JP6787977B2 - 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 in which oily components and aqueous components are allowed to flow in the pores of a micromixer and collide with each other.

In Patent Document 2, an aqueous component is allowed to flow, an oil component containing melted ceramide and a nonionic surfactant is flowed, and a fluid in which they are merged is circulated through the pores of a micromixer to form an emulsion. A method for producing a ceramide fine particle dispersion, which is produced and then cooled to solidify the ceramide, is disclosed.

Japanese Unexamined Patent Publication No. 2008-142588 Japanese Unexamined Patent Publication No. 2008-037842

An object of the present invention is to produce a dispersion in which fine particles of an oily component are dispersed in an aqueous component.

The present invention is a merging step in which an oily component containing a surfactant having a neutralizable functional group and an oil agent as a main component and an aqueous component containing a neutralizing agent having a salt-forming ability with the surfactant are merged. And the pore flow step in which the fluid merged in the merge step is circulated in the pores, and the dispersion operation of the aqueous component and the oil component has a segregation index (Xs) of 0.1 or less. This is a method for producing a dispersion liquid in which the surfactant is neutralized with the neutralizing agent in the merged fluid under the conditions.

According to the present invention, a surfactant having a neutralizable functional group, an oily component containing an oil agent as a main component, and an aqueous component containing a neutralizing agent having a salt-forming ability with the surfactant are merged. The surfactant was later circulated in the pores, and at this time, the dispersion operation of the aqueous component and the oily component was performed under the condition that the segregation index (Xs) was 0.1 or less, and the surfactant was merged. By neutralizing with the neutralizing agent, a dispersion liquid in which fine particles of an oily component are dispersed in an aqueous component 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. (A) is a vertical cross-sectional view showing a micromixer having a second configuration, (b) is a cross-sectional view of IVB-IVB in FIG. 4 (a), and (c) is a cross-sectional view of IVC-IVC in FIG. 4 (a). It is a figure. (A) is a vertical cross-sectional view showing a modified example of the micromixer having the second configuration, and (b) is a VB-VB cross-sectional view in FIG. 5 (a). It is a vertical sectional view which shows the micro mixer of the 3rd structure. It is a vertical sectional view which shows the modification of the micromixer of 3rd structure. It is a vertical cross-sectional view which shows the other modification of the micromixer of 3rd structure. It is a vertical cross-sectional view which shows another modification of the micromixer of 3rd composition. It is a vertical sectional view which shows the micro mixer of the 4th structure.

Hereinafter, embodiments will be described in detail.

The method for producing a dispersion according to the present embodiment is a salt formation of a surfactant having a neutralizable functional group, an oily component containing an oil as a main component, and a surfactant having a neutralizable functional group. It includes a merging step in which an aqueous component containing a neutralizing agent having a function is merged, and a pore circulation step in which the fluid merged in the merging step is circulated through pores having a pore diameter of 0.03 to 3 mm. Then, at this time, the surfactant is neutralized with the neutralizing agent in the merged fluid.

By the way, in the technique disclosed in Patent Document 1, since the aqueous component contains a surfactant, in order to obtain fine particles, the aqueous component contains a large amount of the surfactant with respect to the amount of the oily component. There is a need. Further, in the technique disclosed in Patent Document 2, since the oily component contains a nonionic surfactant, it is necessary to contain a large amount of the surfactant in the oily component in order to obtain fine particles. On the other hand, in the field of cosmetics applied to skin, hair, etc., it may be desired to prepare a dispersion liquid in which fine particles are dispersed with a small amount of surfactant.

On the other hand, in the method for producing a dispersion according to the present embodiment, a salt of an oily component containing a surfactant having a neutralizable functional group and an oil agent and a surfactant having a neutralizable functional group thereof. An aqueous component containing a neutralizing agent having a forming ability is merged and circulated in the pores, and after the pores flow out, both components are agitated by turbulent flow. Therefore, it is possible to efficiently supply a surfactant having a neutralizable functional group from the dispersed oily component to the oil-water interface in a short time from the contact between the oily component and the aqueous component until the shearing force is applied. Can be done. At this time, in the process in which the oily component and the aqueous component merge to flow and flow out of the pores, the surfactant is neutralized by the neutralizing agent, and as a result, the content of the surfactant is small. Also, it is possible to produce a dispersion liquid in which fine liquid or solid particles of an oily component are dispersed in an aqueous component.

The dispersion produced by the method according to the present embodiment includes both an emulsion in which droplet particles of an oily component are dispersed in an aqueous component and a dispersion in which solid particles of an oily component are dispersed in an aqueous component. ..

(Oil component)
The oily component contains a surfactant having a neutralizable functional group.

Here, the "surfactant having a neutralizable functional group" does not exhibit ionicity in an unneutralized state and forms a cationic or anionic salt by mixing with a predetermined neutralizing agent. Refers to a surfactant that is used. Hereinafter, "surfactant having a neutralizable functional group" is referred to as "surfactant A".

Examples of the surfactant A which is mixed with a predetermined neutralizing agent to form a cationic salt include a surfactant having an amino group and a hydrophobic group. If such a surfactant is used, dispersion can be performed well.

Hydrophobic groups include, for example, saturated or unsaturated linear or branched hydrocarbon groups. The number of carbon atoms contained in the hydrocarbon group is preferably 8 or more, more preferably 10 or more, still more preferably 12 or more, and from the viewpoint of obtaining a dispersion liquid in which fine particles are dispersed by performing good dispersion. It is preferably 30 or less, more preferably 22 or less, still more preferably 20 or less, and even more preferably 18 or less. Specific hydrocarbon groups include, for example, 2-ethylhexyl group, octyl group, nonyl group, isononyl group, decyl group, undecyl group, dodecyl group, tridecyl group, isotridecyl group, tetradecyl group, pentadecyl group, hexadecyl group and heptadecyl. Examples include an alkyl group such as a group, an octadecyl group and an isooctadecyl group; and an alkenyl group such as an oleyl group. From the viewpoint of producing a dispersion in which fine particles are dispersed with a small amount of surfactant A, hexadecyl group, heptadecyl group, octadecyl group and isooctadecyl group are preferable, and octadecyl group and isooctadecyl group are more preferable.

Surfactants having an amino group and a hydrophobic group include primary amine compounds, secondary amine compounds, and tertiary amine compounds.

Examples of the primary amine compound include long-chain alkylamines. The carbon number of the long-chain alkyl group of the long-chain alkylamine is preferably 8 or more, more preferably 10 or more, still more preferably 12 or more, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. Also, it is preferably 30 or less, more preferably 22 or less, still more preferably 20 or less, still more preferably 18 or less. The same applies to the preferable number of carbon atoms of the long chain described below.

Secondary amine compounds include, for example, dialkylamines having long-chain alkyl groups such as long-chain alkylmethylamine, long-chain alkylethylamine, and long-chain alkylpropylamine and short-chain alkyl groups; sphingosins (eg, 1- (2-Hydroxyethylamino) -3-isostearyloxy-2-propanol) and the like. Examples of the short-chain alkyl group include alkyl groups having 1 to 4 carbon atoms such as methyl group, ethyl group, n-propyl group, i-propyl group, n-butyl group, i-butyl group and t-butyl group. Can be mentioned. The same examples of short-chain alkyl groups described below can be mentioned.

Examples of sphingosines include the following (i) to (iv).

Examples of the tertiary amine compound include trialkylamines having long-chain alkyl groups and short-chain alkyl groups such as long-chain alkyldimethylamine, long-chain alkyldipropylamine, and long-chain alkyldipropylamine; dimethylaminopropyl stearate. Long-chain fatty acids dialkylaminoethylamides such as amides and diethylaminoethylamide stearate and long-chain fatty acids dialkylaminopropylamides; hexadecyloxypropyl dimethylamine, stearoxypropyl dimethylamine, stearoxyethyl dimethylamine, octadecyloxypropyl dimethylamine Examples thereof include araquiloxypropyl dimethylamine such as (N, N-dimethyl-3-octadecyloxypropylamine), acyloxyethyldialkylamine such as beheniroxypropyldimethylamine, and acyloxypropyldialkylamine. The number of carbon atoms contained in the long chain fatty acid or the acyl group is preferably 8 or more, more preferably 10 or more, still more preferably 12 or more, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. Further, it is preferably 30 or less, more preferably 22 or less, still more preferably 20 or less, still more preferably 18 or less. Specific examples of the hydrocarbon group contained in the long chain fatty acid or the acyl group include the same ones listed as the above-mentioned examples of the hydrophobic group. The alkyl group contained in the dialkyl is a short-chain alkyl group having 1 to 4 carbon atoms such as a methyl group, an ethyl group, an n-propyl group, an i-propyl group, an n-butyl group, an i-butyl group and a t-butyl group. Is preferable.

As the surfactant A which is mixed with a predetermined neutralizing agent to form an anionic salt, for example, one or 2 selected from the group consisting of a carboxy group, a sulfonic acid group, a phosphonic acid group, and a phosphoric acid group. Surfactants having more than one kind of functional group and hydrophobic group can be mentioned. If such a surfactant is used, dispersion can be performed well.

Examples of the hydrophobic group include the same as in the case of a surfactant having an amino group and a hydrophobic group.

Examples of the surfactant having a carboxy group and a hydrophobic group include fatty acids, alkyl ether carboxylic acids, N-long-chain acyl amino acids and the like.

Examples of the fatty acid include those represented by the following formula (1).

R ^1- COOH (1)
(In the formula, R ¹ means the same as the above-mentioned hydrophobic group, preferably a saturated or unsaturated hydrocarbon having 8 to 22 carbon atoms, more preferably 12 to 18 carbon atoms. Indicates a group.)
Examples of the fatty acid represented by the formula (1) include lauric acid, myristic acid, oleic acid and the like. Of these, oleic acid is preferable from the viewpoint of producing a dispersion liquid in which fine particles are dispersed.

Examples of the alkyl ether carboxylic acid include those represented by the following formula (2).

R ² O- (C ₂ H ₄ O) _n- CH ₂ COOH (2)
(In the formula, R ² means the same as the above-mentioned hydrophobic group, and is preferably 8 to 20 carbon atoms, more preferably from the viewpoint of obtaining a dispersion liquid in which fine particles are dispersed by performing good dispersion. It represents a saturated or unsaturated hydrocarbon group of a linear or branched chain having 12 to 18 carbon atoms, and n represents a number of 1 to 12, preferably 1 to 3, and means an average number of added moles.)
Examples of the N-long-chain acyl amino acid include N-palmitoyl acylglycine, N-stearoylalanine, N-palmitoyl aspartic acid, N-palmitoyl acylglutamic acid, N-stearoyl acylglycine, N-stearoyl-L-glutamic acid and the like. Be done. Of these, N-stearoyl-L-glutamic acid is preferable from the viewpoint of producing a dispersion liquid in which fine particles are dispersed.

Examples of the surfactant having a sulfonic acid group and a hydrophobic group include alkylbenzene sulfonic acid.

Examples of the alkylbenzene sulfonic acid include those represented by the following formula (3).

R ^31- CHR ^32- C ₆ H _4- SO ₃ H (3)
(In the formula, R ³¹ means the same as the above-mentioned hydrophobic group, and is preferably 8 to 20 carbon atoms, more preferably from the viewpoint of obtaining a dispersion liquid in which fine particles are dispersed by performing good dispersion. It represents a saturated or unsaturated hydrocarbon group of a linear or branched chain having 12 to 18 carbon atoms, and R ³² represents a hydrogen atom, a methyl group, an ethyl group, an isopropyl group, or a t-butyl group).
Examples of the surfactant having a phosphoric acid group and a hydrophobic group include a monoalkyl phosphate ester.

Examples of the monoalkyl phosphate ester include those represented by the following formula (4).

R ^4- O-PO ₃ H ₂ (4)
(In the formula, R ⁴ means the same as the above-mentioned hydrophobic group, and is preferably 8 to 20 carbon atoms, more preferably from the viewpoint of obtaining a dispersion liquid in which fine particles are dispersed by performing good dispersion. Indicates a saturated or unsaturated hydrocarbon group of a linear or branched chain having 12 to 18 carbon atoms.)
The oily component preferably contains, as the surfactant A, one or more selected from the group consisting of the above-mentioned surfactants. From the viewpoint of producing a dispersion liquid in which fine particles are dispersed with a small amount of surfactant A, the surfactant A to be included in the oily component includes a surfactant having an amino group and a hydrophobic group, and a carboxy group and hydrophobicity. Surfactants with groups are preferred.

The content of the surfactant A in the oily component is preferably 15% by mass or less, more preferably 10% by mass or less, still more preferably, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed with a small amount of the surfactant A. Is 9% by mass or less, and may be preferably 5% by mass or less, and even more preferably 3% by mass or less, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed with a small amount of surfactant A. From the same viewpoint, it is preferably 0.3% by mass or more, more preferably 1% by mass or more, still more preferably 2% by mass or more, still more preferably 2.5% by mass or more.

The surfactant A may be partially neutralized as long as the action and effect of producing a dispersion liquid in which fine particles are dispersed are not impaired.

The oily component contains an oil agent (hereinafter referred to as "oil agent B") as a main component.

The oil agent B may be composed of only liquid oil, may be composed of only solid fat, and may be further composed of both liquid oil and solid fat. Here, the "liquid oil" refers to an oil agent that is liquid at 25 ° C. "Solid fat" refers to an oil that is solid at 25 ° C.

The oil agent B preferably contains a liquid oil from the viewpoint of producing a dispersion liquid in which fine particles are dispersed with a small amount of the surfactant A. The content of the liquid oil in the oil agent B is preferably 30% by mass or more, more preferably 50% by mass or more, still more preferably 80% by mass or more, still more preferably 90% by mass or more.

Examples of the oil agent B include hydrocarbon oils, ester oils, dialkyl ethers, fats and oils, higher alcohols, silicones and the like. The oil agent B is one or more functional groups selected from the group consisting of an ester group, a keto group, an aldehyde group, a carboxyl group, a hydroxyl group, and an ether group from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. An oil agent having is preferable.

Examples of the hydrocarbon oil include paraffin, squalene, squalane and the like.

Examples of the ester oil include ethylene glycol difatty acid ester, fatty acid monoglyceride (for example, glycerin monocaprate), fatty acid diglyceride, fatty acid glyceride such as fatty acid triglyceride, neopentyl glycol difatty acid ester (for example, neopentyl glycol dicaprate) and the like. Be done. The number of carbon atoms contained in the fatty acid is preferably 8 to 22 from the viewpoint of obtaining a dispersion liquid in which fine particles are dispersed by performing good dispersion, and preferably 5 or more, more preferably 8 or more from the same viewpoint. From the same viewpoint, it is preferably 22 or less, more preferably 18 or less, still more preferably 12 or less.

Examples of the dialkyl ether include a diether having a saturated or unsaturated linear or branched alkyl group. The number of carbon atoms contained in the alkyl group is preferably 8 to 22 from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed.

Examples of fats and oils include vegetable oils such as soybean oil, coconut oil, palm kernel oil, linseed oil, cottonseed oil, rapeseed oil, millet oil, and castor oil.

Examples of the higher alcohol include saturated or unsaturated linear or branched alcohols (for example, 2-octyldodecanol). The number of carbon atoms contained in the higher alcohol is preferably 8 to 22 from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed.

Examples of silicones include methylpolysiloxane, methylphenylsiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, methylhydrogenpolysiloxane, silicone resin, amino-modified silicone, alkyl-modified silicone and the like.

Examples of the oil agent B include organic ultraviolet absorbers such as 2-ethylhexyl paramethoxycinnamate; fragrances and the like.

The oil agent B may be either volatile or non-volatile.

The oily component preferably contains, as the oil agent B, one or more selected from the group consisting of the oil agents listed above. As the oil agent B to be included in the oily component, ester oil and higher alcohol are preferable, and fatty acid glyceride is more preferable, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed.

The molecular weight of the oil agent B is preferably 40 or more, more preferably 100 or more, still more preferably 150 or more, and from the viewpoint of producing a dispersion liquid in which fine particles are dispersed, it is preferably 2000 or less, more preferably 1500. Below, it is more preferably 1000 or less, and even more preferably 500 or less.

The viscosity of the oil agent B is preferably 0.1 mPa · s or more, more preferably 1 mPa · s or more, and further, at the temperature of the oily component when the oily component and the aqueous component are merged, from the viewpoint of good liquid feeding. It is preferably 5 mPa · s or more, and is preferably 1000 mPa · s or less, more preferably 500 mPa · s or less, still more preferably 300 mPa · s or less, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. For the viscosity of the oil agent B, a Brookfield type (B type) rotational viscometer was used, and the rotor No. 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.

The melting point of the oil agent B is preferably 95 ° C. or lower, more preferably 90 ° C. or lower, still more preferably 80 ° C. or lower, still more preferably 50 ° C. or lower, still more, from the viewpoint of merging the oily component and the aqueous component well. It is preferably 25 ° C. or lower. The melting point of the oil agent B can be determined, for example, by the endothermic peak in the differential scanning calorimetry (DSC).

The amount of the oil agent B dissolved in 100 g of water is preferably 10 g or less, more preferably 5 g or less, still more preferably 5 g or less, at the temperature of the oil component when the oil component and the aqueous component are merged, from the viewpoint of good dispersion. It is 3 g or less, more preferably 1 g or less.

The content of the oil agent B in the oily component is contained as a main component from the viewpoint of producing a dispersion liquid in which fine particles are dispersed, and is preferably 70% by mass or more, more preferably 80% by mass or more, and further preferably 85% by mass. % Or more, more preferably 90% by mass or more, even more preferably 91% by mass or more, and from the viewpoint of producing a dispersion liquid in which fine particles are dispersed by containing the surfactant A in an oily component, it is preferable. It is 99.7% by mass or less, more preferably 99% by mass or less, still more preferably 98% by mass or less, still more preferably 97.5% by mass or less, still more preferably 93% by mass or less. The main component means that the content is the largest among the oily components.

The total content of the surfactant A and the oil agent B in the oily component is preferably 85% by mass or more, more preferably 90% by mass or more, still more preferably 95% by mass from the viewpoint of dispersing the oil agent B by the surfactant A. % Or more, more preferably 100% by mass.

The mass ratio of the content of the surfactant A to the content of the oil agent B in the oily component (surfactant A / oil agent B) is preferably 0.01 or more from the viewpoint of dispersing the oil agent B by the surfactant A. It is more preferably 0.02 or more, still more preferably 0.03 or more, even more preferably 0.05 or more, still more preferably 0.08 or more, and fine particles are dispersed with a small amount of surfactant A. From the viewpoint of producing the above-mentioned dispersion liquid, it is preferably 0.2 or less, more preferably 0.15 or less, still more preferably 0.12 or less, still more preferably 0.1 or less.

Further, the oily component may contain an organic solvent such as methanol or dimethyl ethyl ketone as long as the action and effect of producing a dispersion liquid in which fine particles are dispersed are not impaired. The content of the oily component is preferably 5% by mass or less, more preferably 3% by mass or less, and further preferably 1% by mass or less. Further, the oily component may include a nonionic surfactant.

The form of the oily component is not particularly limited, but it is preferable that the surfactant A is dissolved in the oily agent B at a temperature at which the oily component and the aqueous component are merged.

The oily component has fluidity because it merges with the aqueous component. The viscosity of the oily component is preferably 0.1 mPa · s or more, more preferably 1 mPa · s or more, still more preferably 5 mPa · s at the temperature at which the oily component and the aqueous component are merged from the viewpoint of good liquid feeding. From the viewpoint of producing a dispersion liquid in which fine particles are dispersed, the temperature is preferably 1000 mPa · s or less, more preferably 500 mPa · s or less, and further preferably 300 mPa · s or less. The method for measuring the viscosity of the oily component is the same as the method for measuring the viscosity of the oil agent B described above.

(Aqueous component)
The aqueous component is an aqueous solution in which a neutralizing agent having a salt-forming ability with the surfactant A is dissolved in water.

Here, the "neutralizing agent having a salt-forming ability with the surfactant A" refers to an acidic compound or a basic compound having a salt-forming ability with the surfactant A. Hereinafter, the "neutralizing agent having a salt-forming ability with the surfactant A" is referred to as "neutralizing agent C".

Examples of the neutralizing agent C include acidic compounds and basic compounds.

When the surfactant A is a surfactant having an amino group and a hydrophobic group, the neutralizing agent C is preferably an acidic compound.

Examples of acidic compounds include inorganic acids and organic acids.

Examples of the inorganic acid include phosphoric acid, hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, carbonic acid and the like.

Examples of organic acids include monocarboxylic acids such as formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid and valeric acid; dicarboxylic acids such as succinic acid, phthalic acid, fumaric acid, oxalic acid, malonic acid and glutaric acid; glycol. Oxycarboxylic acids such as acids, citric acid, lactic acid, pyruvate, malic acid and tartrate; amino acids such as L-glutamic acid and aspartic acid can be mentioned. The number of carbon atoms contained in the organic acid is preferably 2 to 7, more preferably 2 to 6 carbon atoms, and further preferably 3 to 6 from the viewpoint of good dispersion.

As the acidic compound, an organic acid is preferable from the viewpoint of good dispersion, an organic acid containing 3 to 6 carbon atoms is more preferable, and one or more selected from amino acids and oxycarboxylic acids is more preferable, and L- One or more selected from glutamic acid and lactic acid are more preferable.

When the surfactant A is a surfactant having one or more functional groups and a hydrophobic group selected from the group consisting of a carboxy group, a sulfonic acid group, a phosphonic acid group, and a phosphoric acid group, the neutralizing agent C Is preferably a basic compound.

Examples of the basic compound include inorganic bases and organic bases.

Examples of the inorganic base include hydroxides of alkali metals such as sodium hydroxide and potassium hydroxide, and ammonia.

Examples of the organic base include aniline; monoalkylamines such as methylamine; dialkylamines such as dimethylamine; alkanolamines such as monoethanolamine; and basic amino acids such as L-arginine.

As the basic compound, alkali metal hydroxides, alkanolamines or basic amino acids are preferable, and alkali metal hydroxides or basic amino acids are preferable from the viewpoints of good dispersion, availability and handleability. Is more preferred, and potassium hydroxide or L-arginine is even more preferred.

The aqueous component is one or 2 selected from the group consisting of the acidic compounds or basic compounds listed above as the neutralizing agent C from the viewpoint of obtaining a dispersion liquid in which fine particles are dispersed by performing good dispersion. It is preferable to include seeds or more.

The content of the neutralizing agent C in the aqueous component is preferably 0.01% by mass or more, more preferably 0.03% by mass or more, still more preferably 0.05% by mass, from the viewpoint of neutralizing the surfactant A. The above is more preferably 0.1% by mass or more, still more preferably 0.11% by mass or more, and from the viewpoint of considering the amount of the neutralizing agent C dissolved in water, it is preferably 5% by mass or less. , More preferably 3% by mass or less, still more preferably 1% by mass or less, still more preferably 0.5% by mass or less, still more preferably 0.4% by mass or less, still more preferably 0.3% by mass or less. is there.

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, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. , More preferably 95% by mass or more, even more preferably 98% by mass or more, preferably 99.9% by mass or less, still more preferably 99.7% by mass or less.

Preservatives may be included in the aqueous component. Examples of the preservative include paraoxybenzoic acid esters such as methyl 4-hydroxybenzoate (methylparaben), ethyl 4-hydroxybenzoate (ethylparaben), and propyl 4-hydroxybenzoate (propylparaben). The content of the preservative in the aqueous component is preferably 2% by mass or less, more preferably 1% by mass or less, still more preferably 0.5, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. It may be 0% by mass or less, substantially 0% by mass, or 0.1% by mass or more.

The aqueous component can include a polyhydric alcohol from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. Examples of the polyhydric alcohol include glycerin and dipropylene glycol. The content of the polyhydric alcohol in the aqueous component is preferably 1% by mass or more, more preferably 5% by mass or more, and preferably 50% by mass or less, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is preferably 30% by mass or less, more preferably 20% by mass or less.

The aqueous component may include other solutes and water-soluble organic solvents as long as the action and effect of producing a dispersion liquid in which fine particles are dispersed are not impaired.

The aqueous component has fluidity because it merges with the oil component. The viscosity of the aqueous component is preferably 0.1 mPa · s or more, more preferably 1 mPa · s or more, still more preferably 5 mPa · s at the temperature at which the oil component and the aqueous component are merged from the viewpoint of good liquid feeding. From the viewpoint of producing a dispersion liquid in which fine particles are dispersed, the temperature is preferably 1000 mPa · s or less, more preferably 500 mPa · s or less, and further preferably 300 mPa · s or less. The viscosity of the aqueous component may be the same as or different from the viscosity of the oil component. The method for measuring the viscosity of the aqueous component is the same as the method for measuring the viscosity of the oil agent B described above.

(Merge step)
In the merging step, the oily component of the flowing liquid and the aqueous component of the flowing liquid are merged. At this time, in the combined fluid, the surfactant A is neutralized by the neutralizing agent C in the process in which the oily component and the aqueous component merge to flow and flow out of the pores.

This molar equivalent ratio (neutralizing agent C / surfactant A) is preferably 0.3 or more, more preferably 0.3 or more, from the viewpoint of neutralizing the surfactant A and finely dispersing the oily component containing the oil agent B. It is 0.5 or more, more preferably 0.6 or more, still more preferably 0.7 or more, and from the viewpoint of considering the amount of the neutralizing agent C dissolved in water, it is preferably 5 or less, more preferably 5. It is 3 or less, more preferably 2 or less, and even more preferably 1.2 or less.

Further, in the merged fluid, the content (mass%) of the surfactant A x the molar equivalent ratio (neutralizing agent C / surfactant A) / the content of the oil agent B (mass%) is the surfactant. From the viewpoint of finely dispersing the oily component containing the oil agent B by A, it is preferably 0.01 or more, more preferably 0.02 or more, still more preferably 0.03 or more, still more preferably 0.06 or more. Further, from the viewpoint of finely dispersing the oily component containing the oil agent B with a smaller amount of the surfactant A, it is preferably 0.2 or less, more preferably 0.16 or less, still more preferably 0.14 or less, still more preferable. Is 0.12 or less, more preferably 0.11 or less.

In the merging step, the flow rate of the oily components before merging is preferably 0.01 L / h or more, more preferably 0.1 L / h, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. Above, more preferably 0.15 L / h or more, preferably 150 L / h or less, more preferably 100 L / h or less, still more preferably 50 L / h or less, still more preferably 10 L / h or less. It is even more preferably 2 L / h or less, even more preferably 0.5 L / h or less, and even more preferably 0.18 L / h or less. The flow rate of the aqueous component before merging is preferably 0.1 L / h or more, more preferably 1 L / h or more, still more preferably 2 L, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. / H or more, preferably 300 L / h or less, more preferably 200 L / h or less, still more preferably 100 L / h or less, still more preferably 20 L / h or less, still more preferably 10 L / h or less. Even more so, it is 3 L / h or less. The flow rate ratio of the aqueous component to the oil component (flow rate of the aqueous component / flow rate of the oil component) before merging is preferably 1 or more from the viewpoint of obtaining an O / W type dispersion liquid with a small amount of surfactant A. It is preferably 2 or more, more preferably 5 or more, still more preferably 10 or more, still more preferably 15 or more, and preferably 200 or less, more preferably 200 or less, from the viewpoint of increasing the content of the oily component in the dispersion liquid. Is 100 or less, more preferably 50 or less, still more preferably 30 or less, still more preferably 25 or less, still more preferably 21 or less.

In the merging step, the temperature of the oily components at the time of merging is preferably 5 ° C. or higher, more preferably 10 ° C. or higher, and more preferably 10 ° C. or higher, from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. It is preferably 95 ° C. or lower, more preferably 90 ° C. or lower, still more preferably 80 ° C. or lower, still more preferably 60 ° C. or lower, still more preferably 40 ° C. or lower. The temperature of the aqueous component at the time of merging is preferably 5 ° C. or higher, more preferably 10 ° C. or higher, and preferably 95 ° C. from the viewpoint of satisfactorily dispersing and obtaining a dispersion liquid in which fine particles are dispersed. Below, it is more preferably 90 ° C. or lower, still more preferably 80 ° C. or lower, still more preferably 60 ° C. or lower, still more preferably 40 ° C. or lower. The temperature of the oily component and the temperature of the aqueous component at the time of merging may be the same and can be set arbitrarily.

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

Examples of the collision mode (angle, etc.) when the oil-based component and the aqueous component are merged include a mode in which both are head-on collisions and merged (counter-current collision), and one is collided from a direction orthogonal to the other. A mode of merging, a mode of colliding one with the other diagonally from the rear and merging, a mode of colliding one with the other diagonally from the front and merging, a mode of contacting one along the other and merging, one of the other An embodiment in which collisions occur from all around and merges can be mentioned. Of these, as a mode of collision at the time of merging, from the viewpoint of producing an O / W type dispersion liquid in which fine particles are dispersed, a mode in which both are head-on collided and merged (countercurrent collision). Is preferably collided from the entire circumference of the other and merged, and more preferably the oily component is collided and merged from the entire circumference of the aqueous component.

Further, as the mode (number, etc.) of the merging method when the oily component and the aqueous component are merged, 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 to be merged. There is an aspect of causing the collision. In the former, it is preferable to collide both of them from two or more directions, and it is preferable to collide from four or less directions from the viewpoint of productivity, although there is no particular upper limit. In the latter, it is preferable to collide one with the other from two or more directions, and it is preferable to collide one with the other from four or less directions from the viewpoint of productivity, although there is no particular upper limit.

Further, the oily component and / or the aqueous component is circulated in the pores having the same composition as the pores through which the fluid merged in the pore circulation step described later is circulated, or is circulated in the pores and they are circulated. May be merged.

(Pore distribution step)
In the pore circulation step, the fluid merged in the merging step is circulated in the pores.

Examples of the cross-sectional shape of the pores include a circle, a semicircle, an ellipse, a semi-elliptical shape, a square, a rectangle, a trapezoid, a parallelogram, a star shape, and an indefinite shape. Of these, a circular shape is preferable from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. 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 oily component and / or the flow direction of the aqueous component from the viewpoint of producing a dispersion liquid in which fine particles are dispersed.

The pore diameter of the pores is 0.03 to 3 mm. The pore diameter of the pores is preferably 0.07 mm or more, more preferably 0.1 mm or more from the viewpoint of obtaining high productivity, and preferably 1 from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is 5.5 mm or less, more preferably 1 mm or less, still more preferably 0.5 mm or less, still more preferably 0.3 mm or less. Here, the pore diameter is the diameter when the cross-sectional shape of the pore is circular, but when the cross-sectional shape of the pore is non-circular, the equivalent hydraulic diameter (4 × flow path area / cross section). 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, still more preferably 0, from the viewpoint of enhancing the mixing property of the oily component and the aqueous component. From the viewpoint of producing a dispersion liquid having a size of 5 mm or more and in which an oily component and an aqueous component are instantly mixed and fine particles are dispersed, the thickness is preferably 5 mm or less, more preferably 3 mm or less, still more preferably 1. It is 5 mm or less, and more preferably 1 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 oily component and the aqueous component, it is preferably 7 mm ² or less, more preferably 2 mm ² or less, still more preferably 0.5 mm ² or less, still more preferably 0.1 mm ² or less, and more. More preferably, it is 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, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. .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 9 or less. Is.

In the pore circulation step, as a method of circulating the fluid in which the oily component and the aqueous component are merged in the merging step, the oily component and the aqueous 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 producing a dispersion liquid in which fine particles are dispersed, a confluence of the oil-based component and the aqueous component is provided immediately before the pores, or the oil-based component is used. It is preferable to combine the aqueous component with the pores.

In the pore circulation step, the flow rate of the fluid when the fluid obtained by merging the oily component and the aqueous component in the merging step is circulated through the pores is determined from the viewpoint of increasing the pressure loss and producing a dispersion of fine particles. It is preferably 0.1 L / h or more, more preferably 1 L / h or more, and preferably 300 L / h or less, more preferably 250 L, from the viewpoint of preventing excessive pressure loss from causing damage to the equipment. / H or less, more preferably 100 L / h or less, still more preferably 50 L / h or less, still more preferably 20 L / h or less, still more preferably 8 L / h or less.

The pressure loss is the pressure difference before and after the pore circulation, so that the size of the jet can be evaluated. The pressure loss is preferably 0.05 MPa or more, more preferably 0.1 MPa or more, still more preferably 0.2 MPa or more, still more preferably 0.3 MPa or more, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. Also, from the viewpoint of preventing excessive pressure loss from causing damage to the equipment, it is preferably 10 MPa or less, more preferably 5 MPa or less, still more preferably 3 MPa or less, still more preferably 1.5 MPa or less. In the dispersion liquid manufacturing system S described later, the pressure before the pore circulation is the pressure measured by the second pressure gauge 46b (the pressure on the oily component side), and the pressure after the pore circulation is the open system. Since there is, it is 0.

From the viewpoint of increasing the stirring efficiency of the oil phase component and the aqueous phase component in the flow path expansion region after the pore flow, in the pore flow step, the fluid merged in the merging step is formed into pores under turbulent flow conditions. It is preferable to distribute it. The Reynolds number at this time is preferably 1000 or more, more preferably 1800 or more, still more preferably 2700 or more, from the viewpoint of increasing the stirring efficiency of the oil phase component and the aqueous phase component in the flow path expansion region after pore circulation. From the viewpoint of mixing in the channel expansion region, it is preferably 150,000 or less, more preferably 100,000 or less, still more preferably 30,000 or less, still more preferably 10,000 or less, still more preferably 7200, still more preferably. Is less than 6000. Here, the Reynolds number is 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 a general Reynolds number calculation formula (Reynolds number Re = duρ / μ) of the pipe flow using the value of.

In the pore circulation step, the fluid obtained by merging the oily component and the aqueous component in the merging step is circulated through the pores and then discharged to the flow path expansion portion. As a result, turbulence is likely to occur, and the particles can be made finer.

Examples of the cross-sectional shape of the flow path of the flow path expansion portion include a circle, a semicircle, an ellipse, a semi-elliptical shape, a square, a rectangle, a trapezoid, a parallelogram, a star shape, and an indefinite shape. Of these, a circular shape is preferable from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. The cross-sectional shape of the flow path enlarged portion is preferably the same shape along the length direction, but different shapes may be included along the length direction.

From the viewpoint of producing a dispersion liquid in which fine particles are dispersed, 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 (θ ₁₂ in FIG. 2) is preferably 90 ° or more, more preferably 100 ° or more, and preferably 180 ° or less, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is more preferably 170 ° or less, still more preferably 140 ° or less.

The maximum flow path diameter of the flow path expanding portion is preferably 2 times or more, more preferably 3 times or more, still more preferably 5 times or more, more preferably the pore size of the pores, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is more preferably 7 times or more, preferably 50 times or less, more preferably 40 times or less, still more preferably 30 times or less, still more preferably 20 times or less, still more preferably 10 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.

(Dispersion)
In the method for producing a dispersion liquid according to the present embodiment, a dispersion liquid in which particles of an oil-based component are dispersed in an aqueous component is produced by circulating a fluid in which an oil-based component and an aqueous component are merged through pores.

The average particle size of the produced dispersion is preferably 1 μm or less, more preferably 0.7 μm or less, still more preferably 0.5 μm or less, still more preferably, from the viewpoint of producing a dispersion in which fine particles are dispersed. It is 0.3 μm or less, and is preferably 0.01 μm or more, more preferably 0.05 μm or more, from the viewpoint of the productivity of the dispersion liquid. Here, the average particle size of the particles in the dispersion is a median size measured by a laser scattering / diffraction method using a laser diffraction / scattering type particle size distribution measuring device.

Further, the produced dispersion has an average particle diameter of the oil component preferably 1/100 or less, more preferably 1/100 or less of the pore diameter, from the viewpoint of producing a dispersion in which fine particles of the oil component are dispersed. It is 200 or less, more preferably 1/300 or less, even more preferably 1/400 or less, even more preferably 1/500 or less, and there is no particular lower limit, but from the viewpoint of dispersion liquid productivity. Therefore, 1/10000 or more is preferable, 1/15000 or more is more preferable, and 1/2000 or more is further preferable.

The content of the surfactant A 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% by mass, from the viewpoint of good dispersion. % Or more, more preferably 0.3% by mass or more, and from the viewpoint of producing a dispersion liquid in which fine particles are dispersed with a small amount of surfactant A, preferably 1% by mass or less, more preferably 0. It is 8.8% by mass or less, more preferably 0.7% by mass or less, still more preferably 0.5% by mass or less.

The content of the oil agent B in the produced dispersion is preferably 1% by mass or more, more preferably 3% by mass or more, still more preferably 4% by mass, from the viewpoint of satisfactorily mixing the oily component and the aqueous component. % Or more, and from the viewpoint of producing a dispersion liquid in which fine particles are dispersed, preferably 50% by mass or less, more preferably 30% by mass or less, still more preferably 10% by mass or less, still more preferably 5% by mass. % Or less.

The content of the neutralizing agent C in the produced dispersion is preferably 0.01% by mass or more, more preferably 0, from the viewpoint of producing a dispersion in which fine particles are dispersed with a small amount of the surfactant A. It is 0.03% by mass or more, more preferably 0.05% by mass or more, still more preferably 0.1% by mass or more, and from the same viewpoint, preferably 1.0% by mass or less, more preferably 0. It is 8% by mass or less, more preferably 0.6% by mass or less, still more preferably 0.5% by mass or less, still more preferably 0.4% by mass or less, still more preferably 0.3% by mass or less.

The produced dispersion is used, for example, in cosmetics and the like.

In the dispersion operation of the oily component and the aqueous component in the method for producing the dispersion liquid according to the present embodiment, a dispersion liquid in which fine particles are dispersed has a segregation index (Xs) obtained by the method described later. From the viewpoint, it is preferably 0.1 or less, more preferably 0.08 or less, still more preferably 0.06 or less, still more preferably 0.04 or less, still more preferably 0.02 or less, still more preferably 0. It is preferable to carry out the operation under the conditions of 01 or less, more preferably 0.008 or less, still more preferably 0.005 or less, still more preferably 0.004 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 oily component and the aqueous component in the method for producing the dispersion according to the present embodiment, and the smaller the value, the higher the mixing property. The segregation index (Xs) is an index that is academically used for evaluation of the mixing performance of a mixer, and can be derived from the following equation using the Villermaux / Dushman reaction. For details of this reaction system, refer to P.I. 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 solution 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 (I) and the redox reaction (II) produced by iodine proceed at the same time. The two liquids are mixed under the condition that the boric acid buffer solution becomes excessive in the state after mixing. That is, a boric acid buffer solution is used as the aqueous component.

(Dispersion liquid manufacturing system S)
FIG. 1 shows an example of a dispersion liquid manufacturing system S that can be used in the dispersion liquid manufacturing method according to the present embodiment.

The dispersion liquid manufacturing system S is composed of a micromixer 100 and ancillary parts such as a fluid supply system.

2 and 3 show the micromixer 100 having the first configuration.

The micromixer 100 having the first configuration includes a fluid flow path portion 10, a fluid confluence condensing section 20 continuously provided on the downstream side thereof, and a fluid outflow section 30 continuously provided on the downstream side thereof. And.

The fluid flow path portion 10 has a small diameter pipe 11 and a large diameter pipe 12. The large-diameter pipe 12 accommodates the small-diameter pipe 11, which have a common length direction and are arranged coaxially. As a result, in the fluid flow path portion 10, the first flow path 11a is formed inside the small diameter pipe 11, and the second flow path 12a is formed inside the large diameter pipe 12 and outside the small diameter pipe 11. The first flow path 11a in the small diameter pipe 11 communicates with the aqueous component supply unit 101 provided at one end of the device, and the second flow path 12a in the large diameter tube 12 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 tube 11 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 amorphous. And so on. The cross-sectional shape of the hole of the large-diameter tube 12 is also not particularly limited, and like the small-diameter tube 11, for example, circular, semicircular, elliptical, semi-elliptical, square, rectangular, trapezoidal, parallelogram, etc. It may be star-shaped, irregular-shaped, or the like. However, the outer shape and the cross-sectional shape of both the outer shape and the hole of the small-diameter pipe 11 and the hole of the large-diameter pipe 12 are preferably circular from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. Further, the small-diameter pipe 11 and the large-diameter pipe 12 are preferably provided so that the cross-sectional shapes are symmetrical and coaxial from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. Therefore, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed, the small-diameter pipe 11 and the large-diameter pipe 12 have a circular cross-sectional shape of the first flow path 11a and a second flow as shown in FIG. It is preferable that the road 12a is provided so that the cross-sectional shape of the road 12a is a donut shape.

From the viewpoint of producing a dispersion liquid in which fine particles are dispersed, both the outer shape and the cross-sectional shape of the hole of the small diameter pipe 11 shall have the same shape along the length direction except for the pipe end portion 11b described later. Is preferable. The cross-sectional shape of the holes of the large-diameter pipe 12 is also the same along the length direction except for the portion corresponding to the pipe end portion 11b of the small-diameter pipe 11 from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. Is preferable.

When both the outer shape and the cross-sectional shape of the hole of the small diameter tube 11 are circular, the outer diameter D ₁₁ is preferably 1.6 mm or more, more preferably 1.6 mm or more, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is 2 mm or more, preferably 25 mm or less, more preferably 15 mm or less, still more preferably 10 mm or less, still more preferably 4 mm or less. The inner diameter D ₁₂ of the small diameter tube 11, that is, the flow path diameter of the first flow path 11a is preferably 0.8 mm or more, more preferably 1 mm or more, and more preferably 1 mm or more, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is preferably 20 mm or less, more preferably 10 mm or less, still more preferably 5 mm or less, still more preferably 3 mm or less. When the cross-sectional shape of the hole of the large-diameter pipe 12 is circular, the inner diameter D ₁₃ is preferably 1.8 mm or more, more preferably 4 mm or more, and preferably 50 mm or less, more preferably 20 mm or less. It is more preferably 10 mm or less, still more preferably 6 mm or less. Gap delta ₁ of the second flow path 12a between the small diameter tube 11 and large diameter pipe 12, from the viewpoint of producing a fine particles are dispersed dispersion, preferably 0.1mm or more, more preferably more than 0.3mm It is more preferably 0.7 mm or more, and more preferably 12.5 mm or less, more preferably 6 mm or less, still more preferably 3 mm or less, still more preferably 1 mm or less.

As shown in FIG. 2, the tube end portion 11b on the downstream side of the small-diameter tube 11 preferably has a tapered outer peripheral portion from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is more preferable that the cross-sectional shape in the longitudinal direction is formed into a spire shape that is sharp on the inner peripheral side.

The gap δ _{1 which} is a part of the second flow path 12a formed between the inner wall of the large-diameter pipe 12 and the pipe end portion 11b of the small-diameter pipe 11 is from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. , It is preferable that the fluid flow direction is uniform. The gap δ ₁ is preferably 0.02 mm or more, more preferably 0.05 mm or more, still more preferably 0.1 mm or more, and preferably 12 from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is 5.5 mm or less, more preferably 6 mm or less, still more preferably 1 mm or less, still more preferably 0.40 mm or less.

The fluid confluence condensing portion 20 is configured with a fluid confluence portion 21 in front of the pipe end of the small diameter pipe 11, and pores 22 are continuously perforated in the fluid confluence portion 21. In the fluid merging section 21, the aqueous component flowing through the first flow path 11a and the oily component flowing through the second flow path 12a merge, and in the pores 22, the oily component and the aqueous component immediately after merging at the fluid merging section 21 Ingredients are distributed. Therefore, in the micromixer 100 having the first configuration, neither the oily component nor the aqueous component before merging is circulated in the pores, and only the fluid in which they are merged is circulated in the pores 22 to distribute the dispersion liquid. To manufacture.

The fluid merging portion 21 is not particularly limited, but has a tapered cone shape that converges toward the pores 22 as shown in FIG. 2 from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is preferably formed. The cone convergence angle θ ₁₁ is preferably 90 ° or more, more preferably 100 ° or more, and preferably 180 ° or less, more preferably 170 °, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. Below, it is more preferably 140 ° or less. From the viewpoint of producing a dispersion liquid in which fine particles are dispersed, the cone convergence angle θ ₁₁ is preferably the same as the cone expansion angle θ ₁₂ when the flow path expanding portion 31 has a cone shape. The pipe end of the small-diameter pipe 11 of the fluid merging portion 21, that is, the length L ₁ from the end of the fluid flow path portion 10 to the pores 22, is preferably 0 from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is .02 mm or more, more preferably 0.2 mm or more, still more preferably 0.3 mm or more, and preferably 20 mm or less, more preferably 10 mm or less, still more preferably 1 mm or less.

The cross-sectional shape of the pores 22, the extending direction, the pore diameter d ₁ , the length l ₁ , the flow path area s ₁ , and the ratio of the length l _{1 to} the pore diameter d ₁ (length l ₁ / pore diameter d ₁ ) have already been described. It is a street.

The fluid outflow portion 30 has a flow path expanding portion 31 formed in front of the pores 22. The fluid flowing through the pores 22 flows out to the flow path expanding portion 31. The flow path expanding portion 31 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 30, the cone enlargement angle θ ₁₂ , and the maximum flow path diameter D ₁₄ of the flow path enlargement portion 31 are as described above.

The micromixer 100 having the first configuration may be composed of a plurality of members each made of metal, ceramics, resin, or the like, and the fluid flow path portion 10 and the fluid confluence contraction may be formed by combining these members. The flow portion 20 and the fluid outflow portion 30 may be configured.

In the micromixer 100 having the first configuration, the aqueous component supply pipe 42a extending from the aqueous component storage tank 41a is connected to the aqueous component supply unit 101 communicating with the first flow path 11a. A first pump 43a for circulating the aqueous component, a first flow meter 44a for detecting the flow rate of the aqueous component, and a first filter 45a for removing impurities of the aqueous component are interposed in the aqueous component supply pipe 42a in 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 component supply pipe 42b extending from the oil component storage tank 41b is connected to the oil component supply unit 102 communicating with the second flow path 12a. 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, and includes 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 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 31 and is connected to the dispersion liquid recovery tank 49.

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

When the dispersion liquid production system S 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. It is continuously supplied to the first flow path 11a of the small diameter pipe 11 of the fluid flow path portion 10. 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.

In the second pump 43b, the oily component to be the particles of the dispersed phase is passed through the oily component storage tank 41b, the oily component supply pipe 42b, the second flow meter 44b, and the second filter 45b in order, and the fluid flow path portion 10 It is continuously supplied to the second flow path 12a between the large diameter pipe 12 and the small diameter pipe 11. 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 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 is based on the set flow rate information and the set pressure information of the oil 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.

In the micromixer 100 having the first configuration, in the fluid flow path portion 10, the aqueous component flows through the first flow path 11a and the oily component flows through the second flow path 12a. At this time, the pressure of the aqueous component is, for example, 0.01 to 5 MPa. The pressure of the oily component is, for example, 0.01 to 5 MPa. Then, the flow rate (L / h) of the aqueous component is adjusted by setting the flow rate and pressure of the aqueous component, and the flow rate (L / h) of the oil component is adjusted by setting the flow rate and pressure of the oil component, respectively, as described above.

In the fluid merging and condensing section 20, the oily component and the aqueous component flowing out from the fluid flow path section 10 collide with the flowing aqueous component in the fluid merging section 21 from diagonally behind and from the entire circumference thereof. Meet in a mode. At this time, the fluid merging and condensing section 20 adjusts the flow rate (L / h) of the fluid including the oily component and the aqueous component as described above. This flow velocity can be controlled by setting the flow rates and pressures of the oil-based component and the aqueous component, respectively.

The oily component and the aqueous component merged in the fluid merging portion 21 are mixed in the process of flowing through the pores 22. At this time, the flow conditions of the oily component and the aqueous component merged in the fluid confluence area 21 can be controlled by setting the flow rates and pressures of the oily component and the aqueous component, respectively.

In the fluid outflow section 30, the fluid containing the oily component and the aqueous component flowing through the pores 22 flows out in the flow path expanding section 31, and a dispersion liquid is produced by convection mixing between the oily component and the aqueous component.

From the dispersion liquid recovery unit 103 communicating with the flow path expansion unit 31, the produced dispersion liquid is collected in the dispersion liquid recovery tank 49 via the dispersion liquid recovery pipe 48.

4 (a) to 4 (c) show the micromixer 100 having the second configuration. The part having the same name as the first configuration is indicated by the same code as the first configuration.

The micromixer 100 having the second configuration includes a fluid flow path portion 10, a fluid confluence condensing section 20 continuously provided on the downstream side thereof, and a fluid outflow section 30 continuously provided on the downstream side thereof. And.

The fluid flow path portion 10 has one small-diameter pipe 11 and a large-diameter pipe 12. The large-diameter pipe 12 accommodates the small-diameter pipe 11, which have a common length direction and are arranged coaxially. As a result, in the fluid flow path portion 10, the first flow path 11a is formed inside the small diameter pipe 11, and the second flow path 12a is formed inside the large diameter pipe 12 and outside the small diameter pipe 11. The tube end surface of the small diameter tube 11 is formed on a surface perpendicular to the axial direction. The first flow path 11a in the small diameter pipe 11 communicates with the water-based component supply unit 101, and the second flow path 12a in the large-diameter pipe 12 communicates with the oil-based component supply unit 102. As a result, the aqueous component flows through the first flow path 11a, and the oily component flows through the second flow path 12a. The micromixer 100 having a second configuration in which the fluid flow path portion 10 has a simple double-tube structure is easy to maintain by disassembling and cleaning.

The fluid confluence condensing portion 20 has a pipe structure continuous with the large-diameter pipe 12, and the front end thereof is sealed by a wall perpendicular to the axial direction, and a pore 22 is formed in the center of the wall. As a result, the fluid merging and condensing portion 20 is configured with the fluid merging portion 21 in the cylindrical space in front of the pipe end of the small diameter pipe 11. The length of the fluid confluence portion 21, that is, the length L ₂ from the end of the fluid flow path portion 10 to the pores 22, is preferably 0.1 mm or more from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is more preferably 0.2 mm or more, further preferably 0.5 mm or more, and preferably 3.0 mm or less, more preferably 2.0 mm or less, still more preferably 1.5 mm or less. In the fluid merging section 21, the aqueous component flowing through the first flow path 11a and the oily component flowing through the second flow path 12a merge, and in the pores 22, the oily component and the aqueous component merging in the fluid merging section 21 are used. Fluid circulates. Therefore, in the micromixer 100 of the second configuration, as in the micromixer 100 of the first configuration, neither the oily component nor the aqueous component before merging is circulated in the pores, and only the fluid in which they are merged is used. A dispersion liquid is produced by circulating it in the pores 22.

The fluid outflow portion 30 includes a flow path expanding portion 31 in a cylindrical space in front of the pores 22. The fluid flowing through the pores 22 flows out to the flow path expanding portion 31. The flow path expanding section 31 communicates with the dispersion liquid recovery section 103.

Other configurations and operations are the same as in the case of the micromixer 100 having the first configuration.

By the way, the oily component and the aqueous component that flow out from the fluid flow path portion 10 and come into contact with the fluid confluence portion 21 are finally mixed by the pores 22. At this time, in order to obtain higher speed mixing performance, it is sufficient that the mixed state of the fluid merging portion 21 is composed of minute segments of each liquid. Therefore, it is preferable that the number of the first flow paths 11a is larger, and as shown in FIGS. 4 (a) and 4 (b), there is more than one small diameter tube 11 (a) and (b). As shown in the above, when there are a plurality of small diameter tubes 11, faster mixing characteristics can be obtained. Further, when there are three or more first flow paths 11a as shown in FIGS. 5A and 5B, it is possible to distribute the third liquid to any of the first flow paths 11a.

In the micromixer 100 having the first and second configurations, the inside of the small diameter pipe 11 is the second flow path through which the oily component is circulated, and the inside of the large diameter pipe 12 and the outside of the small diameter pipe 11. It can also be used as a first flow path for circulating an aqueous component.

FIG. 6 shows a micromixer 100 having a third configuration. The part having the same name as the first configuration is indicated by the same code as the first configuration.

The micromixer 100 having the third configuration is composed of a straight pipe portion 110 and a T-shaped pipe including a branch pipe portion 120 branched from the central portion of the straight pipe portion 110 and extending in the orthogonal direction. Such a T-tube micromixer 100 has a simple device configuration and is easy to maintain by disassembling and cleaning.

One end of the straight pipe portion 110 is connected to the aqueous component supply unit 101, the other end of the straight pipe portion 110 is connected to the oil component supply unit 102, and the end of the branch pipe portion 120 is connected to the dispersion liquid recovery unit 103. It is configured.

The straight pipe portion 110 is composed of large pore diameter portions on both sides, while the central portion is configured in a small pore diameter portion in which the flow path is discontinuously narrowed from the large pore diameter portion, of which one end side is the first flow. The path 11a and the other end side are configured in the second flow path 12a.

The branch pipe portion 120 has pores 22 extending along the pipe axis and communicating with each other in the straight pipe portion 110, and the central portion of the straight pipe portion 110, that is, the inside of the branch portion to the branch pipe portion 120. Is configured in the fluid confluence 21 continuous with the pores 22. The branch pipe portion 120 is configured with a flow path expanding portion 31 in a cylindrical space in which the flow path is discontinuously expanded following the pores 22.

The inner diameters D ₃₁ , D ₃₂ , and D ₃₄ of the large pore diameter portions on both sides of the straight pipe portion 110 and the flow path expansion portion 31 of the branch pipe portion are preferably 0. From the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is 3 mm or more, more preferably 0.5 mm or more, preferably 5.0 mm or less, more preferably 3.0 mm or less, still more preferably 1.0 mm or less. Each of the first flow path 11a and the second flow path 12a has an inner diameter D ₃₃ and a flow path cross-sectional area, that is, a pore area equal to or similar to that of the pore 22. Therefore, in the micromixer 100 having the third configuration, the water-based component and the oil-based component before merging are circulated to the first flow path 11a and the second flow path 12a forming the pores, respectively, and merged, and then they are merged. , The dispersion liquid is produced by circulating the fluid in which they are merged through the pores 22. From the viewpoint of suppressing the pressure loss to be small, it is preferable that the lengths of the first flow path 11a and the second flow path 12a, that is, the hole lengths are the same as or about the same as the pores 22.

The configuration such as the shape and size of the pores 22 and the operation in the production of the dispersion liquid are the same as in the case of the micromixer 100 having the first configuration.

By the way, in the micromixer 100 having the third configuration shown in FIG. 6, the flow directions of the oil-based component and the aqueous component toward the fluid confluence 21 and the extension direction of the pores 22 are different from each other. The present invention is not limited to this, and for example, as shown in FIG. 7, one end of the straight pipe portion 110 is connected to the water-based component supply unit 101, and the end of the branch pipe portion 120 is connected to the oil-based component supply unit 102. Further, the other end of the straight pipe portion 110 is formed in the dispersion liquid recovery portion 103, and one of the flow directions of the oil-based component and the aqueous component toward the fluid confluence portion 21 is the same as the extension direction of the pores 22. It may be configured to be. However, from the viewpoint of obtaining high mixing performance, as in the micromixer 100 having the third configuration shown in FIG. 6, the flow directions and pores of the oily component and the aqueous component toward the fluid confluence 21 are respectively. It is preferable that the extending directions of the 22 are different from each other.

Further, the micromixer 100 having the third configuration shown in FIG. 6 has a configuration having a first flow path 11a and a second flow path 12a in which the flow path in the central portion of the straight pipe portion 110 is narrowed. For example, as shown in FIG. 8, a configuration in which a uniform flow path is formed from one end to the other end may be formed in the straight pipe portion 110. In the micromixer 100 shown in FIG. 8, neither the oily component nor the aqueous component before merging is circulated in the pores, and only the fluid in which they are merged is circulated in the pores 22 to produce a dispersion liquid. To do.

Further, in the micromixer 100 having the third configuration shown in FIG. 6, the straight pipe portion 110 and the branch pipe portion 120 are communicated with each other through the pores 22, but the present invention is not particularly limited to this. For example, as shown in FIG. 9, the main body portion is composed of a T-shaped pipe having a straight pipe portion 110 and a branch pipe portion 120 having a uniform flow path, and the end opening of the branch pipe portion 120 is closed. A plate-shaped member 130 having pores 22 formed in the center may be provided. Even in the micromixer 100 shown in FIG. 9, neither the oily component nor the aqueous component before merging is circulated in the pores, and only the fluid in which they are merged is circulated in the pores 22 to produce a dispersion liquid. To do.

FIG. 10 shows a micromixer 100 having a fourth configuration. The part having the same name as the first configuration is indicated by the same code as the first configuration.

The micromixer 100 having the fourth configuration is composed of a Y-shaped tube in which three first to third tubes 111 to 113 are abutted and connected to communicate with each other. Such a Y-tube micromixer 100 has a simple apparatus configuration and is easy to maintain by disassembling and cleaning.

The end of the first pipe 111 is to the aqueous component supply unit 101, the end of the second pipe 112 is to the oil component supply unit 102, and the end of the third pipe 113 is to the dispersion liquid recovery unit 103. It is configured.

Each of the first to third pipes 111 to 113 is composed of a large pore diameter portion on the end side, and a small pore diameter portion in which the flow path is discontinuously narrowed from the large pore diameter portion on the coupling end side. The first pipe 111 is configured with a first flow path 11a, the second pipe 112 is configured with a second flow path 12a, and the third pipe 113 is configured with pores 22. The small hole diameter portion of the first pipe 111 constituting the first flow path 11a, the small pore diameter portion of the second pipe 112 forming the second flow path 12a, and the connecting portion of the pores 22 are formed in the fluid confluence portion 21. Has been done. The third tube 113 is configured with a flow path expanding portion 31 in a cylindrical space in which the flow path is discontinuously expanded following the pores 22.

The large pore size portions of the first to third pipes 111 to 113 and the inner diameters D ₄₁ , D ₄₂ , and D ₄₅ of the flow path expanding portion 31 are preferably 0, respectively, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. It is 5 mm or more, more preferably 1.0 mm or more, preferably 5.0 mm or less, more preferably 3.0 mm or less, still more preferably 1.2 mm or less. Further, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed, it is preferable that D ₄₁ , D ₄₂ and D ₄₅ are the same. Further, each of the first flow path 11a and the second flow path 12a has inner diameters D ₄₃ and D ₄₄ , and the flow path cross-sectional area, that is, the pore area is the same as or about the same as the pore 22. Therefore, in the micromixer 100 having the fourth configuration, the water-based component and the oil-based component before merging are circulated to the first flow path 11a and the second flow path 12a forming the pores, respectively, and merged, and then they are merged. , The dispersion liquid is produced by circulating the fluid in which they are merged through the pores 22. From the viewpoint of suppressing the pressure loss to a small value, it is preferable that the lengths L ₄₃ and L _{44 of} the first flow path 11a and the second flow path 12a, that is, the hole length is the same as or about the same as the pore 22.

Fine particles are dispersed in the angle Θ ₄₁ formed by the extending direction of the first flow path 11a and the extending direction of the pore 22 and the angle Θ ₄₂ formed by the extending direction of the second flow path 12a and the extending direction of the pore 22. From the viewpoint of producing the above-mentioned dispersion liquid, each is preferably more than 90 °, more preferably 100 ° or more, further preferably 120 ° or more, still more preferably 140 ° or more, and from the same viewpoint, preferably 180 ° or more. It is less than °, more preferably 170 ° or less, still more preferably 160 ° or less. Further, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed, it is preferable that Θ ₄₁ = Θ ₄₂ . The angle Θ ₄₃ formed by the first flow path 11a and the second flow path 12a preferably exceeds 0 °, more preferably 20 ° or more, still more preferably 20 ° or more, from the viewpoint of producing a dispersion liquid in which fine particles are dispersed. 40 ° or more, and from the same viewpoint, preferably less than 180 °, more preferably 160 ° or less, still more preferably 120 ° or less, still more preferably 80 ° or less.

The configuration such as the shape and size of the pores 22 and the operation in the production of the dispersion liquid are the same as in the case of the micromixer 100 having the first configuration.

(Dispersion liquid manufacturing experiment)
A dispersion liquid production experiment was conducted using a dispersion liquid production system S having the same configuration as that shown in FIG. 1 of the above embodiment.

In Examples 1 to 4 and 6 to 8 and Comparative Examples 5 and 6, the micromixer 100 having the first configuration shown in FIGS. 2 and 3 has an outer diameter D ₁₁ : 3 mm of the small diameter pipe 11 and a small diameter pipe 11. Inner diameter D ₁₂ : 2 mm, inner diameter D ₁₃ of the large diameter pipe 12: 4.71 mm, gap between the small diameter pipe 11 and the large diameter pipe 12 Δ ₁ : 0.855 mm, gap between the small diameter pipe 11 and the large diameter pipe 12 δ ₁ : 0.25 mm, length from the end of the fluid flow path portion 10 to the pore 22 L ₁ : 0.68 mm, cone convergence angle θ ₁₁ : 120 ° of the fluid confluence portion 21, pore diameter d ₁ : 0 of the pore 22 .22 mm, pore 22 length l ₁ : 0.55 mm, pore 22 flow path area s ₁ : 0.038 mm ² , pore 22 length l ₁ / pore 22 pore diameter d ₁ : 2. 5. The cone enlargement angle θ ₁₂ : 120 ° of the flow path expanding portion 31, the maximum flow path diameter D ₁₄ : 2 mm of the flow path expanding portion 31, and the pore diameter d ₁ : 9.1 of the maximum flow path diameter D ₁₄ / pore 22. The one with the configuration was used. In Examples 5 and 9 and Comparative Example 11, the pore size of the pores 22 _d 1: 0.40 mm and the flow passage area _s 1 of the pores 22: Change in 0.126 mm ^2, the length of the pores 22 l _{The configuration of 1} / pore 22 pore diameter d ₁ : 1.4 and maximum flow path diameter D ₁₄ / pore 22 pore diameter d ₁ : 5.0 was used.

In Examples 10 to 12, the micromixer 100 having the second configuration shown in FIGS. 4 (a) to 4 (c) has an outer diameter D _{21 of} the small diameter pipe 11: 3.18 mm and an inner diameter D _{22 of the} small diameter pipe 11. : 2.18 mm, inner diameter D of large diameter pipe 12 ₂₃ : 4.35 mm, gap between small diameter pipe 11 and large diameter pipe 12 Δ ₂ : 0.59 mm, length from the end of fluid flow path portion 10 to pore 22 L ₂ : 1.0 mm, pore diameter d ₂ : 0.3 mm, pore 22 length l ₂ : 0.9 mm, pore 22 flow path area s ₂ : 0.071 mm ² , pores length of 22 _{l 2} / pore size of the pores 22 _d 2: 3.0, the maximum passage diameter _D 24 of the enlarged flow path portion 31: 1.6 mm, and the maximum flow path diameter _{D 24} / pore 22 pore diameter _d 2: The one having the configuration of 5.3 was used.

In Examples 13 to 15, in the micromixer 100 having the third configuration shown in FIG. 6, the length L _{31 of} the straight tube portion 110: 33.52 mm, and the inner diameter D of the large hole diameter portions on both sides of the straight tube portion 110. ₃₁ , D ₃₂ : 0.8 mm, inner diameter of the small hole diameter portion constituting the first flow path 11a and the second flow path 12a D ₃₃ : 0.3 mm, length of the small hole diameter portion L ₃₂ : 2.6 mm, pores 22 pore diameter d ₃ : 0.3 mm, pore 22 length l ₃ : 0.9 mm, pore 22 flow path area s ₃ : 0.071 mm ² , pore 22 length l ₃ / pore 22 Pore diameter d ₃ : 3.0, maximum flow path diameter D ₃₄ : 0.8 mm of the flow path expansion portion 31 in the dispersion liquid recovery unit 103, and maximum flow path diameter D ₃₄ / pore 22 pore diameter d ₃ : 2.7. The one with the configuration was used.

In Examples 16 and 17, in the fourth configuration micromixer 100 shown in FIG. 10, the inner diameters of the large pore diameter portions of the aqueous component supply section 101 and the oil component supply section 102 are large, D ₄₁ , D ₄₂ : 1.09 mm. Hole diameter portion length L ₄₁ , L ₄₂ : 30.0 mm, inner diameter of the small pore diameter portion constituting the first flow path 11a and the second flow path 12a D ₄₃ , D ₄₄ : 0.15 mm, length of the small hole diameter portion L ₄₃ , L ₄₄ : 1.2 mm, pore diameter d ₄ : 0.15 mm, pore length l ₄ : 1.2 mm, flow path area of pore 22 s ₄ : 0.018 mm ² , Pore 22 length l ₄ / Pore 22 pore diameter d ₄ : 8.0, maximum flow path diameter D ₄₅ : 1.09 mm of the flow path expansion section 31 in the dispersion liquid recovery section 103, length of the flow path expansion section 31 L ₄₅ : 30.0 mm, and the maximum flow path diameter D ₄₅ / pore diameter d ₄ : 7.3, and the angle formed by the extension direction of the first flow path 11a and the extension direction of the pore 22 Θ ₄₁ : 150 °, the angle formed by the extending direction of the second flow path 12a and the extending direction of the pore 22 Θ ₄₂ : 150 °, and the angle formed by the first flow path 11a and the second flow path 12a Θ ₄₃ : 60 °. The one with the configuration was used.

In Comparative Examples 1 to 4 and 7 to 10, a homomixer TK homomixer MARKII2.5 (manufactured by Primix Corporation) was used.

Tables 1 and 2 and Table 7 show the compositions of the oily and aqueous components, respectively. The materials used are as follows.

-Surfactant A-
-Cantic surfactant Secondary amine compound 1- (2-Hydroxyethylamino) -3-isostearyloxy-2-propanol: manufactured by Kao Corporation The following formula (1)

-Anionic surfactant N-long-chain acyl amino acid N-stearoyl-L-glutamic acid Amisoft HA-P: Ajinomoto Co., Inc. formula (2)

・ Cationic surfactant Tertiary amine N, N-dimethyl-3-octadecyloxypropylamine Farmin DM E-80: manufactured by Kao Corporation ・ Anionic surfactant fatty acid oleic acid Lunac O-LL-V: manufactured by Kao Corporation -Oil B-
・ Glycerin monocaprate Homotex PT: manufactured by Kao Corporation ・ 2-octyldodecanol Calcol 200GD: manufactured by Kao Corporation ・ Neopentyl glycol dicaplateate manufactured by Estemol N-01: manufactured by Nisshin Oillio Co.
・ L-Glutamic acid: Ajinomoto Co., Inc. formula (3)

・ L-Arginine: Ajinomoto Co., Inc. formula (4)

・ Lactic acid Musashino lactic acid: manufactured by Musashino Chemical Research Institute ・ Potassium hydroxide aqueous solution 1M KOH: manufactured by Kishida Chemical Co., Ltd. ―Others―
-Methyl 4-hydroxybenzoate: manufactured by Kishida Chemical Co., Ltd.-86% glycerin Japanese Pharmacopoeia Glycerin: manufactured by Kao Corporation Tables 3 and 4 and Table 8 show the mixing conditions of the oily component and the aqueous component.

The Reynolds number is the pore diameter d (m) of the pores, the average flow velocity u (m / s) in the pipe calculated from the pore diameter of the pores and the flow rate of the fluid flowing through the pores, and water as a representative value of the aqueous component. It was calculated based on the above-mentioned Reynolds number calculation formula (Reynolds number Re = duρ / μ) using a viscosity μ: 0.001 (Pa · s) and a water density ρ: 1000 (kg / m ³ ).

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 as described above. 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 each Example or Comparative Example, and the absorbance of the solution 1 minute after mixing with respect to light having a wavelength of 353 nm was measured. The absorbance was measured using a spectrophotometer (device name: UVmini-1240 manufactured by Shimadzu Corporation). Then, the segregation index (Xs) was calculated from the measurement result of the absorbance according to the above-mentioned equation (IV).

Tables 5 and 6 and Table 9 show the composition of the obtained dispersion and the average particle size of the droplet particles.

The average particle size of the droplet particles was determined as the median size of the oily component measured by the laser scattering / diffraction method using a laser diffraction / scattering type particle size distribution measuring device LA-920 (manufactured by Horiba Seisakusho Co., Ltd.). In the measurement, a flow type measurement cell was used, and the measurement was performed at 25 ° C. using a circulation speed of 4 and a relative refractive index (dispersive refractive index / dispersion medium refractive index): 1.20.

<Example 1>
As an oil component, 8.00% by mass of 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol, which is a secondary amine which is a cationic surfactant A, and monocapric acid, which is an oil agent B, are used. A uniform solution containing 51.60% by mass of glycerin and 40.40% by mass of 2-octyldodecanol, which is an oil agent B, was prepared and charged into the oil component storage tank 41b. Therefore, the content of the surfactant A in the oily component is 8.00% by mass, and the content of the oily agent B is 92.00% by mass. The total content of the surfactant A and the oil agent B in the oily component is 100% by mass, and the mass ratio of the surfactant A to the oil agent B is 0.09. This oily component was a liquid at room temperature (25 ° C.).

As aqueous components, the neutralizing agent C, L-glutamic acid, was 0.13% by mass, methyl 4-hydroxybenzoate was 0.21% by mass, 86% glycerin was 21.05% by mass, and ion-exchanged water was 78. A uniform solution containing 61% by mass of each was prepared and charged into the aqueous component storage tank 41a. Therefore, the content of the neutralizing agent C in the aqueous component is 0.13% by mass.

Then, the dispersion liquid production system S is operated so that the mixed mass ratio of the aqueous component / oil component becomes 95.0 / 5.0 (= 19.0) at room temperature (25 ° C.) in the micromixer 100. , The flow rate of the oily component is 0.17 L / h and the flow rate of the aqueous component is 2.83 L / h, therefore the mixed flow rate ratio of the aqueous component / oily component is 16.6 and the flow rate of the fluid flowing through the pores 22 is 3. A dispersion (emulsion) was obtained by mixing an oily component and an aqueous component at .00 L / h.

In the merged fluid, the molar equivalent ratio of the neutralizing agent C to the surfactant A (neutralizing agent C / surfactant A) is 0.79. The content (mass%) of the surfactant A x molar equivalent ratio (neutralizing agent C / surfactant A) / oil agent B content (mass%) is 0.065. The Reynolds number of the fluid in the pores 22 of the micro mixer 100 is 4.8 × 10 ^3. For the calculation of the Reynolds number, the in-pipe average flow velocity u: 21.9 m / s calculated from the pore diameter d ₁ : 0.22 mm and the fluid flow rate: 3.00 L / h was used. The pressure loss before and after the pores 22 of the micromixer 100 was 0.75 MPa.

The content of each component in the obtained dispersion was 0.40% by mass for 1- (2-hydroxyethylamino) -3-isostearyloxy-2-propanol, 2.58% by mass for glycerin monocaprate, and 2-octyldodecanol is 2.02% by mass, L-glutamic acid is 0.12% by mass, methyl 4-hydroxybenzoate is 0.20% by mass, and glycerin is 20.0% by mass (86% glycerin equivalent, the same applies hereinafter). ), And ion-exchanged water was 74.68% by mass.

The average particle size of the droplet particles of the oily component in the obtained dispersion was 0.167 μm.

<Examples 2 to 9>
In Examples 2 to 9, the oil-based component and the aqueous component having the compositions shown in Table 1 were used, and the dispersion liquid production system S was operated under the conditions shown in Table 3 in the same manner as in Example 1, and the dispersion liquid shown in Table 5 was operated. (Emulsion) was obtained.

Segregation index in the dispersion procedure of Example 6-8 _{(X S)} was 3.4 × ^{10 -3.} The I ₃ ^- ion after 1 minute of mixing was 3.94 × ^10-6 mol / L, which was 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 3.13 × 10 ^-7 mol / L, respectively, so Y was 9.95 × 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.

<Comparative Examples 1 to 4>
In Comparative Examples 1 to 4, as shown in Table 2, oily components and aqueous components having the same composition as in Examples 1 to 4 were prepared, mixed in a beaker, and then 8000 r / min using a homomixer. The mixture was mixed at the same rotation speed for 1 minute to obtain a dispersion (emulsion) shown in Table 6. At this time, in Comparative Examples 1 to 3, 40.0 g of the oily component and 760.0 g of the aqueous component were mixed (mixed mass ratio of aqueous component / oily component: 95.0 / 5.0 (= 19.0)). .. In Comparative Example 4, 37.4 g of the oily component and 762.6 g of the aqueous component were mixed (mixed mass ratio of aqueous component / oily component: 95.3 / 4.7 (= 20.3)).

Segregation index in the dispersion operation of Comparative Example 1 to 4 _{(X S)} was 2.3 × ^{10 -1.} The I ₃ ^- ion after 1 minute of mixing was 2.68 × 10 ^-4 mol / L, which was a value obtained from the absorbance with respect to light having a wavelength of 353 nm. ^{Also, [H} _{+] 0} and so _{[I 2]} were, respectively, 0.171 mol / L and ^{2.13 × 10 -5 mol / L,} Y was 6.76 × ^{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. This also applies to Comparative Examples 7 to 10 described later.

<Comparative Examples 5 and 6>
In Comparative Examples 5 and 6, the oily component and the aqueous component having the compositions shown in Table 2 were used, and the dispersion liquid production system S was operated under the conditions shown in Table 4 in the same manner as in Example 1, and the dispersion liquid shown in Table 6 was operated. (Emulsion) was obtained. In Comparative Examples 5 and 6, the surfactant A was not contained in the oily component but was contained in the aqueous component.

<Comparative Examples 7-9>
In Comparative Examples 7 to 9, as shown in Table 2, oily components and aqueous components having the same composition as in Examples 6 to 8 were prepared, mixed in a beaker, and then 8000 r / min using a homomixer. The mixture was mixed at the same rotation speed for 1 minute to obtain a dispersion (emulsion) shown in Table 6. At this time, in Comparative Example 7, 38.4 g of the oily component and 761.6 g of the aqueous component were mixed (mixed mass ratio of aqueous component / oily component: 95.2 / 4.8 (= 19.8)). In Comparative Example 8, 44.8 g of the oily component and 755.2 g of the aqueous component were mixed (mixed mass ratio of the aqueous component / oily component: 94.4 / 5.6 (= 16.9)). In Comparative Example 9, 40.0 g of the oily component and 760.0 g of the aqueous component were mixed (mixed mass ratio of aqueous component / oily component: 95.0 / 5.0 (= 19.0)).

<Comparative Example 10>
In Comparative Example 10, the oily component and the aqueous component having the composition shown in Table 2 were prepared, and after 52.8 g of the oily component and 747.2 g of the aqueous component were mixed in a beaker (mixed mass ratio of the aqueous component / oily component). : 93.4 / 6.6 (= 14.2)), mixed for 1 minute at a rotation speed of 8000 r / min using a homomixer to obtain a dispersion (emulsion) shown in Table 6. In Comparative Example 10, a large amount of surfactant A was contained in the oily component, and a dispersion was prepared using a homomixer.

<Comparative Example 11>
In Comparative Example 11, using the oily component and the aqueous component having the compositions shown in Table 2, the dispersion liquid production system S was operated under the conditions shown in Table 4 in the same manner as in Example 1, and the dispersion liquid (emulsification) shown in Table 6 was operated. I got a thing). In Comparative Example 11, the oily component did not contain the surfactant A, the aqueous component contained a large amount of the surfactant A, and a dispersion liquid was prepared using the micromixer 100.

<Examples 10 to 17>
In Examples 10 to 17, as shown in Table 7, the dispersion liquid production system S was operated under the conditions shown in Table 8 using the oily component and the aqueous component having the same composition as those used in Example 1, and the dispersion liquid production system S is shown in Table 9. A dispersion (emulsion) was obtained.

(Result consideration)
The first configuration is an oily component containing a surfactant having a neutralizable functional group and an oily agent, and an aqueous component containing a neutralizing agent C having a salt-forming ability with the surfactant A contained in the oily component. In Examples 1 to 9, the molar equivalent ratio of the neutralizing agent C to the surfactant A (neutralizing agent C / surfactant A) was 0.5 or more, which was mixed and dispersed by the micromixer 100 of the above. The average particle size of the droplet particles of the oily component in the obtained dispersion was 1 μm or less.

Comparing Example 1 and Comparative Example 1, the average particle size of the droplet particles of the oily component in the dispersion obtained by using the micromixer 100 in Example 1 was obtained by using the homomixer in Comparative Example 1. It can be seen that the average particle size of the droplet particles of the oily component in the obtained dispersion is 1/10 or less. Further, even if the amount of the surfactant A is 5 times that of Comparative Example 1 as in Comparative Example 10, a dispersion liquid in which fine droplet particles of an oily component are dispersed in an aqueous component as obtained in Example 1 is obtained. It turns out that you can't get it.

Comparing Example 1 with Comparative Example 5 in which the surfactant A was included in the aqueous component, the average particle size of the droplet particles of the oily component in the dispersion obtained in Example 1 was found in Comparative Example 5. It can be seen that the average particle size of the droplet particles of the oily component in the obtained dispersion is 1/10 or less. Further, even if the amount of the surfactant A is about four times that of Comparative Example 5 as in Comparative Example 11, a dispersion liquid in which fine droplet particles of an oily component are dispersed in an aqueous component as obtained in Example 1. It turns out that you can't get.

In Example 5, although the amount of the surfactant A is reduced to 1/4 of that of Example 1, it can be seen that a dispersion liquid in which fine droplet particles of the oily component are dispersed in the aqueous component can be sufficiently obtained. ..

According to Examples 10 to 17, it can be seen that even when the micromixer 100 having the second to fourth configurations is used, a dispersion liquid in which fine droplet particles of an oily component are dispersed in an aqueous component can be obtained.

The present invention is useful for methods of producing dispersions.

S Dispersion liquid production system 100 Micromixer 101 Aqueous component supply unit 102 Oil component supply unit 103 Dispersion liquid recovery unit 110 Straight pipe part 111 1st pipe 112 2nd pipe 113 3rd pipe 120 Branch pipe part 130 Plate-shaped member 10 Fluid flow Road portion 11 Small diameter pipe 11a First flow path 11b Pipe end part 12 Large diameter pipe 12a Second flow path 20 Fluid merging condensing part 21 Fluid merging area 22 Pore 30 Fluid outflow part 31 Flow path expanding 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 flow meter 44b Second flow meter 45a First filter 45b Second filter 46a First pressure gauge 46b Second pressure gauge 47 Flow controller 48 Dispersion fluid recovery pipe 49 Dispersion fluid recovery tank

Claims (10)

A merging step of merging an oily component containing a surfactant having a neutralizable functional group and an oil agent as a main component, and an aqueous component containing a neutralizing agent having a salt-forming ability with the surfactant.
A hole circulation step in which the fluid merged in the merging step is circulated in the hole,
Including
The dispersion operation of the aqueous component and the oily component is performed under the condition that the segregation index (Xs) is 0.1 or less, and the surfactant is neutralized with the neutralizing agent in the merged fluid. A method for producing a dispersion
A method for producing a dispersion liquid in which, in the merging step, the oily component is merged with the aqueous component flowing out from a flow path having a flow path diameter larger than the pore diameter of the hole from the entire circumference thereof . A merging step of merging an oily component containing a surfactant having a neutralizable functional group and an oil agent as a main component, and an aqueous component containing a neutralizing agent having a salt-forming ability with the surfactant.
A hole circulation step in which the fluid merged in the merging step is circulated in the hole,
Including
The dispersion operation of the aqueous component and the oily component is performed under the condition that the segregation index (Xs) is 0.1 or less, and the surfactant is neutralized with the neutralizing agent in the merged fluid. A method for producing a dispersion
In the merging step, the oily component and the aqueous component are made to collide and merge.
A method for producing a dispersion liquid in which in the pore flow step, the extending direction of the pores through which the fluid merged in the merging step is circulated is different from the flow directions of the aqueous component and the oil component. The method for producing a dispersion according to claim 1 or 2, wherein the surfactant has an amino group and a hydrophobic group, and the neutralizing agent is an acidic compound. The surfactant has one or more functional groups and hydrophobic groups selected from the group consisting of a carboxy group, a sulfonic acid group, a phosphonic acid group, and a phosphoric acid group, and the neutralizing agent is a base. The method for producing a dispersion according to any one of claims 1 to 3 , which is a sex compound. The method for producing a dispersion according to any one of claims 1 to 4 , wherein the mass ratio (surfactant / oil) of the surfactant to the oil in the oily component is 0.15 or less. The dispersion according to any one of claims 1 to 5 , wherein the molar equivalent ratio (neutralizing agent / surfactant) of the neutralizing agent to the surfactant in the merged fluid is 0.3 to 5. Liquid manufacturing method. The dispersion according to any one of claims 1 to 6 , 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 to 200. Manufacturing method. Wherein the hole distribution step, the flow rate of the 0.1~300L / h of the fluid when circulating the in merging step are merged with said aqueous component and the oily component fluid in the hole, according to claim 1 to 7 The method for producing a dispersion liquid according to any one of. The method for producing a dispersion liquid according to any one of claims 1 to 8 , wherein the pressure loss is 1.5 MPa or less in the pore flow step. The method for producing a dispersion liquid according to any one of claims 1 to 9 , wherein the average particle size of the particles contained in the produced dispersion liquid is 0.01 to 1 μm.

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