Aqueous mixture and method for producing the aqueous mixture

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).

Description

Technical Field

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

Background Art

[0002] Polysaccharides are widely used in daily life. For example, polysaccharides are used to add texture to sauces and dressings, improve the feel of lotions and emulsions, solidify various liquids to make jelly, uniformly disperse cocoa powder, corn, pulp, etc. in beverages, enhance the dispersion stability of ballpoint pen inks, and improve the sag resistance of paints. Thus, polysaccharides are used in various fields such as food, cosmetics, various paints, and inks. Polysaccharides have functions such as a thickening function to make a liquid viscous, a gelling function to firmly solidify a liquid, and a stabilizing function to keep solids floating in a liquid. Taking advantage of such functions of polysaccharides, aqueous mixtures containing polysaccharides are used as various thickeners and additives. By the way, in a method for producing spherical composite powder for cosmetics used in cosmetic formulations, a step of obtaining an aqueous solution of a water-soluble polysaccharide using a mechanical stirrer is described (for example, see Patent Document 1, Claim 6).

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0004] To take advantage of the benefits of using polysaccharides, it is important that the aqueous mixture containing polysaccharides exhibits a certain level of viscosity. However, if the viscosity of the aqueous mixture is too high, it can lead to problems such as losses during handling in production mixing operations, and insufficient penetration into fibers or wrinkles in the skin, as the degree of penetration does not meet the desired standards. Therefore, when using polysaccharides as thickeners or additives, there is a need for an aqueous mixture containing polysaccharides within a desired viscosity range, which has a lower viscosity than the aqueous mixture obtained by mixing polysaccharides with an aqueous medium, and a method for producing such a low-viscosity aqueous mixture. However, the present inventors have confirmed that the method for obtaining an aqueous solution of water-soluble polysaccharides described in Patent Document 1 is insufficient for obtaining a low-viscosity aqueous mixture. The present invention aims to provide an aqueous mixture with lower viscosity compared to the aqueous mixture obtained by mixing polysaccharides and an aqueous medium, and a method for producing such a low-viscosity aqueous mixture. [Means for solving the problem]

[0005] To solve the above problems, the present inventors conducted studies and found that by mixing polysaccharides with an aqueous medium and then using a combination of stirring with a stirrer and dispersion with a disperser to produce the aqueous mixture, it is possible to provide an aqueous mixture that solves the above problems, as well as a method for producing the aqueous mixture. Based on this, the present invention, which has the following gist, has been completed.

[0006] In other words, the present invention encompasses the following embodiments. [1] An aqueous mixture containing polysaccharides and an aqueous medium, Formula (1): [(AB) / 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. An aqueous mixture in which the percentage change in viscosity (%) before and after the dispersion treatment is 20% or more. [2] The aqueous mixture according to [1], wherein the content of the polysaccharide is 1.0% or less of 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 step of mixing polysaccharides with an aqueous medium and stirring the resulting aqueous mixture with a stirrer, A method for producing an aqueous mixture, comprising the step of dispersing the stirred aqueous mixture using a disperser. A method for producing an aqueous mixture described in any of [1] to [3], A step of mixing polysaccharides with an aqueous medium and stirring the resulting aqueous mixture with a stirrer, and A method for producing an aqueous mixture, comprising the step of dispersing the stirred aqueous mixture using a disperser. [6] The method for producing an aqueous mixture 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-in-one motor, and a magnetic stirrer. [7] A method for producing an aqueous mixture according to any one of [4] to [6], wherein the disperser is at least one selected from the group consisting of a sand mill, bead mill, pebble mill, ball mill, pearl mill, basket mill, attritor, dyno mill, bore mill, visco mill, motor mill, SC mill, dry mill, paint conditioner, ultrasonic disperser (ultrasonic homogenizer), high-pressure homogenizer, nanomizer, ultimateizer, roll mill, Henschel mixer, pressurized kneader, intensive mixer, Banbury mixer, and planetary mixer. [Effects of the Invention]

[0007] The present invention provides an aqueous mixture with lower viscosity compared to the aqueous mixture obtained by mixing polysaccharides with an aqueous medium, and a method for producing such a low-viscosity aqueous mixture. [Modes for carrying out the invention]

[0008] The present invention will be described in detail below. The following description of the constituent elements is illustrative for illustrating the present invention, and the present invention is not limited to these elements.

[0009] (Aqueous mixed liquid) The aqueous mixture of the present invention contains polysaccharides and an aqueous medium. The aqueous mixture of the present invention Formula (1): [(AB) / A] × 100 …… (1) (In formula (1), A is the viscosity (millipascal seconds (mPa·s) = centipoise (cP)) of the aqueous mixture before dispersion treatment. B is the viscosity (millipascal seconds (mPa·s) = centipoise (cP)) of the aqueous mixture after dispersion treatment. The percentage change in viscosity (%) of the aqueous mixture before and after the dispersion treatment, as represented by [formula], is 20% or more. The aqueous mixture of the present invention may further contain other components such as humectants and preservatives, in addition to the polysaccharides and aqueous medium described above.

[0010] <Polysaccharide> Polysaccharides are a general term for substances formed by the polymerization of many monosaccharide molecules through glycosidic bonds. They exhibit properties different from the monosaccharides (such as glucose) that make up their constituent units. In a broader sense, they also include sugars in which multiple monosaccharides (two or more molecules) are bonded together. Generally, substances are solid and hydrophilic, but their physical properties vary. Some are insoluble in water (cellulose, chitin, etc.), while others form gels when heated (starch, glycogen, agarose, pectin, etc.).

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

[0012] The polysaccharides of natural origin are preferably, for example, polysaccharides 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 kind of sulfated polysaccharide derived from the following algae is included. Red macroalgae selected from the Rhodophyceae that produce agar, carrageenan, porphyrin, furan, or complex sulfated galactan, belonging to the genera Gracilaria, Halymenia, Gelidium, Pterocladia, Acanthopeltis, Campylaephora, Ceranium, Eucheuma, Chondrus, Porphyra, Laurencia, Furcellaria, Gloiopeltis and Iridea; Green macroalgae selected from the Chlorophyceae that produce polysaccharides, such as ulvan, belonging to the genus Ulva; Brown macroalgae selected from the Pheophyceae that produce sulfated furan, belonging to the genera Fucus, Aschophyllum or Cladosiphon. Cyanobacteria such as Aphanothece sacrum.

[0013] Among the polysaccharides derived from the above-mentioned algae, it is preferably a sulfated polysaccharide derived from Euglena gracilis. Euglena gracilis is a kind of freshwater cyanobacterium having photosynthetic ability belonging to the order Chlorococcales. The Euglena gracilis grows naturally in a specific area of Kyushu, Japan, and is a freshwater cyanobacterium in which a plurality of cells form a flat-shaped colony. Further, the outer surface of the colony is covered with a gel-like secretion formed by polysaccharides and the like, and the diameter of the colony grows to about 50 mm. The ultra-high molecular weight (average molecular weight: 2,000,000 or more) sulfated polysaccharide extracted from Euglena gracilis has a repeating structure of sugar chain units in which a sugar structure having a hexose structure and a sugar structure having a pentose structure are linked linearly or branched by an α-glycoside bond or a β-glycoside bond. In the sugar chain unit, 2.7 or more hydroxyl groups per 100 hydroxyl groups are sulfated, or it is a sugar derivative in which sulfur element occupies 1.5% by weight or more in all elements, and the sugar chain unit is a sugar derivative containing a sulfated sugar lactated as a sugar structure. The sulfated polysaccharide extracted from Euglena gracilis is known to be excellent in moisture retention, barrier property, and anti-inflammatory effect, and is industrially produced as "Sakuran (the description of "registered trademark" may be omitted hereinafter)", and is sold by, for example, Green Science Material Co., Ltd.

[0014] In the broad sense, "Sakuran" in the present invention means a polymer containing the same structural unit as the polymer extracted from Euglena gracilis. Sakuran is not limited to those derived from Euglena gracilis, but is preferably a sulfated polysaccharide derived from Euglena gracilis. Sakuran may be, for example, a sulfated polysaccharide containing monosaccharides such as 6-deoxy sugar (and / or pentose), uronic acid, hexopyranose, and sulfated muramic acid as structural units. An example of a method for extracting Sakuran from Euglena gracilis is described in International Publication WO2008 / 062574. For example, a specific method for extracting sacran from Suizenji-nori includes freezing and washing an appropriate amount of Suizenji-nori with water to remove water-soluble pigments, then removing lipid-soluble pigments with an organic solvent such as ethanol, and drying the Suizenji-nori algae. Subsequently, 0.1N sodium hydroxide is added to the dried Suizenji-nori algae, and the mixture is stirred at 60-80°C for 6 hours. After neutralizing the sugar derivative solution obtained from the above operation, it is filtered, concentrated, and dried. Another example is that sacran can be extracted from Suizenji-nori by heating an aqueous dispersion of Suizenji-nori in an autoclave at 135°C for 30 minutes. The extracted sacran may be purified by centrifugation, filtration, or alcohol washing. Alternatively, before extracting sacran from Suizenji-nori, the Suizenji-nori may be frozen and then thawed, followed by a step to remove pigments.

[0015] Furthermore, 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 hyaluronic acid salts (e.g., sodium hyaluronate, zinc hyaluronate, low molecular weight zinc hyaluronate, etc.) and hyaluronic acid derivatives (acetylated hyaluronic acid or its salts (e.g., acetylated sodium hyaluronate, acetylated zinc hyaluronate, etc.)).

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

[0017] <Aqueous medium> In the aqueous mixture of the present invention, a water-soluble solvent and / or an aqueous medium such as 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 are preferred from the standpoint 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. It is particularly preferable to use compounds selected from the group consisting of ketones with 3 to 6 carbon atoms and alcohols with 1 to 5 carbon atoms. In addition, other water-soluble organic solvents that can dissolve in water can also be used. Examples 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 diols of the same group; glycol esters such as propylene glycol laurate; glycol ethers such as cellosolve containing diethylene glycol monoethyl, diethylene glycol monobutyl, 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 alcohols of the same group; or sulfolanes; lactones such as γ-butyrolactone; lactams such as N-(2-hydroxyethyl)pyrrolidone; glycerin and its derivatives; polyoxyethylene benzyl alcohol ether, and various other solvents known as water-soluble organic solvents. These water-soluble organic solvents can be used individually or in combination of two or more. Among these, polyhydric alcohols such as glycols and diols, which have high boiling points, low volatility, and high surface tension, are preferred, and glycols such as diethylene glycol and triethylene glycol are particularly preferred.

[0019] <Other ingredients> Furthermore, if necessary, binders, crosslinking agents, humectants (wetting agents), preservatives, viscosity modifiers, pH adjusters, chelating agents, plasticizers, antioxidants, ultraviolet absorbers, and the like can 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. Furthermore, 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 per 100 parts by mass of sulfated polysaccharides.

[0021] When the aqueous mixture of the present invention is used as a fiber treatment agent as described later, it is preferable that it 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 is preferred. Examples of aqueous crosslinking agents include Epocross 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 Co., Ltd.

[0022] Examples of humectants include amino acids such as glutamine, histidine, and arginine; and polyhydric alcohols having two or more hydroxyl groups, such as propylene glycol, 1,3-butylene glycol, and glycerin. 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 polysaccharide content 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, based on the total mass of the aqueous mixture.

[0024] <Regarding the viscosity of aqueous mixtures> The percentage change in viscosity (%) of the aqueous mixture of the present invention before and after dispersion treatment is 20% or more. If the percentage change in viscosity is 20% or more, inconveniences during handling in production compounding operations and other processes, as well as problems caused by insufficient penetration, can be sufficiently suppressed. On the other hand, in order to maintain the effect of containing polysaccharides, it is preferable that the aqueous mixture after dispersion treatment exhibits a certain degree of viscosity. Therefore, it is preferable that the viscosity change rate is 85% or less. The percentage change in viscosity is expressed by the following formula (1).

[0025] [(AB) / 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.

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

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

[0028] The uses of the aqueous mixture of the present invention are not particularly limited and can be used in cosmetics, food products, etc. Furthermore, the aqueous mixture of the present invention can be used, for example, as a fiber treatment agent. A fiber treatment agent is one that imparts some functionality to a fiber substrate by being attached to it. For example, an aqueous mixture is attached to the fiber substrate, and then a drying process is carried out to remove water from the attached fiber treatment agent composition, resulting in the agent adhering to the surface of the fiber substrate. Functional properties include hygroscopicity, water absorption, quick drying, moisture release, stain resistance, antistatic properties, a pleasant feel, and wash resistance, where these functionalities do not disappear after washing. Fiber processed products can be suitably used in various fields, such as clothing including gloves, underwear, socks, shirts, clothes, sportswear, hats, and inner caps; mask materials such as face masks and surgical masks; materials for disposable diapers; cosmetic sheets such as cleansing lotion sheets; bedding such as futon covers, sheets, and pillowcases; and daily necessities such as curtains, towels, hand towels, cooking aprons and bibs, rugs / carpets / mats, wall materials, padding, and filters, taking advantage of the above functionalities. Furthermore, if it has excellent antistatic properties, it can be suitably used in curtains, suit linings, coats, work clothes worn in manufacturing sites, cleanroom wear, painting clothes, etc. Also, if it has a good feel against the skin, it can be used in applications where comfort is required, such as bandages, elbow and knee joint supports, medical white coats, arm covers, arm slings, leg covers, triangular bandages, medical gauze, and bedding, as well as in applications where comfort and smoothness are required, such as stockings, tights, ties, dresses / drapes.

[0029] (Method for producing aqueous mixtures) The method for producing an aqueous mixture of the present invention is as follows: The process involves mixing polysaccharides with an aqueous medium and stirring the resulting aqueous mixture with a stirrer, and The process includes the step of dispersing the stirred aqueous mixture using a disperser. Furthermore, in the present invention, it is preferable that the aqueous mixture in the method for producing the aqueous mixture of the present invention is an aqueous mixture represented by formula (1) above, as described in the (aqueous mixture) section above, which exhibits a viscosity change rate (%) of 20% or more with respect to the aqueous mixture before and after the dispersion treatment.

[0030] <Steps involving stirring with a stirrer> Agitation refers to the process of stirring or mixing substances together, or combining multiple types of substances. In the present invention, the stirring step refers to the step of mixing a mixture of polysaccharides and an aqueous medium by stirring the aqueous mixture in a stirrer. As for the agitator, there are no particular restrictions as long as it achieves the effects of the present invention, and it can be appropriately selected according to the purpose. Examples include homodispers, emulsifiers, line mixers, three-in-one motors, magnetic stirrers, etc.

[0031] There are no particular restrictions on the conditions in the stirring process, and they can be appropriately selected according to the purpose as long as the effects of the present invention are achieved. For example, the stirring time is preferably 1 to 48 hours. Also, the temperature during stirring is preferably 20 to 80°C.

[0032] <Processes that are dispersed by a disperser> Dispersion refers to the process of reducing the particle size of a substance by applying impact or shear force, thereby scattering these smaller particles of other substances within a single phase of the substance. In the present invention, the dispersion step refers to the step of stirring the aqueous mixture after stirring by applying impact force or shear force in a disperser, thereby reducing the particle size of the polysaccharides and scattering the smaller polysaccharide particles in the aqueous medium. Even when an aqueous mixture is mixed using only the above-mentioned agitator, polysaccharides exist in the aqueous medium with large particle sizes and entangled fibers. However, by using a disperser, it is possible to disperse the polysaccharides as smaller particles within the aqueous medium. As for the disperser, there are no particular limitations as long as it achieves the effects of the present invention, and it can be appropriately selected according to the purpose. Examples of dispersers include those that utilize the kinetic energy of spherical dispersion media with a diameter of about 0.1 to 10 mm made of steel, stainless steel, zirconia, alumina, silicon nitride, glass, etc., those that utilize shear force due to mechanical stirring, those that utilize the force generated due to pressure changes, flow path changes, or collisions of the high-speed supplied flux of the liquid to be processed, and dispersers of ultrasonic dispersers. More specifically, examples of media dispersers include sand mills, bead mills, pebble mills, ball mills, pearl mills, basket mills, attritors, dyno mills, bore mills, visco mills, motor mills, SC mills, dry mills, and paint conditioners. Also, media-less dispersers that do not use media include ultrasonic dispersers (ultrasonic homogenizers), high-pressure homogenizers, nanomizers, and ultimateizers. Furthermore, kneading dispersers that use strong shear forces to disperse materials include roll mills such as three-roll mills, Henschel mixers, pressure kneaders, intensive mixers, Banbury mixers, and planetary mixers.

[0033] There are no particular restrictions on the conditions in the dispersion process, and they can be appropriately selected according to the purpose as long as the effects of the present invention are achieved. For example, the dispersion time is preferably 1 to 24 hours. Furthermore, the temperature during dispersion is preferably between 1 and 80°C. In the case of dispersion using a disperser with spherical dispersion media, for example, the packing density of the spherical dispersion media in the dispersion chamber is preferably 20-90%, and the peripheral speed of the rotating body that imparts kinetic energy to the spherical dispersion media is preferably 5-20 m / sec.

[0034] Specific embodiments of the dispersion method include, for example, a dispersion method using a wet bead mill operated at a predetermined peripheral speed of the disperser with a predetermined power density, due to its high dispersion capability and dispersion efficiency. Various conditions, such as the type and size (capacity) of the apparatus, the type and amount of the dispersed sample (a mixture of polysaccharides and water), the peripheral speed of the disperser, and the flow rate of the dispersed sample, are set as appropriate. [Examples]

[0035] The present invention will be further described below with reference to examples, but the present invention is not limited to these examples. In the following examples, the unit of viscosity, cP, is synonymous with mPa·s.

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

[0037] <Dispersion> The stirred mixture and 100 parts by mass of 0.3 mmΦ YTZ balls (manufactured by Nikkatoh) were placed in a plastic bottle and set in a paint conditioner (manufactured by Toyo Seiki Co., Ltd.). The mixture was dispersed for 2 hours to obtain the aqueous mixture of Example 1.

[0038] (Comparative Example 1) In Example 1, the aqueous mixture obtained by performing only the stirring step before the dispersion step is referred to as the aqueous mixture of Comparative Example 1 in this invention.

[0039] (Viscosity reduction rate in the aqueous mixture of Example 1) The viscosity of the aqueous mixture of Example 1 after the dispersion process was measured using a VISCOMETER TVE-25L E-type viscometer (manufactured by Toki Sangyo Co., Ltd.). As a result, the viscosity of the aqueous mixture of Example 1 after the dispersion process 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 dispersion process was also measured using the same method 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 in the aqueous mixture of Example 1 can be determined by the following formula. [(44.7-31.9) / 44.7]×100 The result was approximately 29%.

[0040] (Examples 2-5, Comparative Examples 2-5) Examples 2-5 (corresponding to Comparative Examples 2-5 before the dispersion process) were obtained in the same manner as in Example 1, 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 viscosity of the aqueous mixtures in Examples 2-5 was measured in the same manner as in Example 1. The viscosity measurement results for the aqueous mixtures in Examples 2-5 and Comparative Examples 2-5, as well as the viscosity reduction rate results for the aqueous mixtures in Examples 2-5, are shown in Table 1.

[0041] [Table 1]

[0042] (Examples 6-8, Comparative Examples 6-8) Examples 6-8 (corresponding to Comparative Examples 6-8 before the dispersion process) were obtained in the same manner as in Example 1, except that the type of polysaccharide was changed to Sacran (registered trademark, manufactured by Green Science Material Co., Ltd., sulfated polysaccharide derived from Suizenji Nori, molecular weight: approximately 2 million to approximately 20 million), the stirrer was changed to a magnetic stirrer KS-1X (manufactured by AZONE Co., Ltd.), 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 viscosity of the aqueous mixtures in Examples 6-8 was measured in the same manner as in Example 1. The viscosity measurement results for the aqueous mixtures in Examples 6-8 and Comparative Examples 6-8, as well as the viscosity reduction rate results for the aqueous mixtures in Examples 6-8, are shown in Table 2.

[0043] (Examples 9-11) Aqueous dispersions for Examples 9-11 were obtained in the same manner as in Examples 6-8 (corresponding to Comparative Examples 6-8 before the dispersion step), except that the sacran content and dispersion time were changed as shown in Table 2. The viscosity of the aqueous mixtures in Examples 9 to 11 was measured in the same manner as in Example 1. The viscosity measurement results for the aqueous mixtures in Examples 9 to 11, and the viscosity reduction rates of the aqueous mixtures in Examples 9 to 11 compared with Comparative Examples 6 to 8, are shown in Table 2.

[0044] (Example 12, Comparative Example 9) In addition to the above Example 1 (corresponding to Comparative Example 1 before the dispersion process), the type of polysaccharide was changed to Sacran (registered trademark, manufactured by Green Science Material Co., Ltd.), the disperser was changed to a bead mill Labstar Mini MGF015 (manufactured by Ashizawa Finetech Co., Ltd.), the bead filling rate was set to 80%, the peripheral speed to 8 m / sec, and the Sacran content and dispersion time were further changed as shown in Table 2. Except for these changes, an aqueous dispersion of Example 12 (corresponding to Comparative Example 9 before the dispersion process) was obtained in the same manner as in Example 1. The viscosity of the aqueous mixture in Example 12 was measured in the same manner as in Example 1. The viscosity measurement results for the aqueous mixtures in Example 12 and Comparative Example 9, and the viscosity reduction rate of the aqueous mixture in Example 12 are shown in Table 2.

[0045] [Table 2]

[0046] (Example 13) <Stirring> 0.5 parts by mass of Sacran (registered trademark, manufactured by Green Science Material Co., Ltd., sulfated polysaccharide derived from Suizenji Nori, molecular weight: approximately 2 million to 20 million) was added to 99.5 parts by mass of ion-exchanged water, and the mixture was stirred at 70°C for 8.5 hours using a three-in-one motor equipped with a propeller shaft, "FBL600" (product name, manufactured by HEIDON). After that, the mixture was further stirred at room temperature for 3 minutes using a homodisperser stirrer.

[0047] <Dispersion> Beads were packed into a bead mill disperser "Bead Mill Labstar Mini MGF015" (product name, manufactured by Ashizawa Finetech Co., Ltd.) at a packing rate of 80%, and the mixture after stirring was dispersed at a peripheral speed of 8 m / s for 0.5 hours to obtain the aqueous mixture of Example 13.

[0048] (Example 14) The 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 changed to 1 hour.

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

[0050] (Comparative Example 10) In Example 13, the mixed composition obtained by performing only the stirring step before the dispersion step was designated as Comparative Example 10.

[0051] (Comparative Example 11) Comparative Example 11 was obtained by performing only the stirring step before the dispersion step in Example 15.

[0052] Table 3 shows the viscosity and viscosity reduction rate of the fiber treatment agent solutions for each sacran in Example 13 (corresponding to Comparative Example 10 before the dispersion process), Example 14, and Example 15 (corresponding to Comparative Example 11 before the dispersion process). Viscosity was measured using the viscometers shown in Table 3. The E-type viscometer is the one described above, and the B-type viscometer used was "DV2T" (product name, manufactured by Eiko Seiki Co., Ltd.).

[0053] [Table 3]

[0054] (Example 16) <Stirring> 0.5 parts by mass of Sacran (registered trademark, manufactured by Green Science Material Co., Ltd., sulfated polysaccharide derived from Suizenji Nori, molecular weight: approximately 2 million to 20 million) was added to 99.5 parts by mass of ion-exchanged water, and the mixture was stirred at 75°C for 8 hours using a three-one motor equipped with a propeller shaft, "FBL600" (product name, manufactured by HEIDON). Subsequently, the mixture was further stirred at room temperature for 5 minutes using a high-flex disperser stirring device, "HG92" (product name, manufactured by SMT Co., Ltd.).

[0055] <Dispersion> Beads were packed into a bead mill "Labostar Mini MGF015" (product name, manufactured by Ashizawa Finetech Co., Ltd.) to a packing rate of 80%, and the mixture after stirring was dispersed at a peripheral speed of 8 m / s for 90 minutes to obtain aqueous mixture A, which is the mixture of Example 16.

[0056] The aqueous mixture A from Example 16, the crosslinking agent "Prominate XC-830" (product name, manufactured by Aica Kogyo Co., Ltd.), and the binder "DEXCEL HPS PAD 602" (product name, manufactured by DIC Corporation) were mixed with ion-exchanged water so that the total amount of the final composition was 1000 parts by mass to obtain fiber treatment agent composition A. The results are shown in Table 4.

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

[0058] (Comparative Example 12) In Example 16, the mixture obtained by performing only the stirring step before the dispersion step was designated as the aqueous mixture D of Comparative Example 12.

[0059] [Table 4]

[0060] The fiber treatment agent compositions of the comparative examples obtained above showed a viscosity reduction rate of less than 20%, while fiber treatment agent compositions A to C showed a viscosity reduction of 20% or more. Each of these fiber treatment agent compositions was applied using a mangle coating machine (manufactured by Tsujii Dyeing Machinery Co., Ltd.) at a rate of 70-80 g / m² relative to the fiber base material, polyester P-110 (obtained from Irozome Co., Ltd. as "polyester decyne" for dyeing tests). 2 The substrates were coated with the specified basis weight (the amount of each fiber treatment agent composition applied per unit area of ​​the substrate). Subsequently, the fiber substrates coated with fiber treatment agent compositions A to D were dried under the conditions shown in Table 5 to obtain the fiber processed products for 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] [Table 5]

[0062] In Examples 16-18 and Comparative Example 12 described above, the workability in the preparation process of the fiber treatment agent, the workability when applying the fiber treatment agent composition to the substrate, and the uniform coating properties 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: Neither good nor bad

Claims

1. A step of mixing polysaccharides with an aqueous medium and stirring the resulting aqueous mixture with a stirrer, and A method for producing an aqueous mixture, comprising the step of dispersing the stirred aqueous mixture using at least one disperser selected from a bead mill and a paint conditioner for 0.5 hours or more (however, if only a paint conditioner is used, for 2 hours or more), The aforementioned polysaccharide is at least one selected from the group consisting of hyaluronic acid and sacran. The content of the polysaccharide relative to the total amount of the aqueous mixture is 1.0% by mass or less. 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 process. B is the viscosity (mPa·s) of the aqueous mixture after the dispersion step. The viscosity shall be measured at 20°C using an E-type viscometer. A method for producing an aqueous mixture, wherein the percentage decrease in viscosity (%) of the aqueous mixture before and after the dispersion step is 20% or more.

2. The method for producing an aqueous mixture according to claim 1, wherein the agitator is at least one selected from the group consisting of a homodisper, an emulsifier, a line mixer, a three-in-one motor, and a magnetic stirrer.

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