JP5399665B2 - Method for producing gel composition - Google Patents

Description

  The present invention relates to a method for producing a gel composition having a lamellar structure, which is particularly suitably used for cosmetics and the like.

  In cosmetics represented by cream, an emulsion type is common. In recent years, it has been found that lyotropic liquid crystals formed of amphiphilic molecules and water contribute to the production of emulsion cosmetics. Based on such knowledge, in order to obtain fine emulsified particles, the oil phase was directly added and dispersed in the liquid crystal to obtain a gel-like O / LC (oil in liquid crystal) emulsion, and then the remaining aqueous phase Is added to make an O / W emulsion.

  For example, Patent Document 1 discloses that (A) a hydrogenated phospholipid having a phosphatidylcholine content of 50% by mass or more and a water-soluble polyhydric alcohol are heated and mixed at 60 to 85 ° C. with water in a gel mixture. To form a lamellar liquid crystal, and then (B) polyethylene glycol monostearate and an oil phase are added, and an aqueous phase heated to 60 to 85 ° C. is added, mixed and stirred, and then cooled to room temperature. An oil-in-water milk cosmetic product is described.

  Furthermore, cosmetics comprising a lamellar liquid crystal type dosage form have been proposed by taking advantage of the lamellar forming ability formed by an analog of ceramide present in the skin. For example, Patent Document 2 describes that a liquid crystal composition having a lamellar structure containing a polyhydric alcohol and a sterol compound such as ceramide and glucosylceramide is used as a skin cosmetic. This liquid crystal composition is produced by mixing the above-mentioned components and heating them at 70 to 90 ° C. for 5 to 10 minutes, followed by cooling and stirring until a gel-like mixture is obtained.

  In the cosmetic production process described above, usually, an operation of mixing raw material components under heating to form a liquid crystal structure and then cooling with stirring is performed. However, depending on the cooling and stirring conditions, the lamellar structure formed under heating during the cooling step may be destroyed. When the lamella structure is destroyed, there may be a disadvantage that the feeling of use and storage stability of the cosmetic are lowered.

JP 2007-314442 A JP 2000-264826 A

  An object of the present invention is to provide a method for producing a gel having a lamellar structure that can eliminate the disadvantages of the above-described conventional techniques.

The present invention is a method for producing a gel having a lamellar structure, comprising a step of cooling a liquid crystal or gel fluid formed at high temperature,
In a tubular casing, using a vibration type stirring and mixing device provided with a stirrer composed of a drive shaft and a stirring blade attached to the drive shaft, the drive shaft being configured to vibrate in the axial direction, The present invention provides a method for producing a gel having a lamellar structure, comprising a step of continuously cooling the fluid by passing through a vibration type stirring and mixing device.

  According to the present invention, the cooling process can be performed without destroying the lamella structure in the cooling step. As a result, it is possible to provide a gel having a lamellar structure with a good feeling of use and excellent storage stability.

  The present invention will be described below based on preferred embodiments with reference to the drawings. FIG. 1 shows a schematic view of an apparatus suitably used in the method of the present invention. The apparatus 10 shown in FIG. 1 is roughly divided into a heating and mixing unit 20 and a cooling unit 30. The heating and mixing unit 20 is filled with all or a part of the blended raw material of the gel having the target lamellar structure, and is used for mixing the filled raw material under heating. The cooling unit 30 is used to cool the heat-mixed fluid and obtain a gel having a target lamellar structure.

  The heating and mixing unit 20 includes a mixing tank 21. The mixing tank 21 is heated or cooled by the jacket 22 and adjusted to a predetermined temperature. A stirring blade 23 is installed in the mixing tank 21. The stirring blade 23 is connected to a motor 25 installed outside the mixing tank 21 via a shaft 24 and is rotatable. A pipe 26 for taking out a fluid mixed in the tank 21 is connected to the bottom of the mixing tank 21. The pipe 26 is connected through a valve 27 to a metering pump 28 comprising a MONO pump (registered trademark, Hyojin Equipment Co., Ltd.) and the like. The metering pump 28 is used for metering the fluid into the cooling unit 30 through the pipe 29.

  The cooling unit 30 includes a vibration type stirring and mixing device 40. The vibration type stirring and mixing device 40 has a substantially cylindrical structure, and has an inlet 31 connected to the pipe 29 on one end side and a discharge port 32 on the other end side. The discharge port 32 is connected to a discharge pipe 33. The fluid supplied from the heating and mixing unit 20 is supplied into the vibrating stirring and mixing device 40 through the inlet 31, passes through the device 40, and is discharged from the end of the discharge pipe 33 through the discharge port 32. . The fluid is further mixed and continuously cooled while passing through the vibrating stirring and mixing device 40. In order to perform continuous cooling, the vibration type stirring and mixing device 40 has four jackets 34, 35, 36, and 37 on the outside of the substantially cylindrical structure from the inlet 31 side toward the outlet 32 side. They are installed in this order. Cooling water circulates in each jacket. The temperature of the cooling water can be appropriately set, and these jackets can cool the fluid continuously or stepwise from the inlet 31 side toward the outlet 32 side.

  FIG. 2 shows a schematic diagram of a longitudinal section of the vibration type stirring and mixing apparatus 40. The apparatus 40 includes a stirring body 44 including a drive shaft 42 and a stirring blade 43 attached to the drive shaft 42 in a tubular casing 41. The drive shaft 42 is configured to vibrate up and down along the axial direction by a vibrator 45a.

  The casing 41 has a tubular shape with a circular cross section, and an inflow port 31 is provided in the vicinity of the lower portion thereof. A discharge port 32 is provided near the upper portion of the casing 41. The fluid flowing in from the inflow port 31 passes through the casing 41 and is discharged from the discharge port 32.

  In the casing 41, the above-described stirring body 44 is disposed. The drive shaft 42 of the stirring body 44 extends in the longitudinal direction (vertical direction) of the casing 41. The upper end of the drive shaft 42 is connected to the vibrator 45a through a joint 45b. The vibrator 45a includes a motor (not shown) and a known cam mechanism (not shown) connected to its output shaft. The cam mechanism includes a rotating part (not shown) and a swinging part (not shown). The rotating part is attached eccentrically with respect to the output shaft of the motor. The oscillating part is oscillated by the eccentric rotation of the rotating part. Then, the swing of the swing portion is transmitted to the drive shaft 42 as vertical vibration.

  A plurality of annular partition portions 46 are provided on the inner wall of the casing 41. All of the partition portions 46 have the same shape, and protrude in the horizontal direction from the inner wall of the casing 41. The drive shaft 42 is inserted into a circular hole formed in the center of the partition 46. The diameter of this circular hole is larger than the diameter of the drive shaft 42. A plurality of mixing chambers 47 are defined in the casing 41 by two adjacent partitions. The mixing chamber 47 is arranged in series along the longitudinal direction (vertical direction) of the casing 41.

  3A and 3B are enlarged views of the main part of the stirring body 44. FIG. The stirrer 44 includes a drive shaft 42 and a stirring blade 43 spirally attached to the peripheral surface thereof. In the figure, the stirring blades 43 are attached in a spiral shape with three rounds. The stirring bodies 44 in this state are provided as a set, and the stirring bodies 44 are arranged in the mixing chambers 47 in the casing. Therefore, the number of sets of stirring bodies 44 is the same as the number of mixing chambers 47. In each set of stirring bodies 44, the spiral directions of the stirring blades 43 are the same.

  One or more apertures 48 and / or one or more notches 49 are provided in the stirring blades 43 in each set of stirring bodies 44. The opening 48 and the notch 49 are provided so that the formation positions do not coincide between the upper and lower stirring blades when the stirring body 44 is viewed from the axial direction of the drive shaft 42 (see FIG. 3A). ing. The reason for this is to prevent the occurrence of a short circuit flow in the axial direction and enhance the stirring and mixing effect.

  As the vibration type stirring and mixing apparatus 40 having the above-described configuration, for example, the one described in JP-A-4-235729 can be used. A commercially available product can also be used as the vibration type stirring and mixing device 40. Examples of such commercially available products include Vibro Mixer (registered trademark) manufactured by Chilling Industries Co., Ltd.

  The gel production method using the apparatus 10 having the above configuration will be described. First, the mixing tank 21 is filled with all or a part of the blended raw material of the gel having the target lamellar structure. When a part of the blended raw material of the gel having a lamella structure is filled, the remainder of the blended raw material can be supplied from the middle of the vibration type stirring and mixing device 40 as described later.

  The blending raw material filled in the mixing tank 21 contains at least a composition that forms a lamellar gel material. The composition forming a gel-like substance having a lamellar structure includes a composition forming an α gel. Hereinafter, these compositions are collectively referred to as a lamella gel-forming composition. Depending on the type of the lamella gel-forming composition, a neutralizing agent for the lamella gel-forming composition (for example, a neutralizing agent for fatty acids) or the like is also added as a kind of blending raw material.

  The α-gel is generally formed when a compound having a hydrophilic group and a lipophilic group such as a surfactant is used as a lamellar gel-forming composition, and a hexagonal α-type structure ( It is a gel in a state where a large amount of water is held between layers of hexagonal.

  Lamella gel-forming compositions generally include components that are solid at 25 ° C. When the filling of the blended raw material is completed, the mixing tank 21 is heated to a high temperature to bring the lamellar gel-forming composition contained in the blended raw material into a molten state. The heating temperature can be appropriately set according to the melting point of the component contained in the lamellar gel-forming composition and the liquid crystal-gel phase transition temperature. Generally, it may be set to a temperature higher than the melting point of the component having the highest melting point in the lamellar gel-forming composition, whether it is below the liquid crystal-gel phase transition temperature or above. good. The melting point and liquid crystal-gel phase transition temperature of the components contained in the lamella gel-forming composition can be determined by differential scanning calorimetry (DSC method). The lamellar gel-forming composition is melted by heating, and the inside of the mixing tank 21 is stirred by rotating the stirring blade 23 in this state, so that the components of the lamellar gel-forming composition are sufficiently uniformly mixed. The fluid in this state expresses a lamellar liquid crystal or lamellar gel structure.

  A lamellar liquid crystal fluid or a lamellar gel fluid previously formed by high-temperature heating may be introduced into the mixing tank 21 with stirring by the stirring blade 23.

When the lamella liquid crystal or lamella gel fluid is sufficiently formed, the valve 27 attached to the bottom of the mixing tank 21 is opened, and the fluid in the tank 21 is taken out. The fluid is introduced into the metering pump 28, and a certain amount thereof is supplied to the vibration type stirring and mixing device 40. The metering pump 28 also serves as an extrusion pressure source for the fluid to pass through the vibration type stirring and mixing device 40. The viscosity of the fluid introduced into the vibration type stirring device 40 is preferably ¹ to 10000 mPa · s, particularly 10 to 1000 mPa · s when the shear rate = 100 s ^{−1 at} the introduced temperature.

  Although not shown in FIG. 1, instead of directly supplying the fluid obtained in the mixing tank 21 to the vibration type stirring and mixing device 40, it passes through a continuous dispersing device such as an in-line homomixer or a milder. Then, it may be supplied to the vibration type stirring and mixing apparatus 40.

  As described above, four jackets 34, 35, 36, and 37 are attached to the vibration type stirring and mixing device 40 on the outside of the substantially cylindrical structure. In each jacket, cooling water of a predetermined temperature circulates, and heat exchange for cooling the fluid is performed. For example, hot water circulates in the jacket 34 and is maintained at about 80 ° C., and the jacket 35 is maintained at about 50 to 40 ° C. The remaining two jackets 36 and 37 are both kept at 10 to 0 ° C. That is, the vibration type agitation and mixing device 40 is provided with a temperature gradient that decreases from the inlet 31 side toward the outlet 32 side.

  In the vibration type stirring and mixing apparatus 40, the stirring body 44 vibrates up and down along the axial direction thereof, so that the fluid passing through the casing 41 is provided in the flow along the stirring body 44 and the stirring blade 43. Mixing is achieved by turbulence in the flow through the apertures 48 and notches 49. Since the fluid existing in the position corresponding to the jacket 34 is in a state of high fluidity because the jacket 34 is maintained at about 80 ° C., mixing is promoted by the vibration of the stirring body 44, Following the mixing in the mixing tank 21 described above, redispersion is performed.

  The fluid is then pushed out to a position corresponding to the jacket 35. Since the temperature at this position is lower than the temperature at the position corresponding to the jacket 34, the fluid is cooled and its fluidity is lowered. When the temperature of the fluid is equal to or lower than the liquid crystal-gel phase transition temperature of the fluid during cooling, a phase transition from lamellar liquid crystal to lamella gel occurs and the fluidity is further lowered. Even if the fluidity of the fluid significantly decreases, the fluid is cooled while being mixed by the flow along the stirring body 44 and the disturbance of the flow through the opening 48 and the notch 49 provided in the stirring blade 43. Therefore, uneven cooling is less likely to occur. Moreover, heat conductivity becomes favorable by mixing, for example, a cooling rate becomes quicker than the cooling by the batch type stirring apparatus conventionally used. Furthermore, since there is almost no dead space in the vibration type stirring and mixing device 40, uneven stirring is less likely to occur. Moreover, unlike the conventional method using a batch type stirring device, the vibration type stirring and mixing device 40 can perform good stirring and mixing regardless of whether the fluidity of the fluid is high or low. In addition, mixing and cooling using the vibration type stirring and mixing device 40 are performed under a low shear stress. These advantages of the vibratory stirring and mixing device 40 have a favorable effect of maintaining the lamellar structure contained in the fluid. In addition, the vibration type agitation and mixing device 40 is advantageous in that the temperature control is easy because the calorific value is small.

  The fluid cooled at the position corresponding to the jacket 35 is then sequentially pushed out to the position corresponding to the jackets 36 and 37 and further cooled at the position. In this way, the fluid is continuously cooled, and the gel in which the lamellar structure is maintained is discharged from the discharge pipe 33 through the discharge port 32 of the vibration type stirring and mixing apparatus 40. The temperature of the gel in this state is 25-30 ° C.

  If the target gel contains a heat-sensitive component or a component that adversely affects the gel by heat, the mixing tank 21 is not filled with the component, and the vibration type By supplying the stirring and mixing apparatus 40 into the apparatus 40 from a position in the middle, it is possible to avoid inconvenience due to heat. For example, since the fluid is cooled to a certain degree at the position corresponding to the jacket 35, inconvenience due to heat can be avoided by supplying the component to the position using a metering pump. Since the stirring and mixing of the fluid by the vibration type stirring and mixing device 40 is almost a piston flow, even if the above components are supplied from the middle of the device 40, the mixing of the components and the fluid can be performed successfully. Examples of the above-mentioned components include components that easily change in temperature, such as certain active agents, volatile components, latexes, fragrances, plant extracts, and wax fine dispersions. In order to supply such components, one or a plurality of auxiliary injection ports can be provided in the middle of the vibration type stirring and mixing apparatus 40.

  In cooling using the vibration type stirring and mixing device 40, it is preferable to set the average cooling rate to 0.1 to 5 ° C./s. The average cooling rate is a value obtained by dividing the difference between the temperature when the fluid enters the vibrating stirring and mixing device 40 and the temperature when it exits by the residence time. Moreover, the frequency of the vibration type stirring and mixing apparatus 40 is preferably in the range of 5 to 30 strokes / s, and the amplitude is preferably about 4 to 15 mm. Furthermore, the total amount of vibration given while being cooled by the vibration type stirring and mixing apparatus 40 is preferably 50 to 100,000 strokes, particularly 200 to 20,000 strokes.

  In this way, the fluid is cooled to room temperature (25 ° C.) to obtain a lamella gel (including α-gel) in which the lamella structure is maintained. In addition, when the raw material for forming a phase other than the lamellar gel phase is included in the blended raw material, a dispersion of the lamellar gel in which the lamellar gel phase is dispersed in the phase other than the lamellar gel phase, a dispersion in which the dispersed phase is dispersed in the lamellar gel phase, or An emulsion having a lamellar gel phase at the interface between the oil phase and the aqueous phase is obtained. The lamella gel-forming composition is in a lamellar liquid crystal or lamella gel state depending on the type of lamellar gel-forming composition, the heating and mixing temperature, and the temperature during cooling. In the cooling step according to this production method, the lamellar liquid crystal phase changes to become a lamellar gel phase, or the lamellar gel phase is cooled as it is. The phase transition temperature of the lamellar liquid crystal-lamellar gel is preferably 35 to 80 ° C., particularly 40 to 70 ° C. from the viewpoint of storage stability of the product. Gels with a lamellar structure maintained (including α-gel), dispersions of lamellar gels, dispersions in which a dispersed phase is dispersed in a lamellar gel phase, or emulsions in which a lamellar gel phase is present at the interface between an oil phase and an aqueous phase Using this as it is or adding a desired component, a cosmetic is obtained. The cosmetic thus obtained has a good feeling of use due to the lamellar structure and has excellent storage stability.

  Next, the raw material of the lamella gel manufactured by this invention is demonstrated. As described above, the blending raw material filled in the mixing tank 21 includes at least a lamella gel-forming composition. Typical components of the lamella gel-forming composition are fatty acids or salts thereof and aliphatic alcohols. As the fatty acid, those having an average carbon number of 12 to 36, particularly 16 to 22 are preferably used. Particularly preferred are palmitic acid, stearic acid, behenic acid and the like. The counter ion when the fatty acid forms a salt is not particularly limited, and alkali metal salts such as sodium and potassium, monoethanolamine, diethanolamine, triethanolamine, aminomethylpropanol, aminomethylpropanediol, trishydroxymethylamino Examples include organic amines such as methane and morpholine, and other basic amino acids such as L-arginine. Fatty acids or salts thereof can be used alone or in combination of two or more.

  As the aliphatic alcohol, those having an average carbon number of 12 to 36, particularly 18 to 24 are preferably used. Particularly preferred are cetyl alcohol, stearyl alcohol, aralkyl alcohol, behenyl alcohol, 2-octyl lauryl alcohol, 2-hexyldecyl alcohol, and isostearyl alcohol. These aliphatic alcohols can be used singly or in combination of two or more.

  Components other than the lamellar gel-forming composition can also be added to the blending raw material. For example, when the lamella gel-forming composition contains a fatty acid or a salt thereof, a neutralizing agent can be added. Examples of the neutralizing agent include monoethanolamine, diethanolamine, triethanolamine, aminomethylpropanol, aminomethylpropanediol, trishydroxymethylaminomethane, organic amines such as morpholine, and other basic amino acids such as L-arginine. be able to. The neutralizing agent is preferably added in an amount of 0.1 to 1 mol, particularly 0.2 to 0.6 mol, with respect to the fatty acid or a salt thereof, from the viewpoint of successfully forming a liquid crystal.

When the lamella gel-forming composition contains an aliphatic alcohol, a tertiary amine or a salt thereof, or a quaternary ammonium salt can be added. As the tertiary amine or a salt thereof, for example, a compound represented by R ¹ —O— (CH ₂ ) ₃ NR ² R ³ or a salt thereof can be used. In the formula, R ¹ represents a linear or branched alkyl group or alkenyl group having 12 to 24 carbon atoms, particularly 14 to 22 carbon atoms, and an alkyl group is particularly preferable. R ² and R ³ represent an alkyl group having 1 to 6 carbon atoms and — (CH ₂ CH ₂ O) nH (n is 1 to 3, particularly preferably 1), and at least one of R ² and R ³ is In particular, it is preferable that both of them are an alkyl group having 1 to 6 carbon atoms, particularly a methyl group or an ethyl group. Preferable specific examples of the tertiary amine include N, N-dimethyl-3-hexadecyloxypropylamine and N, N-dimethyl-3-octadecyloxypropylamine. The salt of the tertiary amine may be any salt of inorganic acid and organic acid. Examples of the inorganic acid include phosphoric acid, hydrochloric acid, sulfuric acid and the like. Examples of organic acids include monocarboxylic acids such as acetic acid and propionic acid; dicarboxylic acids such as malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid, fumaric acid, and phthalic acid; glycolic acid, lactic acid, hydroxyacrylic acid, and glycerin. Examples thereof include hydroxycarboxylic acids such as acid, malic acid, tartaric acid and citric acid; polycarboxylic acids such as polyglutamic acid; acidic amino acids such as glutamic acid and aspartic acid. Of these, inorganic acids (particularly hydrochloric acid), dicarboxylic acids (particularly maleic acid, succinic acid), hydroxycarboxylic acids (particularly glycolic acid, citric acid, lactic acid, malic acid) and acidic amino acids (particularly glutamic acid) are preferred. A tertiary amine or a salt thereof can be used alone or in combination of two or more. The compounding amount of the aliphatic alcohol is preferably 0.5 to 20 times mol, particularly 2 to 7 times mol for the tertiary amine or a salt thereof. Moreover, when using the salt of a tertiary amine, the compounding quantity of the said inorganic acid or organic acid has preferable 0.1-4 times mole with respect to a tertiary amine.

As the quaternary ammonium salt, for example, a compound represented by R ¹ (CH ₃ ) ₃ N ⁺ X ⁻ can be used. In the formula, R ¹ represents a linear or branched alkyl or alkenyl group having preferably 12 to 28 carbon atoms, more preferably 16 to 24 carbon atoms. Examples of X ⁻ include halogen ions such as chlorine ion and bromine ion, and organic anions such as methosulfate, ethosulfate, methophosphate, ethophosphate, methocarbonate, halogen ion is preferable, and chlorine ion is particularly preferable. preferable. Preferred specific examples of the quaternary ammonium salt are cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, aralkyltrimethylammonium chloride, behenyltrimethylammonium chloride and the like. Quaternary ammonium salts can be used singly or in combination of two or more. The blending amount of the aliphatic alcohol is preferably 0.5 to 20 times mol, particularly 2 to 7 times mol for the quaternary ammonium salt.

  You may add surfactant to a compounding raw material. As the surfactant, nonionic surfactants, anionic surfactants, cationic surfactants, amphoteric surfactants and the like that are generally used in cosmetics can be used alone or in combination.

  In addition to the above-described components, other components can be blended in the blending raw material. For example, when producing mascara as a cosmetic, in addition to the above-described fatty acid or a salt thereof and a neutralizing agent, the components described in JP-A-2004-10495 and JP-A-2006-169194 may be added. it can. Moreover, when manufacturing hair cosmetics, such as hair rinse, as cosmetics, in addition to the above-mentioned aliphatic alcohol, tertiary amine, its salt, or quaternary ammonium salt, JP2002-29937A or JP2004. The components described in JP-A-67534 can be added.

  Examples of the cosmetics to be subjected to the production method of the present invention include hair conditioners, hair waxes, cosmetic creams, gel cosmetics, etc. in addition to the mascara and hair rinse.

  As mentioned above, although this invention was demonstrated based on the preferable embodiment, this invention is not restrict | limited to the said embodiment. For example, in the above-described embodiment, one vibration type agitation and mixing device 40 is used, but instead of this, as shown in FIG. 4, two or more vibration type agitation and mixing devices 40 and 40 ′ are connected in series. Can be used. In this case, by supplying a heat-sensitive component or the like from the middle of the second vibration-type stirring and mixing device 40 ′ located on the downstream side, the stirring condition and the mixing condition of the component are separately selected appropriately. can do.

  Hereinafter, the present invention will be described in more detail with reference to examples. However, the scope of the present invention is not limited to such examples. Unless otherwise specified, “%” means “mass%”.

[Example 1]
An α gel having the composition shown in Table 1 below was prepared using the apparatus shown in FIGS. First, components 1 to 6 were dissolved by heating at 80 ° C. to obtain an aqueous phase. Separately, components 8 to 9 were dissolved at 80 ° C. to obtain an oil phase. The oil phase was added to the aqueous phase at the same temperature (80 ° C.), and component 7 was added while dispersing with a homomixer to obtain a lamellar liquid crystal fluid. This lamellar liquid crystal fluid is supplied at the same temperature (80 ° C.) to a vibrating stirring and mixing device (Vibro mixer manufactured by Chilling Industries Co., Ltd.) with a metering pump, and continuously stirred at 30 ° C. or lower while stirring in the device. To obtain a gel having a lamellar structure. In the vibration type stirring and mixing apparatus, the temperature of the jacket 34 was set to 80 ° C., the temperature of the jacket 35 was set to 45 ° C., the temperature of the jacket 36 was set to 0 ° C., and the temperature of the jacket 37 was set to 0 ° C. The average cooling rate was 0.7 ° C./s. Further, the vibration type mixing device had a vibration frequency of 5 strokes / s, an amplitude of about 5 mm, and a total vibration amount of 210 strokes. FIG. 5 shows a differential interference micrograph of the obtained gel having a lamellar structure (which was found to be an α-type structure from the X-ray diffraction pattern). Further, FIG. 6 shows a differential interference microscopic image of the gel composition obtained by subjecting to standing cooling at room temperature (cooling time: 3 hours) without using a vibration type stirring and mixing apparatus as an object. From the comparison between FIG. 5 and FIG. 6, it can be seen that according to the method of the present invention, a gel having a lamellar structure close to a stationary and standing state can be obtained in a short time.

  At the time of preparing the α gel described above, the wax fine dispersion shown in Table 2 below was continuously mixed in the ratio shown in the table from the position corresponding to the jacket 36 to obtain a mascara-based cosmetic. The method for preparing the wax fine dispersion is as follows. Under heating at 85 ° C., each component of the fine wax dispersion shown in the table is emulsified and dispersed with a homomixer at a rotational speed of 5000 rpm, and then quantified into a vibration type stirring and mixing device (Vibro mixer manufactured by Chilling Industries Co., Ltd.). Supplied with a pump. While stirring in the apparatus, the mixture was continuously cooled to 30 ° C. or lower to obtain a fine wax dispersion. In the vibration type stirring and mixing apparatus, the temperature of the jacket 34 was set to 85 ° C., the temperature of the jacket 35 was set to 45 ° C., the temperature of the jacket 36 was set to 0 ° C., and the temperature of the jacket 37 was set to 0 ° C. The average cooling rate was 0.7 ° C./s. In addition, the vibration type mixing apparatus had a vibration frequency of 30 strokes / s, an amplitude of about 5 mm, and a total vibration amount of 1260 strokes. In the obtained mascara-based cosmetic, wax fine particles were dispersed in the lamellar gel phase.

[Examples 2 to 4]
The gel is the same as in Example 1 except that the frequency of the vibration type agitation mixer is 10 strokes / s (Example 2), 20 strokes / s (Example 3), and 30 strokes / s (Example 4). And a mascara-based cosmetic were obtained. Observation with a differential interference microscope confirmed that the gels having these lamellar structures were not destroyed.

[Comparative Examples 1 and 2]
In place of the vibratory stirring and mixing apparatus used in Example 1, T.P. K. Cooling was performed using an Adihomomixer (registered trademark). The rotation speeds were 5000 rpm (Comparative Example 1) and 1500 rpm (Comparative Example 2). Except this, it carried out similarly to Example 1, and obtained the gel-like composition and the mascara base cosmetics. The differential interference microscope image of the obtained gel composition is shown in FIGS. From the comparison between FIG. 7 and FIG. 8 and FIG. 5 described above, it can be seen that the lamellar structure is destroyed when the method of the comparative example is used.

[Evaluation]
About the gel-like composition obtained by the Example and the comparative example, the viscosity measurement and storage stability evaluation were performed with the following method. Moreover, about the mascara base cosmetics, the usability | use_condition was evaluated with the following method. The results are shown in Table 3 below.

(Measurement of viscosity of gel composition)
Using a rheometer (manufactured by PHYSICA, MCR300), the viscosity at 25 ° C. and shear rate = 100 s ⁻¹ was measured.

[Evaluation of storage stability of gel composition]
The gel was put in a glass container with a lid and sealed, and the appearance after storage at 40 ° C. for 1 month was evaluated according to the following criteria.
◎: No water separation ○: Some water separation ×: Water separation

[Evaluation of feeling of use of mascara cosmetics]
Ten specialized panelists were allowed to freely apply mascara base to their eyelashes, and the panelists themselves evaluated their feeling of use. The evaluation criteria are as follows.
◎: Satisfied ○: Slightly satisfied △: Normal ×: Dissatisfied

  As is apparent from the results shown in Table 3, it can be seen that according to the method of the present invention, a mascara-based cosmetic having a higher viscosity and higher storage stability can be obtained compared to the method of the comparative example. Moreover, it turns out that the usability | use_condition of cosmetics becomes favorable.

Example 5
A hair conditioner having the composition shown in Table 4 below was prepared using the apparatus shown in FIGS. The ingredients 11 and 2 were dissolved by heating at 70 ° C. to obtain an aqueous phase. Components 1 and 3 to 10 were dissolved at 70 ° C. to obtain an oil phase. The oil phase was added to the aqueous phase and dispersed with a homomixer to obtain a lamellar gel fluid. This lamellar gel fluid is supplied to a vibrating stirring and mixing device (Vibro mixer manufactured by Chilling Industry Co., Ltd.) with a metering pump, and continuously cooled to 30 ° C. or lower while stirring in the device to obtain a hair conditioner. It was. In the vibration type stirring and mixing apparatus, the temperature of the jacket 34 was set to 80 ° C., the temperature of the jacket 35 was set to 45 ° C., the temperature of the jacket 36 was set to 0 ° C., and the temperature of the jacket 37 was set to 0 ° C. The average cooling rate was 0.7 ° C./s. Further, the vibration type mixing device had a vibration frequency of 5 strokes / s, an amplitude of about 5 mm, and a total vibration amount of 210 strokes.

[Examples 6 to 7]
A hair conditioner was obtained in the same manner as in Example 5 except that the frequency of the vibration type stirring and mixing apparatus was 10 stroke / s (Example 6) and 20 stroke / s (Example 7).

[Comparative Example 3]
In place of the vibration-type stirring and mixing apparatus used in Example 5, T.P. K. Cooling was performed using an Adihomomixer (registered trademark). The rotation speed was 5000 rpm. Except this, it carried out similarly to Example 5, and obtained the hair conditioner.

〔sensory evaluation〕
About the hair conditioner obtained by the Example and the comparative example, 5 expert panelists were made to perform sensory evaluation with respect to each evaluation item shown in the following Table 5. The evaluation criteria are as follows. The results are shown in the same table below.
◎: Satisfied ○: Slightly satisfied △: Normal ×: Dissatisfied

[Evaluation of storage stability of hair conditioner]
The hair conditioner was stored in a glass container with a lid, and the appearance after storage at 50 ° C. for 1 month was evaluated according to the following criteria. The results obtained are shown in Table 5.
◎: No water separation ○: Some water separation ×: Water separation

It is the schematic which shows the suitable apparatus which enforces the manufacturing method of this invention. It is a schematic diagram of the longitudinal cross-section of the vibration type stirring and mixing apparatus shown in FIG. It is a principal part enlarged view of the stirring body in the vibration type stirring mixing apparatus shown in FIG. It is the schematic which shows another suitable apparatus which enforces the manufacturing method of this invention. 2 is a differential interference microscope image of the gel composition obtained in Example 1. FIG. It is a differential interference microscope image of the gel-like composition obtained by standing still cooling. 2 is a differential interference microscopic image of the gel composition obtained in Comparative Example 1. FIG. 3 is a differential interference microscope image of the gel composition obtained in Comparative Example 2. FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Apparatus 20 Heating mixing part 30 Cooling part 40 Vibrating stirring mixing apparatus 41 Casing 42 Drive shaft 43 Stirring blade 44 Stirring body

Claims (14)

A method for producing a gel having a lamellar structure, comprising a step of cooling a fluid containing liquid crystal or gel formed at a temperature of 70 ° C. or higher ,
In the tubular casing, an agitating body comprising a drive shaft and a stirring blade spirally attached to the peripheral surface of the drive shaft is provided, and the drive shaft is vibrated in an axial direction. Using a mixing device, and continuously cooling the fluid by passing through the vibrating stirring and mixing device ,
A method for producing a gel having a lamellar structure, wherein a stirring blade is provided with one or more apertures and / or one or more notches . A method for producing a gel having a lamellar structure, comprising a step of cooling a fluid containing a liquid crystal or gel formed at a temperature equal to or higher than the melting point of the component having the highest melting point in the lamella gel-forming composition,
In the tubular casing, an agitating body comprising a drive shaft and a stirring blade spirally attached to the peripheral surface of the drive shaft is provided, and the drive shaft is vibrated in an axial direction. Using a mixing device, and continuously cooling the fluid by passing through the vibrating stirring and mixing device,
A method for producing a gel having a lamellar structure, wherein a stirring blade is provided with one or more apertures and / or one or more notches. The method for producing a gel having a lamellar structure according to claim 1 or 2, wherein the fluid contains a fatty acid and / or a salt thereof, or an anionic or cationic surfactant. The method for producing a gel having a lamellar structure according to claim 3 , wherein the fatty acid has an average carbon number of 12 to 36. Method for producing a gel having a lamellar structure of claims 1 to 3, wherein the fluid contains an aliphatic alcohol. The method for producing a gel having a lamellar structure according to claim 5 , wherein the aliphatic alcohol has an average carbon number of 12 to 36. The method for producing a gel having a lamellar structure according to any one of claims 1 to 6 , wherein a phase transition temperature of the liquid crystal-gel is 35 to 80 ° C. The lamellar according to any one of claims 1 to 7 , wherein the vibration type agitation and mixing device includes a cooling jacket in which cooling water circulates outside the casing, and cools the fluid by passing through the casing. A method for producing a gel having a structure. The method for producing a gel having a lamellar structure according to any one of claims 1 to 8 , wherein an average cooling rate in the cooling step using the vibration type stirring and mixing device is 0.1 to 5 ° C / s. The method for producing a gel having a lamellar structure according to any one of claims 1 to 9 , wherein a vibration frequency of the vibration type stirring and mixing device in the cooling step using the vibration type stirring and mixing device is 5 to 30 strokes / s. A step of supplying at least one component selected from the group consisting of latex, fragrance, plant extract, and wax fine dispersion from an injection port provided at one or a plurality of locations in the vibrating stirring and mixing device; The manufacturing method of the gel which has a lamellar structure in any one of Claim 1 thru | or 10. The method for producing a gel having a lamellar structure according to claim 11, wherein a wax fine dispersion is contained as the component. A gel having a lamellar structure obtained by the production method according to claim 12 . A cosmetic comprising a gel having a lamellar structure obtained by the production method according to claim 12 .