JP2013067712A - Method of producing pearlescent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method of producing a pearlescent composition that is excellent in whiteness degree and has a smaller amount of coarse particles, by simple equipment and operation.SOLUTION: The method of producing the pearlescent composition includes: a step 1 of stirring and mixing 10 to 50 mass% of fatty acid glycol ester (A), a fatty acid monoalkylol amide (B), an alkyl sulfate salt (C), and water (E), at temperature equal to or larger than a melting point of the component (A) to produce an emulsified liquid that contains emulsion particles each having a volume average particle size of 1 to 9 μm; and a step 2 of cooling the obtained emulsified liquid to crystallize pearlescence-forming particles containing the component (A).

Description

  The present invention relates to a method for producing a pearly luster composition. More specifically, the present invention relates to a method for producing a pearly luster composition that can be suitably used to increase the added value of shampoos, rinses, body shampoos, liquid detergents and the like.

  Conventionally, bases that give a pearly luster have been used to increase the added value of shampoos, rinses, body shampoos, cosmetics, liquid detergents and the like. Accordingly, various pearly luster compositions containing a major component for imparting pearly luster have been studied.

  Various studies have been made on fatty acid glycol ester as a main component in the pearly luster composition, and a method of directly cooling and crystallizing in a product or a method of preparing a concentrated dispersion in advance and blending it into the product are used. In the method of preparing a concentrated dispersion in advance, when the blending amount of the fatty acid glycol ester is increased in order to obtain a sufficient pearly luster, the viscosity at room temperature increases and the fluidity decreases. Therefore, a pearly luster composition using a specific nonionic surfactant has been proposed (see Patent Document 1).

  Another object of the present invention is to provide a pearly luster composition having a high turbidity while maintaining a strong pearly luster, comprising a fatty acid glycol ester, an alkyl sulfate ester salt, a polyoxyalkylene type nonionic surfactant and water. A pearly luster composition comprising a fatty acid in an amount of 0.3 to 3% by weight (see Patent Document 2) has been proposed.

  Furthermore, with the object of providing a pearly luster composition having a high turbidity while maintaining a strong pearly luster, a pearly luster composition comprising a fatty acid glycol ester and water, further comprising an aliphatic alcohol, There has been proposed a pearly luster composition containing 0.3 to 3% by weight of at least one aliphatic compound selected from the group consisting of fatty acid monoglycerides and aliphatic ethers (see Patent Document 3).

  However, in these cases, there is a problem that a specific crystallization additive is required.

JP 2000-212031 A JP 2008-255110 A JP 2009-19194 A

  When blending a pearly luster composition into cosmetics, cleaning agents, etc., it has a fine pearly luster texture. In other words, a pearly luster composition having a fine size, in other words, high whiteness is required. However, such a pearly luster composition proposed in the prior art is greatly limited in apparatus and operation during production. Furthermore, when coarse particles are present in the pearly luster composition, the feeling of use is impaired.

  Generally, the larger the scale of the production facility, the lower the cooling rate in the cooling operation, and the lower the uniformity in the blending tank in the stirring operation. In order to improve productivity, there is a demand for a pearly luster composition with high whiteness that can be produced without being limited to apparatuses and operations.

  Therefore, the subject of this invention is providing the manufacturing method of the pearl luster composition which is excellent in whiteness and there are few coarse particles even if it is a simple apparatus and operation.

  Thus, as a result of intensive studies, the present inventors focused on an emulsion obtained by stirring components such as fatty acid glycol esters, and surprisingly, by controlling the particle size of the emulsion particles constituting the emulsion to a specific range. In addition, the inventors have found that a pearly luster composition with few coarse particles can be produced by a simple apparatus and operation, and completed the present invention.

That is, the gist of the present invention is as follows.
[1] (A) 10-50 mass% of fatty acid glycol ester,
(B) fatty acid monoalkylolamide,
(C) alkyl sulfate salt, and (E) water,
Are mixed with stirring at a temperature equal to or higher than the melting point of component (A) to produce an emulsion containing emulsion particles having a volume average particle size of 1 to 9 μm (step 1), and the obtained emulsion is Cooling and crystallizing the pearly luster-forming particles containing the component (A) (step 2),
A process for producing a pearly luster composition comprising:
[2] The method for producing a pearly luster composition according to the above [1], wherein the molar ratio (C / B) of the component (C) to the component (B) is 0.50 to 0.95;

[3] The molar ratio (C / B) of the component (C) to the component (B) is 0.50 or more and less than 0.80, and as stirring conditions in the step 1, stirring is dropped per unit volume of the emulsion. The method for producing a pearly luster composition according to the above [1] or [2], wherein the power is 4 (W / m ³ ) or more;
[4] The molar ratio (C / B) of the component (C) to the component (B) is 0.80 to 0.95, and the stirring power in the emulsion liquid per unit volume as the stirring condition in the step 1 The method for producing a pearly luster composition according to the above [1] or [2], wherein is 20 (W / m ³ ) or more;
[5] The fatty acid glycol ester is an ester of a fatty acid and glycol containing stearic acid and palmitic acid, and the mass ratio of stearic acid to palmitic acid (stearic acid / palmitic acid) is 20/80 to 85/15 The method for producing a pearly luster composition according to any one of the above [1] to [4];
[6] The method for producing a pearly luster composition according to any one of the above [1] to [5], wherein the content of the component (B) is 5 to 10% by mass;
[7] The method for producing a pearly luster composition according to any one of claims 1 to 6, wherein the content of the component (C) is 5 to 10% by mass; and [8] The emulsion obtained in step 1 is And (D) the method for producing a pearly luster composition according to any one of [1] to [7] above, which further comprises a polyoxyalkylene type nonionic surfactant.

  According to the present invention, an effect that a pearly luster composition with few coarse particles can be produced with a simple apparatus and operation is exhibited. Moreover, the pearly luster composition obtained in the present invention has high whiteness and few coarse particles.

  In the method for producing the pearly luster composition of the present invention, the emulsion particles in the emulsion obtained by mixing the following (A) component, (B) component, (C) component and (E) component under stirring are used. By making the volume average particle size 1 to 9 μm finer than before (step 1), the emulsion is cooled, and the pearly luster-forming particles containing the component (A) are crystallized (step 2). ), A pearly luster composition having high whiteness and few coarse particles can be obtained. Even when the emulsion is cooled to crystallize the pearly luster-forming particles containing the component (A), it is preferable to maintain the volume average particle diameter of 1 to 9 μm by continuing stirring.

  In order to obtain emulsified particles having a fine particle diameter of 1 to 9 μm, for example, the component (A) is adjusted by adjusting the molar ratio of the component (B) and the component (C) as described later. This can be achieved by the balance between crystallization and dropping power (stirring power). Thereby, by changing the existence state of the (B) component and the (C) component at the oil-water interface of the emulsified particles, a large amount of nucleation of the (A) component is promoted, and fine crystals by the (A) component are obtained. It is thought that.

  The pearly luster composition obtained by the present invention contains (A) fatty acid glycol ester, (B) fatty acid monoalkylolamide, (C) alkyl sulfate ester salt, and (E) water, and (D) polyoxy It is preferable to contain an alkylene type nonionic surfactant. Hereinafter, each component will be described.

[Pearl gloss composition]
Examples of the fatty acid glycol ester of the component (A) used in the present invention include the formula (I):
Y—O— (CHR ¹ CH ₂ O) _p —COR ² (I)
(Wherein R ¹ represents a hydrogen atom or a methyl group, R ² represents a linear or branched saturated or unsaturated hydrocarbon group having 13 to 21 carbon atoms, and Y represents a hydrogen atom or —COR ² ( R ² represents the same as described above, and p is a number of 1 to 3, which means an average number of added moles).

As described above, R ² is a linear or branched saturated or unsaturated hydrocarbon group having 13 to 21 carbon atoms. Therefore, in view of the fact that the fatty acid glycol ester is composed of a fatty acid and a glycol, the fatty acid corresponds to a linear or branched saturated or unsaturated fatty acid having 14 to 22 carbon atoms. From the viewpoint of whiteness of the pearly luster composition, the fatty acid preferably includes stearic acid and palmitic acid, and contains other saturated, unsaturated fatty acids having 14, 15, 17, 19 to 22 carbon atoms. It may be.

  The fatty acid constituting the fatty acid glycol ester preferably includes stearic acid and palmitic acid from the viewpoint of the whiteness of the pearly luster composition, and the total content thereof includes all fatty acids constituting the fatty acid glycol ester. Preferably it is 80 mass% or more, More preferably, it is 90 mass% or more, More preferably, it is 95 mass% or more, More preferably, it is 95 mass% or more, Most preferably, it is 100 mass%.

  In the present invention, the fatty acid constituting the fatty acid glycol ester is a fatty acid that can be a raw material of the fatty acid glycol ester. For example, the fatty acid is obtained by transesterification of a fatty acid ester of a lower alcohol having 1 to 3 carbon atoms with a glycol. Even when a glycol ester is produced, it is converted as a fatty acid.

  For example, the reaction of a mixture of palmitic acid and stearic acid with ethylene glycol gives a mixture of ethylene glycol dipalmitate, ethylene glycol monopalmitate, monostearate monostearate, and ethylene glycol distearate.

  From the viewpoint of whiteness of the pearly luster composition, the fatty acid glycol ester is an ester of a fatty acid and glycol containing stearic acid and palmitic acid, and the mass ratio of stearic acid and palmitic acid (stearic acid / palmitic acid) is The ratio is preferably 20/80 to 85/15, more preferably 35/65 to 82/18, further preferably 40/60 to 80/20, and still more preferably 45/55 to 75/25.

  p is 1 to 3, and 1 is preferable from the viewpoint of whiteness of the pearly luster composition.

Moreover, as represented by the formula (I), the fatty acid glycol ester may be either a monocarboxylic acid ester when Y is a hydrogen atom or a dicarboxylic acid ester when Y is —COR ^2. However, from the viewpoint of whiteness and light luminance, a dicarboxylic acid ester when Y is —COR ² is preferable. In the dicarboxylic acid ester, R ² may be the same or different.

  As the component (A), it is preferable that two or more fatty acid glycol esters are used in combination from the viewpoint of whiteness of the pearly luster composition. When two or more fatty acid glycol esters are used in combination, they may be a mixture of each prepared fatty acid glycol ester, and a fatty acid glycol obtained by reacting a mixture of fatty acids having different alkyl chain lengths and glycol. It may be a mixture of esters. That is, the maximum proportion of a single fatty acid in the total fatty acids is preferably 85% by mass or less, more preferably 80% by mass or less, still more preferably 75% by mass or less, and still more preferably 70% by mass. It is a thing of the mass% or less, Preferably it is a 15 mass% or more thing, More preferably, it is a 20 mass% or more thing, More preferably, it is a 25 mass% or more thing, More preferably, it is a 45 mass% or more thing. In 2 or more types, 2-5 types are preferable and 2-3 types are more preferable. From these viewpoints, the maximum proportion of a single fatty acid in the total fatty acids is preferably 15 to 85% by mass, more preferably 20 to 80% by mass, even more preferably 25 to 75% by mass, The thing of 45-70 mass% is still more preferable.

  Examples of the glycol constituting the fatty acid glycol ester include those corresponding to the above formula (I), that is, ethylene glycol and 1,2-propylene glycol. Among these, ethylene glycol is preferable from the viewpoint of controlling crystallinity.

  The content of the fatty acid glycol ester in the pearly luster composition is preferably 10% by mass or more, more preferably 15% by mass or more, further preferably 18% by mass or more from the viewpoint of imparting pearly luster, and from the viewpoint of fluidity, 50 mass% or less is preferable, 30 mass% or less is more preferable, and 25 mass% or less is further more preferable. From these viewpoints, the content of the fatty acid glycol ester is preferably 10 to 50% by mass, more preferably 15 to 30% by mass, and still more preferably 18 to 25% by mass in the pearly luster composition.

The fatty acid monoalkylolamide as the component (B) used in the present invention is effective in improving the pearly luster. For example, the formula (II):
^{R 3 CO-NH-R 4} OH (II)
(In the formula, R ³ represents a linear or branched saturated or unsaturated hydrocarbon group having 7 to 20 carbon atoms, and R ⁴ represents an ethylene group or a propylene group)
The thing represented by is mentioned.

In the formula (II), R ³ is preferably an alkyl group or alkenyl group having 7 to 20 carbon atoms, and specific examples include an undecyl group, a tridecyl group, a heptadecyl group, and the like. Examples of R ⁴ include an ethylene group, an n-propylene group, and an isopropylene group.

  Examples of fatty acid monoalkylolamides include lauric acid monoethanolamide, lauric acid monopropanolamide, lauric acid monoisopropanolamide, myristic acid monoethanolamide, palmitic acid monoethanolamide, stearic acid monoethanolamide, oleic acid monoethanolamide, Oleic acid monoisopropanolamide, coconut oil fatty acid monoethanolamide, coconut oil fatty acid monopropanolamide, coconut oil fatty acid monoisopropanolamide, coconut plant oil fatty acid monoethanolamide, etc. may be mentioned alone or in combination of two or more. Can be used. Of these, coconut oil fatty acid monoethanolamide, lauric acid monoethanolamide, palmitic acid monoethanolamide, and stearic acid monoethanolamide are preferred.

  The content of the fatty acid monoalkylolamide in the pearly luster composition is preferably 5% by mass or more, more preferably 6% by mass or more, further preferably 10% by mass or more, from the viewpoint of crystal refining, and the pearly luster composition. 10 mass% or less is preferable from a viewpoint of suppressing the raise of the viscosity of this and improving fluidity | liquidity. From these viewpoints, the content of the fatty acid monoalkylolamide is preferably 5 to 10% by mass, more preferably 6 to 10% by mass, and further preferably 7 to 10% by mass in the pearly luster composition.

The alkyl sulfate ester salt of the component (C) used in the present invention is effective for uniformly mixing each component. For example, the formula (III):
R ⁵ —O— (R ⁶ O) _r —SO ₃ M (III)
(In the formula, R ⁵ represents a linear or branched saturated or unsaturated hydrocarbon group having 8 to 20 carbon atoms, R ⁶ represents an ethylene group or a propylene group, and M represents an alkali metal or alkaline earth metal. , An ammonium ion or a hydroxyalkyl-substituted ammonium having 2 or 3 carbon atoms, wherein r is a number of 0 to 8 and means an average addition mole number), and an alkyl optionally having a polyoxyalkylene group Examples thereof include sulfate ester salts.

In the formula (III), R ⁵ is preferably an alkyl group or an alkenyl group having 8 to 20 carbon atoms, preferably 10 to 14 carbon atoms, specifically, a lauryl group, a myristyl group, a palmityl group, a stearyl group, or the like. Is mentioned. Examples of R ⁶ include an ethylene group and a propylene group, and an ethylene group is preferable. r is preferably 0 to 4, and more preferably 1 to 3.

  Preferable examples of the alkyl sulfate ester salt include sodium lauryl sulfate, triethanolamine lauryl sulfate, sodium polyoxyethylene lauryl ether sulfate (average added mole number of ethylene oxide (EO): 1 to 4), ammonium polyoxyethylene lauryl ether sulfate (Average number of added moles of EO: 1 to 4) and polyoxyethylene lauryl ether sulfate triethanolamine (average number of added moles of EO: 1 to 4). It may be.

  The content of the alkyl sulfate ester salt in the pearly luster composition is preferably 5% by mass or more, more preferably 6% by mass or more, even more preferably 7% by mass or more, from the viewpoint of uniformly mixing the components, From the viewpoint of improving the whiteness due to crystallization, it is preferably 10% by mass or less, and more preferably 9% by mass or less. From these viewpoints, the content of the alkyl sulfate salt is preferably 5 to 10% by mass, more preferably 6 to 9% by mass, and still more preferably 7 to 9% by mass.

  The total amount of the component (B) and the component (C) in the pearly luster composition of the present invention is preferably 10% by mass or more from the viewpoint of uniformly mixing each component, improving whiteness and fluidity of the composition. In view of the above, 20% by mass or less is preferable. From these viewpoints, the total amount of the component (B) and the component (C) in the pearly luster composition is preferably 10 to 20% by mass, more preferably 12 to 20% by mass, and further 14 to 20% by mass. preferable.

  Regarding the molar ratio of the component (B) and the component (C) in the pearly luster composition of the present invention, it is preferable that the component (C) / (B) is 0.50 to 0.95. It is preferable for obtaining a pearly luster composition having a high degree and a fine pearly luster texture. The molar ratio (C / B) between the component (B) and the component (C) is preferably 0.50 or more from the viewpoint of uniformly mixing the components and from the viewpoint of fluidity. Moreover, from a viewpoint of obtaining a pearly luster composition with high whiteness, 0.95 or less is preferable. From these viewpoints, the molar ratio between the component (B) and the component (C) in the pearly luster composition is preferably (C) component / (B) component = 0.50-0.95, preferably 0.55- 0.92 is preferable, 0.60 to 0.90 is more preferable, and 0.65 to 0.90 is still more preferable.

  With this molar ratio and the constant stirring and dropping power described below, a large amount of fine pearly luster-forming particles containing a fatty acid glycol ester, which is a pearly luster-forming component, is precipitated, and a pearly luster composition with high whiteness is obtained. Conceivable. Although details are unknown, it is considered that due to this molar ratio, the presence state of the component (B) and the component (C) easily promotes a large amount of nucleation of the component (A). In the present invention, as a value indicating the whiteness of the pearly luster composition, the W value shown in Examples described later can be used. The W value is preferably 16 to 25, more preferably 17 to 23, and still more preferably 18 to 21 from the viewpoint of imparting gloss.

  The (D) component polyoxyalkylene type nonionic surfactant used in the present invention is effective in reducing the viscosity of the pearly luster composition. For example, a polyoxyalkylene such as a polyoxyethylene group or a polyoxypropylene group is used. The thing which has group is mentioned. Specific examples of the polyoxyalkylene type nonionic surfactant include polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether, polyoxyalkylene sorbitan fatty acid ester, polyoxyalkylene fatty acid monoalkanolamide, polyoxyalkylene fatty acid dialkanolamide, etc. And two or more of them may be used in combination.

Of these, formula (IV):
^{R 7 -O- (R 8 O)} q -H (IV)
(In the formula, R ⁷ represents a linear or branched saturated or unsaturated hydrocarbon group having ^{8 to} 20 carbon atoms, R ⁸ represents an ethylene group or a propylene group, and q is preferably 1 to 12, more preferably. A polyoxyalkylene alkyl ether represented by the number of 1 to 6 (meaning the average number of moles added) is preferred.

In formula (IV), R ⁷ is preferably an alkyl or alkenyl group having 8 to 20 carbon atoms, preferably 10 to 14 carbon atoms. Examples of R ⁷ include an ethylene group, an n-propylene group, and an isopropylene group. q is preferably 3-6.

From the viewpoint of suppressing emulsification of the pearly luster composition and controlling the viscosity, the HLB of the polyoxyalkylene type nonionic surfactant is preferably less than 18, more preferably 9-15, and even more preferably 9-12. HLB is an index indicating a hydrophilic-lipophilic balance. In the present invention, the formula (V) by Oda and Teramura et al.
HLB = (Σinorganic value / Σorganic value) × 10 (V)
It is a value when calculated using.

  The content of the polyoxyalkylene type nonionic surfactant in the pearly luster composition is preferably 0.5% by mass or more from the viewpoint of reducing the viscosity of the pearly luster composition, and from the viewpoint of obtaining good pearly luster, 10 The mass% or less is preferable. From these viewpoints, the content of the polyoxyalkylene type nonionic surfactant in the pearly luster composition is preferably 0.5 to 10% by mass, more preferably 0.5 to 8% by mass, and 1 to 6% by mass. Is more preferable, and 2 to 6% by mass is more preferable.

  The pearly luster composition of the present invention contains water as the component (E), and the water content in the pearly luster composition is preferably 25 to 70% by mass from the viewpoint of concentration and viscosity adjustment of the pearly luster composition. 40-70 mass% is more preferable, and 50-65 mass% is further more preferable.

  The pearly luster composition may further contain a pH adjuster, preservative, salts, alcohols, polyols and the like as appropriate.

[Method for producing pearly luster composition]
The method for producing the pearly luster composition of the present invention comprises:
(A) 10-50 mass% fatty acid glycol ester,
(B) fatty acid monoalkylolamide,
(C) 5-10% by mass of alkyl sulfate ester salt, and (E) water,
Are mixed with stirring at a temperature equal to or higher than the melting point of component (A) to produce an emulsion containing emulsion particles having a volume average particle size of 1 to 9 μm (step 1), and the obtained emulsion is Cooling and crystallizing the pearly luster-forming particles containing the component (A) (step 2),
Is a method for producing a pearly luster composition. Furthermore, you may mix | blend (D) component at the process 1 as needed. In this case, the component (D) is contained in the emulsion.

Process 1
The order of adding the raw materials of the components (A) to (E) may be any. (A) By stirring at the time of melt-mixing each component at a temperature equal to or higher than the melting point of the component to obtain an emulsion, the oily component containing the fatty acid glycol ester becomes emulsified particles and is dispersed in the melt-mixed solution. Emulsification of the molten mixture proceeds by stirring, and an emulsion is obtained. The droplet diameter (volume average particle diameter) of the emulsified particles in the obtained emulsion is 1 to 9 μm, preferably 1 to 8.5 μm, more preferably 2 to 8.5 μm (B It is necessary to determine the molar ratio between the component (C) and the component (C) and the stirring conditions in order to obtain a uniform pearly luster composition having high whiteness and few coarse particles. When the droplet diameter is larger than 9 μm, the whiteness is lowered, coarse particles are generated, and the appearance and feel during use are impaired, which is not good.

The temperature at which the emulsion is obtained, that is, the emulsification temperature is a temperature equal to or higher than the melting point of the component (A), preferably the melting point of the component (A) + 3 ° C. to less than 100 ° C., and the melting point of the component (A) + 5 ° C. to 95 ° C. It is more preferable that the temperature is less than ° C.

  As an apparatus for preparing the emulsion, a tank equipped with a stirring means for stirring each component and a temperature adjusting means for heating and cooling each component is preferable. As a stirring means, a batch type stirring tank provided with a rotating blade is simple, versatile and preferable.

The size of the vessel is not particularly limited, it is possible to use the bath of 20 m ^3, for example, from 0.3 L. When mass-producing on an industrial scale, it is preferable to use a mixing tank of 100 L to 20 m ³ .

The preferred molar ratio (C / B) between the component (C) and the component (B) when producing the emulsion is 0.50 to 0.95, but this molar ratio is 0.5 or more and 0.8. If it is less than the range, the emulsified particles are extremely small, and the stirring force for obtaining the emulsified particles having a volume average particle diameter of 1 to 9 μm may be small. Therefore, when the molar ratio (C / B) of the component (C) to the component (B) is 0.5 or more and less than 0.8, the stirring condition is the stirring dropping power per unit volume of emulsion (W / m ³ ) is preferably 4 or more, more preferably 8 or more, still more preferably 10 or more, preferably 4 to 2000, more preferably 8 to 2000, and still more preferably 10 to 1000.

When the molar ratio (C / B) of the component (C) and the component (B) in producing the emulsion is 0.8 or more and 0.95 or less, emulsion particles having a volume average particle diameter of 1 to 9 μm are obtained. The stirring power for stirring, that is, the stirring dropping power per unit volume of the emulsion is preferably 20 (W / m ³ ) or more, more preferably 50 or more, still more preferably 100 or more, preferably 20 to 5000, more preferably 50 to 5000. Preferably, 100 to 3000 is even more preferable.

In addition, as an index of the stirring condition, in this application, stirring dropping power per unit volume of the emulsion is used. In general, the stirring drop power per unit volume of the emulsion can be determined by a method (Formula VII) that is calculated based on the power characteristics of the stirring device. The emulsion density at the emulsification temperature is ρ (kg / m ³ ), the emulsion charge is M (kg), the stirring rotation speed is N (r / s), and the maximum blade diameter (diameter) is d (m). And The emulsified liquid unit volume is the volume at the emulsification temperature.
Stirring drop power (W / m ³ ) = Np × ρ ² × N ³ × d ⁵ / M (VII)

Np is a power number (dimensionless), which represents the power characteristics of the used stirring device, and is a value determined by the shape / dimension of the stirring device and the stirring Reynolds number Re. Several formulas for estimating the number of powers applicable to various stirring devices have been reported, and a preferred example thereof is the Kamei / Hiraoka formula for paddle blades without a baffle (Formula VIII).
Np = (1.2π ⁴ β ² ) / (8d ³ / D ² / H) × f (VIII)

Here, D (m) is the tank inner diameter (maximum inner diameter), and H (m) is the liquid depth (maximum depth of the charged liquid). β is an operation value defined by the formula (IX).
β = 2ln (D / d) / (D / dd−D) (IX)

f is a coefficient of friction. f _{is, Re d, C L, C} t, C tr, has a function of F∞, details of formula are described in the following known documents.
Note that C _L , C _t , and C _tr are expressed as functions such as d, D, H, b, and n _P.
b: Maximum blade width (height) (m), n _P : Number of blades

  Kamei, N., S. Hiraoka, Y. Kato, Y. Tada, H. Shida, YS Lee, T. Yamaguchi and ST Koh; "Power Correlation for Paddle Impellers in Spherical and Sylindrical Agitated Vessels," Kagaku Kogaku Ronbunshu, 21 , 41-48 (1995)

That is a parameter of the shape and dimensions of the stirring device used d, D, by providing H etc., that the equation of Kamei Hiraoka (Formula VIII) Np represents a device-specific function that depends only on Re _d it can. Incidentally, Re _d is defined by the following equation X.
^{_{Re d = Nd 2 ρ / μ}} (X)

  Here, μ (Pa · s) is the liquid viscosity. The liquid viscosity can be measured with a B-type viscometer. The measurement temperature is the emulsification temperature, the measurement conditions are a rotation speed of 60 RPM, the measurement time is 1 minute, and the rotor is based on No. 3, but if the viscosity is too high to be measured, No. 4 is measured and the viscosity is too low. If you can't, use # 2 etc. sequentially.

  The shape of the stirring blades equipped in the stirring device may be those used in general mixing operations, and preferably includes paddles (including pitched paddles), propellers, turbines, anchors, helical ribbons, etc. Baffles, fixed wings, and scraping wings may be attached. The molten mixed liquid in the present invention is a fluid having a relatively high viscosity of about 0.2 to 2 Pa · s. In such a case, from the viewpoint of uniform mixing, the shape of the stirring blade is paddle, anchor, helical Ribbons are preferred and paddles are more preferred. In particular, a stirring device with a fixed blade and a scraping blade is preferable. For example, a vacuum emulsification stirring device VQ type manufactured by Mizuho Industry Co., Ltd. K aji homomixer etc. are mentioned.

  In general, the stirring speed (r / s) is preferably from 0.1 to 5, and more preferably from 0.2 to 3.

  The time for stirring the emulsified droplets so that the droplet diameter (volume average particle size) of the emulsified particles is 1 to 9 μm depends on the scale, but is preferably 10 minutes or more, more preferably 30 minutes or more, Within 5 hours is preferable, and within 3 hours is more preferable. That is, the stirring time is preferably 10 minutes to 5 hours, more preferably 30 minutes to 5 hours, and even more preferably 30 minutes to 3 hours.

  The temperature of the raw melt mixture is preferably equal to or higher than the melting end temperature of the fatty acid glycol ester mixture, and preferably equal to or lower than the boiling point of the mixture. Moreover, the temperature 1-20 degreeC higher than the melting completion temperature of fatty-acid glycol ester is more preferable, and the temperature 1-10 degreeC higher is more preferable.

Process 2
In step 2, the obtained emulsion is cooled to crystallize the pearly luster-forming particles containing the component (A). The average upper cooling rate is preferably 20 ° C./min, more preferably 15 ° C./min, further preferably 10 ° C./min, still more preferably 5 ° C./min. 1 ° C./min is most preferable. The lower limit is preferably 0.05 ° C / min, more preferably 0.1 ° C / min, and still more preferably 0.15 ° C / min. From this viewpoint, the cooling rate is preferably 0.05 to 20 ° C / min, more preferably 0.1 to 15 ° C / min, further preferably 0.15 to 10 ° C / min, and more preferably 0.15 to 5 ° C. More preferably, 0.15-1 degreeC is still more preferable.

  After the pearly luster-forming particles are crystallized, it is preferable to cool them further to stabilize the crystals, and it is desirable to cool them until the liquid temperature becomes 10 to 45 ° C, preferably 15 to 40 ° C.

  The emulsion is preferably cooled while stirring so that the solution does not separate.

  The cooling is preferably a method in which the temperature distribution is more uniform. As a specific method, for example, there is a method in which a molten mixed solution is prepared in a blending tank attached with a jacket, and coolant water is passed through the jacket.

  The obtained pearly luster composition can be mixed with an appropriate detergent component such as a surfactant to form a detergent. The pearly luster composition (pure component) in the cleaning agent is preferably 0.5 to 5% by mass, more preferably 1 to 3% by mass.

  In the following, aspects of the invention will be further described and disclosed by means of examples. These examples are merely illustrative of the invention and are not meant to be limiting in any way.

Various properties of the pearly luster composition obtained in each example and each comparative example were measured by the following methods.
<Measurement of emulsion particle size>
Two blocks of block-shaped dry ice were prepared. About 1 g of the emulsified liquid before the cooling operation was sampled, quickly dropped on one dry ice, and sandwiched between the other dry ice, thereby rapidly cooling and solidifying the emulsified liquid between the dry ice planes. By pouring the solidified product into 100 times amount (mass) of room temperature water, it is possible to obtain a preparation liquid in which the emulsified particles in the emulsified liquid before the cooling operation are dispersed in a solidified state without changing its size and shape. It was. This could be confirmed by microscopic observation at the emulsification temperature with a hot plate. The volume-based average droplet diameter of the solidified emulsified droplets dispersed in the preparation liquid is measured with a laser scattering / diffraction particle size distribution analyzer (HORIBA LA-920) under a condition of a relative refractive index of 1.2. This value was taken as the volume average particle size of the emulsified particles.

<Whiteness of pearly luster composition>
Dilute the pearly luster composition 33.3 times (mass ratio) with an aqueous solution containing 19.5% by mass of pure polyoxyethylene (2) sodium lauryl ether sulfate (product name: EMAL E-27C) 1 g was measured on a round cell (Nippon Denshoku, 35Φ × 15H, part No. 2301) mounted in a black folder. After this was left for 5 minutes, the C light source of the color difference meter (manufactured by KONICA MINOLTA, CR-400) was used to shield L (brightness) and b (hue / saturation) from the bottom of the round cell. Measured below, the W value was determined by the following equation defined by ASTM (American Society for Testing and Materials) (E-313).
W value = (7L ² -40Lb) / 700

  The W value was used as an index representing the whiteness of the pearly luster composition, in other words, turbidity. The higher the W value, the whiter and darker the pearly luster composition will be.

<Pearl luster of pearl luster composition>
The pearly luster composition was diluted 20 times (mass ratio) with water, the appearance of the pearly luster was observed with the naked eye, and evaluated according to the following criteria. In addition, the thing in which the bubble was mixed was evaluated by visual observation after centrifuging and defoaming.

〔Evaluation criteria〕
A: Strong gloss is recognized.
B: Gloss is recognized.
C: There is no gloss.

<Presence of coarse particles>
About 1 g of the pearly luster composition was thinly spread on a black plate using a ruler or the like, and visually observed. The same operation was performed 3 times, and it was evaluated according to the following criteria whether particles having a size that can be visually confirmed exist. In addition, the particle | grains of the magnitude | size which can be confirmed visually are generally 50 micrometers or more in size.

〔Evaluation criteria〕
A: Neither was confirmed three times.
B: Only confirmed once.
C: Confirmed twice or more.

<Melting point of fatty acid glycol ester>
Using a differential scanning calorimeter (Thermo plus DSC8230, manufactured by Rigaku), the fatty acid glycol ester was heated at 5 ° C./min, and the resulting melting peak top was taken as the melting point.

Examples 1-9 and Comparative Examples 1-4
The fatty acid glycol ester, fatty acid monoalkylolamide, alkyl sulfate ester salt, polyoxyalkylene type nonionic surfactant, water and other components shown in Tables 1 and 2 An emulsion was obtained by mixing and stirring at 80 ° C. for 1 hour using a Kazi homomixer (manufactured by PRIMIX Corporation). The apparatus scale (preparation amount M) was 100 L (60 kg) in Examples 4 to 6, and 5 L (3 kg) in the other examples. Stirring was performed using paddle blades. The production conditions in each production example are shown in the table. In addition, the density ρ and the viscosity μ at 80 ° C. of the emulsified liquid were the same in each example, and were 950 kg / m ³ and 0.7 Pa · s, respectively. Viscosity μ was obtained by rounding off the second digit of the decimal point.

  The stirring drop power in each example was calculated using Formula VII and shown in the table. After performing the sampling operation for measuring the emulsion particle size, the sample was cooled to 20 ° C. at a cooling rate of 0.2 ° C./min to obtain a pearly luster composition. The stirring operation during cooling was performed under the same conditions as in melt mixing.

Note) The composition in the table indicates mass% of the pure component. The numbers in parentheses indicate the number of moles of ethylene oxide added.
Difatty acid ethylene glycol: ester of a mixture of palmitic acid (C16) / stearic acid (C18) = 50/50 (mass ratio) and ethylene glycol, melting point: 61.8 ° C.
1) Coconut oil fatty acid monoethanolamide (manufactured by Kawaken Fine Chemical Co., Ltd., trade name: Amizole CME): average molecular weight 267.1 (however, this average molecular weight was calculated with the average carbon number of the raw material palm oil fatty acid being 12.8) Value.)
2) Sodium polyoxyethylene (2) lauryl ether sulfate (product of Kao, trade name: Emar E-27C, concentration 27%): molecular weight 376.6 (however, the composition values in the table are polyoxyethylene (2) lauryl ether) Effective portion of sodium sulfate)
3) Polyoxyethylene (4) lauryl ether [HLB: 9.7] (trade name: Emulgen 504K, manufactured by Kao Corporation)

  From the above results, in Examples 1 to 9, the emulsion droplet diameter in the molten mixture at the time of manufacture is 1 to 9 μm, and the obtained pearly luster composition has a high whiteness pearly luster and is fluid It was found that there were almost no coarse particles that could be observed with the naked eye.

  On the other hand, in Comparative Examples 1 to 3, the emulsion droplet diameter in the molten mixture at the time of production was larger than 9 μm, and the presence of coarse particles was confirmed in the pearly luster composition. A pearly luster composition in which the emulsion droplet diameter is larger than 9 μm and the molar ratio of the component (C) to the component (B) (C) / (B) is greater than 0.95 (Comparative Example 4) Then, it was found that pearly luster with high whiteness could not be obtained although there were almost no coarse particles.

  Further, a pearly luster composition obtained under production conditions in which the molar ratio of component (C) / component (B) is 0.80 to 0.95 and the stirring and dropping power during melt mixing is less than 20 (Comparative Example 2) 3) was found to contain a lot of coarse crystals although it had a slightly higher whiteness than Comparative Example 4. Further, the pearly luster composition (Comparative Example 1) obtained under production conditions in which the molar ratio value of component (C) / component (B) is less than 0.80 and the stirring and dropping power during melt mixing is less than 4. Although it has high whiteness, it turned out that many coarse crystals are included.

The pearly luster composition of the present invention is suitably used for shampoos, rinses, body shampoos, liquid detergents and the like.

Claims (8)

(A) 10-50 mass% fatty acid glycol ester,
(B) fatty acid monoalkylolamide,
(C) alkyl sulfate salt, and (E) water,
Are mixed with stirring at a temperature equal to or higher than the melting point of component (A) to produce an emulsion containing emulsion particles having a volume average particle size of 1 to 9 μm (step 1), and the obtained emulsion is Cooling and crystallizing the pearly luster-forming particles containing the component (A) (step 2),
A method for producing a pearly luster composition, comprising:   The manufacturing method of the pearly luster composition of Claim 1 whose molar ratio (C / B) of (C) component and (B) component is 0.50-0.95. The molar ratio (C / B) of the component (C) to the component (B) is 0.50 or more and less than 0.80, and the stirring power in the emulsion liquid unit volume is 4 as the stirring condition in the step 1. The manufacturing method of the pearly luster composition of Claim 1 or 2 which is (W / m < ³ >) or more. The molar ratio (C / B) of the component (C) to the component (B) is 0.80 to 0.95, and the stirring power in the emulsion liquid unit volume is 20 ( it is W / m ³⁾ or more, the production method according to claim 1 or 2 pearly luster composition.   The fatty acid glycol ester is an ester of a fatty acid and glycol containing stearic acid and palmitic acid, and the mass ratio of stearic acid to palmitic acid (stearic acid / palmitic acid) is 20/80 to 85/15. The manufacturing method of the pearly luster composition in any one of Claims 1-4.   (B) The manufacturing method of the pearly luster composition in any one of Claims 1-5 whose content of a component is 5-10 mass%.   The manufacturing method of the pearly luster composition in any one of Claims 1-6 whose content of (C) component is 5-10 mass%. The method for producing a pearly luster composition according to any one of claims 1 to 7, wherein the emulsion obtained in step 1 further comprises (D) a polyoxyalkylene type nonionic surfactant.