Perfume delivery particles
Patent Information
- Application Number
- JP2024158511
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-09-14
- Filing Date
- 2024-09-12
- Publication Date
- 2025-03-27
AI Technical Summary
【0008】 本発明によれば、繊維製品の洗濯工程において、洗浄工程やすすぎ工程を経ても、香料が繊維製品に多くとどまることができる香料送達粒子を提供することができる。更には、好ましい香りの質を繊維製品に付与できる香料送達粒子を提供することができる。
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Abstract
Description
[Technical field]
[0001] The present invention relates to perfume delivery particles, a method for making perfume delivery particles, and a method for perfuming textile products. [Background technology]
[0002] In recent years, research has been conducted into techniques for imparting fragrances having functions such as fragrance, bactericidal properties, disinfecting properties, antibacterial properties, and ultraviolet protection properties to clothes using auxiliary ingredients other than detergent when washing clothes. In particular, attempts have been made to attach fragrance components to clothes by adding a granular composition in which a fragrance is supported on a solid carrier, i.e., fragrance delivery particles, separately from detergent during washing.
[0003] Patent Document 1 discloses a technology for granulated powder in which microcapsules containing beneficial substances and fragrances are supported on a solid carrier. Patent Document 2 discloses a technology for fragrance powder in which anhydrous magnesium sulfate is impregnated with a fragrance emulsion. Patent Document 3 discloses a technology for fragrance-containing particles containing polyethylene glycol, a water-soluble filler, and a fragrance component. [Prior art documents] [Patent documents]
[0004] [Patent Document 1] JP 2020-512452 A [Patent Document 2] Japanese Patent Application Publication No. 1-188597 [Patent Document 3] Patent Publication No. 2021-529869 Summary of the Invention [Problem to be solved by the invention]
[0005] When such perfume delivery particles are used in the washing process, it is necessary that the perfume remains on the textile product even after the process of removing dirt with a cleaning component during washing and the rinsing process of removing the cleaning component. For this reason, a method is desired in which the perfume delivery particles do not dissolve in the presence of cleaning components, but dissolve in the rinsing stage. The perfume delivery particles have a problem of remaining undissolved at the end of washing, while if the perfume delivery particles dissolve too quickly during the washing process, the perfume is unlikely to remain on the textile product at the end of washing. Therefore, a technology is required for the perfume to remain sufficiently on the textile product at the end of washing. In addition, 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, and the effect of the microcapsules is significantly reduced. Therefore, a technology is required for the perfume and microcapsules to remain sufficiently on the textile product at the end of washing. [Means for solving the problem]
[0006] In one embodiment, the present invention provides 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.
[0007] In another embodiment, the present invention provides 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. Effect of the Invention
[0008] 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 steps in the washing process of textile products, and further, it is possible to provide perfume delivery particles that can impart a desirable fragrance quality to textile products. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0009] [Fragrance delivery particles] The fragrance delivery particle of the present invention contains (A) a water-soluble solid [hereinafter, component (A)] and (B) a fragrance [hereinafter, component (B)], and the moisture content of the fragrance delivery particle measured by the Karl Fischer evaporation method (JIS K 0113) is 1% by mass or more and 35% by mass or less.
[0010] <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.
[0011] Component (A) may have pores on the surface, and the average pore size may be, for example, preferably 1 nm or more, more preferably 10 nm or more, from the viewpoint of further increasing the storage stability and strength of the perfume delivery particles, and preferably 1000 μm or less, more preferably 100 μm or less, from the viewpoint of the strength of the resulting perfume delivery particles. The average pore size of the pores present on the surface of component (A) is measured by mercury intrusion using a mercury porosimeter (e.g., Autopore IV9500 (manufactured by Shimadzu Corporation)), and the value of the average pore size can be calculated using AveragePoreDiameter (4V / A).
[0012] 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.
[0013] The component (A) may, for example, preferably have an average particle size of 1.0 mm or more, more preferably 3.0 mm or more, and preferably have an average particle size of 20 mm or less, more preferably 15 mm or less, even more preferably 10 mm or less, and even 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.
[0014] Examples of the component (A) include water-soluble inorganic salts, and are, for example, preferably at least one selected from water-soluble inorganic sulfates such as magnesium sulfate, sodium sulfate, etc., water-soluble inorganic chlorides such as sodium chloride, magnesium chloride, etc., and water-soluble inorganic carbonates such as sodium carbonate, etc. From the viewpoint of preventing changes in the quality of the fragrance, the component (A) may be, for example, preferably a water-soluble inorganic sulfate, more preferably magnesium sulfate.
[0015] 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, the component (A) can be prepared by drying a water-soluble solid carrier having a moisture content of more than 20% by mass as measured by 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 such as magnesium sulfate and sodium sulfate (preferably water-soluble inorganic sulfates having water of crystallization), and water-soluble inorganic chlorides such as sodium chloride and magnesium chloride (preferably water-soluble inorganic chlorides having water of crystallization). 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.
[0016] In addition, from the viewpoint of further increasing the strength of the fragrance delivery particles and from the viewpoint of storage stability, component (A) may 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.
[0017] 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 an infrared moisture meter is, 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, 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, even more preferably 15% by mass or less.
[0018] 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, for example, from the viewpoint of improving the quality of the fragrance, be 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, still more preferably 8% by mass or more, and from the same viewpoint, be preferably 20% by mass or less, more preferably 18% by mass or less, even more preferably 15% by mass or less, and still more preferably 14% by mass or less.
[0019] 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 (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)
[0020] In addition, the component (A) can be prepared, for example, by drying a water-soluble solid. In one embodiment of the component (A), a water-soluble solid having a moisture content of more than 20% by mass as measured by an infrared moisture meter may be dried to adjust the moisture content as measured by the infrared moisture meter to a range of 0.1% by mass to 20% by mass.
[0021] From the standpoint of solubility, the content of component (A) may, for example, be 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.
[0022] <(B) component> The fragrance of component (B) is, for example, (B1) a fragrance encapsulated in a microcapsule [hereinafter component (B1)] and (B2) a fragrance not encapsulated in a microcapsule [hereinafter component (B2)].
[0023] The fragrance here is not particularly limited as long as it is one or more selected from fragrances and fragrance precursors. As the fragrance, for example, fragrance compounds described in Motoki Nakajima, "Fundamentals of Fragrance and Fragrance Preparation," 4th edition, Sangyo Tosho Co., Ltd., April 20, 2005, and fragrance compounds known to be blended in fabric softeners through patent documents and the like can be used. The fragrance compound may be a single one or a mixture of two or more kinds. In addition, as the fragrance compound, a fragrance component or a fragrance composition prepared by a fragrance manufacturer can be used. The fragrance may be a single one of the fragrance compounds or a fragrance composition mixed with two or more kinds of the fragrance compounds, and the fragrance composition may contain a fragrance diluent or a solvent in addition to the fragrance compound. In addition, a fragrance precursor can be used as the fragrance.
[0024] 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, even more preferably 5.0 or less. If the ClogP value is within such a range, the support and retention on component (A) will be good. 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 inside of component (A), preferably the inner surface of pores that connect the outer surface to the inside of component (A) [also referred to as the inner pores of component (A)]. In addition, the term "support / retention" used herein means that when component (B) is supported on component (A), the encapsulated component (B), preferably component (B1) or component (B2), suppresses evaporation or leakage (leakage).
[0025] Here, the logP value is the logarithm of the 1-octanol / water partition coefficient of a compound, and means the ratio of the equilibrium concentration of a solute in each solvent at the 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 "logP" to the base 10. The logP value can be calculated using the program "CLOGP" (DaylightCIS) or the like. 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, PG Sammes, JB Taylor and CARamsden,Eds.), p.295, Pergamon Press, 1990", and is the ClogP value calculated by the program CLOGPv4.01. When a fragrance mixture contains multiple fragrances, the ClogP value of the fragrance mixture can be calculated by multiplying the ClogP value of each fragrance by its volume ratio in the fragrance mixture and taking the sum of the results.
[0026] From the viewpoint of the support and retention of component (B2) on component (A), the fragrance compound that can be used in component (B) preferably has 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, with a contact angle meter "DropMaster DM-501" (product name, manufactured by Kyowa Interface Science Co., Ltd.).
[0027] Examples of fragrance compounds that can be used in component (B) include the following fragrance compounds, where 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), bromelain (4.0), benzyl salicylate (4.0), benzyl acetate ... -geonal (3.9), ot-butylcyclohexyl acetate (4.4), pt-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-damascone (4.3), β-damascone (4.4), δ-damascone (4.2), decanane (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), Fructose (registered trademark) (3.6), geraniol (3.5), geranyl acetate (4.5), geranyl nitrile (3.9), hexyl cinnamic alginate (3.6), Dehyde (4.8), hexyl acetate (4.8), hexyl salicylate (5.1), cis-3-hexenyl salicylate (4.8), Iso E Super (5.2), alpha-ionone (3.9), beta-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), nerolin yara yara (3.3), γ-nonalactone (2.1), nonanal (3.3), octanal (2.8), phenylhexanol (3.5), propan-2-yl-2-methylbutanoate (2.7), sandalwood core (registered trademark) and one or more fragrance compounds selected from the following: tetrahydrolinalool (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).
[0028] Examples of the fragrance precursor that can be used in the component (B) include compounds that react with water to release fragrance components, compounds that react with light to release fragrance components, etc. Examples of the compound that reacts with water to release fragrance components include silicate ester compounds having an alkoxy component derived from fragrance alcohol, fatty acid ester compounds having an alkoxy component derived from fragrance alcohol, acetal compounds or hemiacetal compounds obtained by reacting a carbonyl component derived from fragrance aldehyde or fragrance ketone with an alcohol compound, Schiff base compounds obtained by reacting a carbonyl component derived from fragrance aldehyde or fragrance ketone with a primary amine compound, and hemiaminal compounds or hydrazone compounds obtained by reacting a carbonyl component derived from fragrance aldehyde or fragrance ketone with a hydrazine compound. Examples of compounds that release fragrance components 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 the reaction product of some carboxy groups of polyacrylic acid with a fragrance alcohol.
[0029] There are no particular limitations on the component (B1) 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 the textile product, and after drying, the capsules are broken by applying a stimulus such as rubbing, releasing the fragrance. Therefore, by blending the component (B1) in the present invention, the persistence of the fragrance of the textile product can be improved.
[0030] The preparation method of the perfume microcapsules is not particularly limited, and known microencapsulation methods can be used.Specific examples include chemical methods (interfacial polymerization method, insitu polymerization method, orifice method), physicochemical methods (coacervation method), mechanical and physical methods (air suspension coating method, spray drying method, high-speed air current impact method), etc.The outer shell of the perfume microcapsules can be, for example, various polymer compounds such as polyurethane, polyamide, melamine resin, urea resin, alginate, gelatin, gum arabic, starch, etc., as well as inorganic compounds such as silica.
[0031] More specifically, the method for producing perfume microcapsules may be described in "Making + Using Microcapsules" (Koishi Masumi et al., Kogyo Chosakai, published in 2005), JP 2008-63575 A, JP 2006-249326 A, JP 2006-518790 A, JP 11-216354 A, JP 5-222672 A, etc. A preferred method for producing perfume microcapsules includes a method in which an emulsifier such as ethylene-maleic anhydride copolymer, a perfume, and an optional diluent or solvent are dispersed in water to obtain an emulsion, and then a wall material such as melamine-formaldehyde resin is added to the emulsion and stirred to obtain a slurry of perfume microcapsules. Another example is a method in which a monomer that will become the resin that will form the wall material is mixed with an emulsifier such as isobutylene-maleic anhydride copolymer or acrylic acid-acrylamide copolymer in water to prepare a wall material-emulsifier mixture, and then this wall material-emulsifier mixture is emulsified with fragrance and an optional diluent or solvent, and formaldehyde is added to the emulsion and stirred to obtain a slurry of fragrance microcapsules.
[0032] In 100% by mass of the slurry containing the fragrance microcapsules obtained by the above-mentioned method for producing fragrance microcapsules, the content of the fragrance compound 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 blending amounts when the fragrance-encapsulating microcapsules are prepared.
[0033] In 100% by mass of the slurry containing the component (B1), the content of the perfume-containing 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 the 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 the perfume-containing microcapsules blended when they are prepared.
[0034] The water content in 100% by mass of the slurry containing the 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 perfume 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 the perfume microcapsules containing the component (B1).
[0035] 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.
[0036] 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 the (B1) component 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 the (B1) component can be measured, for example, using a laser diffraction / scattering type particle size distribution measuring device "LA-950" (manufactured by HORIBA, Ltd.).
[0037] The component (B2) is, for example, a fragrance not incorporated in the microcapsules (also called an external fragrance), and may be one or more selected from the fragrance compounds described above, or may be a fragrance composition containing two or more of them. Also, it may be the same as the fragrance compound encapsulated in the fragrance-encapsulating microcapsules, which are the component (B1).
[0038] The content of the (B1) component 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, based on 100% by mass of the perfume delivery particle of the present invention. The content may be the content of the perfume compound encapsulated as an effective amount (which may be the blend amount of the perfume compound when preparing the (B1) component) as the content of the (B1) component. For example, it may be based on the blend amount of the slurry containing the (B1) component when producing the perfume delivery particle of the present invention.
[0039] The content of the (B2) component 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, 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 particle of the present invention. These contents may be based on the blending amount when producing the perfume delivery particle of the present invention.
[0040] 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, 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, 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 blend amount of the fragrance compound when preparing the (B1) component). For example, it may be based on the blend amount of the slurry containing the (B1) component when producing the fragrance delivery particle of the present invention. Also, the content of the (B2) component may be based on the blend amount when producing the fragrance delivery particle of the present invention.
[0041] The (B) component 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, based on 100% by mass of the (B) component, from the viewpoint of promoting the support and retention of the (B2) component inside the pores of the (A) component and from the viewpoint of stability (such as suppression of volatilization and exudation of the fragrance ((B2) component) supported and retained in the (A) component during particle storage), and from the viewpoint of the intensity of the fragrance, it may be 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., selected from alcohols, glycols, and esters having 1 to 10 carbon atoms, glycols, and esters having 6 to 20 carbon atoms, other than fragrance compounds. Specifically, examples of alcohols include methanol, ethanol, and glycerin; examples of glycols include ethylene glycol, diethylene glycol monoethyl ether, propylene glycol, dipropylene glycol, dipropylene glycol monoethyl ether, and 3-methoxy-3-methylbutanol; examples of esters include diethyl phthalate, isopropyl myristate, benzyl myristate, triethyl citrate, diisobutyl adipate, and hydrogenated methyl abietic acid; and examples of paraffins include liquid paraffin and isoparaffin.
[0042] In terms of the aroma release by friction, the mass ratio of the content of the (A) component to the content of the (B1) component [(B1) / (A)] of the fragrance delivery particle of the present invention 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, it may be preferably 0.20 or less, more preferably 0.15 or less, even more preferably 0.10 or less. Here, the aroma release by friction refers to the aroma release after rubbing a dry cloth. 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 blend amount of the fragrance compound when preparing the (B1) component). For example, it may be based on the blend amount of the slurry containing the (B1) component when producing the fragrance delivery particle of the present invention. Also, the content of the (B2) component may be based on the blend amount when producing the fragrance delivery particle of the present invention.
[0043] In the perfume delivery particle of the present invention, from the viewpoint of further increasing the strength of the perfume delivery particle and from the viewpoint of the fragrance intensity immediately after dehydration, the mass ratio of the content of the (A) component to the content of the (B2) component [(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 the perfume delivery particle of the present invention is produced.
[0044] 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, for example, preferably 0.3 mass% or more, more preferably 0.5 mass% or more, even more preferably 1.0 mass% or more, and preferably 5.0 mass% or less, more preferably 4.0 mass% or less, as a solid form. <Composition, etc.>
[0045] The moisture content of the fragrance delivery particles of the present invention by Karl Fischer vaporization method (JIS K 0113) [hereinafter referred to as KF moisture content] is 1% by mass or more, and from the viewpoint of the strength of the obtained fragrance delivery particles, it may be, for example, preferably 3% by mass or more, more preferably 5% by mass or more, even more preferably 8% by mass or more, still more preferably 10% by mass or more, still more preferably 20% by mass or more, and 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. The moisture content of the fragrance delivery particles of the present invention by Karl Fischer vaporization method (JIS K 0113) can be measured by the method described in the Examples.
[0046] Although the mechanism of action of the present invention is not clear, the present inventors speculate as follows. The present inventors discovered a phenomenon in which the perfume-containing microcapsules of the component (B1) break when the components (B1) and (B2) are stored in contact with each other. For this reason, when the components (B1) and (B2) are mixed in a normal manner and supported on the water-soluble solid of the component (A), the capsules break down and do not adhere to the clothes after washing / rinsing, and the capsule effect is not obtained. The component (B2) supported and held inside the pores of the component (A) exists inside the component (A). On the other hand, the component (B1) does not easily enter the pores of the component (A), and further, by mixing the component (D) and the component (B1) in advance, the component (B1) is supported and held near the surface of the component (A), and the stability of the component (B1) can be improved. If the KF moisture content of the fragrance delivery particles is low, the strength of the fragrance delivery particles decreases and storage stability is impaired, whereas if the KF moisture content is high, the supported and held fragrance of component (B2) seeps out onto the surface of component (A), causing the capsule (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 adsorption efficiency to textile products can be optimized.
[0047] The perfume delivery particles of the present invention are not particularly limited, but may be preferably spherical, granular or powdery, with spherical being preferred from the standpoint of appearance and ease of use.
[0048] From the viewpoint of solubility and handling, 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 spherical equivalent diameter of 250 particles using image analysis software ImageJ.
[0049] From the viewpoint of more easily obtaining the effects of the present invention due to the difference 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 spherical equivalent diameter of 250 particles using image analysis software ImageJ.
[0050] From the viewpoint of the volume during use, the perfume delivery particle 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, and from the viewpoint of ease of use and solubility during use, a bulk density of preferably 1000 g / L or less, more preferably 800 g / L or less. The bulk density can be measured, for example, by a bulk specific gravity measuring device according to JIS K7365.
[0051] In one embodiment, the perfume delivery particle of the present invention is preferably one in which the water-soluble solid of component (A), preferably a water-soluble inorganic salt, supports or retains component (B).
[0052] <(C) component> In order to promote the adsorption of component (B1) to textile products, the fragrance delivery particles of the present invention may further contain, for example, (C) one or more types selected from water-soluble cationic polymeric compounds and cationic surfactants (hereinafter, component (C)).
[0053] 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), 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, cationized locust bean gum, and the like. Among these, preferably, one or more selected from polydiallyldimethylammonium chloride and its copolymer poly(diallyldimethylammonium chloride), poly(acrylic acid-co-diallyldimethylammonium chloride), and poly(acrylamide-co-acrylic acid-co-diallyldimethylammonium chloride) are used, and more preferably, one or more selected from poly(acrylamide-co-diallyldimethylammonium chloride) and poly(diallyldimethylammonium chloride).
[0054] Examples of the cationic surfactant include alkylamine salts and alkyl quaternary ammonium salts.
[0055] The alkylamine salt may be, for example, preferably a salt of a secondary amine or a tertiary amine, 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, that is, a methyl group. Examples of the alkylamine salt include alkylamine salts such as long-chain monoalkyl monomethyl secondary amine salts and long-chain monoalkyl dimethyl tertiary amine salts, in which the long-chain alkyl group is in the above-mentioned carbon number range. Examples of the long-chain monoalkyl dimethyl tertiary amine salts include alkylamine acetates such as lauryl dimethylamine acetate and stearyl dimethylamine acetate.
[0056] 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, that is, a methyl group. Examples of the alkyl quaternary ammonium salt include long-chain alkyl tri-short-chain alkyl quaternary ammonium salt, di-long-chain alkyl di-short-chain alkyl quaternary ammonium salt, and long-chain alkyl benzyl di-short-chain alkyl quaternary ammonium salt, in which the long-chain alkyl group and the short-chain alkyl group are each in the above-mentioned carbon number range. 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; 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 dialkyl dimethyl ammonium chlorides such as distearyl dimethyl ammonium chloride; and dialkyl 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.
[0057] Among these, the cationic surfactant is, for example, preferably an alkyl quaternary ammonium salt, more preferably an alkyltrimethylammonium salt having an alkyl group having from 10 to 22 carbon atoms, even more preferably an alkyltrimethylammonium chloride having an alkyl group having from 10 to 22 carbon atoms, still more preferably one or more selected from lauryltrimethylammonium chloride, stearyltrimethylammonium chloride, and cetyltrimethylammonium chloride, and even more preferably cetyltrimethylammonium chloride.
[0058] When the perfume delivery particle of the present invention contains 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 particle of the present invention, from the viewpoint of promoting the adsorption of the (B1) component to the textile product. These contents may be based on the blending amount when the perfume delivery particle of the present invention is produced. Moreover, the above contents do not include the cationic surfactant in the present invention.
[0059] When the perfume delivery particle of the present invention contains 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 particle of the present invention, from the viewpoint of promoting the adsorption of the (B1) component to the textile product. The content may be based on the amount of the compounding when the perfume delivery particle of the present invention is produced. The mass of the cationic surfactant is used as a value converted to a chlorine salt.
[0060] <(D) component> The fragrance delivery particle of the present invention may further contain, for example, a water-soluble nonionic polymer (D) [hereinafter, component (D)] from the viewpoint of the strength, solubility, and stability of the resulting fragrance delivery particle (such as suppression of volatilization and exudation of the fragrance (component (B2)) supported and held by component (A) during particle storage). Component (D) may, for example, be preferably polyethylene glycol (PEG), polypropylene glycol, polyoxyethylene alkyl ether, or polyoxyethylene phenol ether, more preferably polyethylene glycol or polypropylene glycol. Furthermore, the number average molecular weight of component (D) may be, for example, preferably 2000 or more, more preferably 3000 or more, even more preferably 4000 or more, and preferably 20000 or less, more preferably 15000 or less, and even more preferably 10000 or less, as measured by GPC method using polystyrene as the standard, from the viewpoint of the strength, solubility, and stability of the resulting fragrance delivery particle (such as suppression of volatilization and exudation of the fragrance (component (B2)) supported and held by component (A) during particle storage). When measuring the molecular weight of polyethylene glycol, water / ethanol is used as the solvent.
[0061] When the fragrance delivery particle of the present invention contains component (D), the content of component (D) may be, 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 particle, from the viewpoint of the strength, solubility, and stability of the resulting fragrance delivery particle (such as suppression of evaporation and exudation 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 particle 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 above content may be based on the amount blended when producing the fragrance delivery particle of the present invention.
[0062] 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, for example, 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, even more preferably 7.0 or more from the viewpoint of solubility, and from the viewpoint of product stability (such as suppression of volatilization and exudation of the fragrance (component (B2)) supported / held in 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.
[0063] <(E) component> The perfume delivery particle of the present invention may further contain, for example, (E) an oxidation stabilizer (hereinafter referred to as (E) component). As the oxidation stabilizer, for example, an antioxidant such as butyl hydroxytoluene (BHT), butyl hydroxyanisole (BHA), distyrenated cresol, sodium sulfite, and sodium hydrogen sulfite can be used.
[0064] When the perfume delivery particle of the present invention contains the (E) component, the content of the (E) component 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 of the perfume delivery particle of the present invention when it is produced.
[0065] The fragrance delivery particle 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 support and retention of the (B2) component inside the pores of the (A) component, and from the viewpoint of stability (such as suppressing the evaporation and seepage of the fragrance ((B2) component) supported and retained in the (A) component during particle storage). When the fragrance delivery particle of the present invention contains an organic solvent, it may be the same as the organic solvent optionally contained in the (B) component, and may be, for example, 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 particle of the present invention. The above range may include the organic solvent optionally contained in the (B) component.
[0066] Method for making perfume delivery particles The perfume delivery particle of the present invention can be obtained, for example, by mixing the (A) component and the (B) component. That is, the present invention provides a method for producing a perfume delivery particle by mixing the (A) component, the (B1) component, and the (B2) component. Specific examples and preferred examples of the (A) component and the (B) component may be the same as those of the perfume delivery particle of the present invention described above. From the viewpoint of adjusting the moisture content of the perfume delivery particle of the present invention, for example, the (A) component may be one that has been dried in advance and adjusted to a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter, and a water-soluble solid having a moisture content of more than 20% by mass as measured by an infrared moisture meter may be dried and adjusted to a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter.
[0067] The water content of the water-soluble solid can be adjusted by drying the component (A) using, for example, an electric dryer (shelf drying), fluidized bed drying, reduced pressure drying, microwave drying, etc. From the viewpoint of suppressing the collapse 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.
[0068] The drying process may be either a batch type or a continuous type, and is not particularly limited. For example, the batch type may be, for example, a drying method using an electric shelf dryer or a hot air dryer, or a drying method using a batch type fluidized bed, and for example, the continuous type may be, for example, a fluidized bed, a vibration fluidized bed, a rotary dryer, a steam tube dryer, etc.
[0069] 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 the following drying times.
[0070] 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 even more preferably 130° C. or lower.
[0071] 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.
[0072] The water-soluble solid may be, for example, compressed in advance into granules, flakes, or beads, and then dried. The molding method may be a known method. For example, the compression molding method, the extrusion granulation method, the rolling granulation method, the stirring granulation method, and the compaction granulation method may be used. Among these, for example, the compression molding method is preferable.
[0073] When compressing a water-soluble solid, the manufacturing machine to be used is not limited as long as it can produce, for example, briquettes or tablets, and well-known briquette machines, tablet presses, etc. can be used. A briquette machine is a device in which two rolls, on the periphery of which pockets that serve as the matrix of the desired compressed product are engraved, feed granulated material between the rolls that rotate at the same speed while biting into each other, and continuously compress and mold the material. As a well-known briquette machine, for example, a briquetting machine (manufactured by Shinto Kogyo Co., Ltd.) can be used. A tablet press is a device in which a granulated material is filled in a mortar and compressed between a lower punch and an upper punch to mold the material. Tablet presses include a single-shot tablet press in which a pair of upper and lower punches move up and down in a single mortar to compress the material, and a rotary tablet press in which mortars are embedded at equal intervals on 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 a well-known tablet press, for example, a single punch tablet press manufactured by Riken Co., Ltd. can be used, and as a rotary tablet press, for example, a tablet press manufactured by Kikusui Chemical Co., Ltd. can be used.
[0074] When molding is performed by a method other than compression molding, for example, well-known extrusion granulators such as Pelleter Double, Dome Gran, Twin Dome Gran, Disk Pelleter (Dalton Co., Ltd.), basket type granulator (Kikusui Seisakusho Co., Ltd.), etc., as well as rolling granulators, etc. can be used. After molding, granulation can be performed as necessary. As a machine used for granulation, well-known pulverizers (or crushers) can be used, for example, Marmerizer (Dalton Co., Ltd.), Fitz Mill (Dalton Co., Ltd.), Power Mill (Powrex Co., Ltd.), Comil (Quadro), etc. can be used.
[0075] In one embodiment of the perfume delivery particle of the present invention, the perfume delivery particle can be produced by mixing a mixture obtained by mixing the (A) component and the (B2) component with the (B1) component. In another embodiment of the perfume delivery particle of the present invention, the perfume delivery particle can be produced by mixing a mixture obtained by mixing the (A) component and the (B2) component with a mixture obtained by mixing the (B1) component and the (D) component. By mixing the (A) component and the (B2) component in advance, and mixing the mixture obtained by mixing the (B1) component and the (D) component with the (A) component and the (B2) component in a state in which the (B2) component is supported and held inside the (A) component, the mixture of the (B1) component and the (D) component can be supported and held on the surface of the (A) component, and the stability of the perfume delivery particle supporting and holding the (B1) component can be improved.
[0076] In addition, as another embodiment of the perfume delivery particle of the present invention, the perfume delivery particle can be produced by mixing the mixture obtained by mixing the (A) component and the (B1) component with the (B2) component. In addition, as another embodiment of the perfume delivery particle of the present invention, the perfume delivery particle can be produced by mixing the mixture obtained by mixing the (A) component and the (B1) component with the mixture obtained by mixing the (B2) component and the (D) component. By mixing the mixture obtained by mixing the (B2) component and the (D) component with the mixture of the (A) component and the (B1) component, the mixture of the (B2) component and the (D) component can be supported and held on the surface of the (A) component, and the stability of the perfume delivery particle supporting and holding the (B2) component can be improved. As the mixture obtained by mixing the (A) component and the (B1) component, a mixture obtained by mixing the (A) component with a slurry containing the (B1) component can also be used.
[0077] In another embodiment, the perfume delivery particle of the present invention can be produced by dividing the component (A) and mixing it stepwise. Specifically, the production method includes the following steps (i) to (iii).
[0078] Step (i) A step of mixing a part of the component (A) with the component (B2) to obtain a mixture. Step (ii) mixing the mixture obtained in step (i) with the remaining component (A); Step (iii) mixing the mixture obtained in step (ii) with component (B1) to produce perfume delivery particles.
[0079] 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) and (B1) components (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 the perfume-containing particles containing the (A) and (B1) components, depending on the situation.
[0080] 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, for example, be 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 components.
[0081] When the perfume delivery particle of the present invention is produced by mixing the (A) component step by step, the mixed liquid added in step (iii) is considered to be uniformly distributed in a part of the (A) component in step (i), the mixture of the (B2) component and the optional (E) component, and the remaining part of the (A) component in step (ii). Therefore, the content ratio of the perfume delivery particle in the obtained mixed particle can be calculated by calculating the ratio of the amount (active component) of the step (i) in the total amount of the amount (active component) of the step (i) and the amount (active component) of the step (ii), and multiplying the ratio by the amount (active component) of the mixed liquid added in step (iii).
[0082] 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.
[0083] When the (A) component is mixed in stages to produce the fragrance delivery particles of the present invention, the mass ratio of the remainder 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, be preferably 0.0033 or more, more preferably 0.0066 or more, and preferably 0.030 or less, more preferably 0.025 or less.
[0084] When the (A) component is mixed in stages to produce the fragrance delivery particles of the present invention, the mass ratio of a portion of the (A) component mixed in step (i) to the remainder 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.
[0085] Another embodiment of the fragrance delivery particles of the present invention includes a method in which component (A) is divided and mixed in stages to produce fragrance delivery particles, specifically, a method of producing the fragrance delivery particles by the following steps (i') to (iii').
[0086] Step (i'): A step of mixing a part of the component (A) with the component (B1) to obtain a mixture. Step (ii'): mixing the mixture obtained in step (i') with the remaining component (A). Step (iii'): mixing the mixture obtained in step (ii') with component (B2) to produce perfume delivery particles.
[0087] 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) and (B2) components (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) and (B2) components, depending on the situation.
[0088] In addition, 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 100 / 10 or less, more preferably 80 / 20 or less, and even more preferably 70 / 30 or less.
[0089] Furthermore, when using mixed particles containing the fragrance delivery particles of the present invention and fragrance-containing particles, 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, still more preferably 10% by mass or more, even more preferably 20% by mass or more, and 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.
[0090] The preferred range of the mass ratio [step (i') / step (ii')] of the part of the blend amount of component (A) mixed in step (i') to the remainder of the blend amount of component (A) mixed in step (ii') may be the same as the above-mentioned mass ratio [step (i) / step (ii)].
[0091] In addition, as another embodiment, the perfume delivery particle of the present invention can be produced by further mixing a mixture obtained by mixing the (A) component with the (B2) component and the (E) component, and a mixture obtained by mixing the (B1) component with the (C) component and the (D) component, from the viewpoint of suppressing the volatilization of the (B2) component and the fragrance stability. In addition, as another embodiment, the perfume delivery particle of the present invention can be produced by further mixing a mixture obtained by mixing the (A) component with the (B2) component with the (C) component and the (D) component, and a mixture obtained by mixing the (B1) component with the (E) component, from the viewpoint of suppressing the leakage of the encapsulated components of the (B1) component.
[0092] In addition, as 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 standpoint of preventing leakage of the encapsulated components of component (B1), the strength of component (A), and the storage stability of component (B1).
[0093] The mixer for the component (A), the component (B), and any optional components is not particularly limited as long as they can be mixed substantially uniformly, and may be a mixer having a heating means. Examples of the 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 Machinery Works, Ltd.), a ribbon blender (manufactured by Hosokawa Micron Corporation), and a container rotation type granulator (manufactured by Sugiyama Heavy Industries, Ltd.).
[0094] When mixing the (A) component, the (B) component, and the optional components, it is preferable to use, for example, a container rotation type granulator so that the (A) component does not collapse due to strong shearing. As the container rotation type granulator, for example, a drum type granulator and a pan type granulator are preferable. As the drum type granulator, there is no particular limitation as long as the drum-shaped cylinder rotates to perform processing. A horizontal or slightly inclined drum type granulator can also be used. These devices may be, for example, either a batch type or a continuous type. In addition, when the wall friction coefficient between the (A) component and the inner wall of the container rotation type granulator is small and it is difficult to apply a sufficient upward motive force to the powder, it is preferable to provide, for example, a plurality of baffles (baffles) on the inner wall of the container to assist mixing. By providing the baffles, it is possible to impart an upward motive force to the powder, improving powder mixability and solid-liquid mixability.
[0095] The operating conditions of the container-rotating granulator are not particularly limited as long as the water-soluble solid in the granulator can be flowed and stirred as uniformly as possible. From the viewpoint of obtaining granules having good disintegration strength, the Froude number defined by the following formula (1) can be, for example, preferably 0.01 or more, more preferably 0.05 or more, and even more preferably 0.09 or more, and from the viewpoint of obtaining non-compacted granules, the upper limit can be 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.
[0096] Froude number: Fr=V 2 / (R×g) (1) V: Circumferential speed [m / s] R: Radius from the center of rotation to the circumference of the rotating object [m] g: Gravitational acceleration [m / s 2 ]
[0097] In addition, in a drum type granulator or a pan type granulator in which granulation progresses by the rotation of the main body barrel, for example, V and R are the values of the main body barrel, in a horizontal or vertical type 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.
[0098] The mixing temperature may be, for example, preferably 20°C or higher, more preferably 30°C or higher, from the viewpoint of fluidity and handleability, and preferably 60°C or lower, more preferably 50°C or lower, from the viewpoint of the volatilization stability of the (B2) component.
[0099] From the viewpoint of uniform mixing, the rotation speed of the mixer may be, for example, preferably 10 rpm or more, more preferably 20 rpm or more, and from the viewpoint of suppressing disintegration of water-soluble solids, it may be preferably 100 rpm or less, more preferably 50 rpm or less.
[0100] 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.
[0101] When mixing the (A) component and the (B) component, for example, the (B) component may be dropped from a pipe using a pump, or may be supplied using a nozzle. As the nozzle, for example, a one-fluid nozzle or a multi-fluid nozzle may be used for supply. By using a multi-fluid nozzle, the (B) component 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. In addition, the mixing section of the flavoring and the atomization gas may be, for example, either an internal mixing type in which mixing is performed within the nozzle tip, or an external mixing type in which mixing is performed 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.
[0102] When the multi-fluid nozzle is used to supply the component (B) to the component (A), the supply temperature may be, for example, preferably 20° C. or more, more preferably 30° C. or more, from the viewpoint of fluidity and handleability, and preferably 60° C. or less, more preferably 50° C. or less, from the viewpoint of the volatilization stability of the component (B2).
[0103] 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 / min or more, more preferably 5 parts by mass / min or more, and preferably 20 parts by mass / min or less, more preferably 15 parts by mass / min or less, per 100 parts by mass of the component (A).
[0104] 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, which comprises adding the perfume delivery particles to the textile products in the washing process of the textile products to treat the textile products.
[0105] When the perfume delivery particles of the present invention are added in the washing process of textile products, the amount of perfume delivery particles of the present invention 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 products. The textile products may be treated with only the perfume delivery particles of the present invention, or may be treated with a textile treatment composition containing the perfume delivery particles of the present invention.
[0106] When the perfume delivery particles of the present invention are added in the washing process of a textile product, the perfume delivery particles of the present invention can be added to at least one of the washing water and the rinsing water of the laundry, and the perfume delivery particles of the present invention can also be added to both the washing water and the rinsing water of the laundry.
[0107] When the perfume delivery particles of the present invention are added in the washing process of textile products, for example, the perfume delivery particles are added to water at a concentration of 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 to a washing machine, it is preferable to use it in washing water, but it is also possible to add it to rinsing water. The washing water and rinsing water of washing may contain a textile washing detergent component. EXAMPLES
[0108] 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 composition in Tables 3 to 7 indicates the mass% of the actual product (for the fragrance microcapsule slurry, the mass% of the amount of fragrance compound encapsulated as an effective amount). The physical properties were measured by the following methods.
[0109] (1) Bulk density Calculated using a bulk density measuring device in accordance with JIS K7365.
[0110] (2) Average particle size of the fragrance-delivering particles The spherical equivalent diameter of 250 particles was calculated using the image analysis software ImageJ.
[0111] (3) Moisture content of fragrance delivery particles The KF moisture content of the perfume delivery particles was measured by the Karl Fischer vaporization method (JIS K 0113). The HIRANUMA automatic moisture measurement device AQV-2200A (manufactured by Hitachi High-Tech Corporation) was used as the moisture measurement device. 50 mL of dehydrated methanol was placed as a titration solvent in a titration tank with a capacity of about 150 mL of the moisture measurement device and stirred with a magnetic stirrer. An inlet pipe for introducing the moisture vaporized from the moisture vaporizer was placed in the dehydrated methanol (product name: dehydrated methanol (manufactured by Katayama Chemical Industry 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 anhydrous methanol, and 2.5 ml of the commercially available Karl Fischer reagent Aqualite KF5 (manufactured by HIRANUMA Corporation, titer 5.0 mg / mL) was added dropwise to make the titration tank anhydrous. 0.05g of each fragrance delivery particle was weighed out and placed in a sample heating boat of a moisture vaporizer EV-2000 (Hitachi High-Tech Corporation), which was heated at 210°C for 2 minutes to vaporize the moisture of the fragrance delivery particle, and introduced into anhydrous methanol in a titration tank of a HIRANUMA automatic moisture measurement device AQV-2200A (Hitachi High-Tech Corporation) with a carrier gas (nitrogen) of 200mL / min. This was titrated using Karl Fischer reagent Aqualite KF5 (HIRANUMA Corporation) to measure the amount of vaporized moisture. In addition, the same measurement as above was performed three times using the same sample to measure the amount of moisture. The amount of vaporized moisture was also calculated using the following formula. W = F x V x 100 / (S x 103) W: Moisture (%) F: Karl Fischer reagent titer (mg / mL) V: Amount of Karl Fischer reagent used in titration (mL) S: mass of sample (g)
[0112] [Ingredients 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 Advantech Toyo low-temperature blower 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 (A1) above) was dried in a fluidized bed dryer (Okawahara Manufacturing Slit Flow) with 120°C hot air at 4 m 3 / min for 25 minutes (5.1% by mass moisture content measured by infrared meter, bulk density 590g / L) (A3): Magnesium sulfate heptahydrate (the same as (A1) above) was dried in a fluidized bed dryer (Okawahara Manufacturing Slit Flow) with 120°C hot air at 4 m 3 / min for 15 minutes (16.4% by mass moisture content measured by infrared meter, bulk density 650g / L) (A4): Magnesium sulfate heptahydrate (the same as (A1) above) was dried in a fluidized bed dryer (Okawahara Manufacturing Co., Ltd. Slit Flow) with 120°C hot air at 4 m 3 / min for 5 minutes (water content measured by infrared meter: 26.0% by mass, bulk density: 730 g / L) (A5): 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)
[0113] The water contents of the above (A1) to (A5) were calculated by the following method. 2 g of sample (water-soluble solid) was weighed into an aluminum container with a diameter of 11.5 cm. After that, the mass of the sample (component (A)) after drying was measured using an infrared moisture meter (Shimadzu Corporation, MOC63u) in the moisture standard moisture measurement mode at a temperature of 105°C under Auto conditions (when the change in the measured value became within 0.05% in 30 seconds, it was considered to be the final measured value and the measurement was terminated). The moisture content was calculated using the following formula. Moisture content (mass%) = {mass before drying (g) - mass after drying (g)} / mass before drying (g)
[0114] <(B) component> (B1) Component: (B1-1) Fragrance microcapsule slurry obtained in the following production example 1.7 g of diisobutylene-maleic anhydride copolymer (Demol EP, solid content 25%, Kao Corporation) was neutralized with hydrochloric acid, and then further diluted with ion-exchanged water to obtain an aqueous solution with a solid 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, emulsified using a homomixer, and heated to 50°C. Next, an aqueous solution in which 12 g of partially methylolated melamine resin (trade name Cyme1385, solid content 80%, Cytec Industries Inc.) and 35 g of ion-exchanged water were mixed was dropped. This was kept at 50°C for 2 hours, further kept at 70°C for 1 hour, and further kept at 80°C for 3 hours to complete the encapsulation. After this, it was allowed to cool to obtain a fragrance microcapsule slurry with an average particle size of 7 μm and an active 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 performed at a concentration that showed a transmittance of around 90%, to determine the average particle size (median diameter).
[0115] [Table 1]
[0116] (B2) Ingredient: (B2-1) Fragrance composed of the fragrance compounds shown in Table 2 below
[0117] [Table 2]
[0118] (C) Component "Polyquaternium-7" (manufactured by Lubrizol Advanced Materials, Inc.) (D) Component ·PEG (polyethylene glycol, number average molecular weight 8500) (E) Component ·BHT (oxidation stabilizer, Fujifilm Wako Pure Chemical Industries, Ltd.)
[0119] Preparation of perfume delivery particles Example 1 The component (A1) (solid temperature of component (A1) 50°C) was charged into a 75L drum-type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 3, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixed liquid of components (B2) and (E) was added through a pipe in the amount shown in Table 3 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the formula (1)). Furthermore, the mixed liquid of components (B1), (C) and (D) was added through a pipe in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend 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.
[0120] Example 2 The component (A2) (solid temperature of component (A2) 50°C) was charged into a 75L drum-type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 3, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixed liquid of components (B2) and (E) was added through a pipe in the amount shown in Table 3 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the above formula (1)). Furthermore, the mixed liquid of components (B1), (C) and (D) was added through a pipe in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend 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.
[0121] Example 3 The (A3) component (solid temperature of (A3) component 50°C) was charged into a 75L drum type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 3, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixture of (B2) component and (E) component was added by piping in the amount shown in Table 3 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the above formula (1)). Furthermore, the mixture of (B1) component, (C) component and (D) component was added by piping in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend 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.
[0122] Example 4 In step (i), component (A1) (solid temperature of component (A1) 50°C) was charged in an amount of 1 / 2 of the composition shown in Table 3 into a 75L drum-type granulator (φ40cm×L60cm) equipped with a baffle plate, and while stirring under conditions of Froude number 0.118 / drum angle 12.6°, a mixture of components (B2) and (E) was added in an amount shown in Table 3 through a pipe and mixed for 30 seconds (mixture 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in formula (1)). In step (ii), the remaining 1 / 2 of the amount shown in Table 3 of component (A1) was further added to the mixture obtained in step (i) and mixed for 10 seconds. In step (iii), the mixture obtained in step (ii) was added with a mixture of the (B1), (C) and (D) components in the amount shown in Table 3 through a pipe and mixed for 3 minutes and 30 seconds (mixture 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5 kg (total blend amount). Through steps (i) to (iii), a mixture of perfume-delivering particles X containing the (A1), (B1) and (B2) components and perfume-containing particles Y containing the (A1) and (B1) components was obtained. The obtained mixture 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.
[0123] 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). 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.
[0124] Comparative Example 1 The (A4) component (solid temperature of (A4) component 50°C) was charged into a 75L drum type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 3, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixed liquid of (B2) component and (E) component was added by piping in the amount shown in Table 3 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the above formula (1)). Furthermore, the mixed liquid of (B1) component, (C) component and (D) component was added by piping in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend 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.
[0125] Comparative Example 2 Magnesium sulfate heptahydrate (component (A5)) was not dried and the amount shown in Table 3 was put into a 75L drum-type granulator (φ40cm×L60cm) with a baffle plate, and while mixing under the conditions of Froude number 0.118 / drum angle 12.6°, a mixed solution of components (B2) and (E) was added by 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=0.48m / s, R=0.2m in the above formula (1)). Furthermore, a mixed solution of components (B1), (C) and (D) was added by 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 6.5kg (total blend amount). The obtained perfume delivery particles were unable to sufficiently support the perfume, and the obtained particles were sticky. Furthermore, the KF moisture content of the obtained particles was forcibly measured and found to be 41.2% by mass.
[0126] <Fragrance Intensity Rating 1, 2, 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 28L of water (water temperature 25°C), and charged with 18.7g of commercially available unscented liquid detergent and 10.1g of the fragrance delivery particles of the present invention. Eight cotton towels and five cotton T-shirts (total dry weight of cotton towels and cotton T-shirts is 1.4kg) were washed for 9 minutes, rinsed twice, and dehydrated for 3 minutes. The scent intensity of the cotton towels immediately after dehydration and the cotton towels after drying for one day indoors (temperature 25°C, humidity 65%) were evaluated according to the following evaluation criteria. The scent intensity of the cotton towels immediately after dehydration was evaluated as 1, and the scent intensity of the dried cotton towels was evaluated as 2. In addition, the scent intensity of the cotton towels when the surface of the dried cotton towels was traced with two fingers was evaluated as 3. The evaluation was based on the average value of the evaluations by three expert panelists.
[0127] 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, and the fragrance intensity of the cotton towels was evaluated as a rating of 4, and the fragrance intensity of the cotton towels when the surface of the dried cotton towels was traced with two fingers was evaluated as a rating of 5. The evaluation results were the average value of the evaluations by three expert panelists. The evaluation results are shown in Table 3.
[0128] <<Evaluation criteria>> 0: Odorless 1: Very slightly felt 2: Feeling weak 3: I feel it clearly 4: I feel strongly 5: Feels quite strong 6: Feels very strongly
[0129] [Table 3]
[0130] It was confirmed that the perfume-delivery particles of Examples 1 to 4 were able to retain a large amount of perfume on textile products even after the washing and rinsing steps 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 storage for 20 days at 40°C, and it is predicted that the inclusion of fragrance-containing particles containing the (A1) and (B1) components in the mixed particles is effective in preventing leakage of the encapsulated components of the fragrance-encapsulated microcapsules.
[0131] Formulation examples 1-1~1-4 The component (A1) (solid temperature of component (A1) 50°C) was charged into a 75L drum-type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 4, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixed liquid of components (B2) and (E) was added through a pipe in the amount shown in Table 4 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the formula (1)). Furthermore, the mixed liquid of components (B1), (C) and (D) was added through a pipe in the amount shown in Table 4 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (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 used to carry out the same evaluations 1, 2, and 3 as in the Examples, high fragrance intensity was obtained in all cases.
[0132] [Table 4]
[0133] Formulation examples 2-1~2-3 [Ingredients used] The components used other than the following component (A) in Table 5 were the same as those used in the Examples. <Component (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 Advantech Toyo low-temperature blower dryer DRM620TE (moisture content measured by an infrared meter: 10.0% by mass, bulk density: 600 g / L)
[0134] The (A6) component (solid temperature of (A6) component 50°C) was charged into a 75L drum type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 5, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixed liquid of (B2) component and (E) component was added by piping in the amount shown in Table 5 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the above formula (1)). Furthermore, the mixed liquid of (B1) component, (C) component and (D) component was added by piping in the amount shown in Table 5 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend amount). The perfume delivery particles obtained in Formulation Examples 2-1 to 2-3 had a KF moisture content of 20 to 30% by mass. The perfume delivery particles obtained in Formulation Examples 2-1 to 2-3 were used to evaluate their solubility in 20°C Wakayama City water by the following method. The results are shown in Table 5.
[0135] <Solubility evaluation> 0.5 g of the perfume 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 according to the time required for complete dissolution using the following criteria. The results are shown in Table 5. Incidentally, "completely dissolved" refers to a state in which no solid components remain.
[0136] <<Evaluation Criteria>> ◎: Dissolved within 3 minutes after addition of fragrance delivery particles. ◯: Dissolved within 3 to 6 minutes after addition of the fragrance delivery particles. △: Dissolved within 6 to 9 minutes after addition of the fragrance delivery particles.
[0137] [Table 5]
[0138] Mixture Examples 3-1 to 3-3 (Table 6) and Mixture Examples 4-1 to 4-3 (Table 7) [Ingredients used] The components used in Tables 6 and 7 other than the following component (A) were the same as those in Examples and Formulation Examples 1 and 2. <Component (A)> (A7): Sodium sulfate decahydrate (product name: "Sodium sulfate decahydrate", Fujifilm Wako Pure Chemical Industries, Ltd., 0.1 to 5.0 mm columnar object, moisture content by infrared moisture meter: 56.6% by mass, bulk density: 711 g / L)) dried at 120°C for 4 hours using a constant temperature incubator made by Yamato Scientific Co., Ltd. (moisture content by infrared meter: 0.4% by mass, bulk density: 400 g / L to 800 g / L) (A8): Sodium carbonate decahydrate (product name: "Sodium carbonate decahydrate", Fujifilm Wako Pure Chemical Industries, 0.1-5.0 mm columnar object, moisture content by infrared moisture meter: 62.2% by mass, bulk density: 825 g / L)) dried at 120°C for 3 hours using a constant temperature incubator made by Yamato Scientific Co., Ltd. (moisture content by infrared meter: 15% by mass, bulk density: 400 g / L to 800 g / L)
[0139] The components (A6) to (A8) (solid temperature of components (A6) to (A8) 50°C) were charged into a 75L drum-type granulator (φ40cm×L60cm) with a baffle plate in the compositions shown in Tables 6 and 7, and mixed under the conditions of Froude number 0.118 / drum angle 12.6°. The mixed liquid of components (B2) and (E) was added through a pipe in the amount shown in Tables 6 and 7 and mixed for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the formula (1)). Furthermore, the mixed liquid of components (B1), (C) and (D) was added through a pipe in the amount shown in Tables 6 and 7 and mixed for 3 minutes and 30 seconds (mixed liquid 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend 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. In addition, the fragrance delivery particles obtained in Formulation Examples 3-1 to 3-3 and Formulation Examples 4-1 to 4-3 were used to evaluate the fragrance intensity and fragrance quality by the following method. The results are shown in Tables 6 and 7, respectively.
[0140] <Fragrance Intensity Rating 1, 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 28L of water (water temperature 25°C), and loaded with 18.7g of commercially available unscented liquid detergent and 10.1g of the fragrance delivery particles of the present invention. Eight cotton towels and five cotton T-shirts (total dry weight of cotton towels and cotton T-shirts is 1.4kg) were washed for 9 minutes, rinsed twice, and dehydrated for 3 minutes. The scent intensity of the cotton towels immediately after dehydration and the cotton towels after drying for one day indoors (temperature 25°C, humidity 65%) were evaluated according to the following evaluation criteria. The scent intensity of the cotton towels immediately after dehydration was evaluated as 1, and the scent intensity of the dried cotton towels was evaluated as 2. The evaluation results were the average value of the evaluations by three expert panelists.
[0141] <<Evaluation criteria>> 0: Odorless 1: Very slightly felt 2: Feeling weak 3: I feel it clearly 4: I feel strongly 5: Feels quite strong 6: Feels very strongly
[0142] <Fragrance quality rating 1, 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 28L of water (water temperature 25°C), and loaded with 18.7g of commercially available unscented liquid detergent and 10.1g of the fragrance delivery particles of the present invention. Eight cotton towels and five cotton T-shirts (total dry weight of cotton towels and cotton T-shirts is 1.4kg) were washed for 9 minutes, rinsed twice, and dehydrated for 3 minutes. The scent quality of the cotton towels immediately after dehydration and the cotton towels after drying for one day indoors (temperature 25°C, humidity 65%) were evaluated according to the following evaluation criteria. The scent quality of the cotton towels immediately after dehydration was evaluated as 1, and the scent quality of the dried cotton towels was evaluated as 2. The evaluation results were the average value of the evaluations by three expert panelists. Regarding the "fragrance balance" in the evaluation criteria below, good fragrance balance means that the fragrance is as designed and the quality of the fragrance is good, while poor balance means that the fragrance is different from the designed fragrance and therefore the quality of the fragrance is poor.
[0143] <<Evaluation criteria>> ◎: Very well balanced fragrance ○: Good balance of aromas △: The scent is slightly unbalanced. ×: Poorly balanced scent
[0144] [Table 6]
[0145] [Table 7]
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 Karl Fischer evaporation method (JIS K 0113), is 1% by mass or more and 35% by mass or less.
2. The perfume delivery particle of claim 1 , wherein component (A) is a water-soluble inorganic salt.
3. The perfume delivery particle according to claim 1 or 2, wherein component (A) is a water-soluble inorganic sulfate.
4. The perfume delivery particle according to claim 1 or 2, wherein the mass ratio [(B1) / (B2)] of the content of the component (B1) to the content of the component (B2) in the component (B) is 0.005 or more and 5.0 or less.
5. The perfume 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, 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 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.
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. The method for producing perfume delivery particles according to claim 6, further 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. The method for perfumery of claim 9, wherein the perfume delivery particles of claim 1 or 2 are added to at least one of wash water and rinse water during the washing process of the textile product.
Citation Information
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