Perfume delivery particles

Abstract

Provided are perfume delivery particles for a fiber product. These perfume delivery particles contain a water-soluble solid (A) (hereinafter referred to as component (A)) and a perfume (B) (hereinafter referred to as component (B)). Component (B) is a perfume (B1) contained inside a microcapsule (hereinafter referred to as component (B1)) and a perfume (B2) that is not contained inside a microcapsule (hereinafter referred to as component (B2)). The water content in the perfume delivery particle, as measured using the Karl Fischer vaporization method (JIS K 0113), is 1-35 mass%.

Description

fragrance delivery particles

[0001] BACKGROUND OF THE INVENTION The present invention relates to perfume delivery particles, a method for producing perfume delivery particles, and a method for perfumery of textile products.

[0002] In recent years, research has been conducted into techniques for imparting fragrances having functions such as fragrance, sterilization, disinfection, antibacterial properties, and UV protection to clothing using auxiliary ingredients other than detergent during laundry washing. In particular, attempts have been made to attach fragrance components to clothing by adding a granular composition in which a fragrance is supported on a solid carrier, i.e., fragrance delivery particles, separately from detergent during laundry washing.

[0003] JP 2020-512452 A discloses a technology for granulated powder in which microcapsules containing beneficial substances and fragrances are supported on a solid carrier. JP 1-188597 A discloses a technology for fragrance powder in which anhydrous magnesium sulfate is impregnated with a fragrance emulsion. JP 2021-529869 A discloses a technology for fragrance-containing particles containing polyethylene glycol, a water-soluble filler, and a fragrance component. Summary of the Invention

[0004] When such perfume delivery particles are used in the laundry process, it is necessary for the perfume to remain on textile products even after the process of removing dirt with detergent components during washing and the rinsing process of removing the detergent components. Therefore, a method is desired in which the perfume delivery particles do not dissolve in the presence of detergent components but dissolve during the rinsing stage. While the perfume delivery particles have the problem of remaining undissolved at the end of washing, if the perfume delivery particles dissolve too quickly during the laundry process, the perfume does not remain on the textile products at the end of washing. Therefore, a technology is needed to ensure that the perfume remains sufficiently on the textile products at the end of washing. Furthermore, when microcapsules and perfume components not encapsulated in the microcapsules (hereinafter referred to as external perfumes) are used in combination, the adsorption of the microcapsules to the fibers is reduced, resulting in a significant reduction in the effectiveness of the microcapsules. Therefore, an object of the present invention is to provide perfume delivery particles that have a technology that ensures that the perfume and microcapsules remain sufficiently on the textile products at the end of washing.

[0005] In one embodiment, the present invention provides fragrance delivery particles containing (A) a water-soluble solid (hereinafter, component (A)) and (B) a fragrance (hereinafter, component (B)), wherein component (B) is (B1) a fragrance encapsulated in a microcapsule (hereinafter, component (B1)) and (B2) a fragrance not encapsulated in a microcapsule (hereinafter, component (B2)), and the moisture content of the fragrance delivery particles, as measured by Karl Fischer evaporation method (JIS K 0113), is 1% by mass or more and 35% by mass or less.

[0006] In another embodiment, the present invention provides a method for producing fragrance delivery particles, which comprises mixing (A) a water-soluble solid (hereinafter referred to as component (A)) and (B) a fragrance (hereinafter referred to as component (B)), wherein component (B) is (B1) a fragrance encapsulated in a microcapsule (hereinafter referred to as component (B1)) and (B2) a fragrance not encapsulated in a microcapsule (hereinafter referred to as component (B2)), and the moisture content of the fragrance delivery particles, as measured by Karl Fischer evaporation method (JIS K 0113), is 1% by mass or more and 35% by mass or less.

[0007] According to the present invention, it is possible to provide perfume delivery particles that can retain a large amount of perfume on textile products even after the washing and rinsing processes in the washing process of textile products.Furthermore, it is possible to provide perfume delivery particles that can impart a desirable fragrance quality to textile products.

[0008] [Fragrance delivery particles] The fragrance delivery particles of the present invention contain (A) a water-soluble solid (hereinafter referred to as component (A)) and (B) a fragrance (hereinafter referred to as component (B)), and the moisture content of the fragrance delivery particles measured by the Karl Fischer evaporation method (JIS K 0113) is 1% by mass or more and 35% by mass or less.

[0009] <Component (A)> The water-soluble solid of component (A) may be, for example, one that exhibits a solubility of 1.0 g or more in 100 g of water at 20°C, and preferably one that exhibits a solubility of 1.0 g or more and 60 g or less.

[0010] Component (A) may have pores on its surface, and the average pore diameter is, for example, preferably 1 nm or more, more preferably 10 nm or more, from the viewpoint of further enhancing storage stability and the strength of the fragrance delivery particles, and preferably 1,000 μm or less, more preferably 100 μm or less, from the viewpoint of the strength of the resulting fragrance delivery particles. The average pore diameter of the pores present on the surface of component (A) is measured by mercury intrusion porosimetry using a mercury porosimeter (e.g., Autopore IV9500 (manufactured by Shimadzu Corporation)), and the value of the average pore diameter can be calculated using an Average Pore Diameter (4V / A).

[0011] From the viewpoint of further increasing the strength of the perfume delivery particles, the (A) component may have, for example, a bulk density of preferably 450 g / L or more, more preferably 500 g / L or more, and from the viewpoint of solubility, a bulk density of preferably 750 g / L or less, more preferably 650 g / L or less. The bulk density of the (A) component is calculated using a bulk specific gravity measuring device in accordance with JIS K7365.

[0012] Component (A) may have, for example, an average particle size of preferably 1.0 mm or more, more preferably 3.0 mm or more, and preferably 20 mm or less, more preferably 15 mm or less, even more preferably 10 mm or less, and still more preferably 5 mm or less. The average particle size can be measured by calculating the equivalent spherical diameter of 250 particles using image analysis software ImageJ.

[0013] Examples of component (A) include water-soluble inorganic salts, and are preferably at least one selected from water-soluble inorganic sulfates such as magnesium sulfate and sodium sulfate, water-soluble inorganic chlorides such as sodium chloride and magnesium chloride, and water-soluble inorganic carbonates such as sodium carbonate. From the viewpoint of preventing changes in the quality of the fragrance, component (A) may be, for example, preferably a water-soluble inorganic sulfate, more preferably magnesium sulfate.

[0014] Component (A) can be prepared, for example, by drying a water-soluble solid carrier, preferably a water-soluble inorganic salt having water of crystallization. In one embodiment, component (A) can be prepared by drying a water-soluble solid carrier having a moisture content of more than 20% by mass as measured with an infrared moisture meter, preferably a water-soluble inorganic salt having water of crystallization. Examples of the water-soluble solid carrier, preferably a water-soluble inorganic salt having water of crystallization, include water-soluble inorganic sulfates (preferably water-soluble inorganic sulfates having water of crystallization) such as magnesium sulfate and sodium sulfate, and water-soluble inorganic chlorides (preferably water-soluble inorganic chlorides having water of crystallization) such as sodium chloride and magnesium chloride. From the viewpoint of preventing changes in the quality of the fragrance compound, the water-soluble solid carrier may be, for example, preferably a water-soluble inorganic sulfate, more preferably a water-soluble inorganic sulfate having water of crystallization, and even more preferably magnesium sulfate having water of crystallization.

[0015] In addition, from the viewpoint of further increasing the strength of the fragrance delivery particles and storage stability, component (A) can be, for example, a water-soluble solid having a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter.

[0016] When a water-soluble solid having a moisture content of 0.1% by mass or more and 20% by mass or less as measured with an infrared moisture meter is used as component (A), the moisture content as measured with the infrared moisture meter may be, for example, preferably 1% by mass or more, and from the viewpoint of further increasing the strength of the fragrance delivery particles, more preferably 1.6% by mass or more, even more preferably 2.0% by mass or more, even more preferably 5% by mass or more, and even more preferably 8% by mass or more, and from the viewpoint of storage stability, preferably 20% by mass or less, more preferably 18% by mass or less, and even more preferably 15% by mass or less.

[0017] On the other hand, when a water-soluble solid having a moisture content of 0.1% by mass or more and 20% by mass or less as measured with an infrared moisture meter is used as component (A), the moisture content as measured with the infrared moisture meter may be, for example, from the viewpoint of improving the quality of the fragrance, preferably 1% by mass or more, more preferably 1.6% by mass or more, even more preferably 2.0% by mass or more, still more preferably 5% by mass or more, and still more preferably 8% by mass or more, and from the same viewpoint, preferably 20% by mass or less, more preferably 18% by mass or less, even more preferably 15% by mass or less, and even more preferably 14% by mass or less.

[0018] When a water-soluble solid having a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter is used as component (A), the moisture content of component (A) may be measured, for example, using an infrared moisture meter. For example, it can be measured using an infrared moisture meter (e.g., MOC63u, manufactured by Shimadzu Corporation) at a measurement temperature of 105°C. The moisture calculated here means the moisture content of the water-soluble solid. The moisture content (mass%) of component (A) is calculated based on the following formula by measuring the mass of the water-soluble solid before and after drying using an infrared moisture meter: Moisture content (mass%) = {mass before drying (g) - mass after drying (g)} / mass before drying (g)

[0019] Component (A) can also be prepared, for example, by drying a water-soluble solid. In one embodiment of component (A), a water-soluble solid having a moisture content of more than 20% by mass as measured with an infrared moisture meter may be dried to adjust the moisture content as measured with the infrared moisture meter to a range of 0.1% by mass to 20% by mass.

[0020] From the viewpoint of solubility, the content of component (A) may be, for example, preferably 50% by mass or more, more preferably 70% by mass or more, even more preferably 75% by mass or more, and preferably 99% by mass or less, more preferably 95% by mass or less, even more preferably 93% by mass or less, and even more preferably 90% by mass or less, based on 100% by mass of the fragrance delivery particles of the present invention.

[0021] <Component (B)> The fragrance of component (B) is, for example, (B1) a fragrance encapsulated in a microcapsule [hereinafter referred to as component (B1)] and (B2) a fragrance not encapsulated in a microcapsule [hereinafter referred to as component (B2)].

[0022] The fragrance referred to here is not particularly limited as long as it is one or more selected from fragrances and fragrance precursors. Examples of fragrances that can be used include fragrance compounds described in Nakajima Mototaka's "Fundamentals of Fragrances and Fragrances," 4th edition, Sangyo Tosho Co., Ltd., April 20, 2005, and fragrance compounds known to be incorporated into fabric softeners through patent documents. The fragrance compounds may be a single compound or a mixture of two or more compounds. Furthermore, fragrance components or fragrance compositions prepared independently by fragrance manufacturers may be used as the fragrance compounds. The fragrance may be a single fragrance compound or a fragrance composition containing two or more fragrance compounds, and the fragrance composition may contain a fragrance diluent or solvent in addition to the fragrance compound. Furthermore, fragrance precursors may be used as the fragrance.

[0023] The fragrance compound that can be used in component (B) may have a ClogP of, for example, preferably 1.0 or more, more preferably 1.5 or more, even more preferably 2.0 or more, even more preferably 2.3 or more, even more preferably 2.5 or more, and preferably 30 or less, more preferably 20 or less, even more preferably 10 or less, even more preferably 6.0 or less, even more preferably 5.5 or less, and even more preferably 5.0 or less. A ClogP value within this range ensures good support and retention on component (A). "Supported" here refers to a state in which component (B), preferably component (B1), is attached to the surface of component (A), preferably the outer surface of component (A), or a state in which component (B), preferably component (B2), is attached to the interior of component (A), preferably the inner surfaces of pores connecting the outer surface to the interior of component (A) (also referred to as the interior of pores of component (A)). Furthermore, the term "supporting / retaining ability" used herein means that when the component (B) is supported on the component (A), the encapsulated component of the component (B), preferably the component (B1), or the component (B2) suppresses evaporation or leakage (leakage).

[0024] Here, the log P value is the logarithm of the 1-octanol / water partition coefficient of a compound, and means the ratio of the equilibrium concentrations of the solute in each solvent at partition equilibrium when the compound is dissolved as a solute in a two-phase solvent system of 1-octanol and water, and is generally expressed in the form of logarithm "log P" to the base 10. The log P value can be calculated using a program such as "CLOGP" (Daylight CIS). In the program "CLOGP," the logP value is the "calculated logP (ClogP)" calculated by the method described in "A. Leo in "Comprehensive Medicinal Chemistry," Vol. 4, (C. Hansch, P. G. Sammes, J. B. Taylor and C. A. Ramsden, Eds.), p. 295, Pergamon Press, 1990," and is the ClogP value calculated using the program CLOGP v4.01. When a fragrance contains multiple fragrances, the ClogP value of the fragrance mixture can be determined by multiplying the ClogP value of each fragrance by its volume ratio in the fragrance mixture and calculating the sum of the results.

[0025] From the viewpoint of the ability of component (B2) to be supported and retained by component (A), fragrance compounds that can be used in component (B) preferably have an oil-water interfacial tension of, for example, 7 mN / m or more, more preferably 10 mN / m or more, and even more preferably 13 mN / m or more at 25° C. The oil-water interfacial tension can be measured, for example, using a contact angle meter "DropMaster DM-501" (trade name, manufactured by Kyowa Interface Science Co., Ltd.).

[0026] Examples of fragrance compounds that can be used in component (B) include the following fragrance compounds. Here, the numbers in parentheses are ClogP values: amyl cinnamic aldehyde (4.3), 2-methylundecanal (4.7), ethyl-3-methyl-3-phenyloxirane-2-carboxylate (3.0), allyl amyl glycolate (2.3), allyl caproate (3.2), allyl cyclohexyl propionate (4.5), allyl heptanoate (3.2), ambrettolide (5.4), Ambroxan (registered trademark) (4.8), amyl salicylate (4.6), isoamyl salicylate (4.5), benzyl benzoate (4.0), benzyl salicylate ( 4.3), benzyl acetate (2.0), bougeonal (3.9), o-t-butylcyclohexyl acetate (4.4), p-t-butylcyclohexyl acetate (4.4), Cashmeran (registered trademark) (4.5), cedryl methyl ether (5.0), 1,4-cineole (3.1), 1,8-cineole (3.1), citronellol (3.6), citronellyl acetate (4.6), citronellyl nitrile (3.6), cyclamen aldehyde (3.9), cyclohexyl salicylate (4.9), damascenone (4.2), α-damascena damascone (4.3), β-damascone (4.4), δ-damascone (4.2), decanal (3.8), dihydromyrcenol (3.5), dimethyltetrahydrobenzaldehyde (2.9), diphenyl oxide (4.1), (1-cyclohexyl-2-methylpropan-2-yl) butanoate (4.4), ethylene brassylate (4.7), ethylene dodecanedioate (4.2), ethyl-2-methylbutyrate (2.3), ethyl vanillin (1.6), eugenol (2.7), Flute (registered trademark) ( 3.6), geraniol (3.5), geranyl acetate (4.5), geranyl nitrile (3.9), hexyl cinnamic aldehyde (4.8), hexyl acetate (4.8), hexyl salicylate (5.1), salicylic acid cis-3-hexenyl (4.8), iso E super (5.2), α-ionone (3.9), β-ionone (4.4), propan-2-yl-2-methylbutanoate (2.7), Javanol (registered trademark) (4.7), Lilial (registered trademark) (4.4), limonene (4.9), linalool (3.3),Linalyl acetate (4.4), Lyral (registered trademark) (3.3), manzanate (2.8), methyl dihydrojasmonate (3.0), methyl anthranilate (2.3), methyl β-naphthyl ketone (2.9), γ-methyl ionone (4.8), methyl salicylate (2.6), 11-oxa-16 hexadecanolide (4.9), nectaryl (5.1), nerol (3.7), nerol (3.3), γ-nonalactone (2.1), nonanal (3.3), octanal (2.8), phenylhexanol (3.5), propanediol and one or more fragrance compounds selected from the group consisting of benzoyl-2-yl-2-methylbutanoate (2.7), Sandalmysole Core (registered trademark) (4.7), terpineol (3.3), terpinyl acetate (4.3), tetrahydrolinalool (3.6), tricyclodecenyl acetate (2.9), tricyclodecenyl propionate (3.3), γ-undecalactone (3.1), florosa (2), isoamyl acetate (2.3), stearyl acetate (2.5), triplal (2.9), and Dynascon (registered trademark) (4.5).

[0027] Examples of fragrance precursors that can be used as component (B) include compounds that release fragrance components in response to water, compounds that release fragrance components in response to light, etc. Examples of compounds that release fragrance components in response to water include silicate ester compounds having an alkoxy component derived from a fragrance alcohol, fatty acid ester compounds having an alkoxy component derived from a fragrance alcohol, acetal compounds or hemiacetal compounds obtained by reacting a carbonyl component derived from a fragrance aldehyde or fragrance ketone with an alcohol compound, Schiff base compounds obtained by reacting a carbonyl component derived from a fragrance aldehyde or fragrance ketone with a primary amine compound, and hemiaminal compounds or hydrazone compounds obtained by reacting a carbonyl component derived from a fragrance aldehyde or fragrance ketone with a hydrazine compound. Examples of compounds that release a fragrance component in response to light include 2-nitrobenzyl ether compounds having an alkoxy component derived from a fragrance alcohol, α-ketoester compounds having a carbonyl component derived from a fragrance aldehyde or fragrance ketone, coumaric acid ester compounds having an alkoxy component derived from a fragrance alcohol, etc. These fragrance precursors may be used as polymers, such as reaction products of some carboxy groups of polyacrylic acid with a fragrance alcohol.

[0028] The component (B1) is not particularly limited as long as it is a microcapsule in which a fragrance is encapsulated in a shell (hereinafter also referred to as a fragrance-encapsulated microcapsule, fragrance microcapsule, or microencapsulated fragrance), and the encapsulated fragrance may be one or more selected from the fragrance compounds described above, or may be a fragrance composition containing two or more. The component (B1) is adsorbed to a textile product, and after drying, application of a stimulus such as rubbing causes the capsules to break down, releasing the fragrance. Therefore, by incorporating the component (B1) in the present invention, the fragrance persistence of the textile product can be improved.

[0029] The method for preparing perfume microcapsules is not particularly limited, and known microencapsulation methods can be used. Specific examples include chemical production methods (interfacial polymerization, in situ polymerization, orifice method), physicochemical methods (coacervation), and mechanical / physical methods (air suspension coating, spray drying, high-velocity air current impact method). Examples of the outer shell of perfume microcapsules include various polymeric compounds such as polyurethane, polyamide, melamine resin, urea resin, alginate, gelatin, gum arabic, and starch, as well as inorganic compounds such as silica.

[0030] More specifically, methods for producing fragrance microcapsules can be employed, such as those described in "Making and Using Microcapsules" (Koishi Masumi et al., Industrial Research Institute, published in 2005), JP 2008-63575 A, JP 2006-249326 A, JP 2006-518790 A, JP 11-216354 A, and JP 5-222672 A. A preferred method for producing fragrance microcapsules involves dispersing an emulsifier such as ethylene-maleic anhydride copolymer, a fragrance, and an optional diluent or solvent in water to obtain an emulsion, and then adding a wall material such as melamine-formaldehyde resin to the emulsion and stirring the mixture to obtain a slurry of fragrance microcapsules. Another example is a method in which a monomer that will become the resin that will form the wall material and an emulsifier such as isobutylene-maleic anhydride copolymer or acrylic acid-acrylamide copolymer are mixed in water in advance to prepare a wall material / emulsifier mixture, and then this wall material / emulsifier mixture is emulsified with a fragrance and an optional diluent or solvent, and formaldehyde is added to the emulsion and stirred to obtain a slurry of fragrance microcapsules.

[0031] The content of the fragrance compound in 100% by mass of a slurry containing fragrance microcapsules obtained by the above-described method for producing fragrance microcapsules may be, for example, preferably 15% by mass or more, more preferably 18% by mass or more, even more preferably 20% by mass or more, and preferably 60% by mass or less, more preferably 50% by mass or less, even more preferably 40% by mass or less. These contents may be based on the amounts blended when the fragrance-encapsulating microcapsules are prepared.

[0032] In 100% by mass of the slurry containing component (B1), the content of the perfume-encapsulated microcapsules may be, for example, preferably 5.0% by mass or more, more preferably 10.0% by mass or more, even more preferably 15% by mass or more, and even more preferably 20% by mass or more, from the viewpoint of the stability of component (B1), and preferably 70% by mass or less, more preferably 60% by mass or less, and even more preferably 50% by mass or less, from the viewpoint of improving the strength of the perfume-delivery particle of the present invention. These contents may be based on the amount of perfume-encapsulated microcapsules blended when prepared.

[0033] The water content in 100% by mass of the slurry containing component (B1) may be, for example, preferably 30% by mass or more, more preferably 40% by mass or more, and preferably 85% by mass or less, more preferably 80% by mass or less, and even more preferably 60% by mass or less. The water content of the fragrance delivery particles of the present invention, as measured by the Karl Fischer evaporation method (JIS K 0113), can also be adjusted, for example, by the amount of the slurry of fragrance microcapsules containing component (B1).

[0034] Furthermore, it is also possible to use capsules in which a fragrance is encapsulated in a silica shell formed by a sol-gel reaction using an alkoxysilane as a shell precursor, as described in JP-A-2023-8936.It is also possible to use capsules in which a fragrance is encapsulated in a shell obtained from a water-soluble monomer or a crosslinkable monomer having two or more (meth)acryloyl groups, as described in JP-A-2016-534159.

[0035] From the viewpoint of the fragrance intensity of the textile product after treatment and further the fragrance intensity when the textile product after drying is subjected to stimulation such as rubbing, the average particle size of component (B1) may be, for example, preferably 0.1 μm or more, more preferably 1 μm or more, and preferably 50 μm or less, more preferably 40 μm or less. The average particle size (median size) of component (B1) can be measured, for example, using a laser diffraction / scattering particle size distribution analyzer "LA-950" (manufactured by HORIBA, Ltd.).

[0036] Component (B2) is, for example, a fragrance not incorporated into the microcapsules (also referred to as an external fragrance), and may be one or more fragrance compounds selected from the fragrance compounds described above, or may be a fragrance composition containing two or more fragrance compounds. It may also be the same fragrance compound as the fragrance compound encapsulated in the fragrance-encapsulating microcapsules that are component (B1).

[0037] The content of the (B1) component, based on 100% by mass of the fragrance delivery particle of the present invention, may be, for example, preferably 0.05% by mass or more, more preferably 0.1% by mass or more, even more preferably 0.2% by mass or more, even more preferably 0.3% by mass or more, even more preferably 0.4% by mass or more, and preferably 6.5% by mass or less, more preferably 6.0% by mass or less, even more preferably 5.5% by mass or less, even more preferably 5.0% by mass or less, and even more preferably 4.5% by mass or less. The content of the fragrance compound encapsulated as an effective amount (which may be the amount of the fragrance compound blended when preparing the (B1) component) may be considered to be the content of the (B1) component. For example, it may be based on the amount of a slurry containing the (B1) component blended when producing the fragrance delivery particle of the present invention.

[0038] The content of component (B2) may be, for example, preferably 1.0% by mass or more, more preferably 2.0% by mass or more, even more preferably 3.0% by mass or more, and even more preferably 5.0% by mass or more, and preferably 10.0% by mass or less, more preferably 9.0% by mass or less, based on 100% by mass of the perfume delivery particles of the present invention. These contents may be based on the amount blended when producing the perfume delivery particles of the present invention.

[0039] The mass ratio of the content of the (B1) component to the content of the (B2) component [(B1) / (B2)] may be, for example, preferably 0.005 or more, more preferably 0.01 or more, and even more preferably 0.1 or more from the viewpoint of improving the quality of the fragrance, and preferably 5.0 or less, more preferably 3.0 or less, even more preferably 2.5 or less, and even more preferably 2.0 or less, even more preferably 0.7 or less, and even more preferably 0.6 or less from the viewpoint of improving the quality of the fragrance. The content of the (B1) component may be regarded as the content of the fragrance compound encapsulated as an effective amount (which may be the amount of the fragrance compound blended when preparing the (B1) component). For example, it may be based on the amount of a slurry containing the (B1) component blended when producing the fragrance delivery particle of the present invention. Furthermore, the content of the (B2) component may be based on the amount blended when producing the fragrance delivery particle of the present invention.

[0040] The component (B) may contain an organic solvent, and the content of the organic solvent is, for example, preferably 0.5% by mass or more, more preferably 1% by mass or more, relative to 100% by mass of the component (B), from the viewpoints of promoting the support and retention of the component (B2) inside the pores of the component (A) and of stability (such as suppressing the volatilization and exudation of the fragrance (component (B2)) supported and retained on the component (A) during particle storage). From the viewpoint of the intensity of the fragrance, the content of the organic solvent may be, for example, preferably 30% by mass or less, more preferably 25% by mass or less. The organic solvent in the present invention may be, for example, one or more organic compounds that are liquid at 20° C., other than fragrance compounds, selected from alcohols and glycols having from 1 to 10 carbon atoms, esters having from 6 to 20 carbon atoms, and paraffins. Specific examples of alcohols include methanol, ethanol, and glycerin; glycols include ethylene glycol, diethylene glycol monoethyl ether, propylene glycol, dipropylene glycol, dipropylene glycol monoethyl ether, and 3-methoxy-3-methylbutanol; esters include diethyl phthalate, isopropyl myristate, benzyl myristate, triethyl citrate, diisobutyl adipate, and hydrogenated methyl abietate; and paraffins include liquid paraffin and isoparaffin.

[0041] In the fragrance delivery particles of the present invention, from the viewpoint of aroma release by friction, the mass ratio of the content of the (A) component to the content of the (B1) component [(B1) / (A)] may be, for example, preferably 0.0001 or more, more preferably 0.0003 or more, even more preferably 0.0005 or more, and from the viewpoint of improving the quality of the fragrance, preferably 0.20 or less, more preferably 0.15 or less, even more preferably 0.10 or less. Here, aroma release by friction refers to the aroma released after rubbing a dry cloth. The content of the (B1) component may be considered to be the content of the fragrance compound encapsulated as an effective amount (which may be the amount of the fragrance compound blended when preparing the (B1) component). For example, it may be based on the amount of a slurry containing the (B1) component blended when producing the fragrance delivery particles of the present invention. Furthermore, the content of the (B2) component may be based on the amount blended when producing the fragrance delivery particles of the present invention.

[0042] In the fragrance delivery particles of the present invention, from the viewpoint of further increasing the strength of the fragrance delivery particles and from the viewpoint of fragrance intensity immediately after dehydration, the mass ratio of the content of component (A) to the content of component (B2) [(B2) / (A)] is, for example, preferably 0.01 or more, more preferably 0.015 or more, even more preferably 0.03 or more, and even more preferably 0.05 or more, and from the viewpoint of improving the quality of the fragrance, it may be preferably 0.20 or less, more preferably 0.15 or less, even more preferably 0.12 or less, and even more preferably 0.10 or less. The above contents may be based on the amounts blended when producing the fragrance delivery particles of the present invention.

[0043] In addition, in the production of the fragrance delivery particles of the present invention, a slurry containing component (B1) may be blended into the fragrance delivery particles of the present invention in an amount of, for example, preferably 0.3% by mass or more, more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and preferably 5.0% by mass or less, more preferably 4.0% by mass or less, as a solid form.

[0044] The fragrance delivery particles of the present invention have a moisture content measured by Karl Fischer evaporation method (JIS K 0113) (hereinafter referred to as KF moisture content) of 1% by mass or more, and from the viewpoint of the strength of the resulting fragrance delivery particles, for example, preferably 3% by mass or more, more preferably 5% by mass or more, even more preferably 8% by mass or more, even more preferably 10% by mass or more, and even more preferably 20% by mass or more, and 35% by mass or less, and from the viewpoint of improving the quality of the fragrance, preferably 32% by mass or less. The moisture content of the fragrance delivery particles of the present invention measured by Karl Fischer evaporation method (JIS K 0113) can be measured by the method described in the Examples.

[0045] Although the mechanism of action of the present invention is unclear, the present inventors speculate as follows. The present inventors discovered that when components (B1) and (B2) are stored in contact with each other, the perfume-encapsulating microcapsules of component (B1) break down. Therefore, when a mixture of components (B1) and (B2) obtained by a conventional method is supported on a water-soluble solid (component (A)), the capsules collapse and do not adhere to clothing after washing and rinsing, resulting in the loss of capsule efficacy. Component (B2), which is supported and retained even within the pores of component (A), exists within component (A). On the other hand, component (B1) does not easily enter the pores of component (A). Furthermore, by premixing component (D) and component (B1), component (B1) is supported and retained near the surface of component (A), improving the stability of component (B1). If the KF moisture content of the perfume delivery particles is low, the strength of the perfume delivery particles decreases and storage stability is impaired, whereas if the KF moisture content is high, the perfume carried and held in component (B2) seeps out onto the surface of component (A), causing the capsules (shape of component (B1)) to collapse. It is believed that by adjusting the moisture content to the specific level of the present invention, the strength of the delivery particles, the strength of the capsules, and the efficiency of adsorption to textile products can be optimized.

[0046] The perfume delivery particles of the present invention are not particularly limited, but may preferably be spherical, granular or powdery, with spherical particles being preferred from the standpoint of appearance and ease of use.

[0047] From the viewpoint of solubility and handleability, the perfume delivery particles of the present invention may have an average particle size of, for example, preferably 1.0 mm or more, more preferably 1.5 mm or more, even more preferably 2.0 mm or more, and preferably 20 mm or less, more preferably 10 mm or less, even more preferably 5 mm or less. The average particle size can be measured, for example, by calculating the equivalent spherical diameter of 250 particles using image analysis software ImageJ.

[0048] From the viewpoint of more easily achieving the effects of the present invention due to the differences in the specific requirements of the present invention, the perfume delivery particles of the present invention may have an average particle size of, for example, preferably 1.0 mm or more, more preferably 1.5 mm or more, even more preferably 2.0 mm or more, and preferably 20 mm or less, more preferably 10 mm or less, even more preferably 5 mm or less. The average particle size can be measured, for example, by calculating the equivalent spherical diameter of 250 particles using image analysis software ImageJ.

[0049] The perfume delivery particles of the present invention may have, for example, a bulk density of preferably 400 g / L or more, more preferably 500 g / L or more, from the viewpoint of volume during use, and a bulk density of preferably 1000 g / L or less, more preferably 800 g / L or less, from the viewpoint of ease of use and solubility during use. The bulk density can be measured, for example, using a bulk specific gravity measuring device in accordance with JIS K7365.

[0050] In one embodiment, the perfume delivery particles of the present invention are preferably those in which the water-soluble solid of component (A), preferably a water-soluble inorganic salt, supports or retains component (B).

[0051] <Component (C)> In order to promote the adsorption of component (B1) onto textile products, the fragrance delivery particles of the present invention may further contain, for example, (C) one or more selected from water-soluble cationic polymeric compounds and cationic surfactants [hereinafter referred to as component (C)].

[0052] Specific examples of the water-soluble cationic polymer compound include polydiallyldimethylammonium chloride such as poly(diallyldimethylammonium chloride), poly(acrylic acid-co-diallyldimethylammonium chloride), poly(acrylamide-co-diallyldimethylammonium chloride), and poly(acrylamide-co-acrylic acid-co-diallyldimethylammonium chloride), and copolymers thereof; poly(2-(methacryloyloxy)ethyltrimethylammonium chloride), polyethyleneimine, polyallylamine, cationized cellulose, cationized guar gum, cationized tara gum, cationized fenugreek gum, and cationized locust bean gum. Among these, preferably, one or more selected from polydiallyldimethylammonium chloride and its copolymers poly(diallyldimethylammonium chloride), poly(acrylic acid-co-diallyldimethylammonium chloride), and poly(acrylamide-co-acrylic acid-co-diallyldimethylammonium chloride), and more preferably, one or more selected from poly(acrylamide-co-diallyldimethylammonium chloride) and poly(diallyldimethylammonium chloride).

[0053] Examples of cationic surfactants include alkylamine salts and alkyl quaternary ammonium salts.

[0054] The alkylamine salt may be, for example, preferably a salt of a secondary amine or a tertiary amine, and more preferably a salt of a tertiary amine. The alkylamine salt is, for example, a compound having at least one long-chain alkyl group, and optionally, preferably, at least one group selected from a long-chain alkyl group, a short-chain alkyl group, and a benzyl group. The carbon number of the long-chain alkyl group is, for example, preferably 10 or more, more preferably 12 or more, even more preferably 14 or more, and preferably 22 or less, more preferably 20 or less, and even more preferably 18 or less. The carbon number of the short-chain alkyl group is, for example, preferably 1 or more and preferably 4 or less, more preferably 1 or 2, and even more preferably 1, i.e., a methyl group. Examples of alkylamine salts include alkylamine salts in which the long-chain alkyl group has the above carbon number range, such as long-chain monoalkyl monomethyl secondary amine salts and long-chain monoalkyl dimethyl tertiary amine salts. Examples of long-chain monoalkyl dimethyl tertiary amine salts include alkylamine acetates such as lauryl dimethylamine acetate and stearyl dimethylamine acetate.

[0055] The alkyl quaternary ammonium salt is, for example, a compound having at least one long-chain alkyl group, and optionally, preferably, at least one group selected from a long-chain alkyl group, a short-chain alkyl group, and a benzyl group. The carbon number of the long-chain alkyl group is, for example, preferably 10 or more, more preferably 12 or more, even more preferably 14 or more, and preferably 22 or less, more preferably 20 or less, and even more preferably 18 or less. The carbon number of the short-chain alkyl group is, for example, preferably 1 or more and preferably 4 or less, more preferably 1 or 2, and even more preferably 1, i.e., a methyl group. Examples of alkyl quaternary ammonium salts include long-chain alkyl tri-short-chain alkyl quaternary ammonium salts, di-long-chain alkyl di-short-chain alkyl quaternary ammonium salts, and long-chain alkyl benzyl di-short-chain alkyl quaternary ammonium salts, in which the long-chain alkyl group and the short-chain alkyl group each have the carbon number within the above-mentioned ranges. Examples of long-chain alkyl tri-short-chain alkyl quaternary ammonium salts include alkyl trimethyl ammonium chlorides such as lauryl trimethyl ammonium chloride, cetyl trimethyl ammonium chloride, and stearyl trimethyl ammonium chloride; and alkyl trimethyl ammonium bromides such as lauryl trimethyl ammonium bromide, cetyl trimethyl ammonium bromide, and stearyl trimethyl ammonium bromide. Examples of di-long-chain di-short-chain alkyl quaternary ammonium salts include di-alkyl dimethyl ammonium chlorides such as distearyl dimethyl ammonium chloride; and di-alkyl dimethyl ammonium bromides such as distearyl dimethyl ammonium bromide. Examples of long-chain alkyl benzyl di-short-chain alkyl quaternary ammonium salts include alkyl benzyl dimethyl ammonium chloride and alkyl benzyl dimethyl ammonium bromide.

[0056] Among these, the cationic surfactant is, for example, preferably an alkyl quaternary ammonium salt, more preferably an alkyltrimethylammonium salt having an alkyl group with from 10 to 22 carbon atoms, even more preferably an alkyltrimethylammonium chloride having an alkyl group with from 10 to 22 carbon atoms, even more preferably one or more selected from lauryltrimethylammonium chloride, stearyltrimethylammonium chloride, and cetyltrimethylammonium chloride, and even more preferably cetyltrimethylammonium chloride.

[0057] When the perfume delivery particles of the present invention contain a water-soluble cationic polymeric compound, the content of the water-soluble cationic polymeric compound may be, for example, preferably 0.01% by mass or more, more preferably 0.03% by mass or more, even more preferably 0.05% by mass or more, and preferably 2.0% by mass or less, more preferably 1.0% by mass or less, based on 100% by mass of the perfume delivery particles of the present invention, from the viewpoint of promoting adsorption of component (B1) to textile products. These contents may be based on the amounts blended when producing the perfume delivery particles of the present invention. Furthermore, the above contents do not include the cationic surfactant of the present invention.

[0058] When the perfume delivery particles of the present invention contain a cationic surfactant, the content of the cationic surfactant in the present invention may be, for example, preferably 0.01% by mass or more, more preferably 0.05% by mass or more, and preferably 2.0% by mass or less, more preferably 1.0% by mass or less, based on 100% by mass of the perfume delivery particles of the present invention, from the viewpoint of promoting the adsorption of component (B1) to textile products. The content may be based on the amount blended when producing the perfume delivery particles of the present invention. The mass of the cationic surfactant is used as a value converted to a chloride salt.

[0059] <Component (D)> The fragrance delivery particle of the present invention may further contain, for example, a water-soluble nonionic polymer (D) [hereinafter referred to as component (D)] from the viewpoint of the strength, solubility, and stability of the resulting fragrance delivery particle (such as suppressing the evaporation and exudation of the fragrance (component (B2)) supported and held by component (A) during particle storage). Component (D) may be, for example, preferably polyethylene glycol (PEG), polypropylene glycol, polyoxyethylene alkyl ether, or polyoxyethylene phenol ether, more preferably polyethylene glycol or polypropylene glycol. Furthermore, from the viewpoint of the strength, solubility, and stability of the resulting fragrance delivery particles (such as suppression of volatilization and exudation of the fragrance (component (B2)) supported and held by component (A) during particle storage), the number average molecular weight of component (D) may be, for example, preferably 2,000 or more, more preferably 3,000 or more, even more preferably 4,000 or more, and preferably 20,000 or less, more preferably 15,000 or less, and even more preferably 10,000 or less, as measured by GPC using polystyrene as the standard. When measuring the molecular weight of polyethylene glycol, water / ethanol is used as the solvent.

[0060] When the fragrance delivery particles of the present invention contain component (D), the content of component (D) is, for example, preferably 0.5% by mass or more, more preferably 1% by mass or more, based on 100% by mass of the fragrance delivery particles, from the viewpoint of the strength, solubility, and stability of the resulting fragrance delivery particles (such as suppressing the evaporation and seepage of the fragrance (component (B2)) supported and held by component (A) during particle storage), and from the viewpoint of improving the solubility and fragrance quality of the fragrance delivery particles of the present invention, preferably 30% by mass or less, more preferably 25% by mass or less, and even more preferably 20% by mass or less. The content may be based on the amount blended when producing the fragrance delivery particles of the present invention.

[0061] When the fragrance delivery particle of the present invention contains component (D), the mass ratio of the content of component (A) to the content of component (D), [(A) / (D)], is, from the viewpoint of solubility, preferably 0.1 or more, more preferably 0.2 or more, even more preferably 0.3 or more, even more preferably 0.5 or more, even more preferably 1.0 or more, even more preferably 5.0 or more, and even more preferably 7.0 or more, and from the viewpoint of product stability (such as suppression of volatilization and exudation of the fragrance (component (B2)) supported and held by component (A) during particle storage), it may be preferably 100 or less, more preferably 95 or less, even more preferably 50 or less, even more preferably 30 or less, even more preferably 25 or less, and even more preferably 20 or less. The above contents may be based on the amounts blended when producing the fragrance delivery particle of the present invention.

[0062] <Component (E)> The perfume delivery particle of the present invention may further contain, for example, (E) an oxidation stabilizer [hereinafter referred to as component (E)]. Examples of the oxidation stabilizer that can be used include antioxidants such as butylhydroxytoluene (BHT), butylhydroxyanisole (BHA), distyrenated cresol, sodium sulfite, and sodium hydrogen sulfite.

[0063] When the perfume delivery particle of the present invention contains component (E), the content of component (E) may be, for example, preferably 0.01% by mass or more, more preferably 0.02% by mass or more, and preferably 0.50% by mass or less, more preferably 0.30% by mass or less, based on 100% by mass of the perfume delivery particle of the present invention. The content may be based on the amount blended when producing the perfume delivery particle of the present invention.

[0064] The fragrance delivery particles of the present invention may optionally contain the above-mentioned components (C), (D), and (E), and may further contain, for example, an organic solvent from the viewpoint of promoting the loading and retention of component (B2) inside the pores of component (A) and from the viewpoint of stability (such as suppressing the evaporation and exudation of the fragrance (component (B2)) loaded and retained in component (A) during particle storage). When the fragrance delivery particles of the present invention contain an organic solvent, it may be the same as the organic solvent optionally contained in component (B). For example, the organic solvent may be preferably 0.02% by mass or more, more preferably 0.05% by mass or more, and preferably 3.0% by mass or less, more preferably 2.5% by mass or less, and even more preferably 1.5% by mass or less, based on 100% by mass of the fragrance delivery particles of the present invention. The above range may include the organic solvent optionally contained in component (B).

[0065] [Method for producing fragrance delivery particles] The fragrance delivery particles of the present invention can be obtained, for example, by mixing component (A) and component (B). That is, the present invention provides a method for producing fragrance delivery particles by mixing component (A), component (B1), and component (B2). Specific examples and preferred examples of component (A) and component (B) may be the same as those of the fragrance delivery particles of the present invention described above. From the perspective of adjusting the moisture content of the fragrance delivery particles of the present invention, for example, component (A) can be one that has been dried in advance and has a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter. Alternatively, a water-soluble solid with a moisture content of more than 20% by mass as measured by an infrared moisture meter can be dried and the moisture content as measured by the infrared moisture meter can be adjusted to a range of 0.1% by mass or more and 20% by mass or less.

[0066] The moisture content of the water-soluble solid can be adjusted by drying component (A) using, for example, an electric dryer (shelf drying), fluidized bed drying, reduced pressure drying, microwave drying, etc. From the viewpoint of suppressing disintegration of the water-soluble solid during drying, for example, a drying method that applies as little strong shear force as possible is preferred, and from the viewpoint of equipment, for example, shelf drying, fluidized bed drying, and reduced pressure drying are preferred.

[0067] The drying treatment may be either a batch type or a continuous type, and is not particularly limited. For example, batch types include drying methods using an electric shelf dryer or a hot air dryer, and drying methods using a batch type fluidized bed, and continuous types include fluidized beds, vibration fluidized beds, rotary dryers, steam tube dryers, etc.

[0068] The drying conditions are not particularly limited as long as the moisture content of the water-soluble solid as measured by an infrared moisture meter can be adjusted to a range of, for example, preferably 0.1 mass % or more and preferably 20 mass % or less. For example, the drying conditions can be adjusted by combining the following drying temperatures and drying times.

[0069] The drying temperature can be appropriately determined taking into consideration the drying rate, and may be, for example, preferably 60° C. or higher, more preferably 80° C. or higher, and even more preferably 100° C. or higher. In addition, from the viewpoint of heat load and adhesion of water-soluble solids, the upper limit may be preferably 200° C. or lower, more preferably 180° C. or lower, even more preferably 150° C. or lower, and still more preferably 130° C. or lower.

[0070] The drying time varies depending on the moisture content and amount of the water-soluble solid used in the production, but in the case of batch operation using a fluidized bed dryer, it may be, for example, preferably 5 minutes or more, more preferably 15 minutes or more, and preferably 1 hour or less, more preferably 40 minutes or less. In the case of electrical drying, it may be, for example, preferably 10 minutes or more, more preferably 30 minutes or more, and preferably 4 hours or less, more preferably 2 hours or less.

[0071] Alternatively, the water-soluble solid may be compression-molded in advance into granules, flakes, or beads, and then dried. The molding method can be a known method. For example, the method can be compression molding, extrusion granulation, tumbling granulation, stirring granulation, or compaction granulation. Among these, compression molding is preferred.

[0072] When compressing a water-soluble solid, the manufacturing machine used is not limited as long as it can produce, for example, briquettes or tablets, and well-known briquetting machines, tablet presses, etc. can be used. A briquetting machine is a device in which two rolls, each having a pocket engraved on its periphery that serves as a matrix for the desired compressed product, are engaged with each other and rotate at the same speed, feeding granulated material between the rolls and continuously compressing it. Well-known briquetting machines include, for example, a briquetting machine (manufactured by Shinto Kogyo Co., Ltd.). A tablet press is a device in which granulated material is filled into a die and compressed between a lower punch and an upper punch to form the granulated material. Tableting machines include single-shot tablet presses in which a pair of upper and lower punches move up and down within a single die to compress the material, and rotary tablet presses in which die sets are embedded at equal intervals around the periphery of a horizontally rotating turntable, and a series of operations of filling, compression, and discharge are continuously performed while the turntable rotates. As well-known tablet presses, for example, a single punch tablet press manufactured by Riken Co., Ltd. and a rotary tablet press manufactured by Kikusui Chemical Co., Ltd. can be used.

[0073] When molding by a method other than compression molding, for example, well-known extrusion granulators such as Pelleter Double, Dome Gran, Twin Dome Gran, Disk Pelleter (manufactured by Dalton Co., Ltd.), basket-type granulator (manufactured by Kikusui Seisakusho Co., Ltd.), as well as rolling granulators, etc. can be used. Furthermore, after molding, sizing can be performed as necessary. As the machine used for sizing, well-known pulverizers (or crushers) can be used, for example, Marumerizer (manufactured by Dalton Co., Ltd.), Fitz Mill (manufactured by Dalton Co., Ltd.), Power Mill (manufactured by Powrex Corporation), Comill (manufactured by Quadro), etc. can be used.

[0074] In one embodiment, the fragrance delivery particles of the present invention can be produced by mixing a mixture obtained by mixing component (A) and component (B2) with component (B1). In another embodiment, the fragrance delivery particles of the present invention can be produced by mixing a mixture obtained by mixing component (A) and component (B2) with a mixture of component (B1) and component (D). By premixing component (A) and component (B2) so that component (B2) is supported and held within component (A), and then mixing a mixture of component (B1) and component (D) into the mixture of component (A) and component (B2), the mixture of component (B1) and component (D) can be supported and held on the surface of component (A), thereby improving the stability of the fragrance delivery particles supporting and holding component (B1).

[0075] In another embodiment, the fragrance delivery particles of the present invention can be produced by mixing a mixture obtained by mixing component (A) and component (B1) with component (B2). In another embodiment, the fragrance delivery particles of the present invention can be produced by mixing a mixture obtained by mixing component (A) and component (B1) with a mixture obtained by mixing component (B2) and component (D). By mixing the mixture obtained by mixing component (B2) and component (D) with a mixture of component (A) and component (B1), the mixture of component (B2) and component (D) can be supported and retained on the surface of component (A), thereby improving the stability of the fragrance delivery particles supporting and retaining component (B2). As the mixture obtained by mixing component (A) and component (B1), a mixture obtained by mixing component (A) with a slurry containing component (B1) can also be used.

[0076] In another embodiment, the perfume delivery particles of the present invention can be produced by dividing component (A) into portions and mixing them in stages. Specifically, the method includes the following steps (i) to (iii).

[0077] Step (i): mixing a portion of the (A) component with the (B2) component to obtain a mixture; Step (ii): mixing the mixture obtained in step (i) with the remaining (A) component; Step (iii): mixing the mixture obtained in step (ii) with the (B1) component to produce perfume delivery particles.

[0078] When the (A) component is mixed stepwise in this manner, in addition to the perfume delivery particles of the present invention containing the (A), (B1) and (B2) components, perfume-containing particles containing the (A) component and the (B1) component (but not the (B2) component) may be obtained in any ratio. The perfume delivery particles of the present invention may be used in combination with perfume-containing particles containing the (A) component and the (B1) component, depending on the situation.

[0079] When the fragrance delivery particles of the present invention are produced by mixing the (A) component in stages, the content of the fragrance delivery particles of the present invention (i.e., fragrance delivery particles containing the (A) component, the (B1) component, and the (B2) component) in 100% by mass of the total particles obtained may, from the viewpoint of storage stability, be, for example, preferably 25% by mass or more, more preferably 35% by mass or more, and preferably 75% by mass or less, more preferably 65% ​​by mass or less, and the fragrance-containing particles containing the (A) component and the (B1) component may be the remaining component.

[0080] When the perfume delivery particles of the present invention are produced by mixing the (A) component step by step, the mixed liquid added in step (iii) is considered to be uniformly distributed among a portion of the (A) component in step (i), the mixture of the (B2) component and the optional (E) component, and the remaining portion of the (A) component in step (ii). Therefore, the content of perfume delivery particles in the resulting mixed particles can be calculated by calculating the ratio of the amount (active component) of step (i) to the total amount of the amount (active component) of step (i) and the amount (active component) of step (ii), and multiplying this ratio by the amount (active component) of the mixed liquid added in step (iii).

[0081] When the fragrance delivery particles of the present invention are produced by mixing the (A) component in stages, in step (i), the mass ratio of a portion of the (A) component to the (B2) component to be mixed [(B2) component / (A) component (1)] may be, for example, preferably 0.033 or more, more preferably 0.05 or more, and preferably 0.2 or less, more preferably 0.15 or less.

[0082] When the fragrance delivery particles of the present invention are produced by mixing the (A) component in stages, the mass ratio of the remaining amount of the (A) component mixed in step (ii) to the amount of the (B1) component mixed in step (iii) [[(B1) component in step (iii)] / (A) component (2) in step (ii)] may, for example, preferably be 0.0033 or more, more preferably 0.0066 or more, and preferably be 0.030 or less, more preferably be 0.025 or less.

[0083] When the fragrance delivery particles of the present invention are produced by mixing the (A) component in stages, the mass ratio of a portion of the amount of the (A) component mixed in step (i) to the remainder of the amount of the (A) component mixed in step (ii) [step (i) / step (ii)] is, for example, preferably 0.1 or more, more preferably 0.2 or more, and preferably 10 or less, more preferably 5 or less.

[0084] Another embodiment of the fragrance delivery particles of the present invention is a method of producing fragrance delivery particles by dividing component (A) into portions and mixing them in stages, specifically, a method of producing the particles by the following steps (i') to (iii').

[0085] Step (i'): A step of mixing a part of the (A) component with the (B1) component to obtain a mixture. Step (ii'): A step of mixing the mixture obtained in the step (i') with the remaining part of the (A) component. Step (iii'): A step of mixing the mixture obtained in the step (ii') with the (B2) component to produce perfume delivery particles.

[0086] When the (A) component is mixed stepwise in this manner, in addition to the perfume delivery particles of the present invention containing the (A), (B1) and (B2) components, perfume-containing particles containing the (A) component and the (B2) component (but not the (B1) component) may be obtained in any ratio. The perfume delivery particles of the present invention may be used in combination with the perfume-containing particles containing the (A) component and the (B2) component, depending on the situation.

[0087] Furthermore, when using mixed particles containing the fragrance delivery particles of the present invention, i.e., mixed particles containing the fragrance delivery particles of the present invention and fragrance-containing particles, the mass ratio of the content of the fragrance delivery particles of the present invention to the content of the fragrance-containing particles [fragrance delivery particles / fragrance-containing particles] may, for example, preferably be 10 / 100 or more, more preferably 20 / 80 or more, even more preferably 30 / 70 or more, and preferably be 100 / 10 or less, more preferably 80 / 20 or less, even more preferably 70 / 30 or less.

[0088] Furthermore, when mixed particles containing fragrance delivery particles and fragrance-containing particles of the present invention are used, the moisture content of the mixed particles as measured by Karl Fischer evaporation method (JIS K 0113) is, for example, 1% by mass or more, and from the viewpoint of the strength of the resulting mixed particles, it is preferably, for example, 3% by mass or more, more preferably 5% by mass or more, even more preferably 8% by mass or more, even more preferably 10% by mass or more, and even more preferably 20% by mass or more, and may be, for example, 35% by mass or less, and from the viewpoint of improving the quality of the fragrance, it may be preferably 32% by mass or less.

[0089] The preferred range of the mass ratio [step (i') / step (ii')] of a portion of the blending amount of component (A) mixed in step (i') to the remainder of the blending amount of component (A) mixed in step (ii') may be the same as the above-mentioned mass ratio [step (i) / step (ii)].

[0090] In another embodiment, the fragrance delivery particles of the present invention can be produced by further mixing a mixture obtained by mixing component (A), component (B2), and component (E) with a mixture obtained by mixing component (B1), component (C), and component (D) from the viewpoint of suppressing volatilization of component (B2) and fragrance stability. In another embodiment, the fragrance delivery particles of the present invention can be produced by further mixing a mixture obtained by mixing component (A), component (B2), component (C), and component (D) with a mixture obtained by mixing component (B1) and component (E) from the viewpoint of suppressing leakage of the encapsulated components of component (B1).

[0091] In another embodiment, the fragrance delivery particles of the present invention can be produced by further mixing a mixture obtained by mixing component (A), component (B2), and component (E) with a mixture of component (B1), component (C), and component (D), from the viewpoints of preventing leakage of the encapsulated components of component (B1), the strength of component (A), and the storage stability of component (B1).

[0092] The mixer used to mix component (A), component (B), and any optional components is not particularly limited as long as it can mix them substantially uniformly, and may be a mixer equipped with a heating means. Examples of such a mixer include a drum mixer, a ribbon mixer, a Nauta mixer, a V-type blender (manufactured by Powrex Corporation), a double cone mixer (manufactured by Tokuju Kogyosho Co., Ltd.), a ribbon blender (manufactured by Hosokawa Micron Corporation), and a container rotation type granulator (manufactured by Sugiyama Heavy Industries Co., Ltd.).

[0093] When mixing component (A), component (B), and optional components, it is preferable to use, for example, a rotary container granulator to prevent component (A) from being disintegrated by applying strong shear. Preferred rotary container granulators include, for example, drum granulators and pan granulators. Drum granulators are not particularly limited as long as they rotate a drum-shaped cylinder to perform processing. Horizontal or slightly inclined drum granulators can also be used. These devices may be, for example, batch or continuous. If the wall friction coefficient between component (A) and the inner wall of the rotary container granulator is small and it is difficult to apply sufficient upward motive force to the powder, it is preferable to provide, for example, multiple baffles on the inner wall of the container to assist mixing. By providing baffles, it is possible to impart upward motive force to the powder, improving powder mixability and solid-liquid mixability.

[0094] The operating conditions of the rotary container granulator are not particularly limited as long as they allow the water-soluble solid in the granulator to flow and be stirred as uniformly as possible. From the viewpoint of obtaining granules with good disintegration strength, the Froude number defined by the following formula (1) can be set to, for example, preferably 0.01 or more, more preferably 0.05 or more, and even more preferably 0.09 or more. From the viewpoint of obtaining non-compacted granules, the upper limit can be set to preferably 1.0 or less, more preferably 0.4 or less, and even more preferably 0.2 or less. In the present invention, g is 9.80665 m / s ２ is used.

[0095] Froude number: Fr = V ２ / (R×g) (1) V: peripheral speed [m / s] R: radius from the center of rotation to the circumference of the rotating object [m] g: gravitational acceleration [m / s ２ ]

[0096] In addition, in a drum-type granulator or pan-type granulator in which granulation progresses by the rotation of the main body, for example, V and R are the values ​​of the main body, in a horizontal or vertical granulator equipped with a main blade or a crushing blade, V and R are the values ​​of the main shaft, and in a pan-type granulator equipped with a crushing blade, for example, V and R are the values ​​of the crushing blade.

[0097] The mixing temperature may be, for example, preferably 20°C or higher, more preferably 30°C or higher, from the viewpoint of flowability and handleability, and preferably 60°C or lower, more preferably 50°C or lower, from the viewpoint of the vaporization stability of component (B2).

[0098] The rotation speed of the mixer may be, for example, preferably 10 rpm or more, more preferably 20 rpm or more, from the viewpoint of mixing uniformity, and preferably 100 rpm or less, more preferably 50 rpm or less, from the viewpoint of suppressing disintegration of the water-soluble solid.

[0099] The mixing time may be, for example, preferably 1 minute or more, more preferably 3 minutes or more, from the viewpoint of mixing uniformity, and preferably 20 minutes or less, more preferably 10 minutes or less, from the viewpoint of suppressing disintegration of the water-soluble solid.

[0100] When mixing component (A) and component (B), for example, component (B) may be supplied dropwise from a pipe using a pump, or may be supplied using a nozzle. The nozzle may be, for example, a single-fluid nozzle or a multi-fluid nozzle. By using a multi-fluid nozzle, component (B) can be dispersed as fine droplets. A multi-fluid nozzle is a nozzle that mixes and atomizes a liquid and an atomization gas (air, nitrogen, etc.) by passing them through independent flow paths to the vicinity of the nozzle tip, and examples of such nozzles include a two-fluid nozzle, a three-fluid nozzle, and a four-fluid nozzle. Furthermore, the mixing section for the flavoring and the atomization gas may be, for example, an internal mixing type in which mixing occurs within the nozzle tip, or an external mixing type in which mixing occurs outside the nozzle tip. Examples of such multi-fluid nozzles include internal mixing type two-fluid nozzles manufactured by Spraying Systems Japan Co., Ltd., Kyoritsu Alloy Manufacturing Co., Ltd., Ikeuchi Co., Ltd., etc., external mixing type two-fluid nozzles manufactured by Spraying Systems Japan Co., Ltd., Kyoritsu Alloy Manufacturing Co., Ltd., Atmax Co., Ltd., etc., and external mixing type four-fluid nozzles manufactured by Fujisaki Electric Co., Ltd.

[0101] When the component (B) is supplied to the component (A) using a multi-fluid nozzle, the supply temperature may be, for example, preferably 20°C or higher, more preferably 30°C or higher, from the viewpoints of flowability and handleability, and preferably 60°C or lower, more preferably 50°C or lower, from the viewpoint of the vaporization stability of the component (B2).

[0102] Furthermore, from the viewpoint of uniformly supporting and retaining the component (B) in the component (A), the addition rate of the component (B) may be, for example, preferably 1 part by mass / minute or more, more preferably 5 parts by mass / minute or more, and preferably 20 parts by mass / minute or less, more preferably 15 parts by mass / minute or less, per 100 parts by mass of the component (A).

[0103] In one embodiment, the perfume delivery particles of the present invention can be applied in the washing process of textile products. That is, the present invention can provide a method for perfumery of textile products, in which the perfume delivery particles are added to the textile products during the washing process.

[0104] When the perfume delivery particles of the present invention are added during the washing process of textile products, the amount of perfume delivery particles of the present invention to be added may be, for example, preferably 5.0 g or more, more preferably 7.0 g or more, and preferably 10.0 g or less, more preferably 8.0 g or less per 1 kg of textile product. The textile product may be treated with only the perfume delivery particles of the present invention, or may be treated with a fabric treatment composition containing the perfume delivery particles of the present invention.

[0105] When the perfume delivery particles of the present invention are added during the washing process of textile products, the perfume delivery particles of the present invention can be added to at least one of the washing water and rinsing water of the laundry, or the perfume delivery particles of the present invention can be added to both the washing water and rinsing water of the laundry.

[0106] When adding the perfume delivery particles of the present invention to the washing process of textile products, for example, a method of adding them to water so that the concentration is preferably 0.001 ppm or more, more preferably 0.01 ppm or more, and preferably 1000 ppm or less, more preferably 100 ppm or less. From the viewpoint of convenience when adding them to a washing machine, it is preferable to use them in the wash water, but it is also possible to add them to the rinse water. The wash water and rinse water of the washing may contain laundry detergent components for textile products.

[0107] The present invention discloses the following perfume delivery particles, a method for producing perfume delivery particles, and a method for perfumery of textile products.

[0108] <1> Fragrance delivery particles containing (A) a water-soluble solid (hereinafter, component (A)) and (B) a fragrance (hereinafter, component (B)), wherein component (B) is (B1) a fragrance encapsulated in a microcapsule (hereinafter, component (B1)) and (B2) a fragrance not encapsulated in a microcapsule (hereinafter, component (B2)), and the fragrance delivery particles have a moisture content measured by Karl Fischer evaporation method (JIS K 0113) (hereinafter, KF moisture content) of 1% by mass or more and 35% by mass or less.

[0109] <2> The fragrance delivery particle according to <1>, wherein the KF moisture content of the fragrance delivery particle is 3% by mass or more, further 5% by mass or more, further 8% by mass or more, further 10% by mass or more, further 20% by mass or more, and 35% by mass or less, further 32% by mass or less.

[0110] <3> The perfume delivery particle according to <1> or <2>, wherein the component (A) is a water-soluble solid having a solubility of 1.0 g or more in 100 g of water at 20°C, and further having a solubility of 1.0 g or more to 60 g or less.

[0111] <4> The perfume delivery particle according to any one of <1> to <3>, wherein the component (A) is a water-soluble solid having pores on its surface with an average pore size of 1 nm or more, preferably 10 nm or more, and 1000 μm or less, preferably 100 μm or less.

[0112] <5> The perfume delivery particle according to any one of <1> to <4>, wherein the component (A) is a water-soluble solid having a bulk density of 450 g / L or more, preferably 500 g / L or more, and 750 g / L or less, preferably 650 g / L or less.

[0113] <6> The perfume delivery particle according to any one of <1> to <5>, wherein the component (A) is a water-soluble solid having an average particle size of 1.0 mm or more, preferably 3.0 mm or more, and 20 mm or less, preferably 15 mm or less, preferably 10 mm or less, and preferably 5 mm or less.

[0114] <7> The perfume delivery particle according to any one of <1> to <6>, wherein the component (A) is a dried product of a water-soluble solid having water of crystallization and a water-soluble inorganic salt having water of crystallization.

[0115] <8> The fragrance delivery particle according to any one of <1> to <7>, wherein the component (A) is a water-soluble solid having a moisture content of 0.1% by mass or more, further 1% by mass or more, further 1.6% by mass or more, further 2.0% by mass or more, further 5% by mass or more, further 8% by mass or more, as measured by an infrared moisture meter, and 20% by mass or less, further 18% by mass or less, further 15% by mass or less, further 14% by mass or less.

[0116] <9> The fragrance delivery particle according to any one of <1> to <8>, wherein the component (B1) is a fragrance-encapsulating microcapsule in which a fragrance compound exhibiting a ClogP of 1.0 or more, further 1.5 or more, further 2.0 or more, further 2.3 or more, further 2.5 or more, and 30 or less, further 20 or less, further 10 or less, further 6.0 or less, further 5.5 or less, further 5.0 or less is encapsulated in the microcapsule.

[0117] <10> The fragrance delivery particle according to any one of <1> to <9>, wherein the component (B2) is a fragrance not encapsulated in a microcapsule, and has a ClogP of 1.0 or more, further 1.5 or more, further 2.0 or more, further 2.3 or more, further 2.5 or more, and 30 or less, further 20 or less, further 10 or less, further 6.0 or less, further 5.5 or less, further 5.0 or less.

[0118] <11> The fragrance delivery particle according to any one of <1> to <10>, wherein the component (B1) is a fragrance-encapsulating microcapsule in which a fragrance compound exhibiting an oil-water interfacial tension of 7 mN / m or more, preferably 10 mN / m or more, further preferably 13 mN / m or more is encapsulated in the microcapsule.

[0119] <12> The fragrance delivery particle according to any one of <1> to <11>, wherein the component (B2) is a fragrance that is not encapsulated in a microcapsule and has an oil-water interfacial tension of 7 mN / m or more, preferably 10 mN / m or more, and further preferably 13 mN / m or more.

[0120] <13> The perfume delivery particle according to any one of <1> to <12>, wherein the component (B1) is a perfume-encapsulating microcapsule having an average particle size of 0.1 μm or more, further 0.1 μm or more, further 1 μm or more, and 50 μm or less, further 40 μm or less.

[0121] <14> The fragrance delivery particle according to any one of <1> to <13>, wherein the content of the component (B1) is, relative to 100% by mass of the fragrance delivery particle, 0.05% by mass or more, further 0.05% by mass or more, further 0.1% by mass or more, further 0.2% by mass or more, further 0.3% by mass or more, further 0.4% by mass or more, and 6.5% by mass or less, further 6.0% by mass or less, further 5.5% by mass or less, further 5.0% by mass or less, or further 4.5% by mass or less.

[0122] <15> The fragrance delivery particle according to any one of <1> to <14>, wherein the content of the component (B2) is 1.0% by mass or more, further 2.0% by mass or more, further 3.0% by mass or more, further 5.0% by mass or more, and 10.0% by mass or less, further 9.0% by mass or less, based on 100% by mass of the fragrance delivery particle.

[0123] <16> The perfume delivery particle according to any one of <1> to <15>, wherein the mass ratio of the content of the component (A) to the content of the component (B1) [(B1) / (A)] is 0.0001 or more, further 0.0003 or more, further 0.0005 or more, and is 0.20 or less, further 0.15 or less, further 0.10 or less.

[0124] <17> The perfume delivery particle according to any one of <1> to <16>, wherein the mass ratio of the content of the component (A) to the content of the component (B2) [(B2) / (A)] is 0.01 or more, further 0.015 or more, further 0.03 or more, further 0.05 or more, and is 0.20 or less, further 0.15 or less, further 0.12 or less, further 0.10 or less.

[0125] <18> The perfume delivery particles according to any one of <1> to <17>, wherein the perfume delivery particles have an average particle size of 1.0 mm or more, further 1.5 mm or more, further 2.0 mm or more, and 20 mm or less, further 10 mm or less, further 5 mm or less.

[0126] <19> The perfume delivery particle according to any one of <1> to <18>, wherein the perfume delivery particle has a bulk density of 400 g / L or more, further 500 g / L or more, and 1000 g / L or less, further 800 g / L or less.

[0127] <20> The perfume delivery particle according to any one of <1> to <19>, further comprising (C) one or more selected from a water-soluble cationic polymer compound and a cationic surfactant [hereinafter, component (C)].

[0128] <21> The perfume delivery particle according to any one of <1> to <20>, wherein the cationic surfactant as component (C) is one or more selected from alkyl quaternary ammonium salts, alkyltrimethylammonium salts having an alkyl group of 10 to 22 carbon atoms, alkyltrimethylammonium chloride having an alkyl group of 10 to 22 carbon atoms, lauryltrimethylammonium chloride, stearyltrimethylammonium chloride, and cetyltrimethylammonium chloride, and further cetyltrimethylammonium chloride.

[0129] <22> The perfume delivery particle according to any one of <1> to <21>, wherein the content of the cationic surfactant as component (C) is 0.01% by mass or more, further 0.05% by mass or more, and 2.0% by mass or less, further 1.0% by mass or less, based on 100% by mass of the perfume delivery particle.

[0130] <23> The perfume delivery particle according to any one of <1> to <22>, wherein the water-soluble cationic polymer compound as component (C) is one or more selected from poly(acrylamide-co-diallyldimethylammonium chloride) and poly(diallyldimethylammonium chloride).

[0131] <24> The fragrance delivery particle according to any one of <1> to <23>, wherein the water-soluble cationic polymer compound as component (C) is 0.01% by mass or more, further 0.05% by mass or more, and 2.0% by mass or less, further 1.0% by mass or less, based on 100% by mass of the fragrance delivery particle.

[0132] <25> The perfume delivery particle according to any one of <1> to <24>, further comprising (D) a water-soluble nonionic polymer [hereinafter, referred to as component (D)].

[0133] <26> The perfume delivery particle according to any one of <1> to <25>, wherein the component (D) is one or more selected from the group consisting of a water-soluble nonionic polymer having a number average molecular weight of 2,000 or more, preferably 3,000 or more, further 4,000 or more, and 20,000 or less, further 15,000 or less, further 10,000 or less, polyethylene glycol, and polypropylene glycol.

[0134] <27> The fragrance delivery particle according to any one of <1> to <26>, wherein the content of the component (D) is 0.5% by mass or more, further 1% by mass or more, and 30% by mass or less, further 25% by mass or less, further 20% by mass or less, based on 100% by mass of the fragrance delivery particle.

[0135] <28> The perfume delivery particle according to any one of <1> to <27>, wherein the mass ratio of the content of the component (A) to the content of the component (D), [(A) / (D)], is 0.1 or more, further 0.2 or more, further 0.3 or more, further 0.5 or more, further 1.0 or more, further 5.0 or more, further 7.0 or more, and is 100 or less, further 95 or less, further 50 or less, further 30 or less, further 25 or less, or further 20 or less.

[0136] <29> The perfume delivery particle according to any one of <1> to <28>, further comprising (E) an oxidation stabilizer [hereinafter, referred to as component (E)].

[0137] <30> The fragrance delivery particle according to any one of <1> to <29>, wherein the content of the component (E) is 0.01% by mass or more, further 0.02% by mass or more, and 0.50% by mass or less, further 0.30% by mass or less, based on 100% by mass of the fragrance delivery particle of the present invention.

[0138] <31> A method for producing fragrance delivery particles, comprising mixing (A) a water-soluble solid [hereinafter, component (A)] and (B) a fragrance [hereinafter, component (B)], wherein component (B) is (B1) a fragrance encapsulated in a microcapsule [hereinafter, component (B1)] and (B2) a fragrance not encapsulated in a microcapsule [hereinafter, component (B2)], and the fragrance delivery particles obtained by the production method have a water content measured by Karl Fischer evaporation method (JIS K 0113) [hereinafter, KF water content] of 1% by mass or more and 35% by mass or less.

[0139] <32> The method for producing perfume delivery particles according to <31>, wherein the mixture obtained by mixing the component (A) and the component (B2) is mixed with the component (B1) to produce perfume delivery particles.

[0140] <33> The method for producing perfume delivery particles according to either <31> or <32>, wherein a mixture obtained by mixing the component (A) and the component (B2) is mixed with a mixture obtained by mixing the component (B1) and optionally the component (D), to produce perfume delivery particles.

[0141] <34> The method for producing fragrance delivery particles according to any one of <31> to <33>, wherein the mixture obtained by mixing the component (A) and the component (B1) is mixed with the component (B2) to produce fragrance delivery particles.

[0142] <35> The method for producing fragrance delivery particles according to any one of <31> to <34>, wherein a mixture obtained by mixing the component (A) and the component (B1) is mixed with a mixture obtained by mixing the component (B2) and optionally the component (D), to produce fragrance delivery particles.

[0143] <36> A method for scenting a textile product, in a washing step of the textile product, by adding fragrance-delivery particles to treat the textile product, wherein the fragrance-delivery particles contain (A) a water-soluble solid [hereinafter, component (A)] and (B) a fragrance [hereinafter, component (B)], and the component (B) is (B1) a fragrance encapsulated in a microcapsule [hereinafter, component (B1)] and (B2) a fragrance not encapsulated in a microcapsule [hereinafter, component (B2)], and the fragrance-delivery particles have a moisture content measured by Karl Fischer evaporation method (JIS K 0113) [hereinafter, KF moisture content] of 1% by mass or more and 35% by mass or less.

[0144] <37> The method for perfumery of <36>, wherein the perfume delivery particles are added in an amount of 5.0 g or more, further 7.0 g or more, and 10.0 g or less, further 8.0 g or less per 1 kg of the textile product in the washing step of the textile product.

[0145] <38> The method for perfumery of the textile product according to the above <36> or <37>, wherein the perfume is added to water in a washing step of the textile product in an amount of 0.001 ppm or more, further 0.01 ppm or more, and 1000 ppm or less, further 100 ppm or less.

[0146] The components used in the Examples and Comparative Examples are summarized below. In the Examples and Comparative Examples, "%" means "% by mass" unless otherwise specified. The mass % of the blended compositions in Tables 3 to 7 indicates the mass % of the actual amount (for fragrance microcapsule slurries, the mass % of the amount of fragrance compound encapsulated as an effective amount). The physical properties were measured using the following methods.

[0147] (1) Bulk density: Calculated using a bulk specific gravity measuring instrument in accordance with JIS K7365.

[0148] (2) Average particle size of fragrance-delivery particles The spherical equivalent diameter of 250 particles was calculated using image analysis software ImageJ.

[0149] (3) Moisture Content of Fragrance Delivery Particles The KF moisture content of the fragrance delivery particles was measured by the Karl Fischer evaporation method (JIS K 0113). A Hiranuma automatic moisture analyzer AQV-2200A (manufactured by Hitachi High-Technologies Corporation) was used as the moisture content measuring device. 50 mL of dehydrated methanol was placed in a titration tank with a capacity of approximately 150 mL of the moisture content measuring device as the titration solvent, and the mixture was stirred with a magnetic stirrer. An inlet pipe for introducing vaporized water from a water vaporizer was placed in dehydrated methanol (product name: dehydrated methanol (manufactured by Katayama Chemical Co., Ltd., product number 119-2400-5)) in the titration tank, and nitrogen aerated through a desiccant was flowed as a carrier gas at a flow rate of 200 mL / min to bubble the anhydrous methanol. 2.5 mL of the commercially available Karl Fischer reagent Aqualite KF5 (manufactured by Hiranuma Co., Ltd., titer 5.0 mg / mL) was added dropwise to make the titration tank anhydrous. 0.05 g of each fragrance delivery particle was weighed into a sample heating boat of a moisture vaporizer EV-2000 (Hitachi High-Tech Corporation), heated at 210°C for 2 minutes to vaporize the moisture from the fragrance delivery particle, and introduced into anhydrous methanol in the titration tank of a HIRANUMA automatic moisture analyzer AQV-2200A (Hitachi High-Tech Corporation) at 200 mL / min of carrier gas (nitrogen). This was titrated using Karl Fischer reagent Aqualite KF5 (HIRANUMA Corporation) to measure the amount of vaporized moisture. The same measurement as above was also performed three times using the same sample to measure the amount of moisture. The amount of vaporized moisture was calculated using the following formula: W = F x V x 100 / (S x 103) W: Water content (%) F: Titer of Karl Fischer reagent (mg / mL) V: Amount of Karl Fischer reagent used for titration (mL) S: Mass of sample (g)

[0150] [Components Used] <Component (A)> (A1): Magnesium sulfate heptahydrate (product name: "Magnesium Sulfate heptahydrate", manufactured by Laizhou City Laiyu Chemical Co. Ltd., 3-5 mm spheres, moisture content measured by an infrared moisture meter: 31.1% by mass, bulk density: 790 g / L)) dried at 120°C for 2 hours using an Advantec Toyo low-temperature air-blowing dryer DRM620TE (moisture content measured by an infrared moisture meter: 1.7% by mass, bulk density: 510 g / L). (A2): Magnesium sulfate heptahydrate (the same as in (A1) above) was dried at 120°C for 2 hours using a fluidized bed dryer (Slit Flow manufactured by Okawara Manufacturing Co., Ltd.) with 4 m of hot air. ３ (A3): Magnesium sulfate heptahydrate (the same as (A1) above) was dried at 4 m / min at 120°C for 25 minutes (water content measured by an infrared meter: 5.1% by mass, bulk density: 590 g / L). ３ (A4): Magnesium sulfate heptahydrate (the same as in (A1) above) was dried at 4 m / min at 120°C with hot air of 4 m / min for 15 minutes (water content measured by an infrared meter: 16.4% by mass, bulk density: 650 g / L). ３ (A1): Magnesium sulfate heptahydrate (product name: "Magnesium Sulfate heptahydrate", manufactured by Laizhou City Laiyu Chemical Co. Ltd., 3-5 mm spheres, moisture content measured by an infrared moisture meter: 31.1 mass%, bulk density: 790 g / L)

[0151] The moisture content of (A1) to (A5) above was calculated by the following method. 2 g of a sample (water-soluble solid) was weighed into an aluminum container with a diameter of 11.5 cm. Then, using an infrared moisture meter (for example, MOC63u manufactured by Shimadzu Corporation), the mass of the sample (component (A)) after drying was measured in the wet-based moisture measurement mode at a temperature of 105°C under the Auto condition (the measurement was terminated when the change in the measurement value was within 0.05% in 30 seconds, which was considered to be the final measurement value). The moisture content was calculated using the following formula: Moisture content (mass %) = {mass before drying (g) - mass after drying (g)} / mass before drying (g).

[0152] <Component (B)> Component (B1): (B1-1) Fragrance microcapsule slurry obtained in the following Production Example. 1.7 g of diisobutylene-maleic anhydride copolymer (Demol EP, solids content 25%, manufactured by Kao Corporation) was neutralized with hydrochloric acid and further diluted with ion-exchanged water to obtain an aqueous solution with a solids content of 3% and a pH of 4.3. Next, 98 g of a fragrance composed of the fragrance compounds shown in Table 1 below was added to 100 g of the diisobutylene-maleic anhydride copolymer aqueous solution, and the mixture was emulsified using a homomixer and heated to 50°C. Next, an aqueous solution prepared by mixing 12 g of partially methylolated melamine resin (trade name Cyme 1385, solids content 80%, manufactured by Cytec Industries Inc.) and 35 g of ion-exchanged water was added dropwise. This was maintained at 50°C for 2 hours, then at 70°C for 1 hour, and then at 80°C for 3 hours to complete the encapsulation. The mixture was then allowed to cool, yielding a fragrance microcapsule slurry with an average particle size of 7 μm and an active ingredient content of 40% by mass. The average particle size (median diameter) of the fragrance microcapsules was measured using a laser diffraction / scattering particle size distribution analyzer "LA-950" (manufactured by Horiba, Ltd.). A flow cell was used for the measurement, and water was used as the dispersion medium. The refractive index was set to 1.333-i for the dispersion medium and 1.48-0i for the dispersoid. A dispersion liquid containing the particles to be measured was added to the flow cell, and measurements were carried out at a concentration that showed a transmittance of around 90%, to determine the average particle size (median diameter).

[0153]

[0154] (B2) Component: (B2-1) Fragrance composed of fragrance compounds shown in Table 2 below

[0155]

[0156] Component (C): "Polyquaternium-7" (manufactured by Lubrizol Advanced Materials, Inc.) Component (D): PEG (polyethylene glycol, number average molecular weight 8500) Component (E): BHT (oxidation stabilizer, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)

[0157] [Production of Fragrance Delivery Particles] Example 1 The component (A1) (solid temperature of component (A1) 50°C) was charged into a 75 L drum granulator (φ40 cm x L60 cm) equipped with a baffle plate in the composition shown in Table 3. While mixing under conditions of Froude number 0.118 / drum angle 12.6°, a mixture of components (B2) and (E) was added via a pipe in the amount shown in Table 3 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in formula (1)). Furthermore, a mixture of components (B1), (C) and (D) was added via a pipe in the amount shown in Table 3 and mixed for 3 minutes 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). The resulting perfume delivery particles had a KF moisture content of 21.2% by mass, an average particle size of 4 mm, and a bulk density of 600 g / L.

[0158] Example 2: Component (A2) (solid temperature of component (A2) 50°C) was charged to a 75L drum granulator (φ40cm x L60cm) equipped with a baffle plate in the composition shown in Table 3. While mixing under conditions of Froude number 0.118 / drum angle 12.6°, a mixture of components (B2) and (E) was added via piping in the amount shown in Table 3 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in the above formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amount shown in Table 3 and mixed for 3 minutes 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). The resulting perfume delivery particles had a KF moisture content of 27.1% by mass, an average particle size of 4 mm, and a bulk density of 640 g / L.

[0159] Example 3: Component (A3) (solid temperature of component (A3) 50°C) was charged to a 75L drum granulator (φ40cm x L60cm) equipped with a baffle plate in the composition shown in Table 3. While mixing under conditions of Froude number 0.118 / drum angle 12.6°, a mixture of components (B2) and (E) was added via piping in the amount shown in Table 3 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amount shown in Table 3 and mixed for 3 minutes 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). The resulting perfume delivery particles had a KF moisture content of 31.5% by mass, an average particle size of 4 mm, and a bulk density of 670 g / L.

[0160] Example 4 In step (i), component (A1) (solid temperature of component (A1) 50°C) was charged in an amount half the composition shown in Table 3 into a 75 L drum granulator (φ40 cm × L60 cm) equipped with a baffle, and while stirring under conditions of a Froude number of 0.118 and a drum angle of 12.6°, a mixture of components (B2) and (E) in the amount shown in Table 3 was added via piping and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in formula (1)). In step (ii), the remaining half of component (A1) shown in Table 3 was further added to the mixture obtained in step (i), and mixed for 10 seconds. In step (iii), a mixed solution of components (B1), (C), and (D) was added to the mixture obtained in step (ii) via a pipe in the amount shown in Table 3, and mixed for 3 minutes and 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). Steps (i) to (iii) above yielded mixed particles of perfume-delivery particles X containing components (A1), (B1), and (B2), and perfume-containing particles Y containing components (A1) and (B1). The resulting mixed particles had a KF moisture content of 22.7% by mass, an average particle size of 4 mm, and a bulk density of 619 g / L.

[0161] In addition, in Example 4, the mixed liquid of components (B1), (C), and (D) in step (iii) is assumed to be uniformly distributed in the mixture of components (A1), (B2), and (E) in step (i) and the additional component (A1) in step (ii), and as a result, the content of perfume delivery particles X in the mixed particles obtained in Example 4 is determined to be 53% by mass.

[0162] Comparative Example 1: Component (A4) (solid temperature of component (A4) 50°C) was charged to a 75L drum granulator (φ40cm x L60cm) equipped with a baffle plate in the composition shown in Table 3. While mixing under conditions of Froude number 0.118 / drum angle 12.6°, a mixture of components (B2) and (E) was added via piping in the amount shown in Table 3 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amount shown in Table 3 and mixed for 3 minutes 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). The resulting perfume delivery particles had a KF moisture content of 37.6% by mass, an average particle size of 4 mm, and a bulk density of 740 g / L.

[0163] Comparative Example 2: Magnesium sulfate heptahydrate (component (A5)) was not dried and was placed in the amount shown in Table 3 into a 75 L drum granulator (φ40 cm x L60 cm) equipped with a baffle. While mixing under conditions of a Froude number of 0.118 and a drum angle of 12.6°, a mixture of components (B2) and (E) was added via piping in the amount shown in Table 3 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 25°C, V = 0.48 m / s, R = 0.2 m in formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 40°C). The batch size was 6.5 kg (total blend amount). The resulting fragrance-delivery particles were unable to sufficiently support the fragrance, and the resulting particles were sticky. The water content of the obtained particles was measured by KF forcibly and found to be 41.2% by mass.

[0164] <Scent Intensity Ratings 1, 2, and 3> In a room maintained at a room temperature of 25°C and a humidity of 65%, a Toshiba fully automatic washing machine AW-7D8(W) was used, set to use 28 L of water (water temperature 25°C), and loaded with 18.7 g of a commercially available unscented liquid detergent and 10.1 g of the fragrance delivery particles of the present invention. Eight cotton towels and five cotton T-shirts (total dry weight of the cotton towels and cotton T-shirts: 1.4 kg) were washed for 9 minutes, rinsed twice, and spun for 3 minutes. The scent intensity of the cotton towels immediately after spinning and after drying indoors (temperature 25°C, humidity 65%) for one day was evaluated according to the following evaluation criteria. The scent intensity of the cotton towels immediately after spinning was assigned a rating of 1, and the scent intensity of the dried cotton towels was assigned a rating of 2. Furthermore, the scent intensity of the cotton towels when two fingers were traced over the surface of the dried cotton towels was assigned a rating of 3. The evaluation results were calculated as the average of the ratings of three expert panelists.

[0165] For Examples 1 and 4, the fragrance delivery particles stored at 40°C for 20 days were used to wash and dry cotton towels in the same manner as above. The fragrance intensity of the dried cotton towels was evaluated as a rating of 4, and the fragrance intensity of the cotton towels when two fingers were run over the surface of the dried cotton towels was evaluated as a rating of 5. The evaluation results were calculated as the average of the ratings of three expert panelists. The evaluation results are shown in Table 3.

[0166] <<Evaluation criteria>> 0: No odor 1: Very slight odor 2: Weak odor 3: Clear odor 4: Strong odor 5: Fairly strong odor 6: Very strong odor

[0167]

[0168] It was confirmed that the fragrance-delivery particles of Examples 1 to 4 were able to retain a large amount of fragrance on textile products even after the washing and rinsing processes in the washing process of textile products. Furthermore, it was confirmed that the mixed particles containing the fragrance-delivery particles of Example 4 had improved fragrance intensity (ratings 4 and 5) after 20 days of storage at 40°C, and it is predicted that the inclusion of fragrance-containing particles containing components (A1) and (B1) in the mixed particles is effective in preventing leakage of the encapsulated components of the fragrance-encapsulated microcapsules.

[0169] Blending Examples 1-1 to 1-4: The component (A1) (solid temperature of component (A1) 50°C) was charged to a 75L drum granulator (φ40cm x L60cm) equipped with a baffle plate in the composition shown in Table 4. While mixing under conditions of a Froude number of 0.118 and a drum angle of 12.6°, a mixture of components (B2) and (E) was added via piping in the amount shown in Table 4 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in the formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amount shown in Table 4 and mixed for 3 minutes and 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total blend amount). The fragrance delivery particles obtained in Formulation Examples 1-1 to 1-4 had a KF moisture content of 20 to 30% by mass. When the fragrance delivery particles obtained in Formulation Examples 1-1 to 1-4 were subjected to the same evaluations 1, 2, and 3 as in Examples, high fragrance intensity was obtained in all cases.

[0170]

[0171] Formulation Examples 2-1 to 2-3 [Ingredients Used] The ingredients used in Table 5 other than the following ingredient (A) were the same as those in the Examples. <Ingredient (A)> (A6): Magnesium sulfate heptahydrate (product name "Magnesium Sulfate heptahydrate", manufactured by Laizhou City Laiyu Chemical Co. Ltd., 3-5 mm spheres, moisture content measured by an infrared moisture meter: 31.1% by mass, bulk density: 790 g / L)), dried at 120°C for 2 hours using an Advantec Toyo low-temperature blower dryer DRM620TE (moisture content measured by an infrared moisture meter: 10.0% by mass, bulk density: 600 g / L).

[0172] The component (A6) (solid temperature of component (A6) 50°C) was charged to a 75L drum granulator (φ40cm x L60cm) equipped with a baffle plate in the composition shown in Table 5. While mixing under conditions of Froude number 0.118 / drum angle 12.6°, a mixture of components (B2) and (E) was added via piping in the amount shown in Table 5 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in the formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amount shown in Table 5 and mixed for 3 minutes 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). The fragrance delivery particles obtained in Formulation Examples 2-1 to 2-3 had a KF moisture content of 20 to 30% by mass. Using the fragrance delivery particles obtained in Formulation Examples 2-1 to 2-3, the solubility in 20°C Wakayama City water was evaluated using the following method. The results are shown in Table 5.

[0173] <Solubility Evaluation> 0.5 g of the fragrance delivery particles obtained in Formulation Examples 2-1 to 2-3 was placed in a 0.5 L beaker containing 500 mL of water at 20°C, and dissolved by stirring at 600 rpm using a 3.5 cm long rod-shaped stirring bar and a magnetic stirrer. Complete dissolution was confirmed by visual inspection, and the solubility was evaluated based on the time required for complete dissolution using the following criteria. The results are shown in Table 5. Note that "complete dissolution" means that no solid components remain.

[0174] <<Evaluation Criteria>> ⊚: Dissolved within 3 minutes after adding the fragrance delivery particles. ◯: Dissolved between 3 and 6 minutes after adding the fragrance delivery particles. Δ: Dissolved between 6 and 9 minutes after adding the fragrance delivery particles.

[0175]

[0176] Formulation Examples 3-1 to 3-3 (Table 6) and Formulation Examples 4-1 to 4-3 (Table 7) [Ingredients Used] The ingredients used in Tables 6 and 7 other than the following ingredient (A) were the same as those used in the Examples and Formulation Examples 1 and 2. <Ingredient (A)> (A7): Sodium sulfate decahydrate (product name "Sodium Sulfate Decahydrate", manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., 0.1 to 5.0 mm columns, moisture content 56.6% by mass as measured by an infrared moisture meter, bulk density 711 g / L)), dried at 120°C for 4 hours using a constant temperature air-blowing incubator manufactured by Yamato Scientific Co., Ltd. (moisture content 0.4% by mass as measured by an infrared moisture meter, bulk density 400 g / L to 800 g / L). (A8): Sodium carbonate decahydrate (product name: "Sodium Carbonate Decahydrate", manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., 0.1 to 5.0 mm columns, moisture content of 62.2% by mass as measured by an infrared moisture meter, bulk density of 825 g / L)) dried at 120°C for 3 hours in a constant temperature incubator with a blower manufactured by Yamato Scientific Co., Ltd. (moisture content of 15% by mass as measured by an infrared moisture meter, bulk density of 400 g / L to 800 g / L).

[0177] The components (A6) to (A8) (solid temperature of components (A6) to (A8) 50°C) were charged into a 75 L drum granulator (φ40 cm × L60 cm) equipped with a baffle plate in the compositions shown in Tables 6 and 7. While mixing under conditions of a Froude number of 0.118 and a drum angle of 12.6°, a mixture of components (B2) and (E) was added via piping in the amounts shown in Tables 6 and 7 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in the formula (1)). Furthermore, a mixture of components (B1), (C), and (D) was added via piping in the amounts shown in Tables 6 and 7 and mixed for 3 minutes and 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total amount). The KF moisture content of the fragrance delivery particles obtained in Formulation Examples 3-1 to 3-3 and Formulation Examples 4-1 to 4-3 is shown in Tables 6 and 7, respectively. The fragrance delivery particles obtained in Formulation Examples 3-1 to 3-3 and Formulation Examples 4-1 to 4-3 were also evaluated for fragrance intensity and fragrance quality using the methods described below. The results are shown in Tables 6 and 7, respectively.

[0178] <Scent Intensity Ratings 1 and 2> In a room maintained at a room temperature of 25°C and a humidity of 65%, a Toshiba fully automatic washing machine AW-7D8(W) was used, set to use 28 L of water (water temperature 25°C), and loaded with 18.7 g of a commercially available unscented liquid detergent and 10.1 g of the fragrance delivery particles of the present invention. Eight cotton towels and five cotton T-shirts (total dry weight of the cotton towels and cotton T-shirts: 1.4 kg) were washed for 9 minutes, rinsed twice, and spun for 3 minutes. The scent intensity of the cotton towels immediately after spin-drying and after drying indoors (temperature 25°C, humidity 65%) for one day was evaluated according to the following evaluation criteria. The scent intensity of the cotton towels immediately after spin-drying was assigned a rating of 1, and the scent intensity of the dried cotton towels was assigned a rating of 2. The evaluation results were calculated as the average of the ratings of three expert panelists.

[0179] <<Evaluation criteria>> 0: No odor 1: Very slight odor 2: Weak odor 3: Clear odor 4: Strong odor 5: Fairly strong odor 6: Very strong odor

[0180] <Scent Quality Ratings 1 and 2> In a room maintained at a room temperature of 25°C and a humidity of 65%, a Toshiba fully automatic washing machine AW-7D8(W) was used, set to use 28 L of water (water temperature 25°C), and loaded with 18.7 g of a commercially available unscented liquid detergent and 10.1 g of the fragrance delivery particles of the present invention. Eight cotton towels and five cotton T-shirts (total dry weight of the cotton towels and cotton T-shirts: 1.4 kg) were washed for 9 minutes, rinsed twice, and spun for 3 minutes. The scent quality of the cotton towels immediately after spin-drying and after drying indoors (temperature 25°C, humidity 65%) for one day was evaluated according to the following evaluation criteria. The scent quality of the cotton towels immediately after spin-drying was assigned a rating of 1, and the scent quality of the dried cotton towels was assigned a rating of 2. The evaluation results were calculated as the average of the ratings from three expert panelists. Regarding the "fragrance balance" in the evaluation criteria below, a good fragrance balance means that the fragrance is as designed and the quality of the fragrance is good, while a poor balance means that the fragrance is different from the designed fragrance and therefore the quality of the fragrance is poor.

[0181] <<Evaluation criteria>> ◎: Very well balanced fragrance ○: Well balanced fragrance △: Slightly unbalanced fragrance ×: Unbalanced fragrance

[0182]

[0183]

Claims

1. A fragrance delivery particle containing (A) a water-soluble solid [hereinafter component (A)] and (B) a fragrance [hereinafter component (B)], wherein component (B) is (B1) a fragrance encapsulated in a microcapsule [hereinafter component (B1)] and (B2) a fragrance not encapsulated in a microcapsule [hereinafter component (B2)], and the moisture content of the fragrance delivery particle, as measured by the Karl Fischer evaporation method (JIS K 0113), is 1% by mass or more and 35% by mass or less.

2. The fragrance delivery particle of claim 1, wherein component (A) is a water-soluble inorganic salt.

3. The fragrance delivery particle according to claim 1 or 2, wherein component (A) is a water-soluble inorganic sulfate.

4. The fragrance delivery particle according to claim 1 or 2, wherein the mass ratio [(B1) / (B2)] of the content of the (B1) component to the content of the (B2) component in the (B) component is 0.005 or more and 5.0 or less.

5. The fragrance delivery particle according to claim 1 or 2, wherein the content of component (A) is 50% by mass or more and 99% by mass or less.

6. A method for producing fragrance delivery particles, which comprises mixing (A) a water-soluble solid [hereinafter component (A)] and (B) a fragrance [hereinafter component (B)], wherein component (B) is (B1) a fragrance encapsulated in a microcapsule [hereinafter component (B1)] and (B2) a fragrance not encapsulated in a microcapsule [hereinafter component (B2)], and the moisture content of the fragrance delivery particles, as measured by the Karl Fischer evaporation method (JIS K 0113), is 1% by mass or more and 35% by mass or less.

7. The method for producing the perfume delivery particles according to claim 6, wherein the components (A) and (B) are mixed using a container rotary granulator.

8. A method for producing perfume delivery particles according to claim 6, comprising mixing the mixture obtained by mixing the components (A) and (B2) with the component (B1).

9. A method for perfumery of textile products, comprising adding the perfume delivery particles according to claim 1 or 2 during the washing process of the textile products.

10. A method for perfumery of textile products according to claim 9, comprising adding the perfume delivery particles according to claim 1 or 2 to at least one of wash water and rinse water during the washing process of textile products.

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