic polymer to produce the first mixture at a temperature equal to or higher than the melting point of the polymer or wax, or, in the case of a mixture, at the melting point of the best melting polymer or wax; The active or biologically active ingredient is thoroughly mixed with at least one hydrophobic polymer and / or at least one hydrophobic wax.

(2) To produce a second mixture which is an aqueous solution (eg, an aqueous solution of sodium chloride or propylene glycol), an aqueous solution of water (eg,
A mixture of sodium chloride and water, or a mixture of propylene glycol and water, or water itself) is thoroughly mixed with a surface treatment (defined above).

(3) The first mixture and the second mixture are
From about 60 ° C to an aqueous solution (eg, water boiling at 100 ° C,
Or a mixture of water and propylene glycol boiling at 120 ° C.) up to the boiling point at atmospheric pressure. Thereby, a microemulsion is formed.
And (4) producing a composition containing a hydrophobic active ingredient or a physiologically active ingredient (eg, a perfume) in the solid phase to form (when cooled to 25 ° C.) an aqueous suspension of solid phase particles. .

Therein, the weight percent of the active ingredient or bioactive ingredient (eg, flavoring composition or aroma substance) to form the first mixture is about It is between 5% and about 60%. Also, the weight percent of the surface treatment agent in the second mixture is from about 0.01% to about 5% of the weight of the second mixture. In practice, the cooling step, i.e., cooling the aqueous suspension, is performed at a temperature from about 10C to about 30C.

The above steps are preferably performed by using a homogenizer and / or a rotor / stator high shear mixer. Of the present invention,
Examples of homogenizers useful in this embodiment include:
Laboratory homogenizers 15MR and 31MR manufactured by APV Gaulin, Inc., Everett Garden Street 44, Massachusetts.

An example of a rotor / stator high shear mixer is 01028 Massachusetts East Long Meadow Chestnut Street 355 PO Box 5
A high shear in-line mixer manufactured by Silverson Machine Company, Inc. 89 and Scott Process Equipment Company, Inc., Sparta PO Box 619, New York.

The rotor / stator high shear mixer can be used first, and then the homogenizer described above and the rotor / stator high shear mixer can be used in turn to further reduce particle size. . The resulting emulsion is then further homogenized using a laboratory homogenizer such as a 15MR and 31MR homogenizer. Details of the above-described homogenizer and rotor / stator high shear mixer are described in the detailed description of the drawings below.

The present invention also includes a method for producing a composition (for example, a perfume composition) containing the above-mentioned hydrophobic active or physiologically active ingredient, comprising the following steps. (1) forming a first single liquid phase mixture at a temperature equal to or higher than the melting point of the polymer or wax described above, or, in the case of a mixture, at the melting point of the polymer or wax that is best dissolved in the mixture; For at least one hydrophobic active or bioactive substance (eg, perfume (perf)
ume) the composition), (a) at least one hydrophobic polymer and / or at least one hydrophobic wax, and (b) at least one surface treatment agent.

(2) an aqueous composition containing water (for example, water itself or a mixture of propylene glycol and water or a mixture of sodium chloride and water, for example, a 5% sodium chloride solution or a 20% aqueous propylene glycol solution); Mix the first single liquid phase mixture. Thereby, a microemulsion is formed. And (3) an aqueous suspension of solid phase particles in which a composition containing a hydrophobic active or physiologically active ingredient (for example, a composition containing a perfume or a composition containing an aroma compound) is present as a solid phase. Cooling the resulting suspension between about 10 ° C to about 30 ° C). Here, the weight percentage of the active ingredient or the bioactive ingredient for forming the first mixture is between about 5% and 60% of the weight of the first mixture. The weight percent of the surface treatment agent in the first mixture is about 0.01% to 5% of the weight of the first mixture.

In addition, as described above, regarding the method first described for producing the composition containing the hydrophobic active ingredient or the physiologically active ingredient of the present invention, the mixing step will be described later in detail in the detailed description of the drawings. As indicated, this is done by using a homogenizer and / or a rotor / stator high shear mixer.

The present invention also includes an apparatus for performing the above-described method for producing a composition containing a hydrophobic active ingredient or a physiologically active ingredient. The device has the following configuration. (1) at least as high as the melting point of the polymer or wax, and in the case of a mixture, at the melting point of the best-dissolved component in the mixture, at least to form a first single liquid phase mixture A means for thoroughly mixing a substance containing one hydrophobic active ingredient or a physiologically active ingredient with at least one hydrophobic polymer or at least one hydrophobic wax.

(2) To form a second mixture that is an aqueous solution (eg, using a homogenizer and / or a rotor / stator high shear mixer)
Means for thoroughly mixing the aqueous composition containing water and the surface treatment agent. (3) means for mixing the first mixture with the second mixture at a temperature between 60 ° C. and the boiling point of the aqueous composition at atmospheric pressure (for example, as described above, a homogenizer and / or Or using a rotor / stator high shear mixer). Thereby, a microemulsion is formed. And (4) means for forming a composition containing a hydrophobic active ingredient or a physiologically active ingredient as a solid phase, and forming an aqueous suspension of the solid phase particles (for example, a mixture at 10 ° C.
Using cooling means to cool to from 30 ° C. to 30 ° C., for example using a device with a cooling coil).

Another apparatus for producing a composition containing a hydrophobic active or physiologically active ingredient of the present invention has the following constitution. (1) A composition containing at least one hydrophobic active ingredient or a physiologically active ingredient, (a) at least one hydrophobic polymer and / or at least one hydrophobic wax, and (b) at least one surface treatment agent To form a first single liquid phase mixture at a temperature equal to or higher than the melting point of the polymer or wax and, in the case of a mixture, of the best dissolved material of the materials in the mixture. Means to mix well at the melting point,

(2) Means for mixing the first single liquid phase mixture and the aqueous composition containing water (for example, using the above-mentioned homogenizer and / or rotor / stator high shear mixer). Thereby, a microemulsion is formed. And (3) means for producing a composition containing a hydrophobic active ingredient or a physiologically active ingredient in a solid phase and forming an aqueous suspension of the solid phase particles (for example, a suspension at a temperature between 10 ° C and 30 ° C). Cooling coil for cooling).

The dispersibility (diffusivit) of the flavoring substance of the present invention
y) and the characteristics and intensity of the odor are measured using the fragrance diffusion evaluation device described below.
apparatus) and the method of use of the apparatus.

The apparatus for evaluating aroma dispersibility includes a container having at least one opening in which a test sample is present (hollow container), a flow means for air for passing air through the inside of the container means, and an air flow. Where the intensity and aroma attributes are determined based on temperature and time. The sample is weighed initially and at time intervals while the air passes through the cylinder at a constant or varying speed.

Further, in the present invention, the dispersibility, odor intensity and characteristics of a flavoring substance selected from the group consisting of one or more aroma compounds and one or more flavoring compositions having the following constitutions are provided. Are also used to test X, X, and Z in a three-dimensional space called XYZ.

(A) A space (ho) having the following structure
llow) is a substantially cylindrical container arranged vertically. (1) a central axis parallel to the Z axis; (2) an internal cavity (void); (3) a substantially annular bottom wall of a first solid material without holes located in the first XY plane; The bottom wall is arranged substantially perpendicular to the Z axis and has an inner cavity (inne).
r void) and an outside wall.

(4) A continuous, non-perforated cylindrical sidewall surrounding the inner void in a vertical direction and disposed parallel to and substantially equidistant from the Z axis. Wherein the side wall comprises a top annular rim disposed in a second XY plane, an upper intermediate portion and a lower intermediate portion, and a bottom rim disposed in the first XY plane. The bottom rim is tightly sealed along the entire periphery of the bottom rim with respect to the periphery of the bottom wall, and the side wall is located at the lower middle portion in a third XY plane. A first orifice provided through the side wall and a second orifice provided through the side wall in the fourth XY plane and substantially opposite to the first orifice. And the fourth XY plane is a third XY plane.
It is arranged at a position between the plane and the first XY plane and parallel to the third XY plane, and no other side wall is provided.

(5) A top substantially annular cover made of a third solid, non-porous material, wherein the cover covers all of the periphery of the annular rim relative to the periphery of the annular rim at the top of the sidewall. The second X
A cover opening having an inner cavity (void) side disposed on the Y plane and an outer wall surface and having an inner peripheral portion disposed substantially equidistant from the Z axis; The opening has a diameter of about 20% to about 40% of the outer diameter of the top cover.

(B) Attached to sensor support means which is inserted in a seal shape through the first orifice and is connected to temperature monitoring means outside the vessel, and is disposed in the internal cavity (void). A temperature sensing end sensitive to temperature fluctuation mounted in a seal through the first orifice, and (c) a seal in a seal through the second orifice and in the internal cavity. A supply pipe having an open end disposed therein and connected to the supply pipe and supplying air from an air supply means disposed outside the container to the internal cavity. Air flow means for flowing air;

(D) suspending means for suspending the test sample disposed in said internal cavity (void), said suspending means being substantially two opposing anti-opposed positions of said second X A substantially flexible support fixedly supported at attachment points located in the same XY plane as the -Y plane, each support being attached to the top rim of the side wall, from which the attachment points of the attachment point are located. The test sample has the odorant initially suspended on a suspension means, suspended in a substantially intermediate position therebetween.

Thereby, the temperature monitor is activated when the air supply means generates the air to be flowed through said air flow means. Constant temperature T or fluctuating temperature T
The air at (θ) has a constant flow rate Q or a variable flow rate Q
Pass the sample at (θ). Retaining the fragrance material in G ₁ gram C ₁ g-mol concentration per liter in the sample after a certain time θ with Introduction liters per C ₀ gram mole concentration of G ₀ grams area A which holds a fragrance material of It will be. During time θ,
At the intersection of the second XY plane and the Z axis, the odor properties and strength can be measured and determined.

[0064] Also provided therein is (1) the temperature of the air supplied by the air supply means is controlled, and (2) the probe of the temperature sensor has programmed feedback means associated with the air supply means. An aroma dispersibility evaluation device such as that described above can also be used.

The present invention further includes an apparatus having various orifices in different side walls, each of which is provided with a probe of a temperature sensor in a seal shape. Each of the probes of such a temperature sensor has a program for a feedback unit connected to the air supply unit, and controls the temperature of the air supplied by the air supply unit.

The odor properties and intensity can be measured using an electronic aroma test apparatus.

Further, in the present invention, one or more aroma compounds or one or more fragrances comprising the following steps
e) A method of simultaneously testing the dispersibility and odor properties and strength of the flavoring substance selected from the group consisting of the composition can be used. (A) comprising a device as defined above,
(B) suspending the test sample containing the odorant by the suspension means of the device as defined above, and (c) activating the air supply means and the temperature monitoring means.

Here, when the air supply means generates the air to be flowed through the air flow means, the temperature monitor operates. The air at the constant temperature T or the changing temperature T (θ) passes through the sample having the area A at the constant flow rate Q or the changing flow rate Q (θ). C ₀ per liter
It said having a area A with the beginning of the fragrance material in the G ₀ grams of gram moles concentration samples would be odorant in G ₁ gram C ₁ gram moles concentration per liter during a predetermined time theta. During time θ, the nature and intensity of the odor can be measured and determined substantially at the intersection of the second XY plane and the Z axis.

In the present invention, the bottom wall, the side wall, and the entire inner cavity (voide) side of the top cover are covered with an absorbing material such as aluminum foil in order to prevent the flavor material from being absorbed into the bottom wall, the side wall, and the top cover. The above-described device covered with an inhibitor can also be used.

The present invention includes devices which comprise two cylinders operating simultaneously, in addition to devices which use only one cylinder. In the present invention, an apparatus having the following container inside can be used. (1) Height between about 50 and about 75 cm (2) Radius between about 15 and 30 cm (3) Capacity between 0.1 and about 0.2 m ³ (4) About 10 to 30 cm from bottom wall (5) Air flow vertically away from about 3 to about 10 cm from the bottom wall Opening provided in the top cover with an inside diameter of about 15 to 30 cm Book In the invention, the pressure in the internal cavity is about 0.5 to 2 ps.
The method described above can be used such that the flow rate is maintained between about 900 to about 1,000 ml per minute while being kept at ig.

[0071]

Embodiments of the present invention will be described in detail with reference to the drawings. First, a brief description of the drawings will be given. FIG. 1 is an enlarged (2,000 ×) view of a fabric treated with a fabric softener without using the particulate composition of the present invention. FIG. 2 is a photograph (magnified to 2,000 ×) of a fabric treated with a fabric softener without using the particulate composition of the present invention.

FIG. 3 is a view of an expanded fabric (2,000 ×) washed with wax fine particles containing a flavoring agent of the present invention.
FIG. 4 is an enlarged photograph (2,000) of a woven fabric (towel) washed with a capsule-like flavoring agent in the wax fine particles of the present invention.
x). FIG. 5 shows an enlarged strand of hair shampooed without using the particulate composition of the present invention (2,00
0x). FIG. 6 is an enlarged photograph (2,000 ×) of a strand of hair washed with shampoo without using the particulate composition of the present invention. FIG. 7 is an enlarged strand (2,000 ×) of hair washed with a shampoo containing a flavoring agent in capsule form within the wax microparticles of the present invention.

FIG. 8 is an enlarged photograph (2,000 ×) of a hair strand washed with a shampoo and a capsule-like flavoring agent in the wax fine particles of the present invention. FIG. 9 is an enlarged strand (2,000x) of the hair washed with a conditioner without using the particulate composition of the present invention. FIG.
0 is a photograph of a hair strand washed with a conditioner without using the particulate composition of the present invention (1,500 ×
It was expanded to).

FIG. 11 shows enlarged strands (1, 1 and 2) of hair washed with a conditioner containing the wax fine particles of the present invention.
It is a figure of 500x). FIG. 12 is a photograph of an enlarged strand (1,500x) of hair washed with a conditioner containing the fine wax particles of the present invention. FIG. 13 is a conceptual diagram of a typical woven fabric obtained by weaving a bundle of interwoven fibers. Shown are particles trapped in holes between the bundles.

FIG. 14 is a conceptual diagram of a typical woven fabric obtained by weaving a bundle of interwoven fibers.
The particles are trapped in the holes between the bundles and are directly attached by the physical force between the particles and the bundle.
FIG. 15 is a cross-sectional view of an apparatus used to perform an IFF permeability test to determine the permeability of a flavorant through a given polymer in the presence or absence of a surface treatment. .

FIG. 16 is a perspective view of the permeability test apparatus (dispersion cell) of FIG. FIG. 17 shows an aroma compound having each of the following structural formulas, ethyl tiglate

Embedded image Aldehide C-8

Embedded image Wax of β-pinene and β-pinene

Embedded image 5 is a graph showing the permeability of the.

FIG. 18 is another graph showing the penetration of carnauba wax into aroma compounds such as ethyl tiglate, aldehyde C-8 and β-pinene. FIG.
Is ethyl tiglate, aldehyde C-8 and pinene,
It is another graph which shows the permeability of the carnauba wax to the aroma compounds, such as ethyl tiglate and (beta) -pinene which are not trapped as a control.

FIG. 20 is a graph showing the penetration of polyethylene wax (molecular weight 500) into aroma compounds such as ethyl tiglate, aldehyde C-8 and β-pinene, determined by the apparatus of FIGS. . FIG. 21 is a graph showing the permeability of β-pinene using a wax and a control such as cetyl palmitate (trade name: CUTINA wax), carnauba wax, polyethylene wax (molecular weight: 500), candelilla wax.

FIG. 22 is an enlarged view of that portion of FIG. 21 such that the weight loss of the tested product is between about 0 and 1 (mg-mm) / cm ² . FIG. 23 is a graph showing the permeability of ethyl tiglate using a wax such as cetyl palmitate (trade name CUTINA wax), carnauba wax, polyethylene wax, candelilla wax and a control. FIG. 24 shows the permeability of hydroxypropylcellulose to the aroma compounds such as β-pinene and ethyl tiglate and the control (the release control polymer of the present invention).
Or without wax).

FIG. 25 is a graph showing the penetration of polyvinyl alcohol into aroma compounds such as ethyl tiglate and β-pinene, and a graph showing the use of a control without using polyvinyl alcohol. FIG.
6 is a bar graph showing the geraniol substantivity on a piece of pure geraniol and a piece of geraniol cotton fabric encapsulated in candelilla wax microparticles. Substantivity is shown on the vertical axis.

FIG. 27 shows the persistence of geraniol on a piece of pure geraniol and a piece of geraniol polyester fabric encapsulated with candelilla wax microparticles.
7 is a bar graph showing tivity). Sustainability
y) is shown on the vertical axis. FIG. 28 shows the substantivity of the trade name GALAXOLIDE (trademark of IFF, New York, NY), a mixture of compounds having the following structural formulas, pure GAL
Figure 4 is a bar graph showing the substantivity on AXOLIDE and GALAXOLIDE brand cotton fabric pieces encapsulated with candelilla wax microparticles. Sustainability (su
bstantivity) is shown on the vertical axis.

[0082]

Embedded image FIG. 29 shows the brand name GALAXOLIDE and the brand name GA encapsulated in candelilla wax microparticles.
FIG. 4 is a bar graph showing the substantivity of geraniol on LAXOLIDE polyester fabric pieces.

FIG. 30 is a graph showing that a pure aroma compound, GALAXOLIDE (trade name), and a product obtained by encapsulating the same in a raw wax fine particle are continuously dispersed for two or more days. FIG. 31 is a graph showing the emission of geraniol having the following structural formula from particulate slurry applied to brown hair washed with water.

[0084]

Embedded image

Emissions from the slurry include both pure and encapsulated aroma compound geraniol. FIG. 32 is a graph showing the relationship between the odor intensity and the elapsed time of the flavoring agent S used together with the flavoring agent 361 encapsulated and the flavoring agent S used together with the flavoring agent 361 not encapsulated.

FIG. 33 shows the encapsulated flavoring agent 361.
5 is a graph showing the relationship between the odor dispersibility and the elapsed time of a mixture of the flavoring agent S used together with the flavoring agent S and the flavoring agent S used together with the flavoring agent 361 not encapsulated. FIG.
Is a graph showing the relationship between the odor intensity and the elapsed time of the flavoring agent S used with the encapsulated flavoring agent 885 and the flavoring agent S used with the unencapsulated flavoring agent 885.

FIG. 35 shows the encapsulated flavor 885
5 is a graph showing the relationship between the odor dispersibility and the elapsed time of the flavoring agent S used together with the flavoring agent S used together with the flavoring agent 885 not encapsulated. FIG. 36 is a graph showing the relationship between the odor intensity and the elapsed time of the fragrance S of the fragrance 075 encapsulated in carnauba wax and the fragrance S of the fragrance 075 not encapsulated. is there.

FIG. 37 shows the relationship between the dispersibility of the odor of the flavoring agent S of the flavoring agent 075 encapsulated with carnauba wax and the flavoring agent S of the flavoring agent 075 not encapsulated and the elapsed time. FIG. FIG. 38 shows the flavoring agent S.
4 is a graph showing the relationship between the odor intensity of flavoring agent S encapsulated with carnauba wax and elapsed time. FIG.
9 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S used together with the flavoring agent 361 encapsulated with carnauba wax and the elapsed time alone.

FIG. 40 is a graph showing the relationship between the odor intensity of the flavoring agent S used alone and the flavoring agent S used together with the flavoring agent 885 encapsulated with carnauba wax, and the elapsed time. FIG. 41 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S used together with the flavoring agent 885 encapsulated with the carnauba wax alone and the elapsed time.

FIG. 42 is a graph showing the relationship between the odor intensity and the elapsed time of the flavoring agent S used together with the flavoring agent S and the encapsulated flavoring agent 075. FIG. 43 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S used together with the flavoring agent 075 encapsulated in carnauba wax and the elapsed time only.

FIG. 44 is a side sectional view of the fine particles of the present invention. It shows a substantially hydrophilic surface treatment, such as in the form of a continuous submicron thick layer of the surface treatment, which is substantially coated and fixed over the entire outer surface of the single phase solid solution. . FIG. 45 shows the solid solution-fine particles of the present invention. The substantially hydrophilic surface treatment agent is almost directly (pr
oximate to and immediately) located below the outer surface of the solid solution and within the inner matrix volume.

FIG. 46 shows the particles of the present invention. A substantially hydrophilic surface treatment agent is substantially coated and immobilized on the outer surface of the single phase solid solution in the form of a continuous submicron thick layer; and (b) It is located proximate to and immediately below the outer surface of the solid solution and within the inner matrix volume.
FIG. 47 is a schematic diagram showing a side view of a dispersibility test apparatus for testing the dispersibility of a trapped or untrapped flavoring substance including an aroma compound and a flavoring composition.

FIG. 48 shows the apparatus of FIG. 47 viewed from above. FIG. 49 is a perspective perspective view of the first stage during operation of the rotor / stator high shear mixer. Inside, a precision made mixed workhead
The high-speed rotation of the rotating blade inside the
tor) Strong suction of liquid and solid substances into the device. FIG. 50 is a perspective perspective view of the second stage during operation of the rotor / stator high shear mixer used in the method and apparatus of the present invention. There, the material is moved around the work head by centrifugal force and crushed in a precisely created gap between the end of the rotating blade and the inner wall of the stator.

FIG. 51 illustrates a rotor / stator useful in practicing the apparatus and method of the present invention.
FIG. 7 is a perspective perspective view of a third stage during operation of the high shear mixer. In the second stage, following the first step, as the material emerges at high speed from the holes in the stator through the machine outlet and along the pipe, intense hydraulic shearing takes place. At the same time, there is a constant mixing and discharging cycle, with new material constantly being drawn into the workhead.

FIG. 52 is a side view of a homogenizer for performing the mixing step of the method of the present invention and as part of the apparatus of the present invention. FIG. 53 is a side sectional view of a valve component used in a single-stage homogenization section of the apparatus of the present invention.
FIG. 54 is a side cross-sectional view of a two-stage homogenization valve component used in the homogenization apparatus in the mixing step of the method of the present invention and the apparatus of the present invention.

FIG. 55 is a cross-sectional side view of a rotor / stator mixing component useful in performing the mixing step of the apparatus and method of the present invention. FIG. 56 is a block flow diagram showing the steps of the present invention when producing the particulate composition of the present invention. FIG. 56 is also a schematic diagram of the device of the present invention. FIG. 57 is a block flow diagram illustrating the steps of the present invention of a method useful in making the compositions of the present invention. FIG. 57 is also a schematic diagram of the device of the present invention.

FIG. 58 shows a schematic diagram of the apparatus and method of FIG. 56, which also shows an overview of the effective use of an electronic program controller (eg, a computer system). Thereby, information that is in demand in the marketplace, etc., can be used to automatically modify the variables of the method of the invention in which the components are mixed, heated and cooled. FIG. 59 shows a schematic diagram in which a device utilizing an electronic program controller (for example, a computer system) is added to the device of FIG. 57. Thereby, market demand information and the like can be used to automatically modify and adjust variables (eg, mixing, heating, ratio, cooling and flow rate) of the method and apparatus of the present invention.

FIG. 60 is a schematic flowchart showing a method for treating wax fine particles containing an active or physiologically active ingredient of the present invention. FIG. 61 shows the relationship between the vapor pressure, the total flavor component, and the logarithm of three different flavors, namely, flavors (described in Table 5), flavor A-2, and flavor A-3. It is a graph. The flavoring agents other than the flavoring agent A shown in the present embodiment are each composed of a unique composition, for example, Bulgarian rose oil: β-phenylethyl alcohol: β-ionone = 50: 25: 25.

FIG. 62 shows a low vapor pressure substance, a high vapor pressure substance,
Figure 4 is a graph showing the normalized weight loss (% by weight) versus time for different groups of three components, a mixture of high and low vapor pressure substances. FIG. 63 shows the weight percent and weight of the high vapor compression fragrance, Flavor A-3, both from the aroma dispersancy evaluation system (FIGS. 47 and 48) and the prior art gravimetric analysis system. Decrease ratio (1
6 is a graph showing a comparison with (% by weight per minute). FIG. 64 shows benzyl alcohol, geraniol, farnesol having the following structural formula and trade name GA
It is a graph which shows the relationship between the loading efficiency of the aroma compound of a compound such as LAXOLIDE (registered trademark of IFF) and log ₁₀ P.

[0100]

Embedded image Here, P represents the partition coefficient of octanol-water with respect to the aroma compound. The fine particles in this graph are candelilla wax fine particles.

FIG. 65 shows a surfactant having the following structural formula, 1.2% cetyltrimethylammonium chloride, 10% candelilla wax and 10% flavoring agent P-504.
Using a composition containing No. 48, a rotor / stato
r) The size distribution of the fine particles discharged from the mixer is shown. The graph shows the ratio between the volume percentage and the diameter of the fine particles.

[0102]

Embedded image FIG. 66 is a graph showing the relationship between the diameter and the volume percentage of the fine particles discharged from the homogenizer mixing device. Fine particles include cetyltrimethylammonium chloride 5%
And candelilla wax 10% and 10% flavoring agent IB-X-
016 is included.

FIG. 67 shows the elapsed time (minutes) of air flow (ml per minute) in the system of the present invention using the two cylinders connected in parallel shown in FIG. 48 described in detail above. 6 is a graph showing a relationship with the graph.

Next, embodiments of the present invention will be described in detail with reference to the drawings. 1 and 2, the number 10 refers to the fabric itself and the number 11
Means the space between the fabrics. With reference to FIGS. 3 and 4, the number 12 refers to the wax particles on the fabric surface. 5 and 6, the numeral 20 refers to the strand of hair itself.

Referring to FIGS. 7 and 8, reference numeral 21 denotes wax fine particles on the surface of the hair strand.
9 and 10, the number 23 refers to a strand of hair that has been washed with a conditioner. Referring to FIGS. 11 and 12, the number 24 refers to the wax particles on the surface of the hair strand.

Referring to FIG. 13, numerals 30a and 30b refer to bundles of fabric. Numeral 32 indicates particles trapped in holes between bundles. Number three
1 means the space between the bundles. FIG. 13 is an enlarged view of a portion 3A in FIG. Referring to FIG. 14, reference numeral 33 denotes a bundle of fabrics. The number 36 trapped in the space 37 indicates the fine particles trapped between the bundles. Numbers 33a and 33b and number 3
4 and 34b mean bundles of fabric. Number 35
Denotes fine particles directly attached through physical force to the bundle.

Referring to FIGS. 15 and 16, the fluid 46 is in the jar 44. The jar 44 has a side arm (side
arm) 45. Fluid 46 has reached fluid level 47. Directly above the fluid level 47 is the membrane tissue 41. Bolts 401a and 4 for tightening flanges in place
By using the flange 43 and the jar lip 42, the dispersed film structure 41 is disposed at a predetermined place.
The sidearm 45 is closed using a stopper 49. Numeral 40 indicates a permeable device.

The IFF penetration test is performed using the apparatus of FIGS. The weight of the membrane tissue 41 is first measured before being placed on the flange 43 and the jar lip 42. The substance 46 whose permeability is to be measured is placed in the jar 44 to a fluid level 47. The device containing the fluid 46 is located at a fixed location for a predetermined period of time. At the end of that time, bolt 4
The bolts 401a and 401b similar to 01c are loosened, and the flange 43 and the membrane 41 are removed and the weight is measured. Thereby, sufficient data for determining the permeability of the specific substance 46 is collected.

Referring to FIG. 17, numeral 52 is the data point for aldehyde C-8. Numeral 53 is the data point for ethyl tiglate. The Y-axis is a measure of weight loss, indicated by the numeral 54. The X-axis shows time (minutes) and is indicated by the numeral 55. Weight loss is measured in ^{(mg-mm) / cm 2} . Number 51 indicates the standard deviation of the data.

In FIG. 18, reference numeral 503 denotes a data point of aldehyde C-8. Numeral 502 represents a data point for β-pinene. Number 58 represents the data point for ethyl tiglate. Numeral 501 indicates a graph of the relationship between the elapsed time of ethyl tiglate and weight loss. This shows the permeability of carnauba wax into ethyl tiglate. The Y-axis represents weight loss by number 56 and the X-axis represents time by number 57. The number 59 represents the standard deviation of the ethyl tiglate data.

Referring to FIG. 19, reference numeral 507 is the encapsulated ethyl tiglate. Reference numeral 508 is a graph of the weight loss of ethyl tiglate versus elapsed time, showing the penetration of carnauba wax into ethyl tiglate. Number 506 is the data point for β-pinene in carnauba wax. Numeral 510 is an ethyl tiglate data point that is not trapped by a control release system such as carnauba wax. Numeral 509 is a data point for control of β-pinene without carnauba wax. Numeral 511 represents a graph of untrapped ethyl tiglate. Number 5
Reference numeral 12 represents a graph of β-pinene which is not trapped. The Y-axis indicating weight loss is designated by the numeral 505. Numeral 504 is an X axis indicating time (minute).

Referring to FIG. 20, numeral 515 represents the data points for ethyl tiglate in polyethylene (500 molecular weight) wax. Numeral 520 is a graph showing the relationship between time and weight loss. Numeral 516 is the data point for aldehyde C-8 in polyethylene wax. Number 517 is the data point for β-pinene in polyethylene wax. Reference numeral 519 refers to a graph of aldehyde C-8 in polyethylene wax. It shows the permeability of aldehyde C-8 to polyethylene wax. Reference numeral 520 shows a graph of ethyl tiglate in polyethylene wax showing the permeability of ethyl tiglate into the polyethylene wax. Number 513 is the X axis and number 514 is the Y axis.

Referring to FIG. 21, reference numeral 528 is cetyl palmitate (trade name CUTINA wax). Numeral 527 is the data point for carnauba wax. Number 526 is the data point for polyethylene wax. Numeral 525 is the data point for candelilla wax. Number 5
23 shows the control of β-pinene without wax (reference data). All data points except the control data on FIG. 21 indicate the penetration of β-pinene into the wax. The X axis of number 521 indicates time (minutes), and the Y axis of number 522 is (mg-
mm) / cm ² indicates weight loss.

FIG. 22 shows the part of FIG. There, the weight loss of β-pinene contained in the wax is from 0 to 1.4. In FIG. 22, reference numeral 533 indicates a standard deviation line. The number 521 means the X axis,
The number 522 means the Y axis of the weight reduction. Number 52
8 is the data point for cetyl palmitate. Number 526
Indicates data points for polyethylene wax (molecular weight 500). Reference numeral 530 represents a graph showing the relationship between time and weight loss of polyethylene wax containing β-pinene. Number 533a is the standard deviation line of the data showing polyethylene wax containing β-pinene. Number 52
9 shows a graph of carnauba wax containing β-pinene, showing the permeability of β-pinene into carnauba wax.

Referring to FIG. 23, reference numeral 538 indicates data points for cetyl palmitate (trademark CUTINA wax). Numeral 540 indicates a data point for carnauba wax. No. 541 is polyethylene (molecular weight 5)
00) Wax data points. Numeral 542 is the data point for candelilla wax. Number 537 is the control data point for ethyl tiglate without wax. Reference numeral 536 is a graph showing the evaporation rate of the control of ethyl tiglate without wax. No. 539 is cetyl palmitate (trademark CUTIN)
3 is a graph showing the permeability of ethyl tiglate into A wax). No. 543 is a graph showing the permeability of ethyl tiglate into carnauba wax. The number 534 indicates the X axis of time (minute). The number 535 means the Y axis of weight loss (mg-mm) / cm ² .

Referring to FIG. 24, reference numeral 562 is the data point for β-pinene contained in hydroxypropylcellulose. The number 564 is the data point for β-pinene not contained in any polymer and merely indicates the evaporation rate of β-pinene. Number 569 represents the standard deviation of the data for β-pinene not included in hydroxypropylcellulose. Number 563 is the data point for ethyl tiglate contained in hydroxypropylcellulose. Number 565 is the data point for ethyl tiglate that is not included in any polymer and merely indicates the evaporation rate of ethyl tiglate. No. 567 is a graph showing the permeability of ethyl tiglate into hydroxypropyl cellulose. Reference numeral 568 represents a graph showing the evaporation of ethyl tiglate (not included in any polymer). Reference numeral 566 represents a graph showing the evaporation of β-pinene not present in any polymer. The number 561 is the X axis representing time (minutes), and the number 560 is (mg-mm) / cm ² , meaning the Y axis of weight loss.

Referring to FIG. 25, numeral 552 is the data point for ethyl tiglate contained in the polyvinyl alcohol. The number 553 is polyvinyl alcohol (9
Data points for β-pinene contained in 9% hydrolyzed polyvinyl acetate). Numeral 554 is a data point of ethyl tiglate not contained in the polyvinyl alcohol, and simply indicates the evaporation ratio of ethyl tiglate. Number 555 is the data point for β-pinene not contained in any polyvinyl alcohol,
It simply shows the evaporation ratio of β-pinene. Reference numeral 557 shows a graph showing the evaporation ratio of β-pinene not contained in any polyvinyl alcohol. Number 559 is the data point for ethyl tiglate and β-pinene not contained in any polyvinyl alcohol. The number 551 is the X axis representing time (minutes). The number 560 means the weight loss (mg-mm) / cm ^{2 on} the Y axis.

Referring to FIG. 26, reference numeral 60 indicates a substantial percentage in the Y axis. Numeral 61a shows a bar graph of pure geraniol using pure water. The bar graph of geraniol washed with pure water contained in the fine particles of candelilla wax is indicated by reference numeral 61b. A bar graph of pure geraniol with detergent is shown at number 62a. A bar graph of pure geraniol contained within the candelilla wax microparticles is indicated by detergent number 62b. Number 63a shows a bar graph of fabric softener of pure geraniol. Numeral 63b indicates a bar graph of geraniol contained in the fine particles of candelilla wax.

Referring to FIG. 27, reference numeral 64 indicates a substantial existence ratio (%) on the Y axis. The number 65a represents the substantial abundance of pure geraniol washed with pure water on the polyester fabric. Reference numeral 65a 'represents a standard deviation line of pure geraniol to be washed with pure water. Number 65b represents the use of pure geraniol encapsulated with candelilla wax microparticles when washed with pure water. The number 65b 'represents the standard deviation line of geraniol encapsulated in candelilla wax washed with pure water. The number 66a indicates the use of pure geraniol contained in a detergent on polyester fabric. Reference numeral 66b indicates the use of geraniol encapsulated in candelilla wax microparticles used in a cleaning agent. Number 67a represents the use of pure geraniol in a fabric softener on polyester fabric. Number 67b represents the use of geraniol encapsulated in candelilla wax microparticles used in a fabric softener on polyester fabric.

Referring to FIG. 28, reference numeral 601 indicates the Y axis representing the substantial existence ratio in percentage. The number 602a represents the use of the pure trade name GALAXOLIDE contained in a detergent on cotton fabric. Number 60
2b is GALAXOLID brand name encapsulated in candelilla wax microparticles contained in a detergent on cotton fabric
E is used. No. 603a is the pure trade name GALAXOLIDE contained in a fabric softener on cotton fabric.
Represents the use of. The number 603b represents the use of GALAXOLIDE® encapsulated in candelilla wax microparticles contained in a detergent on cotton fabric.

Referring to FIG. 29, the substantial existence ratio (%)
Is represented on the Y axis using the number 604. In FIG. 29, the number 605a represents the use of the pure trade name GALAXOLIDE contained in the detergent on the polyester fabric. The number 605b represents the use of GALAXOLIDE® encapsulated in candelilla wax microparticles contained in a detergent on polyester fabric. The number 605b 'represents the standard deviation when using GALAXOLIDE.RTM. Encapsulated in candelilla wax microparticles with a detergent on a polyester fabric.

The number 606a is the pure trade name GALAXOLI contained in a fabric softener on polyester fabric.
Indicates the use of DE. No. 606a 'is a pure brand name GAL contained in a fabric softener on polyester fabric.
AXOLIDE represents the standard deviation of the data. Number 606b represents the use of GALAXOLIDE® encapsulated in candelilla wax microparticles contained within a fabric softener on polyester fabric. Number 606
b 'is GALA brand name encapsulated with candelilla wax microparticles with fabric softener on polyester fabric
It represents the standard deviation of XOLIDE data.

Referring to FIG. 30, there is shown a sustained release of GALAXOLIDE® over two or more days as a pure aroma compound and when encapsulated with candelilla wax microparticles.
The number 70 represents the Y axis. The number 71 represents the X axis of time in days.

Number 72 is the pure trade name GALAXOLI
4 shows a graph of the use of DE. The number 72 'represents the data point under the pure trade name GALAXOLIDE.
Numeral 73 represents a graph of GALAXOLIDE (trade name) contained in the fine particles of candelilla wax. Number 7
03 represents data points of the trade name GALAXOLIDE encapsulated in candelilla wax microparticles. Reference numeral 704 represents the standard deviation of the data points of the brand name GALAXOLIDE encapsulated in candelilla wax microparticles.

Referring to FIG. 31, reference numeral 74 denotes Y representing the proportion of the aroma compound (geraniol) remaining in the brown hair.
Axis. Numeral 75 is the X-axis meaning release time in days. Reference numeral 76 represents a graph showing the release ratio of pure geraniol. Number 7
01 is the data point for pure geraniol. Number 702
Represents the standard deviation of the data points for pure geraniol. Reference numeral 77 indicates a graph of the geraniol emission ratio encapsulated in candelilla wax microparticles. Number 79 represents data points for geraniol encapsulated with candelilla wax microparticles. Number 78 represents the standard deviation of the data points for geraniol encapsulated with candelilla wax microparticles.

Referring to FIG. 32, the Y axis, which means odor intensity on a scale of 1 to 10, is designated by the numeral 80. The X axis indicating the time in hours (hr) is number 81
Indicated by Numeral 82 represents a graph showing the relationship between the odor intensity of the flavoring agent S combined with the encapsulated flavoring agent 361 and time. Numeral 83 represents a graph showing the relationship between odor intensity and time for a combination of the flavoring agent S and the encapsulated flavoring agent 361.

Referring to FIG. 33, the Y-axis is indicated by numeral 84 and represents the odor dispersibility on a scale of 1 to 10. Numeral 85 represents the X-axis which means the time in hours (hr). Numeral 86 indicates the encapsulated flavoring agent 36
This means a graph showing the relationship between the dispersibility of the odor of the flavoring agent S bound to No. 1 and time. Reference numeral 87 denotes a graph showing the relationship between the odor dispersion of the flavoring agent S bound to the non-encapsulated flavoring agent 361 and time.

Referring to FIG. 34, reference numeral 801 denotes the flavoring agent S.
And a graph showing the relationship between odor intensity and time for the encapsulated flavoring agent 361. Number 802
Means a graph showing the relationship between odor intensity and time for flavoring agent S and flavoring agent 361 which is not encapsulated.

Referring to FIG. 35, the number 803 indicates the flavoring agent S.
And a graph showing the relationship between the dispersibility of the odor for encapsulated flavoring agent 885 and time. Number 804
Means a graph showing the relationship between odor dispersibility and time of flavoring agent S combined with unencapsulated flavoring agent 885.

Referring to FIG. 36, the number 805 indicates the flavoring agent S.
And a graph showing the relationship between odor intensity and time for encapsulated flavoring agent 075. Number 806
Means a graph showing the relationship between odor intensity and time for flavoring agent S and flavoring agent 075 not encapsulated.

Referring to FIG. 37, reference numeral 807 indicates the flavoring agent S.
And a graph showing the relationship between dispersibility of odor and time for encapsulated flavoring agent 075. Number 80
Reference numeral 8 denotes a graph showing the relationship between the odor dispersibility (diffusivity) and time for the flavoring agent S and the non-encapsulated flavoring agent 075. According to these graphs, it can be assumed that the carrier is in the topnotes during storage and is attached to the hair.

Referring to FIG. 38, reference numeral 809 indicates the flavoring agent S.
Is a graph showing the relationship between odor intensity and time only, and reference numeral 810 represents a graph showing the relationship between odor intensity and time for the encapsulated flavor 361 and flavor S.

Referring to FIG. 39, reference numeral 811 denotes the flavoring agent S.
4 shows a graph showing the relationship between the odor dispersiveness (diffusivity) and time with respect to time alone. Numeral 812 is a graph showing the relationship between the odor diffusivity and time when the encapsulated flavoring agent 361 and flavoring agent S coexist. Systems containing encapsulated flavors are clearly superior to pure oils. The observed difference in odor intensity in these systems is noticeable.

Referring to FIG. 40, the graph denoted by reference numeral 813 shows the relationship between odor intensity and time for only the flavoring agent S. The graph with reference numeral 814 is a graph showing the relationship between odor intensity and time for the flavoring agent S taken out together with the encapsulated flavoring agent 885.

Referring to FIG. 41, the graph with reference numeral 815 shows the odor diffusivity for the flavoring agent S alone.
And the relationship between time and time. The graph with the number 816 shows the relationship between the odor diffusivity and time for the flavoring agent S coexisting with the encapsulated flavoring agent 885.

Referring to FIG. 42, the graph indicated by reference numeral 817 shows the relationship between odor intensity and time for the flavoring agent S alone. The graph with the number 818 shows the relationship between odor intensity and time for the flavoring agent S coexisting with the encapsulated flavoring agent 075.

Referring to FIG. 43, the graph with reference numeral 819 shows the relationship between the dispersibility of the odor and the time for only the flavoring agent S. The graph with reference numeral 820 shows the relationship between odor dispersibility and time for the flavoring agent S coexisting with the encapsulated flavoring agent 075. These graphs show the volume and tenacity of the encapsulated flavoring 075.
Indicates that up to 5 hours is higher than the flavoring agent S alone. Encapsulation systems are used to increase substantivity.

Referring to FIG. 44, the substantially hydrophilic surface treating agent 93 is substantially firmly fixed over the entire outer surface 95 of the single phase solid solution 91 in the form of a continuous submicron layer of the surface treating agent 92. ing. Microparticles having a surface treatment agent covered within a submicron layer are designated by the numeral 90.

Referring to FIG. 45, the substantially hydrophilic surface treatment agent 903 is substantially located almost directly below the entire outer surface 905 of the solid solution 901 (located proximate to and suture).
bstantially beneath the entirety of outersurfac
e) and substantially within the inner matrix volume. The charge of the microparticle is indicated using the number 904,
The particles themselves are designated by the numeral 900.

Referring to FIG. 46, both of the substantially hydrophilic surface treatment agents 917 and 913 are (a) surface treatment agent 9
It is substantially covered and firmly fixed over the outer surface 915 of the single-phase solid solution 911 in the form of twelve continuous submicron layers, and (b) substantially directly below the entire outer surface of the solid solution 915. At least substantially within the interior matrix volume. The surface treatment in the matrix volume is indicated by the numeral 917. The surface treatment in the submicron layer is designated by the numeral 913. The particles are designated by the numeral 910. The charge on the outer surface 916 of the particle is indicated by the numeral 914.

FIGS. 47 and 48 show a system for evaluating the dispersibility of a flavoring agent for determining the dispersibility and permeability of a flavoring substance and other active or physiologically active ingredients used in the embodiment of the present invention. Represents. The test sample on blotting paper, designated by the number 1001, has an opening 1 to the atmosphere.
004 is supported by a support 1002 in a container 1003 having a 004. Air flow through line 1010
Air is supplied from an air supply 1005 through a tube 1006 having a pressure meter 1007 for measuring air flow.
The container 1003 has a side wall 1012 through which a temperature sensing probe 1009 is located. A temperature monitor 1008 is attached to the temperature detecting end (probe) 1009. The container 1003 has a bottom wall 1011. The entire device is indicated by the number 1000. FIG.
47 is a top view of the apparatus of FIG. 47 showing the use of two tandem chambers 1003a and 1003b. The container 1003a is supplied with airflow through a tube 1010a having a pressure meter 1007a in the airflow line. The pressure meter 1 in the air flow line is provided in the container 1003b.
An air flow is supplied through a tube 1010b having 007b. Air supply from location 1005 is provided through line 1006a with in-line pressure gauge 1007 for measuring air flow. The airflow then
Line 1006b (for flowing air to container 1003b) and line 1006c (for flowing air to container 1003b).

The temperature detecting end (probe) 1009a is the container 1
003a, the temperature probe (probe) 10
09b is used for the container 1003b. The temperature detection end 1009b is attached to the temperature monitor 1008b. The temperature detection end 1009a is attached to a temperature monitor 1008a. The container 1003a has an opening 100 at the top.
4a. The container 1003b has an opening 1
004b. Whole device having a tandem container for testing purposes is indicated by reference numeral 1000 ^1.

The systems illustrated by FIGS. 47 and 48 are based on time, in a temperature and air mixing controlled environment, with respect to comfort, strength, volatile content and weight loss. The main purpose is to simultaneously evaluate the effect of freshening the air. Flavoring agent dispersibility evaluation systems are between laboratory systems that are only allowed to make analytical measurements and full-scale tests of odor effects in specially designed rooms where only sensory tests are allowed. Is something in between. The flavoring agent dispersibility evaluation system provides a control environment at which the flavoring action can be measured sensorially and analytically at low cost.

The flavor dispersant evaluation system illustrated by FIGS. 47 and 48 has a height of about 50 to about 75 cm, a radius of about 15 to 30 cm, and a diameter of about 0.1 to 0.2 m ^3.
Consists of a cylinder having a volume of. The interior is covered with aluminum foil to prevent fragrance from being absorbed into the wall. Air flow from bottom to about 3 to 10
Supplied from a tube that penetrates the sides of cm and extends to the center of the chamber. The temperature is about 10 to 30 from the bottom
It is constantly monitored by scales located between cm. An opening with a diameter of 15 to 30 cm for air flow and for testing the intensity of the odor is on the top of the cylinder. On average, the air flow is between 900 and 1,000 ml per minute. This air flow replaces the entire volume of the aroma dispersancy evaluation system with fresh air every two hours. Air flow through the chamber is about 0.5 to 2
Constant at pressures between psig.

Referring to FIG. 49, the high speed rotation of rotary blade 1106 in a precision made mixing work head applies liquid and solid material 1 to rotating stator assembly 1100.
Water is strongly absorbed at the location 1101 so as to draw the 104a. Rotation occurs at access 1102. Discharge from assembly 1100 occurs at location 1103. The number 1105 indicates a work head. Number 1100
Means the entire device.

Referring to FIG. 50, the centrifugal force moves the material 1104a around the work head, where grinding occurs in a precisely created gap between the end of the rotary blade and the inner wall of the stator. Referring to FIG. 51, the second stage (stage
2) is performed in the following procedure. First, substance 110
4b is accelerated while exiting along the pipework 1103 through the hole in the stator 1106 and then through the exit of the machine, causing intense hydraulic shear. At the same time, the new material constantly mixes and pumps out while the work head (wo
rkhead).

Referring to FIG. 53, a single stage homogenous valve assembly, valve handle 1112a, is used to regulate flow, inward at location 1113a and outwardly at 1114a, respectively.

Referring to FIG. 54, FIG. 54 illustrates the two-stage valve assembly of the homogenizer. Valve handle 1111 is used to adjust the first stage, and valve handle 1112 is used to adjust the second stage. Two-stage valve assembly seal 111
7 and intervals 1115 and 1116. Number 11
Reference numeral 13 denotes an inlet of the two-stage valve assembly, and number 1
114 represents the outlet of the two-stage valve assembly. Numeral 1118 represents the passage between the inlet 1113 and the outlet 1114. The entire second stage valve assembly is numbered 1110
Is attached.

FIG. 52 is an overall view of the homogenizing apparatus. Mixer 1120, including mixing shaft 1112, is a feed tank heated by steam. The homogenizer is shown with a two-stage pressure regulation system. The first stage handle is number 11
The second stage handle is indicated by the numeral 1112, indicated by 11. Pressure meter 1122
Is used to observe the flow of the fluid containing the emulsion through the cooling coil 1130 and the three-way bypass valve to the recycle line 1114. A temperature meter 1124 monitors the temperature of the fluid flowing through line 1113 to the two-stage valve assembly attached to gearbox 1123. The entire homogenizer is number 1110
Indicated by

Referring to FIG. 55, the rotor / stater (s
The first mixing operation in the mixer is performed in a steam heated feed tank 1140 equipped with a stirrer 1146. Fluid flows through line 1144 to a controlled rotator / stator mixing head 1142 to control box 1141. The fluid then flows through line 1142a to three-way valve 1150. The fluid flows through cooling coils 1143 and 1143a. The fluid also passes through a three-way valve and returns to the supply tank 1140 through circulation lines 1147 and 1147a. The mixed rotor / stator assembly is numbered 1190.

Referring to FIG. 56, the flavoring substance from the container 1201 is controlled by the valve 1202 and
Flow through At the same time, polymer and / or wax flows through line 1207, controlled by valve 1206, from vessel 1204 heated using heater 1205. Both the odorant and the polymer and / or wax flowing through lines 1203 and 1207 are mixed in mixing tank 12 where heater 1221 is installed.
08. The mixing thus performed is combined with the material discharged from the mixer 1215 through a controlled line 1219 by a valve 1218 and the blender.
der) 1220. The surface treatment agent from the container 1209 is supplied to the line 1214 via the control valve 1211.
Flow through

At the same time, the water or aqueous mixture from the container 1210, which has been preheated using the heater 1230, is mixed with the mixing container 121 in which the heater 1231 is installed.
5 through control valve 1212 through line 1213. The surface treatment / aqueous mixture is then passed through line 1217 via control valve 1216 to mixer 1220 with material from line 1219.
Mixer 1220 is a homogenizer and / or a rotor / stator high shear mixer. Upon completion of mixing using a homogenizer and / or a rotor / stator high shear mixer, the material passes through line 1223 via control valve 1222 and solid phase particle forming apparatus 1225 with cooling coil 1224 installed.
Flows to The integrated component 1190 shown in FIG. 55 or FIG. 52 in which the device components 1220 and 1225 are integrated.
May flow to the assembly part 1110 shown in FIG. The resulting particulate slurry then passes through line 1227 via control valve 1226 for further utilization.

Referring to FIG. 57, flavoring material is supplied from container 1250 via control valve 1258 through line 1259 to mixer 1260 with heater 1261. At the same time, the container 12 with the heater 1252
From valve 51 through control line 1256 via valve 1257 the polymer and / or wax is mixed into mixer 126
0. At the same time, the valve 12
The surface treating agent is supplied to the mixing vessel 1260 through the line 1254 via 55. While the mixing vessel 1260 is mixing the odorant, polymer or wax and the surface treatment agent, the aqueous composition heated through the heater 1265 in the vessel 1264 passes through the control valve 1267 through the line 1266 to the mixer 1268. Supplied to

The substance mixed in the container 1260 passes through the control valve 1263 and through the line 1262 to the mixer 1
268. Mixer 1268 can be a homogenizer and / or a rotor / stator high shear mixer. The resulting material is then fed via line 1269 via valve 1270 to a solid phase particle forming vessel 1271 equipped with cooling coil 1272. Further, the containers 1271 and 1268 can be combined to form the device 1190 shown in FIG. 55 or the device 1110 shown in FIG. The material comprising solid particulate particles having a continuous surface is then
It is sent to the container 1275 through 74 via the line 1273 for efficient use of the slurry.

The apparatus shown in FIG. 56 is used in connection with an electronic program controller 1300 as shown in FIG. The electronic program controller 1300
Market input information from source 1299 is used. Market input information for controlling the apparatus shown in FIGS. 56 and 58 via a control line is provided by control line 1299c.
Via the source 1299 to the electronic program controller 1300.

Thus, the device illustrated in the schematic diagram of FIG. 56 is also illustrated in the schematic diagram of FIG. 58 as being associated via a control line with an electronic program controller (computer system).

Further, the control valve 120 is
Control of the odorant sent via line 1203 via line 2 is performed via control line 1202c. Similarly, the container 1204 through the valve 1206 and the line 1207
The flow of polymer and / or wax delivered from is controlled via control line 1206c.

The heating rate and the amount of thermal energy to the container 1204 using the heater 1205 are controlled by the control line 1204.
5c. Flavoring substances, polymers and / or
Alternatively, the mixer 1208 for mixing the wax is a heater 1221 controlled through a control line 1221c.
Heated through. The mixing energy in the mixer 1208 is controlled through a control line 1208c. The surface treatment agent contained in the container 1209 is mixed with the mixer 121.
5 through line 1214 via valve 1211, the water or aqueous solution from vessel 1210 is heated by heater 1230 and flows to mixer 1215 via valve 1212.

The valve 121 for the aqueous solution from the container 1210
2 is controlled through control line 1212c. The amount of heat energy to the aqueous solution in the container 1210 is
It is controlled through a control line 1230c. Mixer 12
The flow rate of the surface treatment agent from the container 1209 to 15 is controlled through a control line 1211c. Heater 123
Heat input from 1 to mixer 1215 is applied to control line 12
31c. The surface treatment agent / water solution mixture made in the container 1215 is supplied to the mixer 1220 through the line 1217.

The mixing energy in the mixer 1220 is controlled through a control line 1220c. Valve 1218
Mixing vessel 122 via line 1219 via
The flow of material from container 1208 to 0 (eg, a homogenizer) is controlled through control line 1218c. The control of the supply of the surface treatment agent / aqueous composition from the mixing vessel 1215 to the mixer 1220 through the valve 1216 and the line 1217 is performed by a control line 121.
6c.

The supply amount of the emulsion from the mixer 1220 through the valve 1222 and the line 1223 is controlled through the control line 1222c, and the cooling energy using the cooler 1224 of the solid phase particle forming vessel 1225 is controlled through the control line 1224c. Controlled. The mixing energy in the solid phase particle forming container 1225 is controlled through the control line 1225c. Solid phase particle forming container 12 for effective use, storage and recording of container 1228
25 is controlled through control line 1226c so that market input and output information is
Collected through c.

Similarly, the apparatus of FIG. 59 can be used in connection with an electronic program controller 1302, which uses market input information from a source 1301.
Market input information for controlling the apparatus shown in FIGS. 57 and 59 via a control line is provided to an electronic program controller 1302.

Thus, the device shown in the diagram of FIG. 57 is also shown schematically in FIG. 59 which is associated with an electronic program controller (computer mechanism) via a control line.

Further, a line 125 passes through a valve 1258.
Perfume from container 1250 passing through 9 is controlled by control line 1258c. Control line 1257c includes polymer and / or wax from vessel 1251 passing through line 1256 via control valve 1257.
Controlled by. At the same time, a container 12 for heating the polymer and / or wax using the heater 1252
The heat input to 51 is via control line 1252c
Is controlled by At the same time, the surface treatment agent from vessel 1253 flowing through line 1254 via valve 1255 is controlled by control line 1255c.

The surface treating agent, the polymer and / or the wax, and the odorant are mixed in the mixing container 1260. The mixing energy is controlled by the control line 1260c, and the heat input to the mixing vessel 1260 is controlled by the control line 1261.
c. The aqueous composition comprises a thermal element (12).
Heated in vessel 1264 through 65. Heating element 1
265 is controlled by a control line 1265c. The aqueous composition flowing through line 1266 via valve 1267 is controlled by control line 1267c. The mixture of odorant, polymer and / or wax, and surface treatment agent in mixing vessel 1260 is then
It flows through line 1262 via 263. The flow of the mixture to the mixer (e.g., homogenizer) 1268 is controlled by control line 1263c. Valve 12
The flow of the aqueous composition from vessel 1264 to mixer (eg, homogenizer) 1268 via line 1266 via 67 is controlled by control line 1267c.

The homogenizing energy of mixer 1268 is controlled by control line 1268c. Dispersion (diff) from mixer 1268 through valve 1270 and line 1269
The material to be usion has a controlled flow through control line 1270c. The solid phase particle forming component 1271 of the device of the present invention is provided with a controlled cooling coil 1272 through a control line 1272c.

The operation of the solid phase particle forming component of the apparatus of the present invention is controlled through a control line 1271c. The flow from the solid phase particle forming vessel to a location 1275 for utilizing, storing, inventorying and marketing the slurry via valve 1273 via line 1274 is controlled via control line 1273c. Marketing inputs and outputs to location 1275 are controlled through control line 1275c.

As shown in FIG. 60, the wax layer at location 1306 is mixed with fragrance oil at location 1308, mixed with additives if necessary, and poured into container 1309.
At the same time, the emulsion and water warmed to 90 ° C. at location 1305 are also mixed with the surfactant at location 1307 and poured into container 1309. The liquid in the container 1309 is returned to the container 1309 again within a certain time (for example, one minute) via a mixer or a homogenizer 1310. Place 1
This liquid at 311 is again cooled via the homogenizer 1312 using the heat exchanger at location 1313 and becomes solid.

As shown in FIG. 61, reference numeral 1403 represents a data point of the flavoring agent A-1. Number 1404 is the data point for flavor A-2 and number 1405 is the flavor A
-3 data points respectively. The number 1406 shows a graph of the data points 1403, 1404 and 1405. The Y axis indicated by the number 1401 is ｛log
₁₀ [VP] Represents 圧 (vapor pressure). The X axis indicated by reference numeral 1402 is the total accumulation (% by weight) of the fragrance components of the flavoring agents A-1, A-2, and A-3. Curve 1406 is also represented by the following equation. {Log ₁₀ [VP]} = (0.046) S ³ + (1.6
^{73) S 2 - (16.41)} S-4

Here, S represents the total accumulation (% by weight) of the fragrance components, and {log10 [VP]} represents the record of the vapor pressure of each fragrance component.

As shown in FIG. 62, the Y-axis has the number 1501
And represented by the symbol W in the formula, and represents a standardized weight loss (% by weight). The X axis of the number 1502 is indicated by the symbol θ and represents time. Reference numeral 1503 represents a data point when the high vapor pressure substance and the low vapor pressure substance are mixed at 50:50. No. 1504 is a low vapor pressure substance (<0.01 mm / H
g), and number 1505 is a high vapor pressure substance (> 0.1 m
m / Hg). Numeral 1508 is a graph showing the weight loss and time of the mixture (50:50) of the high vapor pressure substance and the low vapor pressure substance, and is expressed by the following equation. W = 94.583-0.29497θ

The number 1509 is expressed by the following equation representing the relationship between the weight loss of a low vapor pressure substance and time. W = 98.679−0.094778θ The number 1507 is a graph showing the weight loss of the high vapor pressure substance versus time, and is expressed by the following equation. W = 95.679-0.43843θ

FIG. 63 shows a method for evaluating the aroma dispersibility, in which the Y axis representing the rate of weight loss (% by weight / minute) is indicated by reference numeral 1601 and is expressed by the term (dw / dθ). The X axis, which represents the weight percent of the formula for flavoring agent A-3, is designated by reference numeral 1602 and is designated by the term W. Numeral 1603 represents the weight loss percentage vs. weight% data point of the equation as determined by gravimetric analysis. The number 1604 is shown in FIG.
50 represents data points of percent weight loss vs. weight% of the equation measured by the Aroma Dispersibility Evaluation System (FES) of FIGS. 7 and 48. The number 1604a indicates the standard deviation of the data point 1604. Numeral 1605 is a graph of weight loss rate (speed) vs. weight% in the equation measured by the evaluation system, and is represented by the following equation.

[0174] (dw / dθ) = 0.10675 + 0.003965W and _{Ln e (0.10675 + 0.00395W) =} θ Here, numbers 1606 and the weight loss rate (speed) versus weight percent of the graphs as measured by thermogravimetric analysis And is represented by the following equation: (Dw / dθ) = 0.061929 + 0.00319W and _{Ln e (0.061929 + 0.00319w) =} θ

Prior art thermogravimetric analysis (TGA) is
The details of Kroschwitz's "Polymers: Polymer Characteristics and Analysis", pages 837 to 848 (Chapter of Thermal Analysis), published by John Wiley and Sons in 1990, are incorporated herein by reference. ing.

As shown in FIG. 64, the Y axis is numbered 1701.
And represents an aroma compound having an efficiency indicated by the symbol ε. X axis is number 170
2 and represents the log ₁₀ value. Here, P is benzyl alcohol, geraniol,
Farnesol, n for brand name GALAXOLIDE
Octanol-water partition coefficient. Number 1703 is the data point for benzyl alcohol. Number 170
4 is the data point for geraniol. Number 170
4a represents the data point standard deviation of geraniol. Numeral 1705 is a data point of Furnessor having the following structural formula.

[0177]

Embedded image

The number 1705a represents the standard deviation of the data points of Furnesol. The number 1706 is a data point of the trade name GALAXOLIDE. No. 1708 is a graph of the efficiency of the aroma compound against the log ₁₀ P value. Here, P is the partition coefficient of n-octanol water for the aroma compound. The graph is also represented by the following equation: ε = 16.1433 {log ₁₀ P} −5.922 An aroma compound having an efficiency ε is represented by the following equation. _{ε = (m c / mγ)} × 100 where m _c term represents the amount of aroma compound encased microparticulate. The term mγ represents the total amount of the microparticle slurry.

The n of the perfume substance represented by the item P
The octanol water partition coefficient is the ratio between the equilibrium concentration in n-octanol and the equilibrium concentration in water. The fragrance of the present invention (pe
The rfume) feed has an n-octanol water partition coefficient P value ranging from about 10 to about 10 ⁸ . The perfum of the present invention (perfum
e) The distribution coefficient of the composition has a numerical value in the range of 10 to 10 ⁸ , so that the logarithmic form defining ₁₀ , log ₁₀
P is conveniently given. Thus, perfume materials useful in practicing the present invention have log ₁₀ P values ranging from about 1 to about 8 as indicated above.

The log _{10 of} many perfume compositions
P-values can be found, for example, in Daylight Chemical Information Systems, Inc. of California;
ht CIS), for example, reported in the Pomona 92 database, and includes many with citations of source documents. However, the log ₁₀ P values are based on the “CLOG” also available at Daylight CIS.
Calculations by the P "program are most often used.
The program also records the experimental log ₁₀ P values as obtained by the Pomona 92 database. "Calculated log ₁₀ P" has been measured by the Hans and Leo fragmentation approach (C. Hans
ch, PGSammons, JBTaylor and CARamsdem, edit, 29
"Comprehensive Medicinal," edited by Pergamon Press, 1990, page 5.
In carrying out the “Chemistry”, Volume 4 is incorporated herein by reference). This component approach is based on the chemical composition of each component of the perfume material and is based on the number and type of atoms.
y) is chemically bonded. This calculated log ₁₀
The value of P is the most reliable and widely used assessment of this physicochemical property, and rather the empirical log ₁₀ P value when choosing a perfume material in practicing our invention. Is used instead of

FIG. 65 shows a rotator / stator mixer using 10% candy lila wax, 10% flavoring agent P-50448 and 1.2% cetyltrimethylammonium chloride having the following structure: The created particle size distribution is shown.

[0182]

Embedded image

The particle size distribution is shown by reference numeral 1803. The X axis is the number 1802 which indicates the particle diameter in microns.
It is represented by Y axis is volume% of each particular particle diameter
And is represented by the number 1801. The average particle size of the particles is 2.4 microns and the distribution is as follows:

90% of the particles are finer than 3.8 microns 75% of the particles are finer than 2.8 microns 50% of the particles are finer than 2.0 microns 25% of the particles are finer than 1.4 microns 10 of the particles finer than 1.4 microns % Is finer than 1.1 micron

In FIG. 66, the particle size homogenized using 10% of candelilla wax, 10% of aroma agent IB-X-016 and 0.5% of cetyltrimethylammonium chloride having the following structure is shown. Show.

[0186]

Embedded image

The particle size distribution is as follows. Average particle size: 0.74 micron 90% of particles finer than 2.60 microns 75% of particles finer than 0.70 microns 50% of particles finer than 0.19 microns 25% of particles finer than 0.19 microns 0.14 10% of particles finer than 0.1 micron are finer than 0.12 micron

The X axis is designated by the numeral 1812 and indicates the particle diameter in microns. The Y axis is designated by the numeral 1811 and indicates the volume percentage of particles of a particular particle diameter. Number 1813 indicates those particles having a particle diameter from zero to about 0.4 microns. Reference numeral 1814 indicates those particles having a particle diameter from about 0.4 to about 1 micron. Number 1815
Indicates those particles having a particle diameter from about 1.3 to about 1.6 microns.

Referring to FIG. 67, the Y axis is represented by numeral 1906, and the X axis indicating time (minutes) is represented by numeral 1905. Number 1901 represents the second airflow data point for the two cylinders. Numeral 1902 indicates the airflow data point for the first of the two cylinders in FIG. Numeral 1903 shows a graph of air flow versus time for the first of the two cylinders of FIG. Numeral 1904 shows a graph of air flow versus time in the first of the two cylinders shown in FIG.

The following examples specifically illustrate the present invention. All claims, all parts, percentages and ratios referred to herein are by weight unless otherwise indicated.

The flavoring compositions shown in Table 5 below were prepared for use in Examples 1-4 below.

[0192]

[Table 5]

Example 1 Preparation of Fine Particles Use of Silverson L4R Laboratory Mixer of FIG. 55

The following procedure was performed using the Silverson L4R laboratory mixer previously shown in FIG.
grance) and candelilla wax. The resulting composition is 84.7% water, 10% candelilla wax, 5% fragrance in Table 5, 0.3% cetyltrimethylammonium chloride having the following composition:

[0195]

Embedded image

(1) 37.5 grams of candelilla wax is placed in a 125 ° C. oven and melted. (2) Put 314.87 grams of deionized water into a 1 gallon tank steam jacket. (3) The bottom of the tank is connected to the suction pipe side of the Silverson in-line L4R laboratory rotor / state mixer. The output from the mixer is recycled to the tank via a pipe. (4) Slowly rotate the mixer, pour water into the mixer, and suck back into the tank. (5) Add 3.88 grams of 29% cetyltrimethylammonium chloride aqueous solution to the water.

(6) Steam is put in a jacket, and a solution of water and a surface treating agent is heated to 90 ° C. A counter-rotating propeller mixer installed in the tank ensures that the temperature of the water is equalized. (7) Remove the candelilla wax from the oven and manually mix 18.75 grams of the fragrance of Example A into the wax using a glass rod. (8) Inject the mixture of fragrance and wax into the tank. The rotation speed of the counter-rotating propeller mixer is accelerated to disperse the wax and oil in the water so that a uniform emulsion is maintained. (9) Set the mixer to the maximum speed and emulsify for one minute. Adjust the steam rate so that the product maintains a temperature of 90 ° C. (10) Reduce the speed of the mixer to a minimum, divert it from the three-way valve at the outlet of the mixer and pass it through the Parker double heat transfer coil to solidify the emulsified wax and match the temperature of the slurry with the surroundings To lower.

Example 2 A method for producing fine particles using the Gorin 15MR homogenizer shown in FIG. 52 and the pressure regulating valve system shown in FIG. 54.

The following procedure involved the use of candelilla wax and the fragrance of Table 5 (fra) using a Gaulin 15 MR homogenizer.
grance) to produce fine particles. 84.7% water 10% candelilla wax 5% fragrance of Example A 0.3% cetyl totimethylammonium chloride having the following structural formula

[0200]

Embedded image

The procedure is as follows. (1) 75 g of candelilla wax is placed in a 125 ° C. oven and melted. (2) Place 629.74 grams of deionized water in a 1 gallon tank steam jacket. (3) Connect the bottom of the tank to the water absorption side of the Gorin 15MR-8TA laboratory homogenizer by pipe connection. The output from the mixer is recycled to the tank via a pipe. (4) Switch on the homogenizer set to a second pressure of 500 psig. Allow the water to be drawn into the homogenizer and back into the tank. (5) Add 7.78 grams of 29% active cetyltrimethylammonium chloride aqueous solution to the water.

(6) Steam is put in a jacket, and a solution of water and a surface treating agent is heated to 90 ° C. A counter-rotating propeller mixer installed in the tank keeps the temperature of the water uniform. (7) Remove the candelilla wax from the oven and manually mix 37.5 grams of the fragrance of Example A into the wax using a glass rod. (8) Inject the mixture of the flavor and the wax into the tank. Accelerate the speed of the counter-rotating propeller mixer to disperse the wax and oil in the water,
Keep the emulsion homogenous. (9) The second stage pressure of the homogenizer is 6000 ps.
ig and emulsify for 1 minute. 90 ° C product
The steam rate is adjusted to maintain the temperature of. (10) The emulsified wax is solidified by diverting from the three-way valve at the discharge section of the mixer and through a Parker double heat transfer coil to lower the temperature of the slurry to match that of the surroundings.

The products made in Examples 1 to 4 are:
Very pleasant and long lasting fragrance when used in the manufacture of hair care agents as in the examples of the following patents
Create an effect. US Patent 5,653,968 issued August 5, 1997
No. 5, “RISE-OFF HAIR CARE COMPOSITIONS” US Pat. No. 5,653,969 issued Aug. 5, 1997.
No., "LOW RESIDUE HAIRCARE COMPOSITIONS"

Example 3 Use of Shampoo and Conditioner 0.98 grams of the slurry of Example 1 as shown in US Pat. No. 5,658,868 issued Aug. 19, 1997 referred to herein. With 14 grams of the shampoo composition. The configuration is as follows.

5% (by weight) 2-decine sulphate 15% (by weight) Sulfocinnamic acid sodium salt of n-decanolamide 25% (by weight) Lauro amphoteric carboxyglycinate (l)
auroamphocarboxyglycinate) 4% (weight) Coconut amide 3% (weight) Glycol distearate 4% (weight) Aloe vera 1% (weight) Malt oil (wheat germ oil) 43% (weight) Water

The mixture obtained is applied for washing the hair.
Keep your hair dry. After 24 hours, the washed and dried hair has a very pleasant aroma as described below. (1) Persistence on a scale of 1 to 10 9 (2) Quality on a scale of 1 to 10 10 (3) Strength on a scale of 1 to 10

Example 4 Use of a Fabric Softener 2.25 grams of the slurry of Example 2 was mixed with August 1997
Fabric softener composition 2 shown in U.S. Patent No. 5,656,585, issued on May 12, and referred to herein.
Mix with 5 grams.

100 grams of an unscented powdered detergent as set forth in US Pat. No. 5,658,875, issued Aug. 19, 1997, which is incorporated herein by reference, and the fabric softener described above. Apply the mixture to 14 hand towels (cotton fabric, area;
(6 inches x 6 inches, 100 grams each) in a washing machine under the trade name KENMORE.

After washing, the towel is hung for 24 hours and dried.
After 24 hours, the towel so dried has a very pleasant aroma: (1) Persistence on a scale of 1 to 10 9 (2) Quality on a scale of 1 to 10 10 (3) Strength 5 on a scale of 1 to 10

[Brief description of the drawings]

FIG. 1 is an enlarged (2,000 ×) view of a fabric treated with a fabric softener without using the particulate composition of the present invention.

FIG. 2 is a photograph (magnified to 2,000 ×) of a fabric treated with a fabric softener without using the particulate composition of the present invention.

FIG. 3 is a view of an enlarged fabric (2,000 ×) washed with wax fine particles containing a flavoring agent of the present invention.

FIG. 4 is an enlarged photograph (2,000) of a woven fabric (towel) washed with a capsule-like flavoring agent in the wax fine particles of the present invention.
x).

FIG. 5 is an enlarged strand (2,000 ×) of hair that has been washed with shampoo without using the particulate composition of the present invention.

FIG. 6 is an enlarged photograph of a hair strand washed with shampoo without using the fine particle composition of the present invention (2,000).
x).

FIG. 7 is an enlarged strand (2,000 ×) of hair washed with shampoo containing a flavoring agent in capsule form within the wax microparticles of the present invention.

FIG. 8 is an enlarged photograph (2,000 ×) of a hair strand washed with a shampoo and a capsule-like flavoring agent in the wax fine particles of the present invention.

FIG. 9 shows an enlarged strand of hair (2,000) which has been washed with a conditioner without using the particulate composition of the present invention.
It is a figure of x).

FIG. 10 is a photograph (1, 5) of a hair strand washed with a conditioner without using the particulate composition of the present invention.
00x).

FIG. 11 is an enlarged strand (1,500 ×) of hair washed with a conditioner containing wax fine particles of the present invention.
FIG.

FIG. 12 is an enlarged strand (1,500 ×) of hair washed with a conditioner containing the fine wax particles of the present invention.
It is a photograph of.

FIG. 13 is a conceptual diagram of a typical woven fabric obtained by weaving a bundle of interwoven fibers.

FIG. 14 is a conceptual diagram of a typical woven fabric obtained by weaving a bundle of interwoven fibers.

FIG. 15 is a cross-sectional view of an apparatus used to perform an IFF penetration test to determine the penetration of a flavorant through a given polymer in the presence or absence of a surface treatment. .

FIG. 16 is a perspective view of the permeability test apparatus (dispersion cell) of FIG.

FIG. 17 The following structural formulas

Embedded image

Embedded image

4 is a graph showing the permeability of candelilla wax of an aroma compound having the formula, ethyl tiglate, aldehyde C-8 and β-pinene.

FIG. 18 is another graph showing the penetration of carnauba wax into aroma compounds such as ethyl tiglate, aldehyde C-8 and β-pinene.

FIG. 19 is another graph showing the permeability of carnauba wax to aroma compounds such as ethyl tiglate, aldehyde C-8 and pinene, and non-trapped ethyl tiglate and β-pinene as controls.

FIG. 20 is a graph showing the permeability of polyethylene wax (molecular weight 500) into aroma compounds such as ethyl tiglate, aldehyde C-8 and β-pinene, determined by the apparatus of FIGS. 15 and 16;

FIG. 21: Cetyl palmitate (trade name CUTINA)
7 is a graph showing the permeability of β-pinene using wax and a control, such as wax), carnauba wax, polyethylene wax (molecular weight 500), candelilla wax.

FIG. 22: Weight loss of tested product is about 0 to 1
FIG. 22 is an enlarged view of that portion of FIG. 21 as between (mg-mm) / cm ² .

FIG. 23: Cetyl palmitate (trade name CUTINA)
3 is a graph showing the permeability of ethyl tiglate using wax and a control such as wax), carnauba wax, polyethylene wax, and candelilla wax.

FIG. 24 shows the aroma compounds such as β-pinene and ethyl tiglate and the permeability of hydroxypropylcellulose to the control (the release control polymer (control
3 is a graph showing release polymer) or without wax).

FIG. 25 is a graph showing the penetration of polyvinyl alcohol into aroma compounds such as ethyl tiglate and β-pinene, and a graph showing the use of a control without polyvinyl alcohol.

FIG. 26 is a bar graph showing the persistence of geraniol on cotton fabric pieces of geraniol encapsulated within pure geraniol and candelilla wax microparticles.

FIG. 27 is a bar graph showing the geraniol substantivity on geraniol polyester fabric pieces encapsulated with pure geraniol and candelilla wax microparticles.

FIG. 28: Structural formula

GALAX, a mixture of compounds having the formula:
4 is a bar graph showing the substantivity of OLIDE (trademark of IFF, New York, NY).

FIG. 29. Trade name G encapsulated in pure trade name GALAXOLIDE and candelilla wax microparticles
Figure 3 is a bar graph showing the persistence of geraniol on a piece of polyester fabric of ALAXOLIDE.

FIG. 30 is a graph showing that a pure aroma compound, GALAXOLIDE, trade name, and its encapsulated in fine particles of wax are continuously diffused for two or more days.

FIG. 31 Structural formula

3 is a graph showing the radiation of geraniol having the following formula from a particulate slurry applied to brown hair washed with water.

FIG. 32. Flavor S and non-encapsulated flavor 361 for use with encapsulated flavor 361
5 is a graph showing the relationship between the intensity of the odor of the flavoring agent S used together with the elapsed time.

FIG. 33. Fragrance S for use with encapsulated flavor 361 and unencapsulated flavor 3
It is a graph which shows the relationship between the dispersibility of the odor of the mixture of the flavoring agent S used with 61, and elapsed time.

FIG. 34. Flavor S and unencapsulated flavor 885 for use with encapsulated flavor 885
5 is a graph showing the relationship between the intensity of the odor of the flavoring agent S used together with the elapsed time.

FIG. 35. Flavor S for use with encapsulated flavor 885 and unencapsulated flavor 88
5 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S used together with No. 5 and the elapsed time.

FIG. 36 is a graph showing the relationship between the odor intensity of the flavoring agent S of the flavoring agent 075 encapsulated with carnauba wax and the flavoring agent S of the flavoring agent 075 not encapsulated and the elapsed time. is there.

FIG. 37 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S of the flavoring agent 075 encapsulated with carnauba wax and the flavoring agent S of the flavoring agent 075 not encapsulated and the elapsed time It is.

FIG. 38 is a graph showing the relationship between the odor intensity and the elapsed time of the flavoring agent S and the flavoring agent S encapsulated in carnauba wax.

FIG. 39 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S used together with the flavoring agent 361 encapsulated with carnauba wax and the elapsed time.

FIG. 40 is a graph showing the relationship between the odor intensity and the elapsed time of the fragrance S used together with the fragrance S alone and the fragrance 885 encapsulated with carnauba wax.

FIG. 41 is a graph showing the relationship between the odor dispersibility of the flavoring agent S used alone and the flavoring agent S used together with the flavoring agent 885 encapsulated with carnauba wax, and the elapsed time.

FIG. 42. Flavoring agent 0 encapsulated with only flavoring agent S
It is a graph which shows the relationship between the intensity | strength of the odor of the flavoring agent S used together with 75, and elapsed time.

FIG. 43 is a graph showing the relationship between the dispersibility of the odor of the flavoring agent S used together with the flavoring agent 075 encapsulated in carnauba wax and the elapsed time alone.

FIG. 44 is a side sectional view of the fine particles of the present invention.

FIG. 45 is a cross-sectional view of the solid solution-fine particles of the present invention.

FIG. 46 is a cross-sectional view of the particles of the present invention.

FIG. 47 is a schematic view showing a side view of a dispersibility test apparatus for testing the dispersibility of a trapped or untrapped flavoring substance including an aroma compound and a flavoring composition.

FIG. 48 shows the device of FIG. 47 as viewed from above.

FIG. 49 is a perspective perspective view of a first stage during operation of a rotor / stator high shear mixer.

FIG. 50 is a perspective perspective view of a second stage during operation of the rotor / stator high shear mixer used in the method and apparatus of the present invention.

FIG. 51 is a perspective perspective view of a third stage during operation of a rotor / stator high shear mixer useful in practicing the apparatus and method of the present invention.

FIG. 52 is a side view of a homogenizer for performing the mixing step of the method of the present invention and as part of the apparatus of the present invention.

FIG. 53 is a side sectional view of a valve component used in a single-stage homogenization section of the apparatus of the present invention.

FIG. 54 is a side cross-sectional view of a two-stage homogenization valve component used in the homogenization apparatus of the mixing step of the method of the present invention and the apparatus of the present invention.

Figure 55. A rotor / stator useful in performing the mixing step of the apparatus and method of the present invention.
It is a sectional side view of a mixing part.

FIG. 56 is a block flow chart showing the steps of the present invention when producing the particulate composition of the present invention. FIG. 56 is also a schematic diagram of the device of the present invention.

FIG. 57 is a block flow diagram illustrating the steps of the present invention of a method useful in making the compositions of the present invention. Fig. 57
Is also a schematic diagram of the device of the present invention.

FIG. 58 is a schematic diagram of the apparatus and method of FIG. 56, which also includes an overview of effective use of an electronic program controller (eg, a computer system).

FIG. 59 is a schematic diagram in which a device using an electronic program controller (for example, a computer system) is added to the device of FIG. 57;

FIG. 60 is a schematic flowchart showing a method for treating wax fine particles containing an active or physiologically active ingredient of the present invention.

FIG. 61. Flavoring agents of Table 5, Flavoring Agent A-2, Flavoring Agent A-
3 is a graph showing the relationship between the vapor pressure of three different flavoring agents of No. 3, the total flavoring component, and the logarithm.

FIG. 62 is a graph showing normalized weight loss (% by weight) versus time for different groups of three components: low vapor pressure substance, high vapor pressure substance, and mixture of high and low vapor pressure substances.

FIG. 63. Fragrance dispersibility evaluation systems (FIGS. 47 and 48) and prior art thermodynamic (gravim)
3 is a graph showing the weight percent of perfume A-3, which is a high vapor pressure fragrance, versus the weight loss rate (% weight per minute) by both etric) analysis systems.

FIG. 64. Benzyl alcohol, geraniol,

FIG. ₁₀ is a graph showing the relationship between log ₁₀ P and the loading efficiency of aroma compounds of compounds having the structural formulas of farnesol and GALAXOLIDE (registered trademark of IFF).

FIG. 65

Using a composition having the structural formula: 1.2% cetyltrimethylammonium chloride, 10% candelilla wax and 10% flavoring agent P-50448, a rotor / stator mixer 2 shows the size distribution of the fine particles released from the. The graph shows the ratio between the volume percentage and the diameter of the fine particles.

FIG. 66 is a graph showing the relationship between the diameter of the fine particles discharged from the homogenizer mixer and the volume%.

FIG. 67: Relationship of air flow (ml per minute) to elapsed time (minutes) in a system of the invention using two cylinders connected in parallel as shown in detail in FIG. FIG.

[Explanation of symbols]

90 Fine particles 91 Single phase solid solution 92 Surface treatment agent 93 Hydrophilic surface treatment agent 95 Outer surface 900 Fine particles 901 Solid solution 903 Hydrophilic surface treatment agent 904 Charge of fine particles 905 Outer surface 910 Particle 911 Single phase solid solution 912 Surface treatment agent 913, 917 hydrophilic surface treatment agent 915 outer surface 916 outer surface of particles 1001 test sample on blotting paper 1002 container support 1003 containers 1003a, 1003b tandem chamber 1004 opening to atmosphere 1005 air supply unit 1006 tube 1007 pressure measurement for air flow measurement Vessel 1008 temperature monitor 1009 temperature probe 1010 air flow line 1011 container bottom wall 1012 container side wall 1100 rotating stator assembly 1104a solid material 1106 rotation in mixed work head Blade 1110 Second stage valve assembly 1111, 1112 Valve handle 1117 Seal 1120 Mixer 1122 Pressure meter 1123 Gear box 1124 Temperature meter 1130 Cooling coil 1140 Supply tank 1141 Control box 1142 Rotor / stator mixing head 1143, 1272 Cooling coil 1146 Stirrer 1190 Assembly parts 1201, 1204, 1209, 1210, 1250
Containers 1205, 1221, 1230, 1231, 1261,
1252 Heater 1208 Mixing tank 1211, 1212, 1226, 1258, 1267
Control valve 1215, 1260 Mixer 1215, 1260, 1268, 1312 Mixing container 1220 Blender 1224 Cooling coil 1225 Solid phase particle forming device 1251, 1253, 1264, 1309 Container 1256 Control line 1265 Heater 1271 Solid phase particle forming container 1300 1302 Electronic program controller

 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Adi Schaefer United States, New Jersey, Middlesex County, East Brunswick, Jason Drive, 14 (72) Inventor Keith Jay McDermott United States of America, New Jersey, Summer Sett County, Boundbrook, Donner Erod, 1635 (72) Inventor Shmuel David Schaefer United States, New Jersey, Middlesex County, East Brunswick, Jason Drive, 14 (72) Inventor Chetek Tan United States, New Jersey State, Monmouth County, Middletown, Ha Long Road, 91

Claims (8)

[Claims] 1. A fragrance substance selected from the group consisting of (a) at least one aroma compound and at least one perfume composition, and (b) tetra (a) having the following structural formula: 2-hydroxypropyl) ethylenediamine A composition with high fragrance persistence, consisting of a mixture with 2. The composition of claim 1, wherein said composition comprises at least one substantially elliptical hydrophobic particle having a continuous outer surface and a matrix volume therein, said particle substantially having an outer surface having a surface treatment agent. (surfactant) is a solid solution,
Also, the particles consist essentially of (1) a single phase solid solution of a matrix material selected from the group consisting of at least one hydrophobic polymer and at least one hydrophobic wax, wherein each of the polymer and wax comprises
(A) having a melting point ranging from 35 ° C. to 120 ° C. at 1 atm and dissolving at least one hydrophobic fragrance substance, wherein said solid solution has a matrix volume on its outer surface and inside; ) A fragrance substance;
(2) The above tetra (2-hydroxypropyl) ethylenediamine, the outer surface of which is substantially a hydrophilic surface treating agent (surfactant) Wherein the fragrance material is 1 to 8 l
having a calculated og ₁₀ P (where P represents the partition coefficient of the fragrance substance between n-octanol and water), wherein the hydrophobic particles have an outer diameter ranging from 0.05 to 20 microns. Fragrance in the polymer or wax
e) The concentration of the substance ranges from 5% by weight to 60% by weight of the particles.
% By weight, and the weight ratio of the surface treatment agent is from 0.01% by weight to 5% by weight of the weight of the particles, and the wax, the surface treatment agent and the polymer are the fragrance (fr.
2. A high aroma according to claim 1, characterized in that it is a composition for fragrancing at least one perfumable raw material and its closest environment, which do not react with the substances. fragrance)
A persistent composition. 3. The permeation rate of the fragrance substance through a wax or a polymer is determined to be 10 ^-8 (mg-mm) / (cm ² -mi, as measured by an IFF penetration test.
n) to 8 × 10 ⁻³ (mg-mm) / (cm ² −mi)
3. The composition with high fragrance persistence according to claim 2, wherein the composition is in the range of n). 4. The substantially hydrophilic surface treatment agent substantially completely covers the entire outer surface of the single phase solid solution in the form of a continuous submicron thick layer of the surface treatment agent. And
3. High fragrance according to claim 2, characterized in that it is fixedly bonded to the entire outer surface of the single-phase solid solution.
e) Persistent compositions. 5. The substantially hydrophilic surface treatment agent is substantially immediately below the entire outer surface of the solid solution and is disposed substantially within the volume of the inner matrix. 3. A composition having high fragrance persistence according to claim 2. 6. The substantially hydrophilic surface treatment (a) is substantially completely coated over the outer surface of the single phase solid solution in the form of a continuous submicron thick layer of the surface treatment. 3. The fixed matrix of claim 2, wherein (b) is substantially immediately below the entire outer surface of the solid solution and is substantially disposed in the volume of said inner matrix. A composition having a high fragrance persistence. 7. A surface treatment agent having the following structural formula: tetra (2-hydroxypropyl) ethylenediamine And the matrix comprises (a) a polyamide having a molecular weight in the range of 6,000 to 12,000 (b) carnauba wax (c) candelilla wax (d) a mixture of cetyl palmitite and carnauba wax (e A) a mixture of cetyl palmitite and candelilla wax; (f) a ozokerite wax; (g) a ceresin wax; (h) a low density polyethylene wax having a molecular weight in the range of 500 to 6,000. 3. A composition having high fragrance persistence according to claim 2. 8. A fragrance substance selected from the group consisting of at least one aroma compound and at least one perfume composition, and tetra (2-hydroxypropyl) ethylenediamine having the following structural formula: To increase the amount and concentration of fragrance material to increase the persistence of the fragrance substance. Embedded image