JP6421028B2 - Method for producing fine particle dispersion - Google Patents

Description

  The present invention relates to a method for producing a fine particle dispersion containing an oil component such as wax.

  The present applicant has previously proposed a manufacturing method described in Patent Document 1 as a manufacturing method of an emulsified cosmetic or an oily cosmetic. In the production method described in Patent Document 1, a raw material containing a solid oily component at 25 ° C. is mixed under heating to form a fluid, and the obtained fluid is stirred in a tubular casing with a drive shaft and agitator. In this method, cooling is performed using a vibration type stirring and mixing device provided with a stirring body including blades and configured so that the drive shaft vibrates in the axial direction.

JP 2008-214212 A

  According to the method described in Patent Document 1, it is possible to produce a cosmetic material in which oily component particles are uniformly refined, have a good feeling of use, have a good finish, have a high cosmetic effect, and have good stability. However, in recent years, there has been a need to further refine the oily component particles to improve the feeling of use and to further enhance the cosmetic effect.

  Therefore, the subject of this invention is providing the manufacturing method of the fine particle dispersion which the usability | use_condition improved and the cosmetic effect improved compared with the prior art mentioned above.

  The present invention provides fine particles having an emulsification step of forming an emulsion by mixing a component containing one or more solid oily components at 25 ° C. with water under heating, and a cooling step of cooling the formed emulsion A method for producing a dispersion, wherein the emulsification step uses a high-pressure emulsifier or an ultrasonic emulsifier, and the cooling step includes a drive shaft and a stirring blade attached to the drive shaft in a tubular casing. Using a vibratory stirring and mixing device provided with a stirring body comprising: a drive shaft that vibrates in an axial direction, wherein the stirring blade has one or more apertures and / or one or more notches In the cooling step, the emulsion obtained in the emulsification step is continuously cooled to below the solidification temperature of the oily component by passing through the vibration type stirring and mixing device. Fine particle dispersion to produce fine particle dispersion There is provided a method of manufacturing.

  According to the present invention, the emulsified particles containing solid fat are further refined at 25 ° C., the usability is improved, and the cosmetic effect is further enhanced.

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.

The present invention will be described below based on preferred embodiments with reference to the drawings.
FIG. 1 shows a schematic view of a production apparatus suitably used in the method of the present invention. The manufacturing apparatus 100 shown in FIG. 1 is an emulsifying unit 20 that forms an emulsion by mixing a component containing at least one oily component (hereinafter also referred to as “solid fat”) at 25 ° C. with water under heating. And a cooling unit 30 for cooling the formed emulsion. The emulsifying unit 20 includes a first emulsifying unit 21 and a second emulsifying unit 22. The first emulsifying unit 21 is used to fill all or part of the components constituting the target fine particle dispersion, and to mix the filled components with water under heating to obtain a preliminary emulsion. It is. The 2nd emulsification part 22 is located in the downstream of the 1st emulsification part 21, and is used in order to add a high energy to the preliminary | backup emulsion obtained by the 1st emulsification part 21, and to obtain a fine emulsion. . The cooling unit 30 is located on the downstream side of the emulsifying unit 20 and is used to cool the heat-mixed emulsion to a temperature equal to or lower than the solidification temperature of the oily component that is solid at 25 ° C. to obtain a desired fine particle dispersion. It is what

  The 1st emulsification part 21 of the emulsification part 20 is provided with the mixing tank 211 as shown in FIG. The mixing tank 211 is heated by a jacket 212 that covers the side of the mixing tank 211 and is adjusted to a predetermined temperature. A stirring blade 213 is installed in the mixing tank 211. The stirring blade 213 is connected to a motor 215 installed outside the mixing tank 211 via a shaft 214 and is rotatable. A pipe 216 for taking out the preliminary emulsion mixed in the tank 211 is connected to the bottom of the mixing tank 211. The pipe 216 is connected to the second emulsifying unit 22 through a valve. Note that a metering pump (not shown) may be interposed in the middle of the pipe 216 as needed for the purpose of quantitatively supplying the preliminary emulsion obtained in the first emulsifying unit 21.

  As the 1st emulsification part 21 which has the above structure, TK combi mix (trade name) manufactured by PRIMIX Co., Ltd., TK ADD homomixer (trade name) manufactured by PRIMIX CO., LTD., Etc. can be used. Although these stirring apparatuses are mainly used independently, depending on the case, you may use them suitably combining 2 or more types.

  The 2nd emulsification part 22 of the emulsification part 20 is provided with the high energy process part 221 as shown in FIG. The high energy processing unit 221 can apply high energy to the preliminary emulsion obtained in the first emulsification unit 21 using a high-pressure emulsifier or an ultrasonic emulsifier. A pipe 222 is connected to a downstream portion of the high energy processing unit 221 for taking out the emulsion to which high energy is added in the high energy processing unit 221. The emulsion obtained in the second emulsification unit 22 is supplied to the cooling unit 30 through the pipe 222. Note that a metering pump (not shown) may be interposed in the middle of the pipe 222 as necessary for the purpose of metering the emulsion obtained by the second emulsifying unit 22.

  When a high pressure emulsifier is used as the second emulsifier 22 having the above-described configuration, for example, a starburst mini (part number: HJP-25001) (manufactured by Sugino Machine) or an optimizer (manufactured by Sugino Machine) is a high pressure emulsifier. ), Gorin (manufactured by APV Runny), microfluidizer (manufactured by Microfluidics), high-pressure jet emulsifier (manufactured by Nippon BEE) and the like.

  When an ultrasonic emulsifier is used as the second emulsifier 22, for example, an IKASONIC (part number: U200S) (manufactured by IKA) equipped with an ultrasonic generation horn, an ultrasonic homogenizer (manufactured by Nippon Seiki Seisakusho), A sonic homogenizer (manufactured by Ultrasonic Industrial Co., Ltd.) or the like can be used. These high-pressure emulsifiers or ultrasonic emulsifiers described above are mainly used alone, but in some cases, two or more kinds may be used as appropriate.

  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 a pipe 222 on one end side and an outlet 32 on the other end side. The discharge port 32 is connected to a discharge pipe 33. The emulsion supplied from the emulsifying unit 20 is supplied into the vibration type 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 supplied emulsion is further mixed by passing through the vibration type stirring and mixing device 40 and continuously cooled to a temperature equal to or lower than the solidification temperature of the oily component which is solid at 25 ° C. In order to perform continuous cooling, the vibration-type stirring and mixing device preferably includes a cooling jacket in which cooling water circulates outside the casing 41 described later. Four jackets 34, 35, 36, and 37 are attached in this order from the 31 side toward the discharge port 32 side. Cooling water circulates in each jacket. The temperature of the cooling water can be appropriately set, and these jackets can cool the supplied emulsion 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 connected to a vibrator 45a and is vibrated up and down along the axial direction by the 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 emulsion flowing in from the inflow port 31 is mixed while passing through the casing 41, continuously cooled, and 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. As such a commercial item, the apparatus provided with the cooling jacket in the Vibro mixer (trademark) made from a refrigeration industry, for example is mentioned.

  The production method of the fine particle dispersion using the production apparatus 100 having the above configuration will be described. First, the components constituting the target fine particle dispersion in the mixing tank 211 of the first emulsification unit 21 of the emulsification unit 20 are described. All or a part is filled (water as a dispersion medium is included as a component filled in the mixing tank 211). When a part of the components constituting the fine particle dispersion is filled, other components may be supplied from, for example, the high energy processing unit 221 of the second emulsification unit 22 or the vibration type stirring and mixing device 40. Good. When two or more types of the first emulsifying unit 21 are provided, the upstream first emulsifying unit 21 may be filled with all of the components constituting the target fine particle dispersion, The emulsifying part 21 may be partially filled with components constituting the target fine particle dispersion. By partially filling, the mixing conditions of each component can be adjusted individually and appropriately.

  The component filled in the mixing tank 211 includes at least one oily component that is solid at 25 ° C. When the filling of the target component into the mixing tank 211 is completed, the mixing tank 211 is heated by the jacket 212 to bring the oily component that is solid at 25 ° C. into a molten state. Then, each component is mixed and dispersed by the stirring blade 213 in the mixing tank 211 to obtain a preliminary emulsion. The heating temperature can be appropriately set according to the melting point of the solid fat. Generally, it is preferable to set the temperature higher by about 10 ° C. than the melting point of the solid fat having the highest melting point.

  When the components filled in the mixing tank 211 are stirred and sufficiently mixed, a valve attached to the bottom of the mixing tank 211 is opened, and the preliminary emulsion in the mixing tank 211 is taken out. The preliminary emulsion is supplied to the high energy processing unit 221 of the second emulsification unit 22 through the pipe 216.

式中、Q：体積流量、ΔP：操作圧力、ρ：密度、V：マイクロジェット空間体積、t：時間、d：内径である。

超音波乳化機

式中、ρ：密度、W：出力、A：ホーン面積、V：混合場容積、t：時間である。

ホモミキサー

式中、ρ：密度、Np：動力数、n：回転数、d：翼径、V：混合場体積、t：時間である。

また、高エネルギー処理部２２１の通過回数は、１回以上であることが好ましい。複数回高エネルギー処理部２２１の通過させる際には、各高エネルギー処理部２２１の通過の際に加えられた投下エネルギーすべての総投下エネルギーを意味する。 In the high energy processing unit 221, high energy is applied to the preliminary emulsion obtained in the first emulsifying unit 21 using a high-pressure emulsifier or an ultrasonic emulsifier to obtain an emulsion. The dropping energy applied by the high-pressure emulsifier or the ultrasonic emulsifier is preferably 5 × 10 ⁴ J / kg or more, preferably 2 × 10 ⁵ J / kg or more, from the viewpoint of reducing the particle size. Further preferred. The upper limit value of the dropped energy is not particularly limited, and the larger the dropped energy, the better. Here, “drop energy” is a value that can be calculated by the following equations (1) to (3) in each emulsifier.
High pressure emulsifier

In the formula, Q: volume flow rate, ΔP: operating pressure, ρ: density, V: microjet space volume, t: time, d: inner diameter.

Ultrasonic emulsifier

In the formula, ρ: density, W: output, A: horn area, V: mixing field volume, t: time.

Homo mixer

In the formula, ρ: density, Np: power number, n: rotational speed, d: blade diameter, V: mixing field volume, t: time.

Moreover, it is preferable that the frequency | count of passage of the high energy process part 221 is 1 time or more. When passing through the high energy processing unit 221 a plurality of times, it means the total dropped energy of all of the dropped energy added when each high energy processing unit 221 passes.

  When the target energy is dropped, the valve attached to the high energy processing unit 221 is opened, and the emulsion in the high energy processing unit 221 is taken out. The emulsion is supplied to the vibratory stirring and mixing device 40 via a tube 222. The transition time from the emulsification step (emulsification unit 20) to the cooling step (cooling unit 30) is preferably within 60 seconds from the viewpoint of preventing the emulsion obtained in the emulsification unit 20 from aggregating. More preferably, it is within 10 seconds. The lower limit value of the transition time is not particularly limited, and the shorter the time, the better. The transition time from the emulsifying unit 20 to the cooling unit 30 is the emulsion obtained in the second emulsifying unit 22 from the second emulsifying unit 22 of the emulsifying unit 20 to the vibrating stirring and mixing device 40 of the cooling unit 30 through the pipe 222. Is the time to reach. The transition time can be adjusted by the length of the tube 222, for example.

  As described above, four jackets 34, 35, 36, and 37 are attached to the vibration type stirring and mixing device 40 as cooling jackets. The cooling jacket is disposed outside the casing 41 so as to cover the cylindrical casing 41 shown in FIG. 2, and cooling water of a predetermined temperature is circulated through each jacket, and the emulsification obtained in the emulsification unit 20 By passing the object through the casing 41, heat exchange for cooling the fluid is performed.

  The upper limit of the total flow rate of the cooling water circulating through the cooling jacket is not particularly limited and is preferably as high as possible from the viewpoint of efficiently cooling the emulsion obtained in the emulsifying unit 20 without agglomerating. Specifically, the total flow rate of the cooling water is preferably 10 times or more, more preferably 30 times or more with respect to the flow rate of the emulsion. Here, the flow rate of the emulsion means the flow rate when the emulsion obtained in the emulsification unit 20 passes through the casing 41. Further, the total flow rate of the cooling water is the total flow rate of all the cooling water flows circulating through each jacket when the four jackets 34, 35, 36, and 37 are provided as in the vibration type stirring and mixing device 40. means.

  The temperature of the cooling water can be appropriately set, and these jackets can cool the emulsion continuously or stepwise from the inlet 31 side toward the outlet 32 side. In this case, the temperature of the cooling water flowing through the four jackets 34, 35, 36, and 37 may be gradually lowered from the inlet side to the outlet side of the stirring and mixing device 31, or all may be set to the same temperature. Also good.

  The cooling water of the four jackets 34, 35, 36, and 37 is, for example, for the emulsion flowing from the inlet 31 side (upstream side) to the outlet 32 side (downstream side) of the vibration type stirring and mixing device 40. Further, it may be circulated from the upstream side to the downstream side in the order of the flow of the emulsion or from the downstream side to the upstream side against the flow of the emulsion.

  In the vibration type stirring and mixing device 40, the stirring body 44 vibrates up and down along the axial direction thereof, so that the emulsion passing through the casing 41 is provided in the flow along the stirring body 44 and the stirring blade 43. Further mixing occurs without agglomeration due to turbulence in the flow through the perforations 48 and notches 49. Therefore, it is possible to highly disperse fine particles of solid fat.

  And when an emulsion is cooled by heat exchange with cooling water, the fluidity | liquidity will fall. The emulsion is cooled while being mixed by the flow along the stirrer 44 and the disturbance of the flow through the opening 48 and the notch 49 provided in the stirring blade 43, so that uneven cooling is less likely to occur. Further, since there is almost no dead space in the vibration type stirring and mixing device 40, uneven stirring is less likely to occur. The vibration type agitation and mixing device 40 can perform good agitation and mixing even when the flowability of the emulsion is high or low. These advantages of the vibration type stirring and mixing device 40 bring about a preferable effect that the emulsified particles containing the solid fat (wax component and the like) contained in the emulsion can be uniformly refined. In addition, since the vibration type agitation and mixing device 40 has a small calorific value, it is excellent in cooling efficiency and can be quickly cooled while the emulsion particles are uniformly refined, so that the emulsion particles containing solid fat can be dispersed well. Is possible. A small calorific value is advantageous from the viewpoint of easy temperature control.

  Thus, since the emulsion is cooled to a solid fat or lower solidification temperature or less without being continuously agglomerated, the fine particle dispersion is highly productive and can provide a fine particle dispersion with excellent quality. The target dispersion 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 target dispersion in this state is about 30 ° C.

  In cooling using the vibration type stirring and mixing device 40, the average cooling rate is preferably set to 0.1 to 8 ° C / sec, more preferably set to 0.5 to 5 ° C / sec. More preferably, it is set to 8 to 5 ° C./sec. 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 2.5 to 30 Hz, and particularly preferably in the range of 5 to 25 Hz. The amplitude of the vibration type stirring and mixing device 40 is preferably 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.

  Thus, the fine particle dispersion obtained by the manufacturing apparatus 100 has fluidity at 25 ° C., and includes, for example, a paste or cream. Specifically, such a fine particle dispersion can be applied to cosmetics such as skin creams and UV protection emulsions. The fine particle dispersion obtained in the manufacturing apparatus 100 is cooled with the solid fat uniformly refined in the high energy processing unit 221 and the solid fat is uniformly refined in the cooling unit 30, so that the feeling of use is improved. It is good and the cosmetic effect is enhanced. The cosmetic effect will be specifically described. When the fine particle dispersion is applied to a skin cream, among other cosmetics, the moisturizing property is improved, and particularly when applied to a UV protective emulsion, the UV preventing property is improved. Say that will improve.

  Next, the component which comprises the target fine particle dispersion manufactured by this invention is demonstrated. As a component filled in the mixing tank 211, as described above, at least one oily component that is solid at 25 ° C. is included. The total content of oily components that are solid at 25 ° C. is preferably 2% by mass or more, and preferably 3% by mass or more in the total components constituting the fine particle dispersion, from the viewpoint of the feeling of use and the cosmetic effect. More preferably, it is more preferably 4% by mass or more, further preferably 5% by mass or more, more preferably 10% by mass or less, still more preferably less than 10% by mass, Specifically, it is preferably 2% by mass or more and 10% by mass or less, more preferably 4% by mass or more and 10% by mass or less, and further preferably 5% by mass or more and less than 10% by mass.

Examples of oily components that are solid at 25 ° C. include plant waxes such as candelilla wax, rice wax, sunflower wax, carnauba wax, and tree wax; animal waxes such as beeswax and whale wax; montan wax and ozokerite Mineral wax; petroleum wax such as microcrystalline wax, paraffin, ceresin; hardened castor oil, hydrogenated jojoba oil, 12-hydroxystearic acid, stearamide, phthalic anhydride, silicone wax, fluorine wax, polyethylene wax, Synthetic waxes such as synthetic beeswax; fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, lanolin fatty acid; cetyl alcohol, stearyl alcohol, behenyl alcohol, hydrogenated dilinoleyl alcohol Higher alcohols call like; ethyl stearate, stearyl stearate, tetra myristate pentaerythritol, and the like fatty acid esters such as cholesteryl stearate. These can be used alone or in combination of two or more.
Of the oily components described above, fatty acids and higher alcohols contribute to the formation of a lamellar gel material, and are therefore referred to as lamellar gel-forming compositions in the present specification.

  The fine particle dispersion produced by the above method can be used for cosmetics. The cosmetic produced using the oily component that is solid at 25 ° C. as a component constituting the fine particle dispersion is specifically applied as a skin cream or the like, and the emulsified particles containing solid fat are Since it is uniformly miniaturized, the feeling of use is good and cosmetic effects such as moisture retention are improved. In particular, a cosmetic produced using the above-mentioned lamella gel-forming composition as a component constituting a fine particle dispersion is specifically applied as a UV protection emulsion or the like, and emulsified particles containing solid fat are used. Since it is uniformly miniaturized, the feeling of use is good and cosmetic effects such as UV protection are improved.

  Cosmetics obtained by applying the fine particle dispersion produced in the present invention include, as raw materials, color pigments and other powders commonly used for cosmetics, oily components other than solid oily components at 25 ° C. , Moisturizing agents, surfactants and the like can be used.

  Examples of the color pigment include red 201, red 202, red 104 (1) aluminum lake, red 218, red 223, yellow 4 aluminum lake, yellow 5 aluminum lake, yellow 401, blue 1 Examples include organic pigments such as No. Aluminum Lake and Blue No. 404, and inorganic pigments such as zinc oxide, titanium oxide, silica, gold, silver, bitumen, and ultramarine blue.

  Examples of other powders include spherical powders such as silica, PMMA, polymethylsilsesquioxane, and urethane powder; plate-shaped powders such as lauroyl lysine, barium sulfate, and boron nitride.

  Examples of oil components other than solid oil components at 25 ° C. include oil agents and volatile oil agents that are liquid at 25 ° C., such as fatty acids and ester hydrocarbon oils thereof.

  Examples of the humectant include polyhydric alcohols such as glycerin and 1,3-butylene glycol, ceramides, stearyl glycyrrhetinate, and the like.

  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.

  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, a plurality of vibration type agitation and mixing devices 40 can be connected in series and used.

  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.

[Example 1]
As shown in Table 1, a skin cream containing 5% by mass of the component of the oily component 1 solid at 25 ° C. in all the components (components 1 to 6) was prepared. After the ingredients 1 to 6 were dispersed with a homomixer under heating at 85 ° C., a high-pressure emulsifier (Starburst Mini HJP-25001 manufactured by Sugino Machine) was used as the high energy processing part, and 2.8 × 10 ⁵ J / kg. Was added to obtain an emulsion. In addition, the number of passes (number of passes) of the high-pressure emulsifier was 1. This emulsion is supplied to a vibration type stirring and mixing apparatus (Vibro mixer manufactured by Chilling Industries Co., Ltd.) with a transition time of 10 seconds while maintaining the temperature at 85 ° C., and the stirring body is vibrated up and down in the apparatus to give the emulsion. Was continuously cooled to 30 ° C. or lower while stirring to obtain a skin cream. In the vibration type stirring and mixing apparatus, the flow rate of the emulsion is 1 g / sec, the total flow rate of the cooling water circulating through the cooling jacket is 10 g / sec, and the total flow rate is 10 times the flow rate of the emulsion. Cooled by cooling water. The average cooling rate at this time was 0.83 ° C./sec. Moreover, the vibration frequency of the vibration type stirring and mixing apparatus was 20 Hz.

[Example 2]
A skin cream was obtained in the same manner as in Example 1 except that the number of passes (pass number) of the high-pressure emulsifier was changed to 5 and the drop energy shown in Table 2 was changed.

Example 3
A skin cream was obtained in the same manner as in Example 1 except that the energy dropped was changed to the drop energy shown in Table 2.

[Examples 4 to 5]
A skin cream was obtained in the same manner as in Example 1 except that the high-energy treatment unit was changed to an ultrasonic emulsifier (IKASONIC (product number: U200S) manufactured by IKA) and changed to the drop energy shown in Table 2.

Example 6
A skin cream was obtained in the same manner as in Example 1 except that the vibration frequency of the vibration type stirring and mixing apparatus shown in Table 2 was changed.

Example 7
A skin cream was obtained in the same manner as in Example 1 except that the transition time of the emulsion to the vibratory stirring and mixing apparatus was changed to the time shown in Table 2.

Example 8
In Table 1, a skin cream was obtained in the same manner as in Example 1 except that the blending component was changed to 2% by mass of ceresin and 96.21% by mass of purified water.

Example 9
In Table 1, a skin cream was obtained in the same manner as in Example 1 except that the compounding component was changed to 9.8% by mass of ceresin and 88.41% by mass of purified water.
Example 10
A skin cream was obtained in the same manner as in Example 1 except that the total flow rate of the cooling water supplied to the vibration type stirring and mixing apparatus shown in Table 2 was changed.

[Comparative Example 1]
A skin cream was obtained in the same manner as in Example 1 except that the emulsified product was directly supplied to the vibration type stirring and mixing device after being dispersed with a homomixer without using a high energy treatment unit. The energy dropped by the homomixer was 3.9 × 10 ⁴ J / kg.

[Comparative Example 2]
A skin cream was obtained in the same manner as in Example 1 except that a homomixer was used instead of the vibration type stirring and mixing apparatus.

[Comparative Example 3]
Using an ultrasonic emulsifier (IKASONIC (product number: U200S) manufactured by IKA) as the high energy processing unit, changing to the drop energy shown in Table 2, and then using a homomixer instead of the vibration type stirring and mixing device, A skin cream was obtained in the same manner as in Example 1.

<Evaluation>
For the skin creams obtained in Examples 1 to 10 and Comparative Examples 1 to 3, the relative water evaporation amount and the particle size of the emulsified particles containing solid fat were measured. The measuring method is as follows. The obtained results are shown in Table 2.

<Measurement method of relative water evaporation>
In a 50 mL vial (Pierce Vial CV-400; manufactured by ASONE), 20 g of water is placed. 0.05 g of each skin cream is uniformly applied to a filter paper (ADVANTEC FILTER PAPER 5C; manufactured by Toyo Roshi Kaisha, Ltd.) having a diameter of about 2 cm, and after standing for 30 min, the application surface is directed upward and placed on the mouth of the vial. Did. Thereafter, the sample was stored in a room at 30 ° C. and a humidity of 30% for 24 hours, and the relative moisture evaporation was measured by measuring the weight before and after storage.

<Measuring method of particle diameter of emulsified particles containing solid fat>
The average particle size of the emulsified particles containing solid fat contained in each skin cream is determined by a laser diffraction / scattering method using a laser diffraction / scattering particle size distribution measuring device (model number: LA-920, manufactured by Horiba, Ltd.). The standard median diameter was measured at a temperature of 25 ° C.

  As is clear from the results shown in Table 2, the skin creams obtained in Examples 1 to 10 were more emulsified particles containing solid fat than those obtained in Comparative Examples 1 to 3. The diameter was found to be very fine. Therefore, it can be expected that the feeling of use of the skin cream is improved. The skin creams obtained in Examples 1 to 10 have improved moisturizing properties and higher cosmetic effects than those obtained in Comparative Examples 1 to 3.

Example 11
As shown in Table 3, a UV protective emulsion containing 9.8% by mass of components of oily components 2 to 5 solid at 25 ° C. in all blended raw materials (components of 1 to 10) was prepared. After the raw material components 1 to 9 were dispersed with a homomixer under heating at 85 ° C., a high-pressure emulsifier (Starburst Mini HJP-25001 manufactured by Sugino Machine) was used as a high energy processing unit, and 2.8 × 10 ⁵ J / kg. Was added to obtain an emulsion. In addition, the number of passes (number of passes) of the high-pressure emulsifier was 1. This emulsion is supplied to a vibration type stirring and mixing device (Vibro mixer manufactured by Chilling Industries Co., Ltd.) with a transition time of 10 seconds, and continuously cooled to 30 ° C. or lower while stirring in the device, Obtained. In the vibration type stirring and mixing apparatus, the flow rate of the emulsion is 1 g / sec, the total flow rate of the cooling water circulating through the cooling jacket is 10 g / sec, and the total flow rate is 10 times the flow rate of the emulsion. Cooled by cooling water. The average cooling rate at this time was 0.8 ° C./sec. Moreover, the vibration frequency of the vibration type stirring and mixing apparatus was 20 Hz.

Example 12
A UV protective emulsion was obtained in the same manner as in Example 11 except that the energy dropped was changed to the drop energy shown in Table 4.

[Examples 13 to 14]
A UV protective emulsion was obtained in the same manner as in Example 11 except that the high-energy treatment unit was changed to an ultrasonic emulsifier and the drop energy shown in Table 4 was changed.

Example 15
A UV protective emulsion was obtained in the same manner as in Example 11 except that the vibration frequency of the vibration type stirring and mixing apparatus shown in Table 4 was changed.

Example 16
A UV-protective emulsion was obtained in the same manner as in Example 11 except that the transition time of the emulsion to the vibratory stirring and mixing apparatus was changed to the time shown in Table 4.

[Comparative Example 4]
A UV-protective emulsion was obtained in the same manner as in Example 11 except that the emulsion was dispersed with a homomixer without using a high-energy treatment unit, and then the emulsion was directly supplied to the vibration type stirring and mixing apparatus. The energy dropped by the homomixer was 3.9 × 10 ⁴ J / kg.

[Comparative Example 5]
A UV-protective emulsion was obtained in the same manner as in Example 11 except that a homomixer was used instead of the vibration type stirring and mixing apparatus.

[Comparative Example 6]
Using a supersonic emulsifier as the high energy processing unit, changing to the drop energy shown in Table 4, and then using a homomixer instead of the vibration type stirring and mixing device, the UV protective emulsion was applied in the same manner as in Example 11. Obtained.

<Evaluation>
For the UV protection emulsions obtained in Examples 11 to 16 and Comparative Examples 4 to 6, the relative water evaporation, the particle size of the emulsified particles containing solid fat, and the UV protection (in vitro SPF) It was measured. The measuring method of the particle size of the emulsified particles containing the relative water evaporation amount and the solid fat is as described above. Moreover, the measuring method of SPF in vitro is as follows. Table 4 shows the obtained results.

<Measurement method of SPF in vitro>
Each UV protection emulsion was uniformly applied to the PMMA plate to 1.3 mg / cm ² , allowed to stand for 15 minutes or more and dried, and then the PMMA plate was irradiated with ultraviolet rays from a certain distance (10 mm). Transmitted ultraviolet rays at that time were detected with an SPF analyzer (UV-2000S, manufactured by Labsphere) at 9 or more locations on the PMMA plate in the range of 250 to 450 nm, and averaged spectra were obtained. In vitro SPF values were calculated by multiplying this spectrum by the effect factor.

  As is clear from the results shown in Table 4, the UV protective emulsions obtained in Examples 11 to 16 were more emulsified particles containing solid fat than those obtained in Comparative Examples 4 to 6. The diameter was found to be very fine. Therefore, it can be expected that the feeling of use of the UV protection emulsion is improved. The UV protection emulsions obtained in Examples 11 to 16 have improved moisture retention, higher SPF values and improved UV protection than those obtained in Comparative Examples 4 to 6. Therefore, the makeup effect can be expected to increase.

DESCRIPTION OF SYMBOLS 100 Apparatus 20 Emulsification part 21 1st emulsification part 211 Mixing tank 22 2nd emulsification part 221 High energy processing part 30 Cooling part 34,35,36,37 Jacket 40 Vibrating stirring mixing apparatus 41 Casing 42 Drive shaft 43 Stirring blade 44 Stirring Body 45a Vibrator 45b Joint 46 Partition 47 Mixing chamber 48 Open hole 49 Notch

Claims (5)

Production of a fine particle dispersion having an emulsification step in which an emulsion is formed by mixing a component containing one or more solid oil components at 25 ° C. with water under heating, and a cooling step in which the formed emulsion is cooled. A method,
The emulsification step uses a high-pressure emulsifier or an ultrasonic emulsifier,
The cooling step includes an agitating and mixing apparatus that includes a stirrer including a drive shaft and a stirring blade attached to the drive shaft in a tubular casing, and the drive shaft vibrates in the axial direction. Using an apparatus, the stirring blade is provided with one or more apertures and / or one or more notches,
The emulsion obtained in the emulsification step is continuously cooled to below the solidification temperature of the oily component by passing through the vibration type stirring and mixing device in the cooling step to produce a fine particle dispersion. A method for producing a fine particle dispersion.   The method for producing a fine particle dispersion according to claim 1, wherein the component containing less than 10% by mass of the oily component that is solid at 25 ° C. is used. The method for producing a fine particle dispersion according to claim 1 or 2, wherein a drop energy applied by the high-pressure emulsifier or the ultrasonic emulsifier is 5 x 10 ⁴ J / kg or more.   The method for producing a fine particle dispersion according to any one of claims 1 to 3, wherein a transition time from the emulsification step to the cooling step is within 60 seconds. The vibratory stirring and mixing device includes a cooling jacket in which cooling water circulates outside the casing,
The emulsion is cooled by passing through the casing,
The total flow rate of the cooling water is at least 10 times the flow rate of the emulsion passing through the casing.
The method for producing a fine particle dispersion according to any one of claims 1 to 4.

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