JP3531735B2 - Method for producing thickener and cosmetic - Google Patents

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a thickener mainly used in the fields of cosmetics, pharmaceuticals and the like. More specifically, it does not have a sticky feeling, has excellent usability, does not cause a decrease in the viscosity of the system even when a large amount of water-soluble drug components, salts, etc. are mixed, and does not cause water separation etc. over a long period of time, The present invention relates to a novel method for producing a thickener, a thickener obtained by the method, and a cosmetic containing the thickener.

[0002]

2. Description of the Related Art Conventionally, as a thickening method for cosmetics, a method using a polysaccharide such as xanthan gum, a hydrophilic synthetic polymer such as polyacrylic acid, or a clay mineral such as bentonite as a thickener is known. .

However, when a polysaccharide such as xanthan gum is used as a thickening agent, the stability in a system in which a drug component and salts are simultaneously mixed is excellent, but there is a problem in usability such as a sticky feeling. . In addition, when a hydrophilic synthetic polymer such as polyacrylic acid is used, a sticky feeling and a refreshing feeling are obtained, and the usability is good, but the salt resistance and the ionic resistance are low, so that a drug component or a salt is used. When a large amount of is added, there is a problem that the viscosity of the system is lowered. Furthermore, when a clay mineral such as bentonite is used as a thickener, there is a problem in usability such as a squeaky feeling.

[0004]

DISCLOSURE OF THE INVENTION The present invention has no sticky feeling or squeaky feeling, has excellent usability, and can cause a decrease in viscosity even when a drug component or salt is highly blended. The purpose of the present invention is to obtain a new type of thickener that is stable and does not cause water separation for a long period of time.

[0005]

Means for Solving the Problems As a result of intensive studies conducted by the present inventors in order to solve the above problems, as a result, a compound having gelling ability such as agar, which has been conventionally used as a gelling agent, is solidified. After gelling it, it was pulverized and used as a microgel as a thickener, so that it did not have a sticky feeling, and it was a water-soluble substance that was a problem when using conventional thickeners. The inventors have found that even if a high content of a drug component or various salts and the like is added, the problem of decreasing the viscosity of the system does not occur, and have completed the present invention.

That is, in the present invention, a hydrophilic compound having gelling ability, or a hydrophilic compound having gelling ability and a thickening compound having no gelling ability are dissolved in water or an aqueous component. The present invention relates to a method for producing a thickener, which is obtained by obtaining a thickener by allowing to stand and cool to form a gel, and then crushing the gel to obtain a microgel having an average particle size of 0.1 to 1,000 μm.

In the above, the average particle size of the microgel is 1 to
300 μm is preferable.

The present invention also relates to a thickener obtained by the above-mentioned manufacturing method.

The present invention also relates to a cosmetic containing the above thickener.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below.

The hydrophilic compound having a gelling ability used in the method for producing a thickener of the present invention may be a water-soluble compound having a gelling ability, which can be used in the fields of cosmetics and pharmaceuticals. However, it is not particularly limited. Specifically, hydrophilic proteins having gelling ability such as gelatin and collagen, hydrophilic polysaccharides such as agar, curdlan, scleroglucan, schizophyllan, gellan gum, alginic acid, carrageenan, mannan, pectin, hyaluronic acid, etc. Is exemplified. Among them, gelatin, agar, curdlan, gellan gum, alginic acid, carrageenan,
It is particularly preferably used because it is hardly affected by salts and ions and a stable gel can be prepared. One type or two or more types of hydrophilic compounds having gelling ability can be used.

Then, these hydrophilic compounds having gelling ability are dissolved in water or an aqueous component and then left to cool to solidify to form a gel. The above compound can be dissolved in water or an aqueous component by mixing, heating or the like.

The gelation (solidification) is carried out by stopping the heating after the dissolution and leaving (standing) until the temperature becomes lower than the gelation temperature (solidification temperature).

The aqueous component is not particularly limited as long as it is an aqueous component that can be used in the fields of cosmetics and pharmaceuticals. For example, glycols such as 1,3-butylene glycol and propylene glycol, ethanol, propanol and the like. In addition to the lower alcohols mentioned above, it is possible to contain components that are generally blended as an aqueous phase component of cosmetics.
Specific examples thereof include chelating agents such as metaphosphates and edetates, pH adjusters, preservatives, etc., but are not limited to these examples.

The gel strength of the gel is not particularly limited as long as the gel itself can maintain its shape and a microgel in the next step can be obtained. In the present invention, a gel having a considerably high gel strength can be used, for example, a jelly having a high jelly strength of about 1,000 g / cm ² (day cold water measurement) or less can be used. Jelly strength 30g / cm
Microgels can be obtained with a fairly weak gel strength of about ² . Jelly strength of 100g /
It is preferably about cm ² .

In addition to the above-mentioned hydrophilic compound having gelling ability, a thickening compound having no gelling ability may be used together for the purpose of changing the feeling of use. Examples of thickening compounds having no gelling ability include hydrophilic synthetic polymers such as polyacrylic acid, polyethylene glycol, polyacrylamide, polyalkylacrylamide / polyacrylamide copolymer, carboxymethyl cellulose, cationized cellulose, and pluronic. Xanthan gum, succinoglycan, guar gum,
In addition to hydrophilic natural polymers such as locust bean gum, hydrophilic thickening compounds such as hydrophilic clay minerals such as laponite, bentonite and smectite are exemplified.
Further, by using together these hydrophilic thickening compounds having no gelling ability, the gel strength of the obtained gel can be freely adjusted. The gel strength is lowered by increasing the blending ratio of the thickening compound having no gelling ability. As the thickening compound having no gelling ability, xanthan gum, succinoglycan, polyacrylic acid, polyethylene glycol, polyacrylamide, and polyalkylacrylamide / polyacrylamide copolymer are particularly preferable. Further, salts of these compounds are also preferably used. As the thickening compound having no gelling ability, one kind or two or more kinds can be used.

The blending ratio of the hydrophilic thickening compound having no gelling ability varies depending on the intended use of the thickening agent, etc., but is 1 to 100 relative to the hydrophilic compound having a gelling ability.
It can be blended in a proportion of about wt%.

Next, the gel thus formed is crushed with a homogenizer, a disper, a mechanical stirrer or the like to obtain a desired microgel. In the present invention, the average particle size of the microgel is 0.1 to 1,000 μm, preferably about 1 to 300 μm, more preferably 10 to 200 μm.
It is about μm. The average particle size of the microgel is 1,000μ
If it exceeds m, there may be a problem in usability such as poor finger performance. On the other hand, if it is less than 0.1 μm, the viscosity as a gel formulation may not be maintained. The degree of crushing can be adjusted according to the purpose to the extent that the average particle size of the obtained microgel does not deviate from the range of the present invention, and if smoother usability is required, high-speed stirring can be performed. Crush well to make a microgel of fine particle size, while
When the feel of the microgel itself is required, the degree of crushing is weakened by light stirring to obtain a microgel having a slightly larger particle size.

The viscosity of the thus-obtained microgel cannot be unequivocally determined because the required viscosity varies depending on the application. For example, when agar is used, the agar concentration is 0.5 to.
B type viscometer (rotation speed 0.6 rpm, 25
2,000 to 1,000,000 mP measured by
a. It is preferably about s.

By using the microgel obtained by the present invention as a thickening agent in cosmetics and the like, it is possible to improve the feeling of use (no sticky feeling), and at the same time, it is possible to use a high content of drug components and salts, such as cosmetics. Even when about 20% by weight was contained in the total amount of the cosmetic, it was possible to maintain the viscosity of the cosmetic system without lowering the viscosity of the system. In addition, it is stable for a long period of time and does not cause water separation. It should be noted that the compounding amount of the drug components, salts and the like is preferably about 0.1% by weight or more based on the total amount of the cosmetic in order to obtain the desired effect of the compounding of these components.

The above-mentioned drug components and salts may be either water-soluble or oil-soluble.

Examples of the drug component include vitamins, anti-inflammatory agents, antibacterial agents and the like. Specific examples of the drug component include vitamins B and P, vitamins such as water-soluble vitamins A and D and derivatives thereof, pantotenyl ethyl ether, calcium pantothenate, glycyrrhizin, glycyrrhizinate, glycyrrhetin, glycyrrhetinate, -Jar jelly, polyphenols, nicotinic acid and its derivatives (for example nicotinic acid amide), resorcin, sulfur, salicylic acid and its derivatives, urea, xylitol, trehalose, caffeine and the like.

The salts include organic acid salts, amino acid salts, inorganic salts and the like. Examples of organic acid salts include hydrochlorides such as citric acid, lactic acid, oxalic acid, and sulfonic acid, metal salts (sodium salt, potassium salt), amine salts, and the like. Examples of the amino acid salt include hydrochlorides such as glycine, alanine, proline, lysine, aspartic acid and glutamic acid, metal salts (sodium salt, potassium salt), amine salts and the like. As the inorganic salt, sodium, potassium, magnesium, calcium and the like carbonates, phosphates,
Examples thereof include nitrates, borates, sulfates, sulfites, halogen compounds (sodium chloride, potassium chloride, etc.).

The thickener of the present invention or the cosmetic containing the thickener has a high salt resistance, which is the case when these salts are blended or the above-mentioned drug components are blended in the form of a salt. However, the stability of the system is not affected by the other components that are mixed together, and the usability is excellent.

Conventionally, compounds having gelling ability such as agar, carrageenan, curdlan and gelatin were sometimes used as thickeners. In such a case, these compounds are heated, dissolved and gradually stirred while stirring. By cooling, a viscous state was obtained without solidification (gelation) (for example, JP-A No. 11-209262). However, as shown in the above-mentioned conventional method, when the compound having gelling ability is gradually cooled with stirring to form a thickener, the degree of thickening of the system is limited. In particular, when a drug component or salt is added, the viscosity of the system decreases.

On the other hand, in the present invention, these compounds are once completely gelled (solidified) and then pulverized into a microgel to be used as a thickener. The thickener of the present invention thus obtained, unlike the thickener polysaccharides or synthetic polymer thickeners conventionally used in cosmetics, does not exert a thickening effect by entanglement at the molecular level, This is due to friction between crushed microgels. Therefore, the spinnability characteristic of the polymer solution is not observed at all, and a very refreshing feeling of use can be realized. Further, the polymer solution may be affected by the drug to be blended, the salt, etc. to cause a decrease in viscosity, and the blending may be limited, but in the case of the present invention, there is no such concern, and the range of prescription of cosmetics etc. Can be extended.

When a water-soluble drug component or salt is used in the present invention, it is dissolved in water or an aqueous component together with the above-mentioned hydrophilic component having gelation ability and then left to cool and solidify. May be used as a microgel by crushing the gel to form a gel, or alternatively, the hydrophilic component having gelling ability is dissolved in water or an aqueous component and then left standing to cool and solidify. The gel thus obtained may be pulverized into a microgel, and a drug component, salts or the like may be mixed and used.

On the other hand, when an oil-soluble drug component, salt or the like is used, the hydrophilic component having the gelling ability is dissolved in water or an aqueous component and then left to cool and solidify to form a gel. Forming and then crushing the gel into a microgel, while separately preliminarily emulsifying an oil-soluble drug component, salts, etc. with other oily components in an aqueous system, the preemulsion and the microgel It is preferable to use after mixing and emulsifying.

When the thickener obtained by the present invention is used in a cosmetic composition, it is generally used as an additive component that can be incorporated in the cosmetic composition, such as a moisturizer, an antiseptic, a powder, a pigment, a fragrance, and a pH.
A regulator and the like can be appropriately blended within a range that does not impair the objects and effects of the present invention. The cosmetics are not particularly limited in their form and dosage form, such as aqueous, liquid, gel, chrome and the like. For example, it is preferably applied to moisturizing creams, massage creams, beauty essences, lotions, emulsions, makeup cosmetics, sun care products, hair cosmetics such as hair setting agents and hair creams, hair dyes, and body care products.

[0030]

The present invention will be described in more detail based on the following examples, but the invention is not intended to be limited thereto.

Examples 1 to 14 and Comparative Examples 1 to 7 Thickeners having the compositions shown in Tables 1 and 2 below were prepared.

In Examples 1 to 14, a hydrophilic compound having a gelling ability and a thickening compound having no gelling ability were mixed in an aqueous system, heated at 90 ° C., dissolved and then cooled to form a gel. did. This gel was crushed using a homogenizer to produce a microgel (average particle size 100 μm). The other ingredients were mixed with this microgel and stirred to obtain a thickener.

On the other hand, in Comparative Examples 1 to 7, after mixing the respective components, the mixture was allowed to stand for 12 hours at room temperature to obtain a thickener.

Using the samples obtained in Examples 1 to 14 and Comparative Examples 1 to 7, the thickening effect, usability (no sticky feeling), and long-term stability were evaluated according to the following evaluation criteria. The results are shown in Tables 1 and 2. In Tables 1 and 2, "sodium polyacrylate" means "Hibiswako 105".
(Wako Pure Chemical Industries, Ltd.) neutralized with an aqueous sodium hydroxide solution to PH7 was used.

[Thickening Effect] The viscosity (25 ° C.) of the obtained sample was measured using a B-type viscometer (rotation number: 0.6 rpm) to evaluate the thickening effect. (Evaluation) ◎: Very excellent thickening effect (viscosity 50,000 mPa · s or more) ○: Excellent thickening effect (viscosity 5,000 to less than 50,000 mPa · s) Δ: No significant thickening effect (viscosity 500 ~ 5,000 m
(Less than Pa · s) ×: no thickening effect (viscosity less than 500 mPa · s)

[Lightness (no stickiness)] A female panel (20 persons) was asked to actually use each sample.
The feeling of use was evaluated according to the following criteria. (Evaluation) ◎: 18 or more people answered that there was no sticky feeling ○: 15 to 17 people answered that there was no sticky feeling △: 6 to 14 people answered that there was no sticky feeling ×: 5 people or less Answered that there is no stickiness

[Long-term stability (no water separation)] The degree of water separation after storage for 1 month at 40 ° C. was visually observed and evaluated according to the following evaluation criteria. (Evaluation) ◎: No syneresis was observed at all ○: Almost no syneresis was seen △: Slight oozing of water was observed ×: Water oozing was observed

[0038]

[Table 1]

[0039]

[Table 2]

As is clear from the results shown in Tables 1 and 2, the thickener according to the present invention exhibits a stable thickening effect even in the presence of a high concentration of salt, and is excellent in the feeling of use and the long-term stability. It was a thing.

(Examples 15 to 16 and Comparative Examples 8 to 9) Samples having the compositions shown in Table 3 below were prepared.

In Examples 15 and 16, the components were mixed, and 90
After heating and melting at 0 ° C, the mixture was slowly cooled to form a gel. This gel was crushed using a homogenizer to produce a microgel (average particle size 100 μm).

On the other hand, in Comparative Examples 8 and 9, each component was added at 90 ° C.
After mixing, the heating was stopped and the mixture was left at room temperature.

When the properties of the samples obtained in Examples 15 and 16 and Comparative Examples 8 and 9 were examined, as shown in Table 3, the samples obtained in Examples 15 and 16 were viscous. ,
On the other hand, the samples obtained in Comparative Examples 8 and 9 were gels (solid) without thickening.

[0045]

[Table 3]

(Example 17, Comparative Example 10) O / W cream [thickener A] (composition component) (% by weight) (1) agar 1 (2) keltrol 0.1 (3) ion exchange Water 98.9 (Production method) The above (1) to (3) are mixed and heated to 90 ° C.
After dissolution, the mixture was slowly cooled to form a gel. The gel was crushed using a homogenizer to obtain a microgel (thickener A) having an average particle size of 100 μm.

[Emulsified Part A] (Compounding Component) (wt%) (1) Polyacrylic acid-alkyl acrylate copolymer 0.1 (2) Polydimethylsiloxane (6 mPa · s) 8 (3) Hydroxylation Potassium 0.1 (4) Ion-exchanged water 91.8 (Production method) (3) is added to (4), and (1),
(2) was added, mixed and stirred to obtain an emulsified part A.

As Example 17, 48% by weight of the above thickener A, 2% by weight of salt and 48% by weight of the emulsified portion A were mixed and stirred to emulsify to prepare an O / W cream.

On the other hand, as Comparative Example 10, an O / W cream was prepared in the same manner as above except that 2% by weight of salt and 98% by weight of emulsified portion A were used.

O / O obtained in these Example 17 and Comparative Example 10
For W cream, B type viscometer (rotation speed 0.6 rpm)
The viscosity (25 ° C.) was measured using
Is 400,000 mPa · s, and Comparative Example 10 is 18.0
It was 00 mPa · s.

As is clear from these results, it can be seen that in a system in which the emulsion alone does not thicken (a system having weak salt resistance), it is possible to increase the viscosity by adding the microgel.

(Example 18) Massage cream (O / W) (composition component) (% by weight) (1) Solid paraffin 5 (2) Beeswax 10 (3) Vaseline 15 (4) Liquid paraffin 31 (5) Glycerin 4 (6) Glycerin monostearate 2 (7) POE (20) Sorbitan monolaurate 2 (8) Borax 1 (9) Carrageenan 0.3 (10) Succinoglycan 0.1 (11) Purified water Residue Remainder (12) Preservative proper amount (13) Antioxidant proper amount (14) Perfume proper amount (production method) (8) was added to a part of (11) and heated to 70 ° C. (aqueous phase). After heating and dissolving the oil ((1) to (6)),
(7) was added and maintained at 70 ° C. This was gradually added to the previously prepared aqueous phase for preliminary emulsification. The emulsion particles were homogenized with a homomixer (emulsification section).

On the other hand, (9) and (10) are added to the rest of (11).
Was melted at 90 ° C., cooled and gelled, and then sufficiently crushed with a homomixer to obtain a microgel (average particle size 80 μm). This microgel was added to the emulsified part, stirred, degassed, filtered and cooled to obtain a massage cream (O / W).

(Example 19) Hair setting gel (composition component) (% by weight) (1) Carboxyvinyl polymer 0.7 (2) Polyvinylpyrrolidone 2 (3) Glycerin 3 (4) Sodium hydroxide Appropriate amount ( 5) Hydrochloric acid Appropriate amount (6) Ethanol 5 (7) Curdlan 1 (8) Xanthan gum 0.2 (9) Polyoxyethylene octyldodecyl ether Appropriate amount (10) Perfume Appropriate amount (11) Chelating agent Appropriate amount (12) Purified water The rest (production method) (1) was dispersed in (3) and part of (12).
(2), some (4), (6), (9) to (11) were dissolved in the remaining (12), and this was mixed with the above dispersion to obtain a mixed solution. (7) was dissolved in the remaining (4), (8) was added and dissolved, and the mixture was neutralized in (5). This is mixed with the above mixed solution, heated at 80 ° C. for 10 minutes, crushed the gel with a homogenizer to obtain a microgel (average particle size 80 μm), filtered, degassed and cooled to obtain a hair setting gel. It was

(Example 20) O / W cream [emulsified part B] (composition) (wt%) (1) stearic acid 8 (2) stearyl alcohol 4 (3) butyl stearate 6 (4) propylene Glycol 5 (5) Glycerin monostearate 2 (6) Potassium hydroxide 0.4 (7) Ion-exchanged water An oily component was added to the residual aqueous phase portion, mixed and stirred to obtain an emulsified portion B.

30% by weight of this emulsified part B, 1% by weight of caffeine and 69% by weight of the thickener A obtained in Example 11 were mixed to obtain an O / W cream.

(Example 21) O / W cream [emulsified part C] (composition component) (% by weight) (1) solid paraffin 5 (2) beeswax 10 (3) petrolatum 15 (4) liquid paraffin 41 ( 5) 1,3 butylene glycol 4 (6) Glycerin monostearate 2 (7) POE (20) Sorbitan monolaurate 2 (8) Boric acid 0.2 (9) Ion-exchanged water Residual oil phase oil component Was added, mixed and stirred to obtain an emulsified part C.

70% by weight of this emulsified part C, 1% by weight of aspartic acid, and 29% by weight of the thickener A obtained in Example 11.
Mixed to obtain an O / W cream.

(Example 22) Pack [emulsified part D] (composition component) (% by weight) (1) polyvinyl acetate emulsion 15 (2) polyvinyl alcohol 10 (3) sorbitol 5 (4) polyethylene glycol (PEG400 ) 5 (5) Jojoba oil 4 (6) POE sorbitan monostearate 1 (7) Titanium oxide 5 (8) Talc 10 (9) Ethanol 10 (10) Ion-exchanged water 37 Add an oily component to the water phase part, Emulsified part D was obtained by mixing and stirring.

80% by weight of this emulsified part D, 0.5% by weight of dipotassium glycyrrhizinate, and 19.5% by weight of the thickener A obtained in Example 11 were mixed to obtain a pack.

All of the skin external preparations obtained in Examples 17 to 22 were excellent in thickening property, had no sticky feeling, and had a refreshing feeling of use. It was also excellent in long-term stability.

(Example 23, Comparative Example 11) O having the following composition
With respect to the / W cream, a comparison of the viscosities by the manufacturing method was performed.

(Composition) (% by weight) (1) Squalane 10 (2) Vaseline 5 (3) 1,3 Butylene glycol 4 (4) Glycerin monostearate 2 (5) POE (20) sorbitan monolauric acid Ester 2 (6) Agar 1.5 (7) Celtrol 0.2 (8) Ion-exchanged water Residual [Production method 1] (8) was added with (3) to (7), and heated to 90 ° C. to dissolve. After that, continuously stirring, adding (1) and (2) at 70 ° C., stirring and cooling to room temperature, and O / W
A cream was prepared.

[Production method 2] (8) 50% by weight (3),
After adding (6) and (7), heating and melting, cooling gelation and crushing this, microgel (average particle size 80 μm)
And A paste-like aqueous gel thus obtained,
(8) (4) and (5) were dissolved in the rest, and an O / W cream containing (1) and (2) was well mixed at 70 ° C. to prepare an emulsion (O / W cream).

The viscosity (25 ° C.) of the O / W cream obtained by the manufacturing method 1 and the manufacturing method 2 was measured by a B type viscometer (rotation speed 0.6 p.
m). As a result, in the O / W cream obtained by the manufacturing method 1, 140,000 mPa · s, the manufacturing method 2
300,000mP for O / W cream obtained by
It was a.s. That is, it can be seen that even if the composition is exactly the same, the viscosity of the system containing the crushed gel microgel is excellent.

(Example 24) Moisture gel (composition component) (% by weight) (1) Ion-exchanged water residue (2) Agar 2 (3) Dipropylene glycol 10 (4) Trimethylglycine 5 (5) Hyalurone Acid 0.1 (6) Polyacrylic acid Na 0.2 (7) Polyacrylamide 0.5 (8) Silica powder 1 (9) EDTA Appropriate amount (10) Citric acid Appropriate amount (11) Perfume Appropriate amount (12) Preservatives (2) to (7) and (9) to (12) were added to an appropriate amount (manufacturing method) (1), dissolved at 85 ° C or higher, and then left to cool to 30 ° C or lower to solidify. Add (8) to this, and pulverize it sufficiently with a homogenizer to form a microgel (average particle size 60
μm) and then uniformly dispersed to obtain a moisture gel.

(Example 25) Moisture cream (composition component) (% by weight) (1) Ion-exchanged water balance (2) Agar 1.5 (3) Dipropylene glycol 10 (4) Xylitol 5 (5) Hyaluronic acid 0.1 (6) Polyacrylamide 0.5 (7) Cyclic silicon 5 (8) Squalane 5 (9) Acrylic acid-alkyl acrylate copolymer 0.2 (10) EDTA Suitable amount (11) Triethanolamine Suitable Amount (12) Citric acid Appropriate amount (13) Perfume Appropriate amount (14) Preservative Appropriate amount (Manufacturing method) (2) to (6), (10),
After adding (12) and (14) and melting at 85 ° C or higher,
It was left to cool to 30 ° C. or lower and solidified. This was thoroughly pulverized with a homogenizer to give a microgel (average particle size 70
μm). Here, (7) to (9) in part of (1),
(13) was added, and (11) was added to what was uniformly dispersed with a homomixer, and an emulsion prepared by preparing emulsion particles was further added with a homomixer to perform uniform dispersion to obtain a moisture cream.

(Example 26) Pack (composition component) (% by weight) (1) Residue of ion-exchanged water (2) Agar 1.5 (3) Glycerin 15 (4) Polyethylene glycol (PEG300) 5 (5 ) Montmorillonite 3 (6) Spherical resin powder (alkyl polyacrylate) 3 (7) Zinc white 1 (8) Glycyrrhizinate proper amount (9) Xanthan gum 0.2 (10) EDTA proper amount (11) Lactic acid proper amount ( 12) Perfume Proper amount (13) Preservative Proper amount (manufacturing method) (2) to (4) and (8) to (13) were added to (1), dissolved at 85 ° C or higher, and then allowed to stand at 30 ° C or lower. Cooled and solidified. This was sufficiently pulverized with a homogenizer to form a microgel (average particle size 60 μm). (5) to (7) were added thereto, and the mixture was uniformly mixed and dispersed to obtain a pack.

(Example 27) Eye gel (composition component) (% by weight) (1) Ion-exchanged water residue (2) Agar 2 (3) Glycerin 10 (4) Polyvinyl alcohol 1 (5) Polyacrylamide 0 .2 (6) Trimethylsiloxysilicic acid 1 (7) Dimethylpolysiloxane 5 (8) Salt 0.5 (9) Acrylic acid-alkyl acrylate copolymer 0.1 (10) EDTA Suitable amount (11) Citric acid Suitable amount (12) Perfume proper amount (13) Preservative proper amount (manufacturing method) (2) to (5), (8), (1
0), (11), and (13) were added, and the mixture was melted at 85 ° C or higher and then left to cool to 30 ° C or lower to solidify. This was sufficiently pulverized with a homogenizer to form a microgel (average particle size 70 μm). Here (1) to the rest (6),
(7), (9) and (12) were added, and the mixture was uniformly dispersed with a homomixer and further dispersed to obtain an eye gel.

(Example 28) Jelly-like pack (composition component) (% by weight) (1) Ion-exchanged water balance (2) Agar 1.5 (3) Ptyrene glycol 10 (4) Ethanol 12 (5) ) Polyacrylamide 0.2 (6) Carboxyvinyl polymer 0.5 (7) Salt 0.5 (8) Potassium hydroxide proper amount (9) EDTA proper amount (10) Citric acid proper amount (11) Perfume proper amount ( 12) Preservatives (2) to (12) were added to an appropriate amount (production method) (1), dissolved at 85 ° C or higher, then left to cool to 30 ° C or lower, solidified, and sufficiently ground with a homogenizer. Microgelation (average particle size 80 μm) was performed to obtain a jelly-like pack.

The external preparations for skin obtained in Examples 24 to 28 were all excellent in thickening property, had no sticky feeling, and had a refreshing feeling of use. It was also excellent in long-term stability.

(Example 29) Two-component hair nail polish (acidic hair dye) (composition component) (% by weight) [1 formulation] ethanol 16 purified water to 40 benzyl alcohol 8 glycolic acid 1.6 sodium lactate (50 %) 0.6 Dye 0.06 [2 agents] Ethanol 4 Purified water to 60 Agar (“Ina agar AX100”) 2 Methylparaben Appropriate amount (manufacturing method) 1 agent: Obtained by mixing ethanol and benzyl alcohol with purified water. Glycolic acid and sodium lactate were dissolved in the mixture, and a dye was added and dissolved therein to obtain one agent.

Agent 2: Dissolve agar in purified water (75 ° C.), mix methylparaben and ethanol, and mix at room temperature for 12 hours.
It was left to stand for a time to be solidified (gelled). This gel was pulverized with a disper to give a microgel (average particle size 70 μm) to obtain 2 parts (agar microgel).

The acidic hair dye obtained by mixing the first agent and the second agent (agar microgel) is excellent in thickening property and has no stickiness.
It had a refreshing feel. It was also excellent in long-term stability and adhesiveness.

(Example 30) One-agent hair nail polish (acidic hair dye) (composition component) (% by weight) (1) Purified water balance (2) 1,3-butylene glycol 20 (3) Benzyl alcohol 8 (4) Glycolic acid 0.2 (5) Dye Appropriate amount (6) Hydroxyethyl cellulose 0.5 (7) Agar (“Ina agar AX100”) 2 (8) Amino-modified silicone 0.5 (9) Dimethylpolysiloxane (20 cs) 0.1 (10) Stearyl trimethyl ammonium chloride 0.1 (Production method) (7) was dissolved in a part (75 ° C.) of (1) to give 6
Let stand until it reaches 0 ° C., then (2)-(4),
(6) was added and dissolved, and allowed to stand at room temperature for 12 hours for gelation (solidification). This gel was pulverized with a disper to form a microgel (average particle size 50 μm). This microgel was mixed with (5) dissolved in another part of (1), and finally with (10) dissolved in the rest of (8), (9), and (1). Thus, an acidic hair dye was obtained.

The acidic hair dye thus obtained was excellent in thickening property, had no sticky feeling, and had a refreshing feeling of use. It was also excellent in long-term stability and adhesiveness.

[0077]

EFFECTS OF THE INVENTION The thickener obtained by the present invention has no spinnability characteristic of polymer solutions conventionally used as a thickener, and realizes a very refreshing feeling. We were able to. In addition, the polymer solution was affected by the drug components to be blended, salts, etc. to cause a decrease in viscosity, and the blending was sometimes limited, but with the thickener of the present invention, there is no such problem, and the formulation width of cosmetics is wide. Can be extended.

─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. ⁷ Identification code FI A61K 7/032 A61K 7/032 7/11 7/11 7/13 7/13 7/48 7/48 // C08J 3/075 C08J 3/075 3/12 3/12 C08L 5/00 C08L 5/00 89/00 89/00 101/00 101/00 (72) Inventor Toshio Yanaki 1050 Shinba-cho, Kohoku-ku, Yokohama-shi, Kanagawa Shiseido Co., Ltd. In the Daiichi Research Center (56) Reference JP-A-10-279693 (JP, A) JP-A-2000-26229 (JP, A) JP-A-5-255538 (JP, A) (58) Fields investigated (Int .Cl. ⁷ , DB name) C09K 3/00 103 A61K ^7/ 00-7/50

Claims (10)

(57) [Claims] 1. A hydrophilic compound having a gelling ability is dissolved in water or an aqueous component and then left to cool to form a gel, which is then crushed to have an average particle size of 0.1 to 100.
A method for producing a thickener, which comprises obtaining a thickener by forming a 0 μm microgel. 2. The average particle size of the microgel is 1 to 300 μm.
The method for producing a thickener according to claim 1, wherein 3. The thickening agent according to claim 1, wherein the hydrophilic compound having a gelling ability is one or more selected from agar, carrageenan, curdlan, gelatin, gellan gum, and alginic acid. Method of manufacturing agent. 4. A hydrophilic compound having a gelling ability and a thickening compound having no gelling ability are dissolved in water or an aqueous component and then left to cool to form a gel.
4. The method for producing a thickener according to any one of 3 above. 5. The thickening compound having no gelling ability is one or two selected from xanthan gum, succinoglycan, polyacrylic acid, polyethylene glycol, polyacrylamide, and polyalkylacrylamide / polyacrylamide copolymer. The above is the method for producing a thickener according to claim 4. 6. A thickener obtained by the manufacturing method according to claim 1. 7. A viscosity of 2,000 to 1,000,000 m
Pa · s (B type viscometer, 0.6 rpm, 25 ° C), The thickener according to claim 6. 8. A cosmetic containing the thickener according to claim 6 or 7. 9. A drug component or salt selected from 1
The cosmetic according to claim 8, further comprising one or more species. 10. The cosmetic according to claim 9, which comprises 0.01 to 20% by weight in the total amount of the cosmetic, of one or more selected from drug components and salts.