Aqueous mixture, and method for producing aqueous mixture

JPWO2024143133A5Active Publication Date: 2025-08-07DIC CORP
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Patent Information

Application Number
JP2024567697
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2023-12-21
Filing Date
2023-12-21
Publication Date
2025-08-07
Estimated Expiration
2043-12-21

AI Technical Summary

Technical Problem

Existing methods for producing aqueous mixed solutions with polysaccharides result in high viscosity, leading to handling issues and inadequate penetration, which is not suitable for various applications such as cosmetics and paints.

Method used

A method involving the mixing of polysaccharides with an aqueous medium, followed by a stirring process using a stirrer and a dispersion process using a disperser, achieving a viscosity reduction of 20% or more, specifically using a combination of polysaccharides like cellulose, chitin, and sulfated polysaccharides from algae, and dispersion machines like sand mills or ultrasonic homogenizers.

Benefits of technology

The method effectively reduces viscosity to a desired range, enhancing handling and penetration properties, making the aqueous mixed solutions suitable for use in cosmetics, paints, and fiber treatment agents.

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Abstract

This aqueous mixture contains a polysaccharide and an aqueous medium, wherein the change rate (%) in viscosity with respect to the aqueous mixture before and after distribution processing is at least 20%, said change rate being represented by the following expression (1): (1) [(A-B) / A]×100 (in expression (1), A represents the viscosity (mPa∙s) with respect to the aqueous mixture before distribution processing, and B represents the viscosity (mPa∙s) with respect to the aqueous mixture after distribution processing).
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Description

Aqueous mixture and method for producing the same

[0001] The present invention relates to an aqueous mixture and a method for producing an aqueous mixture.

[0002] Polysaccharides are widely used in our daily lives. Examples of uses of polysaccharides include thickening sauces and dressings, improving the texture of lotions and emulsions, solidifying various liquids to make jellies, uniformly dispersing cocoa powder, corn, and fruit pulp in beverages, improving the dispersion stability of ballpoint pen inks, and improving the anti-sagging properties of paints. Polysaccharides are thus used in a variety of fields, including food, cosmetics, and various paints and inks. Polysaccharides have functions such as thickening (thickening liquids or changing their texture), gelling (solidifying liquids), and stabilizing (keeping solids suspended in liquids). Taking advantage of these functions, aqueous mixtures containing polysaccharides are used as various thickeners and additives. Incidentally, a method for producing spherical composite powders for use in cosmetic formulations has been described, which involves using a mechanical stirrer to obtain an aqueous solution of a water-soluble polysaccharide (see, for example, Patent Document 1, claim 6).

[0003] Japanese Patent Application Laid-Open No. 2021-8442

[0004] To fully utilize the benefits of using polysaccharides, it is important that aqueous mixtures containing polysaccharides exhibit a certain degree of viscosity (viscosity). However, if the viscosity of the aqueous mixture is too high, it can result in problems such as loss during handling during blending operations during production, and a lower than desired level of penetration, resulting in insufficient penetration into wrinkles in fibers or skin. Therefore, in order to obtain aqueous mixtures containing polysaccharides within the desired viscosity range when used as thickeners or additives, it is desirable to provide aqueous mixtures with lower viscosity than those obtained by mixing polysaccharides with an aqueous medium, as well as methods for producing such aqueous mixtures with lower viscosity. However, the present inventors have confirmed that the method for obtaining an aqueous solution of a water-soluble polysaccharide described in Patent Document 1 is insufficient for obtaining aqueous mixtures with lower viscosity. The present invention aims to provide aqueous mixtures with lower viscosity than those obtained by mixing polysaccharides with an aqueous medium, and methods for producing such aqueous mixtures with lower viscosity.

[0005] The present inventors have conducted studies to solve the above-mentioned problems, and as a result have found that an aqueous mixed solution that solves the above-mentioned problems and a method for producing the aqueous mixed solution can be provided by mixing a polysaccharide with an aqueous medium and subjecting the resulting aqueous mixed solution to a stirring step using a stirrer and a dispersion step using a disperser in combination, and have thus completed the present invention, which has the following gist:

[0006] That is, the present invention encompasses the following aspects: [1] An aqueous mixture containing a polysaccharide and an aqueous medium, wherein the change in viscosity (%) of the aqueous mixture before and after a dispersion treatment, expressed by the following formula (1): [(A-B) / A] x 100 (1) (in formula (1), A is the viscosity (mPa s) of the aqueous mixture before a dispersion treatment, and B is the viscosity (mPa s) of the aqueous mixture after a dispersion treatment), is 20% or more. [2] The aqueous mixture according to [1], wherein the content of the polysaccharide is 1.0% or less relative to the total mass of the aqueous mixture. [3] The aqueous mixture according to [1] or [2], wherein the polysaccharide is at least one selected from the group consisting of cellulose, chitin, starch, glycogen, agarose, pectin, carrageenan, xanthan gum, gelatin, collagen, hyaluronic acid, and sacran. [4] A method for producing an aqueous mixture, comprising the steps of mixing a polysaccharide with an aqueous medium and stirring the resulting aqueous mixture with a stirrer, and dispersing the stirred aqueous mixture with a disperser. [5] A method for producing an aqueous mixture according to any of [1] to [3], comprising the steps of mixing a polysaccharide with an aqueous medium and stirring the resulting aqueous mixture with a stirrer, and dispersing the stirred aqueous mixture with a disperser. [6] The method for producing an aqueous mixed liquid according to [4] or [5], wherein the agitator is at least one selected from the group consisting of a homodisper, an emulsifier, a line mixer, a three-one motor, and a magnetic stirrer. [7] The method for producing an aqueous mixed liquid according to any one of [4] to [6], wherein the disperser is at least one selected from the group consisting of a sand mill, a bead mill, a pebble mill, a ball mill, a pearl mill, a basket mill, an attritor, a Dyno Mill, a bore mill, a Viscomill, a motor mill, an SC mill, a dry mill, a paint conditioner, an ultrasonic disperser (ultrasonic homogenizer), a high-pressure homogenizer, a Nanomizer, an Ultimizer, a roll mill, a Henschel mixer, a pressure kneader, an intensive mixer, a Banbury mixer, and a planetary mixer.

[0007] The present invention can provide an aqueous mixture having a lower viscosity than that obtained by mixing a polysaccharide with an aqueous medium, and a method for producing such an aqueous mixture having a lower viscosity.

[0008] The present invention will be described in detail below. Note that the following explanation of the constituent elements is an example for explaining the present invention, and the present invention is not limited to these contents.

[0009] (Aqueous Mixture) The aqueous mixture of the present invention contains a polysaccharide and an aqueous medium. The aqueous mixture of the present invention has a viscosity change (%) of 20% or more before and after a dispersion treatment, as expressed by the following formula (1): [(A-B) / A] x 100 (1) (in formula (1), A is the viscosity of the aqueous mixture before a dispersion treatment (millipascal seconds (mPa s) = centipoise (cP)), and B is the viscosity of the aqueous mixture after a dispersion treatment (millipascal seconds (mPa s) = centipoise (cP))). The aqueous mixture of the present invention can further contain other components such as a humectant and a preservative, in addition to the polysaccharide and the aqueous medium.

[0010] <Polysaccharides> Polysaccharides are a general term for substances formed by the polymerization of many monosaccharide molecules via glycosidic bonds. They exhibit properties different from those of their constituent monosaccharide units (such as glucose). In a broad sense, they also include sugars in which multiple (two or more) monosaccharide molecules are bonded to a single monosaccharide. They are generally solid and hydrophilic, but their physical properties vary, with some being insoluble in water (such as cellulose and chitin) and others forming gels by dissolving when heated (such as starch, glycogen, agarose, and pectin).

[0011] The polysaccharides in the present invention may be naturally occurring or artificially produced, but are preferably naturally occurring polysaccharides. Here, naturally occurring polysaccharides refer to polysaccharides obtained as biosynthetic products by living organisms, and exist as, for example, structural polysaccharides (cellulose and pectin in plant cell walls, chitin in the exoskeletons of arthropods and fungi, agarose (agar) and carrageenan in algae cells), energy storage substances (starch, glycogen), or gel-like substances secreted by microorganisms (xanthan gum).

[0012] The naturally occurring polysaccharide is preferably, for example, a polysaccharide derived from algae. Examples of polysaccharides derived from algae include polysaccharides derived from macroalgae, microalgae, or cyanobacteria (blue-green algae). More specifically, at least one sulfated polysaccharide derived from the following algae may be used: Gracilaria, Halymenia, Gelidium, Pterocladia, Acanthopelitis, Campylaephora, Ceranium, Eucheuma, Chondrus, and the like. red macroalgae selected from among the Rhodophyceae of the genera Porphyra, Porphyra, Laurencia, Furcellaria, Gloiopeltis, and Iridea that produce agar, carrageenan, porphyrin, furan, or complex sulfated galactans; green macroalgae selected from the Chlorophyceae of the genus Ulva that produce polysaccharides, such as ulvan; brown macroalgae selected from the Pheophyceae of the genera Fucus, Aschophyllum, or Cladosiphon that produce sulfated furans. Cyanobacteria such as Aphanothece sacrum (Suizenji moss).

[0013] Among the polysaccharides derived from the above algae, sulfated polysaccharides derived from A. sacchariflorus are preferred. A. sacchariflorus is a type of freshwater cyanobacterium that belongs to the Chroococcales order and has photosynthetic ability. A. sacchariflorus grows naturally in a specific area of ​​Kyushu, Japan, and is a freshwater cyanobacterium that forms flat colonies of multiple cells. The outer surface of the colonies is covered with a gel-like secretion formed from polysaccharides and the like, and the colonies grow to a diameter of approximately 50 mm. Ultra-high molecular weight (average molecular weight: 2,000,000 or more) sulfated polysaccharides extracted from Aphanothece sacrum have a repeating structure of sugar chain units in which sugar structures having hexose structures and sugar structures having pentose structures are linked in a linear or branched chain via α-glycosidic or β-glycosidic bonds, and in which 2.7 or more hydroxyl groups per 100 hydroxyl groups are sulfated, or the sulfur content of all elements is 1.5% by weight or more, and the sugar chain units are sugar derivatives containing lactated sulfated sugars as sugar structures. Sulfated polysaccharides extracted from Aphanothece sacrum are known to have excellent moisturizing, barrier, and anti-inflammatory effects, and are industrially produced under the trade name "Sakuran" (registered trademark; hereinafter, the term "registered trademark" may be omitted) and are sold, for example, by Green Science Materials Co., Ltd.

[0014] In the present invention, "sacran" in the broad sense refers to a polymer containing the same structural units as the polymer extracted from A. sacran is not limited to that derived from A. sacran, but is preferably a sulfated polysaccharide derived from A. sacran. Sacran may be, for example, a sulfated polysaccharide containing monosaccharides such as 6-deoxysugars (and / or pentoses), uronic acid, hexapyranose, or sulfated muramic acid as structural units. An example of a method for extracting sacran from A. sacran is described in International Publication WO 2008 / 062574. For example, a specific method for extracting sacran from A. sacran involves freezing an appropriate amount of A. sacran and washing it with water to remove water-soluble pigments, then removing fat-soluble pigments with an organic solvent such as ethanol, and drying the A. sacran algae. Thereafter, 0.1 N sodium hydroxide is added to the resulting dried A. sacran algae, and the mixture is stirred at 60-80°C for 6 hours. Examples of methods include neutralizing the sugar derivative solution obtained from the above procedure, filtering, concentrating, and drying. In another example, sacran can be extracted from A. saccharinum by heating an aqueous dispersion of A. saccharinum in an autoclave at 135°C for 30 minutes. The extracted sacran may be purified by centrifugation, filtration, alcohol washing, or the like. Furthermore, before extracting sacran from A. saccharinum, the A. saccharinum may be frozen and then thawed, followed by a step of removing pigments.

[0015] The polysaccharide may be gelatin, collagen, or hyaluronic acid. Hyaluronic acid includes hyaluronic acid (including hydrolyzed hyaluronic acid, low-molecular-weight hyaluronic acid, etc.), as well as salts of hyaluronic acid (e.g., sodium hyaluronate, zinc hyaluronate, low-molecular-weight zinc hyaluronate, etc.) and hyaluronic acid derivatives (acetylated hyaluronic acid or its salts (e.g., sodium acetylated hyaluronate, zinc acetylated hyaluronate, etc.)).

[0016] The mass average molecular weight of the polysaccharide before dispersion treatment is not particularly limited, but is preferably 500,000 to 30,000,000, more preferably 1,000,000 to 25,000,000, and particularly preferably 2,000,000 to 20,000,000.

[0017] <Aqueous Medium> In the aqueous mixture of the present invention, an aqueous medium such as a water-soluble solvent and / or water is used as the solvent. These may be water alone or a mixed solvent consisting of water and a water-soluble solvent. Specific examples of water include natural water, purified water, distilled water, ion-exchanged water, pure water, and ultrapure water (e.g., Milli-Q water). Among these, purified water, distilled water, ion-exchanged water, pure water, or ultrapure water is preferred from the viewpoint of having fewer impurities.

[0018] Examples of water-soluble solvents include ketones such as acetone, methyl ethyl ketone, methyl butyl ketone, and methyl isobutyl ketone; alcohols such as methanol, ethanol, 2-propanol, 2-methyl-1-propanol, 1-butanol, and 2-methoxyethanol; ethers such as tetrahydrofuran, 1,4-dioxane, and 1,2-dimethoxyethane; and amides such as dimethylformamide and N-methylpyrrolidone. In particular, it is preferable to use a compound selected from the group consisting of ketones having 3 to 6 carbon atoms and alcohols having 1 to 5 carbon atoms. Other water-soluble organic solvents that can be dissolved in water can also be used. Examples of suitable water-soluble organic solvents include glycols such as ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, polyethylene glycol, and polypropylene glycol; diols such as butanediol, pentanediol, hexanediol, and related diols; glycol esters such as propylene glycol laurate; glycol ethers such as cellosolves containing diethylene glycol monoethyl, diethylene glycol monobutyl, and diethylene glycol monohexyl ethers, propylene glycol ether, dipropylene glycol ether, and triethylene glycol ether; alcohols such as methanol, ethanol, isopropyl alcohol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, butyl alcohol, pentyl alcohol, and related alcohols; lactones such as sulfolane; lactones such as γ-butyrolactone; lactams such as N-(2-hydroxyethyl)pyrrolidone; and various other solvents known as water-soluble organic solvents, such as glycerin and its derivatives, and polyoxyethylene benzyl alcohol ether. These water-soluble organic solvents can be used alone or in combination. Among these, polyhydric alcohols such as glycols and diols, which have a high boiling point, low volatility and high surface tension, are preferred, and glycols such as diethylene glycol and triethylene glycol are particularly preferred.

[0019] <Other Components> Furthermore, if necessary, binders, crosslinking agents, moisturizers (humectants), preservatives, viscosity adjusters, pH adjusters, chelating agents, plasticizers, antioxidants, ultraviolet absorbers, and the like may be added to the aqueous mixture of the present invention.

[0020] Examples of binders include acrylic resins, urethane resins, polyester resins, silicone resins, and cationic resins. The binder content is preferably 0.1 to 30% by mass, more preferably 0.5 to 20% by mass, and even more preferably 1 to 10% by mass. The binder content is preferably 0.5 to 100 parts by mass, more preferably 1 to 50 parts by mass, and even more preferably 3 to 30 parts by mass, relative to 100 parts by mass of the sulfated polysaccharide.

[0021] When the aqueous mixture of the present invention is used as a fiber treatment agent, as described below, it preferably contains a crosslinking agent. The crosslinking agent is not particularly limited, but when the polysaccharide is a compound having a carboxyl group, such as sacran, an aqueous crosslinking agent that is expected to undergo a crosslinking reaction with the crosslinking agent is preferred. Examples of aqueous crosslinking agents include EPOCROS WS-500 manufactured by Nippon Shokubai Co., Ltd., PROMINATE XC-830 manufactured by Aica Kogyo Co., Ltd., and CARBODILITE V-02-L2 manufactured by Nisshinbo Chemical Inc.

[0022] Examples of moisturizing agents include amino acids such as glutamine, histidine, and arginine; polyhydric alcohols having two or more hydroxyl groups such as propylene glycol, 1,3-butylene glycol, and glycerin; and examples of preservatives include alcohols such as 1,2-hexanediol, 1,2-pentanediol, and 1,3-butylene glycol; sodium benzoate; salicylic acid; potassium sorbate; and phenoxyethanol.

[0023] The content of the polysaccharide is 0.001 to 50.0% by mass, preferably 0.002 to 20.0% by mass, more preferably 0.003 to 10.0% by mass, even more preferably 0.01 to 5.0% by mass, particularly preferably 0.02 to 2.0% by mass, and most preferably 0.03 to 1.0% by mass, relative to the total mass of the aqueous mixture.

[0024] <Regarding the Viscosity of the Aqueous Mixture> The viscosity change rate (%) of the aqueous mixture of the present invention before and after the dispersion treatment is 20% or more. If the viscosity change rate is 20% or more, it is possible to sufficiently suppress inconveniences during handling during blending operations during production, etc., and adverse effects due to insufficient penetration. On the other hand, in order to maintain the effects of containing polysaccharides, it is preferable that the aqueous mixture after the dispersion treatment exhibits a certain degree of viscosity. Therefore, it is preferable that the viscosity change rate is 85% or less. The viscosity change rate (%) is expressed by the following formula (1):

[0025] [(A-B) / A] x 100 (1) In formula (1), A is the viscosity (mPa·s) of the aqueous mixed liquid before dispersion treatment, and B is the viscosity (mPa·s) of the aqueous mixed liquid after dispersion treatment.

[0026] The change rate (%) of viscosity of the aqueous mixture of the present invention before and after dispersion treatment is more preferably 30% or more, and more preferably 75% or less.

[0027] [Viscosity Measurement] For example, an E-type viscometer (VISCOMETER TV-25 TYPE L, manufactured by Toki Sangyo Co., Ltd.) can be used to measure the viscosity at a temperature of 20° C. Alternatively, a B-type viscometer "DV2T" (trade name, manufactured by Eiko Seiki Co., Ltd.) can be used instead of the E-type viscometer.

[0028] The application of the aqueous mixture of the present invention is not particularly limited, and it can be used in cosmetics, foods, etc. Furthermore, the aqueous mixture of the present invention can be used, for example, as a fiber treatment agent. A fiber treatment agent is a substance that imparts some functionality by being attached to a fiber substrate; for example, an aqueous mixture is attached to the fiber substrate, and then a drying process is performed to remove water from the attached fiber treatment agent composition, and the fiber substrate is then attached to the surface of the fiber substrate. Examples of functionality include moisture absorption, water absorption, quick-drying, moisture-releasing, stain resistance, antistatic properties, good texture, and washing durability, which means that these functionalities are not lost even after washing. By utilizing the above-mentioned functionality, the processed textile products can be suitably used in various fields, for example, clothing such as gloves, underwear, socks, shirts, suits, sportswear, hats, and inner caps; mask materials such as face masks and surgical masks; materials for disposable diapers; cosmetic sheets such as lotion wipes; bedding such as futon covers, sheets, and pillowcases; and daily necessities such as curtains, towels, hand towels, kitchen aprons and aprons, rugs / carpets / mats, wall materials, batting, and filters. Furthermore, if the processed textile products have excellent antistatic properties, they can be suitably used in curtains, suit linings, coats, workwear worn in manufacturing sites, clean room wear, painting clothes, and the like. Furthermore, if the processed textile products have a good feel to the skin, they can be used in applications requiring comfort, such as bandages, elbow and knee joint supports, medical lab coats, arm covers, arm slings, leg covers, triangular bandages, medical gauze, and bedding, as well as applications requiring comfort and slipperiness, such as stockings, tights, neckties, and dresses / drapes.

[0029] (Method for producing aqueous mixture) The method for producing an aqueous mixture of the present invention comprises the steps of: mixing a polysaccharide with an aqueous medium and stirring the obtained aqueous mixture with a stirrer; and dispersing the stirred aqueous mixture with a disperser. In addition, in the present invention, the aqueous mixture in the method for producing an aqueous mixture of the present invention is preferably an aqueous mixture that exhibits a change in viscosity (%) of 20% or more before and after dispersion treatment, as represented by the above formula (1), as described in the above section (Aqueous mixture).

[0030] <Step of Stirring with a Stirrer> Stirring refers to mixing substances together to mix multiple types of substances. In the present invention, the step of stirring refers to a step of mixing the polysaccharide and the aqueous medium by stirring an aqueous mixture containing the polysaccharide and the aqueous medium in a stirrer. The stirrer is not particularly limited as long as it can achieve the effects of the present invention and can be appropriately selected depending on the purpose. Examples of the stirrer include a homodisper, an emulsifier, a line mixer, a three-one motor, and a magnetic stirrer.

[0031] The conditions for the stirring step are not particularly limited and can be appropriately selected depending on the purpose as long as the effects of the present invention are achieved, but for example, the stirring time is preferably 1 to 48 hours, and the temperature during stirring is preferably 20 to 80°C.

[0032] <Step of Dispersing Using a Disperser> Dispersion refers to the process of applying impact or shear force to a substance to reduce the particle size of the substance, thereby dispersing smaller particles of the substance within a substance in one phase. In the present invention, the dispersing process refers to the process of applying impact or shear force to the stirred aqueous mixture in a disperser to reduce the particle size of the polysaccharide and disperse the smaller particles of the polysaccharide in the aqueous medium. When the aqueous mixture is mixed using only the agitator, the polysaccharide exists as large particles with entangled fibers in the aqueous medium. However, by using a disperser, the polysaccharide can be dispersed as smaller particles in the aqueous medium. The disperser is not particularly limited as long as it achieves the effects of the present invention and can be appropriately selected depending on the purpose. Examples include dispersers that utilize the kinetic energy of spherical dispersion media with diameters of approximately 0.1 to 10 mm and made of steel, stainless steel, zirconia, alumina, silicon nitride, glass, etc., dispersers that utilize shear forces due to mechanical stirring, dispersers that utilize forces generated by pressure changes, flow path changes, or collisions in the flux of the liquid being treated supplied at high speed, and ultrasonic dispersers. More specific examples include media dispersers such as sand mills, bead mills, pebble mills, ball mills, pearl mills, basket mills, attritors, dyno mills, bore mills, viscomills, motor mills, SC mills, dry mills, and paint conditioners. Other examples include media-less dispersers that do not use media, such as ultrasonic dispersers (ultrasonic homogenizers), high-pressure homogenizers, nanomizers, and ultimizers. Other examples include a roll mill such as a three-roll mill, a Henschel mixer, a pressure kneader, an intensive mixer, a Banbury mixer, a planetary mixer, and other kneading dispersers that apply a strong shear force to disperse the components.

[0033] The conditions for the dispersion step are not particularly limited and can be selected appropriately depending on the purpose as long as the effects of the present invention are achieved, but for example, the dispersion time is preferably 1 to 24 hours. The temperature during dispersion is preferably 1 to 80°C. When dispersion is performed using a disperser that uses spherical dispersion media, for example, the filling rate of the spherical dispersion media in the dispersion chamber is preferably 20 to 90%, and the peripheral speed of the rotor that imparts kinetic energy to the spherical dispersion media is preferably 5 to 20 m / s.

[0034] A specific embodiment of the dispersion method is, for example, a dispersion method using a wet bead mill operated at a predetermined peripheral speed of the disperser at a predetermined power density, because this method has high dispersion ability and dispersion efficiency. Various conditions, such as the type and size (volume) of the apparatus, the type and amount of the dispersion sample (a mixture of polysaccharide and water), the peripheral speed of the disperser, and the flow rate of the dispersion sample, are set appropriately.

[0035] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to these examples. In the examples, the viscosity unit cP has the same meaning as mPa·s.

[0036] Example 1 <Stirring> A mixture having the following composition was placed in a Dispermat (manufactured by Eiko Seiko Co., Ltd.) and stirred for 2 hours at 70°C and 2000 rpm: 0.1 parts by mass of sodium hyaluronate (FCH60, manufactured by Kikkoman Biochemifa Corporation) 99.9 parts by mass of ion-exchanged water

[0037] <Dispersion> The stirred mixture and 100 parts by mass of 0.3 mm diameter YTZ balls (manufactured by Nikkato Corporation) were placed in a plastic bottle, which was then placed in a paint conditioner (manufactured by Toyo Seiki Seisakusho) and subjected to a dispersion treatment for 2 hours, thereby obtaining an aqueous mixed liquid which was the mixture of Example 1.

[0038] Comparative Example 1 In Example 1, the aqueous mixture was obtained by carrying out only the <stirring> step before being subjected to the <dispersion> step, whereas in the present invention, this aqueous mixture is referred to as the aqueous mixture of Comparative Example 1.

[0039] (Viscosity Reduction Rate in Aqueous Mixture of Example 1) The viscosity of the aqueous mixture of Example 1 after the dispersing step was measured using an E-type viscometer VISCOMETER TVE-25L (manufactured by Toki Sangyo Co., Ltd.). As a result, the viscosity of the aqueous mixture of Example 1 after the dispersing step was 31.9 (cP) (i.e., 31.9 mPa·s). In Example 1, the viscosity of the aqueous mixture (corresponding to the aqueous mixture of Comparative Example 1) before being subjected to the dispersing step was also measured in the same manner as in Example 1. As a result, the viscosity of the aqueous mixture of Comparative Example 1 was 44.7 (cP) (i.e., 44.7 mPa·s). The viscosity reduction rate of the aqueous mixture of Example 1 can be calculated using the following formula: [(44.7-31.9) / 44.7]×100 The result was approximately 29%.

[0040] (Examples 2 to 5, Comparative Examples 2 to 5) Aqueous dispersions of Examples 2 to 5 (corresponding to Comparative Examples 2 to 5 before the dispersion step) were obtained in the same manner as in Example 1 above (corresponding to Comparative Example 1 before the dispersion step), except that the type and content of sodium hyaluronate, or the type of disperser and dispersion time were changed as shown in Table 1. The viscosities of the aqueous mixed solutions in Examples 2 to 5 were measured in the same manner as in Example 1. The measurement results of the viscosity of the aqueous mixed solutions of Examples 2 to 5 and Comparative Examples 2 to 5, and the results of the viscosity reduction rates of the aqueous mixed solutions of Examples 2 to 5 are shown in Table 1.

[0041]

[0042] (Examples 6 to 8, Comparative Examples 6 to 8) In Example 1 (corresponding to Comparative Example 1 before the dispersion step), the type of polysaccharide was changed to SACRAN (registered trademark, manufactured by Green Science Materials Co., Ltd., sulfated polysaccharide derived from Aphanothece sacrum, molecular weight: approximately 2 million to approximately 20 million), the stirrer was changed to a Magnetic Stirrer KS-1X (manufactured by AZONE), the disperser was changed to a Paint Conditioner (manufactured by Toyo Seiki Co., Ltd.), and the SACRAN content and dispersion time were changed as shown in Table 2. The aqueous dispersions of Examples 6 to 8 (corresponding to Comparative Examples 6 to 8 before the dispersion step) were obtained in the same manner as in Example 1. The viscosity of the aqueous mixtures in Examples 6 to 8 and Comparative Examples 6 to 8 was measured in the same manner as in Example 1. The measurement results of the viscosity of the aqueous mixtures of Examples 6 to 8 and Comparative Examples 6 to 8, as well as the viscosity reduction rates of the aqueous mixtures of Examples 6 to 8, are shown in Table 2.

[0043] Examples 9 to 11 Aqueous dispersions of Examples 9 to 11 were obtained in the same manner as in Examples 6 to 8 (which correspond to Comparative Examples 6 to 8 before the dispersion step) except that the content of SACRAN and the dispersion time were changed as shown in Table 2. The viscosities of the aqueous mixed solutions of Examples 9 to 11 were measured in the same manner as in Example 1. Table 2 shows the results of measuring the viscosity of the aqueous mixed solutions of Examples 9 to 11 and the results of the viscosity reduction rates of the aqueous mixed solutions of Examples 9 to 11 compared with Comparative Examples 6 to 8, respectively.

[0044] (Example 12, Comparative Example 9) In comparison with the above Example 1 (which corresponds to Comparative Example 1 before the dispersion step), the type of polysaccharide was changed to SACRAN (registered trademark, manufactured by Green Science Materials Co., Ltd.), the disperser was changed to a Bead Mill Labostar Mini MGF015 (manufactured by Ashizawa Finetech Co., Ltd.), the bead filling rate was set to 80%, the peripheral speed was set to 8 m / sec, and the SACRAN content and dispersion time were changed as shown in Table 2. Except for this, an aqueous dispersion of Example 12 (which corresponds to Comparative Example 9 before the dispersion step) was obtained in the same manner as Example 1. The viscosity of the aqueous mixture in Example 12 was measured in the same manner as Example 1. The viscosity measurement results of the aqueous mixtures of Example 12 and Comparative Example 9, and the viscosity reduction rate of the aqueous mixture of Example 12 are shown in Table 2.

[0045]

[0046] Example 13 <Stirring> 99.5 parts by mass of ion-exchanged water was added to 0.5 parts by mass of SACRAN (registered trademark, manufactured by Green Science Materials Co., Ltd., sulfated polysaccharide derived from Aphanothece sacrum, molecular weight: approximately 2 million to approximately 20 million), and the mixture was stirred at 70°C for 8.5 hours using a Three-One Motor "FBL600" (trade name, manufactured by HEIDON Co., Ltd.) equipped with a propeller shaft. Thereafter, the mixture was further stirred for 3 minutes at room temperature using a Homo Disper stirrer.

[0047] <Dispersion> A bead mill disperser "Bead Mill Labostar Mini MGF015" (trade name, manufactured by Ashizawa Finetech Co., Ltd.) was filled with beads at a filling rate of 80%, and the mixture after stirring was subjected to a dispersion treatment at a peripheral speed of 8 m / sec for 0.5 hours, thereby obtaining an aqueous mixed liquid which was the mixture of Example 13.

[0048] Example 14 An aqueous mixture of Example 14 was obtained in the same manner as in Example 13, except that the bead mill dispersion in the <Dispersion> step was performed for 1 hour.

[0049] (Example 15) The aqueous mixture of Example 15 was obtained in the same manner as in Example 13, except that the stirring time with a three-one motor in the <stirring> step was changed to 9 hours and the bead mill dispersion time in the <dispersion> step was changed to 1.5 hours.

[0050] Comparative Example 10 A mixed composition obtained in Example 13 by carrying out only the <stirring> step before subjecting it to the <dispersion> step was designated as Comparative Example 10.

[0051] Comparative Example 11 A mixed composition obtained in Example 15 by carrying out only the <stirring> step before subjecting it to the <dispersion> step was used as Comparative Example 11.

[0052] The viscosity and viscosity reduction rate of each SACRAN fiber treatment agent solution in Example 13 (corresponding to Comparative Example 10 before the dispersion step), Example 14, and Example 15 (corresponding to Comparative Example 11 before the dispersion step) are shown in Table 3. The viscosity was measured using the viscometer shown in Table 3. The E-type viscometer used was the one described above, and the B-type viscometer used was "DV2T" (trade name, manufactured by Eiko Seiki Co., Ltd.).

[0053]

[0054] Example 16 <Stirring> 99.5 parts by mass of ion-exchanged water was added to 0.5 parts by mass of SACRAN (registered trademark, manufactured by Green Science Materials Co., Ltd., sulfated polysaccharide derived from Aphanothece sacrum, molecular weight: approximately 2 million to approximately 20 million), and the mixture was stirred at 75°C for 8 hours using a Three-One Motor "FBL600" (trade name, manufactured by HEIDON Co., Ltd.) equipped with a propeller shaft. Thereafter, the mixture was further stirred at room temperature for 5 minutes using a Hi-Flex Disper Stirrer "HG92" (trade name, manufactured by SMT Co., Ltd.).

[0055] <Dispersion> A bead mill "Labostar Mini MGF015" (trade name, manufactured by Ashizawa Finetech Co., Ltd.) was filled with beads at a filling rate of 80%, and the mixture after stirring was subjected to a dispersion treatment at a peripheral speed of 8 m / sec for 90 minutes, thereby obtaining an aqueous mixture A, which was the mixture of Example 16.

[0056] The aqueous mixture A from Example 16, a crosslinking agent "PROMINATE XC-830" (trade name, manufactured by Aica Kogyo Co., Ltd.), and a binder "DEXCEL HPS PAD 602" (trade name, manufactured by DIC Corporation) were mixed with ion-exchanged water so that the total amount of the final composition was 1,000 parts by mass, to obtain a fiber treatment composition A. The results are shown in Table 4.

[0057] Examples 17 and 18 Fiber treatment compositions B to C were obtained in the same manner as in Example 16, except that the compositions shown in Table 4 were used.

[0058] Comparative Example 12 A mixture obtained by carrying out only the <stirring> step before subjecting to the <dispersion> step in Example 16 was designated as aqueous mixture D of Comparative Example 12.

[0059]

[0060] The fiber treatment composition of the comparative example obtained above showed a viscosity reduction rate of less than 20%, while fiber treatment compositions A to C showed a viscosity reduction rate of 20% or more. Each of these fiber treatment compositions was applied to a fiber substrate, polyester P-110 (obtained from Shikisensha Co., Ltd. as "Polyester Decine", a fiber for dyeing tests), at a rate of 70 to 80 g / m using a mangle coater (manufactured by Tsujii Senki Kogyo Co., Ltd.). 2The fiber substrates coated with fiber treatment compositions A to D were then dried under the conditions shown in Table 5 to obtain the processed fiber products of each example. Condition 1: Heat treatment at 150°C for 2 minutes Condition 2: Heat treatment at 70°C for 1 minute + heat treatment with high-temperature steam at 180°C Condition 3: Heat treatment at 70°C for 1 minute

[0061]

[0062] In Examples 16 to 18 and Comparative Example 12, the workability in the preparation process of the fiber treatment agent, the workability when applying the fiber treatment agent composition to a substrate, and the uniformity of application of the resulting fiber processed product were evaluated according to the following evaluation criteria. The results are shown in Table 5. A: Very good B: Good C: Fair / neither good nor bad

Claims

1. An aqueous mixture containing a polysaccharide and an aqueous medium, The following formula (1): [(A-B) / A]×100...(1) (In formula (1), A is the viscosity (mPa s) of the aqueous mixture before dispersion treatment, B is the viscosity (mPa·s) of the aqueous mixture after dispersion treatment. The viscosity reduction rate (%) of the aqueous mixture before and after the dispersion treatment is 20% or more, The aqueous mixture is characterized in that the polysaccharide is at least one selected from the group consisting of hyaluronic acid and sacran.

2. 2. The aqueous mixture according to claim 1, wherein the content of the polysaccharide is 1.0% or less based on the total mass of the aqueous mixture.

3. a step of mixing the polysaccharide with an aqueous medium and stirring the resulting aqueous mixture with a stirrer; and A method for producing an aqueous mixture, comprising: dispersing the stirred aqueous mixture using a disperser, The polysaccharide is at least one selected from the group consisting of hyaluronic acid and sacran, The following formula (1): [(A-B) / A]×100...(1) (In formula (1), A is the viscosity (mPa s) of the aqueous mixture before being subjected to the dispersion step, B is the viscosity (mPa·s) of the aqueous mixture after the dispersion step. The method for producing an aqueous mixed liquid, wherein a viscosity reduction rate (%) of the aqueous mixed liquid before and after the dispersion step is 20% or more, represented by

4. 4. The method for producing an aqueous mixed liquid according to claim 3, wherein the agitator is at least one selected from the group consisting of a homodisper, an emulsifier, a line mixer, a three-one motor, and a magnetic stirrer.

5. 5. The method for producing an aqueous mixed liquid according to claim 3 or 4, wherein the dispersing machine is at least one selected from the group consisting of a sand mill, a bead mill, a pebble mill, a ball mill, a pearl mill, a basket mill, an attritor, a Dyno Mill, a bore mill, a Viscomill, a mortar mill, an SC mill, a drys mill, a paint conditioner, an ultrasonic dispersing machine (ultrasonic homogenizer), a high-pressure homogenizer, a Nanomizer, an Ultimizer, a roll mill, a Henschel mixer, a pressure kneader, an intensive mixer, a Banbury mixer, and a planetary mixer.