JP6842518B2 - Dispersion liquid manufacturing method - Google Patents

Description

The present invention relates to a method for producing a dispersion.

A method of producing a dispersion using a micromixer is known.

Patent Document 1 discloses a method for producing a dispersion liquid (emulsification liquid) in which each of an aqueous component and an oil component is allowed to flow in the pores of a micromixer and collide with each other.

In Patent Document 2, an aqueous component is flowed, an oily component containing a melted ceramide and a nonionic surfactant is flowed, and a fluid obtained by merging them is circulated in the pores of a micromixer to prepare an emulsion. After that, a method for producing a ceramide fine particle dispersion liquid that cools the ceramide and solidifies the ceramide is disclosed.

Patent Document 3 describes a dispersion (emulsion) in which an aqueous component is allowed to flow through a microchannel of a micromixer and an oily component is allowed to flow into the microchannel through an opening area so that the oily component is brought into contact with the aqueous component and dispersed. The manufacturing method is disclosed.

Patent Document 4 discloses a method for producing a dispersion liquid in which an oil component as a continuous phase liquid and an aqueous component as a dispersion phase liquid are merged in a micromixer, and then the merged fluid is circulated to an orifice. Has been done.

Japanese Unexamined Patent Publication No. 2008-142588 Japanese Unexamined Patent Publication No. 2008-037842 Special Table 2007-516066 Special Table 2006-507921

In dispersions used in the fields of cosmetics, pharmaceuticals, etc., it is desirable that fine particles are dispersed from the viewpoint of usability and the like.

However, in the technique disclosed in Patent Document 1, since the aqueous component contains a surfactant, the surfactant contained in the aqueous component is used to participate in the formation of emulsified droplets, so that a specific HLB nonionic is used. A sex surfactant is required. Therefore, the range of application of the obtained dispersion liquid as a blending technology for cosmetics and pharmaceuticals is narrowed.

In the technique disclosed in Patent Document 2, since the oily component contains ceramide which is a solid fat, the particles obtained after cooling are not emulsified droplets but solid dispersed particles.

Since the techniques disclosed in Patent Documents 3 to 4 do not use a water-soluble solvent, it is difficult to obtain a dispersion liquid of fine emulsified droplets.

An object of the present invention is to produce a dispersion liquid in which fine particles are dispersed.

The present invention includes a merging step in which an aqueous component and an oily component are merged, the aqueous component before merging in the merging step, the oily component before merging in the merging step, and the aqueous component in the merging step. An average particle having a pore circulation step in which one or two or more of the fluids after merging with the oily component are circulated through the pores under the condition that the segregation index (Xs) is 0.15 or less. A method for producing a dispersion of particles having a diameter of 10 μm or less, wherein the oily component is one or more selected from the group of an oil agent and a compound represented by the following general formulas (I) to (III). Contains at least one of the surfactant and the surfactant precursor that forms the surfactant when combined with the aqueous component.

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. P1, p2, p3, q1, q2, q3, r1, r2, and r3 represent the average number of added moles, respectively. ≦ p1 + p2 + p3 ≦ 20, 0 ≦ q1 + q2 + q3 ≦ 10, and 0 ≦ r1 + r2 + r3 ≦ 10, and 1 ≦ p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 ≦ 40. EO, PO, and BO are added randomly or in blocks).

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. S, t, and u represent the average number of moles added. 1 ≦ s ≦ 70, 0 ≦ t ≦ 70, and 0 ≦ u ≦ 10 and 1 ≦ s + t + u ≦ 100. EO, PO, and BO are added in a random or block shape. R ¹ is a hydrocarbon group having 2 or more and 5 or less carbon atoms. .)

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. V1, v2, w1, w2, x1, and x2 represent the average number of moles added. 1 ≦ v1 + v2 ≦ 10, 0, respectively. ≦ w1 + w2 ≦ 9, 0 ≦ x1 + x2 ≦ 9, and 1 ≦ v1 + v2 + w1 + w2 + x1 + x2 ≦ 10. EO, PO, and BO are added in a random or block shape. R ² and R ³ are independent of each other. It is a hydrocarbon group having 1 or more and 4 or less carbon atoms. N is a number of 1 or more and 4 or less.)

According to the present invention, at least one of a surfactant precursor that forms a surfactant when the oily component is mixed with an oil agent, a water-soluble solvent having a specific structure, a surfactant, and the aqueous component. The segregation index (Xs) is 0.15 or less for one or more of the aqueous component before merging, the oily component before merging, and the fluid after merging them. By circulating the particles in the pores under the conditions, a dispersion liquid in which fine particles having an average particle diameter of 10 μm or less are dispersed can be produced.

It is a figure which shows the structure of the dispersion liquid manufacturing system. It is a partial vertical sectional view of the main part in the micromixer of 1st structure. FIG. 3 is a sectional view taken along line III-III in FIG. It is (a) partial vertical sectional view of the main part in the modified example of the micromixer of 1st structure, and (b) IVB-IVB cross-sectional view in FIG. 4 (a). It is a vertical sectional view of the micromixer of the 2nd structure. It is a vertical cross-sectional view of the modification of the micromixer of 2nd structure. (A) Partial vertical cross section of the main part of the micromixer of the third configuration, (b) VIIB-VIIB cross section in FIG. 7 (a), and (c) VIIC-VIIC cross section in FIG. 7 (a). It is a figure. It is (a) partial vertical sectional view and (b) VIIIB-VIIIB cross-sectional view in FIG. 8A of the main part in the modification of the micromixer of 3rd structure.

The method for producing the dispersion liquid according to the present embodiment includes a merging step in which the aqueous component and the oily component are merged, an aqueous component before merging in the merging step, an oily component before merging in the merging step, and an aqueous component in the merging step. It has a pore circulation step in which one or two or more of the fluids after the components and the oily components are merged are circulated through pores having a pore diameter of 0.1 mm or more and 3 mm or less. Then, the oily component is combined with an oil agent, one or more water-soluble solvents selected from the group of compounds represented by the following general formulas (I) to (III), a surfactant and an aqueous component. It contains at least one of the surfactant precursors that form the surfactant when

The surfactant precursor is an oily component that is neutralized by an alkaline component in the aqueous component to form an anionic surfactant, or is neutralized by an acid component in the aqueous component. It is a component that forms a cationic surfactant.

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. P1, p2, p3, q1, q2, q3, r1, r2, and r3 represent the average number of added moles, respectively. ≦ p1 + p2 + p3 ≦ 20, 0 ≦ q1 + q2 + q3 ≦ 10, and 0 ≦ r1 + r2 + r3 ≦ 10, and 1 ≦ p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 ≦ 40. EO, PO, and BO are added randomly or in blocks).

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. S, t, and u represent the average number of moles added. 1 ≦ s ≦ 70, 0 ≦ t ≦ 70, and 0 ≦ u ≦ 10 and 1 ≦ s + t + u ≦ 100. EO, PO, and BO are added in a random or block shape. R ¹ is a hydrocarbon group having 2 or more and 5 or less carbon atoms. .)

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. V1, v2, w1, w2, x1, and x2 represent the average number of moles added. 1 ≦ v1 + v2 ≦ 10, 0, respectively. ≦ w1 + w2 ≦ 9, 0 ≦ x1 + x2 ≦ 9, and 1 ≦ v1 + v2 + w1 + w2 + x1 + x2 ≦ 10. EO, PO, and BO are added in a random or block shape. R ² and R ³ are independent of each other. It is a hydrocarbon group having 1 or more and 4 or less carbon atoms. N is a number of 1 or more and 4 or less.)

Generally, in a dispersion liquid used in the fields of cosmetics, pharmaceuticals, etc., it is desired that fine particles are dispersed from the viewpoint of usability and the like. On the other hand, according to the method for producing a dispersion liquid according to the present embodiment, a surfactant is formed when the oil-based component is mixed with a water-soluble solvent having a specific structure, a surfactant and the aqueous component. One or two or more of the aqueous component before merging, the oily component before merging, and the fluid after merging them containing at least one of the surfactant precursors have a pore size of 0. By circulating in pores of 1 mm or more and 3 mm or less, a dispersion liquid in which fine particles are dispersed can be produced.

This is because, in the method for producing a dispersion liquid according to the present embodiment, among the aqueous component before merging in the merging step, the oily component before merging in the merging step, and the fluid after merging the aqueous component and the oily component in the merging step. Since one or two or more are circulated through pores having a pore diameter of 0.1 mm or more and 3 mm or less, the interface existing in the oily component due to the stirring effect due to the turbulent flow at the time of merging or after merging the oily component and the aqueous component. The diffusion of the activator into the aqueous component without contributing to the dispersion is effectively suppressed so that the surfactant is efficiently supplied to the oil-water interface and, in addition, the specific contained in the oily component. It is considered that the water-soluble solvent having a structure significantly reduces the interfacial tension of oil and water.

In the conventional method for producing a dispersion liquid using a homomixer or the like, the same effect cannot be obtained even if the oily component contains the same water-soluble solvent, surfactant, or the like. It is considered that this is because both the water-soluble solvent and the surfactant diffuse into the aqueous component before the oily component reaches the shearing field.

Hereinafter, a detailed description will be given.

The method for producing a dispersion liquid according to the present embodiment includes a merging step and a pore circulation step.

[Merge step]
In the merging step, the aqueous component of the liquid and the oily component of the liquid are merged.

(Aqueous component)
The aqueous component is preferably composed only of water from the viewpoint of easy preparation, but other than that, for example, an aqueous solution in which a solute such as a salt is dissolved in water or a mixed solution of water and a water-soluble solvent. It may be. In that case, the content of water in the aqueous component is preferably 50% by mass or more, more preferably 70% by mass or more, still more preferably 90% by mass or more, still more preferably, from the viewpoint of obtaining a dispersion liquid of fine particles. It is 95% by mass or more, more preferably 98% by mass or more. Examples of the water-soluble solvent include alcohols having 1 or more and 6 or less carbon atoms such as methanol, ethanol, glycerin, propylene glycol, dipropylene glycol, and 1,3-butylene glycol.

In addition, the aqueous component may contain an alkaline component or an acid component that neutralizes the surfactant precursor.

Examples of the alkaline component include alkali metal hydroxides, ammonia, alkanolamines, etc., which neutralize the surfactant precursor to form an anionic surfactant.

Examples of the acid component include mineral acids such as phosphoric acid and hydrochloric acid, and organic acids such as carboxylic acids and amino acids, which neutralize surfactant precursors to form cationic surfactants.

(Oil component)
The oily component contains an oil agent, a water-soluble solvent having a specific structure, and at least one of a surfactant and a surfactant precursor.

<Oil>
Examples of the oil agent include liquid oils that are liquid at 20 ° C. and solid fats that are solid at 20 ° C. The oily component may contain only liquid oil as an oil agent, may contain only solid fat, or may contain both of them. When a solid fat is used, the oily component is heated to a temperature equal to or higher than the melting point of the solid fat to melt it.

Examples of the liquid oil include liquid higher alcohols, liquid ester oils, liquid hydrocarbon oils, liquid silicone oils, liquid dialkyl ethers, liquid fats and oils, liquid functional oils, liquid fragrances and the like. .. Of these, from the viewpoint of obtaining a dispersion liquid of fine particles, liquid higher alcohol, liquid ester oil, liquid hydrocarbon oil, and liquid silicone oil are preferable, and liquid higher alcohol, liquid ester oil, and the like. And liquid hydrocarbon oils are more preferred, liquid higher alcohols and liquid ester oils are even more preferred, and liquid higher alcohols are even more preferred. The liquid oil may be either volatile or non-volatile.

Liquid higher alcohols include, for example, saturated or unsaturated linear or branched liquid alcohols. The liquid higher alcohol is preferably a saturated alcohol from the viewpoint of obtaining a dispersion of fine particles, and is preferably a branched-chain alcohol from the same viewpoint. The carbon number of the liquid higher alcohol is preferably 8 or more, more preferably 10 or more, still more preferably 12 or more, still more preferably 16 or more, still more preferably 18 or more, from the viewpoint of obtaining a dispersion of fine particles. From the same viewpoint, it is preferably 22 or less. Specific examples thereof include 2-octyldodecane-1-ol.

Examples of the liquid ester oil include liquid fatty acid glycerides such as liquid neopentyl glycol difatty acid ester, ethylene glycol difatty acid ester, fatty acid monoglyceride, fatty acid diglyceride, and fatty acid triglyceride. As the liquid ester oil, neopentyl glycol difatty acid ester is preferable from the viewpoint of obtaining a dispersion liquid of fine particles.

The acyl group of the liquid ester oil is preferably a straight chain or a branched chain, and more preferably a straight chain, from the viewpoint of obtaining a dispersion of fine particles. From the same viewpoint, the number of carbon atoms of the acyl group of the liquid ester oil is preferably 6 or more, more preferably 8 or more, and from the same viewpoint, preferably 22 or less, more preferably 18 or less, still more preferably 16. Below, it is even more preferably 14 or less, and even more preferably 12 or less. Preferred liquid ester oils include neopentyl glycol dicaprate from the viewpoint of obtaining a dispersion of fine particles.

Examples of the liquid hydrocarbon oil include liquid paraffin, squalene, squalene and the like. The liquid hydrocarbon oil is preferably a linear or branched hydrocarbon, more preferably a branched hydrocarbon from the viewpoint of obtaining a dispersion of fine particles, and from the same viewpoint, a saturated or unsaturated hydrocarbon. Is preferred, and saturated hydrocarbons are more preferred. The carbon number of the liquid hydrocarbon oil is preferably 16 or more, more preferably 22 or more, still more preferably 28 or more from the viewpoint of obtaining a dispersion of fine particles, and preferably 50 or less from the same viewpoint. It is more preferably 40 or less, still more preferably 32 or less. Preferred hydrocarbon oils include squalane from the viewpoint of obtaining a dispersion of fine particles.

Examples of the liquid silicone oil include dimethylpolysiloxane, methylpolysiloxane, methylphenylsiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, methylhydrogenpolysiloxane, silicone resin, amino-modified silicone, and alkyl-modified silicone. Examples thereof include polyether-modified silicone, glyceryl-modified silicone, and silicone wax. The liquid silicone oil is preferably one or more selected from these, and more preferably dimethylpolysiloxane, from the viewpoint of obtaining a dispersion of fine particles.

Examples of the liquid dialkyl ether include ethers having a saturated or unsaturated linear or branched alkyl group or alkenyl group (preferably having 8 or more and 22 or less carbon atoms). Examples of liquid fats and oils include vegetable oils such as soybean oil, palm oil, palm kernel oil, linseed oil, cottonseed oil, rapeseed oil, millet oil, and castor oil.

Liquid functional oils include, for example, liquid ceramides, organic UV absorbers such as 2-ethylhexyl paramethoxycinnamate, and 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol. Examples include liquid sphingolipids. Examples of the liquid fragrance include general ones that have been conventionally used.

Examples of the solid fat include solid ceramide, solid paraffin, solid higher alcohol, petrolatum, solid silicone, hydrogenated oil, solid fragrance and the like. The solid fat is preferably a solid ceramide or a solid fragrance, and more preferably a solid ceramide, from the viewpoint of the remarkable effect of obtaining a dispersion liquid of fine particles.

Examples of the solid ceramide include N- (2-hydroxy-3-hexadecyloxypropyl) -N-2-hydroxyethylhexadecanamide, which has good dispersion stability.

Examples of the solid paraffin include paraffin wax and microcrystalline wax described in JIS K 2235, selecin, soft wax, paraffin of the Japanese Pharmacopoeia, and the like.

Examples of the solid higher alcohol include myristyl alcohol, cetyl alcohol, cetostearyl alcohol, stearyl alcohol, arachidyl alcohol, behenyl alcohol and the like. Examples of the solid silicone include alkyl-modified silicones and high molecular weight silicone / alkyl co-modified acrylic resins.

Examples of the hydrogenated oil include hydrogenated oil in which the raw material oil is coconut oil, palm oil, beef tallow, and the like. Examples of solid fragrances include menthol and cedrol.

The oil agent is preferably one or more selected from the group of liquid oils and solid fats listed above.

The oil agent preferably has one or more functional groups containing a heteroatom from the viewpoint of obtaining a dispersion liquid of fine particles. Examples of such a functional group include an ester group, an amide group, a hydroxyl group, an ether group, a carbonyl group and the like, and an ester group, an amide group or a hydroxyl group is preferable from the viewpoint of obtaining a dispersion liquid of fine particles.

The content of the oil agent in the oily component is preferably 8% by mass or more, more preferably 10% by mass or more, still more preferably 15% by mass, still more preferably 20% by mass or more from the viewpoint of obtaining a dispersion liquid of fine particles. , More preferably 30% by mass or more, still more preferably 40% by mass or more, and from the same viewpoint, preferably 95% by mass or less, more preferably 90% by mass or less, still more preferably 80% by mass or less. , More preferably 60% by mass or less, still more preferably 50% by mass or less.

When a solid fat is used as the oil agent, the content of the oil agent in the oily component is preferably 30% by mass or less, more preferably 25% by mass or less, from the viewpoint of obtaining a dispersion liquid of fine particles.

<Water-soluble solvent>
The oily component contains an oil agent and one or more water-soluble solvents selected from the group of compounds represented by the following general formulas (I) to (III).

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. P1, p2, p3, q1, q2, q3, r1, r2, and r3 represent the average number of added moles, respectively. ≦ p1 + p2 + p3 ≦ 20, 0 ≦ q1 + q2 + q3 ≦ 10, and 0 ≦ r1 + r2 + r3 ≦ 10, and 1 ≦ p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 ≦ 40. EO, PO, and BO are added randomly or in blocks).

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. S, t, and u represent the average number of moles added. 1 ≦ s ≦ 70, 0 ≦ t ≦ 70, and 0 ≦ u ≦ 10 and 1 ≦ s + t + u ≦ 100. EO, PO, and BO are added in a random or block shape. R ¹ is a hydrocarbon group having 2 or more and 5 or less carbon atoms. .)

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. V1, v2, w1, w2, x1, and x2 represent the average number of moles added. 1 ≦ v1 + v2 ≦ 10, 0, respectively. ≦ w1 + w2 ≦ 9, 0 ≦ x1 + x2 ≦ 9, and 1 ≦ v1 + v2 + w1 + w2 + x1 + x2 ≦ 10. EO, PO, and BO are added in a random or block shape. R ² and R ³ are independent of each other. It is a hydrocarbon group having 1 or more and 4 or less carbon atoms. N is a number of 1 or more and 4 or less.)

In the water-soluble solvent represented by the general formula (I), p1 + p2 + p3 is 1 or more and 20 or less, but from the viewpoint of obtaining a dispersion liquid of fine particles, it is preferably 3 or more, more preferably 5 or more, still more preferably. It is 6 or more, and from the same viewpoint, it is preferably 15 or less, more preferably 10 or less.

Although q1 + q2 + q3 is 0 or more and 10 or less, it is preferably 1 or more, more preferably 3 or more, still more preferably 4 or more, and preferably from the same viewpoint, from the viewpoint of obtaining a dispersion liquid of fine particles. It is 8 or less, more preferably 6 or less.

r1 + r2 + r3 is 0 or more and 10 or less, but is preferably 1 or more, more preferably 2 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and preferably 6 or less, more preferably 6 or less from the same viewpoint. It is 4 or less.

p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 is 1 or more and 40 or less, but is preferably 5 or more, more preferably 10 or more, still more preferably 12 or more, and preferably from the same viewpoint, from the viewpoint of obtaining a dispersion liquid of fine particles. It is 30 or less, more preferably 20 or less.

EO, PO, and BO are added in a random or block shape, but from the viewpoint of obtaining a dispersion of fine particles, EO and PO are added in a random or block shape, and BO is in a block shape at the end. One or more water-soluble solvents selected from the group of compounds represented by the following general formula (IV) added to the above are preferable.

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. P1, p2, p3, q1, q2, q3, r1, r2, and r3 represent the average number of added moles, respectively. ≦ p1 + p2 + p3 ≦ 20, 1 ≦ q1 + q2 + q3 ≦ 10, 1 ≦ r1 + r2 + r3 ≦ 10, and 3 ≦ p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 ≦ 40. EO and PO are added in a random or block shape.)

In the water-soluble solvent represented by the general formula (IV), p1 + p2 + p3 is 1 or more and 20 or less, but from the viewpoint of obtaining a dispersion liquid of fine particles, it is preferably 3 or more, more preferably 5 or more, still more preferably. It is 6 or more, and from the same viewpoint, it is preferably 15 or less, more preferably 10 or less.

Although q1 + q2 + q3 is 1 or more and 10 or less, it is preferably 3 or more, more preferably 4 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and preferably 8 or less, more preferably 8 or less from the same viewpoint. It is 6 or less.

r1 + r2 + r3 is 1 or more and 10 or less, but is preferably 2 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and is preferably 6 or less, more preferably 4 or less from the same viewpoint.

p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 is 3 or more and 40 or less, but is preferably 5 or more, more preferably 10 or more, still more preferably 12 or more, and preferably from the same viewpoint, from the viewpoint of obtaining a dispersion liquid of fine particles. It is 30 or less, more preferably 20 or less.

In the water-soluble solvent represented by the general formula (II), s is 1 or more and 70 or less, but from the viewpoint of obtaining a dispersion liquid of fine particles, it is preferably 2 or more, more preferably 5 or more, still more preferably. It is 10 or more, more preferably 15 or more, even more preferably 25 or more, still more preferably 28 or more, and from the same viewpoint, preferably 50 or less, more preferably 40 or less, still more preferably 35 or less. Even more preferably, it is 32 or less.

When a solid fat is used as the oil agent, s is more preferably 10 or less, still more preferably 3 or less, from the viewpoint of obtaining a dispersion liquid of fine particles.

t is 0 or more and 70 or less, but from the viewpoint of obtaining a dispersion liquid of fine particles, t is preferably 1 or more, more preferably 5 or more, still more preferably 10 or more, still more preferably 15 or more, still more preferably 25. The above is even more preferably 28 or more, and from the same viewpoint, it is preferably 50 or less, more preferably 40 or less, still more preferably 35 or less, and even more preferably 32 or less.

When a solid fat is used as the oil agent, t is more preferably 10 or less, still more preferably 5 or less, still more preferably 1 or less from the viewpoint of obtaining a dispersion liquid of fine particles.

u is 0 or more and 10 or less, but is preferably 5 or less, more preferably 1 or less, and further preferably 0 from the viewpoint of obtaining a dispersion liquid of fine particles.

Although s + t + u is 1 or more and 100 or less, it is preferably 2 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and from the same viewpoint, it is preferably 80 or less, more preferably 70 or less, still more preferably. It is 64 or less.

When a solid fat is used as the oil agent, s + t + u is preferably 20 or less, more preferably 10 or less, and further preferably 3 or less from the viewpoint of obtaining a dispersion liquid of fine particles.

EO, PO, and BO are added in a random or block form.

The carbon number of R ¹ is 2 or more and 5 or less, but is preferably 4 or less from the viewpoint of obtaining a dispersion liquid of fine particles.

In the water-soluble solvent represented by the general formula (III), v1 + v2 is 1 or more and 10 or less, but from the viewpoint of obtaining a dispersion liquid of fine particles, it is preferably 1 or more, more preferably 2 or more, still more preferably. It is 3 or more, and from the same viewpoint, it is preferably 10 or less, more preferably 7, and further preferably 5 or less.

Although w1 + w2 is 0 or more and 9 or less, it is preferably 5 or less, more preferably 1 or less, and further preferably 0 from the viewpoint of obtaining a dispersion liquid of fine particles.

Although x1 + x2 is 0 or more and 9 or less, it is preferably 5 or less, more preferably 1 or less, and further preferably 0 from the viewpoint of obtaining a dispersion liquid of fine particles.

v1 + v2 + w1 + w2 + x1 + x2 is 1 or more and 10 or less, but is preferably 2 or more, more preferably 3 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and preferably 7 or less, more preferably 7 or less from the same viewpoint. It is 5 or less.

EO, PO, and BO are added in a random or block form.

The carbon number of R ² and R ³ is 1 or more and 4 or less, but is preferably 2 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and is preferably 3 or less from the same viewpoint.

n is 1 or more and 4 or less, but is preferably 2 or more from the viewpoint of obtaining a dispersion liquid of fine particles, and is preferably 3 or less from the same viewpoint.

The water-soluble solvent is one or more selected from the group of compounds represented by the general formulas (I) to (III), but from the viewpoint of obtaining a dispersion liquid of fine particles, the general formula (I) It is preferable that the compound is one or more selected from the group of compounds represented by (III).

The content of the water-soluble solvent in the oily component is preferably 4% by mass or more, more preferably 10% by mass or more, still more preferably 20% by mass or more, still more preferably 30 from the viewpoint of obtaining a dispersion liquid of fine particles. It is mass% or more, more preferably 40% by mass or more, and from the same viewpoint, preferably 90% by mass or less, more preferably 80% by mass or less, still more preferably 75% by mass or less, still more preferably 70. It is mass% or less, more preferably 60% by mass or less, still more preferably 50% by mass or less.

The mass ratio of the content of the water-soluble solvent to the content of the oil agent in the oil-based component (water-soluble solvent / oil agent) is preferably 0.1 or more, more preferably 0.2, from the viewpoint of obtaining a dispersion liquid of fine particles. The above is more preferably 0.3 or more, still more preferably 0.5 or more, still more preferably 0.8 or more, and from the same viewpoint, preferably 9 or less, more preferably 8 or less, still more preferable. Is 5 or less, more preferably 3.5 or less, still more preferably 2 or less, still more preferably 1.5 or less, still more preferably 1.2 or less.

<Surfactant>
The oily component further contains at least one of the surfactant precursor and the surfactant precursor that forms the surfactant when combined with the surfactant and the aqueous component. Therefore, the oily component may contain only the surfactant, may contain only the surfactant precursor, or may further contain both of them.

Examples of the surfactant include a nonionic surfactant, an anionic surfactant, and a cationic surfactant.

Examples of the nonionic surfactant include polyoxyethylene hydrogenated castor oil, polyoxyethylene castor oil, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene glycerin fatty acid ester, and polyoxyethylene fatty acid. Oxyethylene ether ester type nonionic surfactant; polyoxyethylene ether type nonionic surfactant such as polyoxyethylene alkyl ether and polyoxyethylene alkyl phenyl ether; sorbitan fatty acid ester, sucrose fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid Polyhydric alcohol fatty acid ester-type nonionic surfactant such as ester; Polyvalent alcohol alkyl ether type nonionic surfactant such as alkyl glycoside; Nitrogen-containing nitrogen-containing fatty acid monoalkanolamide, polyoxyethylene alkylamine, alkylpolyoxyethylene fatty acid amide, etc. Examples include type nonionic surfactants.

Among these, nonionic surfactants are polyoxyethylene ether ester type nonionic surfactants, polyoxyethylene ether ester type nonionic surfactants, and polyoxyethylene ether type nonionic surfactants from the viewpoint of obtaining a dispersion of fine particles. One or more selected from activators, polyhydric alcohol fatty acid ester type nonionic surfactants, polyhydric alcohol alkyl ether type nonionic surfactants and nitrogen-containing nonionic surfactants are preferable, and polyoxyethylene ether ester type One or more selected from nonionic surfactants are more preferable, one or more selected from polyoxyethylene hydrogenated castor oil and polyoxy fatty acid is further preferable, and one selected from polyoxyethylene hydrogenated castor oil. Alternatively, two or more types are more preferable.

The average number of moles of polyethylene oxide added to the polyethylene-hardened castor oil is preferably 1 mol or more, more preferably 10 mol or more, still more preferably 20 mol or more, from the viewpoint of obtaining a dispersion liquid of fine particles, and the same viewpoint. Therefore, it is preferably 100 mol or less, more preferably 70 mol or less, still more preferably 50 mol or less, still more preferably 30 mol or less.

The HLB of the nonionic surfactant is preferably 7 or more, more preferably 8 or more, still more preferably 9 or more, still more preferably 10 or more, still more preferably 12 or more, from the viewpoint of obtaining a dispersion of fine particles. Also, from the same viewpoint, it is preferably 20 or less, more preferably 18 or less, still more preferably 16 or less, still more preferably 15 or less. The HLB is obtained based on the formula described in "Emulsification / Solubilization Technology" Engineering Book Co., Ltd. (Showa 59-5-20) p.8-12. More specifically, in the case of a polyhydric alcohol fatty acid ester type nonionic surfactant, the formula: [HLB] = 20 (1-S / A) (in the formula, S is the saponification value of the ester and A is the acid of the fatty acid. It is calculated based on (indicating the value).

In the case of polyoxyethylene ether ester type nonionic surfactant, it is based on the formula: [HLB] = (E + P) / 5 (in the formula, E indicates ethylene oxide content (mass%) and P indicates alcohol content (mass%)). Is required.

In the case of polyoxyethylene alkyl ether, it is obtained based on the formula: [HLB] = E / 5 (in the formula, E is the same as described above). Here, the acid value and the saponification value can be determined by JIS K0070-1992.

In the case of nonionic surfactants other than these, the formula: [HLB] = 7 + 11.71 log (Mw / Mo) (in the formula, Mw is the molecular weight of the hydrophilic group of the surfactant, and Mo is the hydrophobic group of the surfactant. The molecular weight and log are determined based on (the base indicates a logarithm of 10).

When two types of surfactants A and B having different HLBs are used in combination as the nonionic surfactants, assuming that the respective HLBs are HLB _A and HLB _B , the HLB of the nonionic surfactant in which both are mixed is each mass fraction (mass%) _W a, when a _{W B,} wherein: based on the [HLB] _{= [(W a × HLB a} ) + (W B × HLB B)] ÷ (W a + W B) Is required. Further, when three or more kinds of surfactants are used in combination as the nonionic surfactant, the HLB of the nonionic surfactant in which they are mixed can be obtained in the same manner as described above.

Examples of the anionic surfactant include sulfate ester-type anionic surfactants such as alkyl sulfates, alkenyl sulfates, polyoxyalkylene alkyl ether sulfates, and polyoxyalkylene alkenyl ether sulfates; alkylbenzene sulfonates. , Sulfosulfate alkyl ester salt, polyoxyalkylene sulfosuccinic acid alkyl ester salt, secondary alkyl sulfonate, α-olefin sulfonic acid, α-sulfo fatty acid ester salt, acyl acetylate, N-acyl-N-methyl taurine salt Sulfonic acid type anionic surfactants such as; carboxylic acid type anionic surfactants such as fatty acid salts, ether carboxylates, alkenyl succinates, N-acyl amino acid salts; alkyl phosphate ester salts, polyoxyalkylene alkyl ether phosphorus Examples thereof include phosphoric acid ester type anionic surfactants such as acid ester salts.

Of these, the anionic surfactant is preferably a carboxylic acid type anionic surfactant, more preferably a fatty acid salt or an alkyl ether carboxylate, and even more preferably a fatty acid salt, from the viewpoint of obtaining a dispersion of fine particles.

The number of carbon atoms of the fatty acid salt is preferably 8 or more, more preferably 12 or more, still more preferably 16 or more from the viewpoint of obtaining a dispersion of fine particles, and preferably 22 or less, more preferably 20 or more from the same viewpoint. It is as follows.

The alkyl chain of the fatty acid salt is preferably a straight chain from the viewpoint of obtaining a dispersion of fine particles.

Specific examples of the fatty acid salt include salts of coconut oil fatty acid, oleic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid and the like.

Of these, the fatty acid salt is preferably a sodium salt or potassium salt of coconut oil fatty acid, oleic acid, lauric acid, or myristic acid, and a sodium salt of coconut oil fatty acid or oleic acid, from the viewpoint of obtaining a dispersion of fine particles. Alternatively, a potassium salt is more preferable, a sodium salt or a potassium salt of oleic acid is further preferable, and potassium oleate is even more preferable.

Examples of the cationic surfactant include a quaternary ammonium salt, a pyridinium salt, a tertiary amine or a secondary having a hydrocarbon group having 12 to 28 carbon atoms which may be partitioned by an amide group, an ester group or an ether group. Examples include mineral acid of amines or salts of organic acids. Further, as the tertiary amine or the secondary amine, a compound represented by the following general formula (V) can be mentioned from the viewpoint of obtaining a dispersion liquid of fine particles.

(R ⁴ represents a linear or branched hydrocarbon group having 1 to 22 carbon atoms which may be substituted with a hydroxyl group, and R ⁵ , R ⁶ , R ⁷ , R ⁸ and R ⁹ are the same or different and represent a hydrogen atom or a hydroxyl group substituted by carbon atoms and optionally 1 to 22 hydrocarbon group, X is -O- or -CO-O-(where carbonyl group is combined with R ⁴ To).)

Here, In the formula (V), the carbon number of R ⁴ is, from the viewpoint of obtaining a dispersion of fine particles, preferably 8 or more, more preferably 12 or more, more preferably 18 or more, same From the viewpoint of, it is preferably 22 or less, more preferably 20 or less. R ⁵ , R ⁶ , R ⁷ , R ⁸ and R ⁹ are preferably hydrogen atoms from the viewpoint of availability of a cationic surfactant and the viewpoint of obtaining a dispersion liquid of fine particles. X is preferably —O— from the viewpoint of availability of a cationic surfactant and the viewpoint of obtaining a dispersion liquid of fine particles.

Specifically, examples of the quaternary ammonium salt include monolong-chain alkyltrimethylammonium salts such as cetyltrimethylammonium salt, stearyltrimethylammonium salt, behenyltrimethylammonium salt, and octadesiloxypropyltrimethylammonium salt, and distearyldimethyl. Examples thereof include dilong-chain alkyldimethylammonium salts such as ammonium salts and diisotetradecyldimethylammonium salts. Examples of the tertiary amine salt include stearyldimethylamine, behenyldimethylamine, octadecyloxypropyldimethylamine, dimethylaminopropylstearic acid amide hydrochloride, and monolong-chain alkyldimethylamine salts such as citric acid or lactate. Can be mentioned. Examples of the secondary amine salt include 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol or 1- (2-hydroxyethylamino) -3- (12-hydroxystearyloxy) -2. -Amine salts such as propanol hydrochloride, glutamate, citric acid, or lactate can be mentioned.

Among these, the cationic surfactant may have 12 or more and 28 or less carbon atoms which may be separated by an amide group, an ester group or an ether group from the viewpoint of obtaining a dispersion liquid of fine particles by using an oil agent of a liquid oil. A quaternary ammonium salt having a hydrocarbon group is preferable, a di-long chain alkyldimethylammonium salt is more preferable, and a di-long chain alkyldimethylammonium chloride is further preferable.

The carbon number of each alkyl group of the dilong-chain alkyldimethylammonium salt is preferably 8 or more, more preferably 12 or more, still more preferably 16 or more from the viewpoint of obtaining a dispersion of fine particles, and from the same viewpoint. It is preferably 22 or less, more preferably 20 or less.

The carbon number of each alkyl group of the dilong-chain alkyldimethylammonium salt may be the same or different, but the same is preferable from the viewpoint of obtaining a dispersion liquid of fine particles.

The cationic surfactant is a salt of 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol and 1-(from the viewpoint of obtaining a dispersion of fine particles using a solid fat oil agent. A salt of 2-hydroxyethylamino) -3- (12-hydroxystearyloxy) -2-propanol is preferable, and a salt of 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol is more preferable.

Examples of the surfactant precursor that neutralizes to form an anionic surfactant include carboxylic acids and sulfonic acids that form the anionic surfactant ^{by using Na +} and K ^{+ contained in the aqueous component as counterions.} Examples include phosphoric acid ester. Of these, the preferred surfactant precursor is one that forms the preferred carboxylic acid type anionic surfactant from the viewpoint of obtaining a dispersion of fine particles, and more preferably the preferred fatty acid salt. , Or an alkyl ether carboxylate, and more preferably the above-mentioned fatty acid salt.

Examples of the surfactant precursor that neutralizes to form a cationic surfactant include an amine compound that reacts with an acid component contained in an aqueous component to form the cationic surfactant. Of these, from the viewpoint of obtaining a dispersion liquid of fine particles by using an oil agent of a liquid oil, the one forming the above-mentioned preferable quaternary ammonium salt is preferable, and the above-mentioned preferable di-long chain alkyldimethylammonium salt is formed. Those forming the above-mentioned di-long chain alkyldimethylammonium chloride are more preferable. From the viewpoint of obtaining a dispersion of fine particles using a solid fat oil, those forming a salt of 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol are preferable, and 1- (2-(2-hydroxyethylamino) -3-isostearyloxy-2-propanol is preferable. Those that form the glutamate of 2-hydroxyethylamino) -3-isostearyloxy-2-propanol are more preferred.

The surfactant may be one or more selected from the group of nonionic surfactants, anionic surfactants, and cationic surfactants listed above from the viewpoint of obtaining a dispersion liquid of fine particles. preferable. Nonionic surfactants are preferable from the viewpoint that the dispersibility is not easily affected by pH, and anionic surfactants are preferable from the viewpoint of the stability of the dispersion, and the affinity for the skin when applied to the skin. From the viewpoint of, a cationic surfactant is preferable.

The content of the surfactant and the surfactant precursor in the oily component is preferably 30% by mass or less, more preferably 20% by mass or less, and further, from the viewpoint of obtaining a dispersion liquid of fine particles with a small amount of the surfactant. It is preferably 15% by mass or less, more preferably 12% by mass or less, still more preferably 10% by mass or less, and preferably 0.5% by mass or more from the viewpoint of dispersing the oily component in the aqueous component. It is preferably 2% by mass or more, more preferably 4% by mass or more, still more preferably 6% by mass or more, still more preferably 8% by mass or more.

The aqueous component may also contain a surfactant, but the content of the aqueous component is preferably 2% by mass or less, more preferably 1% by mass or less from the viewpoint of obtaining a dispersion of fine particles. More preferably, it is 0.5% by mass or less, may be substantially 0% by mass, or may be 0.1% by mass or more.

<Self-emulsifying property>
The oily component preferably has self-emulsifying property with respect to the aqueous component from the viewpoint of obtaining a dispersion liquid of fine particles. Here, the presence or absence of self-emulsifying property can be determined as follows.

First, 90 ml of the aqueous component and 10 ml of the oil component are weighed. Then, the oily component is charged into the aqueous component at a rate of 10 ml / min using an injection needle (outer diameter: 1.58 mm, inner diameter: 0.25 mm). At this time, the tip of the injection needle is immersed in the aqueous component, and stirring is not performed. After adding the entire amount of the oil component, a laser diffraction / scattering type particle size distribution measuring device, for example, LA-910 (manufactured by HORIBA, Ltd.) is used, and the average of the volume standard of the particles in the dispersion liquid by the laser scattering / diffraction method. Measure the dispersed particle size. Then, when the measured average dispersed particle size is 0.25 mm or less in the inner diameter of the injection needle, it is judged that there is "self-emulsifying property", while when it is larger than 0.25 mm, it is judged that "it is not self-emulsifying". to decide.

(Merge of aqueous component and oil component)
In the merging step, the flow rate of the aqueous component before merging is preferably 0.1 L / h or more, more preferably 1 L / h or more, and further, from the viewpoint of enhancing the effect of turbulent flow and obtaining a dispersion liquid of fine particles. It is preferably 2 L / h or more, more preferably 2.5 L / h or more, and preferably 300 L / h or less from the viewpoint of improving the mixing property after merging to obtain a dispersion liquid of fine particles. It is preferably 200 L / h or less, more preferably 100 L / h or less, still more preferably 30 L / h or less, still more preferably 20 L / h or less, still more preferably 10 L / h or less, still more preferably 4 L / h or less. , More preferably 3 L / h or less. The flow rate of the oily component before merging is preferably 0.01 L / h or more, more preferably 0.1 L / h or more, and further, from the viewpoint of enhancing the effect of turbulent flow and obtaining a dispersion liquid of fine particles. It is preferably 0.2 L / h or more, and is preferably 150 L / h or less, more preferably 100 L / h or less, from the viewpoint of improving the mixing property after merging to obtain a dispersion liquid of fine particles. It is still more preferably 50 L / h or less, still more preferably 2 L / h or less, still more preferably 1 L / h or less, still more preferably 0.5 L / h or less, still more preferably 0.3 L / h or less.

In the merging step, the flow rate ratio of the aqueous component to the oily component (flow rate of the aqueous component / flow rate of the oily component) before merging is preferably 1 or more, more preferably 2 or more from the viewpoint of obtaining a dispersion liquid of fine particles. Yes, more preferably 5 or more, and from the viewpoint of increasing the content of the oil agent in the dispersion, preferably 200 or less, more preferably 100 or less, still more preferably 50 or less, still more preferably 25 or less, still more. It is preferably 15 or less. The mixed mass ratio of the aqueous component and the oil component is preferably 1 or more, more preferably 2 or more, still more preferably 5 or more, from the viewpoint of obtaining an O / W type dispersion having a small average particle size of the particles. Further, from the viewpoint of increasing the content of the oil agent in the dispersion liquid, it is preferably 200 or less, more preferably 100 or less, still more preferably 50 or less, still more preferably 25 or less, still more preferably 15 or less.

In the merging step, the temperature of the aqueous component before merging is preferably 5 ° C. or higher, more preferably 10 ° C. or higher, still more preferably 15 ° C. or higher, and preferably 95 ° C. or lower, more preferably 90 ° C. or lower. It is still more preferably 85 ° C. or lower, even more preferably 60 ° C. or lower, and even more preferably 50 ° C. or lower. The temperature of the oily component before merging is preferably 5 ° C. or higher, more preferably 10 ° C. or higher, preferably 95 ° C. or lower, more preferably 90 ° C. or lower, still more preferably 85 ° C. or lower, still higher. It is preferably 50 ° C. or lower. The temperature of the aqueous component and the temperature of the oil component before merging may be the same or different, but are preferably the same from the viewpoint of obtaining a dispersion liquid of fine particles.

In the merging step, the viscosities of both the aqueous component and the oily component before merging are preferably 0.1 mPa · s or more, more preferably 0.1 mPa · s or more at each temperature at the time of merging from the viewpoint of good liquid feeding. It is 1 mPa · s or more, more preferably 5 mPa · s or more, and from the viewpoint of obtaining a dispersion liquid of fine particles, it is preferably 1000 mPa · s or less, more preferably 500 mPa · s or less, still more preferably 300 mPa · s or less. Is. The viscosity of the aqueous component and the viscosity of the oily component may be the same or different. For the viscosities of the aqueous component and the oil component, a Brookfield type (B type) rotational viscometer was used, and the rotor No. 3 is used as standard (if the viscosity cannot be measured, the rotor is changed to No. 1, 2 or 4), and the measurement is performed under the conditions of a rotation speed of 30 r / min and a measurement time of 1 minute.

In the merging step, the mode of merging the aqueous component and the oily component is not particularly limited.

Examples of the collision mode (angle) when the aqueous component and the oil component are merged include a mode in which both are head-on collided and merged, a mode in which one is collided from a direction orthogonal to the other and merged, and one is the other. There are a mode in which one is collided diagonally from the rear and merged, a mode in which one is collided with the other diagonally from the front and merged, and a mode in which one is brought into contact along the other to merge.

Further, as an aspect (number, etc.) of the merging method when the aqueous component and the oily component are merged, for example, both are collided from a plurality of directions to be merged, and one is made to collide with the other from a plurality of directions. There is a mode of merging with each other, and a mode of colliding one of them from the entire circumference of the other to join them. In the embodiment in which both are collided from a plurality of directions to merge, it is preferable to collide from two or more directions, respectively, from the viewpoint of obtaining a dispersion liquid of fine particles, and there is no particular upper limit, but productivity. From the viewpoint of the above, it is preferable to collide from four or less directions. In the embodiment in which one is made to collide with the other from a plurality of directions and merged, it is preferable that one is made to collide with the other from two or more directions, and there is no particular upper limit, but from the viewpoint of productivity, one is used. It is preferable to collide with the other from four or less directions.

Of these, as a mode of collision at the time of merging, from the viewpoint of obtaining a dispersion liquid of fine particles, a mode in which an oily component collides with an aqueous component from a direction orthogonal to the water component or diagonally behind is preferable, and a mode of the merging method From the viewpoint of obtaining a dispersion liquid of fine particles, it is preferable that the oily components collide with each other from the entire circumference of the aqueous components and merge.

[Pore distribution step]
In the pore flow step, one or two of the aqueous component before merging in the merging step, the oily component before merging in the merging step, and the fluid after merging the aqueous component and the oily component in the merging step. The above is circulated in the pores. Here, "before merging" means just before merging.

Therefore, it may be the first aspect in which neither the aqueous component before merging nor the oily component before merging is circulated in the pores, and only the fluid after merging is circulated in the pores. A second embodiment may be used in which the oily component before merging is not circulated in the pores, and the aqueous component before merging and the fluid after merging are each circulated in the pores. It may be a third embodiment in which the aqueous component before merging is not circulated in the pores and the oily component before merging and the fluid after merging are each circulated in the pores.

Further, it may be a fourth aspect in which the aqueous component before merging and the oily component before merging are each circulated in the pores, and the fluid after merging is not circulated in the pores. A fifth aspect may be in which only the aqueous component before merging is circulated in the pores and neither the oily component before merging nor the fluid after merging is circulated in the pores. A sixth embodiment may be in which only the oily component before merging is circulated in the pores and neither the aqueous component before merging nor the fluid after merging is circulated in the pores.

Further, it may be the seventh aspect in which any of the aqueous component before merging, the oily component before merging, and the fluid after merging are circulated in the pores.

Of these, from the viewpoint of obtaining a dispersion liquid of fine particles, the first to third and seventh aspects in which the fluid after the merging of the aqueous component and the oily component in the merging step is circulated through the pores are preferable.

The cross-sectional shape of the pores is preferably circular from the viewpoint of obtaining a dispersion of fine particles, but semicircular, elliptical, semi-elliptical, square, rectangular, trapezoidal, parallelogram, star-shaped, It may be non-circular such as irregular shape. The cross-sectional shape of the pores is preferably the same along the length direction.

The direction in which the pores extend is preferably the same as the flow direction of the aqueous component and / or the flow direction of the oil component from the viewpoint of obtaining a dispersion liquid of fine particles.

The pore diameter of the pores is 0.1 mm or more and 3 mm or less, but is preferably 0.2 mm or more from the viewpoint of obtaining high productivity, and from the viewpoint of obtaining a dispersion liquid of fine particles by the generation of turbulent flow. It is preferably 1.0 mm or less, more preferably 0.50 mm or less, more preferably 0.45 mm or less, still more preferably 0.30 mm or less, still more preferably 0.25 mm or less. Here, the pore diameter is the diameter when the cross-sectional shape of the pore is circular, but the equivalent hydraulic diameter (4 × flow path area / cross section) when the cross-sectional shape of the pore is non-circular. Long).

The length of the pores is preferably 0.05 mm or more, more preferably 0.1 mm or more, still more preferably 0.3 mm or more, from the viewpoint of increasing the pressure loss and increasing the mixing property of the aqueous component and the oily component. Further, from the viewpoint of obtaining a dispersion liquid of fine particles by instantly mixing the aqueous component and the oil component after merging, the mixture is preferably 5 mm or less, more preferably 3 mm or less, more preferably 2 mm or less, still more preferably 1 mm or less. , More preferably 0.8 mm or less.

Flow area of pores, in view of preventing to bring the fault to equipment caused excessive pressure loss, preferably 0.01 mm ² or more, more preferably 0.03 mm ² or more, the pressure loss From the viewpoint of increasing the mixing property of the aqueous component and the oily component, it is preferably 7 mm ² or less, more preferably 2 mm ² or less, further preferably 1 mm ² or less, ^{still more preferably 0.5 mm 2} or less, still more preferably 0. .15Mm ² or less, even more preferably 0.1 mm ² or less, even more preferably 0.05 mm ² or less.

The ratio of the pore length to the pore diameter (length / pore diameter) is preferably 0.15 or more, more preferably 0.2 or more, still more preferably 0.2 or more, from the viewpoint of obtaining a dispersion liquid of fine particles by the generation of turbulent flow. Is 0.5 or more, more preferably 1 or more, still more preferably 2 or more, and from the same viewpoint, preferably 40 or less, more preferably 20 or less, still more preferably 10 or less, still more preferably. It is 5 or less, more preferably 3 or less.

In the pore circulation step, as a method of circulating the fluid after the merging of the aqueous component and the oily component in the merging step into the pores, the aqueous component and the oily component are once merged in the liquid reservoir, and they are mixed. The fluid may be circulated through the pores, but from the viewpoint of obtaining a dispersion liquid of fine particles, a confluence portion of the aqueous component and the oil component is provided immediately before the pores or is confluent within the pores. Is preferable.

In the pore flow step, the flow rate when the fluid after the merging of the aqueous component and the oil component in the merging step is circulated through the pores is preferably 0 from the viewpoint of increasing the pressure loss and obtaining a dispersion liquid of fine particles. .1 L / h or more, more preferably 1 L / h or more, further preferably 2.0 L / h or more, still more preferably 2.5 L / h or more, and from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferably 300 L / h or less, more preferably 200 L / h or less, still more preferably 100 L / h or less, still more preferably 30 L / h or less, still more preferably 15 L / h or less, still more preferably 10 L / h or less. It is even more preferably 5 L / h or less, and even more preferably 3.5 L / h or less.

In the pore circulation step, it is preferable to distribute the aqueous component and the oil component in the pores under turbulent flow conditions from the viewpoint of obtaining a dispersion liquid of fine particles. The Reynolds number at this time is preferably 1000 or more, more preferably 2000 or more, and preferably 150,000 or less from the viewpoint of enhancing the stirring efficiency of the aqueous component and the oily component after pore circulation. , More preferably 100,000 or less. Here, the Reynolds number is a value of the average flow velocity u (m / s) in the pores, the pore diameter d (m), the viscosity μ (Pa · s) of the fluid, and the density ρ (kg / m ³ ) of the fluid. It can be obtained by the general Reynolds number calculation formula (Reynolds number Re = duρ / μ) of the pipe flow using.

From the viewpoint of obtaining a dispersion liquid of fine particles in the pore flow step, it is preferable to allow the fluid after the merging of the aqueous component and the oil component in the merging step to flow through the pores and flow out to the flow path expansion portion. As a result, turbulent flow due to both components is generated, so that the particles can be miniaturized. In particular, when the fluid after the merging of the aqueous component and the oil component is circulated through the pores having a pore diameter of 0.1 mm or more and 3 mm or less, both components are agitated by turbulent flow in the flow path expansion region after the pore circulation. As a result, the surfactant is more efficiently supplied from the oily component to the oil-water interface. As a result, a dispersion of fine particles can be obtained with a small amount of surfactant.

The cross-sectional shape of the flow path of the flow path expansion portion is preferably circular from the viewpoint of obtaining a dispersion liquid of fine particles, but is semi-circular, elliptical, semi-elliptical, square, rectangular, trapezoidal, or parallelogram. It may be non-circular, such as a shape, a star, or an indefinite shape. The cross-sectional shape of the flow path enlarged portion is preferably the same shape along the length direction, but may include different shapes along the length direction.

From the viewpoint of obtaining a dispersion liquid of fine particles, the flow path expanding portion is preferably formed so as to expand in a cone shape from the pores to the portion having the maximum flow path diameter. The cone enlargement angle is preferably 90 ° or more, more preferably 100 ° or more, still more preferably 110 ° or more, and preferably 180 ° or less, more preferably 170 ° or less, still more preferably 150 ° or less. Even more preferably, it is 130 ° or less.

The maximum flow path diameter of the flow path expanding portion is preferably 3 times or more, more preferably 5 times or more, and preferably 50 times or less, more than the pore size of the pores from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferably 40 times or less, more preferably 20 times or less, and even more preferably 15 times or less. Here, the maximum diameter of the flow path expansion portion is the diameter when the cross-sectional shape of the flow path is circular, but is the equivalent hydraulic diameter when the cross-sectional shape of the flow path is non-circular.

In the pore circulation step, the dispersion liquid after flowing through the pores is cooled as needed. As a result, when the oil agent is a liquid oil, a dispersion liquid (emulsion) in which the liquid particles are dispersed is obtained, and when the oil agent is a solid fat, a dispersion liquid in which the solid particles are dispersed is obtained.

The average particle size of the particles in the produced dispersion is preferably 1/100 or less, more preferably 1/200 or less, still more preferably 1/300 of the pore size of the pores from the viewpoint of obtaining a dispersion of fine particles. Below, even more preferably 1/500 or less, even more preferably 1/900 or less, even more preferably 1/3000 or less, even more preferably 1/5000 or less, even more preferably 1/7000 or less, even more preferably. Is 1/8000 or less, and from the viewpoint of productivity, it is preferably 1/20000 or more, more preferably 1/15000 or more, still more preferably 1/11000 or more, still more preferably 1/10000 or more, more preferably. Is 1/9000 or more, more preferably 1/8000 or more, still more preferably 1/6000 or more, still more preferably 1/3000 or more, still more preferably 1/2000 or more, still more preferably 1/1700 or more. Is. Specifically, the average particle size of the particles in the dispersion is preferably 10 μm or less, more preferably 5 μm or less, still more preferably 3 μm or less, still more preferably 2 μm or less, still more, from the viewpoint of the stability of the dispersion. It is preferably 1 μm or less, more preferably 0.5 μm or less, still more preferably 0.3 μm or less, still more preferably 0.15 μm or less, still more preferably 0.1 μm or less, still more preferably 0.05 μm or less. Also, from the viewpoint of productivity, it is preferably 0.02 μm or more, more preferably 0.03 μm or more, still more preferably 0.04 μm or more, still more preferably 0.05 μm or more, still more preferably 0.07 μm or more. , More preferably 0.1 μm or more. Here, the average particle size of the particles in the dispersion is measured by a laser scattering / diffraction method using a laser diffraction / scattering type particle size distribution measuring device, for example, LA-910 (manufactured by Horiba Seisakusho Co., Ltd.). The diameter.

The content of the oil agent in the produced dispersion is preferably 0.5% by mass or more, more preferably 0.6% by mass or more, and more preferably 0.8% by mass from the viewpoint of increasing the content of the oil agent in the dispersion liquid. % Or more, more preferably 1% by mass or more, still more preferably 3% by mass or more, and from the viewpoint of obtaining a dispersion liquid of fine particles, preferably 20% by mass or less, more preferably 15% by mass or less, further. It is preferably 10% by mass or less, more preferably 8% by mass or less, still more preferably 5% by mass or less, still more preferably 2% by mass or less, still more preferably 1.5% by mass or less, still more preferably 1. It is 2% by mass or less.

The content of the water-soluble solvent in the produced dispersion is preferably 0.5% by mass or more, more preferably 1% by mass or more, still more preferably 2% by mass or more, from the viewpoint of obtaining a dispersion of fine particles. It is still more preferably 2.5% by mass or more, still more preferably 3% by mass or more, and from the same viewpoint, it is preferably 20% by mass or less, more preferably 15% by mass or less, still more preferably 10. It is 0% by mass or less, more preferably 8% by mass or less, still more preferably 5% by mass or less, still more preferably 4% by mass or less.

The content of the surfactant in the produced dispersion is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, still more preferably 0.1 from the viewpoint of obtaining a dispersion of fine particles. By mass% or more, more preferably 0.3% by mass or more, even more preferably 0.4% by mass or more, still more preferably 0.6% by mass or more, and from the same viewpoint with a small amount of surfactant. It is preferably 2% by mass or less, more preferably 1.5% by mass or less, and further preferably 1% by mass or less.

The content of water in the produced dispersion is preferably 50% by mass or more, more preferably 70% by mass or more, still more preferably 90% by mass or more, and the same, from the viewpoint of containing an oil agent in the dispersion. From the above viewpoint, it is preferably 99% by mass or less, more preferably 98% by mass or less, still more preferably 97% by mass or less, still more preferably 96% by mass or less, still more preferably 92% by mass or less.

In the dispersion operation of the aqueous component and the oily component in the method for producing the dispersion liquid according to the present embodiment, the segregation index (Xs) obtained by the method described later is determined from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferably 0.15 or less, more preferably 0.1 or less, still more preferably 0.05 or less, still more preferably 0.01 or less, still more preferably 0.0003 or less. There is no particular lower limit, but 0.0001 or more is sufficient, and 0.001 or more may be sufficient.

Here, the segregation index (Xs) indicates the effect of mixing and stirring the aqueous component and the oily component in the method for producing the dispersion according to the present embodiment, and the smaller the value, the higher the mixing property. It is an index that is academically used for the evaluation of mixing performance of mixers, and can be derived from the following equation (iv) using Villermaux / Dushman reaction. Details of this reaction system are described in P. Guichardon and L. Falk, Chemical Engineering Science 55 (2000) 4233-4243.

Specifically, first, 0.171N sulfuric acid and boric acid buffer are prepared as two aqueous solutions that react by mixing. The composition of the boric acid buffer is 0.045 mol / L of boric acid, 0.045 mol / L of sodium hydroxide, 0.00313 mol / L of potassium iodide, and 0.0156 mol / L of potassium iodide. Then, when these two liquids are mixed, the following neutralization reaction (A) and the redox reaction (B) produced by iodine proceed at the same time. The two liquids are mixed under the condition that the alkali becomes excessive in the state after mixing.

According to the above-mentioned method for producing a dispersion liquid according to the present embodiment, a surfactant is formed when the oil-based component is mixed with an oil agent, a water-soluble solvent having a specific structure, a surfactant, and the aqueous component. One or two or more of the aqueous component before merging, the oily component before merging, and the fluid after merging them, which contain at least one of the surfactant precursors to be merged, have a pore size of 0. . By circulating in pores of 1 mm or more and 3 mm or less, a dispersion liquid in which fine particles are dispersed can be produced.

FIG. 1 shows an example of a dispersion liquid production system A that can be used in the dispersion liquid production method according to the present embodiment.

The dispersion liquid manufacturing system A is composed of a micromixer 100 having a first configuration and an accessory portion such as a fluid supply system.

2 and 3 show the micromixer 100 having the first configuration. In the micromixer 100 having the first configuration, neither the aqueous component before merging nor the oily component before merging is circulated in the pores, and only the fluid after merging is passed through the pores. The dispersion is produced according to the mode of distribution to.

The micromixer 100 having the first configuration includes a fluid flow path portion 110, a fluid merging and condensing section 120 continuously provided on the downstream side thereof, and a fluid outflow section 130 continuously provided on the downstream side thereof. And.

The fluid flow path portion 110 has a small diameter pipe 111 and a large diameter pipe 112. The large-diameter pipe 112 accommodates the small-diameter pipe 111, which have a common length direction and are arranged coaxially. As a result, in the fluid flow path portion 110, the first flow path 111a is formed inside the small diameter pipe 111, and the second flow path 112a is formed inside the large diameter pipe 112 and outside the small diameter pipe 111. The first flow path 111a in the small diameter pipe 111 communicates with the aqueous component supply unit 101 provided at one end of the device, and the second flow path 112a in the large diameter tube 112 is provided on the side surface of the device. It communicates with the oil component supply unit 102.

The outer shape of the small-diameter pipe 111 and the cross-sectional shape of the hole are not particularly limited, and are, for example, circular, semicircular, elliptical, semi-elliptical, square, rectangular, trapezoidal, parallelogram, star-shaped, and indefinite. And so on. The cross-sectional shape of the hole of the large-diameter pipe 112 is not particularly limited, and like the small-diameter pipe 111, for example, circular, semicircular, elliptical, semi-elliptical, square, rectangular, trapezoidal, parallelogram, etc. It may be star-shaped, irregular-shaped, or the like. However, it is preferable that both the outer shape and the hole of the small diameter pipe 111 and the cross-sectional shape of the hole of the large diameter pipe 12 are circular. Further, it is preferable that the small diameter pipe 111 and the large diameter pipe 112 are provided so that the cross-sectional shapes are symmetrical and coaxial. Therefore, as shown in FIG. 3, the small-diameter pipe 111 and the large-diameter pipe 112 have a circular cross-sectional shape of the first flow path 111a and a donut-shaped cross-sectional shape of the second flow path 112a. It is preferable that the configuration is provided.

It is preferable that both the outer shape of the small diameter pipe 111 and the cross-sectional shape of the hole have the same shape along the length direction except for the pipe end portion 111b described later. It is preferable that the cross-sectional shape of the hole of the large-diameter pipe 112 is the same along the length direction except for the portion corresponding to the pipe end portion 111b of the small-diameter pipe 111.

When both the outer shape and the cross-sectional shape of the hole of the small diameter tube 111 are circular, the outer diameter D ₁ is preferably 1.6 mm or more, more preferably 2 mm or more, from the viewpoint of obtaining a dispersion liquid of fine particles. Also, from the same viewpoint, it is preferably 25 mm or less, more preferably 15 mm or less, still more preferably 4 mm or less. The inner diameter _{D 2} of the small-diameter pipe 111, i.e., passage diameter of the first flow path 111a, from the viewpoint of obtaining a dispersion of fine particles, preferably 0.8mm or more, more preferably 1mm or more, the same From the viewpoint, it is preferably 20 mm or less, more preferably 10 mm or less, still more preferably 3 mm or less. When the cross-sectional shape of the hole of the large-diameter pipe 112 is circular, the inner diameter D ₃ is preferably 1.8 mm or more, more preferably 4 mm or more, and more preferably 4 mm or more, from the viewpoint of obtaining a dispersion liquid of fine particles. From the same viewpoint, it is preferably 50 mm or less, more preferably 20 mm or less, still more preferably 6 mm or less. Further, the gap Δ of the second flow path 112a between the small diameter pipe 111 and the large diameter pipe 112 is preferably 0.1 mm or more, more preferably 0.3 mm or more, and further, from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferably 0.5 mm or more, more preferably 0.7 mm or more, and from the same viewpoint, it is preferably 12.5 mm or less, more preferably 6 mm or less, still more preferably 1 mm or less.

As shown in FIG. 2, it is preferable that the outer peripheral portion of the pipe end portion 111b on the downstream side of the small diameter pipe 111 is formed in a tapered shape, and the cross-sectional shape in the thickness direction is sharp on the inner peripheral side. It is more preferable that it is formed in a shape.

It is preferable that the gap δ, which is a part of the second flow path 112a formed between the inner wall of the large-diameter pipe 112 and the pipe end portion 111b of the small-diameter pipe 111, is uniform in the fluid flow direction. The gap δ is preferably 0.02 mm or more, more preferably 0.05 mm or more, still more preferably 0.1 mm or more, still more preferably 0.2 mm or more, from the viewpoint of obtaining a dispersion liquid of fine particles. From the same viewpoint, it is preferably 12.5 mm or less, more preferably 6 mm or less, still more preferably 1 mm or less, still more preferably 0.3 mm or less.

The fluid confluence condensing portion 120 is configured with a fluid confluence region 121 in front of the pipe end of the small diameter pipe 111, and pores 122 are continuously perforated in the fluid confluence region 121. In the fluid merging area 121, the aqueous component flowing through the first flow path 111a and the oily component flowing through the second flow path 112a merge, and in the pore 122, the aqueous component and oiliness immediately after merging in the fluid merging area 121. Ingredients are distributed.

The fluid confluence region 121 is not particularly limited, but is formed in a tapered cone shape that converges toward the pores 122, as shown in FIG. 2, from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferable to have. The cone convergence angle θ ₁ is preferably 90 ° or more, more preferably 100 ° or more, still more preferably 110 ° or more, and preferably 180 ° or less, from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferably 170 ° or less, more preferably 130 ° or less. The cone convergence angle θ ₁ is preferably the same as _{the cone enlargement angle θ 2} of the flow path expansion portion 131 described later. The pipe end of the small-diameter pipe 111 in the fluid merging region 121, that is, the distance L from the end of the fluid flow path portion 110 to the pores 122 is preferably 0.02 mm or more from the viewpoint of obtaining a dispersion liquid of fine particles. It is preferably 0.2 mm or more, more preferably 0.3 mm or more, and preferably 20 mm or less, more preferably 3 mm or less, still more preferably 1 mm or less.

The cross-sectional shape of the pore 122, the extending direction, the pore diameter d, the length l, the flow path area s, and the ratio of the length l to the pore diameter d (length l / pore diameter d) are as described above.

The fluid outflow portion 130 includes a flow path expanding portion 131 in front of the pores 122. The fluid flowing through the pores 122 flows out to the flow path expanding portion 131. The flow path expanding portion 131 communicates with the dispersion liquid collecting portion 103 provided at the other end of the device.

The cross-sectional shape and shape of the flow path of the fluid outflow portion 130, the cone enlargement angle θ ₂ , and the maximum flow path diameter D ₄ of the flow path enlargement portion 131 are as described above.

Each of the micromixer 100 may be composed of a plurality of members made of metal, ceramics, resin, or the like, and depending on the combination of these members, the fluid flow path portion 110, the fluid confluence / condensing portion 120, and the fluid confluence / condensing portion 120. The fluid outflow portion 130 may be configured.

In the micromixer 100 having the first configuration, one small diameter tube 111 is housed in the large diameter tube 112, but the present invention is not particularly limited to this, and FIGS. 4A and 4B ), A plurality of small-diameter pipes 111 may be housed in the large-diameter pipe 112.

In this micromixer 100, as shown in FIG. 1, an aqueous component supply pipe 42a extending from the aqueous component storage tank 41a is connected to an aqueous component supply unit 101 communicating with the first flow path 111a. In the water-based component supply pipe 42a, a first pump 43a for circulating the water-based component, a first flow meter 44a for detecting the flow rate of the water-based component, and a first filter 45a for removing impurities of the water-based component are interposed in this order from the upstream side. A first pressure gauge 46a for detecting the pressure of an aqueous component is attached to a portion between the first flow meter 44a and the first filter 45a. Each of the first pump 43a, the first flow meter 44a, and the first pressure meter 46a is electrically connected to the flow controller 47.

An oil-based component supply pipe 42b extending from the oil-based component storage tank 41b is connected to the oil-based component supply unit 102 communicating with the second flow path 112a. A second pump 43b for circulating the oily component, a second flow meter 44b for detecting the flow rate of the oily component, and a second filter 45b for removing impurities of the oily component are interposed in the oily component supply pipe 42b in order from the upstream side. A second pressure gauge 46b for detecting the pressure of the oil component is attached to a portion between the second flow meter 44b and the second filter 45b. Each of the second pump 43b, the second flow meter 44b, and the second pressure meter 46b is electrically connected to the flow controller 47.

The flow rate controller 47 is configured to be able to input the set flow rate and set pressure of the aqueous component, and also incorporates an arithmetic element. The set flow rate information of the aqueous component, the flow rate information detected by the first flow meter 44a, and the flow rate information detected by the first flow meter 44a. The operation of the first pump 43a is controlled based on the pressure information detected by the first pressure gauge 46a. Similarly, the flow rate controller 47 is configured to be able to input the set flow rate and the set pressure of the oil component, and the set flow rate information of the oil component, the flow rate information detected by the second flow meter 44b, and the second pressure meter 46b. The second pump 43b is operated and controlled based on the pressure information detected in.

A dispersion liquid recovery pipe 48 extends from the dispersion liquid recovery unit 103 communicating with the flow path expansion unit 131 and is connected to the dispersion liquid recovery tank 49.

Next, the operation of the dispersion liquid manufacturing system A will be described.

When the dispersion liquid production system A is operated, the first pump 43a passes the aqueous component to be a continuous phase from the aqueous component storage tank 41a via the aqueous component supply pipe 42a, in order, through the first flow meter 44a and the first filter 45a. The fluid flow path portion 110 is continuously supplied to the first flow path 111a of the small diameter pipe 111. The first flow meter 44a sends the detected flow rate information of the aqueous phase to the flow controller 47. Further, the first pressure gauge 46a sends the detected pressure information of the first pressure gauge 46a to the flow controller 47.

The second pump 43b passes the oily component to be the dispersed phase from the oily component storage tank 41b via the oily component supply pipe 42b, and sequentially passes through the second flow meter 44b and the second filter 45b, and has a large diameter of the fluid flow path portion 110. It is continuously supplied to the second flow path 112a between the pipe 112 and the small diameter pipe 111. The second flow meter 44b sends the detected flow rate information of the oil phase to the flow controller 47. Further, the second pressure gauge 46b sends the detected pressure information of the second pressure gauge 46b to the flow controller 47.

The flow rate controller 47 sets the set flow rate of the aqueous component based on the set flow rate information and the set pressure information of the aqueous component, and the flow rate information detected by the first flow meter 44a and the pressure information detected by the first pressure gauge 46a. The operation of the first pump 43a is controlled so that the set pressure is maintained. At the same time, the flow rate controller 47 bases the oil-based component based on the set flow rate information and the set pressure information of the oil-based component, the flow rate information detected by the second flow meter 44b, and the pressure information detected by the second pressure gauge 46b. The operation of the second pump 43b is controlled so that the set flow rate and the set pressure of the above are maintained.

Then, in the micromixer 100, in the fluid flow path portion 110, the aqueous component flows through the first flow path 111a and the oily component flows through the second flow path 112a. At this time, the pressure of the aqueous component is, for example, 0.01 MPa or more and 5 MPa or less. The pressure of the oil component is, for example, 0.01 MPa or more and 5 MPa or less. Then, the flow rate of the aqueous component is set to, for example, 0.05 m / s or more and 2 m / s or less by setting the flow rate and pressure of the aqueous component, and the flow rate of the oil component is set to, for example, 0 by setting the flow rate and pressure of the oil component. It is set to 0.05 m / s or more and 2 m / s or less.

In the fluid merging condensing section 120, the aqueous component and the oily component flowing out from the fluid flow path section 110 merge with the aqueous component in the fluid merging area 121 in a manner in which the oily component collides with the aqueous component from diagonally behind and from the entire circumference thereof. To do. At this time, in the fluid confluence condensing section 120, the flow velocity of the fluid including the aqueous component and the oil component is, for example, 0.05 m / s or more and 2 m / s or less. This flow velocity can be controlled by setting the flow rates and pressures of the aqueous component and the oil component, respectively.

The aqueous component and the oil component merged in the fluid confluence region 121 are mixed in the process of flowing through the pores 122. At this time, the flow conditions of the water-based component and the oil-based component to be merged in the fluid confluence region 121 can be controlled by setting the flow rates and pressures of the water-based component and the oil-based component, respectively.

In the fluid outflow section 130, the fluid containing the aqueous component and the oily component flowing through the pores 122 flows out in the flow path expanding section 131, and the average particle size of the particles is increased by convection mixing between the aqueous component and the oily component. A dispersion having a pore diameter of 1/10 or less of the pores 122 is produced.

From the dispersion liquid recovery unit 103 communicating with the flow path expansion unit 131, the produced dispersion liquid is collected in the dispersion liquid recovery tank 49 via the dispersion liquid recovery pipe 48. At this time, the pressure loss before and after the micromixer 100 is preferably 0.01 MPa or more, more preferably 0.1 MPa or more from the viewpoint of obtaining a dispersion liquid of fine particles, and preferably from the viewpoint of productivity. Is 5 MPa or less, more preferably 3 MPa or less, still more preferably 1 MPa or less, still more preferably 0.7 MPa or less. This pressure loss can be controlled by setting the flow rates and pressures of the aqueous component and the oil component, respectively.

FIG. 5 shows a micromixer 200 having a second configuration. In the micromixer 200 having the second configuration, the dispersion liquid is produced by the above-mentioned seventh aspect, that is, the embodiment in which the aqueous component before merging, the oily component before merging, and the fluid after merging are each circulated in the pores. ..

In the micromixer 200 having the second configuration, a straight pipe portion 210 having one pipe end as an aqueous component supply unit 201 and the other pipe end as an oil component supply unit 202 and a central portion of the straight pipe portion 210 are used. It is composed of a T-shaped pipe that is branched and extends in an orthogonal direction, and the pipe end is a branch pipe portion 220 having a dispersion liquid recovery portion 203. The micromixer 200 having a second configuration with a T-shaped tube has a simple apparatus configuration and is easy to maintain by disassembling and cleaning.

In the straight pipe portion 210, the flow path of the central portion is narrowed, and in the central portion, the aqueous component supply portion 201 side becomes the first flow path 211a, and the oil component supply portion 202 side becomes the second flow path 212a. Each is configured. Therefore, the water-based component supply pipe 42a is connected to the water-based component supply unit 201, and the oil-based component supply pipe 42b is connected to the oil-based component supply unit 202.

The branch pipe portion 220 is formed with pores 222 that extend along the pipe axis and communicate with each other in the straight pipe portion 210. The central portion of the straight pipe portion 210, that is, the inside of the branch portion to the branch pipe portion 220 is configured as a fluid confluence region 221 continuous with the pore 222. Each of the first flow path 211a and the second flow path 212a preferably has a flow path cross-sectional area, that is, a pore area of the same as or about the same as that of the pore 222, and pressure loss can be suppressed to be small. It is preferable that the flow path length, that is, the hole length is also the same as or about the same as the pore 222. The branch pipe portion 220 includes a flow path expansion portion 231 in which the flow path cross-sectional area is continuously expanded in the pores 222. The dispersion liquid recovery pipe 48 is connected to the dispersion liquid recovery unit 203 of the branch pipe portion 220.

The micromixer 200 having the second configuration causes the first liquid of the aqueous component and the second liquid of the oily component to collide head-on and merge with each other, and head toward the fluid merging area 221 of the first liquid and the second liquid, respectively. The flow direction and the extension direction of the pores 222 are different from each other.

The micromixer 200 having the second configuration shown in FIG. 5 has a configuration in which the flow path in the central portion of the straight tube portion 210 is narrowed, but the present invention is not particularly limited to this, and is as shown in FIG. In addition, there may be a configuration in which the flow path is not narrowed and a uniform flow path is provided from the aqueous component supply unit 201 to the oil component supply unit 202. In the micromixer 200 having the second configuration of the modified example shown in FIG. 6, the first aspect, that is, neither the water-based component before merging nor the oil-based component before merging flows through the pores and merges. The dispersion is produced by allowing only the subsequent fluid to flow through the pores.

Further, the micromixer 200 having the second configuration shown in FIG. 5 has a configuration in which pores 222 are formed in the branch pipe portion 220, but the present invention is not particularly limited to this, and the micromixer 200 is continuously connected to the branch pipe portion. A member in which pores are formed may be separately connected.

7 (a) to 7 (c) show the micromixer 300 having the third configuration.

The micromixer 300 having the third configuration is continuously provided on the fluid flow path portion 310 provided in the piping path, the fluid confluence condensing section 320 continuously provided on the liquid outflow side thereof, and the liquid outflow side thereof. The fluid outflow portion 330 is provided.

The fluid flow path portion 310 has a small diameter pipe 311 and a large diameter pipe 312. The large diameter pipe 312 houses the small diameter pipe 311 and they are arranged in the same length direction and coaxially. As a result, in the fluid flow path portion 310, the first flow path 311a is formed inside the small diameter pipe 311 and the second flow path 312a is formed inside the large diameter pipe 312 and outside the small diameter pipe 311. The end of the small-diameter pipe 311 is configured in the water-based component supply unit (not shown), and the end of the large-diameter pipe 312 exposed to the outside of the fluid flow path portion 310 is configured in the oil-based component supply unit (not shown). ing. Therefore, the water-based component supply pipe 42a is connected to the water-based component supply section, and the oil-based component supply pipe 42b is connected to the oil-based component supply section. Such a micromixer 300 having a fluid flow path portion 310 having a double-tube structure has a simple apparatus configuration and is easy to maintain by disassembling and cleaning.

The fluid merging and condensing portion 320 continuously forms an internal region at the liquid outflow end of the fluid flow path portion 310. This internal region is configured in a fluid confluence region 321 in which the first liquid and the second liquid flowing out of the fluid flow path portion 310 come into contact with each other. The fluid confluence condensing portion 320 is perforated with pores 322 continuously provided in the fluid confluence area 321. The pores 322 are formed so as to extend in the same direction as the extending direction of the first flow path 311a and the second flow path 312a.

The fluid outflow section 330 is composed of a tubular dispersion liquid recovery section 303 that is continuously provided in the pores 322. The dispersion liquid recovery unit 303 is configured with a flow path expansion unit 331 in which the flow path cross-sectional area is continuously expanded in the pores 322. The dispersion liquid recovery pipe 48 is connected to the dispersion liquid recovery unit 303.

The micromixer 300 having the third configuration has the same configuration in which the flow directions of the first liquid and the second liquid toward the fluid confluence region 221 and the direction in which the pores 322 extend are the same.

By the way, the first liquid and the second liquid that flow out from the fluid flow path portion 310 and come into contact with each other in the fluid confluence region 321 are finally mixed by the pores 322. At this time, in order to obtain a higher-speed mixing performance, it is preferable that the mixed state thereof in the fluid confluence region 321 is composed of fine segments of each liquid. Therefore, it is preferable that the number of the first flow paths 311a is larger, and as shown in FIGS. 8A and 8B, there are a plurality of small diameter pipes 311 than when there is one small diameter pipe 311. In the case, a faster mixing characteristic can be obtained. Further, when the number of flow paths 311a and 311b is three or more in this way, it is possible to distribute a third liquid different from the first liquid and the second liquid to any of the flow paths 311a and 311b.

In the micromixer 300 having the third configuration, the first liquid of the oily component may be circulated in the first flow path 311a, and the second liquid of the aqueous component may be circulated in the second flow path 312a. it can.

(Manufacturing of emulsion)
1. 1. Experimental Equipment In Examples 1 to 23 and Comparative Examples 1 to 7, the dispersion liquid production system A shown in FIG. 1 in the above embodiment is used by applying the micromixer 100 having the first configuration shown in FIGS. 2 and 3. There was.

In Examples 1 to 17 and Comparative Examples 1 to 7, the configuration of the micromixer 100 is such that the outer diameter of the small diameter pipe 111 is D ₁ : 3 mm, the inner diameter of the small diameter pipe 111 is D ₂ : 2 mm, and the inner diameter of the large diameter pipe 112 is D 3: _3. 4.71 mm, gap Δ: 0.855 mm between the small diameter pipe 111 and the large diameter pipe 112, gap δ: 0.25 mm between the small diameter pipe 111 and the large diameter pipe 112, from the end of the fluid flow path portion 110 to the pore 122 Distance L: 0.68 mm, cone convergence angle θ ₁ : 120 ° of fluid confluence region 121, pore diameter d of pore 122: 0.22 mm, length l of pore 122: 0.55 mm, flow of pore 122 Road area s: 0.038 mm ² , length l of pore 122 / pore diameter d of pore 122, cone enlargement angle θ ₂ : 120 ° of flow path enlargement section 131, maximum of flow path enlargement section 131 The _{flow path diameter D 4} : 2 mm and the maximum flow path diameter D ₄ / pore diameter 122 had a pore diameter d: 9.1.

In Examples 18 to 23, the same micromixer 100 as in Example 1 except that the pore diameter d of the pore 122 was 0.40 mm and the maximum flow path diameter D _{4 / pore diameter 122 of the pore 122 was 5.0.} Was used.

2. Compounds used in Examples 1 to 23 and Comparative Examples 1 to 7 (1) Oil agent / neopentyl glycol dicaprate "Estemol N-01" (manufactured by Nisshin Oillio Group, IOB = 0.25)
・ Squalene "Nikkor Squalene" (manufactured by Nikko Chemicals, IOB = 0)
・ Higher alcohol "Calcol 200GD" (Made by Kao Corporation, IOB = 0.29)
-Dimethylpolysiloxane "Silicone KF-96-50CS" (manufactured by Shin-Etsu Chemical Co., Ltd., IOB = 0)
-N- (2-Hydroxy-3-hexadecyloxypropyl) -N-2-hydroxyethylhexadecanamid "Soft Care Ceramide SLE" (Kao Corporation, IOB = 0.33)

(2) Water-soluble solvent, polyoxybutylene polyoxyethylene polyoxypropylene glyceryl ether "Wilbride S-753" (manufactured by NOF CORPORATION, in general formula (IV), p1 + p2 + p3 = 8, q1 + q2 + q3 = 5, r1 + r2 + r3 = 3, EO and PO are added randomly)
-Polyoxyethylene polyoxypropylene alkyl ether "Unilube 50MB-11" (manufactured by NOF CORPORATION, in general formula (II), s = 9, t = 10, u = 0, EO and PO are randomly added, R ¹ is n-butyl group)
-Polyoxyethylene polyoxypropylene alkyl ether "Unilube 50MB-26" (manufactured by NOF CORPORATION, same as Unilube 50MB-11 except that s = 17 and t = 17 in the general formula (II))
-Polyoxyethylene polyoxypropylene alkyl ether "Unilube 50MB-72" (manufactured by NOF CORPORATION, same as Unilube 50MB-11 except that s = 30 and t = 30 in the general formula (II))
-Polyoxyethylene polyoxypropylene alkyl ether "Unilube 50MB-168" (same as Unilube 50MB-11 except that s = 37 and t = 38 in the general formula (II) manufactured by NOF CORPORATION)
Bisethoxydiglycol succinate "High Aquos Star DCS" (manufactured by Higher Alcohol Industry Co., Ltd., in general formula (III), v1 + v2 = 2, w1 + w2 = 0, and x1 + x2 = 0, n = 2, R ² and R ³ Ethyl group)
-Diethylene glycol monoethyl ether "Seahosol DG-S" (manufactured by Nippon Shokubai Co., Ltd.)
・ Ethanol "Ethanol 1st grade" (manufactured by Wako Pure Chemical Industries, Ltd.)
・ Glycerin "Cosmetic concentrated glycerin" (manufactured by Kao Corporation)
-Polyoxypropylene alkyl ether "Unilube MB-7" (manufactured by NOF CORPORATION, in general formula (II), s = 0, t = 12, u = 0, R ¹ is an n-butyl group)
-Polyoxypropylene alkyl ether "Unilube MB-19" (manufactured by NOF CORPORATION, same as Unilube MB-7 except that t = 24 in the general formula (II))
-Polyoxypropylene alkyl ether "Unilube MB-700" (manufactured by NOF CORPORATION, same as Unilube MB-7 except that t = 52 in the general formula (II))

(3) Surfactant and surfactant precursor-Polyoxyethylene cured castor oil 1 "Emanon CH-60" (manufactured by Kao Corporation, Kenka value = 44 KOHmg / g, EO average number of moles added = 60, HLB = 13 .8)
-Polyoxyethylene hydrogenated castor oil 2 "Emanon CH-25" (manufactured by Kao Corporation, Kenka value = 75 KOHmg / g, EO average number of moles added = 25, HLB = 10.7)
-PEG-30 dipolyhydroxystearate "Cysrol DPHS" (manufactured by Croda Japan, HLB = 5.0)
・ Oleic acid "LUNAC O-LL-V" (manufactured by Kao Corporation)
-Distearyldimethylammonium chloride "Varisoft TA-100" (manufactured by Evonik)
1- (2-Hydroxyethylamino) -3-isostearyloxy-2-propanol (manufactured by Kao Corporation)

3. 3. Calculation of segregation index (Xs) For Examples 1 to 4, 8 and 10 to 23, and Comparative Examples 1 to 5, the segregation index (Xs) was calculated as follows. A boric acid buffer solution to replace the aqueous component and 0.171N sulfuric acid to replace the oily component were prepared. The composition of the boric acid buffer was 0.045 mol / L of boric acid, 0.045 mol / L of sodium hydroxide, 0.00313 mol / L of potassium iodide, and 0.0156 mol / L of potassium iodide. These two solutions were mixed under the same conditions as in Examples or Comparative Examples, and the absorbance of the solution 1 minute after mixing with respect to light having a wavelength of 353 nm was measured using a spectrophotometer UVmini-1240 (manufactured by Shimadzu Corporation). .. Then, the segregation index (Xs) was calculated from the measurement result of the absorbance according to the above formula (iv).

4. Method for measuring the average particle size of particles in an emulsion Laser diffraction / scattering type particle size distribution measuring device "LA-910" (manufactured by Horiba Seisakusho Co., Ltd.), using water as a solvent, and setting the relative refractive index to 1.20. The median diameter of the oily component measured by the laser scattering / diffraction method was taken as the average particle diameter of the particles in the emulsion.

5. Operation and result <Example 1>
Ion-exchanged water was prepared as an aqueous component and charged into the aqueous component storage tank 41a to bring it to room temperature (20 ° C.). Further, as oily components, 45.5% by mass of neopentyl glycol dicaprate, which is a liquid oil as an oil agent, 45.5% by mass of polyoxybutylene polyoxyethylene polyoxypropylene glyceryl ether, which is a water-soluble solvent, and HLB. A uniform solution containing 9.0% by mass of polyoxyethylene hydrogenated castor oil 1 as a nonionic surfactant of 13.8 was prepared and charged into an oil component storage tank 41b to bring it to room temperature (20 ° C.). The oily component used in Example 1 was a liquid at room temperature (20 ° C.) and had self-emulsifying property with respect to ion-exchanged water as an aqueous component.

The dispersion liquid production system A is operated, and the flow rate of the aqueous component is set to 2 so that the mixed mass ratio of the aqueous component / oil component is 91.2 / 8.8 (= 10.4) at room temperature (20 ° C.). The flow rate of .74 L / h and the oily component was set to 0.26 L / h, and they were mixed with a micromixer 100 to obtain an emulsion. At this time, the flow rate ratio of the aqueous component to the oil component (flow rate of the aqueous component / flow rate of the oil component) was 10.5. The flow rate of the fluid after merging the aqueous component and the oil component flowing through the pores 122 was 3.0 L / h. The pressure loss before and after the micromixer 100 was 0.4 MPa.

In the obtained emulsion, the content of neopentyl glycol dicaprate was 4.00% by mass, the content of polyoxybutylene polyoxyethylene polyoxypropylene glyceryl ether was 4.00% by mass, and polyoxyethylene hydrogenated castor oil 1 The content was 0.80% by mass, and the content of ion-exchanged water was 91.20% by mass. The results are shown in Table 1.

The segregation index (Xs) in the emulsification operation of Example 1 was 1.9 × 10 ^-3 . _{[I 3} ⁻ ] 1 minute after mixing ^{was 3.98 × 10 −6} mol / L as a value obtained from the absorbance with respect to light having a wavelength of 353 nm. Further, [H ⁺ ] ₀ and [I ₂ ] were 0.171 ^{mol / L and 3.16 × 10-7} mol / L, _{respectively, and after} V mixing / V _{sulfate water} was 11.4, so Y was It was 5.71 × 10 ^-4. Also, _[IO ³ _{-] 0} and _[H 2 _BO ³ _-] Because ₀ was respectively 0.00313mol / L and 0.045mol / _{L, Y ST} was 0.294. This also applies to Examples 2 to 4, 8 and 10 to 23, and Comparative Examples 1 to 5.

<Examples 2 to 7>
The emulsion was prepared in the same manner as in Example 1 except that the water-soluble solvent in the aqueous component in the oil component was changed to the compound shown in Table 1 and the merging step and the pore circulation step were performed at 40 ° C. Obtained. The results are shown in Table 1. The oily components used in Examples 2 to 7 were liquid at 40 ° C. and had self-emulsifying properties with respect to ion-exchanged water as an aqueous component.

<Comparative Examples 1 to 5>
An emulsion was obtained in the same manner as in Example 1 except that the water-soluble solvent in the oily component was changed to the compound shown in Table 2. The results are shown in Table 2.

In the obtained emulsion, the content of neopentyl glycol dicaprate is 4.00% by mass, the content of polypropylene oxide alkyl ether is 4.00% by mass, and the content of polyethylene oxide-hardened castor oil 1 is 0.80% by mass. % And the content of ion-exchanged water was 91.20% by mass.

<Examples 8 to 10>
An emulsion was obtained in the same manner as in Example 1 except that the oil agent in the oily component was changed to the compound shown in Table 3. The results are shown in Table 3. The oily components used in Examples 8 to 10 were liquid at room temperature (20 ° C.) and had self-emulsifying properties with respect to ion-exchanged water as an aqueous component.

<Comparative Examples 6 and 7>
Emulsions were obtained in the same manner as in Examples 1 and 2, except that a water-soluble solvent was not used. The results are shown in Table 4.

<Comparative Examples 8 and 9>
After mixing 729.6 g of the aqueous component and 70.4 g of the oil component in a beaker (mixed mass ratio of the aqueous component / oil component 729.6 / 70.4 (= 10.4)), the homomixer “TK Homomixer MARKII 2. 5 ”(manufactured by Primix Corporation) was used and mixed at a rotation speed of 8000 r / min for 1 minute to prepare an emulsion, but the same procedure as in Examples 1 and 2 was carried out, respectively. The results are shown in Table 5.

In addition, the segregation index (Xs) in the emulsification operation of Comparative Examples 8 and 9 was 2.3 × 10 ^-1 . _{[I 3} ⁻ ] 1 minute after mixing ^{was 2.68 × 10 -4} mol / L as a value obtained from the absorbance with respect to light having a wavelength of 353 nm. Further, [H ⁺ ] ₀ and [I ₂ ] were 0.171 ^{mol / L and 2.13 × 10-5} mol / L, _{respectively, and after} V mixing / V _{sulfate water} was 20, so Y was 6. It was 76 × ^10-2. Also, _[IO ³ _{-] 0} and _[H 2 _BO ³ _-] Because ₀ was respectively 0.00313mol / L and 0.045mol / _{L, Y ST} was 0.294.

<Examples 11 to 13>
The emulsification was carried out in the same manner as in Example 1 except that the content of polyoxyethylene hydrogenated castor oil 1 which is a nonionic surfactant in the oily component, the flow rate of the aqueous component, and the flow rate of the oily component were changed as shown in Table 6. Got The results are shown in Table 6. The oily components used in Examples 11 to 13 were liquid at room temperature (20 ° C.) and had self-emulsifying properties with respect to ion-exchanged water as an aqueous component.

<Examples 14 to 17>
An emulsion was obtained in the same manner as in Example 1 except that the compound in Table 7 was changed as the surfactant in the oily component. The results are shown in Table 7. In Example 15, a uniform containing 2.54% by mass of 1M potassium hydroxide aqueous solution "1MKOH" (manufactured by Kishida Chemical Co., Ltd.) and 97.46% by mass of ion-exchanged water as aqueous components. A solution was used. The oily components used in Examples 14 to 17 were liquid at room temperature (20 ° C.) and had self-emulsifying properties with respect to ion-exchanged water as an aqueous component.

<Examples 18 to 23>
Examples except that the oily component, the aqueous component and their contents, the flow rate of the oily component and the flow rate of the aqueous component were changed as shown in Table 8, and the merging step and the pore circulation step were performed at 80 ° C. The same procedure as in 1 was carried out to obtain an emulsion. The results are shown in Table 8. The oily components used in Examples 18 to 23 were liquid at 80 ° C. and had self-emulsifying properties with respect to the aqueous components.

(Result consideration)
In Examples 1 to 23, an oily component containing an oil agent, a water-soluble solvent having a specific structure, and a surfactant or a surfactant precursor was dispersed in an aqueous component using a micromixer, the obtained emulsion was obtained. The average particle size of the particles in each of the above was 2.2 μm or less.

On the other hand, in Comparative Examples 1 to 5 in which the water-soluble solvent does not have a specific structure, Comparative Examples 6 and 7 containing no water-soluble solvent, and Comparative Examples 8 and 9 dispersed by a homomixer, the obtained emulsification was obtained. The average particle size of the particles in the object was 3.0 μm or more.

The present invention is useful for methods of producing dispersions.

A Dispersion liquid production system 100, 200, 300 Micromixer 101, 201 Aqueous component supply section 102, 202 Oil component supply section 103, 203, 303 Dispersion solution recovery section 110, 310 Fluid flow path section 111,311 Small diameter pipes 111a, 211a , 311a 1st flow path 111b Pipe end portion 112, 312 Large diameter pipe 112a, 212a, 312a 2nd flow path 120, 320 Fluid confluence constriction part 121,221,321 Fluid confluence area 122,222,322 Pore 130, 330 Fluid outflow part 131,231,331 Flow flow expansion part 210 Straight pipe part 220 Branch pipe part 41a Aqueous component storage tank 41b Oil component storage tank 42a Aqueous component supply pipe 42b Oil component supply pipe 43a First pump 43b Second pump 44a First Flowmeter 44b 2nd flowmeter 45a 1st filter 45b 2nd filter 46a 1st pressure gauge 46b 2nd pressure gauge 47 Flow controller 48 Dispersion fluid recovery pipe 49 Dispersion fluid recovery tank

Claims (9)

A merging step that merges the water-based component and the oil-based component,
One or two of the aqueous component before merging in the merging step, the oily component before merging in the merging step, and the fluid after merging the aqueous component and the oily component in the merging step. A method for producing a dispersion of particles having an average particle diameter of 10 μm or less, which comprises a pore circulation step in which one or more are circulated through pores under a condition that the segregation index (Xs) is 0.15 or less.
The oily component is combined with an oil agent, one or more water-soluble solvents selected from the group of compounds represented by the following general formulas (I) to (III), a surfactant and the water-based component. A method for producing a dispersion liquid containing at least one of surfactant precursors that form a surfactant when the solvent is formed.

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. P1, p2, p3, q1, q2, q3, r1, r2, and r3 represent the average number of added moles, respectively. ≦ p1 + p2 + p3 ≦ 20, 0 ≦ q1 + q2 + q3 ≦ 10, and 0 ≦ r1 + r2 + r3 ≦ 10, and 1 ≦ p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 ≦ 40. EO, PO, and BO are added randomly or in blocks).

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. S, t, and u represent the average number of moles added. 1 ≦ s ≦ 70, 0 ≦ t ≦ 70, and 0 ≦ u ≦ 10 and 1 ≦ s + t + u ≦ 100. EO, PO, and BO are added in a random or block shape. R ¹ is a hydrocarbon group having 2 or more and 5 or less carbon atoms. .)

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. V1, v2, w1, w2, x1, and x2 represent the average number of moles added. 1 ≦ v1 + v2 ≦ 10, 0, respectively. ≦ w1 + w2 ≦ 9, 0 ≦ x1 + x2 ≦ 9, and 1 ≦ v1 + v2 + w1 + w2 + x1 + x2 ≦ 10. EO, PO, and BO are added in a random or block shape. R ² and R ³ are independent of each other. It is a hydrocarbon group having 1 or more and 4 or less carbon atoms. N is a number of 1 or more and 4 or less.) The method for producing a dispersion according to claim 1, wherein the oily component contains one or more water-soluble solvents selected from the group of compounds represented by the following general formula (IV).

(EO represents an ethylene oxide group, PO represents a propylene oxide group, and BO represents a butylene oxide group. P1, p2, p3, q1, q2, q3, r1, r2, and r3 represent the average number of added moles, respectively. ≦ p1 + p2 + p3 ≦ 20, 1 ≦ q1 + q2 + q3 ≦ 10, 1 ≦ r1 + r2 + r3 ≦ 10, and 3 ≦ p1 + p2 + p3 + q1 + q2 + q3 + r1 + r2 + r3 ≦ 40. EO and PO are added in a random or block shape.) The method for producing a dispersion according to claim 1 or 2, wherein the content of the surfactant and the surfactant precursor in the oily component is 10% by mass or less. The production of the dispersion liquid according to any one of claims 1 to 3, wherein in the pore flow step, a fluid after merging the aqueous component and the oil component at least in the merging step is circulated in the pores. Method. In the pore flow step, after the fluid after merging the aqueous component and the oil component in the merging step is circulated in the pores, the maximum flow path diameter is three times or more the pore diameter of the pores. The method for producing a dispersion liquid according to claim 4, wherein the dispersion is discharged to a flow path expansion portion having a size of 50 times or less. In the pore flow step, the flow rate when the fluid after merging the aqueous component and the oil component in at least the merging step is circulated in the pores is 0.1 L / h or more and 300 L / h or less. , The method for producing a dispersion according to claim 4 or 5. The dispersion according to any one of claims 1 to 6, wherein the surfactant is one or more selected from the group consisting of a nonionic surfactant, an anionic surfactant, and a cationic surfactant. Production method. The dispersion according to any one of claims 1 to 7, wherein in the merging step, the flow rate ratio of the aqueous component to the oily component (flow rate of the aqueous component / flow rate of the oily component) before merging is 1 or more and 200 or less. Liquid manufacturing method. The method for producing a dispersion liquid according to any one of claims 1 to 8, wherein in the merging step, the oily component is merged with the aqueous component from the entire circumference thereof.

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