WO2003000787A1

WO2003000787A1 - Aqueous gel composition

Info

Publication number: WO2003000787A1
Application number: PCT/JP2002/006214
Authority: WO
Inventors: Hisanori Kachi; Keiichi Oyama; Masaaki Kojima; Takehiko Sakai
Original assignee: The Nisshin Oillio, Ltd.; Ina Food Industry Co., Ltd.
Priority date: 2001-06-22
Filing date: 2002-06-21
Publication date: 2003-01-03
Also published as: JPWO2003000787A1; JP4074246B2

Abstract

An aqueous gel composition, characterized in that it comprises at least one paste material selected from galactomannans, xanthan gum and one or more of sequestering agents, and is adjusted to have a pH such that it exhibits a sequestering performance of a predetermined level or higher. The aqueous gel composition exhibits high gel strength and high water-holding capability, and also is lowered in its gelling temperature and viscosity in a sol state and thus exhibits excellent processability.

Description

Description Aqueous gel composition [Technical field]

The present invention relates to an aqueous gel composition having excellent strength and excellent processability, in particular, at least one or more pastes selected from galactomannans, xanthan gum, and one or more salts having sequestering ability. The present invention relates to an aqueous gel composition containing a combination of two or more types.

(Background technology)

Aqueous gelling agents are used in pharmaceuticals, medical devices, pharmaceutical materials, cosmetics, household goods, etc., and aqueous synthetic polymers and natural polymers are used. ₍ Typical substances include synthetic polymers. Known natural polymers such as polyvinyl alcohol and sodium polyacrylate include carrageenan, gelatin, dielan gum, agar, and sodium alginate.

In general, when obtaining an aqueous gel composition, the paste and other ingredients are heated and dissolved uniformly, and then filled and cooled to produce a product.In most cases, however, bulk products are inspected before filling. It was stored in a gel state, not a heated and dissolved sol state.After passing the inspection, it was transferred to the filling line and reheated and filled. ₍ Thus, if the aqueous gel composition has a high sol-gel transition temperature, reheat it. In addition to the high energy and time required, the entire line had to be kept at a high temperature, resulting in many cost and equipment constraints, but on the other hand, when the sol-gel transition temperature was lower than 4 Ot: Is not preferred because its properties change during storage and transportation, affecting product stability.

Aqueous gels formed by natural macromolecules are safe in any industrial field without considering environmental issues such as biodegradability, human safety, and wastewater, exhaust gas, and waste solvents generated by chemical synthesis reactions. It is a versatile substance that can be used with care. Carrageenan and dielan gum need to react with metal ions such as calcium and magnesium, and agar produces drainage. Because gelatin is a protein, it has problems such as insolubilization at pH near the isoelectric point.

It is well known that when galactomannans such as oral cast bean gum and xanthan gum are used together, a strong gel with almost no drainage is formed, and it is also applied to foods, cosmetics, household goods, etc. . However, since this gel composition has a high sol-gel transition temperature of 65, when using it as an aqueous gel material, it is necessary to work while maintaining the temperature of the piping etc. at the time of production, especially at the time of filling, and the formulation It was difficult to mix in components with poor stability at high temperatures. In addition, the viscosity of the sol is high, and even if it is a sol, it is not a perfect fluid but has the property of flowing while maintaining its shape, making it difficult to fill a certain amount and causing problems. It was often. For this reason, this gel, despite its outstanding properties as an aqueous gel, such as strength and water retention, has been used less frequently and has been shunned.

[Disclosure of the Invention]

From the above, there is a strong demand for an aqueous gel composition having high gel strength, an appropriate sol-gel transition temperature, and easy-to-process physical properties. The purpose is to obtain an aqueous gel composition that satisfies.

The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have found that at least one or more pastes selected from galactomannans, xanthan gum, and one or more kinds of sequestering agents An aqueous gel composition, which has a high gel strength and an appropriate sol-gel transition temperature, is adjusted to a pH that exhibits a certain level of blocking ability against alkaline earth metal ions. The present invention has been found to provide an aqueous composition which has an easy processability and has completed the present invention.

That is, the present invention relates to an aqueous gel composition comprising A component: a paste consisting of one or more galactomannans, B component: xanthan gum, C component: one or more sequestering agents, and water. The aqueous gel composition The pH of the C component is within the pH range that can block more than 3 Omg of alkaline earth metal ion per 1 g of the C component, and their mass ratio is A component: B component = 1: 4 to 4: 1, And an aqueous gel composition wherein (A component + B component): C component = 1:10 to 99: 1.

In the aqueous gel composition according to the present invention, the content of (A component + B component) in the aqueous gel composition is preferably 0.1 to 10% by mass.

Further, in the aqueous gel composition according to the present invention, the range of pH at which 30 mg or more of alkaline earth metal ions can be sequestered per gram of the C component is preferably in the range of pH 5 to 12.

Furthermore, in the aqueous gel composition according to the present invention, the sol-gel transition temperature is preferably in the range of 45 to 60.

The present invention also provides a pack cosmetic containing the aqueous gel composition.

The gel strength in the text, unless otherwise specified, refers to the breaking strength (g / cm ² ) of the data obtained by rheometer measurement. A polymer compound swells in an aqueous layer such as an aqueous solution or an oil-in-water emulsion to form a three-dimensional cross-linked structure, which changes from a viscous liquid to a very hard solid. The structure does not need to be by a chemical reaction, but can be by a secondary bond such as a hydrogen bond.

The gel composition of conventional galactomannans and xanthan gum has a high sol-gel transition temperature of about 65, and requires heating of 80 or more to form a sol and exhibit fluidity. And the workability was poor.

On the other hand, since the aqueous gel composition of the present invention has a gel-sol transition point in a temperature range of 45 to 60, the gel strength is equal to or higher than the gel composition of galactomannans and xanthung gum. However, it can be easily brought into a sol state by heating at about 60 to 80. This sol-gel transition can be performed reversibly many times. Therefore, the filling process by reheating is easy, and even if it is unstable to heat, it can be blended without adding an extra heat history, and its transition temperature is hardly changed during storage or during transport. Because it is in the temperature range, it is widely used as an unprecedented aqueous gel material. In addition, the viscosity of the sol before solidification of the aqueous gel composition of the present invention and the sol obtained by heating and dissolving the aqueous gel composition are not only low, but also while maintaining the shape unique to the conventional sol of galactomannans and xanthan gum. Since it does not have the ability to flow and exhibits almost perfect fluid properties, it is easy to fill a certain amount. However, if the sol-gel transition temperature is lower than 30, the properties change during storage and transportation, which is undesirable because it affects product stability.

In the present invention, the addition of a sequestering agent is considered to improve the processability by changing the physical properties of the sol in accordance with the decrease in viscosity, so that the processability is good even with a high viscosity. Although it is difficult to discuss the processability only by measuring the viscosity, for example, the concentration of the sum total of at least one or more pastes selected from galactomannans and xanthan gum in the aqueous component is 1%. When the processability of the aqueous gel composition at% by mass is evaluated by the viscosity value of the aqueous sol, it is 1 to 300 mPa · s at 60 T and 6 rpm in a BL type viscometer. Work is easy, and more preferably 1 to: LOOOO mPa * s.

The galactomannans of the present invention are polysaccharides having D-galactose side chains in the D-mannose main chain, and examples of natural polysaccharides include oral cast bean gum, tara gum, guar gum, cassia gum, and fenu. Greek gum and the like. Among them, locust bean gum has the best physical properties. Although unpurified and purified products of these polysaccharides are commercially available, use of either of them does not impair the physical properties of the desired aqueous gel composition.

Xanthan gum is a type of microbial polysaccharide produced by fermentation of carbohydrates such as starch, glirecose and sucrose by the microorganism Xanthomonas campestris. When this is dispersed in water, it gives a thixotropic viscous liquid, and its unique properties have been applied to various fields such as food, cosmetics, and ink. An aqueous solution of galactomannans and an aqueous solution of xanthan gum are viscous liquids, respectively, and it is a well-known fact that when they are combined, an aqueous gel is formed. The mass ratio of galactomannans to xanthan gum is 1: 4. -4: When 1, the gel strength is high and an aqueous gel with almost no drainage can be obtained. Outside of this ratio, a gel with sufficient strength could not be obtained, and almost became a viscous liquid.

Preferably, the total concentration of at least one or more pastes selected from galactomannans and xanthan gum is 0.1 to 10% by mass, preferably 0.3 to 5% by mass in the aqueous composition. When it is preferably 0.5 to 3% by mass, a strong gel is formed. A gelled product can be obtained even at a concentration lower than 0.1% by mass, and is suitable when weak gels fulfill their purpose.

In order to obtain a gel composition having a higher gel strength, a galactomannans and a xanthan gum obtained by partially or entirely heat-treating it may be used. For heat-treated products, the moisture content of galactomannans is 50% or less, and 55 to: L min for 5 minutes to 200 hours, or 100 to 150 for 1 minute to 50 hours It is preferred that the xanthan gum be treated at a water content of 50% or less 55 to 150 for 1 hour to 50 hours. These processing methods are disclosed in JP-A-2000-265504.

Conventionally, sequestering agents have been used in detergents, cosmetics, household goods, dyes, and the like, mainly for the purpose of improving cleaning performance and preventing deterioration and discoloration. In the present invention, one or more of these sequestering agents are mixed, and 1 g of them contains 30 mg or more of alkaline earth metal ions (C a ^{2 +} , Mg ^{2 +,} etc.). The pH is adjusted to less than 100 mg, preferably 50 mg or more and less than 70 mg, more preferably 70 mg or more and less than 50 mg. pH adjusters are known water-soluble and acidic or alkaline Good, not particularly limited.

The ratio of the total weight of the galactomannans and xanthan gum to the total weight of such sequestering agents is 1:10 to 99: 1, preferably 1: 5 to 50: 1, more preferably 1: 1 to 50: 1. : 2 to 25: 1 is good. By using this ratio, the sol-gel transition temperature of the aqueous composition is lowered, and the viscosity of the sol is further lowered, so that a gel composition which can be easily processed can be obtained. When this sol is cooled, an aqueous gel composition having high gel strength is obtained. When the ratio of sequestering agent is lower than this, the degree of decrease in the sol-gel transition temperature is insufficient, and when the ratio is high, the gel strength of the aqueous gelled product finally obtained is low. Therefore, it does not meet the purpose of the present invention. Also, when the sequestering agent is adjusted to a pH of less than 30 mg Zg to sequester the alkaline earth metal ion, the degree of decrease in the sol-gel transition temperature is insufficient, and the present invention Does not fit the purpose of

Preferably, the pH of the aqueous solution is adjusted to 5 to 12. Many sequestering agents in this range are used to sequester alkaline earth metal ions such as calcium ions and magnesium ions in a good range, but they do not depend on pH, as in hydroxyethanediphosphonic acid. This is not necessarily the case because some of them have blocking ability. Although it depends on the intended use of the aqueous gel, in the case of pharmaceuticals, cosmetics, etc. that directly touch the human skin, the pH range is preferable in consideration of safety, considering safety. However, this does not apply to household products such as fragrances, household goods and other dosage forms that do not touch the human body.

Examples of sequestering agents that can be used in the present invention include ethylenediaminetetraacetic acid (EDTA) and salts thereof, hydroxyethylethylenediaminetriacetic acid (HEDTA) and salts thereof, and dihydroxyethylethylenediaminediacetic acid (HEDTA). DHEDDA) and its salts, 1,3-propanediaminetetraacetic acid (1,3 PDTA) and its salts, diethylenetriaminepentaacetic acid (DTPA) and its salts, triethylenetetraminehexaacetic acid (TT HA) and its salts, Triacetic acid (NTA) and its salts, tripo Liphosphoric acid and its salts (TPP), hexamethalic acid and its salts (HMP), hydroxyene diphosphonic acid and its salts (HEDP), phytic acid and its salts, boric acid and its salts, darconic acid and its salts, Acid and its salts; malic acid and its salts; tartaric acid and its salts; succinic acid and its salts.

Among them, it is preferable to use ethylenediaminetetraacetic acid and its salt, tripolyphosphoric acid and its salt, hexamethalic acid and its salt, and hydroxyethanediphosphonic acid and its salt.

Conventionally, citric acid, malic acid, etc. have been widely used as sour agents in the food field, but they may also have the purpose of preventing the growth of bacteria by maintaining the pH at 4 or less. However, under such acidic conditions, the gel strength of galactomannan and xanthan gum is reduced, so that the purpose is different from that of the present invention.

Other components of the aqueous gel composition of the present invention include water-soluble alcohols, water-soluble polymers, surfactants, solid, semi-solid, liquid oils, inorganic salts, organic salts, preservatives and antibacterial agents, Antioxidants, fragrances, etc. may be added according to the desired physical properties. There is no problem in blending other components as long as the characteristics of the present invention are not impaired.

Although not particularly limited, examples include water-soluble alcohols such as lower alcohols such as ethanol and isopropanol; sugar alcohols such as sorbitol, xylitol and maltose; propylene glycol; —Polyhydric alcohols such as butylene glycol, glycerin, diglycerin, and polyethylenedaricol. Examples of the water-soluble polymer include plant-based polymers such as gum arabic, guar gum, carrageenan, pectin, and quince, microbial polymers such as dextran, succinoglucan, and pullulan; and animals such as collagen, casein, and gelatin. Cellulosic polymers such as methylcellulose, methylcellulose, hydroxypropylmethylcellulose, carboxymethylcellulose, etc .; Acryl-based polymers; acryl-based polymers such as polyacrylates, polymer acrylates, polyethylene acrylates, and polyacrylamides.

Nonionic surfactants include polyglycerin fatty acid esters, polyethylene glycol fatty acid esters, polyoxyethylene alkyl ethers, polyoxyethylene fatty acid esters, polyoxyethylene sorbitan fatty acid esters, and polyoxygenated surfactants. Ethylene sorbitol fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene propylene glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, etc .; Anionic surfactants such as sodium stearate and palmitin Fatty acid segen such as acid triamine, alkyl benzene sulfonate, alkyl ether carboxylic acid and its salt, carboxylate such as condensation of amino acid and fatty acid Alkyl sulfonate, dialkyl sulfosuccinate, fatty acid ester sulfonate, fatty acid amide sulfonate, polyoxyethylene alkyl sulfate, alkyl phosphate, N-acyl amino acid activator and the like. .

Oils include natural animal and vegetable oils and fats and semi-synthetic oils, hydrocarbon oils, higher fatty acids, ester oils, silicone oils, etc.Natural animal and vegetable oils and fats and semi-synthetic oils include apogado oil, amaji oil, Almond oil, olive oil, carnauba wax, candelilla wax, tallow, beef tallow, beef tallow, hardened tallow, wheat germ oil, sesame oil, rice germ oil, rice bran oil, safflower oil, soybean oil, camellia oil , Evening primrose oil, corn oil, rapeseed oil, horse fat, palm oil, palm kernel oil, castor oil, hardened castor oil, castor oil, jojoba oil, macadamia nut nut oil, beeswax, mink oil, cottonseed oil, coconut oil, hardened coconut oil, Peanut oil, lanolin, liquid lanolin, reduced lanolin, lanolin alcohol, isopropyl lanolin fatty acid, P 0 E lanolin alcohol Le, La Norin fatty acid polyethylene da recall, POE hydrogenated lanolin alcohol Ruesuteru like; hydrocarbon Sukuwaran, squalene, ceresin, paraffin, paraffin wax, liquid paraffin, micro Christa Phosphorus wax, petrolatum, etc .; higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, pendecylenic acid, oleic acid, linoleic acid, linolenic acid, isostearic acid, and 12-hydroxy siatheline Acids and the like; ester oils include diisobutyl adipate, 2-hexyldecyl adipate, di-2-adipate, heptylpandecyl, isostearyl isostearate, trimethytripropane triisostearate, cetyl 2-ethyl cetyl hexate, diethyl _ Neopentyl glycol 2-ethylhexanoate, trimethylolpropane tri-2-ethylhexanoate, pentaerythritol tetra-2-ethylhexanoate, cetyl octanoate, oleyl oleate, octyldodecyl oleate, olein Decyl, neopentyldaricol dicaprate, 2-ethylhexyl succinate, isocetyl stearate, butyl stearate, diisopropyl sebacate, cetyl lactate, myristyl lactate, 2-ethylhexyl palmitate, 2-hexyldecyl palmitate, Palmitic acid 2-heptyl pendecyl, cholesteryl 12-hydroxy cysteate, diisostearyl lignoate, etc .; glyceride oils include triisophosphate glyceride, triisostearate glyceride, triisopalmitate glyceride, Tri-2-ethylhexanoic acid glyceride, trimyristinic acid glyceride, etc .; silicone oils such as dimethylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, Kuta methylcyclopentene evening hexa siloxane siloxane, the dodeca methylcyclopentane, stearoxy higher alkoxy denatured Rico Ichin such as silicone, alkyl modified silicone, higher fatty acid ester modified silicone one down, higher fatty acid ether-modified silicone, and the like.

Preservatives and antibacterial agents include alkyl paraoxybenzoate, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, phenoxyethanols, salicylic acid, benzalkonium chloride, and the like ₍ antioxidants tocopherol, Examples thereof include butylhydroxyanisole and dibutylhydroxytoluene. The production method of the aqueous gel composition of the present invention will be described below, but the production method is not necessarily limited thereto.

Predetermined amounts of at least one paste selected from galactomannans and xanthan gum are added to water, dispersed using a propeller or the like, and heated to 70 to less than 95 to reduce them. Dissolve completely. After that, a sequestering agent is added, and a pH adjuster is further added to adjust the aqueous solution to a pH that sequesters a predetermined amount or more of alkaline earth metal ions, so that a water-soluble alcohol, a water-soluble polymer, Activators, solid, semi-solid, liquid oils, inorganic salts, organic salts, preservatives / antibacterial agents, antioxidants, fragrances and other added components are added. The obtained sol is poured into a desired mold and cooled at 10 to 30 for 30 to 60 minutes to obtain an aqueous gel composition. At this time, the temperature at which the paste selected from galactomannans and xanthan gum are dissolved may be less than 7, but in order to obtain an aqueous gel composition having higher gel strength, 7 Ot: or more is preferable. . Also, the cooling temperature after pouring into the mold is preferably 30 or less in order to obtain an aqueous gel composition having higher gel strength.

Alternatively, a production method in which a sequestering agent is dissolved in purified water before dissolving the paste, the pH is adjusted to block a predetermined amount or more of the alkaline earth metal ions, and then the paste is added and the mixture is heated and dissolved may be used. The aqueous gel composition thus obtained is exactly the same as the aqueous gel composition obtained by the above-described production method in terms of viscosity, gel strength, and the like.

Also, the aqueous gel composition thus obtained is heated and dissolved in 60 to 80 ^ to return to a sol state, and then the sol is poured into a desired mold, and 30 to 30 in 10 to 30. By cooling for 60 minutes, the aqueous gel composition can be obtained again. The aqueous gel composition thus obtained is completely the same as the aqueous gel composition before reheating in terms of viscosity, gel strength, and the like. Here, the reheating temperature at the time of heating and dissolving the aqueous gel composition once gelled is preferably 60 or more in order to obtain a uniform sol solution. Also, the cooling temperature after heating and dissolving the gelled product and pouring it into the mold, In order to obtain an aqueous gel composition having the same gel strength as the gel, 30X: the following is preferable.

It is preferable to add heat-dissipating substances, such as fragrances, heat-labile substances, and volatile substances, after cooling the paste to 60 after dissolving the paste. In this way, no extra heat history is applied and material loss is reduced.

Also, the aqueous gel composition once gelled is heated and dissolved at 60 to 80 to form a sol state, cooled down to 60, and then the substances are added.Then, the sol is poured into a desired mold. An aqueous gel composition can also be obtained by cooling with 30 ^ for 30 to 60 minutes. The aqueous gel composition thus obtained is completely the same as the aqueous gel composition before reheating in terms of viscosity, gel strength, and the like.

As described above, the aqueous gel composition of the present invention has the property of being easily reheated when it is converted into a sol, so that the reheating time during production is reduced, and the energy cost for solification is reduced. Is cheaper. In addition, since the sol has a certain fluidity, there is no need to heat the piping at the time of filling, and the components do not deteriorate due to heating. In addition, since it is easy to accurately fill a certain amount, filling workability is improved.

Packs are one of the cosmetics that have been used for a long time. They are used not only for the face but also for the neck, shoulders, arms, and legs, as well as the whole body. There are a wide variety of preparations such as Piloff type, wiping or rinsing type, peeling after solidification, rubbing and eve, etc. It makes the skin soft.

The aqueous gel composition of the present invention is highly useful as a gel material for a patch-type pack-shaped cosmetic applied to nonwoven cloth because of its performance and processability.

As a method for obtaining a pack-like cosmetic containing the aqueous gel composition of the present invention, galactomannans, xanthan gum, sequestering agent, glycerin, propylene glycol, and purified water are stirred while adding 80 to 30 minutes. Warm melting Then, adjust the pH to 5 to 12 with a pH adjuster, add other perfume and beauty ingredients, and cool. The obtained gel composition is heated and dissolved, the solution is lightly applied to a non-woven cloth, cooled and solidified, and then cut out into a desired shape such as a face or a square to obtain a pack-shaped cosmetic. The pack cosmetic thus obtained had a good feeling of use without impairing the fragrance and beauty ingredients.

In the aqueous gel composition of the present invention, not only pharmaceuticals, medical devices, pharmaceutical materials, cosmetics, household goods, household goods and foods, but also materials such as architecture, agricultural chemicals, feed, fertilizers, paints, inks, ceramics, resins or resins It can be widely used in industrial fields such as adhesives.

In the present invention, it is an aqueous gel composition made of galactomannans, xanthan gum and a sequestering agent, and has high gel strength, excellent processability, pharmaceuticals, medical devices, pharmaceutical materials, cosmetics, household goods, household goods, It can be widely used not only in food but also in industrial fields such as construction, agrochemicals, feed, fertilizers, paints, inks, ceramics, resins and adhesives. It should be noted that the product of the present invention can be used by blending other third components when it is used in various industries. In this case, it is possible to mix all the components at the same time and to dissolve them, as well as to mix components that are unstable to heat, after reheating the gel composition to obtain a sol state.

[Best mode for carrying out the invention]

Hereinafter, the present invention will be specifically described with reference to Examples and Comparative Examples, but these are intended to illustrate the present invention and do not limit the present invention in any way.

Table 1 shows an example of the amount (mg) of alkaline earth metal ions that can be sequestered by 1 g of the sequestering agent.

Note 1) A commercial product of Teikoku Chemical Industry Co., Ltd. is used as ethylenediaminetetraacetic acid. Note 2) A commercial product of Teikoku Chemical Industry Co., Ltd. is used as trisodium triacetate.

Note 3) A commercially available product manufactured by Wako Pure Chemical Industries, Ltd. is used as sodium tripolyphosphate. Note 4) A commercially available product manufactured by Wako Pure Chemical Industries, Ltd. is used as sodium hexamethyphosphate <Note 5) A commercially available product manufactured by Henkel is used as sodium hydroxyethanediphosphonate.

Note 6) A commercially available product manufactured by Wako Pure Chemical Industries, Ltd. is used as trisodium citrate.

Note 7) A commercially available product manufactured by Wako Pure Chemical Industries, Ltd. is used as sodium dihydrogen phosphate.

1. Preparation of aqueous gel composition

The aqueous gel compositions were prepared with the formulations shown in Tables 2 and 4. Specifically, a paste was gradually added to purified water while stirring the purified water of 25: with a blade-type stirrer. After the paste was dispersed, heating was started and the mixture was stirred at 80 for 30 minutes to dissolve. After adding a sequestering agent and adding a pH adjuster to adjust the pH, purified water at 80 ° C. was adjusted to pH 10 and stirred. The obtained sol was poured into a deep petri dish, and cooled at 25 for 60 minutes to obtain 500 g of each of the aqueous gel compositions of Examples 1 to 10 and the gels of Comparative Examples 1 to 7. I got it.

2. Measurement of gel strength (breaking strength)

The solution prepared in 1 was dispensed so that it slightly overflowed into a deep petri dish (60 mm ψ X 60 mm), and then left at 25 for 24 hours. Thereafter, the portion protruding from the petri dish was cut flat with a knife to obtain a sample. The breaking strength was evaluated using a rheometer (manufactured by Fudo Kogyo: rheometer CW type). A 10 mm diameter disk was attached as an adapter for directly compressing the prototype, and the sample was compressed at a compression speed of 30 cmZ and distorted until it broke, and the breaking strength was measured. The results are shown in Table 3 for Examples 1 to 10 and Table 5 for Comparative Examples 1 to 7.

3. Measurement and evaluation of sol viscosity

Measure the viscosity of the solution prepared in step 1, 60, BL viscometer, 6 rpm, 1 minute The viscosity value was measured by converting the subsequent reading. When performing operations such as casting, if the viscosity of the solution is lower than 1000 OmPas, it is easy to work, and if it exceeds 300 mPas, it becomes difficult. The prices are 〇 (less than l OOO OmP a 's), △ (less than 100 000 m Pa s), X (more than 300 000 mPa a s), and 〇 and △ Was passed and X was rejected. The results are shown in Table 3 for Examples 1 to 10 and Table 5 for Comparative Examples 1 to 7.

4. Measurement and evaluation of sol-gel transition temperature

While gradually cooling the viscosity of the solution prepared in Step 1 at 80, continue measuring it at 6 rpm with a BL viscometer. When the reading rises sharply (more than 3 times that at 8 O) The temperature was measured and taken as the sol-gel transition temperature. The lower the sol-gel transition temperature, the better the workability. Particularly, the workability was good when the temperature was lower than 55. On the other hand, when the sol-gel transition temperature was higher than 60, the workability was significantly reduced. ), X (less than 55 to 60), X (more than 60), 〇 and 合格 were passed, and X was rejected. The results are shown in Table 3 for Examples 1 to 10 and Table 5 for Comparative Examples 1 to 7.

Table 2

Examples 1 to: L 0 (formulation)

α. Τ 100 100 100 100 100 100 100 100 100 100 ρΗ9 10 10 10 10 10 10 10 10 10 10 Note 9) Use commercially available Saneigen F · F · I company.

Note 10) A commercially available product from San-Ei Gen F · F · I is used after heating at 120 for 10 minutes.

Note 1 1) Use a commercial product manufactured by Kelco

Note 1 2) Nisshin Oil Co., Ltd. commercial product is used as the heat-treated xanthan gum.

Table 3

Examples 1 to: L 0 (Result)

Table 4

Comparative Example 7 (Formulation)

Table 5

Comparative Example 7 (Result)

Comparative example No. 1 2 3 4 5 6 7 Breaking strength 252 320 90 109 310 267 285

(g / cm ² ) Viscosity test XXXX 〇 XX

(mP a-s) 32 300 68 200 45 500 39000 6 240 64 200 66 700 Gelation temperature XXX Δ Δ XX Based on these results, the product of the present invention has high breaking strength, low viscosity at 60, and low sol-gel transition temperature. It was shown to be a low aqueous gel. On the other hand, the comparative products 1 to 4 had almost the same breaking strength as the product of the present invention, but had a high viscosity, and some of them had already started to gel at 60: and were difficult to handle. In Comparative Example 5, carrageenan was used in place of xanthan gum, and a product having a breaking strength and a viscosity similar to that of the product of the present invention was obtained. However, drainage due to storage was severe, and the product was not usable. Further, Comparative Examples 6 and 7 differ from the present invention in that they are adjusted to a PH region having a low ability to sequester alkaline earth metal ions and a sequestering agent having a low ability to sequester alkaline earth metal ions. However, the effect of lowering the sol viscosity was small, the sol-gel transition temperature hardly changed, and there was almost no difference compared with Comparative Example 2 in which sol was not added.

5. Preparation and evaluation of face mask

The aqueous gel composition was prepared according to the formulation shown in Table 6. Specifically, a paste was gradually added to the purified water while stirring the purified water 25 with a blade-type stirrer. After the paste was dispersed, heating was started and the mixture was stirred at 80 for 30 minutes to dissolve. After adjusting the pH to 9 by adding a sequestering agent (HMP-6Na: hexamedium phosphate), the mixture was added and stirred with 80 t of purified water adjusted to pH9. . Thereafter, the mixture was allowed to cool to 3 Ot: or less to obtain an aqueous gel composition.

The obtained aqueous gel composition was heated to 65 X: and other components such as limonene were added. Then, it was applied to a non-woven cloth to a thickness of about 1 mm, cut out into a face after cooling, and a face mask coated with the aqueous gel composition was obtained. In the case of 65, if the viscosity was too high to apply it to the non-woven cloth, it was prepared by heating again to make the viscosity sufficiently low, and applying it quickly while keeping the temperature. The face mask obtained as described above was applied to the faces of 10 subjects, and the remaining amount of limonene was verified by the intensity of the scent. At that time limonene not Comparative Example of Addition 10 Assuming that the scent of 0 was the reference 0 (0 point), and the scent became stronger, it was evaluated as + (1 point), ++ (2 points), + + + (3 points), and ∑ ( (Number of people X points). The results are shown in Table 6.

Table 6

Prescription example

Note 1 3) Kao Corporation uses polyoxyethylene hydrogenated castor oil.

From these results, it can be seen that in Examples 11 and 12, the fragrance was more remarkably felt by the limonene blend than the reference, whereas in Comparative Example 8, few people felt the difference from the reference. Only in Comparative Example 9 where the amount was increased, an aroma equivalent to that of Example 11 was obtained. In the comparative example, when the nonwoven cloth was applied, the viscosity was high, and reheating to 80 was necessary. At that time, limonene was volatilized and lost, and it is considered that the above evaluation results were obtained.

Claims

The scope of the claims

1. A component: a paste comprising one or more galactomannans, B component: xanthan gum, C component: one or more sequestering agents, and an aqueous gel composition comprising water, wherein the aqueous gel The pH of the composition is within the pH range where 30 g or more of alkaline earth metal ions can be sequestered per 1 g of the C component, and their mass ratio is A component: B component = 1: 4 to 4: 1. An aqueous gel composition in which (A component + B component): C component = 1: 10 to 99: 1.

2. The aqueous gel composition according to claim 1, wherein the content of (A component + B component) in the aqueous gel composition is 0.1 to 10% by mass.

3. Claim 1 or 2, wherein the range of pH at which 3 g or more of alkaline earth metal ions can be sequestered per 1 g of the C component is within the range of pH 5 to 12. Aqueous gel composition.

4. The aqueous gel composition according to any one of claims 1 to 3, wherein the sol-gel transition temperature is in a range of 45 to 60.

5. A pack cosmetic comprising the aqueous gel composition according to claim 1.