JP2007161683A - Method for producing emulsified liquid - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing an emulsified liquid, by which the O/W emulsion type emulsified liquid such as hair rinse, softener, cream or lotion can be produced by a liquid crystal phase inversion emulsification method. <P>SOLUTION: This method for producing the O/W type emulsion type emulsified liquid using an oil phase as a dispersoid, comprising adding a water phase to the oil phase to form a liquid crystal structure, and further adding and mixing a water phase to the liquid crystal structure to invert the phase, is characterized by preliminarily adding a water-soluble solvent in an amount of 5 to 45 wt.% based on the total amount of the oil phase to disperse a water-soluble polymer in the oil phase, and mixing in a stirring energy of 0.5 to 70 (kW/m<SP>3</SP>×minute) on the formation of the liquid crystal structure. This production method can inhibit the adsorption of water to the water-soluble polymer, even when the water-soluble polymer is dispersed in the oil phase to form the liquid crystals, and enables the production of the good emulsified liquid. In addition, because the water-soluble polymer is dispersed in the oil phase, a tank for dispersing the water-soluble polymer is not needed to be provided separately. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing an emulsified liquid by producing an O / W emulsion type emulsified liquid such as a hair rinse, a softener, a cream, or a lotion by a liquid crystal phase inversion emulsification method.

  Conventionally, after adding a water phase to an oil phase to form a liquid crystal structure, a liquid phase inversion emulsification method in which an aqueous phase for forming an emulsion is further added to the liquid crystal structure and mixed to perform phase inversion, the above oil is obtained. A method for producing an O / W emulsion type emulsified liquid having a phase as a dispersoid has been performed.

  For example, as an emulsion-forming aqueous phase, a production method using an aqueous solution containing 0.1% by weight or more of a cellulose polymer or carboxyl vinyl polymer having a hydrophobic group with respect to the entire emulsion-forming aqueous phase (see, for example, Patent Document 1) , A method of performing phase inversion emulsification by adding a water-soluble polymer to the oil phase, and an emulsification method in which, during this emulsification, the oil phase is an oil phase having a viscosity at least twice that of the water phase (for example, Patent Document 2) is known.

  However, Patent Document 1 does not form a liquid crystal in a system in which a water-soluble polymer is dispersed in an oil phase, and Patent Document 2 is not a method of forming a liquid crystal, and any of the documents The technical idea is completely different from the present invention in that a polymer aqueous solution is used and it is not a dispersion system.

As described above, a manufacturing method for forming liquid crystals by dispersing a water-soluble polymer in an oil phase is not found in the prior art, but in reality, the emulsification apparatus has a complicated structure, so it is added as a powder. There is a problem that a uniform composition cannot be obtained by adhering to the internal structure.
On the other hand, a large amount of water is required to add as a conventional aqueous solution, and there are problems such as a compositional restriction and a separate large-capacity preparation tank, which are further dispersed in a non-aqueous dispersion medium. In order to add after emulsification, there is a problem that an emulsification operation is required again when the dispersion is added.
Therefore, in the production of an emulsified liquid using a water-soluble polymer, ideally, it is efficient to disperse it in the “oil phase” that is a non-aqueous component, but the “liquid crystal conversion” that is the object of the present invention is not. In the `` phase emulsification method '', if a water-soluble polymer is present at the time of liquid crystal formation, the added water is absorbed by the polymer, and a good liquid crystal is not formed, resulting in an insufficient emulsified state at the time of phase inversion. There is a problem in that an emulsified liquid cannot be obtained.
Japanese Patent Laid-Open No. 10-180085 (Claims, Examples, etc.) JP-A-11-156172 (Claims, Examples, etc.)

  In view of the above-mentioned problems of the prior art, the present inventors intend to solve this problem. In the case of forming a liquid crystal by dispersing a water-soluble polymer in an oil phase, in the presence of the water-soluble polymer. However, it aims at providing the manufacturing method of the emulsified liquid which suppresses the water | moisture-content adsorption | suction to water-soluble polymer, and manufactures a favorable emulsified liquid.

As a result of intensive studies on the above-described conventional problems and the like, the present inventors have added a water phase to the oil phase to form a liquid crystal structure, and then added and mixed an aqueous phase to the liquid crystal structure to perform phase inversion. In the method for producing an O / W emulsion type emulsified liquid having the oil phase as a dispersoid, a water-soluble solvent having a specific amount with respect to the total amount of the oil phase is added to the oil phase in advance. The present invention is completed by finding that the above-described method for producing an emulsified liquid can be obtained by dispersing a polymer in an oil phase and mixing with stirring energy that is in a specific range when forming a liquid crystal structure. It came to.
That is, in the method for producing an emulsified liquid according to the present invention, the aqueous phase is added to the oil phase to form a liquid crystal structure, and then the aqueous phase is further added to the liquid crystal structure to be mixed and phase-inverted. In the method for producing an O / W emulsion type emulsified liquid having an oil phase as a dispersoid, 5 to 45% by weight of a water-soluble solvent based on the total amount of the oil phase is added to the oil phase in advance, Dispersed in the oil phase and mixed with stirring energy of 0.5 to 70 (kW / m ³ · min) when forming the liquid crystal structure.
The “emulsified liquid” defined in the present invention refers to a liquid in which substances insoluble in the continuous phase are dispersed as fine particles in the liquid that is the continuous phase. In the present invention, the continuous phase is a water-soluble liquid, and the dispersed particles are oil-soluble substances. Examples thereof include hair rinses, softeners, creams, and lotions.
In addition, “liquid crystal” refers to a liquid crystal that is observed with a polarizing microscope (400 times) at room temperature (25 ° C.), and where shining portions (crossed Nicols) are closely observed.

  According to the present invention, even when a water-soluble polymer is dispersed in an oil phase to form a liquid crystal, the emulsified liquid that can suppress moisture adsorption to the water-soluble polymer and produce a good emulsified liquid. A manufacturing method is provided. Further, the present invention has an advantage in that it is not necessary to separately provide a water-soluble polymer dispersion tank by dispersing the water-soluble polymer in the oil phase.

Hereinafter, embodiments of the present invention will be described in detail.
In the method for producing an emulsified liquid according to the present invention, the water phase is added to the oil phase to form a liquid crystal structure, and then the water phase is further added to the liquid crystal structure and mixed to perform phase inversion. In the method of producing an O / W emulsion type emulsified liquid having a dispersoid as a dispersoid, a water-soluble solvent in an amount of 5 to 45% by weight based on the total amount of the oil phase is previously added to the oil phase, and the water-soluble polymer is added to the oil phase And mixed with stirring energy of 0.5 to 70 (kW / m ³ · min) when forming the liquid crystal structure.

In the present invention, the “oil phase” is composed of various oil components according to the type and purpose of the emulsified liquid, and the solubility in water is 0.5 g or less in 100 g of water at 20 ° C., and And a mixture containing one or more organic compounds having a melting point of 100 ° C. or lower.
Examples of oily components that can be used include synthetic oils such as silicone, mineral oils such as liquid paraffin, vegetable oils such as jojoba oil and olive oil, animal oils such as lanolin and squalane, fatty acids and fatty acid esters such as hexyl laurate and stearic acid. Etc.
Examples of the silicone include methylpolysiloxane, methylphenylpolysiloxane, phenylpolysiloxane, polyoxyethylene / methylpolysiloxane, dimethylsiloxane / methyl (aminopropyl) siloxane copolymer, and aminoethylaminopropylmethylsiloxane / dimethylsiloxane. One type or a mixture of two or more types such as a copolymer may be mentioned. In addition, since a high polymerization degree silicone with a viscosity of 1 million to 15 million mm < ² > / s is hard to melt | dissolve in another oil-based component, it is preferable to add after liquid crystal structure formation.
In addition, the oil phase of the present invention may include a surfactant such as a cation activator or a nonion activator, a solvent such as ethanol or a polyhydric alcohol, an oil-soluble antioxidant, a preservative, a fragrance, or a dye as necessary. -UV absorber can be included in the range which does not impair the effect of this invention.

  The amount of the oily component to be used can be appropriately determined depending on the type, use of the emulsified liquid, etc., but preferably 0.5 to 20% by mass (hereinafter simply referred to as “%”) with respect to the total amount of the emulsified liquid. More preferably, the content is 1 to 15%. If the amount of the oily component is less than 0.5%, the effect of containing the oily component is not sufficient, while if it exceeds 20%, it may be difficult to form a liquid crystal structure and an emulsion.

In the present invention, the water-soluble solvent is used to temporarily suppress the water uptake into the water-soluble polymer and form a good liquid crystal, and is previously oiled in an amount of 5 to 45% based on the total amount of the oil phase. It is added to the phase.
The water-soluble solvent that can be used is not particularly limited as long as it is a solvent that can arbitrarily dissolve in water, and examples thereof include lower alcohols such as ethanol and isopropyl alcohol, propylene glycol, ethylene glycol, 1,3-butylene glycol, and the like. And polyhydric alcohols.
If the addition amount of the water-soluble solvent is less than 5% with respect to the total amount of the oil phase, water intake cannot be suppressed into the water-soluble polymer, so that the intended effect cannot be exhibited. Exceeding is not preferable because the effect does not change and only the amount of the oil phase increases.
A preferable amount of the water-soluble solvent added is preferably 10 to 45% with respect to the total amount of the oil phase from the viewpoint of further effects of the present invention.

The aqueous phase of the present invention includes an aqueous phase for forming a liquid crystal structure and an aqueous phase for inversion of the liquid crystal structure to form an O / W type emulsion, both of which have the same composition, Different compositions may be used.
In the present invention, the “aqueous phase” refers to water or water-soluble solvents such as emulsifiers and water-soluble polymers, ethanol and polyhydric alcohols, inorganic salts, water-soluble organic salts, and dyes as necessary. An aqueous solution in which a chemical substance is dissolved.
The total amount of the aqueous phase to be used can be appropriately determined depending on the type, use of the emulsified liquid, etc., but is preferably 2 to 20 times, more preferably 5 to 15 times the amount of the oil phase. desirable. If the amount of the aqueous phase is less than 2 times, a good O / W emulsion may not be obtained. On the other hand, if the amount exceeds 20 times, the effect of phase inversion emulsification does not change.

  The amount of the aqueous phase used for forming the liquid crystal structure can be appropriately selected depending on the composition of the oil phase, the use of the emulsified liquid, the purpose, etc., but preferably 0.3 to 5 with respect to the amount of the oil phase. It is desirable to make it twice, more preferably 0.5 to 4 times. If the amount of the aqueous phase is less than 0.3 times or more than 5 times, in any case, formation of the liquid crystal structure is insufficient, and a good emulsion may not be obtained.

The water-soluble polymer of the present invention is added and dispersed as a powder in the oil phase. In the present invention, the “water-soluble polymer” refers to a polymer having a solubility in water of 0.5 g or more in 100 g of water at 40 ° C.
The water-soluble polymer that can be used is not particularly limited as long as it is a polymer that can be dissolved in water or a water-soluble solvent and has the above characteristics. For example, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, methylcellulose, carboxyvinyl Examples include polymers.
The addition amount of the water-soluble polymer is preferably 0 to 35% with respect to the total amount of the oil phase, and more preferably 1 to 30%.
If the amount of the water-soluble polymer added is 0%, the desired physical properties of the emulsified liquid may not be obtained, the stability may be deteriorated, and the significance of the present invention will be lost. On the other hand, if it exceeds 35%, the solid matter concentration in the oil phase becomes high, and the physical properties of the oil phase become poor.

In the present invention, a water-soluble solvent of 5 to 45% based on the total amount of the oil phase is previously added to the oil phase having the above structure, and a water-soluble polymer is added and dispersed in the oil phase to form a liquid crystal structure. It is sometimes necessary to mix with a stirring energy of 0.5 to 70 (kW / m ³ · min), and then the liquid phase structure is further mixed with an aqueous phase to perform phase inversion, whereby the oil phase O / W emulsion type emulsified liquid having a dispersoid as a dispersoid is produced.
The “stirring energy” defined in the present invention is stirring power P / V [KW / m ³ ] × stirring time (minutes), and is represented by the following formula (I).

By setting the stirring energy at the time of forming the liquid crystal structure to 0.5 to 70 kW / m ³ · min, water intake into the water-soluble polymer can be suppressed, and good liquid crystal can be formed. An emulsified liquid can be obtained.
Preferably, from the viewpoint of producing a further good emulsifying liquid, a stirring energy 1~50kW / m ³ · min, more preferably, it is desirable that the 1~30kW / m ³ · minute.
If the stirring energy is less than 0.5 kW / m ³ · min, poor mixing occurs and the formation of the liquid crystal structure becomes insufficient. On the other hand, if it exceeds 70 kW / m ³ · min, This is not preferable because uptake cannot be suppressed.

A liquid crystal structure is formed by this stirring energy. Whether or not the liquid crystal structure is formed in this step depends on whether the viscosity of the system is as high as 10 to 100 Pa · s when the liquid crystal structure is formed. At the same time, when observed with a polarizing microscope (400 magnifications), it can be confirmed that the shining portions (cross Nicols) are closely observed.
In addition, the apparatus for forming the liquid crystal structure is not particularly limited, and a known stirring device can be used. For example, stirring can be performed only with a general entire mixing blade such as a paddle, anchor, or ribbon. In view of the high viscosity of the liquid crystal structure, an apparatus equipped with a scraper is preferable. As will be described later, after forming the liquid crystal structure, it is preferable to use a device having a strong shearing force such as a homomixer or a disperser when the phase is changed to an emulsion. A more suitable device is preferred. FIG. 1 shows an emulsifying apparatus used for producing an emulsified liquid according to the present invention, wherein 1 is an emulsifying tank, 2 is an anchor type stirrer, 3 is a homomixer, and 4 is a vacuum apparatus.
The stirring tank used in the present invention preferably has a temperature control function, and specific examples of the temperature control function include a recycling line by external heat exchange, a coil, a jacket outside the tank, and the like. Among these, it is preferable to use a jacket in view of thermal efficiency.

The mixing (stirring) temperature (article temperature) at the time of forming the liquid crystal structure is appropriately selected depending on the type and composition of the oil phase, but is preferably 45 to 90 ° C, more preferably 50 to 85 ° C.
If the mixing temperature is less than 45 ° C, the oil phase may solidify or a liquid crystal structure may not be formed. If it exceeds 90 ° C and the temperature is too high, the evaporation of moisture in the mixture becomes severe and the balance of the composition is lost. In some cases, the liquid crystal structure is not formed.

In the present invention, after the liquid crystal structure is prepared as described above, an aqueous phase is further added to the liquid crystal structure and mixed to cause phase inversion, whereby an O / W emulsion type emulsified liquid having the oil phase as a dispersoid. Is manufactured.
The method for adding the aqueous phase in this step is not particularly limited. For example, the entire amount of the aqueous phase may be added to the liquid crystal structure in a lump or may be added in small portions.

  In addition, the mixing device in this step may be any mixture that can obtain an O / W emulsion type emulsified liquid having the oil phase as a dispersoid, and the same stirring device as the liquid crystal structure can be used. In consideration of efficiently dispersing the liquid crystal structure having a viscosity in the aqueous phase, it is preferable to use a device having a strong shearing force such as a homomixer or a disperser, for example. The stirring conditions at this time are not limited to the above stirring energy, and can be carried out in a normal use range. It is preferable that the peripheral speed of the stirring blade is 1 m / s or more, more preferably 2 to 25 m / s. It is.

The mixing (stirring) temperature (article temperature) in the above step is not particularly limited and can be appropriately selected, but is preferably 40 to 90 ° C, more preferably 45 to 85 ° C. is there. If the mixing temperature is less than 40 ° C., the oil phase may solidify before being uniformly dispersed to form non-uniform particles, and if it exceeds 90 ° C. and becomes too high, the water evaporation becomes intense. The balance of the composition is lost, and it takes a long time for cooling in the subsequent process, which is inefficient.
Further, the mixing (stirring) time of the above step is not particularly limited as long as it is a mixture that can obtain an O / W emulsion type emulsified liquid having the oil phase as a dispersoid, and can be appropriately selected. However, it is desirable to mix for at least 1 minute, especially 2 to 60 minutes. If the mixing time is less than 1 minute, a uniform emulsified liquid may not be obtained. If the mixing time is longer than 60 minutes, no further mixing effect is obtained, which is undesirable in terms of work efficiency. There is.

In the present invention configured as described above, after the water phase is added to the oil phase to form a liquid crystal structure, the water phase is further added to the liquid crystal structure and mixed to perform phase inversion, whereby the oil phase In the method of producing an O / W emulsion type emulsified liquid having a dispersoid as a dispersoid, a water-soluble solvent in an amount of 5 to 45% by weight based on the total amount of the oil phase is previously added to the oil phase, and the water-soluble polymer is added to the oil phase. And forming a liquid crystal structure by mixing with a stirring energy of 0.5 to 70 (kW / m ³ · min) to disperse the water-soluble polymer in the oil phase to form a liquid crystal. Even in this case, swelling of the water-soluble polymer is suppressed, moisture adsorption to the water-soluble polymer is suppressed, and a good emulsified liquid can be produced. In this invention, since it can manufacture without requiring another dispersion medium and a dispersion tank for disperse | distributing water-soluble polymer, it is excellent in manufacturing efficiency and also in cost.
In addition, a high polymerization degree silicone having a viscosity of 1,000,000 to 15 million mm ² / s can be blended in a simple manufacturing process by adding it after forming the liquid crystal structure, and there is no restriction on the degree of polymerization of the silicone used. It has also become possible to improve performance.

Moreover, the emulsion liquid obtained by the production method of the present invention can be further added with various components within a range that does not impair the effects of the present invention after the emulsion is formed.
The emulsified liquid of the present invention suppresses water adsorption to the water-soluble polymer even when the water-soluble polymer is dispersed in the oil phase and forms a good emulsified liquid by the liquid crystal phase inversion emulsification method. For example, it can be suitably used as an emulsified liquid of O / W emulsion type such as hair rinse, softener, cream, lotion and the like.

  EXAMPLES Next, although an Example and a comparative example demonstrate this invention further in detail, this invention is not limited to the following Example.

[Examples 1 to 5 and Comparative Examples 1 to 4]
<Method for manufacturing rinse>
In each Example and Comparative Example, the following oily components were first mixed and dissolved uniformly and adjusted to 80 ° C., and then 6.0 parts of hydroxyethyl cellulose was added and mixed and dispersed.
Stearyl alcohol 35.0 parts Alkyltrimethylammonium chloride (80% product) 22.5 parts Polyglyceryl diisostearate 5.0 parts Polyethylene glycol monostearate 3.0 parts In each of the above mixed dispersions, each Example and Comparative Example The water-soluble solvent (ethanol or propylene glycol) shown in the following Table 1 and Table 2 was added in the same amount as shown in the following Table 1 and Table 2, and uniformly mixed and dispersed to obtain an oil phase.
Mixing conditions: Using a general-purpose paddle stirring vessel, stirring the oil phase component adjusted to 80 ° C. at a rotation speed of 100 rpm, adding hydroxycellulose, mixing and dispersing for 10 minutes, then adding a predetermined amount of water-soluble solvent And mixed for another 5 minutes.

The oil phase was put into an emulsifier (capacity 2 kL) shown in FIG. 1 and adjusted to 80 ° C., and then 100 parts of 80 ° C. purified water was added and mixed to form a liquid crystal. The stirring energy (stirring power and mixing time) in each Example and Comparative Example at this time is shown in Tables 1 and 2 below. The state of the obtained liquid crystal was evaluated according to the following evaluation criteria. The results are shown in Tables 1 and 2 below. The data for calculating the stirring energy is shown in Table 3 below.
Next, silicon oil mix (methylpolysiloxane 23: highly polymerized methylpolysiloxane: 3: highly polymerized dimethylsiloxane / methyl (aminopropyl) siloxane copolymer 4: mixture of polyoxyethylene / methylpolysiloxane copolymer 2) 12.5 parts was added and mixed for 30 minutes, and then 480 parts of 80 ° C. purified water was added and mixed for 10 minutes to invert the phase into an O / W emulsion.
Purified water is added to this phase inversion product and cooled while diluting and mixing so that the total liquid volume becomes 951 parts. At 50 ° C., 30 parts of arginine solution (23 parts of purified water, 3 parts of arginine) , A mixture of 4 parts of 70% glycolic acid) and 12.5 parts of a 40% solution of amodimethicone emulsion, further cooled to 40 ° C., added 6.5 parts of fragrance, and mixed for 15 minutes to produce a rinse.
Mixing conditions: (1) Silicone mixing is paddle 35 rpm.
(2) Phase inversion (purified water added) is paddle 35 rpm, homomixer 2000 rpm.
The emulsified state and physical properties of the obtained emulsified liquid were evaluated according to the following evaluation criteria. These results are shown in Tables 1 and 2 below.

[Evaluation method of liquid crystal state]
Sensory evaluation was performed according to the following evaluation criteria by observation with a polarizing microscope (400 magnifications).
Evaluation criteria:
○: A state in which liquid crystals are neatly formed.
X: A state in which an aqueous component is dispersed in an oily component and almost no liquid crystal is formed.

[Evaluation method of emulsified state]
Sensory evaluation was performed according to the following evaluation criteria by observation with a polarizing microscope (400 magnifications).
Evaluation criteria:
○: A state in which the oil component is dispersed as uniform particles in the aqueous component.
X: A state where coarse particles of the oil component are present or dispersed in a non-uniform state.

[Evaluation method of emulsion properties]
The physical properties of the milk liquid were evaluated according to the following evaluation criteria.
Evaluation criteria:
◯: A property having a predetermined liquid viscosity (at 80 ° C., the liquid viscosity is about 5 Pa · s or less) and does not impair the transportation of the liquid or the product.
X: In a gelled state, physical properties that are difficult to transport or have problems in usability.

  As is clear from the results of Tables 1 and 2, Examples 1 to 5, which are the scope of the present invention, are compared with Comparative Examples 1 to 4, which are outside the scope of the present invention, in the liquid crystal state, the emulsified state and physical properties of the emulsified liquid It turned out to be superior to all of the above.

It is a schematic diagram of the emulsification apparatus used for the Example and the comparative example.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Emulsification tank 2 Anchor type stirrer 3 Homomixer 4 Vacuum apparatus

Claims (1)

An O / W emulsion having the oil phase as a dispersoid by adding a water phase to the oil phase to form a liquid crystal structure, and then adding and mixing the water phase to the liquid crystal structure to cause phase inversion. In the method for producing an emulsified liquid of the type, a water-soluble solvent of 5 to 45% by weight based on the total amount of the oil phase is previously added to the oil phase, the water-soluble polymer is dispersed in the oil phase, and a liquid crystal structure A method for producing an emulsified liquid, comprising mixing at a stirring energy of 0.5 to 70 (kW / m ³ · min) at the time of forming.

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