Benefit agent delivery particles

Abstract

There is provided a benefit agent delivery particle having improved solubility after storage at elevated temperatures (e.g. 40-50 °C) and a method of improving the solubility of a benefit agent delivery particle after storage at elevated temperatures (e.g. 40-50 °C).SOLUTION: (A1) a water-soluble inorganic excipient (hereinafter referred to as ingredient (A1)), (A2) a water-insoluble inorganic excipient (hereinafter referred to as ingredient (A2)), (B) a beneficial ingredient (hereinafter referred to as ingredient (B)), (C) a polyalkylene glycol having a weight-average molecular weight of 2000 or more and 20000 or less (hereinafter referred to as ingredient (C)), and (D) a polyhydric alcohol having a molecular weight of 60 or more and 200 or less (hereinafter referred to as ingredient (D)), the mass ratio of the content of the ingredient (A1) to the total content of the ingredient (A1) and the ingredient (A2), (A1) / [(A1) + (A2)], is 0.80 or more and 1.0 or less, and the mass ratio of the content of the ingredient (D) to the content of the ingredient (C), (D) / (C), is 0.01 or more and 0.2 or less.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention relates to benefit agent delivery particles and methods for improving the post-storage solubility of benefit agent delivery particles. [Background technology]

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

[0003] Patent Document 1 discloses fragrance particles that have excellent stability during transportation and storage and a good appearance, and that contain (A) 5 to 30% by weight of a fragrance, (B) an oil-absorbing carrier having an oil absorption capacity of 100 ml / 100 g or more but less than 800 ml / 100 g as measured according to JIS K5101, (C) a binder, and (D) non-hygroscopic inorganic particles having an oil absorption capacity of less than 100 ml / 100 g as measured according to JIS K5101 and containing 20% ​​or more particles with a particle size of less than 20 μm and 10% or more particles with a particle size of 100 μm or more, and that are compacted by extrusion granulation. Patent Document 2 discloses a packaged particulate composition having a carrier and a shading dye, wherein at least 80% of the particles have a density of less than about 1.25 g / cm3, at least 80% of the particles have a weight of between about 0.1 mg and about 5 g, and each of the particles has a maximum dimension of less than about 10 mm. Patent Document 3 discloses fragrance particles that contain (a) a polyhydric alcohol that is liquid at 25°C and (b) polyethylene glycol, and the weight ratio of component (a) to component (b) is in the range of (a) / (b) = 0.0025 to 0.5, and that suppress fragrance evaporation during storage while rapidly dissolving without impairing particle strength, particularly when stored in a high-humidity environment. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] Japanese Patent Application Laid-Open No. 2005-330362 [Patent Document 2] Special Publication No. 2018-534399 [Patent Document 3] Japanese Patent Application Laid-Open No. 2006-111705 Summary of the Invention [Problem to be solved by the invention]

[0005] These beneficial ingredient delivery particles are formulated by mixing water-insoluble or water-soluble inorganic particles as an excipient with a binder such as polyethylene glycol, and are used. Immediately after granulation, there are no problems with solubility, and there is no problem of the granules remaining undissolved in textile products after washing. However, the inventors have discovered that storing beneficial ingredient delivery particles at relatively high temperatures can result in the generation of water-insoluble matter during washing, which can cause problems.

[0006] The present invention provides benefit agent delivery particles having improved solubility after storage at elevated temperatures (e.g., 40-50°C), and methods for improving the solubility of benefit agent delivery particles after storage at elevated temperatures (e.g., 40-50°C). [Means for solving the problem]

[0007] The present invention relates to beneficial ingredient delivery particles comprising (A1) a water-soluble inorganic excipient (hereinafter referred to as component (A1)), (A2) a water-insoluble inorganic excipient (hereinafter referred to as component (A2)), (B) a beneficial ingredient (hereinafter referred to as component (B)), (C) a polyalkylene glycol having a weight-average molecular weight of 2,000 to 20,000 (hereinafter referred to as component (C)), and (D) a polyhydric alcohol having a molecular weight of 60 to 200 (hereinafter referred to as component (D)), wherein the mass ratio (A1) / [(A1)+(A2)] of the content of component (A1) to the total content of components (A1) and (A2) is 0.80 to 1.0, and the mass ratio (D) / (C) of the content of component (D) to the content of component (C) is 0.01 to 0.2.

[0008] The present invention also relates to a method for improving the solubility of beneficial ingredient delivery particles after storage, comprising the steps of: adding the (D) component to beneficial ingredient delivery particles containing the (A1), (A2), (B), and (C) components, wherein the mass ratio (A1) / [(A1)+(A2)] of the content of the (A1) component to the total content of the (A1) and (A2) components is 0.80 or more and 1.0 or less; and adding the (D) component to the beneficial ingredient delivery particles such that the mass ratio (D) / (C) of the content of the (D) component to the content of the (C) component in the beneficial ingredient delivery particles is 0.01 or more and 0.2 or less. [Effects of the Invention]

[0009] According to the present invention, there are provided beneficial agent delivery particles having improved solubility after storage at elevated temperatures (e.g., 40-50°C), and a method for improving the solubility of beneficial agent delivery particles after storage at elevated temperatures (e.g., 40-50°C). DETAILED DESCRIPTION OF THE INVENTION

[0010] The reasons why the beneficial ingredient delivery particles of the present invention have improved solubility after storage at high temperatures (e.g., 40-50°C) and why the method of the present invention improves the solubility of beneficial ingredient delivery particles after storage at high temperatures (e.g., 40-50°C) are not entirely clear, but are presumed to be as follows. In the case of particles containing beneficial ingredients in inorganic excipients, polyalkylene glycols such as polyethylene glycol are often used as binders to stabilize the particles and improve their strength. However, the inventors have found that when these particles are stored at high temperatures, the polyalkylene glycols increase in crystallinity or transition to a highly oriented crystalline state, raising their melting point. As a result, the dissolution rate of the polyalkylene glycols decreases and the amount of water-insoluble matter increases. In the present invention, beneficial ingredient delivery particles containing a water-soluble inorganic excipient (A1), a water-insoluble inorganic excipient (A2), a beneficial ingredient (B), and a specific polyalkylene glycol (C) are incorporated with a specific polyhydric alcohol (D), and the mass ratios (A1) / [(A1)+(A2)] and (D) / (C) are set within specific ranges. This is presumably because the (D) component has a high affinity with the (C) component, and therefore it is possible to suppress the high melting point of the polyalkylene glycol as described above, and it is believed that this has resulted in the improvement of solubility after storage at high temperatures, which is the objective of the present invention. However, the present invention is not limited to the above-mentioned mechanism of action.

[0011] The benefit agent delivery particles of the present invention contain, as component (A1), a water-soluble inorganic excipient. In the present invention, the water-soluble inorganic excipient refers to an inorganic excipient that dissolves in an amount of 1.0 g or more in 100 g of water at 20°C.

[0012] Examples of component (A1) include one or more water-soluble inorganic excipients selected from alkali metal sulfates, alkaline earth metal sulfates, alkali metal hydrogen sulfates, alkaline earth metal hydrogen sulfates, alkali metal chlorides, and alkaline earth metal chlorides. From the viewpoints of safety for the human body and ease of production, one or more water-soluble inorganic excipients selected from alkali metal sulfates, alkaline earth metal sulfates, alkali metal chlorides, and alkaline earth metal chlorides are preferred. Specifically, one or more water-soluble inorganic excipients selected from sodium sulfate, magnesium sulfate, and sodium chloride are more preferred, and one or more water-soluble inorganic excipients selected from sodium sulfate and magnesium sulfate are even more preferred.

[0013] The beneficial agent delivery particles of the present invention optionally contain a water-insoluble inorganic excipient as component (A2) from the viewpoints of manufacturing and strength of the delivery particles. In the present invention, the water-insoluble inorganic excipient refers to an inorganic excipient that dissolves in an amount of less than 1.0 g in 100 g of water at 20°C.

[0014] The component (A2) includes one or more water-insoluble inorganic excipients selected from amorphous aluminosilicates, calcium silicate, silicon oxide, and crystalline aluminosilicates.

[0015] Examples of amorphous aluminosilicates include Aluminum Silicate P820 (manufactured by Degussa) and TIXOLEX 25 (manufactured by Hanfutsu Chemical Co., Ltd.), and those represented by the following general formula are also preferably used: These compounds are characterized by having ion exchange capacity. xM2O·Al2O3·ySiO2·wH2O (where M represents an alkali metal such as sodium or potassium, and x, y, and w represent the number of moles of each component within the following ranges: 0.2≦x≦2.0; 0.5≦y≦10.0; and w is any positive number including 0) xMeO·yM2O·Al2O3·zSiO2·wH2O (where Me represents an alkaline earth metal such as calcium or magnesium, and M represents an alkali metal such as sodium or potassium, and x, y, z, and w represent the number of moles of each component within the following ranges: 0.001≦x≦0.1; 0.2≦y≦2.0; 0.5≦z≦10.0; and w is any positive number including 0)

[0016] Examples of calcium silicate include Fluorite R (manufactured by Tokuyama Soda Co., Ltd.) and HUBERSORBR 600 (manufactured by Huber).

[0017] Specific examples of silicon oxide include white carbon, and more specific examples include ordinary white carbon and calcined white carbon. Ordinary white carbon is a general term for amorphous silicon dioxide made of SiO2, and is divided into precipitated silica and fumed silica depending on the manufacturing method. Calcined white carbon is white carbon obtained by treating ordinary white carbon at high temperature to hydrophobize the silanol groups on the surface.

[0018] Crystalline aluminosilicates are generally known as zeolites, and are represented by the following formula (1): a'(M2O)·Al2O3·b'(SiO2)·w(H2O) (1) (In the formula, M represents an alkali metal atom, a', b', and w represent the number of moles of each component, generally 0.7≦a'≦1.5, 0.8≦b'<6, and w is any positive number.) Among them, those represented by the following general formula (2): Na2O·Al2O3·n(SiO2)·w(H2O) (2) (where n is a number between 1.8 and 3.0, and w is a number between 1 and 6.) Preferably, the compound represented by the formula: As the crystalline aluminosilicate (zeolite), synthetic zeolites having an average primary particle size of 0.1 to 10 μm, such as A-type, X-type, and P-type zeolites, are preferably used. Zeolites may be used in the form of powder and / or dried zeolite agglomerated particles obtained by drying zeolite slurry.

[0019] From the viewpoint of oil absorption capacity and ensuring the strength of the beneficial ingredient delivery particles, component (A2) is preferably one or more water-insoluble inorganic excipients selected from silicon oxide and calcium silicate, and more preferably silicon oxide.

[0020] In the beneficial ingredient delivery particles of the present invention, the content of component (A1) is preferably 30% by mass or more, more preferably 45% by mass or more, even more preferably 55% by mass or more, and even more preferably 60% by mass or more, from the viewpoint of ensuring the solubility of the beneficial ingredient delivery particles, and is preferably 85% by mass or less, more preferably 80% by mass or less, even more preferably 75% by mass or less, and even more preferably 70% by mass or less, from the viewpoint of ensuring the moisture resistance of the beneficial ingredient delivery particles.

[0021] In the beneficial ingredient delivery particles of the present invention, the content of component (A2) is preferably 3% by mass or more, more preferably 4% by mass or more, and even more preferably 6% by mass or more, from the viewpoint of ensuring the strength of the granulated beneficial ingredient delivery particles, and is preferably 20% by mass or less, more preferably 15% by mass or less, and even more preferably 10% by mass or less, from the viewpoint of ensuring the solubility of the granulated beneficial ingredient delivery particles.

[0022] In the beneficial ingredient delivery particles of the present invention, the mass ratio (A1) / [(A1)+(A2)] of the content of component (A1) to the total content of components (A1) and (A2) is preferably 0.80 or more, more preferably 0.82 or more, even more preferably 0.85 or more, and preferably 1.0 or less, more preferably 0.95 or less, even more preferably 0.92 or less, from the viewpoint of achieving both solubility and robustness of the beneficial ingredient delivery particles.

[0023] The benefit agent delivery particles of the present invention contain a benefit agent as component (B). Component (B) may be a beneficial ingredient, preferably a beneficial ingredient for textiles. That is, the benefit ingredient delivery particle of the present invention may be a particle for delivering component (B) to textiles. Therefore, component (B) may be a compound that is beneficial to textiles and is not easily adsorbed to textiles during a normal washing process.

[0024] 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, it 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.

[0025] Component (B) may also be a compound exhibiting a ClogP of preferably 1.0 or more and 30 or less. ClogP is preferably 1.5 or more, more preferably 2 or more, even 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. A ClogP value within this range ensures good support and retention on component (A1) and / or component (A2). "Supported" here refers to a state in which component (B) is adsorbed on the surface of component (A1) and / or component (A2), preferably on the outer surface of component (A1) and / or component (A2), and on the inner surfaces of pores present on the surface of component (A1) and / or component (A2).

[0026] Here, the logP value is the logarithm of the 1-octanol / water partition coefficient of a compound, and means the ratio of the equilibrium concentrations of the solute in each solvent at partition equilibrium when the compound is dissolved as a solute in a two-phase solvent system of 1-octanol and water. It is generally expressed in the form of a logarithm to the base 10, "logP." The logP value can be calculated using the program "CLOGP" (DaylightCIS) or the like. In the program "CLOGP," the logP value is calculated by the method described in "A. Leo in "Comprehensive Medicinal Chemistry", Vol. 4, (C. Hansch, PG Sammes, The "calculated log P (ClogP)" is calculated by the method described in "J.B. Taylor and C.A. Ramsden, Eds.), p. 295, Pergamon Press, 1990," and is a ClogP value calculated using the program CLOGP v4.01. When multiple beneficial ingredients are contained, the ClogP value of the beneficial ingredient mixture can be calculated by multiplying the ClogP value of each beneficial ingredient by its volume ratio in the beneficial ingredient mixture and then summing the results.

[0027] 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 ability of component (A1) and / or component (A2) to support and retain component (B), 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, using a contact angle meter "DropMaster DM-501" (trade name, manufactured by Kyowa Interface Science Co., Ltd.).

[0028] Specific examples of component (B) include one or more 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 ingredient delivery particles of the present invention are used in textile products, component (B) is preferably one or more selected from (B1) fragrances and fragrance precursors (hereinafter referred to as component (B1)), (B2) disinfectants (hereinafter referred to as component (B2)), and (B3) antioxidants (hereinafter referred to as component (B3)).

[0029] The fragrance of component (B1) is not particularly limited, but examples thereof include fragrance compounds described in Nakajima Mototaka, "Fundamentals of Fragrance and Fragrance Blending," 4th edition, Sangyo Tosho Co., Ltd., April 20, 2005, and fragrance compounds known to be incorporated into fabric softeners through patent documents. The fragrance compounds may be a single compound or a mixture of two or more compounds. Also, fragrance components or blended fragrance compositions independently prepared by fragrance manufacturers can be used. The fragrance may be a single fragrance compound or a fragrance composition containing two or more of the fragrance compounds, and the fragrance composition may contain a fragrance diluent or solvent in addition to the fragrance compound. Furthermore, fragrance precursors can be used as the fragrance.

[0030] From the viewpoint of the ability to be supported and retained on the component (A1) and / or the component (A2), the fragrance compound as the component (B1) may be a fragrance compound having a ClogP value of 1.0 or more and 6.0 or less, and 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.

[0031] Examples of the fragrance compound of component (B1) include the following fragrance compounds, and one or more of these can be used: Here, the numbers in parentheses are ClogP values. Amyl cinnamic aldehyde (4.3), 2-methylundecanal (4.7), ethyl 3-methyl-3-phenyloxirane-2-carboxylate (3.0), allyl amyl glycolate (2.3), allyl caproate (3.2), allyl cyclohexyl propionate (4.5), allyl heptanoate (3.2), ambrettolide (5.4), Ambroxan (4.8), amyl salicylate (4.6), isoamyl salicylate (4.5), benzyl benzoate (4.0), benzyl salicylate (4.3), acetic acid Benzyl (2.0), bougeonal (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), decanal (3.8), dihydromyrcenol (3.5), dimethyltetrahydrobenzaldehyde (2.9), diphenyl oxide (4.1), (1-cyclohexyl-2-methylpropan-2-yl) butanoate (4.4), ethylene brassylate (4.7), ethylene dodecanedioate (4.2), ethyl-2-methylbutyrate (2.3), ethyl vanillin (1.6), eugenol (2.7), Flute (registered trademark) (3.6), geraniol (3 .5), Geranyl Acetate (4.5), Geranyl Nitrile (3.9), Hexyl Cinnamic Aldehyde (4.8), Hexyl Acetate (4.8), Hexyl Salicylate (5.1), Cis-3-Hexenyl Salicylate (4.8), Iso E Super (5.2), α-Ionone (3.9), β-Ionone (4.4), Propan-2-yl-2-methylbutanoate (2.7), Javanol® (4.7), Lilial® (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 yarayara (3.3), γ-nonalactone (2.1), nonanal (3.3), octanal (2.8), phenylhexanol (3.5), propane- 2-yl-2-methylbutanoate (2.7), Sandal Mysore Core® (4.7), Terpineol (3.3), Terpinyl acetate (4.3), Tetrahydrolinalool (3.6), Tricyclodecenyl acetate (2.9), Tricyclodecenyl propionate (3.3), γ-Undecalactone (3.1), Ethylene bresylate (4.7), Florosa (2), Isoamyl acetate (2.3), Stearyl acetate (2.5), Triplal (2.9), Dynascon® (4.5).

[0032] Examples of the fragrance precursor (B1) include compounds that release fragrance components in response to water and light. Examples of compounds that release fragrance components in response to water include silicate ester compounds having an alkoxy component derived from a fragrance alcohol, fatty acid ester compounds having an alkoxy component derived from a fragrance alcohol, acetal compounds or hemiacetal compounds obtained by reacting a carbonyl component derived from a fragrance aldehyde or fragrance ketone with an alcohol compound, Schiff base compounds obtained by reacting a carbonyl component derived from a fragrance aldehyde or fragrance ketone with a primary amine compound, and hemiaminal compounds or hydrazone compounds obtained by reacting a carbonyl component derived from a fragrance aldehyde or fragrance ketone with a hydrazine compound. Examples of compounds that release 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, and coumaric acid ester compounds having an alkoxy component derived from a fragrance alcohol. These perfume precursors may be used as polymers such as reaction products of some carboxy groups of polyacrylic acid with perfume alcohols.

[0033] Examples of the bactericide component (B2) include triclosan (ClogP: 5.5), diclosan (ClogP: 4.9), 3-methyl-4-isopropylphenol (ClogP: 3.4), phenoxyethanol (ClogP: 1.39), and benzyl alcohol (ClogP: 1.1), and one or more selected from the above can be used.

[0034] Examples of the antioxidant of component (B3) include butylhydroxytoluene (BHT / ClogP: 5.2), butylhydroxyanisole (ClogP: 3.0), tocopherol (ClogP: 13.0), and distyrenated cresol (ClogP: 1 to 1.94), and one or more selected from the above can be used.

[0035] In the beneficial agent delivery particles of the present invention, the content of component (B) is preferably 0.05% by weight or more, more preferably 0.1% by weight or more, even more preferably 1.0% by weight or more, even more preferably 2.0% by weight or more, even more preferably 3.0% by weight or more, and preferably 20% by weight or less, more preferably 15% by weight or less, even more preferably 12% by weight or less.

[0036] When the beneficial agent delivery particles of the present invention contain component (B1), the content of component (B1) is preferably 1.0% by mass or more, more preferably 3.0% by mass or more, even more preferably 4.0% by mass or more, even more preferably 6.0% by mass or more, even more preferably 8.0% by mass or more, and preferably 20% by mass or less, more preferably 15% by mass or less, even more preferably 12% by mass or less.

[0037] When the beneficial agent delivery particles of the present invention contain component (B2), the content of component (B2) is preferably 0.05% by mass or more, more preferably 0.10% by mass or more, and preferably 0.50% by mass or less, more preferably 0.30% by mass or less.

[0038] When the beneficial agent delivery particles of the present invention contain component (B3), the content of component (B3) is 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.

[0039] The benefit ingredient delivery particles of the present invention contain component (C), a polyalkylene glycol having a weight average molecular weight of 2,000 or more and 20,000 or less.

[0040] Component (C) may be one or more selected from polyethylene glycol, polypropylene glycol, and a random or block adduct of ethylene oxide and propylene oxide. From the viewpoint of production, such as ease of handling of the raw materials during granulation and high handleability, it is preferably one or more selected from polyethylene glycol and polypropylene glycol, and more preferably polyethylene glycol.

[0041] The weight average molecular weight of component (C) is 2,000 or more, preferably 3,000 or more, more preferably 4,000 or more, even more preferably 6,000 or more, and 20,000 or less, preferably 15,000 or less, even more preferably 13,000 or less, and even more preferably 10,000 or less, from the viewpoint of preventing stickiness of the delivery particle surface during storage in a high-temperature environment and ensuring the solubility of the delivery particle. The weight-average molecular weight of component (C) is determined by gel permeation chromatography (GPC) using a mixed solution of acetonitrile and water (phosphate buffer solution) as the developing solvent and polyethylene glycol as the standard.

[0042] In the beneficial ingredient delivery particles of the present invention, the content of component (C) is preferably 8% by mass or more, more preferably 10% by mass or more, even more preferably 11.5% by mass or more, and preferably 30% by mass or less, more preferably 25% by mass or less, even more preferably 20% by mass or less, even more preferably 15% by mass or less, even more preferably 12.5% ​​by mass or less, and even more preferably 12.0% by mass or less, from the viewpoint of suppressing the evaporation of the beneficial ingredient from the beneficial ingredient delivery particles and the solubility of the beneficial ingredient delivery particles.

[0043] The benefit agent delivery particles of the present invention contain component (D), a polyhydric alcohol having a molecular weight of 60 or more and 200 or less.

[0044] From the viewpoint of the solubility of the beneficial agent delivery particles, component (D) is preferably a dihydric or trihydric alcohol having 2 to 6 carbon atoms which may be separated by an ether group. Specific examples of the component (D) include one or more selected from ethylene glycol, propylene glycol, butylene glycol, glycerin, diethylene glycol, dipropylene glycol, dibutylene glycol, pentanediol, and hexanetriol. From the viewpoint of the solubility of the beneficial substance delivery particles, component (D) is preferably one or more selected from propylene glycol, ethylene glycol, and glycerin, more preferably one or more selected from propylene glycol and glycerin, and even more preferably propylene glycol.

[0045] In the beneficial ingredient delivery particles of the present invention, the content of component (D) is preferably 0.1% by mass or more, more preferably 0.3% by mass or more, even more preferably 0.5% by mass or more, even more preferably 0.6% by mass or more, even more preferably 0.8% by mass or more, even more preferably 1.0% by mass or more, and preferably 5% by mass or less, more preferably 3% by mass or less, even more preferably 2% by mass or less, and even more preferably 1.5% by mass or less, from the viewpoint of preventing a decrease in solubility of the beneficial ingredient delivery particles after storage and preventing stickiness on the surface of the beneficial ingredient delivery particles.

[0046] In the beneficial ingredient delivery particles of the present invention, the mass ratio (D) / (C) of the content of component (D) to the content of component (C) is 0.01 or more, preferably 0.02 or more, more preferably 0.03 or more, even more preferably 0.05 or more, even more preferably 0.07 or more, even more preferably 0.08 or more, and 0.2 or less, preferably 0.15 or less, more preferably 0.12 or less, from the viewpoint of suppressing the decrease in solubility of the beneficial ingredient delivery particles after storage and suppressing stickiness of the beneficial ingredient delivery particle surface.

[0047] The beneficial ingredient delivery particles of the present invention may contain a polysaccharide as component (E) from the viewpoint of the solubility and stability of the beneficial ingredient delivery particles.

[0048] The polysaccharide of component (E) may be one or more selected from dextrin, cellulose and its derivatives, starch, locust bean gum, guar gum, pullulan, chitin, chitosan, agarose, carrageenan, curdlan, etc., and from the viewpoint of preventing leakage of beneficial ingredients from the delivery particles and the solubility of the delivery particles, it is preferably one or more selected from dextrin, cellulose and its derivatives, and starch, and more preferably dextrin.

[0049] Dextrin is obtained by partial hydrolysis of starch. Starch molecules are gradually broken down into smaller molecules through hydrolysis, ultimately becoming glucose. Depending on the degree of hydrolysis, a mixture of various sugars is produced. For example, the dextrin used in the present invention may be water-soluble starch, modified starch, or a derivative thereof, such as one or more selected from esterified starch (e.g., starch phosphate), etherified starch (e.g., carboxymethylated starch), enzyme-modified dextrin (e.g., maltodextrin), and roasted dextrin. Furthermore, it is preferable to use starch prepared by mixing, in a predetermined ratio, non-reducing end starch having a dextrose equivalent value (hereinafter referred to as DE value) of 0 to 8, as defined by the following formula, with water-soluble starch, modified starch, or a derivative thereof in which the glucose end has been converted to a reducing end by hydrogenation. Non-reducing end starch is starch in which both ends are non-reducing ends (having no reducing ends).

[0050] DE value = [direct reducing sugars (expressed as glucose) / solids] x 100 In particular, the dextrin is preferably one having a DE value in the range of 0 to 8 and having been subjected to hydrogenation treatment, and more preferably one containing a starch carrier mixed with starch having a DE value in the range of 0 to 3 and having a glucose end as a reducing end.

[0051] Starch hydrolysis can be carried out by standard methods such as acid-catalyzed or enzyme-catalyzed methods. Specific examples of dextrins include those produced by the method described in Japanese Patent Application Laid-Open No. 8-143603. Among these dextrins, dextrins with a specific volume of 5 m3 or less are preferred due to their oil absorption capacity. 2 / g or more 10m 2 The glass transition temperature of dextrin is preferably 200° C. or higher from the viewpoint of stability at high temperatures.

[0052] The cellulose and its derivatives include one or more selected from carboxymethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, cationized cellulose, and the like. The starch may be one or more selected from corn starch, wheat starch, potato starch, tapioca starch, and the like.

[0053] When the beneficial ingredient delivery particles of the present invention contain component (E), the content of component (E) is, from the viewpoint of ensuring the stability of the beneficial ingredient and the strength of the delivery particles, preferably 1% by mass or more, more preferably 1.5% by mass or more, even more preferably 2.0% by mass or more, even more preferably 3.0% by mass or more, and preferably 35% by mass or less, more preferably 30% by mass or less, even more preferably 25% by mass or less, even more preferably 20% by mass or less, even more preferably 15% by mass or less, even more preferably 10% by mass or less, and even more preferably 8.0% by mass or less.

[0054] The beneficial agent delivery particles of the present invention may contain other ingredients such as fragrances encapsulated in microcapsules, water-soluble cationic polymeric compounds, cationic surfactants, organic solvents, pigments, dyes, etc. (excluding those that fall under components (A1), (A2), (B), (C), (D), and (E)).

[0055] The beneficial ingredient delivery particles of the present invention are not particularly limited, but may preferably be spherical, hemispherical, cylindrical, granular, or powder-like, and from the standpoint of appearance and usability, spherical, hemispherical, or cylindrical shapes are preferred.

[0056] From the viewpoint of solubility and handleability, the beneficial agent delivery particles of the present invention may have an average particle size of preferably 1.0 mm or more, more preferably 1.2 mm or more, even more preferably 1.5 mm or more, and preferably 20 mm or less, more preferably 15 mm or less, even more preferably 10 mm or less, still more preferably 5 mm or less, and even more preferably 3 mm or less. The average particle size can be measured by calculating the spherical equivalent diameter of 250 particles using image analysis software ImageJ.

[0057] The bulk density of the benefit agent delivery particles of the present invention may be, from the viewpoint of the volume when a predetermined amount of particles is measured, preferably 400 g / L or more, more preferably 500 g / L or more, even more preferably 600 g / L or more, and even more preferably 700 g / L or more, and from the viewpoint of ease of use and solubility during use, preferably 1000 g / L or less, more preferably 900 g / L or less. Bulk density can be measured using a bulk specific gravity measuring device in accordance with JIS K7365.

[0058] The benefit agent delivery particles of the present invention are prepared by mixing components (A1), (A2), (B), (C), and (D) in specific weight ratios. That is, the present invention relates to a method for producing beneficial ingredient delivery particles, in which components (A1), (A2), (B), and (C) are mixed in such a manner that the mass ratio (A1) / [(A1)+(A2)] of the amount of component (A1) to the total amount of component (A1) and component (A2) is 0.80 or more and 1.0 or less, and the mass ratio (D) / (C) of the amount of component (D) to the amount of component (C) is 0.01 or more and 0.2 or less. In the method for producing benefit agent delivery particles of the present invention, component (E) can be further mixed. In the method for producing the benefit ingredient delivery particles of the present invention, the other ingredients described above can be further mixed. In the method for producing the beneficial agent delivery particle of the present invention, the aspects described for the beneficial agent delivery particle of the present invention can be appropriately applied, and the components (A1), (A2), (B), (C), (D), and (E) are the same as those described for the beneficial agent delivery particle of the present invention. In the method for producing beneficial ingredient delivery particles of the present invention, the mixed amount of component (A1), the mixed amount of component (A2), the mass ratio (A1) / [(A1)+(A2)] of the mixed amount of component (A1) to the total mixed amount of component (A1) and component (A2), the mixed amount of component (B), the mixed amount of component (C), the mixed amount of component (D), the mass ratio (D) / (C) of the mixed amount of component (D) to the mixed amount of component (C), and the mixed amount of component (E) can be appropriately applied by replacing the content of each component with the mixed amount for the content and mass ratio range of each component described for beneficial ingredient delivery particles of the present invention.

[0059] Specifically, as one example, the method for producing the beneficial agent delivery particles of the present invention includes the following steps: Half of component (A1), component (A2), component (D), and optional component (E) are mixed at room temperature to obtain powder mixture (1). Powder mixture (1) is then heated to 75°C, and the remaining half of component (A1) is added to obtain powder mixture (2). After the temperature of powder mixture (2) reaches 60°C, components (B) and (C) are added to powder mixture (2) and further mixed to obtain powder mixture (3). The resulting powder mixture (3) is extruded through a 2.0 mm sieve using an extrusion granulator (e.g., manufactured by Dalton Co., Ltd.) and granulated by compression molding. The resulting granules are then cooled and milled and sized using a power mill (e.g., manufactured by Dalton Co., Ltd.) to obtain beneficial ingredient delivery particles.

[0060] The mixer used to mix component (A1), component (A2), component (B), component (C), component (D), and any optional components is not particularly limited as long as it can mix them substantially uniformly. It may be a mixer equipped with a heating means, and examples thereof include a Henschel mixer (e.g., manufactured by Mitsui Mining Co., Ltd.), a high-speed mixer (e.g., manufactured by Fukae Kogyo Co., Ltd.), a ribbon mixer (e.g., manufactured by Tokuju Kogyosho Co., Ltd.), a Nauta mixer (e.g., manufactured by Hosokawa Micron Corporation), a V-type blender (e.g., manufactured by Dalton Corporation), and a container-rotating granulator (e.g., manufactured by Sugiyama Heavy Industries Co., Ltd.).

[0061] The mixture can be compression-molded to obtain granules using a known extrusion granulator such as a disc pelletizer (e.g., manufactured by Fuji Paudal Co., Ltd.), a basket-type granulator (e.g., manufactured by Kikusui Seisakusho Co., Ltd.), a granulator (e.g., manufactured by Hosokawa Micron Corporation), or the horizontal extrusion screw-type extrusion granulator described in JP-A-10-192688. A kneading extrusion device such as Extrude-O-Mix (e.g., manufactured by Hosokawa Micron Corporation) can also be used.

[0062] The granules are cooled to prevent the compression-molded product from coalescing or clumping, and then sized. The equipment used to size the extrusion granules is not particularly limited. That is, any known pulverizer (or crusher) can be used. Examples include high-speed mixers (e.g., manufactured by Fukae Industries Co., Ltd.), Marumerizers (e.g., manufactured by Fuji Paudal Co., Ltd.), Spiraflow (e.g., manufactured by Freund Corporation), Fitzmills (e.g., Dalton), Powermills (e.g., manufactured by Powrex Corporation), and Comils (e.g., manufactured by Quadro). From the viewpoint of the amount of fine powder generated and productivity, it is preferable to use a pulverizer such as a power mill with a knife cutter or a Comil, which crushes particles by pressing them against an impeller and a screen.

[0063] A power mill is a device disclosed in, for example, Japanese Patent Application Laid-Open No. 5-96195, and is shaped as shown in FIG. 1, and is a piece of equipment having a cutter blade 1 and a cylindrical screen 2. Particles fed into the power mill inlet fall freely within the power mill, and during this natural fall they are crushed and sized by the crushing blades attached to the cutter blade 1.

[0064] The Comill is a device disclosed in, for example, US Pat. No. 4,759,507, and has a configuration as shown in Fig. 2, and is equipped with an impeller 3 and a screen 4. Particles fed into the Comill inlet are pressed against the screen 4 by the centrifugal force generated by the rotating impeller 3. Small particles instantly rise on the vortex flow generated by the conical shape, and then, as they descend, they are crushed and sized by the impeller 3.

[0065] The beneficial agent 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 attaching beneficial agents to textile products, in which the beneficial agent delivery particles are added to the textile products during the washing process to treat the textile products.

[0066] When the benefit agent delivery particles of the present invention are added to textiles during the washing process, the amount of the benefit agent delivery particles of the present invention added is preferably 3.0 g or more, more preferably 5.0 g or more, and preferably 16.0 g or less, more preferably 12.0 g or less per 1 kg of textiles. The textiles can be treated with the benefit agent delivery particles of the present invention alone, or they can be treated with a textile treatment composition containing the benefit agent delivery particles of the present invention.

[0067] When the beneficial agent delivery particles of the present invention are added during the washing process of textile products, the beneficial agent delivery particles of the present invention can be added to at least one of the washing water and the rinsing water of the laundry, or the beneficial agent delivery particles of the present invention can be added to both the washing water and the rinsing water of the laundry.

[0068] When adding the beneficial agent delivery particles of the present invention to the washing process of textile products, the beneficial agent delivery particles are preferably added to the water at a concentration of 10 ppm or more, more preferably 100 ppm or more, and preferably 2,000 ppm or less, more preferably 1,000 ppm or less. From the viewpoint of convenience when adding to a washing machine, it is preferable to use them in the wash water, but it is also possible to add them to the rinse water. The wash water and rinse water for washing may contain textile laundry detergent components.

[0069] The present invention relates to a method for improving the solubility of beneficial agent delivery particles after storage, comprising: (A1) component, (A2) component, (B) component, and (C) component; wherein the mass ratio (A1) / [(A1)+(A2)] of the content of component (A1) to the total content of components (A1) and (A2) is 0.80 or more and 1.0 or less; and (D) component in the beneficial agent delivery particles, such that the mass ratio (D) / (C) of the content of component (D) to the content of component (C) in the beneficial agent delivery particles is 0.01 or more and 0.2 or less. The beneficial ingredient delivery particles targeted by the method of the present invention for improving the solubility of beneficial ingredient delivery particles after storage are the beneficial ingredient delivery particles of the present invention, and the matters described for the beneficial ingredient delivery particles of the present invention can be applied as appropriate. Components (A1), (A2), (B), (C), (D), and (E) are the same as those described for the benefit agent delivery particles of the present invention. Furthermore, the phrase "containing component (A1), component (A2), component (B), and component (C) in a beneficial ingredient delivery particle in which the mass ratio (A1) / [(A1)+(A2)] of the content of component (A1) to the total content of component (A1) and component (A2) is 0.80 or more and 1.0 or less, and component (D) is contained in the beneficial ingredient delivery particle in such a way that the mass ratio (D) / (C) of the content of component (D) to the content of component (C) in the beneficial ingredient delivery particle is 0.01 or more and 0.2 or less" does not specify the order in which component (A), component (B), component (C), and component (D) are added to the fragrance delivery particle, and there is no restriction on the order in which each component is added.

[0070] In the method of improving the solubility of beneficial ingredient delivery particles of the present invention after storage, component (D) is contained in the beneficial ingredient delivery particles of the present invention in an amount of preferably 0.1% by mass or more, more preferably 0.3% by mass or more, even more preferably 0.5% by mass or more, even more preferably 0.6% by mass or more, even more preferably 0.8% by mass or more, even more preferably 1.0% by mass or more, and preferably 5% by mass or less, more preferably 3% by mass or less, even more preferably 2% by mass or less, and even more preferably 1.5% by mass or less, from the standpoint of preventing a decrease in solubility of the beneficial ingredient delivery particles after storage and preventing stickiness on the surface of the beneficial ingredient delivery particles.

[0071] In the method of improving the solubility of beneficial ingredient delivery particles of the present invention after storage, the beneficial ingredient delivery particles of the present invention contain component (D) such that the mass ratio (D) / (C) of the content of component (D) to the content of component (C) in the beneficial ingredient delivery particles is 0.01 or more, preferably 0.02 or more, more preferably 0.03 or more, even more preferably 0.05 or more, even more preferably 0.07 or more, even more preferably 0.08 or more, and 0.2 or less, preferably 0.15 or less, more preferably 0.12 or less, from the viewpoint of suppressing a decrease in solubility of the beneficial ingredient delivery particles after storage and suppressing stickiness of the surface of the beneficial ingredient delivery particles.

[0072] In the method for improving the solubility of beneficial ingredient delivery particles of the present invention after storage, the content of component (A1), the content of component (A2), the mass ratio (A1) / [(A1)+(A2)] of the content of component (A1) to the total content of components (A1) and (A2), the content of component (B), the content of component (C), and the content of component (E) in the beneficial ingredient delivery particles of the present invention are the same as the ranges described for the beneficial ingredient delivery particles of the present invention. [Example]

[0073] The components used in the Examples, Comparative Examples, and Formulation Examples are listed below.

[0074] <Component (A1)> · Glauber's salt: Sodium sulfate, manufactured by Shikoku Kasei Kogyo Co., Ltd. (crushed A0 Glauber's salt) <(A2) component> White carbon (silica): Amorphous silicon dioxide made from SiO2, manufactured by Tokuyama Corporation

[0075] <(B) component> Fragrance composition 1: A fragrance composition consisting of the fragrance compounds shown in Table 1 below.

[0076] [Table 1]

[0077] <(C) component> Polyethylene glycol: Polyethylene glycol, molecular weight 8,200, manufactured by Kao Corporation <(D) component> Propylene glycol: Propylene glycol, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd. Glycerin: Fujifilm Wako Pure Chemical Industries, Ltd. Dipropylene glycol: Fujifilm Wako Pure Chemical Industries, Ltd. <(E) component> Dextrin: Dextrin CZRM-X, manufactured by Nippon Starch Chemical Co., Ltd.

[0078] Preparation of Beneficial Agent Delivery Particles Half of the (A1) component was mixed with the (A2), (D), and (E) components at room temperature in a Nauta mixer (NX-S model, manufactured by Hosokawa Micron Corporation) to obtain powder mixture (1). The jacket temperature was then raised to 90°C, and the powder mixture (1) was heated to 75°C. The remaining half of the (A1) component was then added. After the internal temperature reached 60°C, component (B) was added and mixed to obtain powder mixture (2). Next, pre-melted component (C) was added to powder mixture (2) and further mixed to obtain powder mixture (3). The resulting powder mixture (3) was then extruded through a 2.0 mm pore size screen in an extrusion granulator (EXR-60 model, manufactured by Dalton Corporation) and compacted. The resulting granules were then cooled and pulverized in a granulator (Power Mill, P-02S model, manufactured by Dalton Co., Ltd.) to obtain beneficial ingredient delivery particles with the compositions listed in Table 2, with an average particle size of 1.5 mm and a bulk density of 800 g / L.

[0079] [Evaluation of solubility after high-temperature storage] 20 g of each of the prepared beneficial ingredient delivery particles listed in Table 2 was placed in a No. 6 screw tube (Maruem) and left to stand for 30 days in a space regulated at 40°C or 50°C to obtain a high-temperature storage sample. The sample before high-temperature storage was also referred to as the pre-storage sample. A 1-liter beaker (cylindrical, 105 mm inner diameter, 150 mm height, manufactured by Iwaki Glass Co., Ltd.) was filled with 1000 mL of tap water at 5°C, and stirred with a stirrer (35 mm length, 8 mm diameter, thin round Teflon (registered trademark) bar manufactured by ADVANTEC) at a rotation speed (1000 rpm) such that the depth of the vortex was approximately 1 / 3 of the water depth. Each pre-storage sample or each high-temperature-storage sample, weighed out to 1.0 g, was poured into the water in the 1-liter beaker and dispersed under stirring, and stirring was continued to obtain a dispersion. Ten minutes after adding each pre-storage sample or each high-temperature storage sample, the dispersion in the beaker was filtered through a 200-mesh standard sieve (mesh opening: 74 μm, sieve diameter: 110 mm) whose dry weight had been measured in advance (hereinafter, sometimes referred to as "mass known"). The collected dispersion residue, together with the sieve, was placed in an electric dryer heated to 105°C and dried for 1 hour. After removing from the electric dryer and cooling to room temperature, the total mass of the dried dispersion residue and the sieve with known mass was measured to calculate the dry mass (g) of the dispersion residue remaining on the sieve, and the undissolved content (mass%) was calculated using the following formula (1). Undissolved content (mass%)=(T / S)×100 (1) S: Mass of high-temperature storage sample (g) T: Dry mass (g) of the soluble matter of the dispersion remaining on the sieve For samples before storage, solubility was judged as follows: E (Excellent) if the undissolved content (mass%) was less than 0.15% by mass, G (Good) if it was 0.15% by mass or more but less than 0.3% by mass, A (Available) if it was 0.3% by mass or more but less than 0.5% by mass, and B (Bad) if it was 0.5% by mass or more. For samples stored at 40°C for 30 days at high temperature, solubility was judged as follows: E (Excellent) if the undissolved content (mass%) was less than 1% by mass, G (Good) if it was 1% by mass or more but less than 2% by mass, A (Available) if it was 2% by mass or more but less than 4% by mass, and B (Bad) if it was 4% by mass or more. In addition, for samples stored at 50°C for 30 days, the solubility was evaluated as follows: E (Excellent) if the undissolved content (mass%) was less than 1%, G (Good) if it was 1% or more but less than 4%, A (Available) if it was 4% or more but less than 6%, and B (Bad) if it was 6% or more. The results are shown in Table 2.

[0080] [Table 2]

[0081] [Prescription example] Formulation examples of benefit agent delivery particles of the present invention are shown in Table 3. The benefit agent delivery particles of these formulation examples can improve solubility after storage at elevated temperatures (eg, 40-50°C).

[0082] [Table 3]

Claims

1. A beneficial ingredient delivery particle comprising (A1) a water-soluble inorganic excipient (hereinafter referred to as the (A1) component), (A2) a water-insoluble inorganic excipient (hereinafter referred to as the (A2) component), (B) a beneficial ingredient (hereinafter referred to as the (B) component), (C) a polyalkylene glycol having a weight-average molecular weight of 2,000 to 20,000 (hereinafter referred to as the (C) component), and (D) a polyhydric alcohol having a molecular weight of 60 to 200 (hereinafter referred to as the (D) component), wherein the mass ratio (A1) / [(A1)+(A2)] of the content of the (A1) component to the total content of the (A1) component and the (A2) component is 0.80 to 1.0, and the mass ratio (D) / (C) of the content of the (D) component to the content of the (C) component is 0.01 to 0.

2.

2. 10. The benefit agent delivery particle of claim 1, wherein component (A1) is one or more water-soluble inorganic excipients selected from alkali metal sulfates, alkaline earth metal sulfates, alkali metal hydrogen sulfates, alkaline earth metal hydrogen sulfates, alkali metal chlorides, and alkaline earth metal chlorides.

3. 3. The benefit agent delivery particle of claim 1 or 2, wherein component (A2) is one or more water-insoluble inorganic excipients selected from amorphous aluminosilicates, calcium silicate, silicon oxide, and crystalline aluminosilicates.

4. 3. The benefit agent delivery particle of claim 1 or 2, wherein component (D) is a dihydric or trihydric alcohol having 2 to 6 carbon atoms, optionally interrupted by an ether group.

5. A method for improving the solubility of beneficial ingredient delivery particles after storage, comprising: (A1) a water-soluble inorganic excipient (hereinafter referred to as component (A1)); (A2) a water-insoluble inorganic excipient (hereinafter referred to as component (A2)); (B) a beneficial ingredient (hereinafter referred to as component (B)); and (C) a polyalkylene glycol having a weight-average molecular weight of 2,000 to 20,000 (hereinafter referred to as component (C)); wherein the mass ratio (A1) / [(A1)+(A2)] of the content of component (A1) to the total content of components (A1) and (A2) is 0.80 to 1.0; and (D) a polyhydric alcohol having a molecular weight of 60 to 200 (hereinafter referred to as component (D)), such that the mass ratio (D) / (C) of the content of component (D) to the content of component (C) in the beneficial ingredient delivery particles is 0.01 to 0.2.

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