JPH09168734A - Preparation of emulsion - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain emulsion having desired viscosity in a condition of small particle size change by controlling only a cooling velocity near an emulsion transition temperature. SOLUTION: Emulsion having desired viscosity is prepared by a method comprising an emulsification process (1) in which (A) a component of 0.1-30wt.% of quaternary ammonium salt, (B) a component of 0.1-30wt.% of higher alcohol, and (C) a residual component of water are mixed to be emulsified and a process (2) in which the emulsion obtained by the process (1) is cooled by controlling only a cooling velocity near an emulsion transition temperature to control the viscosity in a condition of small particle size change of the emulsion.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a method for producing an emulsion. In particular, the present invention relates to a method for producing an emulsion having a desired viscosity in a state where the change in particle size is small.

[0002]

2. Description of the Related Art As a method for producing an emulsion, Japanese Patent Laid-Open No.
No. 154367, "As a conventional method for producing an emulsion, an aqueous phase, an oil phase, and other compounds are charged in a stirring tank having a stirring function, and the mixture is heated, stirred, and mixed to emulsify the desired particle size. There is a batch-type production method in which a product is produced and cooled to stabilize the emulsion. " A method for supplying a preliminary emulsion to produce a preliminary emulsion, and stirring and mixing the preliminary emulsion and the remaining aqueous phase and / or oil phase, which is used in an emulsifier when producing the preliminary emulsion. The average particle diameter of the emulsion can be controlled by changing the feed rate of raw materials and the operating conditions. There is no description and no suggestion of controlling the viscosity of the emulsion.

Further, in Japanese Patent Publication No. Hei 5-500988, a mixture containing an oil component, water, an emulsifier component, etc. is emulsified and the emulsion thus formed is heated at a phase inversion temperature range or higher. A stable low-viscosity emulsion can be prepared by emulsifying the mixture in a phase inversion temperature range or higher and cooling the obtained emulsion to a temperature lower than the above temperature range. , O / W
It is a technique for preparing a rust-preventive emulsion, and unlike the present invention, there is no description or suggestion of controlling the viscosity of the emulsion by controlling the cooling rate in the vicinity of the emulsification transition temperature of the emulsion. .

Further, it is possible to control the viscosity of the emulsion by controlling the particle size of the emulsion, and there is a composition in which there is a correlation between the particle size of the emulsion and the viscosity. It is known that when the particle size of the emulsion changes, for example, the amount of adsorption changes in hair rinses, softeners for clothing, etc., and as a result, its performance changes, so changing the particle size to control viscosity It means that the original performance will change.

[0005] An object of the present invention is to solve the above problems.
An object of the present invention is to provide a method for producing an emulsion, in which the viscosity of the emulsion is controlled while the change in the particle size of the emulsion is small.

[0006]

The inventors of the present invention have conducted extensive studies to solve the above-mentioned problems, and as a result, in the production of an emulsion, in the composition of a specific emulsion, the vicinity of the emulsification transition temperature of the emulsion By controlling the cooling rate of, the inventors have found that the viscosity of the emulsion can be controlled without changing the particle size of the emulsion, and have completed the present invention.

That is, the gist of the present invention is: (1) Production of an emulsion containing the following components (A), (B) and (C), which is characterized by having the following steps (i) and (ii): Method, (A) quaternary ammonium salt 0.1 to 30% by weight (B) higher alcohol 0.1 to 30% by weight (C) residual amount of water (i): component (A), component (B) and ( C) mixing the components and emulsifying, (ii): the emulsion obtained in the step (i) is used to control the viscosity of the emulsion in a state where the change in particle diameter of the emulsion is small. A step of cooling by controlling only the cooling rate in the vicinity of the emulsification rearrangement temperature, (2) The component (A) contains the quaternary ammonium salt of at least branched chain in an amount of 0.05 to 20% by weight. (3) An emulsion containing the following component (D) in addition to the above emulsion: The method for producing an emulsion according to the above (1) or (2), wherein (D) glyceryl etherified polyhydric alcohol 0.01 to 10% by weight, (4) component (C) is divided and a part of the step ( The method for producing an emulsion according to (1) to (3), which is used as a refrigerant in ii), (5) within a temperature range of ± 10 ° C. of the emulsification transition temperature, and a cooling rate of 0.05 to 5 ° C./min. The method for producing an emulsion according to (1) to (4), wherein the method is controlled within the range.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION A method for producing an emulsion of the present invention will be described. That is, the production method of the present invention comprises the following (A)
(B) An emulsion containing the components (C) is prepared by: (A) quaternary ammonium salt 0.1 to 30% by weight (B) higher alcohol 0.1 to 30% by weight (C) water remaining amount It is characterized by being manufactured by (i) and (ii). (I): a step of mixing and emulsifying the component (A), the component (B) and the component (C), (ii): the emulsion obtained in the step (i) is prepared in the vicinity of the emulsification transition temperature of the emulsion. The process of cooling by controlling the cooling rate.

As the component (A), the following general formula (I) is used.

[0010]

Embedded image

(In the formula, R ₁ represents a straight or branched chain saturated or unsaturated hydrocarbon group having 8 to 28 carbon atoms, and R ₂ represents a straight chain or branched chain saturated or unsaturated group having 1 to 3 carbon atoms or An unsaturated hydrocarbon group or a linear or branched saturated or unsaturated hydrocarbon group having 8 to 28 carbon atoms is shown, and R ₃ and R ₄ are each 1 to 3 carbon atoms.
A linear or branched saturated or unsaturated hydrocarbon group, wherein X represents a chlorine or bromine atom)
Secondary ammonium salts.

R ₁ in the general formula (I) has 8 to 2 carbon atoms.
8 alkyl groups, alkenyl groups and the like. For example, stearyl, hexadecyl, behenyl, oleyl,
Dodecyl, octadecyl, decyl tetradecyl, dodecyl hexadecyl, octyl dodecyl, methyl dodecyl,
Methyl tetradecyl, methyl undecyl, methyl tridecyl and the like can be mentioned. R ₂ is an alkyl group having 1 to 3 carbon atoms, an alkenyl group or the like, or an alkyl group having 8 to 28 carbon atoms,
Examples thereof include an alkenyl group. For example, methyl, ethyl, propyl, isopropyl, isopropyl, stearyl, hexadecyl, behenyl, oleyl, dodecyl, octadecyl, decyltetradecyl, dodecylhexadecyl, octyldodecyl, methyldodecyl, methyltetradecyl, methylundecyl, methyltridecyl and the like. To be Examples of R ₃ and R ₄ include alkyl groups and alkenyl groups having 1 to 3 carbon atoms. For example, methyl, ethyl, propyl, isopropyl and the like can be mentioned.

Specific examples of the above quaternary ammonium salt include dilauryldimethylammonium chloride, hexadecyltrimethylammonium chloride, stearyltrimethylammonium chloride, distearyldimethylammonium chloride, diisostearyldimethylammonium chloride and oleyltrimethylammonium. Chloride, dioleyl dimethyl ammonium chloride,
Behenyltrimethylammonium chloride, dodecyltrimethylammonium chloride, dioctadecyldimethylammonium chloride, octadecylhexadecyldimethylammonium chloride, 2-hexyldecyltrimethylammonium chloride, 2-decyltetradecyltrimethylammonium chloride, 2-dodecylhexadecyltrimethylammonium chloride, di 2-hexyldecyldimethylammonium chloride, di-2-octyldodecyldimethylammonium chloride, 2-methyldodecyltrimethylammonium chloride, 2-methyltetradecyltrimethylammonium chloride, di-2-methylundecyldimethylammonium chloride, di-2 -Methyltridecyldimethylammonium chloride, etc. Chill ethyl, which became propyl or isopropyl, such as those chloride becomes bromide and the like. Among them, dilauryldimethylammonium chloride, hexadecyltrimethylammonium chloride, stearyltrimethylammonium chloride, distearyldimethylammonium chloride, 2
-Hexyldecyltrimethylammonium chloride, 2
-Decyltetradecyltrimethylammonium chloride, 2-dodecylhexadecyltrimethylammonium chloride, di-2-hexyldecyldimethylammonium chloride, di-2-methylundecyldimethylammonium chloride, di-2-methyltridecyldimethylammonium chloride are preferred. Particularly preferred are dilauryldimethylammonium chloride, stearyltrimethylammonium chloride, 2-hexyldecyltrimethylammonium chloride, di-2-methylundecyldimethylammonium chloride and di-2-methyltridecyldimethylammonium chloride.

The content of the component (A) in the composition is 0.1 to 30% by weight, preferably 0.2 to 20% by weight. 0.1% by weight or more is preferable to obtain a stable emulsion, and 30% by weight to make the viscosity easy to handle.
The following is preferred.

Of the above-mentioned component (A), in the above general formula (I), R ₁ and R ₂ are the same as those in the general formula (III).

[0016]

Embedded image

(Wherein R ₅ represents a methyl group or an ethyl group, and m represents a number such that the total number of carbon atoms in the alkyl group is 8 to 16) and a compound (a) represented by the general formula (IV) CH _3- (CH ₂ ) _-n (IV) (wherein n represents a number such that the total number of carbon atoms in the alkyl group is 8 to 16), and a mixture with the compound (b), and
(Amount of compound (a) / (amount of compound (a) + compound (b))
Amount)), the branching ratio of R ₁ and R ₂ is 10 to 100.
The branched chain quaternary ammonium salt (hereinafter,
(Referred to as component (A ')) is preferred.

Alternatively, in the above general formula (I), R
₁ is the general formula (V)

[0019]

Embedded image

(Wherein R ₆ and R ₇ represent an alkyl group having 2 to 12 carbon atoms), R ₂ is a compound represented by the general formula (V) or an alkyl group having 1 to 3 carbon atoms. Branched quaternary ammonium salt group ((A ') component)
Is preferred. The use of the component (A ′) is preferable from the viewpoint of controlling the viscosity by further reducing the change in particle diameter, and the amount thereof is at least 0.05 to 20% by weight, preferably at least 0.05 to 15% by weight. And at least 0.
Particularly preferably, it is from 05 to 10% by weight. The amount is preferably 0.05% by weight or more in order to obtain the effect of further reducing the change in particle size, and is preferably 20% by weight or less in order to make the viscosity easy to handle. Further, as the component (A), it is effective to share the component (A ′) with a compound other than that in order to obtain a desired emulsion.

Specific examples of the above-mentioned branched quaternary ammonium salt include 2-hexyldecyltrimethylammonium chloride, 2-decyltetradecyltrimethylammonium chloride, 2-dodecylhexadecyltrimethylammonium chloride and di-2-. Hexyldecyldimethylammonium chloride, di-2-octyldodecyldimethylammonium chloride, 2-methyldodecyltrimethylammonium chloride, 2-methyltetradecyltrimethylammonium chloride, di-2-methylundecyldimethylammonium chloride, di-2-methyltri Examples thereof include decyldimethylammonium chloride and the like, in which methyl is ethyl, propyl or isopropyl, and chloride is bromide. Among them, 2-hexyldecyltrimethylammonium chloride, 2-decyltetradecyltrimethylammonium chloride, 2-dodecylhexadecyltrimethylammonium chloride, di-2-hexyldecyldimethylammonium chloride, di-2-methylundecyldimethylammonium chloride, di- 2-Methyltridecyldimethylammonium chloride is preferred, especially 2
-Hexyldecyltrimethylammonium chloride, di-2-methylundecyldimethylammonium chloride, di-2-methyltridecyldimethylammonium chloride are preferred.

As the component (B), the following general formula (II) R ₈ --OH (II) (wherein R ₈ is a straight chain or branched chain saturated or unsaturated hydrocarbon having 12 to 26 carbon atoms) is used. And a higher alcohol represented by the formula (1). R ₈ in the general formula (II) is not a high melting point from the viewpoint of energy loss, and is not particularly limited as long as it is a higher alcohol having a carbon number of 26 or less in order to make the viscosity easy to handle. And an alkyl group and an alkenyl group thereof.

Specific examples of the above-mentioned higher alcohols include:
Examples thereof include cetyl alcohol, stearyl alcohol, behenyl alcohol, dodecyl alcohol and the like, among which cetyl alcohol, stearyl alcohol and behenyl alcohol are preferable. Particularly, cetyl alcohol and stearyl alcohol are preferable. Note that a mixture of these can also be used.

The content of the component (B) in the composition is 0.1 to 30% by weight, preferably 0.2 to 20% by weight, more preferably 0.3 to 10% by weight. is there. It is preferably 0.1% by weight or more for obtaining a stable emulsion, and 30% by weight or less for making the viscosity easy to handle.

Examples of the water as the component (C) include purified water,
Examples include ion-exchanged water. The blending amount of component (C) is
The amount of the component (A) (including the component (A ′)), the component (B), and the component (D) described later is appropriately adjusted as the remaining amount in the composition.

When the component (A ') is used in addition to the above components, the component (D) can be represented by the general formula (V
I) G [(AO) _a B] _b (VI) (In the formula, G represents a residue excluding hydrogen atoms of all hydroxyl groups in a polyhydric alcohol having 4 or more hydroxyl groups,
A represents an alkylene group having 2 to 4 carbon atoms, one end of which is an ether bond with an oxygen atom derived from a hydroxyl group of a polyhydric alcohol having four or more hydroxyl groups, and the other end of which is bonded to an oxygen atom. Is a group that is bonded to a terminal oxygen atom in the —AO— group or a group that is bonded to an oxygen atom derived from a hydroxyl group of a polyhydric alcohol having four or more hydroxyl groups, and is a hydrogen atom or the general formula (VII).

[0027]

Embedded image

And / or general formula (VIII)

[0029]

Embedded image (In the formula, R ₉ represents a branched chain alkyl group having 16 to 36 carbon atoms. However, at least one of b B groups is represented by the general formula (VII) and / or (VIII). A) is the total number of moles of alkylene oxide added to the hydroxyl groups of a polyhydric alcohol having 4 or more hydroxyl groups / b, the number is 0 to 10, and b is 4 or more hydroxyl groups. The glyceryl etherified polyhydric alcohol represented by (indicates the number of hydroxyl groups in the polyhydric alcohol).

Specific examples of the glyceryl etherified polyhydric alcohol as the component (D) include pentaerythritol isostearyl glycidyl ether, sorbitol isostearyl glycidyl ether and mannitol.
2-octyldodecyl glycidyl ether, methyl glucoside isostearyl glycidyl ether, methyl glucoside 2-octyl dodecyl glycidyl ether,
Maltitol 2-decyl tetradecyl glycidyl ether, 2,3-dihydroxypropyl glucoside isostearyl glycidyl ether, diglycerin isostearyl glycidyl ether, tetraglycerin isostearyl glycidyl ether, diglycerin 2-octyldodecyl glycidyl ether, Examples include ethyl glucoside / isostearyl glycidyl ether, methyl glucoside / 2-heptylundecyl glycidyl ether, and the like. Of these, pentaerythritol isostearyl glycidyl ether, sorbitol isostearyl glycidyl ether, and mannitol 2-octyldodecyl glycidyl ether are preferable, and pentaerythritol isostearyl glycidyl ether is particularly preferable.

By adding such a component (D),
The viscosity of the emulsion can be controlled in a wider range only by controlling the cooling rate in the vicinity of the emulsion transition temperature without changing the particle size. The content of the component (D) in the composition is preferably 0.01 to 10% by weight, more preferably 0.03 to 7% by weight,
Particularly, 0.05 to 5% by weight is preferable. To control the viscosity of the emulsion in a wider range, 0.01% by weight or more is preferable, and 10% by weight or less is preferable to make the viscosity easy to handle.

Furthermore, the following optional components (hereinafter,
(E) component) can be added. That is, solvents such as ethyl alcohol, propylene glycol, glycerin, diethylene glycol monoethyl ether, ethyl diglycol ether, benzyloxyethanol, citric acid, lactic acid, phosphoric acid, hydrochloric acid, caustic soda, triethanolamine, and other pH adjusting agents, parabens. Antiseptics such as, vitamins, anti-dandruff agents and other medicinal agents, hydroxyethyl cellulose, thickeners such as water-soluble polymers such as carboxymethyl cellulose, flavoring agents such as fragrances, coloring agents such as dyes and pigments,
Conditioning agents such as cationic polymers, methylpolysiloxanes and amino-modified silicones, and liquid agents such as liquid paraffin, glycerides, lanolin derivatives, esters, and higher fatty acids.

Suitable emulsions containing the above-mentioned components and obtained by the production method of the present invention include the following. That is, (1) the component (A) is 0.1 to 30% by weight (preferably 0.2 to 20% by weight), and the component (B) is 0.1 to 30% by weight (preferably 0.2 to 20% by weight). %, More preferably 0.3 to 10% by weight), the remaining amount of the component (C), (2) 0.1 to 30% by weight of the component (A) (preferably 0.2 to 20% by weight), ( Of the component (A), at least the component (A ') is 0.05 to 20% by weight (preferably 0.1%).
(05 to 10% by weight), 0.1 to 30% by weight of the component (B)
(Preferably 0.2 to 20% by weight, more preferably 0.3 to 10% by weight), component (C) is the balance, (3) component (A) is 0.1 to 30% by weight (preferably 0). .2 to 20% by weight), and at least (A ') component in the component (A) is 0.05 to 20% by weight (preferably 0.
(05 to 10% by weight), 0.1 to 30% by weight of the component (B)
(Preferably 0.2 to 20% by weight, more preferably 0.3 to 10% by weight), component (D) is 0.01 to 10% by weight (preferably 0.03 to 7% by weight, further preferably 0). .05 to 5% by weight) and the balance of the component (C).

In the present invention, in the case of producing the emulsion of (1) above, by controlling only the cooling rate in the range near the emulsification transition temperature of the emulsion, the change in the particle size of the emulsion is small. It is possible to control the viscosity of the emulsion in the state, and in the case of producing the emulsion of the above (2), it is possible to further reduce the particle size change of the emulsion and control the viscosity of the emulsion. Therefore, in the case of producing the emulsion of (3) above, it is possible to control the viscosity of the emulsion in a wider range by reducing the change in particle diameter of the emulsion. In addition, in order to obtain a desired emulsion, it is possible to add the component (E) to the above emulsion.

In step (i), the components of (A) to (C) are
The emulsion is mixed and emulsified at a temperature higher than the emulsification transition temperature of the emulsion. The temperature equal to or higher than the emulsification rearrangement temperature means a range of 5 to 20 ° C. higher than the emulsification rearrangement temperature, preferably 5
~ 15 ° C. In order to obtain a good emulsion having a sharp particle size distribution, 5 ° C or higher is preferable, and 20 ° C or lower is preferable from the viewpoint of energy loss. The following method can be adopted as a method of adding each component. That is, in the case of batch formulation, (a): a mixture of the components (A) and (B),
A method in which the component (C) is added, mixed and emulsified. (B): A method in which a mixture of the components (A) and (B) is added to the component (C), and the mixture is emulsified. (C): A mixture of the components (A) and (B),
A method in which a mixture of the components (A) and (C) is added, mixed and emulsified. (D): In a mixture of the components (A) and (C),
A method in which a mixture of the components (A) and (B) is added, mixed and emulsified. Among these, (b) and (d)
The method (1) is preferable because it can be blended with a low viscosity ((A) and (C) have a higher viscosity during the blending).

In the continuous blending, (e): a method in which the mixture of the components (A) and (B) and the component (C) are simultaneously added, mixed and emulsified. (F): A method in which a mixture of the components (A) and (C) and the component (B) are simultaneously added, mixed and emulsified. (G): A mixture of the (A) component and the (B) component,
A method in which the component (A) and the component (C) are mixed and emulsified are added simultaneously and mixed to emulsify. (H): A method in which the components (A), (B), and (C) are individually supplied, simultaneously added, mixed, and emulsified. Among these, the methods (e) and (f) are preferable from the viewpoint of equipment and control, and the method (e) is particularly preferable because the melting point of the mixture of the component (A) and the component (B) is the component (B). It is preferable from the standpoint of obtaining a product having a sharper particle size distribution than that of the above.

The following can be said in both cases of batch blending and continuous blending. That is, the above method can be applied even when the component (A) is supplied in the form of a solution. Further, the component (D) is used by adding it to the component (B), and when the component (E) is added, a lipophilic component such as propylene glycol or glycerin is added to the component (B), and hydroxyethyl cellulose, It is preferable that a water-soluble component such as carboxymethyl cellulose or citric acid is added to the component (C), and a component such as ethanol or a fragrance having a heat stability problem is added after emulsification and cooling. Further, the component (C) may be used as the refrigerant in the step (ii) in addition to the case where the entire amount of the component (C) is used in the step (i).

The step (ii) is a step of cooling the emulsion obtained in the step (i) to a temperature equal to or lower than the emulsification rearrangement temperature of the emulsion, particularly in the vicinity of the emulsion rearrangement temperature in order to obtain an emulsion having a desired viscosity. The cooling rate is controlled only to the cooling rate corresponding to the desired viscosity. Therefore, in the present invention, only the cooling rate in the vicinity of the emulsification transition temperature need be controlled in order to obtain the desired viscosity, the cooling rate in the cooling step before and after the vicinity of the emulsification transition temperature does not need to be accurately controlled, and, for example, emulsification There is also an advantage that productivity is improved by rapidly cooling the steps around the dislocation temperature. The emulsification rearrangement temperature is, for example, about 50 to 70 ° C. although it varies depending on various components used, and the vicinity of the emulsification rearrangement temperature means a range of ± 10 ° C. of the temperature, particularly a cooling rate in the range of ± 5 ° C. It is preferable to control. During cooling, a part of the component (C) may be used for emulsification (step (i)) and the rest may be used as a refrigerant in this step. In this case, the cooling rate near the emulsion rearrangement temperature may be controlled by adjusting the addition rate of the component (C) used as a refrigerant. Further, the cooling rate in the cooling step before and after the vicinity of the emulsification dislocation temperature may be controlled by adjusting the addition rate of the component (C). The present invention is characterized in that only the cooling rate in the vicinity of the emulsification transition temperature is intentionally controlled to a cooling rate corresponding to the desired viscosity in order to obtain an emulsion having a desired viscosity. The lower the viscosity, the higher the viscosity, and the slower the cooling rate, the higher the viscosity. Although this has not been specifically clarified, it can be considered as follows. That is, the degree of liquid crystal growth of the emulsion differs depending on the difference in cooling rate. The slower the cooling rate, the more the liquid crystal grows, and as a result, the resistance between the emulsified particles increases and the viscosity increases. It is considered that the growth of the liquid crystal occurs during the cooling process at an emulsification transition temperature of about ± 10 ° C.

In the present invention, although it depends on various components used, for example, the cooling rate is 0.05 to 5 ° C. /
By controlling in the range of min, 500-100,
It is possible to adjust the viscosity in the range of 000 cP.
Furthermore, in the case of obtaining an emulsion having the same composition, when controlling only the cooling rate near the emulsification transition temperature, the viscosity can be controlled within the range shown by the following formula. 1.5 ≦ A / B ≦ 15 A: Viscosity obtained at a cooling rate of 0.05 ° C./min B: Viscosity obtained at a cooling rate of 5 ° C./min Further, the cooling rate other than near the emulsification transition temperature is particularly limited. Although it is not performed, it is generally preferable to perform rapid cooling because the production capacity is increased, but it is preferable to set it appropriately according to the situation because the cooling rate is practically economical in terms of equipment.
The emulsion dislocation temperature can be measured by using a DSC (inspection scanning calorimeter: manufactured by Seiko Denshi Kogyo Co., Ltd.).

[0040]

The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples. The viscosity and the particle size shown in the examples are measured by the following methods.

(1) Viscosity The sample was placed in a constant temperature bath at 30 ° C., the temperature of the sample was kept at 30 ° C., and the viscosity (cP) was measured with a B type viscometer (Tokyo Keiki Co., Ltd.).
Was measured. When bubbles were mixed in the sample, the sample was defoamed by centrifugation.

(2) Particle size (median size) 10 ml of the sample was diluted with water to 100 ml, and then measured using a laser diffraction particle size distribution analyzer LA-700 manufactured by Horiba Ltd.

Example 1 Using the components (A), (B), (C) and (E) shown in Table 1, an emulsion was produced by the following method. In step (i), the oil phase component of component (A), component (B) and component (E), propylene glycol, is mixed and the emulsion rearrangement temperature of this mixture (measured by the above-mentioned method is 61 ° C.). The above-mentioned aqueous phase which was uniformly heated to 75 ° C. and the remaining components (excluding perfume) of the components (C) and (E) were uniformly heated to 75 ° C. and heated to 75 ° C. The oil phase component heated to 75 ° C. was added to the component with stirring to emulsify. Then, as the step (ii),
As shown in Table 2, in the vicinity of the emulsification dislocation temperature (range of 56 to 66 ° C), the cooling rate was changed to further cool to 40 ° C. When cooled to 40 ° C., the fragrance of the component (E) was added and uniformly mixed to obtain a product (rinse). The viscosity and particle size of the products obtained by changing various conditions were measured, and the results are shown in Table 2. In addition, in the range of particle diameter 42 to 48 μm,
Viscosity 1900 to 3200 cP (1.7 times (= 3200 /
1900)).

[0044]

[Table 1]

[0045]

[Table 2]

Example 2 (A) component, (A ') component, (B) component shown in Table 3
Using the components (C) and (E), the following method
An emulsion was produced. As the step (i), the component (A),
Component (A '), component (B) and component (E), the oil phase component of ethyl diglycol ether, are mixed and the emulsion rearrangement temperature of this mixture (measured by the above-mentioned method was 65 ° C.) or more Uniformly heated to 75 ° C., and the water phase components of the remaining components (excluding perfume) of the components (C) and (E) to 7
Heat uniformly to 5 ° C and add 75% to the water phase ingredients heated to 75 ° C.
The oil phase component heated to ℃ was added with stirring to emulsify. Subsequently, as shown in Table 4, in step (ii), the vicinity of the emulsification dislocation temperature (range of 60 to 70 ° C.) was changed to 40 ° C. by changing the cooling rate. When cooled to 40 ° C, the fragrance of the component (E) was added and uniformly mixed to obtain a product (treatment). The viscosity and particle size of the products obtained by changing various conditions were measured, and the results are shown in Table 4. In addition, in the range of particle diameter 30 to 32 μm, the viscosity is 9000
~ 22000cP (2.4 times (= 22000/900
It was possible to control in the range of 0)).

[0047]

[Table 3]

[0048]

[Table 4]

Example 3 (A) component, (A ') component, (B) component shown in Table 5
An emulsion was produced using the components (C), (D) and (E) by the following method. As step (i),
Component (A), component (A '), component (B), component (D) and component (E), the oil phase component of diethylene glycol monoethyl ether, are mixed and the emulsion rearrangement temperature of this mixture (measured by the above-mentioned method As a result, it was uniformly heated to 75 ° C. above 59 ° C., and the water phase components of the remaining components (excluding perfume) of the component (C) and the component (E) were uniformly heated to 75 ° C., The oil phase component heated to 75 ° C. was added to the water phase component heated to 75 ° C. with stirring to emulsify. Subsequently, as shown in Table 6, in step (ii), the vicinity of the emulsification dislocation temperature (range of 54 to 64 ° C.) was changed to 40 ° C. by changing the cooling rate. When cooled to 40 ° C., the fragrance of the component (E) was added and uniformly mixed to obtain a product (conditioner). The viscosity and particle size of the products obtained by changing various conditions were measured, and the results are shown in Table 6.
Incidentally, in the range of particle diameter 28 to 31 μm, the viscosity is 2500 to 8
It was possible to control in the range of 500 cP (3.4 times (= 8500/2500)).

[0050]

[Table 5]

[0051]

[Table 6]

Example 4 (A) component, (A ') component, (B) component shown in Table 7
An emulsion was produced using the components (C), (D) and (E) by the following method. As step (i),
Component (A), component (A '), component (B), component (D) and component (E), the oil phase component of propylene glycol, are mixed and the emulsification rearrangement temperature of this mixture (measured by the above-mentioned method is measured. , 63 ° C.) or higher to 75 ° C., and the remaining components (excluding perfume) of the components (C) and (E) are uniformly heated to 75 ° C. The oil phase component heated to 75 ° C. was added to the water phase component heated to 1 while stirring to emulsify. Then, as the step (ii),
As shown in Table 8, the vicinity of the emulsification dislocation temperature (in the range of 58 to 68 ° C) was further changed to 40 ° C by changing the cooling rate. When cooled to 40 ° C., the fragrance of the component (E) was added and uniformly mixed to obtain a product (rinse). The viscosity and particle size of the products obtained by changing various conditions were measured, and the results are shown in Table 8. In addition, in the range of particle diameter 14 to 16 μm,
Viscosity 1900-7000 cP (3.7 times (= 7000 /
1900)).

[0053]

[Table 7]

[0054]

[Table 8]

Example 5 (A) component, (A ') component, (B) component shown in Table 9
An emulsion was produced using the components (C), (D) and (E) by the following method. As step (i),
Component (A), component (A '), component (B), component (D) and component (E), ethyl diglycol ether, glycerin, and vaseline, which are oil phase components, are mixed and the emulsion transition temperature of the mixture (as described above) is mixed. It was heated to 75 ° C or higher, which was 65 ° C), and the aqueous phase components of hydroxyethyl cellulose (C) and (E) were uniformly heated to 75 ° C. 7 to the water phase ingredients heated to
The oil phase component heated to 5 ° C was added with stirring to emulsify. Subsequently, in step (ii), as shown in Table 10, the vicinity of the emulsification dislocation temperature (range of 60 to 70 ° C) was changed to 40 ° C by changing the cooling rate. When cooled to 40 ° C, the fragrance of the component (E) was added and uniformly mixed to obtain a product (treatment). The viscosity and particle size of the products obtained by changing various conditions were measured, and the results are shown in Table 1.
0 is shown. In addition, in the range of particle diameter 22 to 25 μm, the viscosity is 8
000-31000 cP (3.9 times (= 31000/8
000)).

[0056]

[Table 9]

[0057]

[Table 10]

Example 6 Using the components (A), (A '), (B), (C), (D) and (E) shown in Table 5 used in Example 3, the following components were used. An emulsion was produced by the method of. In step (i), the component (A), the component (A ′), the component (B), the component (D) and the component (E), the oil phase component of diethylene glycol monoethyl ether, are mixed and the emulsion transition temperature of the mixture is mixed. (As a result of measurement by the above-mentioned method, 59 ° C
Was uniformly heated to 75 ° C. or higher, and the component (C)
Part (35% by weight) and the remaining component (E) (excluding perfume), which is an aqueous phase component, is heated uniformly to 75 ° C, and the aqueous phase component, which is heated to 75 ° C, is heated to 75 ° C. The ingredients were added with stirring to emulsify. Subsequently, as the step (ii), first, the emulsion obtained in the step (i) is stirred (C).
The emulsion was cooled to 64 ° C. without using other cooling means (cooling device such as jacket) by adding the remaining part (11% by weight) of the components at 25 ° C. The cooling rate in this case was 8.0 ° C./min. Next, as shown in Table 11, the vicinity of the emulsion transition temperature (range of 54 to 64 ° C) was cooled by changing the cooling rate. By further adding the rest of the component (C) at 25 ° C. while stirring the emulsion,
The emulsion was cooled to 40 ° C. without using other cooling means (cooling device such as a jacket). The cooling rate in this case was 2.0 ° C./min. When cooled to 40 ° C., the fragrance of the component (E) was added and uniformly mixed to obtain a product (conditioner). The viscosity and particle size of the products obtained by changing various conditions were measured, and the results are shown in Table 11. Incidentally, when the particle diameter is in the range of 29 to 32 μm, the viscosity is 2300.
Control was possible in the range of up to 8400 cP (3.7 times = 8400/2300). In step (ii), cooling is performed by controlling the addition rate and temperature of the rest of the component (C) without using a cooling device such as a jacket as a cooling means near the emulsion transition temperature (range of 54 to 64 ° C.). Similar results were obtained when the speed was controlled.

[0059]

[Table 11]

Example 7 The components (A), (A '), (B), (C), (D) and (E) shown in Table 5 used in Example 3 were used. An emulsion was produced by the method of. In step (i), the component (A), the component (A ′), the component (B), the component (D) and the component (E), the oil phase component of diethylene glycol monoethyl ether, are mixed and the emulsion transition temperature of the mixture is mixed. (As a result of measurement by the above-mentioned method, 59 ° C.
Was uniformly heated to 75 ° C. or higher, and the component (C)
(35% by weight) and the remaining component (E) (excluding the fragrance) of the aqueous phase component are uniformly heated to 75 ° C., the aqueous phase component heated to 75 ° C. and the oil phase heated to 75 ° C. Emulsifier with ingredients continuously (manufactured by Noritake Company Limited,
It was emulsified by passing it through a static mixer) and charged into a mixing tank. Subsequently, as the step (ii), first, while stirring the emulsion obtained in the step (i), the remaining part (11% by weight) of the component (C) is added at 25 ° C.,
The emulsion was cooled to 64 ° C. without using other cooling means (cooling device such as jacket). The cooling rate in this case was 8.0 ° C./min. Next, as shown in Table 12, the vicinity of the emulsion transition temperature (range of 54 to 64 ° C) was cooled by changing the cooling rate. While stirring the emulsion (C)
By adding the rest of the components at 25 ° C, the emulsion was cooled to 40 ° C without using other cooling means (cooling device such as a jacket). The cooling rate in this case is 2.0 ℃
/ Min. When cooled to 40 ° C., the fragrance of the component (E) was added and uniformly mixed to obtain a product (conditioner). The viscosity and particle size of the product obtained by changing various conditions were measured, and the results are shown in Table 12. In addition, in the range of particle diameter 29 to 30 μm, the viscosity is 2200 to 8300 c.
It was possible to control in the range of P (3.8 times = 8300/2200)). Further, similar results were obtained even when the step (ii) was continuously performed without charging the emulsion continuously obtained in the step (i) into the blending tank.

[0061]

[Table 12]

[0062]

EFFECTS OF THE INVENTION According to the method for producing an emulsion of the present invention, by controlling only the cooling rate in the vicinity of the emulsification transition temperature of the emulsion, the desired change can be obtained in a state where the particle diameter of the emulsion is small. An emulsion having a viscosity can be obtained.

Claims (5)

[Claims] 1. A method for producing an emulsion containing the following components (A), (B) and (C), which comprises the following steps (i) and (ii). (A) Quaternary ammonium salt 0.1 to 30% by weight (B) higher alcohol 0.1 to 30% by weight (C) residual amount of water (i): component (A), component (B) and (C) A step of mixing the components to emulsify, (ii): emulsification rearrangement of the emulsion obtained in step (i) in order to control the viscosity of the emulsion in a state where the particle size change of the emulsion is small The process of cooling by controlling only the cooling rate near the temperature. 2. The component (A) comprises at least a branched chain fourth group.
The method for producing an emulsion according to claim 1, comprising 0.05 to 20% by weight of a primary ammonium salt. 3. The method for producing an emulsion according to claim 1, wherein the emulsion further comprises the following component (D). (D) Glyceryl etherified polyhydric alcohol 0.01 to 10% by weight 4. The component (C) is divided into a part of the step (i
The method for producing an emulsion according to claim 1, which is used as the refrigerant in i). 5. A temperature range of ± 10 ° C. of the emulsification transition temperature,
The method for producing an emulsion according to claim 1, wherein the cooling rate is controlled in the range of 0.05 to 5 ° C./min.