Textile product treatment composition
The textile product treatment composition uses silica-encapsulated microcapsules with a sol-gel formed shell and a water-soluble carrier to prevent disintegration, ensuring stable fragrance delivery to textiles.
Patent Information
- Application Number
- JP2022111216
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2022-07-11
- Publication Date
- 2025-11-27
- Estimated Expiration
- 2042-07-11
AI Technical Summary
Existing fragrance microencapsulation technologies face issues with microcapsules disintegrating during production and storage, leading to inadequate fragrance retention on textiles.
A textile product treatment composition using microcapsules with a silica shell, formed through a sol-gel reaction, and a water-soluble carrier that remains stable at room temperature, ensuring fragrance retention without disintegration during manufacturing and storage.
The composition maintains fragrance encapsulation integrity, allowing for effective fragrance delivery to textiles during wear.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a textile product treatment composition. [Background technology]
[0002] In recent years, the number of people who want to enjoy fragrances when washing and wearing clothes has been increasing. Until now, liquid detergents and liquid fabric softeners have generally been used to scent clothes during washing, but in recent years there has been a trend to use fragrance additives in combination with these detergents to further adjust the variety and strength of the scent.
[0003] As technologies aimed at adding fragrance, for example, Patent Document 1 proposes a method of separately providing a cleaning product and a fragrance-containing product, Patent Document 2 proposes a method of adjusting the fragrance intensity by adding fragrance tablets in which fragrance is impregnated in polyethylene glycol during the washing process, and Patent Document 3 proposes a method of providing a fabric treatment article consisting of a combination of an unscented / lightly scented fabric softener and a fragrance-containing product.
[0004] Generally, fragrances added to liquid fabric softeners are applied to textile products via water during the rinsing process after the washing process. On the other hand, liquid detergents and fragrance additives added during the washing process are exposed to water during the rinsing process after the fragrance is applied to textile products during the washing process. As a result, the fragrance is not sufficiently attached to the textiles, making it difficult to achieve a sufficient fragrance sensation. Various technologies have been proposed to address this problem.
[0005] As a conventional technique for improving fragrance retention during wear, attempts have been made to incorporate microencapsulated fragrances. Patent Document 4 describes an encapsulated fragrance containing a fragrance composition having a flash point in the range of 50 to 130°C as a core substance. Patent Document 5 describes that fragrance retention is improved by using microcapsules encapsulating fragrances produced by the core-shell method. Patent Document 6 describes that the combined use of microcapsules encapsulating fragrances and polymers containing specific amines enables the fragrance to be applied uniformly at high concentrations to multiple different surfaces. [Prior art documents] [Patent documents]
[0006] Patent Document 1: Japanese Patent Application Laid-Open No. 2000-169898 Patent Document 2 Special Publication No. 2013-509508 Patent Document 3: JP 2020-23776 A Patent Document 4: Japanese Patent Application Laid-Open No. 2006-249326 Patent Document 5 Special Publication No. 2011-517323 Patent Document 6: JP 2018-172687 A Summary of the Invention [Problem to be solved by the invention]
[0007] Microencapsulation of fragrances is useful as a means of improving the fragrance effectiveness, and adjusting the strength and disintegration timing of the microcapsules is essential to enable consumers to experience the fragrance at the desired timing during the process of washing and wearing clothes. However, while low-strength microcapsules exhibit excellent fragrance effectiveness while wearing clothes, they have the problem of disintegrating during the process from production to storage of the textile product treatment composition. When such disintegration occurs, it becomes difficult to deliver the fragrance as designed.
[0008] The present invention provides a textile product treatment composition in which the microcapsules do not break down during the production or storage process and which can provide the desired effects to treated textile products. [Means for solving the problem]
[0009] The inventors have discovered a textile product treatment composition that uses capsules that easily disintegrate with low mechanical force, a water-soluble carrier that is solid at room temperature, and a base that is liquid at room temperature, and thereby is able to retain fragrance without the capsules disintegrating during the manufacturing and storage processes.
[0010] The present invention relates to a textile product treatment composition containing the following components (a), (b), and (c): Component (a): 0.1% by mass to 10% by mass of microcapsules having a shell and a core containing a fragrance compound inside the shell (b) Component: 40% by mass or more and 95% by mass or less of polyethylene glycol having a number average molecular weight of 2000 or more and 13000 or less Component (c): At least one compound that is liquid at 30°C and is selected from fatty acids, alcohols, ester oils, ether oils, cationic surfactants, nonionic surfactants, and anionic surfactants. [Effects of the Invention]
[0011] According to the present invention, there is provided a textile product treatment composition in which the capsules do not break down during the manufacturing process or storage process and the perfume can be retained. DETAILED DESCRIPTION OF THE INVENTION
[0012] <Textile product treatment composition> [Component (a)] The textile treatment composition of the present invention contains, as component (a), microcapsules having a shell and a core containing a fragrance compound inside the shell.
[0013] <shell> The shell of component (a) preferably contains silica. Accordingly, as one embodiment, the present invention provides a textile treatment composition containing, as component (a), microcapsules having a shell containing silica as a constituent and a core containing a fragrance compound inside the shell. Silica is a substance whose structural unit is silicon dioxide. Hereinafter, microcapsules having a shell containing silica as a constituent, such as the microcapsules of component (a), will also be referred to as silica capsules. The fragrance compound can be incorporated into the silica capsules as a fragrance composition containing multiple fragrance compounds.
[0014] The shell of the silica capsule of the present invention contains silica as a constituent component. The shell of the silica capsule of the present invention is characterized in that a part or substantially all of the structure constituting the shell is made of silica as a constituent component. The shell of the silica capsule of the present invention is preferably formed by a sol-gel reaction using an alkoxysilane as a precursor. In the present invention, the "sol-gel reaction" refers to a reaction in which an alkoxysilane undergoes hydrolysis and polycondensation to form silica, a component of the shell, through a sol and a gel state. Specifically, for example, tetraalkoxysilane is hydrolyzed, and a silanol compound undergoes a dehydration condensation reaction and a dealcoholization condensation reaction to generate a siloxane oligomer, and the dehydration condensation reaction further proceeds to form silica.
[0015] In addition, the shell of the silica capsule of the present invention may contain an inorganic polymer other than silica as a constituent component, as long as the effect of the present invention is not impaired. In the present invention, the inorganic polymer refers to a polymer containing an inorganic element. Examples of the inorganic polymer include a polymer consisting only of inorganic elements, a polymer whose main chain is composed only of inorganic elements and has an organic group as a side chain or substituent, and the like. The inorganic polymer is preferably a metal oxide containing a metal element or a metalloid element, and more preferably a polymer formed by a reaction similar to the sol-gel reaction of silica using a metal alkoxide [M(OR)x] as a precursor, where M is a metal or metalloid element and R is a hydrocarbon group. Examples of metal or semimetal elements constituting the metal alkoxide include titanium, zirconium, aluminum, and zinc.
[0016] The alkoxysilane is preferably a tetraalkoxysilane from the viewpoint of increasing the encapsulation rate of the fragrance and exhibiting good delivery performance. From the viewpoint of promoting the sol-gel reaction, the tetraalkoxysilane is preferably one having an alkoxy group having from 1 to 4 carbon atoms, more preferably one or more selected from tetramethoxysilane, tetraethoxysilane, and tetraisopropoxysilane, even more preferably one or more selected from tetramethoxysilane and tetraethoxysilane, and still more preferably tetraethoxysilane.
[0017] (Manufacturing of silica capsules) From the viewpoints of increasing the encapsulation rate of the fragrance compound, improving the long-term retention, and achieving good delivery performance of the fragrance compound, the shell of the silica capsule of the present invention preferably contains, as a constituent, silica formed by a two-stage sol-gel reaction. That is, the silica capsule of the present invention is preferably produced by a method including the following steps 1 and 2. Step 1: A step of subjecting an emulsion obtained by emulsifying an aqueous phase component containing a cationic surfactant and an oil phase component containing a fragrance compound and a tetraalkoxysilane to a sol-gel reaction under acidic conditions to form silica capsules (1) having a core and a first shell composed of silica, and obtaining an aqueous dispersion containing the silica capsules (1). Step 2: A step of adding tetraalkoxysilane to the aqueous dispersion containing the silica capsules (1) obtained in Step 1 to carry out a sol-gel reaction, thereby forming silica capsules having a second shell encapsulating the first shell.
[0018] [Process 1] Step 1 is a step of subjecting an emulsion obtained by emulsifying an aqueous phase component containing a cationic surfactant and an oil phase component containing a fragrance compound and a tetraalkoxysilane to a sol-gel reaction under acidic conditions to form silica capsules (1) having a core and a first shell composed of silica, and obtaining an aqueous dispersion containing the silica capsules (1).
[0019] Examples of cationic surfactants used in step 1 include alkylamine salts and alkyl quaternary ammonium salts. The alkylamine salts are preferably salts of secondary amines or tertiary amines, more preferably salts of tertiary amines. The alkylamine salts and alkyl quaternary ammonium salts are compounds 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, i.e., a methyl group. Examples of alkylamine salts include alkylamine salts in which the long-chain alkyl group has the carbon number within the above range, such as long-chain monoalkyl monomethyl secondary amine salts and long-chain monoalkyl dimethyl tertiary amine salts. Examples of quaternary ammonium salts include long-chain alkyl tri-short-chain alkyl quaternary ammonium salts, di-long-chain alkyl di-short-chain alkyl quaternary ammonium salts, and long-chain alkyl benzyl di-short-chain alkyl quaternary ammonium salts, each of which has a long-chain alkyl group and a short-chain alkyl group within the above-mentioned range of carbon number.
[0020] Examples of alkylamine salts include alkylamine acetates such as lauryl dimethylamine acetate and stearyl dimethylamine acetate. Examples of alkyltrimethylammonium salts include alkyltrimethylammonium chlorides such as lauryltrimethylammonium chloride, cetyltrimethylammonium chloride, and stearyltrimethylammonium chloride; and alkyltrimethylammonium bromides such as lauryltrimethylammonium bromide, cetyltrimethylammonium bromide, and stearyltrimethylammonium bromide. Examples of dialkyldimethylammonium salts include dialkyldimethylammonium chlorides such as distearyldimethylammonium chloride; and dialkyldimethylammonium bromides such as distearyldimethylammonium bromide. Examples of alkylbenzyldimethylammonium salts include alkylbenzyldimethylammonium chloride and alkylbenzyldimethylammonium bromide. Of these, the cationic surfactant is preferably a 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.
[0021] In step 1, other emulsifiers may be contained in addition to the cationic surfactant, provided that the effects of the present invention are not impaired. Examples of other emulsifiers include polymer dispersants, nonionic surfactants, anionic surfactants, and amphoteric surfactants.
[0022] In step 1, the content of cationic surfactant in the aqueous phase component is preferably 0.1% by mass or more, more preferably 0.3% by mass or more, and even more preferably 0.4% by mass or more, from the viewpoint of dispersion stability of the emulsified droplets, and is preferably 10% by mass or less, more preferably 5% by mass or less, and even more preferably 2% by mass or less, from the viewpoint of suppressing the formation of emulsifier micelles by excess emulsifier that does not contribute to the dispersion stability of the emulsion and improving encapsulation efficiency.
[0023] The amount of oil phase components relative to the total amount of the emulsion obtained in step 1 is preferably 5% by mass or more, more preferably 10% by mass or more, and even more preferably 15% by mass or more, from the viewpoint of production efficiency, and is preferably 50% by mass or less, more preferably 45% by mass or less, and even more preferably 40% by mass or less, from the viewpoint of obtaining a stable emulsion.
[0024] The amount of tetraalkoxysilane added in step 1 is preferably 10% by mass or more, more preferably 12% by mass or more, and even more preferably 14% by mass or more, relative to the total amount of fragrance compounds in step 1, from the viewpoint of accelerating the sol-gel reaction and forming a sufficiently dense shell, and is preferably 60% by mass or less, more preferably 50% by mass or less, even more preferably 40% by mass or less, and even more preferably 35% by mass or less, from the viewpoint of preventing excess tetraalkoxysilane from remaining in the fragrance compounds.
[0025] Step 1 preferably includes the following steps 1-1 to 1-4. Step 1-1: Step of preparing an aqueous phase component containing a cationic surfactant Step 1-2: Mixing fragrance and tetraalkoxysilane to prepare an oil phase component Step 1-3: A step of mixing and emulsifying the aqueous phase component obtained in Step 1-1 and the oil phase component obtained in Step 1-2 to obtain an emulsion. Step 1-4: A step of subjecting the emulsion obtained in Step 1-3 to a first-stage sol-gel reaction to form silica capsules having a core and a first shell composed of silica.
[0026] The stirring means used in preparing the emulsion is not particularly limited, and may be a homogenizer, high-pressure disperser, ultrasonic disperser, etc., which have a strong shearing force. Also, a homomixer, such as "Disper" (trade name, manufactured by Primix Corporation), "Clearmix" (trade name, manufactured by M Technique Co., Ltd.), or "Cavitron" (trade name, manufactured by Pacific Machinery Works, Ltd.) may be used.
[0027] Median diameter D of the emulsion droplets in the emulsion of step 1 50is preferably 0.1 μm or more, more preferably 0.2 μm or more, and even more preferably 0.3 μm or more, from the viewpoint of reducing the specific surface area relative to the environment outside the silica capsule and improving long-term storage stability, and is preferably 50 μm or less, more preferably 30 μm or less, even more preferably 10 μm or less, even more preferably 5 μm or less, and even more preferably 3 μm or less, from the viewpoint of the physical strength of the silica capsule. Median diameter of emulsion droplets D 50 can be measured by the method described in the Examples.
[0028] The initial pH of the sol-gel reaction in step 1 is preferably 3.0 or higher, more preferably 3.3 or higher, and even more preferably 3.5 or higher, from the viewpoint of maintaining a balance between the hydrolysis reaction and condensation reaction of the tetraalkoxysilane, and from the viewpoint of suppressing the formation of a highly hydrophilic sol and promoting the progress of encapsulation. The initial pH is preferably 4.5 or lower, more preferably 4.3 or lower, and even more preferably 4.1 or lower, from the viewpoint of suppressing the simultaneous formation of a silica shell and the aggregation of emulsified droplets and obtaining silica capsules with a dense shell.
[0029] Depending on the strength of acidity or alkalinity of the oil phase components including the fragrance compound, any acidic or alkaline pH adjuster may be used to adjust the initial pH to a desired level. The pH of the emulsion may fall below the desired value, in which case it is preferable to adjust it using an alkaline pH adjuster, which will be described later. That is, step 1-4 may preferably be the following step 1-4'. Step 1-4': A step of adjusting the pH of the emulsion obtained in Step 1-3 using a pH adjuster, carrying out a first-stage sol-gel reaction to form silica capsules (1) having a core and a first shell, and obtaining an aqueous dispersion containing the silica capsules (1).
[0030] Examples of acidic pH adjusters include inorganic acids such as hydrochloric acid, nitric acid, and sulfuric acid, organic acids such as acetic acid and citric acid, and solutions of cation exchange resins added to water or ethanol, among which hydrochloric acid, sulfuric acid, nitric acid, and citric acid are preferred. Examples of alkaline pH adjusters include sodium hydroxide, sodium bicarbonate, potassium hydroxide, ammonium hydroxide, diethanolamine, triethanolamine, and trishydroxymethylaminomethane, with sodium hydroxide and ammonium hydroxide being preferred.
[0031] The reaction temperature of the sol-gel reaction in step 1 can be any value that is equal to or higher than the melting point and equal to or lower than the boiling point of water contained as the aqueous phase, but from the viewpoint of controlling the balance between the hydrolysis reaction and the condensation reaction in the sol-gel reaction and forming a dense shell, it is preferable to set the temperature within a certain range, preferably 5°C or higher, more preferably 10°C or higher, even more preferably 15°C or higher, and preferably 60°C or lower, more preferably 50°C or lower, and even more preferably 40°C or lower.
[0032] [Process 2] Step 2 is a step in which tetraalkoxysilane is further added to the aqueous dispersion containing the silica capsules (1) obtained in step 1 to carry out a sol-gel reaction, thereby forming silica capsules having a second shell that encapsulates the first shell.
[0033] The amount of tetraalkoxysilane added in step 2 is preferably 7% by mass or more, more preferably 10% by mass or more, and even more preferably 15% by mass or more, relative to the fragrance compound in step 1, from the viewpoint of forming a second shell that encapsulates the first shell, and is preferably 200% by mass or less, more preferably 170% by mass or less, and even more preferably 150% by mass or less, from the viewpoint of suppressing the formation of silica sol that disperses in the aqueous phase and improving the dispersion stability of the silica capsules.
[0034] In step 2, the tetraalkoxysilane to be added to the aqueous dispersion containing the silica capsules (1) obtained in step 1 may be added all at once, may be added intermittently in divided amounts, or may be added continuously. However, from the viewpoint of forming a highly dense second shell, it is preferable to add it dropwise continuously. When the tetraalkoxysilane is added dropwise continuously, the dropwise addition time can be set appropriately depending on the scale of production, but from the viewpoint of suppressing separation of the added tetraalkoxysilane from the aqueous dispersion, it is preferably 5 minutes or more, more preferably 10 minutes or more, even more preferably 30 minutes or more, and preferably 1200 minutes or less, more preferably 1000 minutes or less, even more preferably 500 minutes or less.
[0035] In the present invention, the total amount of tetraalkoxysilane added, i.e., the total amount of tetraalkoxysilane used in step 1 and step 2, is preferably 30% by mass or more, more preferably 35% by mass or more, even more preferably 40% by mass or more, and is preferably 250% by mass or less, more preferably 200% by mass or less, even more preferably 150% by mass or less, relative to the fragrance compound in step 1. By keeping the total amount of tetraalkoxysilane added within the above range, the encapsulated fragrance compound can be maintained for a long period of time.
[0036] In the present invention, the total amount of the fragrance compound and tetraalkoxysilane in step 1 relative to the total amount of the aqueous dispersion before the addition of the tetraalkoxysilane in step 2 is preferably 20% by mass or less, more preferably 18% by mass or less, even more preferably 15% by mass or less, and even more preferably 10% by mass or less, from the viewpoint of improving the long-term retention of the fragrance compound, and is preferably 2% by mass or more, more preferably 3% by mass or more, and even more preferably 5% by mass or more, from the viewpoint of production efficiency. The adjustment of the total amount of the fragrance compound and tetraalkoxysilane in step 1 relative to the total amount of the aqueous dispersion before the addition of the tetraalkoxysilane in step 2 may be performed by carrying out step 1 so that the amounts of the fragrance compound and tetraalkoxysilane in step 1 and the total amount of the aqueous dispersion obtained in step 1 are within the above-mentioned ranges, or may be performed by further adding water to the aqueous dispersion obtained in step 1 to dilute it.
[0037] In the present invention, from the viewpoint of production efficiency, the aqueous dispersion obtained in step 1 may be diluted with water before the addition of the tetraalkoxysilane in step 2. The total amount of the fragrance compound and tetraalkoxysilane in step 1 relative to the total amount of the aqueous dispersion obtained in step 1 before dilution is preferably 3% by mass or more, more preferably 5% by mass or more, even more preferably 10% by mass or more, still more preferably 15% by mass or more, and is preferably 50% by mass or less, more preferably 40% by mass or less, and even more preferably 30% by mass or less. The dilution ratio is preferably 2 times or more, more preferably 2.5 times or more, and preferably 20 times or less, more preferably 10 times or less, more preferably 7 times or less.
[0038] The reaction temperature for the sol-gel reaction in step 2 can be selected arbitrarily as long as it is equal to or higher than the melting point and equal to or lower than the boiling point of water contained as the dispersion medium, but from the viewpoint of controlling the balance between the hydrolysis reaction and the condensation reaction in the sol-gel reaction and forming a dense shell, the reaction temperature is preferably 5° C. or higher, more preferably 10° C. or higher, even more preferably 15° C. or higher, and preferably 60° C. or lower, more preferably 50° C. or lower, even more preferably 40° C. The sol-gel reaction in step 1 and the sol-gel reaction in step 2 may be carried out at different reaction temperatures.
[0039] In the present invention, in step 2, an organic polymer may be further added to the aqueous dispersion obtained in step 1 for the purpose of stabilizing the aqueous dispersion and suppressing aggregation. Here, the organic polymer means a compound having a weight-average molecular weight of 5,000 or more. The organic polymers include nonionic polymers, cationic polymers, and anionic polymers. The nonionic polymer refers to a water-soluble polymer that has no charge in water. By using a nonionic polymer, it is possible to impart a function to the silica capsule depending on the intended use of the silica capsule. When a nonionic polymer, cationic polymer, or anionic polymer is used as the organic polymer, for example, when the silica capsules of the present invention are used in a fabric treatment composition such as a softener composition, improved adsorption of the silica capsules to fibers can be expected. As used herein, the term "water-soluble polymer" refers to a polymer that, when dried at 105°C for 2 hours and allowed to reach a constant weight, dissolves in 100 g of water at 25°C in an amount of 1 mg or more.
[0040] Examples of nonionic polymers include polymers having structural units derived from nonionic monomers, water-soluble polysaccharides (cellulose-based, gum-based, starch-based, etc.) and derivatives thereof. Examples of nonionic monomers include (meth)acrylates having a hydrocarbon group derived from an aliphatic alcohol having 1 to 22 carbon atoms; styrene-based monomers such as styrene; aromatic group-containing (meth)acrylates such as benzyl (meth)acrylate; vinyl acetate; vinylpyrrolidone; vinyl alcohol; polyalkylene glycol (meth)acrylates such as polyethylene glycol mono(meth)acrylate; alkoxypolyalkylene glycol mono(meth)acrylates such as methoxypolyethylene glycol mono(meth)acrylate and octoxypolyethylene glycol mono(meth)acrylate; (meth)acrylamide, etc. Note that "(meth)acrylate" refers to either acrylate or methacrylate. Similarly, "(meth)acrylic" refers to either acrylic or methacrylic.
[0041] Examples of cationic polymers include polymers containing quaternary ammonium salt groups, polymers having nitrogen-based cationic groups, polymers that can become cationic by adjusting the pH, etc. By using a cationic polymer, it is possible to alleviate the situation in which the silica capsules (1) obtained in step 1 tend to aggregate in the aqueous dispersion, and it is possible to suppress the generation of coarse particles, etc. in the subsequent step 2. Examples of cationic polymers include polydiallyldimethylammonium salts 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, polydiallyldimethylammonium salts and copolymers thereof are preferred, with one or more selected from poly(diallyldimethylammonium chloride), poly(acrylic acid-co-diallyldimethylammonium chloride), and poly(acrylamide-co-acrylic acid-co-diallyldimethylammonium chloride) being more preferred, and poly(diallyldimethylammonium chloride) being even more preferred.
[0042] The cationic group equivalent of the cationic polymer is preferably 1 meq / g or more, more preferably 3 meq / g or more, even more preferably 4.5 meq / g or more, and preferably 10 meq / g or less, more preferably 8 meq / g or less, from the viewpoints of dispersibility of the silica capsules (1), suppression of the generation of coarse particles, and improvement of long-term retention. The cationic polymer may contain anionic groups, and in that case, the anionic group equivalent contained in the cationic polymer is preferably 3.5 meq / g or less, more preferably 2 meq / g or less, even more preferably 1 meq / g or less. In the present invention, the cationic group equivalent of the cationic polymer is calculated based on the monomer composition.
[0043] Examples of anionic polymers include polymers containing monomer units having a carboxyl group, polymers containing monomer units having a sulfonic acid group, and polymers that become anionic upon pH adjustment. Examples of anionic polymers include poly(meth)(acrylic acid), poly(maleic acid), poly((meth)acrylic acid-co-maleic acid), poly((meth)acrylic acid-co-maleic anhydride), poly((meth)acrylic acid-co-isobutylene), poly((meth)acrylic acid-co-styrene), poly(isobutylene-co-maleic acid), poly(styrene-co-maleic acid), carboxymethyl cellulose, etc. Note that (meth)acrylic acid means acrylic acid or methacrylic acid.
[0044] The amount of the organic polymer added is preferably 0.05% by mass or more, more preferably 0.1% by mass or more, even more preferably 0.2% by mass or more, and is preferably 5% by mass or less, more preferably 3% by mass or less, even more preferably 2% by mass or less, based on the amount of the aqueous dispersion obtained in step 1.
[0045] The silica capsules obtained in step 2 are dispersed in water. Depending on the application, they can be used as they are, but in some cases, the silica capsules are separated and used. Separation methods such as filtration and centrifugation can be used.
[0046] <Core> The core of the silica capsule according to the present invention contains a fragrance compound. In the present invention, from the viewpoint of fragrance release when the fabric is wetted with moisture such as sweat, it is preferable that the proportion of fragrance compounds having a logP of 2.0 or more and 5.0 or less and a vapor pressure at 25°C of 0.01 or more and 8.00 or less is 25 mass% or more of the total amount of fragrance compounds.
[0047] In the present invention, the logP value is a coefficient indicating the affinity of an organic compound for water and 1-octanol. The 1-octanol / water partition coefficient P is the ratio of the equilibrium concentrations of a compound in a solvent consisting of two liquid phases, 1-octanol and water, when a trace amount of the compound dissolves as a solute in each solvent and reaches partition equilibrium. It is generally expressed in the form of their logarithm logP to the base 10. Nowadays, the value of "calculated logP (sometimes referred to as ClogP)" is widely used, calculated by a calculation program using fragment values of atomic groups determined by the number of atoms constituting the compound molecule and the type of chemical bond. In the present invention, the ClogP value is also used when selecting compounds.
[0048] In the present invention, the ClogP value is calculated using software EPI Suite (registered trademark: The Estimations Programs Interface for Windows version 4.11) jointly developed by the US Environmental Protection Agency and Syracuse.
[0049] In the present invention, the vapor pressure at 25°C is determined by an actual measurement or by estimating the vapor pressure from the boiling point, or, if the chemical is solid at room temperature, by estimating the vapor pressure from the melting point. Vapor pressure can be estimated by several known methods (such as the Antoine method, the Modified Grain method, and the Mackay method). In the present invention, the vapor pressure is calculated using MPBPWIN, which is included in the EPI suite available from the U.S. Environmental Protection Agency (EPA). If the average of the values calculated by the Antoine method and the Grain method is displayed in the calculation results as the "Selected VP," the average value is used. If no "Selected VP" is displayed, the value calculated by the Modified Grain method is used.
[0050] Examples of fragrance compounds having a log P of 2.0 or more and 5.0 or less and a vapor pressure at 25°C of 0.01 or more and 8.00 or less include γ-undecalactone, 2-cyclohexylidene-2-phenylacetonitrile, damascenone, δ-damascone, α-methyl-β-(pt-butylphenyl)-propionaldehyde, β-ionone, myrrhaldehyde, ethyltricyclo[5.2.1.0-2,6) Decane-2-carboxylate (flute), citronellol, geraniol, α-ionone, patchouli alcohol, 6,7-dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanone, methyl dihydrojasmonate, hexyl cinnamic aldehyde, amyl cinnamic aldehyde, allyl cyclohexyl propionate, dimethylbenzylcarbinyl butyrate, tricyclodecenyl propionate, amyl salicylate, γ-methyl ionone, α-damascenoic acid β-damascone, nerolin yarayara, 2,4,6-trimethyl-4-phenyl-1,3-dioxane, phenylhexanol, 2-methyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol, dodecahydro-3a,6,6,9a-tetramethylnaphtho[2,1-b]furan, γ-nonalactone, methyl β-naphthyl ketone, eugenol, lyral, dimethylbenzylcarbinyl acetate, iso-damascone, 2-cyclohexylidene-2-phenyl Nylacetonitrile, γ-decalactone, α-methyl-3,4-methylenedioxyhydrocinnamic aldehyde, 7-methyl-3,5-dihydro-2H-benzodioxepinone, tricyclodecenyl acetate (tricyclodecenyl acetate), tricyclodecenyl propionate, allyl 2-pentyloxyglycolate, 1-(2-tert-butylcyclohexyloxy)-2-butanol, citronellyloxyacetaldehyde, indole, 4-methyl-3-decen-5-ol, paprika Lamenthan-8-thiol-3-one, 3-(para-tert-butylphenyl)-propanal, ethyl cinnamate, 5-methyl-3-heptanone oxime, methyl anthranilate, terpineol, β-caryophyllene, citronellyl acetate, geranyl acetate, neryl acetate, pt-butylcyclohexyl acetate, tetrahydrogeraniol, 2-isobutyl-4-hydroxy-4-methyltetrahydropyranol (Florosa), α-dynascone, cis-jasmone, bicyclo[3.2.1) Octan-8-one-1,5-dimethyl-oxime, 2,4-dimethyl-4,4α,5,9β-tetrahydroindeno[1,2-d]-m-dioxine, 3-(para-ethylphenyl)-2,2-dimethylpropanal, ethyl-2-tert-butylcyclohexyl-carbonate, hexyl benzoate, 4-acetoxy-3-amyltetrahydropyran, dodecyl aldehyde, dihydro-β-ionone, methyl cyclooctyl carbonate, methylphenyl These include ethyl glycidate, isoeugenol, methyl isoeugenol, diphenyl oxide, 2,2,5-trimethyl-5-pentyl cyclopentanone, thymol, nerolin bromeliad, 5,6-dimethyl-8-isopropenyl, bicyclo[4,4,0]-1-decen-3-one, 3-(4-isopropylphenyl)-propanal, 4-isopropylcyclohexanemethanol, methyl methylanthranilate, and dodecanenitrile-3-dodecenal.
[0051] Furthermore, fragrance compounds with a logP value of less than 2.0 can also be used as the fragrance compound of component (a). Examples of fragrance compounds with a logP value of less than 2.0 include coumarin (1.5), phenylethyl alcohol (1.6), cis-3-hexenol (1.6), raspberry ketone (1.5), and heliotropin (1.8). The numbers in parentheses are logP values.
[0052] Furthermore, fragrance compounds with a logP value of greater than 5.0 can also be used as the fragrance compound of component (a). Examples of fragrance compounds with a logP value greater than 5.0 include 2-[2-(4-methyl-3-cyclohexen-1-yl)propyl]cyclopentanone (5.1), 7-acetyl-1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethylnaphthalene (5.2), acetylcedrene (5.2), nerolidol (5.7), benzyl alcohol (7.1), and caryophyllene (6.3). The numbers in parentheses are logP values.
[0053] Furthermore, as the fragrance compound of component (a), a fragrance compound with a vapor pressure of less than 0.01 Pa can also be used. Examples of fragrance compounds with a vapor pressure of less than 0.01 Pa include 1,4-dioxacycloheptadecane-5,17-dione (0.0000585) and ethylene brassylate (0.0000585). The numbers in parentheses indicate vapor pressure.
[0054] The fragrance compound of component (a) may also be a fragrance compound with a vapor pressure of greater than 8.00 Pa. Examples of fragrance compounds with a vapor pressure of greater than 8.00 Pa include ethyl 2-methylbutyrate (1070), ethyl 2-methylpentanoate (384), limonene (193), allyl 2-pentyloxyglycolate (19.7), 2,4-dimethyl-3-cyclohexenylcarboxaldehyde (46.9), linalool (11.1), linalyl acetate (17.5), tetrahydrolinalool (9.51), 1,8-cineole (208), isobornyl acetate (14.3), ocimene (358), cis-3-hexenol (125), triplal (46.9), and styrallyl acetate (14.9). The numbers in parentheses are vapor pressures.
[0055] The microcapsules of component (a) may contain one or more diluents, solvents, and solidifying agents in addition to the fragrance compound. Examples of diluents and solvents include ethylene glycol, propylene glycol, dipropylene glycol, and glycerin, as well as fatty acid alcohols, lower alcohol esters of fatty acids, and glycerin esters of fatty acids.
[0056] [Silica capsule] The silica capsules of the present invention, for example, the silica capsules produced as described above, are attached to a textile product in an aqueous medium and then break down at the end of the process as water evaporates from the textile product, allowing the encapsulated material to penetrate into the textile product.
[0057] The silica capsule of the present invention is preferably a silica capsule having a core containing the fragrance compound, a first shell encapsulating the core, and a second shell encapsulating the first shell. The first shell of the silica capsule of the present invention encapsulates the core, contains silica as a constituent component, and preferably has an average thickness of 5 nm or more and 20 nm or less, and the second shell encapsulates the first shell, contains silica as a constituent component, and preferably has an average thickness of 10 nm or more and 100 nm or less. The average thickness of the first and second shells of the silica capsules can be measured by observation with a transmission electron microscope (TEM). Specifically, the thickness of the first and second shells is measured on a photograph under a transmission electron microscope. This operation is performed with the field of view changed five times. The distribution of the average thickness of the first and second shells is determined from the obtained data. The magnification of the transmission electron microscope is generally between 10,000 and 100,000 times, but is adjusted appropriately depending on the size of the silica capsules. Here, a transmission electron microscope (TEM) such as the "JEM-2100" (manufactured by JEOL Ltd.) can be used.
[0058] The median diameter D of the component (a) and the silica capsule according to the present invention 50 From the viewpoint of improving the long-term storage property and improving the dispersion stability of the silica capsules, the particle size is preferably 0.1 μm or more, more preferably 0.5 μm or more, and even more preferably 1 μm or more, and from the viewpoint of improving the physical strength and long-term storage property of the silica capsules, the particle size is preferably 100 μm or less, more preferably 50 μm or less, even more preferably 30 μm or less, and even more preferably 10 μm or less. (a) Component, and the median diameter D of the silica capsule 50 can be measured by the method described in the Examples.
[0059] The silica capsules according to the present invention are preferably blended as a silica capsule slurry when preparing a textile product treatment composition. From the viewpoint of improving the dispersibility of the silica capsule slurry in the components mixed when preparing the textile product treatment composition, a surfactant selected from a cationic surfactant, a nonionic surfactant, and an anionic surfactant may be added to the silica capsule slurry.
[0060] The silica capsules of component (a) may be partially aggregated to the extent that the fragrance is not impaired.
[0061] From the viewpoint of imparting a pleasant fragrance to the treated fabric and imparting a lingering fragrance, the textile product treatment composition of the present invention contains component (a) in an amount of 0.1% by mass or more, preferably 0.2% by mass or more, more preferably 0.3% by mass or more, and even more preferably 0.4% by mass or more, as a fragrance compound contained in component (a), and from the viewpoint of storage stability, specifically, preventing fusion of composition particles in a sealed container and preventing melting of the composition during storage at high temperatures, the textile product treatment composition contains 10% by mass or less, preferably 4.0% by mass or less, more preferably 2.0% by mass or less, and even more preferably 1.5% by mass or less.
[0062] In the present invention, polyethylene glycol, fatty acids, alcohols, ester oils, ether oils, cationic surfactants, nonionic surfactants, and anionic surfactants that are incorporated into component (a) during the manufacturing process of component (a), such as the silica capsules of the present invention, are not included in the components (b) and (c).
[0063] [(b) component] The textile treatment composition of the present invention contains, as component (b), polyethylene glycol having a number average molecular weight of 2,000 or more and 13,000 or less. Component (b) is a component that is blended into the composition separately from component (a). Component (b) refers to a component that is present in the composition without being encapsulated in component (a).
[0064] The polyethylene glycol of component (b) has a number average molecular weight of 2000 or more, preferably 3000 or more, more preferably 4000 or more, and even more preferably 5000 or more, from the viewpoints of good granulation ability, storage stability, and water solubility during use of the composition, and from the viewpoint of solubility in a laundry bath, it is 13000 or less, preferably 12000 or less, more preferably 11000 or less, and even more preferably 10000 or less. Here, the number average molecular weight of component (b) is a value measured by the method described in the Quasi-drug Raw Materials Standards: Polyethylene Glycol Average Molecular Weight Test.
[0065] From the viewpoint of good granulation properties and storage stability, the textile product treatment composition of the present invention contains component (b) in an amount of 40% by mass or more, preferably 60% by mass or more, and from the same viewpoint, 95% by mass or less, preferably 90% by mass or less.
[0066] [(c) component] The textile treatment composition of the present invention contains, as component (c), at least one compound that is liquid at 30°C and is selected from fatty acids, alcohols, ester oils, ether oils, cationic surfactants, nonionic surfactants, and anionic surfactants. When component (c) is used together with component (b), it is possible to reduce the breakdown of component (a) during the manufacturing process, storage, etc. Component (c) is a component that is blended into the composition separately from component (a). Component (c) refers to a component that is present in the composition without being encapsulated in component (a).
[0067] Fatty acids that are liquid at 30°C include oleic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, and docosahexaenoic acid.
[0068] Examples of alcohols that are liquid at 30°C include lauryl alcohol, decyltetradecanol, octyldodecanol, isostearyl alcohol, hexyldecanol, and oleyl alcohol.
[0069] Ester oils that are liquid at 30°C include isononyl isononanoate, isotridecyl isononanoate, neopentyl glycol dicaprate, neopentyl glycol diethylhexanoate, ethylhexyl palmitate, glycerin tri-2-ethylhexylate, alkyl benzoate, propanediol dicaprylate / caprate, propanediol diisostearate, glyceryl tricaprylate / caprate, isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, methyl oleate, decyl oleate, hexyldecyl dimethyloctanoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl isostearate, ethylene glycol di-2-ethylhexylate, dipentaerythritol fatty acid esters that are liquid at 30°C, diisostearate malate Tearyl, di-2-heptylundecanoate glycerin, tri-2-ethylhexyl trimethylolpropane, triisostearate trimethylolpropane, tetra-2-ethylhexyl pentaerythritol, triisostearate trimethylolpropane, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, tri-2-heptylundecanoate glyceride, castor oil fatty acid methyl ester, oleyl oleate, Examples include acetoglyceride, 2-heptylundecyl palmitate, diisobutyl adipate, N-lauroyl-L-glutamic acid-2-octyldodecyl ester, di-2-heptylundecyl adipate, ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyldecyl myristate, 2-hexyldecyl palmitate, 2-hexyldecyl adipate, diisopropyl sebacate, and 2-ethylhexyl succinate.
[0070] Examples of ether oils that are liquid at 30°C include 2-ethylhexyl glyceryl ether, cetyl dimethyl butyl ether, ethylene glycol dioctyl ether, and glycerol monooleyl ether.
[0071] Examples of cationic surfactants that are liquid at 30° C. include compounds such as alkyl or alkenyl quaternary ammonium salts and alkyl or alkenyl amines, which are liquid at 30° C. These may have alkyl and / or alkenyl groups with 8 or more, or even 10 or more, and 22 or less, or even 18 or less carbon atoms.
[0072] Examples of nonionic surfactants that are liquid at 30°C include compounds that are liquid at 30°C, such as polyoxyethylene alkyl ethers, glycerin fatty acid esters, polyglycerin fatty acid esters, propylene glycol fatty acid esters, pentaerythritol fatty acid esters, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene glycerin fatty acid esters, polyethylene glycol fatty acid esters, polyoxyethylene phytosterols, polyoxyethylene phytostanols, polyoxyethylene polyoxypropylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, polyoxyethylene lanolin, polyoxyethylene lanolin alcohol, polyoxyethylene beeswax derivatives, polyoxyethylene alkylamines, alkylalkanolamides, and polyoxyethylene fatty acid amides.
[0073] In the present invention, examples of anionic surfactants include compounds that are liquid at 30°C, such as alkyl sulfates, polyoxyethylene alkyl ether sulfates, alkylbenzenesulfonates, alkylnaphthalenesulfonates, dialkyl sulfosuccinates, alkyldiphenylether disulfonates, alkanesulfonates, polyoxyalkylene alkenyl ether sulfates, fatty acid salts, and alkenylsuccinates.
[0074] From the viewpoint of exhibiting the effect of inhibiting microcapsule disintegration during the production process or storage process, the textile product treatment composition of the present invention contains component (c) in an amount of preferably 3% by mass or more, more preferably 5% by mass or more, and even more preferably 7% by mass or more, and from the viewpoint of good granulation properties and storage stability, the amount is preferably 20% by mass or less, more preferably 15% by mass or less, and even more preferably 10% by mass or less.
[0075] [Other ingredients, manufacturing methods, etc.] The textile product treatment composition of the present invention may contain components other than the above-mentioned components (a), (b), and (c) within the range that does not impair the effects of the present invention. Specifically, it may contain the following components (d) and (e), etc.
[0076] [(d) component] The textile treatment composition of the present invention may contain, as component (d), a fragrance compound other than the fragrance compound encapsulated in component (a). In the present invention, even if the fragrance compound is the same as the fragrance compound encapsulated in the microcapsules of component (a), the fragrance compound that is not encapsulated in the microcapsules of component (a) is treated as component (d). In other words, the fragrance compound of component (d) is a fragrance compound dispersed in the textile treatment composition, and these fragrance compounds are sometimes referred to as external fragrances.
[0077] There are no particular restrictions on the fragrance compound that can be used as component (d), and the same fragrance compound as that used in component (a) may be used. Component (d) can be blended into the textile product treatment composition of the present invention as a fragrance composition containing multiple fragrance compounds. Fragrance compounds that can be used as component (d) include, for example, fragrances described in "Fundamentals of Fragrances and Fragrance Blending, edited by Nakajima Mototaka, published by Sangyo Tosho Co., Ltd., 4th printing, April 20, 2005" and fragrance compounds known to be incorporated into fabric softeners and the like through patent documents, as well as fragrance components prepared independently by fragrance manufacturers or blended fragrance compositions themselves. Examples of component (d) include β-ionone (4.4), γ-undecalactone (3.1), γ-nonalactone (2.1), γ-methylionone (4.8), ambroxan (4.8), Iso E Super (5.2), ethyl vanillin (1.6), ethylene brassylate (4.7), eugenol (2.7), cashmeran (manufactured by IFF) (4.5), coumarin (1.5), geraniol (3.5), o,t-butylcyclohexyl acetate (4.4), citronellyl acetate (4.6), dimethylbenzylcarbinyl acetate (3.4), sandalmysole core (4.7), dihydrojasmine (4.8), and methylparaben (4.8). Examples of methyl sucralose (3.5), dihydromyrcenol (3.5), dimethyltetrahydrobenzaldehyde (2.9), Javanol (Givaudan) (4.7), Neroline Yara Yara (3.3), Habanolide (Firmenich) (4.9), Flute (Kao Corporation) (3.6), Paeonil (Givaudan) (4.3), hexyl cinnamic aldehyde (4.8), heliotropin (1.8), methyl β-naphthyl ketone (2.9), methyl anthranilate (2.3), raspberry ketone (1.5), limonene (4.8), and lilial (4.4). The values in parentheses are logP values.
[0078] The textile treatment composition of the present invention may contain a diluent or a fixative for the fragrance compound, such as dipropylene glycol, palmitic acid isopropyl ester, diethyl phthalate, benzyl benzoate, liquid paraffin, isoparaffin, and oils and fats. When a diluent and a retaining agent are used, the amount of the diluent and the retaining agent relative to the total amount of component (d), the diluent and the retaining agent is preferably 0% by mass or more and 20% by mass or less. Note that these diluents and retaining agents can also be used for the fragrance compound encapsulated in the microcapsules of component (a).
[0079] The use of component (d) in combination with component (a) allows for greater flexibility in fragrance design than ever before. Therefore, when a textile product is treated with the textile product treatment composition of the present invention in combination with component (d), it is possible to impart, for example, a fresh and rich fragrance.
[0080] When the textile product treatment composition of the present invention contains component (d), from the viewpoint of ensuring the fragrance derived from component (d), its content in the composition is preferably 0.5% by mass or more, more preferably 1% by mass or more, and even more preferably 1.5% by mass or more, and from the viewpoint of the storage stability of the textile product treatment composition and the balance of the fragrance with component (a), it is preferably 12% by mass or less, more preferably 10% by mass or less, and even more preferably 5% by mass or less. The content of component (d) in the textile product treatment composition can be adjusted according to the product.
[0081] Furthermore, when the textile product treatment composition of the present invention contains component (d), the total content of components (c) and (d) in the composition is preferably 4% by mass or more, more preferably 6% by mass or more, even more preferably 8% by mass or more, and from the viewpoint of storage stability, is preferably 20% by mass or less, more preferably 15% by mass or less, even more preferably 12% by mass or less.
[0082] [(e) component] The textile treatment composition of the present invention can contain a water-soluble cationic polymer as component (e). Component (e) is a component that is preferably incorporated from the viewpoint of enhancing the adsorption of component (a) onto textile products when the composition of the present invention is used to treat textile products. Component (e) refers to a component that is present in the composition without being encapsulated in component (a).
[0083] Examples of cationic polymers include polydiallyldimethylammonium salts 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, polydiallyldimethylammonium salts and copolymers thereof are preferred, and one or more selected from poly(diallyldimethylammonium chloride), poly(acrylic acid-co-diallyldimethylammonium chloride), and poly(acrylamide-co-acrylic acid-co-diallyldimethylammonium chloride) are more preferred.
[0084] The weight-average molecular weight of component (e) is preferably 10,000 or more, more preferably 100,000 or more, and preferably 10,000,000 or less, more preferably 5,000,000 or less. Here, the weight-average molecular weight of component (e) is measured by a technique such as gel permeation chromatography (GPC).
[0085] When the textile product treatment composition of the present invention contains component (e), from the viewpoint of ensuring the adsorption of component (a), the content thereof in the composition is preferably 0.0005% by mass or more, more preferably 0.001% by mass or more, and even more preferably 0.005% by mass or more, and from the viewpoint of formulation ease and preventing inhibition of the cleaning performance of the detergent, the content thereof is preferably 1% by mass or less, more preferably 0.5% by mass or less, and even more preferably 0.1% by mass or less.
[0086] The textile product treatment composition of the present invention may contain, as appropriate, oil-based components other than the above-mentioned components (b), (c), (d), and (e), as well as water-soluble polymers, pigments, dyes, and other components, within the range that does not impair the effects of the present invention.
[0087] The textile product treatment composition of the present invention is preferably in a solid form. The solid form may be, for example, a powder, granules, particles, or tablets. The composition of the present invention may also be a granulated product. The textile product treatment composition of the present invention may be composed of, for example, a plurality of particles, and the average particle size of the particles may be 0.01 mm or more, or even 0.1 mm or more, and 100 mm or less, or even 10 mm or less. The average particle size is measured, for example, by a dry sieving method or other technique.
[0088] The water content of the textile product treatment composition of the present invention may be, for example, 25% by mass or less, further 15% by mass or less, and even further 8% by mass or less.
[0089] The textile treatment composition of the present invention can be produced by mixing components (a), (b), and (c). The order of mixing is not important, but an example of such a method is to add component (c) to molten component (b) to dissolve component (c), and then add component (a) and mix them together. Optional components such as components (d) and (e) may be added in any order, but in this method, it is preferable to mix component (d) with component (c) and component (e) with component (a).
[0090] When the textile product treatment composition of the present invention is produced as granules, it is preferable to use a melt granulation method from the viewpoint of easily producing granules using liquid components. From the viewpoint of solubility in a laundry bath, the average particle size of the resulting granules is preferably 0.1 mm or more, more preferably 0.2 mm or more, even more preferably 0.3 mm or more, still more preferably 0.5 mm or more, and preferably 10 mm or less, more preferably 7 mm or less, even more preferably 3 mm or less, and still more preferably 1.5 mm or less. The average particle size is measured, for example, by a dry sieving method.
[0091] The present invention provides a method for treating textile products, which comprises contacting a textile product with a treatment liquid obtained by mixing the textile product treatment composition of the present invention with water. The same matters as described for the textile product treatment composition of the present invention can be appropriately applied to this treatment method. Examples of textile products that are the subject of the present invention include clothing, fabrics, bedding, towels, etc.
[0092] The single dose of the textile product treatment composition of the present invention per 1 kg of textile products is preferably 1 g or more, more preferably 3 g or more, and even more preferably 4 g or more, from the viewpoint of imparting a good fragrance and lingering fragrance to the textile products, and is preferably 15 g or less, more preferably 12 g or less, and even more preferably 10 g or less, from the viewpoint of preventing the imparting of an excessively strong fragrance. [Example]
[0093] <Component (a)> Fragrance compositions (A-1) to (A-3) were prepared as fragrance compositions as shown in Table 1. Silica capsules (a-1) to (a-3) containing the fragrance compositions (A-1) to (A-3) were prepared according to the following Synthesis Example (a-1).
[0094] [Table 1a]
[0095] [Table 1b]
[0096] [Synthesis Example (a-1): Synthesis of Silica Capsule (a-1)] (Process 1) An aqueous phase component was obtained by diluting 0.91 g of Coatamine 60W (trade name, manufactured by Kao Corporation, cetyltrimethylammonium chloride, active ingredient 30% by mass) with 224.13 g of ion-exchanged water. An oil phase component was prepared by mixing 60.03 g of the fragrance composition (A) (A-1) from the fragrance composition (A) having the blending ratio shown in Table 1 above with 15.10 g of tetraethoxysilane (hereinafter also referred to as "TEOS"), to this aqueous phase component. The mixture was emulsified for 10 minutes at a rotation speed of 9,000 rpm using a homomixer (manufactured by HsiangTai, model: HM-310, the same applies hereinafter) to obtain an emulsion. The median diameter D of the emulsified droplets at this time was 0.03 g. 50 was 1.3 μm. The pH of the resulting emulsion was adjusted to 3.7 using a 1% by mass aqueous solution of sulfuric acid, and then the emulsion was transferred to a separable flask equipped with a stirring blade and a condenser. The emulsion was stirred for 24 hours while maintaining the liquid temperature at 30°C, yielding an aqueous dispersion containing silica capsules having a core made of the fragrance composition (A) in Table 1 and a first shell made of silica.
[0097] (Process 2) To 280.0 g of the aqueous dispersion obtained in step 1, 8.4 g of TEOS was added over 420 minutes. After the dropwise addition, the mixture was stirred for an additional 17 hours to form a second shell encapsulating the first shell, thereby obtaining an aqueous dispersion containing silica capsules (a-1) in which the fragrance composition (A) in Table 1 was encapsulated in amorphous silica. The median diameter D of the silica capsules (a-1) was 50 The median diameter D of the emulsion droplets and silica capsules (a-1) was 2.1 μm. 50 was measured using a laser diffraction / scattering particle size distribution analyzer "LA-960" (trade name, manufactured by Horiba, Ltd.). A flow cell was used for the measurement, and the medium was set to water and the refractive index was set to 1.40-0i. An emulsion or an aqueous dispersion containing silica capsules was added to the flow cell, and measurements were carried out at a concentration where the transmittance was around 90%, and the median diameter D 50 The thickness of the first shell of the silica capsule (a-1) was about 5 nm, and the thickness of the second shell was 5 to 30 nm.
[0098] In Synthesis Example (a-1), the fragrance composition A was replaced with (A-2) to synthesize silica capsules (a-2), and the fragrance composition A was replaced with (A-3) to synthesize silica capsules (a-3). Median system D of silica capsules (a-2) and (a-3) 50 The thickness of the first shell and the thickness of the second shell were all equivalent to those of the silica capsule (a-1).
[0099] <(b) Component> (b-1): K-PEG6000LA (Kao Corporation), polyethylene glycol, number average molecular weight 8500
[0100] <(c) component> [(c-1):fatty acid] (c-1-1): Lunac O.V. (Kao Corporation, oleic acid)
[0101] [(c-2): Alcohol] (c-2-1): Kalcol 2098 (Kao Corporation, lauryl alcohol)
[0102] [(c-3): Ester oil] (c-3-1): Exepar M-OL (Kao Corporation, methyl oleate)
[0103] [(c-4): Ether oil] (c-4-1): Penetol GE-EH (Kao Corporation, 2-ethylhexyl glyceryl ether)
[0104] [(c-5): Cationic surfactant] (c-5-1): Quaternary ammonium salt compound produced in Synthesis Example c-1 below <Synthesis Example c-1>: Preparation of (c-5-1) Triethanolamine and a fatty acid having a composition represented by RCOOH, which will be described later, were subjected to an esterification reaction at a reaction molar ratio (fatty acid / triethanolamine) of 1.87 / 1 to obtain an esterification reaction product. The esterification reaction product contained 1% by mass of unreacted fatty acid (the composition of which is described below). After a quaternization reaction was carried out with dimethyl sulfate so that the methyl group was 0.96 equivalents relative to the amine of the amine compound in the esterification reaction product, ethanol was added.
[0105] The resulting reaction product was analyzed by HPLC for the composition ratio of each component, and quantified using tetraoctylammonium bromide as an internal standard. As a result, the resulting reaction product contained 66% by mass of component (c-5-1), which is component (c), 15% by mass of ethanol, 17% by mass of unreacted amine salt (as methyl sulfate), 1% by mass of unreacted fatty acid, a trace amount of triethanolamine quaternary salt, and other trace components, among which, in the following general formula (1), R 1 is an acyl group, and R 2 and R 3 is a hydrogen atom, and R 4 is a methyl group, and X - is methyl sulfate in the component (c-5-1), and in the following general formula (1), R 1 and R 2 is an acyl group, and R 3 is a hydrogen atom, and R 4 is a methyl group, and X - is methyl sulfate in 58% by mass of the component (c-5-1), and in the general formula (1), R 1 , R 2 and R 3 is an acyl group, and R 4 is a methyl group, and X - The compound in which the quaternization reaction was methyl sulfate accounted for 20 mass% of the component (c-5-1). The quaternization rate was 80 mass%.
[0106] [ka]
[0107] The composition of RCOOH used in the reaction for producing (c-5-1) is shown below. Oleic acid: 80% by mass Linoleic acid: 10% by mass Linolenic acid: 2% by mass Stearic acid: 2% by mass Palmitic acid: 6% by mass The above composition was determined by analyzing the fatty acids used as raw materials by gas chromatography, and the area percentage of each fatty acid was considered to be mass percentage. The values in the formulation table have been converted to component concentrations (c-5-1).
[0108] [(c-6): Nonionic surfactant] (c-6-1): Emulgen 106 (Kao Corporation, polyoxyethylene lauryl ether, alkyl group carbon number 12, average number of ethylene oxide added 4.6, nonionic surfactant in which an average of 4.6 ethylene oxide units are added to a linear primary alcohol having an alkyl group carbon number of 12) (c-6-2): Softanol 33 (manufactured by Nippon Shokubai Co., Ltd., polyoxyethylene alkyl (sec-12-14) ether, a nonionic surfactant in which an average of 3 moles of ethylene oxide are added to a secondary alcohol having an alkyl group with 12 to 14 carbon atoms, and an average of 3 moles of ethylene oxide are added to the secondary alcohol) (c-6-3): Softanol 70H (manufactured by Nippon Shokubai Co., Ltd., polyoxyethylene alkyl (sec-12-14) ether, a nonionic surfactant in which an average of 7 moles of ethylene oxide are added to a secondary alcohol having an alkyl group with 12 to 14 carbon atoms, and an average of 7 moles of ethylene oxide are added to the secondary alcohol) (c-6-4): Leodor SP-L10 (Kao Corporation, sorbitan monolaurate) (c-6-5): Leodor TW-L106 (Kao Corporation, polyoxyethylene sorbitan monolaurate) (c-6-6): Emanon 1112 (Kao Corporation, polyethylene glycol monolaurate) (c-6-7): Amit 105 (Kao Corporation, polyoxyethylene alkylamine)
[0109] [(c-7): Anionic surfactant] (c-7-1): Emal 270J (Kao Corporation, polyoxyethylene lauryl ether sulfate) (c-7-2): Pelex TR (Kao Corporation, sodium dialkyl sulfosuccinate)
[0110] <Component (c'): Comparative component of component (c)> (c'-1-1): Lunac P-95 (Kao Corporation, palmitic acid ) (c'-2-1): Kalcol 8098 (Kao Corporation, stearyl alcohol) (c'-6-1): Leodor SP-S10V (Kao Corporation, sorbitan monostearate) (c'-6-2): Emanon 3299VB (Kao Corporation, polyethylene glycol distearate)
[0111] <(d) component> The fragrance composition (d) was prepared as a blended fragrance (d-1). Details of the fragrance composition are shown in Table 2.
[0112] [Table 2]
[0113] <(e) component> (e-1): Marcote 550 (Lubrizol Corporation, copolymer of acrylamide and diallyldimethylammonium salt; INCI name Polyquaternium-7) (e-2): Poise C-60H (Kao Corporation, salt of the reaction product of trimethylammonium-substituted epoxide and hydroxyethyl cellulose; INCI name Polyquaternium-10)
[0114] [Examples and Comparative Examples] The textile product treatment compositions were prepared by mixing the components to obtain the formulations shown in Tables 3 and 4. Specifically, the formulations are as follows: Note that the mass % of the composition in the tables is the mass % of the active ingredient (the mass % of component (a) is the fragrance compound). Component (b) was first melted at 70°C, and then components (c) and (d) were added and dissolved, followed by uniform mixing. Then, components (a) and (e) were added and mixed until uniformly dispersed. This was then dropped onto a flat plate at 15°C to obtain granules with an average particle size of 1.3 mm. The granules were then left to stand in an open system in a room at 20°C and 40% RH for 4 hours, yielding a textile product treatment composition. Using this textile product treatment composition, the encapsulation rate (%) after storage was calculated according to the following method.
[0115] <Inclusion rate after storage (%)> 300 mL of tap water and 270 mg of a commercially available weak alkaline detergent (Attack, Kao Corporation) were added to a 500 mL beaker and stirred for 1 minute using a commercially available stirrer. Then, 300 mg of the textile treatment composition prepared as described above was added and stirred for 30 minutes to dissolve. After stirring, the tap water in the 500 mL beaker was filtered using a vacuum device (Advantec Co., Ltd.) and a membrane filter (0.45 μm, Merck) to separate the component (a) containing the fragrance composition (A) (membrane filter) from the fragrance composition (A) leaked from the collapsed component (a) (filtrate). After filtration, the membrane filter was placed in a glass bottle, 25 mL of methanol was added, and extraction was performed by ultrasonic treatment for 60 minutes (hereinafter referred to as sample (A)). The amount of methyl dihydrojasmonate in sample (A) was calculated using gas chromatography (Shimadzu Corporation). Using this value, the encapsulation rate after storage was calculated according to the following formula (I). The results are shown in Tables 3 and 4. Encapsulation rate after storage (%) = (amount of index fragrance in sample (A)) / (amount of index fragrance in the added textile treatment composition) × 100 (I) Here, the reference fragrance was methyl dihydrojasmonate when (A-1) and (A-2) were used as fragrance composition (A), and tetrahydrolinalool when (A-3) was used.
[0116] [Table 3]
[0117] [Table 4]
[0118] As can be seen from the results in Tables 3 and 4, the textile product treatment compositions of the Examples had a high encapsulation rate after storage, with more than half of the blended component (a) present in a state in which the fragrance composition (A) was encapsulated. On the other hand, the textile product treatment compositions of the Comparative Examples had a low encapsulation rate after storage, with the majority of the blended component (a) disintegrating during the process from blending to storage, and failing to encapsulate the fragrance composition (A).
Claims
1. A solid textile product treatment composition comprising the following components (a), (b), and (c), and 25 mass % or less of water: Component (a): Microcapsules having a shell and a core containing a fragrance compound inside the shell, 0.1% by mass or more and 10% by mass or less (as the fragrance compound contained in component (a)) Component (b): 60% by mass or more and 95% by mass or less of polyethylene glycol having a number average molecular weight of 2,000 or more and 13,000 or less Component (c): 2.5% by mass or more and 20% by mass or less of at least one compound that is liquid at 30°C and is selected from fatty acids, alcohols, ester oils, ether oils, cationic surfactants, nonionic surfactants, and anionic surfactants.
2. The textile treatment composition according to claim 1, wherein the shell of component (a) contains silica as a constituent component.
3. (a) Median diameter D of component 50 The textile product treatment composition according to claim 1 or 2, wherein the particle size is 0.1 μm or more and 100 μm or less.
4. 3. The textile product treatment composition according to claim 1, wherein component (a) is a microcapsule having a first shell encapsulating the core and having an average thickness of 20 nm or less, and a second shell encapsulating the first shell and having an average thickness of 100 nm or less.
5. 3. The textile product treatment composition according to claim 1, further comprising, as component (d), a fragrance compound other than the fragrance compound encapsulated in component (a).
6. The textile product treatment composition according to claim 1 or 2, which contains a water-soluble cationic polymer as component (e).
7. 3. The textile product treatment composition according to claim 1, which is composed of a plurality of particles, the average particle size of which is 0.5 mm or more and 10 mm or less.
Citation Information
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