Beneficial substance delivery particle
Patent Information
- Application Number
- JP2024158510
- 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
Smart Images

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Abstract
Description
[Technical field]
[0001] The present invention relates to benefit agent delivery particles, methods of making benefit agent delivery particles, and methods of perfuming textile products. [Background technology]
[0002] In recent years, research has been conducted into techniques for imparting beneficial substances having functions such as fragrance, bactericidal properties, germicidal properties, antibacterial properties, and UV protection properties to clothes using auxiliary ingredients other than detergent when washing clothes. In particular, attempts have been made to attach beneficial substance components to clothes by adding a granular composition in which a beneficial substance is supported on a solid carrier, i.e., beneficial substance delivery particles, separately from detergent during washing.
[0003] Patent Document 1 discloses a technology for granulated powder in which a fragrance or microcapsules containing a fragrance are supported on a solid carrier. Patent Document 2 discloses a technology for a 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 beneficial agent delivery particles are used in a washing process, it is necessary that the beneficial agent remains on the textile product even after the process of removing dirt with detergent components during washing and the rinsing process of removing the detergent components. For this reason, a method is desired in which the beneficial agent delivery particles do not dissolve in the presence of detergent components, but dissolve during the rinsing stage. The beneficial agent delivery particles have a problem of remaining undissolved at the end of washing, while if the beneficial agent delivery particles dissolve too quickly during the washing process, the beneficial agent is unlikely to remain on the textile product at the end of washing. Therefore, a technology is required in which the beneficial agent remains sufficiently on the textile product at the end of washing. [Means for solving the problem]
[0006] The present invention relates to beneficial substance delivery particles comprising (a) a water-soluble solid carrier having a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter [hereinafter referred to as (a) component] and (b) a beneficial substance [hereinafter referred to as (b) component] supported thereon.
[0007] The present invention also relates to a method for producing beneficial substance delivery particles, which comprises mixing (a) a water-soluble solid carrier having a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter (hereinafter referred to as component (a)), and (b) a beneficial substance (hereinafter referred to as component (b)). Effect of the Invention
[0008] According to the present invention, it is possible to provide beneficial substance delivery particles for textile products that allow the beneficial substance to retain its function even after the textile products have been washed and dried. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0009] Hereinafter, in this specification, "enhancing the function of a beneficial substance" means, for example, if the beneficial substance is a fragrance, "the strength of the fragrance from the textile product becomes stronger," and if the beneficial substance is an antibacterial agent or a bactericide, "the antibacterial or bactericidal effect against bacteria becomes stronger."
[0010] The component (a) is a water-soluble solid carrier. The water-soluble solid carrier here may have a solubility of 1.0 g or more in 100 g of water at 20° C., and preferably has a solubility of 1.0 g or more and 60 g or less.
[0011] The moisture content of component (a) is 0.1% by mass or more as measured by an infrared moisture meter, and from the viewpoint of enhancing the function of the beneficial substance and further increasing the strength of the beneficial substance delivery particles, it is preferably 1% by mass or more, more preferably 5% by mass or more, and from the viewpoint of further increasing the strength of the beneficial substance delivery particles, it is preferably 1.6% by mass or more, more preferably 2.0% by mass or more, and from the viewpoint of storage stability and better exerting the function of the beneficial substance, the moisture content may be 20% by mass or less, preferably 18% by mass or less, more preferably 15% by mass or less.
[0012] The moisture content of component (a) may be measured using an infrared moisture meter. For example, it can be measured using an infrared moisture meter (e.g., MOC63u, manufactured by Shimadzu Corporation) at a measurement temperature of 105°C. The moisture calculated here means the moisture content of the water-soluble solid carrier. The moisture content of component (a) is calculated based on the following formula by measuring the mass of the water-soluble solid carrier before and after drying using an infrared moisture meter. Moisture content (mass%) = {mass before drying (g) - mass after drying (g)} / mass before drying (g)
[0013] The (a) component may have pores on the surface, and the average pore size is preferably 1 nm or more, more preferably 10 nm or more, from the viewpoints of storage stability, increasing the strength of the beneficial substance delivery particles obtained, and enhancing the function of the beneficial substance, and is preferably 1000 μm or less, more preferably 100 μm or less, from the viewpoints of increasing the strength of the beneficial substance delivery particles and enhancing the function of the beneficial substance. The average pore size of the pores present on the (a) component surface 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, for example, using AveragePoreDiameter (4V / A).
[0014] From the viewpoint of increasing the strength of the beneficial agent delivery particle, the (a) component may have a bulk density of preferably 450 g / L or more, more preferably 500 g / L or more, and from the viewpoint of solubility, may have 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.
[0015] The component (a) may preferably have an average particle size of 1.0 mm or more, more preferably 3.0 mm or more, and preferably 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.
[0016] The 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 water 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). The water-soluble solid carrier may be, from the viewpoint of preventing the quality of the beneficial substance (preferably a fragrance), 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.
[0017] The content of component (a) may be, in 100% by mass of the beneficial substance delivery particle of the present invention, 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. These contents may be based on the blending amount when producing the beneficial substance delivery particle of the present invention.
[0018] The (b) component may be a beneficial agent, preferably a beneficial agent for textile products. That is, the beneficial agent delivery particle of the present invention may be a particle for delivering the (b) component to textile products. Therefore, the (b) component may be a compound that is beneficial to textile products and is difficult to adsorb to textile products during normal washing processes.
[0019] The compound (b) that is beneficial to textile products and is not easily adsorbed to textile products in a normal washing process may be, for example, a compound that has a low molecular weight and does not have an adsorptive group such as a cationic group. Specifically, the compound may be one or more compounds selected from alcohols, esters, ketones, aldehydes, and phenolic compounds, each having a molecular weight of preferably 120 or more, more preferably 130 or more, and preferably 500 or less, more preferably 400 or less.
[0020] In addition, the component (b) may be a compound having a ClogP of preferably 1.0 or more and 30 or less. The ClogP is preferably 1.5 or more, more preferably 2.0 or more, even more preferably 2.3 or more, even more preferably 2.5 or more, and 30 or less, preferably 20 or less, more preferably 10 or less, even more preferably 6.0 or less, even more preferably 5.5 or less, and even more preferably 5.0 or less. If the ClogP value is within such a range, the support and retention of the component (a) is good. The support here refers to a state in which the component (b) is attached to the inside of the component (a), preferably to the inner surface of the pores connecting the outer surface of the component (a) to the inside [also referred to as the inside of the pores of the component (a)]. In addition, the support and retention here refers to a state in which the component (b) is supported by the component (a), and the volatilization of the component (b) is suppressed, or preferably the volatilization or leakage (leakage) of the encapsulated components of the perfume-encapsulated microcapsules described below that are used optionally is suppressed.
[0021] 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 multiple beneficial substances are contained, the ClogP value of the beneficial substance mixture can be calculated by multiplying the ClogP value of each beneficial substance by its volume ratio in the beneficial substance mixture and then taking the sum of the results.
[0022] Furthermore, component (b) may be a compound exhibiting an oil-water interfacial tension of preferably 7 mN / m or more at 25° C. From the viewpoint of the support and retention of component (b) on component (a), the oil-water interfacial tension may be preferably 10 mN / m or more, more preferably 13 mN / m or more. 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.).
[0023] Specific examples of the (b) component include at least one selected from fragrances, fragrance precursors, oils (silicones, oil-soluble polymers), antioxidants, cooling agents, warming agents, antibacterial agents, dyes, pigments, UV absorbers, solvents, skin care ingredients such as moisturizers, cosmetic oils, preservatives, insecticides, and insect repellents. When the beneficial substance delivery particles of the present invention are used in textile products, the (b) component is preferably at least one selected from (b1) fragrances and fragrance precursors (hereinafter (b1) component), (b2) antioxidants (hereinafter (b2) component), and (b3) bactericides (hereinafter (b3) component). The fragrances and fragrance precursors as the (b) component do not include microcapsules in which a fragrance is encapsulated in a shell (sometimes called a shell) (hereinafter also referred to as fragrance-encapsulated microcapsules, fragrance microcapsules, and microencapsulated fragrances) as described below.
[0024] As the component (b1), the fragrance is not particularly limited, but for example, fragrance compounds described in Motoki Nakajima, "Fundamentals of Fragrance and Fragrance Blending," 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 compound or a mixture of two or more compounds. In addition, fragrance components or fragrance compositions prepared independently by fragrance manufacturers can be used. The fragrance may be a single fragrance compound or a fragrance composition mixed with two or more fragrance compounds, and the fragrance composition may contain a fragrance diluent or solvent in addition to the fragrance compound. In addition, fragrance precursors can be used as the fragrance.
[0025] As the component (b1), from the viewpoint of the support and retention on the component (a), the fragrance compound may be a fragrance compound having a ClogP value of 1.0 or more and 6.0 or less. The ClogP value is preferably 1.0 or more, more preferably 2.0 or more, even more preferably 2.3 or more, still more preferably 2.5 or more, and is preferably 6.0 or less, more preferably 5.5 or less, and even more preferably 5.0 or less.
[0026] As the (b1) component, examples of the fragrance compounds 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 (. and one or more fragrance compounds selected from the group consisting of dimethylformamide (registered trademark) (4.7), terpineol (3.3), terpinyl acetate (4.3), tetrahydrolinalool (3.6), tricyclodecenyl acetate (2.9), tricyclodecenyl propionate (3.3), γ-undecalactone (3.1), florosa (2), isoamyl acetate (2.3), stearyl acetate (2.5), triplal (2.9), and Dynascon (registered trademark) (4.5).
[0027] As the component (b1), the fragrance precursor may be a compound that reacts with water to release a fragrance component, or a compound that reacts with light to release a fragrance component. Examples of the compound that reacts with water to release a fragrance component include a silicate ester compound having an alkoxy component derived from a fragrance alcohol, a fatty acid ester compound having an alkoxy component derived from a fragrance alcohol, an acetal compound or a hemiacetal compound obtained by reacting a carbonyl component derived from a fragrance aldehyde or a fragrance ketone with an alcohol compound, a Schiff base compound obtained by reacting a carbonyl component derived from a fragrance aldehyde or a fragrance ketone with a primary amine compound, and a hemiaminal compound or a hydrazone compound obtained by reacting a carbonyl component derived from a fragrance aldehyde or a fragrance ketone with a hydrazine compound. Examples of the compound that reacts with light to release a fragrance component include a 2-nitrobenzyl ether compound having an alkoxy component derived from a fragrance alcohol, an α-ketoester compound having a carbonyl component derived from a fragrance aldehyde or a fragrance ketone, and a coumaric acid ester compound having an alkoxy component derived from a fragrance alcohol. These fragrance precursors may be used as polymers, for example, reaction products of some carboxy groups of polyacrylic acid with fragrance alcohols.
[0028] As the component (b2), the antioxidant may be butylhydroxytoluene (BHT / ClogP: 5.2), butylhydroxyanisole (ClogP: 3.0), tocopherol (ClogP: 13.0), distyrenated cresol (ClogP: 1 to 1.94), etc., and one or more types selected from the above may be used.
[0029] As the component (b3), the bactericide may be one or more selected from the following: triclosan (ClogP: 5.5), diclosan (ClogP: 4.9), 3-methyl-4-isopropylphenol (ClogP: 3.4), phenoxyethanol (ClogP: 1.39), benzyl alcohol (ClogP: 1.1), etc.
[0030] Although the mechanism of action of the present invention is unclear, the present inventors presume as follows. When a beneficial substance is impregnated into a water-soluble solid carrier, preferably a water-soluble inorganic salt, to produce particles carrying and retaining the beneficial substance, if the water-soluble solid carrier has a low moisture content, the strength of the particles decreases, and furthermore, the storage stability decreases, and the solubility of the particles in water increases. For example, when the particles are used in a washing process, they dissolve immediately when added to a washing solution. As a result, the beneficial substance is easily dispersed in the washing solution and flows out during washing and rinsing, making it difficult to adsorb to textile products, etc. On the other hand, if the water-soluble solid carrier has a high moisture content, the beneficial substance cannot be supported and retained inside the pores of the water-soluble solid carrier, but is supported and retained near the surface of the water-soluble solid carrier. For example, when added to a washing solution, the solubility of the particles in the washing solution decreases, but the beneficial substance present on the surface is easily dissolved and flows out into the washing solution or rinsing solution, making it difficult to adsorb to textile products, etc. The beneficial substance delivery particles of the present invention are composed of component (a) with a specific moisture content carrying and retaining component (b), which is believed to provide favorable solubility in the cleaning solution and favorable flow-out properties of component (b), thereby improving the adsorption efficiency onto textile products, etc.
[0031] The content of the (b) component may be, in 100% by mass of the beneficial substance delivery particle of the present invention, preferably 0.05% by mass or more, more preferably 0.1% by mass or more, even more preferably 1.0% by mass or more, even more preferably 2.0% by mass or more, even more preferably 3.0% by mass or more, and preferably 20% by mass or less, more preferably 15% by mass or less. These contents may be based on the blending amounts when producing the beneficial substance delivery particle of the present invention.
[0032] The content of component (b1) may be, in 100% by mass of the beneficial substance delivery particle of the present invention, 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 20% by mass or less, more preferably 15% by mass or less, even more preferably 10% by mass or less, and even more preferably 8% by mass or less.
[0033] The content of component (b2) may be, in 100% by mass of the beneficial substance delivery particle of the present invention, 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.
[0034] The content of component (b3) may be preferably 0.1% by mass or more, more preferably 0.3% by mass or more, and preferably 0.8% by mass or less, more preferably 0.6% by mass or less, based on 100% by mass of the beneficial substance delivery particle of the present invention.
[0035] Furthermore, from the viewpoint of imparting functionality, the content of the (b) component may be preferably 1 part by mass or more, more preferably 3 parts by mass or more, and even more preferably 5 parts by mass or more, per 100 parts by mass of the (a) component, and from the viewpoint of uniformly supporting and retaining the (b) component in the (a) component, the content may be preferably 30 parts by mass or less, more preferably 20 parts by mass or less, and even more preferably 15 parts by mass or less.
[0036] As one embodiment of the component (b), the component (b1) can be used. As another embodiment of the component (b), from the viewpoint of the stability of the component (b1), the components (b1) and (b2) can be used. As yet another embodiment, from the viewpoint of the stability of the fragrance and the antibacterial property, the components (b1), (b2) and (b3) can be used. From the viewpoint of the stability of the fragrance, the component (b) may preferably be the components (b1) and (b2).
[0037] When the component (b) is, for example, a mixture of the components (b1) and (b2), the mass ratio of the content of the component (b1) to the content of the component (b2) [(b2) / (b1)] is preferably 0.01 or more, more preferably 0.02 or more, and is preferably 0.10 or less, more preferably 0.08 or less.
[0038] From the standpoint of increasing the strength of the beneficial substance delivery particle, fluidity (ease of handling as a particle), and stability of the beneficial substance, the mass ratio of the content of component (a) to the content of component (b) [(b) / (a)] is preferably 0.005 or more, more preferably 0.01 or more, even more preferably 0.015 or more, still more preferably 0.03 or more, still more preferably 0.05 or more, and preferably 0.15 or less, more preferably 0.12 or less, and even more preferably 0.1 or less.
[0039] The beneficial substance delivery particles of the present invention are not particularly limited, but may be preferably spherical, granular, or powdery, with spherical particles being preferred from the viewpoint of flowability.
[0040] From the viewpoint of solubility and handling, the beneficial agent delivery particles of the present invention may have an average particle size of 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 by calculating the spherical equivalent diameter of 250 particles using image analysis software ImageJ.
[0041] The beneficial agent delivery particles of the present invention may have a bulk density of preferably 400 g / L or more, more preferably 500 g / L or more, from the viewpoint of volume during use, and may have a bulk density of preferably 1000 g / L or less, more preferably 800 g / L or less, from the viewpoint of ease of use during use. The bulk density can be measured by a bulk specific gravity measuring device according to JIS K7365.
[0042] From the viewpoint of imparting a desirable fragrance to the textile product, the beneficial substance delivery particle of the present invention may further contain a microcapsule in which a perfume is encapsulated in a shell (hereinafter also referred to as a perfume-encapsulated microcapsule or a perfume microcapsule). The encapsulated perfume may be one or more selected from the perfume compounds described above, or may be a perfume composition containing two or more of them. When the beneficial substance delivery particle of the present invention contains a perfume-encapsulated microcapsule, not only the (b) component but also the perfume from the perfume-encapsulated microcapsule can be delivered to and adsorbed on the textile product.
[0043] 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 made of 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.
[0044] 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.
[0045] In 100% by mass of the slurry containing fragrance microcapsules obtained by the above-mentioned method for producing fragrance microcapsules, the content of the fragrance compound is 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.
[0046] 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.
[0047] From the viewpoint of the fragrance intensity of the treated textile product and the fragrance intensity when the dried textile product is rubbed or otherwise stimulated, the perfume microcapsules of the present invention may have an average particle size of 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 perfume microcapsules can be measured using a laser diffraction / scattering type particle size distribution measuring device "LA-950" (manufactured by Horiba, Ltd.).
[0048] When perfume microcapsules are used in the present invention, the content of the perfume compound encapsulated in the perfume microcapsule may be, based on 100% by mass of the beneficial agent delivery particle of the present invention, preferably 0.1% by mass or more, 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 3.0% by mass or less, more preferably 2.0% by mass or less, and even more preferably 1.5% by mass or less. These contents may be based on the amounts blended when the beneficial agent delivery particle of the present invention is produced.
[0049] When perfume microcapsules are used in the present invention, from the viewpoint of the stability of perfume microcapsules, it is preferable to use the microcapsules as an aqueous dispersion (also called perfume microcapsule slurry) in the manufacture of the beneficial substance delivery particle of the present invention.When used as such a dispersion, the content of perfume microcapsules in the dispersion is preferably 5.0% by mass or more, more preferably 10.0% by mass or more, even more preferably 15.0% by mass or more, even more preferably 20.0% by mass or more, and from the viewpoint of particle strength, it is preferably 70.0% by mass or less, more preferably 60.0% by mass or less, even more preferably 50.0% by mass or less.These contents may be based on the blending amount when preparing perfume microcapsules.
[0050] In addition, when a dispersion of perfume microcapsules is used in the production of the beneficial agent delivery particle of the present invention, the content of the dispersion in the beneficial agent delivery particle is preferably 0.3% by mass or more, more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and preferably 5.0% by mass or less, more preferably 4.0% by mass or less. These contents may be based on the amount of the beneficial agent delivery particle when the beneficial agent delivery particle of the present invention is produced.
[0051] The beneficial substance delivery particle of the present invention may further contain one or more selected from water-soluble cationic polymeric compounds and cationic surfactants, from the viewpoint of promoting the adsorption of component (b) to textile products.
[0052] Specific examples of the water-soluble cationic polymer compound include polydiallyldimethylammonium chlorides such as poly(diallyldimethylammonium chloride), poly(acrylic acid-co-diallyldimethylammonium chloride), poly(acrylamide-co-diallyldimethylammonium chloride), and poly(acrylamide-co-acrylic acid-co-diallyldimethylammonium chloride), as well as copolymers thereof; poly(2-(methacryloyloxy)ethyltrimethylammonium chloride), polyethyleneimine, polyallylamine, cationized cellulose, cationized guar gum, cationized tara gum, cationized fenugreek gum, and cationized locust bean gum. Among these, preferably, one or more selected from polydiallyldimethylammonium chloride and its 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).
[0053] Examples of the cationic surfactant include alkylamine salts and alkyl quaternary ammonium salts.
[0054] The alkylamine salt may be preferably a salt of a secondary amine or a tertiary amine, more preferably a salt of a tertiary amine. The alkylamine salt is preferably 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 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, even more preferably 18 or less. The carbon number of the short-chain alkyl group is preferably 1 or more, and preferably 4 or less, more preferably 1 or 2, and even more preferably 1, i.e., a methyl group. Examples of 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.
[0055] The alkyl quaternary ammonium salt is 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 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 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.
[0056] Of these, the cationic surfactant is preferably an alkyl quaternary ammonium salt, more preferably an alkyltrimethylammonium salt having an alkyl group with 10 to 22 carbon atoms, even more preferably an alkyltrimethylammonium chloride having an alkyl group with 10 to 22 carbon atoms, even more preferably one or more selected from lauryltrimethylammonium chloride, stearyltrimethylammonium chloride, and cetyltrimethylammonium chloride, and even more preferably cetyltrimethylammonium chloride.
[0057] The content of the water-soluble cationic polymeric compound in the present invention may be 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 beneficial substance delivery particle of the present invention, from the viewpoint of promoting the adsorption of the (b) component to the textile product. These contents may be based on the blending amount when the beneficial substance delivery particle of the present invention is produced. Moreover, the above content does not include the cationic surfactant of the present invention.
[0058] The content of the cationic surfactant in the present invention may be, in terms of promoting the adsorption of the (b) component to the textile product, 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 beneficial substance delivery particle of the present invention. These contents may be based on the blending amount when the beneficial substance delivery particle of the present invention is manufactured. The mass of the cationic surfactant is used as a value converted to a chlorine salt. The above content does not include the water-soluble cationic polymer compound in the present invention.
[0059] The beneficial substance delivery particle of the present invention may further contain a water-soluble nonionic polymer from the viewpoints of further increasing the strength of the beneficial substance delivery particle, solubility, suppression of volatilization of the supported / held component (b) during storage, suppression of seepage, and other stability, and from the viewpoints of supporting / holding component (b) inside the pores of component (a) and, optionally, supporting / holding perfume microcapsules on the particle surface. The water-soluble nonionic polymer may be preferably polyethylene glycol (PEG), polypropylene glycol, polyoxyethylene alkyl ether, or polyoxyethylene phenol ether, and more preferably polyethylene glycol or polypropylene glycol. The number average molecular weight of the water-soluble nonionic polymer may be preferably 2,000 or more, more preferably 3,000 or more, even more preferably 4,000 or more, and preferably 20,000 or less, more preferably 15,000 or less, even more preferably 10,000 or less, as measured by GPC using polystyrene as the standard, from the viewpoints of increasing the strength of the beneficial substance delivery particles, solubility, and stability such as suppression of volatilization of the supported / held component (b) during storage and suppression of exudation. When measuring the molecular weight of polyethylene glycol, water / ethanol is used as the solvent.
[0060] The content of the water-soluble nonionic polymer may be, from the viewpoint of increasing the strength of the beneficial substance delivery particle and from the viewpoint of solubility, suppression of volatilization of the supported / held (b) component during storage, suppression of seepage, etc., preferably 0.5% by mass or more, more preferably 1% by mass or more, and preferably 30% by mass or less, more preferably 25% by mass or less, and even more preferably 20% by mass or less, based on 100% by mass of the beneficial substance delivery particle. These contents may be based on the amounts blended when producing the beneficial substance delivery particle of the present invention.
[0061] When the beneficial agent delivery particle of the present invention contains a water-soluble nonionic polymer, the mass ratio of the content of component (a) to the content of the water-soluble nonionic polymer [(a) / water-soluble nonionic polymer] may be, from the viewpoint of solubility, preferably 0.1 or more, more preferably 0.2 or more, even more preferably 0.3 or more, even more preferably 1.0 or more, even more preferably 5.0 or more, even more preferably 7.0 or more, and from the viewpoint of product stability (such as suppression of volatilization and exudation of the fragrance (component (b)) supported / held in component (a) during particle storage), 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, even more preferably 20 or less. The aforementioned content may be based on the blending amount when producing the beneficial agent delivery particle of the present invention.
[0062] The beneficial substance delivery particle of the present invention may contain an organic solvent from the viewpoint of promoting the support and retention of the (b) component in the pores of the (a) component, from the viewpoint of suppressing the volatilization of the (b) component during storage, and from the viewpoint of suppressing exudation. The organic solvent is one or more organic compounds that are liquid at 20°C and are selected from alcohols having 1 to 10 carbon atoms, glycols, esters having 6 to 20 carbon atoms, and paraffins other than fragrance compounds. Specifically, the alcohols include methanol, ethanol, and glycerin, the glycols include ethylene glycol, diethylene glycol monoethyl ether, propylene glycol, dipropylene glycol, dipropylene glycol monoethyl ether, and 3-methoxy-3-methylbutanol, the esters include diethyl phthalate, isopropyl myristate, benzyl myristate, triethyl citrate, diisobutyl adipate, and hydrogenated methyl abietic acid, and the paraffins include liquid paraffin and isoparaffin.
[0063] The organic solvent may be the same as the organic solvent optionally contained in the (b) component, and from the viewpoints of promoting the support and retention of the (a) component inside the pores, suppressing the volatilization of the (b) component during storage of the particles, and suppressing the seepage of the (b) component during storage of the particles, the organic solvent may be preferably 0.02% by mass or more, more preferably 0.05% by mass or more, and preferably 3.0% by mass or less, more preferably 2.0% by mass or less, and even more preferably 1.5% by mass or less, based on 100% by mass of the beneficial substance delivery particles. These contents may be based on the amounts blended when the beneficial substance delivery particles of the present invention are produced.
[0064] The beneficial substance delivery particle of the present invention can be obtained by mixing component (a) and component (b). In one embodiment, the beneficial substance delivery particle of the present invention can be obtained by a method for producing beneficial substance delivery particles, which comprises drying a water-soluble solid carrier to prepare component (a), and then mixing component (a) and component (b). In another embodiment, the beneficial substance delivery particle of the present invention can be obtained by a method for producing beneficial substance delivery particles, which comprises drying a water-soluble solid carrier having a moisture content of more than 20% by mass as measured by an infrared moisture meter to prepare component (a), and then mixing component (a) and component (b).
[0065] In order to adjust the moisture content to prepare component (a), the water-soluble solid carrier can be dried using 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 carrier during drying, a drying method that applies as little strong shear force as possible is preferred, and from the viewpoint of equipment, shelf drying, fluidized bed drying, and reduced pressure drying are preferred.
[0066] The drying treatment may be either a batch type or a continuous type, and is not particularly limited. For example, the batch type includes a drying method using an electric shelf dryer or a hot air dryer, and a drying method using a batch type fluidized bed, and the continuous type includes a fluidized bed, a vibration fluidized bed, a rotary dryer, a steam tube dryer, etc.
[0067] The drying conditions are not particularly limited as long as the water content of the water-soluble solid carrier can be adjusted to 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter. For example, the drying conditions can be adjusted by combining the following drying temperatures and the following drying times.
[0068] The drying temperature can be appropriately determined taking into consideration the drying rate, and may be 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 the water-soluble solid carrier, 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.
[0069] The drying time varies depending on the moisture content and amount of the water-soluble solid carrier used in the production, but in the case of batch operation using a fluidized bed dryer, it may be 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 electric drying, it may be preferably 10 minutes or more, more preferably 30 minutes or more, and preferably 4 hours or less, more preferably 2 hours or less.
[0070] The water-soluble solid carrier may be compressed and molded in advance into granules, flakes, or beads, and then dried. The molding method may be a known method. For example, the compression molding method, extrusion granulation method, rolling granulation method, stirring granulation method, and compaction granulation method may be used. Among these, the compression molding method is preferable.
[0071] When compressing a water-soluble solid carrier, the manufacturing machine to be used is not limited as long as it can produce briquettes or tablets, and well-known briquetting machines, tablet presses, etc. can be used. A briquetting 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 briquetting machine, 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. Tableting machines 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 known tablet presses, a single punch tablet press manufactured by Riken Co., Ltd. and a rotary tablet press manufactured by Kikusui Chemical Co., Ltd. can be used.
[0072] 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.
[0073] The beneficial substance delivery particle of the present invention can be produced, as one form, by mixing the (a) component and the (b) component. Alternatively, the beneficial substance delivery particle of the present invention can be produced, as another form, by mixing the (a) component and the (b) component, and further mixing a water-soluble nonionic polymer and other optional components in a state in which the (b) component is supported and held inside the (a) component, from the viewpoint of suppressing the volatilization of the (b) component. Alternatively, the beneficial substance delivery particle of the present invention can be produced, as another form, by mixing a mixture of the (a) component and the (b) component with a water-soluble nonionic polymer from the viewpoint of supporting and holding the (b) component on the particle surface. Alternatively, the beneficial substance delivery particle of the present invention can be produced, as another form, by mixing a mixture of the (a) component and the (b) component with a water-soluble nonionic polymer from the viewpoint of supporting and holding the (b) component inside the (a) component pores, and optionally supporting and holding the perfume microcapsules on the particle surface.
[0074] In addition, the beneficial substance delivery particle of the present invention can be produced, as another embodiment, by mixing the mixture obtained by mixing the components (a), (b1), and (b2) with other optional components (preferably a mixture of a water-soluble nonionic polymer and a fragrance microcapsule component) from the viewpoint of suppressing the volatilization of the component (b) and the stability of the component (b). In addition, the beneficial substance delivery particle of the present invention can be produced, as another embodiment, by mixing the mixture obtained by mixing the components (b1) and (b2) with the water-soluble nonionic polymer with the component (a) and other optional components from the viewpoint of supporting and retaining the component (b) on the particle surface. The preferred mixing mass ratio of the component (a) and the component (b) can be the same as that of the beneficial substance delivery particle of the present invention described above.
[0075] The mixer for mixing component (a), 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.).
[0076] When mixing the (a) component, the (b) component, and the optional components, it is preferable to use a container rotation type granulator in order to prevent the water-soluble solid carrier from being disintegrated by applying strong shear to the water-soluble solid carrier. As the container rotation type granulator, drum type granulators and pan type granulators 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 either a batch type or a continuous type. In addition, when the wall friction coefficient between the water-soluble solid carrier 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 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.
[0077] The operating conditions of the container-rotating granulator are not particularly limited as long as the water-soluble solid carrier in the granulator can be made to flow and be stirred as uniformly as possible. From the viewpoint of obtaining granules having good disintegration strength, etc., the Froude number defined by the following formula (1) can be 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.
[0078] 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 ]
[0079] In addition, in drum-type granulators or pan-type granulators in which granulation progresses by the rotation of the main body, V and R are the values of the main body, in horizontal or vertical granulators equipped with main wings or crushing wings, V and R are the values of the main shaft, and in pan-type granulators equipped with crushing wings, V and R are the values of the crushing wings.
[0080] The mixing temperature may be 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 evaporation stability of component (b).
[0081] From the viewpoint of uniform mixing, the rotation speed of the mixer is preferably 10 rpm or more, more preferably 20 rpm or more, and from the viewpoint of suppressing the breakdown of the water-soluble solid carrier, the rotation speed may be preferably 100 rpm or less, more preferably 50 rpm or less.
[0082] The mixing time may be preferably 1 minute or more, more preferably 3 minutes or more, from the viewpoint of uniform mixing, and preferably 20 minutes or less, more preferably 10 minutes or less, from the viewpoint of suppressing the breakdown of the water-soluble solid carrier.
[0083] When mixing the (a) component and the (b) component, the (b) component may be supplied by dropping it from a pipe using a pump, or may be supplied using a nozzle. As the nozzle, a one-fluid nozzle or a multi-fluid nozzle may be used. 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 circulating them through independent flow paths to the vicinity of the nozzle tip, and examples of such a multi-fluid nozzle include a two-fluid nozzle, a three-fluid nozzle, and a four-fluid nozzle. In addition, the mixing section of the beneficial substance and the atomization gas may be either an internal mixing type that mixes them within the nozzle tip, or an external mixing type that mixes them outside the nozzle tip. Examples of such a multi-fluid nozzle include an internal mixing type two-fluid nozzle manufactured by Spraying Systems Japan Co., Ltd., Kyoritsu Alloy Manufacturing Co., Ltd., Ikeuchi Co., Ltd., etc., an external mixing type two-fluid nozzle manufactured by Spraying Systems Japan Co., Ltd., Kyoritsu Alloy Manufacturing Co., Ltd., Atmax Co., Ltd., etc., and an external mixing type four-fluid nozzle manufactured by Fujisaki Electric Co., Ltd.
[0084] When component (b) is supplied to component (a) using a multi-fluid nozzle, the supply temperature may be 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 component (b).
[0085] Furthermore, from the viewpoint of uniformly supporting and retaining component (b) in component (a), the addition rate of component (b) may be, relative to 100 parts by mass of component (a), 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.
[0086] The benefit substance 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 benefit substance delivery particles to the textile products during the washing process of the textile products to treat the textile products.
[0087] When the benefit substance delivery particles of the present invention are added in the washing process of a textile product, the amount of benefit substance delivery particles of the present invention added may be preferably 5.0 g or more, more preferably 7.0 g or more, and preferably 10.0 g or less, more preferably 8.0 g or less per 1 kg of textile product. The textile product may be treated with only the benefit substance delivery particles of the present invention, or may be treated with a textile treatment composition containing the benefit substance delivery particles of the present invention.
[0088] When the benefit substance delivery particles of the present invention are added during the washing process of a textile product, the benefit substance delivery particles of the present invention can be added to at least one of the wash water and the rinse water of the laundry, or the benefit substance delivery particles of the present invention can be added to both the wash water and the rinse water of the laundry.
[0089] When the beneficial substance delivery particles of the present invention are added in the washing process of textile products, the beneficial substance delivery particles are preferably added to water at a concentration of 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 the wash water, but it is also possible to add it to the rinse water. The wash water and rinse water for washing may contain a textile laundry detergent component.
[0090] The beneficial substance delivery particles of the present invention can be used in the washing process of the textile product, etc., together with the particles carrying the above-mentioned perfume microcapsules, without carrying or retaining the component (b) in the component (a). Such particles can be produced in the same manner as in Example 1 described below, except that the component (b) is not used. EXAMPLES
[0091] The components used in the examples and comparative examples are summarized below. In the examples and comparative examples, "%" is "% by mass" unless otherwise specified. The mass% of the blended composition in Tables 3 and 4 indicates the mass% of the actual product. The measurements of each physical property were performed by the following methods.
[0092] (1) Moisture content of water-soluble solid carrier 2 g of sample (water-soluble solid carrier) 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 content standard moisture measurement mode at a temperature of 105°C under Auto conditions (when the change in the measured value was 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)
[0093] (2) Bulk density Calculated using a bulk density measuring device in accordance with JIS K7365.
[0094] (3) Average particle size of beneficial agent delivery particles The spherical equivalent diameter of 250 particles was calculated using the image analysis software ImageJ.
[0095] <Ingredients used> 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: 31.0% by mass, bulk density: 790 g / L)
[0096] (b) Component (b1-1) Ingredient: Fragrance composed of the fragrance compounds shown in Table 1 below (b2-1) Ingredient: BHT (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (b3-1) Component: 3-methyl-4-isopropylphenol (manufactured by Osaka Kasei Co., Ltd.) (b3-2) Ingredient: Triclosan (Irgasan DP300 [manufactured by Chiba Specialty Chemicals Co., Ltd.])
[0097] [Table 1]
[0098] Fragrance microcapsule slurry obtained in the following manufacturing 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 2 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).
[0099] [Table 2]
[0100] "Polyquaternium-7" (manufactured by Lubrizol Advanced Materials, Inc.) ·PEG (polyethylene glycol, number average molecular weight 8500)
[0101] Production of Beneficial Agent Delivery Particles Beneficial substance delivery particles having the compositions shown in Table 3 (Examples 1 to 4, Comparative Examples 1 to 3) were produced.
[0102] Example 1 Magnesium sulfate heptahydrate was weighed out in a stainless steel tray, and five stainless steel trays were placed in an Advantec Toyo constant temperature air blower DRM620TE, and dried at 120°C for 2 hours. The dried magnesium sulfate heptahydrate had an infrared meter moisture content of 1.7% by mass and a bulk density of 510g / L (hereinafter referred to as (a1) component). The (a1) component (solid temperature of (a1) 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 conditions of Froude number 0.118 / drum angle 12.6°, while adding a mixture of (b1-1) component and (b2-1) component in the amount shown in Table 3 through a pipe and mixing for 30 seconds (mixed liquid 25°C, addition time 30 seconds, particle solid temperature after addition 45°C). Furthermore, the fragrance microcapsule slurry, polyquaternium-7 and PEG mixture was added through piping in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixture 60°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in formula (1) above). The batch size was 6.5kg (total blend amount). The beneficial substance delivery particles obtained had component (b) supported by component (a). The beneficial substance delivery particles obtained had an average particle size of 4mm and a bulk density of 600g / L.
[0103] Example 2 Weigh out 12 kg of magnesium sulfate heptahydrate and place it in a fluidized bed dryer (Okawahara Manufacturing Co., Ltd. Slit Flow) with a floor area of 0.1 m. 2 The powder layer was set to a thickness of 152 mm, and 120°C hot air was blown at a speed of 4 m 3The mixture was dried at 100°C for 25 minutes at 100°C / min. The dried magnesium sulfate heptahydrate had a moisture content of 5.1% by mass as measured by an infrared meter and a bulk density of 590 g / L (hereinafter referred to as component (a2)). Component (a2) (solid temperature of component (a2) 50°C) was charged into a 75 L drum-type granulator (φ40 cm × L60 cm) with a baffle plate in the composition shown in Table 3, and mixed under conditions of Froude number 0.118 / drum angle 12.6°. The mixture of components (b1-1) and (b2-1) 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 = 0.48 m / s, R = 0.2 m in the above formula (1)). Furthermore, the fragrance microcapsule slurry, polyquaternium-7 and PEG mixture was added through piping in the amount shown in Table 3 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). The beneficial substance delivery particles obtained had component (b) supported by component (a). The beneficial substance delivery particles obtained had an average particle size of 4 mm and a bulk density of 640 g / L.
[0104] Example 3 Weigh out 12 kg of magnesium sulfate heptahydrate and place it in a fluidized bed dryer (Okawahara Manufacturing Co., Ltd. Slit Flow) with a floor area of 0.1 m. 2 The powder layer was set to a thickness of 152 mm, and 120°C hot air was blown at a speed of 4 m 3The dried magnesium sulfate heptahydrate had a moisture content of 16.4% by mass as measured by an infrared meter and a bulk density of 650 g / L (hereinafter referred to as component (a3)). The component (a3) (solid temperature of component (a3) 50° C.) was charged into a 75 L drum-type granulator (φ40 cm × L60 cm) with a baffle plate in the composition shown in Table 3, and mixed under conditions of Froude number 0.118 / drum angle 12.6°. The mixture of components (b1-1) and (b2-1) 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=0.48 m / s, R=0.2 m in the above formula (1)). Furthermore, the fragrance microcapsule slurry, polyquaternium-7 and PEG mixture was added through piping in the amount shown in Table 3 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). The beneficial substance delivery particles obtained had component (b) supported by component (a). The beneficial substance delivery particles obtained had an average particle size of 4 mm and a bulk density of 670 g / L.
[0105] Example 4 Magnesium sulfate heptahydrate was weighed out in a stainless steel tray, and five stainless steel trays were placed in an Advantec Toyo constant temperature air blower DRM620TE, and dried at 120°C for 2 hours. The dried magnesium sulfate heptahydrate had an infrared meter moisture content of 0.6% by mass and a bulk density of 538 g / L (hereinafter referred to as (a4) component). The (a1) component (solid temperature of (a1) component 50°C) was charged in a 75L drum type granulator (φ40cm×L60cm) with a baffle plate in the composition shown in Table 3, and mixed under conditions of Froude number 0.118 / drum angle 12.6°, while adding a mixture of (b1-1) component and (b2-1) component in the amount shown in Table 3 through a pipe and mixing for 30 seconds (mixture 25°C, addition time 30 seconds, particle solid temperature after addition 45°C). Furthermore, a mixture of polyquaternium-7 and PEG was added through piping in the amount shown in Table 3 and mixed for 3 minutes and 30 seconds (mixture 60°C, addition time 30 seconds, particle solid temperature after addition 45°C, V = 0.48 m / s, R = 0.2 m in formula (1) above). The batch size was 6.5 kg (total blend amount). The beneficial substance delivery particles obtained had component (b) supported by component (a). The beneficial substance delivery particles obtained had an average particle size of 4 mm and a bulk density of 578 g / L.
[0106] Comparative Example 1 Weigh out 12 kg of magnesium sulfate heptahydrate and place it in a fluidized bed dryer (Okawahara Manufacturing Co., Ltd. Slit Flow) with a floor area of 0.1 m. 2 The powder layer was set to a thickness of 152 mm, and 120°C hot air was blown at a speed of 4 m 3The dried product of magnesium sulfate heptahydrate had an infrared meter moisture content of 26.0% by mass and a bulk density of 730 g / L (hereinafter, comparative (a1) component). The comparative (a1) component (comparative (a1) component solid temperature 50° C.) was charged into a 75 L drum-type granulator (φ40 cm × L60 cm) 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°, while adding the mixed liquid of the (b1-1) component and the (b2-1) component in the amount shown in Table 3 through a pipe and mixing for 30 seconds (mixed liquid 25° C., addition time 30 seconds, particle solid temperature after addition 45° C., V=0.48 m / s, R=0.2 m in the above formula (1)). Furthermore, the fragrance microcapsule slurry, polyquaternium-7 and PEG mixture was added through piping in the amount shown in Table 3 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). The obtained beneficial substance delivery particles had the (b) component supported by the comparative (a1) component. The obtained beneficial substance delivery particles had an average particle size of 4 mm and a bulk density of 740 g / L.
[0107] Comparative Example 2 Magnesium sulfate heptahydrate was not dried, and the amount shown in Table 3 was put into a 75L drum-type granulator (φ40cm×L60cm) with a baffle plate. While mixing under the conditions of Froude number 0.118 / drum angle 12.6°, the mixed liquid of the (b1-1) component and the (b2-1) 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 25°C, V=0.48m / s in the above formula (1), R=0.2m). Furthermore, the mixed liquid of the fragrance microcapsule slurry, polyquaternium-7 and PEG 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 40°C). The batch size was 6.5kg (total blend amount). The obtained beneficial substance delivery particles could not sufficiently carry the fragrance, and the obtained particles were sticky.
[0108] Comparative Example 3 Weigh out 12 kg of magnesium sulfate heptahydrate and place it in a fluidized bed dryer (Okawahara Manufacturing Co., Ltd. Slit Flow) with a floor area of 0.1 m.2 The powder layer was set to a thickness of 152 mm, and 120°C hot air was blown at a speed of 4 m 3 The dried product of magnesium sulfate heptahydrate had an infrared meter moisture content of 26.6% by mass and a bulk density of 738 g / L (hereinafter, comparative (a2) component). The comparative (a2) component (comparative (a2) solid temperature 50° C.) was charged into a 75 L drum-type granulator (φ40 cm × L60 cm) with a baffle plate in the composition shown in Table 3, and mixed under conditions of Froude number 0.118 / drum angle 12.6°, while adding the mixed liquid of the (b1-1) component and the (b2-1) component in the amount shown in Table 3 through a pipe and mixing for 30 seconds (mixed liquid 25° C., addition time 30 seconds, particle solid temperature after addition 45° C., V=0.48 m / s, R=0.2 m in the above formula (1)). Furthermore, the mixture of polyquaternium-7 and PEG was added through piping in the amount shown in Table 3 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). The beneficial substance delivery particles obtained were sticky because the (b) component was not sufficiently supported by the comparative (a2) component. The beneficial substance delivery particles obtained had an average particle size of 4 mm and a bulk density of 686 g / L.
[0109] <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 a commercially available unscented liquid detergent and 10.1g of the beneficial substance 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 a 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. The results are shown in Table 3.
[0110] <Evaluation criteria> 0: Odorless 1: Very slightly felt 2: Feeling weak 3: I feel it clearly 4: I feel strongly 5: Feels quite strong
[0111] [Table 3]
[0112] Formulation examples 1~13 The (a2) component (solid temperature of (a2) component 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 solution of (b) component was added by piping in the amount shown in Table 4 and mixed for 30 seconds (mixed solution 25°C, addition time 30 seconds, particle solid temperature after addition 45°C, V=0.48m / s, R=0.2m in the formula (1)). Furthermore, the mixed solution of the fragrance microcapsule slurry, polyquaternium-7 and PEG was added by piping in the amount shown in Table 4 and mixed for 3 minutes and 30 seconds (mixed solution 60°C, addition time 30 seconds, particle solid temperature after addition 45°C). The batch size was 6.5kg (total blend amount). When the beneficial substance delivery particles obtained in Blending Examples 1 to 13 were used to perform the same evaluations 1 and 2 as in the Examples, high fragrance intensity was obtained in both cases.
[0113] [Table 4]
Claims
1. (a) a water-soluble solid carrier having a moisture content of 0.1% by mass or more and 20% by mass or less as measured by an infrared moisture meter [hereinafter referred to as (a) component], and (b) a beneficial substance [hereinafter referred to as (b) component] supported thereon.
2. The benefit agent delivery particle of claim 1 , wherein the water-soluble solid carrier is a water-soluble inorganic salt.
3. 3. The benefit agent delivery particle of claim 1 or 2, wherein the water-soluble solid carrier is a water-soluble inorganic sulfate.
4. The beneficial agent 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.
5. 3. The benefit agent delivery particle of claim 1 or 2, wherein component (b) is a fragrance.
6. A method for producing beneficial substance delivery particles, comprising mixing (a) a water-soluble solid carrier having a moisture content of 0.1% by weight or more and 20% by weight or less as measured by an infrared moisture meter (hereinafter referred to as (a) component) and (b) a beneficial substance (hereinafter referred to as (b) component).
7. The method for producing a beneficial agent delivery particle according to claim 6, wherein the water-soluble solid carrier is dried to prepare component (a), and then component (a) and component (b) are mixed together.
8. The method for producing a beneficial substance delivery particle according to claim 6 or 7, wherein a water-soluble solid carrier having a moisture content of more than 20% by mass as measured by an infrared moisture meter is molded and then dried to prepare component (a).
9. 8. The method for producing the beneficial agent delivery particles according to claim 6 or 7, wherein component (a) and component (b) are mixed using a container rotary granulator.
10. A method for perfumery of textile products, comprising adding the beneficial agent delivery particles according to claim 1 or 2 during the washing process of the textile products.
11. 11. A method for perfuming a textile product according to claim 10, comprising adding the benefit agent delivery particles according to claim 1 or 2 to at least one of wash water and rinse water during the washing process of the textile product.
Citation Information
Patent Citations
Powderizing method of liquid perfume and detergent composition containing powdery perfume obtained by said method
JP1989188597A
Solid fragrance enhancer composition
JP2020512452A
Packaged Composition
JP2021529869A