JPH09249537A - Oxidation hair dye and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain an oxidation hair dye comprising an oil-in-water type emulsion prepared by a specific means, composed of an oxidation dye-contg. 1st agent and an oxidizing agent-contg. 2nd agent, retaining its viscosity even after mixing the above tow agents, and causing no dripping. SOLUTION: An oil-in-water type emulsion is obtained by first preparing an oil-in-water-soluble solvent type emulsion by adding a hydrophilic nonionic surfactant to a water-soluble solvent followed by adding an oily ingredient to the resultant solution, followed by diluting the resultant emulsion with water. This oxidation hair dye is composed o a 1st agent and a 2nd agent. The above oil-in-water type emulsion can be used in at least one party of the 1st and 2nd agents, and a dripping after mixing the above two agents can be prevented. In particular, when the above emulsion is to be used as the 1st agent, an oxidation dye is added to the water-soluble solvent at the 1st stage of the preparation of this emulsion; thereby the dispensability of the oxidation dye in the system is greatly improved, leading to shortening the time needed for the oxidation hair dye production process.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oxidative hair dye and a method for producing the same, and more specifically, it has good operability (adhesion to hair, easy spreadability) when applied to hair, and moreover, The present invention relates to an oxidative hair dye which has a good feel, has a small decrease in viscosity after application and is less likely to drop, and a method for producing the same.

[0002]

2. Description of the Related Art Hair dyes are required to have an appropriate viscosity in order to be easily held on the hair during use and to prevent the hair from dripping from the hair. For this reason, these hair dyes are often prepared as emulsifiers. Conventionally, these hair dyes have been prepared as oil-in-water emulsions. The reason is that the dye, which is the main agent in hair dyes, is usually water-soluble, and since it is contained in the aqueous phase that is the outer phase in oil-in-water emulsions, it has affinity for hair and penetrates into the hair. This is because it has the advantages that it is easy to apply, that it gives a favorable feeling of use without stickiness during use, and that it can be easily washed off with shampoo.

Hereinafter, as an example of a hair dye using such an oil-in-water emulsion, a two-component oxidative hair dye using an oxidative dye as a main component will be described. The two-part oxidative hair dye is composed of a first part and a second part. The first agent is prepared as an oil-in-water emulsion, and the outer aqueous phase contains an oxidizing agent, ammonia, an alkali agent such as alkanolamine, and the like. On the other hand, the second agent contains an oxidant that reacts with the oxidative dye to develop the color of the oxidative dye. Such a two-component hair dye is mixed immediately before use, and the oxidizing agent acts on the oxidizing dye to apply it to the hair, whereby the oxidation reaction of the oxidizing dye proceeds in the hair to dye the hair. It is a thing.

[0004]

However, in such an oil-in-water emulsion, there is a limitation on the amount and type of oil that can be blended in order to obtain a stable emulsion system. Further, even if each of the first agent and the second agent is stable alone, the stability after mixing the two agents is poor, and there is a problem in that the viscosity may drop and the ink may drop when left after application. It was Therefore, conventionally, it is necessary to use a higher alcohol, a higher fatty acid or the like for maintaining the viscosity, which results in a high cost and is not sufficient from the viewpoint of maintaining the viscosity.

The present invention has been made in view of the above conventional circumstances, and has good operability when applied to hair, moreover, the feel of the hair is good, and a decrease in viscosity during standing after application is small, It is an object of the present invention to provide an oxidative hair dye that does not easily drip and a method for producing the same.

[0006]

Means for Solving the Problems The inventors of the present invention have conducted extensive studies to achieve the above-mentioned object, and as a result, if an oil-in-water emulsion prepared by a specific method was used, the viscosity of the two-agent mixture was increased even after mixing. The inventors have found that an oxidative hair dye that does not drop and does not drip can be obtained, and completed the present invention.

That is, the present invention is a two-part type oxidative hair dye, which comprises a first part containing an oxidative dye and a second part containing an oxidizer, which is mixed immediately before use. The first agent and / or the second agent, as a first step, add a hydrophilic nonionic surfactant to a water-soluble solvent, and then add an oil phase to this to prepare an oil-in-water emulsion. Second
An oxidative hair dye, which comprises an oil-in-water emulsion obtained by adding water to the emulsion as a step.

The manufacturing method is a manufacturing method of a two-pack type oxidative hair dye, which comprises a first agent containing an oxidative dye and a second agent containing an oxidant, which is mixed immediately before use. As a first step, the method for producing the first agent comprises adding an oxidizing dye and a hydrophilic nonionic surfactant in a water-soluble solvent,
Next, an oil phase is added to this to prepare an oil-in-water emulsion, and the second step is to add water to the emulsion.

Next, the structure of the present invention will be described. The Applicant has added a hydrophilic nonionic surfactant to a water-soluble solvent as a first step, and then an oil phase to this to prepare an oil-in-water emulsion, and the second step is It has already been found that an oil-in-water emulsion obtained by adding water to an emulsion is very stable (Japanese Patent Publication No. 57-29213).

The present invention uses the above oil-in-water emulsion, and this oil-in-water emulsion is, for example,
A hydrophilic nonionic surfactant obtained by addition-polymerizing 15 mol or more of ethylene oxide is dissolved in a water-soluble solvent, and then an oil phase is added. It is an oil-in-water emulsion obtained by an emulsification method in which an agent is efficiently oriented and then water is gradually added to act as a water phase in a water-soluble solvent.

The general characteristics of the surfactants used to obtain a stable emulsion in the present invention are as follows:
15 to 120 mol of ethylene oxide added to a lipophilic group having 8 to 30 carbon atoms, or ethylene oxide (15 mol or more) and propylene oxide (1 to 3 mol)
(0 mol). Since all of these hydrophilic nonionic surfactants are high molecular weight substances, it is impossible to use them suddenly in an oil-water system to obtain a stable emulsion having a strong interface film, but it is impossible. As a first step, a method in which a surfactant is added to a water-soluble solvent and then an oil phase is added can efficiently orient a surfactant at an interface, and then a stable emulsion is produced by adding an aqueous phase. Is what you can do.

Next, the hydrophilic nonionic activators used in the present invention are classified into types I to IX and specifically described. Type (I):

[0013]

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(In the formula, R represents an alkane, alkene, aryl or steroid group having 8 or more carbon atoms, X represents an ether or ester group, and n represents an integer of 15 to 120.) In type (I) Particularly preferred as the hydrophilic nonionic surfactant in the present invention are lanolin and fatty acids thereof, and ethylene oxide 15 to 80 of alcohols.
A molar adduct and a 15-60 molar adduct of ethylene oxide of cholestanol or cholesterol. Type (II):

[0015]

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(Wherein R represents an alkane, alkene, aryl or steroid group having 8 or more carbon atoms, X is an ether or ester group, n is an integer of 20 or more, X'is an ester group and R'is carbon. Among the type (II), particularly preferred as the hydrophilic nonionic surfactant in the present invention are lanolin, fatty acids thereof, and ethylene oxide of alcohols 20 to 80.
2-ethylhexanoic acid or isostearic acid ester of a molar adduct and 2-ethylenehexanoic acid and isostearic acid ester of a 15-60 mol adduct of cholesteranol or cholesterol ethylene oxide. Type (III):

[0017]

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(In the formula, R represents an alkane, alkene, aryl or steroid group having 8 or more carbon atoms, X is an ether or ester group, n is an integer of 1 to 30, and n'is 15
The following integers are shown. Among the types (III), particularly preferred as the hydrophilic nonionic surfactant in the present invention are propylene oxide 1 of cetanol, cholestanol and cholesterol.
１２12 mol adduct, and ethylene oxide 20８8
0 mol was added. Type (IV):

[0019]

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(In the formula, R represents an alkane, alkene, aryl or steroid group having 8 or more carbon atoms, X is an ether or ester group, R'is an alkane having 2 to 18 carbon atoms,
Shows an alkene group. Among the types (IV), particularly preferred as the hydrophilic nonionic surfactant in the present invention are propylene oxide 1 to cetanol, cholestanol and cholesterol.
It is 2-ethylhexanoic acid or isostearic acid ester of the compound of type (III) obtained by adding 20 to 80 mol of ethylene oxide to a 12 mol adduct. Type (V):

[0021]

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Wherein R is an alkane having 8 or more carbon atoms, an alkene, an ethylene glycol of a hydroxycarboxylic acid,
Propylene glycol, glycerin, trimethylolethane, trimethylolpropane, sorbitol, sorbitan, pentaerythritol ester residues, n is an integer of 4 to 50, n 'is an integer of 2 to 6, nx
n ′ is 30 or more in any combination. Among the types (V), particularly preferred as the hydrophilic nonionic surfactant in the present invention are 30-80 mol of ethylene oxide adduct of castor oil and hydrogenated castor oil. Type (VI):

[0023]

[Chemical 6]

(Wherein, R represents an alkane having 8 or more carbon atoms, alkene, ethylene glycol of hydroxycarboxylic acid,
Propylene glycol, glycerin, trimethylolethane, trimethylolpropane, sorbitol, sorbitan, an ester residue of pentaerythritol, n is an integer of 4 to 50, n 'is an integer of 2 to 6, X' is an ester R ′ represents an alkane or alkene group having 2 to 18 carbon atoms. Among the types (VI), particularly preferred as the hydrophilic nonionic surfactant in the present invention are 2- Castane oil and 30-80 mol adduct of ethylene oxide of hydrogenated castor oil.
Ethylhexanoic acid or isostearic acid ester. Type (VII):

[0025]

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(In the formula, R is an alkane having 8 or more carbon atoms, an alkene, ethylene glycol of hydroxycarboxylic acid,
The ester residues of propylene glycol, glycerin, trimethylolethane, trimethylolpropane, sorbitol, sorbitan, and pentaerythrit are shown, n is an integer of 1 to 30, n 'is an integer of 4 to 50, and n "is 2
And n ′ × n ″ is 30 or more in any combination.) Among types (VII), particularly preferred as the hydrophilic nonionic surfactant in the present invention are castor oil and castor oil. To 1 to 12 moles of propylene oxide adduct of hydrogenated castor oil,
Further, 30 to 80 mol of ethylene oxide is added. Type (VIII):

[0027]

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(Wherein R represents an alkane or alkene group having 8 or more carbon atoms, X represents an ether or ester group,
Is glycerin having 3 to 6 carbon atoms, trimethylolethane,
Trimethylolpropane, sorbitol, sorbitan,
A pentaerythritol residue, n is an integer of 10 to 50,
n ′ represents an integer of 2 to 5, and n × n ′ is 30 or more in any combination. Of the type (VIII), particularly preferred as the hydrophilic nonionic surfactant in the present invention are 20 to 100 moles of ethylene oxide adduct of oleic acid monoglyceride and stearyl glyceryl ether (batyl alcohol). Type (IX):

[0029]

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(In the formula, R represents an alkane or alkene group having 8 or more carbon atoms, X represents an ether or ester group, and R '
Is glycerin having 3 to 6 carbon atoms, trimethylolethane,
Trimethylolpropane, sorbitol, sorbitan,
A pentaerythritol residue, n is an integer of 1 to 10,
n ′ represents an integer of 10 to 50, n ″ represents an integer of 2 to 5, and n ′ × n ″ is 30 or more in any combination. Among the types (IX), particularly preferred as the hydrophilic nonionic surfactant in the present invention are oleic acid monoglyceride or propylene oxide 1 of batyl alcohol.
１２12 mol adduct, and ethylene oxide 20８8
0 mol was added.

It should be noted that only one of the hydrophilic surfactants may be selected and used, or if necessary, 2
You may use it in combination of 2 or more types. The content of the hydrophilic surfactant in the first agent or the second agent is 0.1 to 10.0% by weight, preferably 1.0 to 5.0% by weight.

Next, the water-soluble solvent has the effect of dissolving the above-mentioned hydrophilic nonionic surfactant and efficiently orienting it at the interface with the oil phase to be added thereafter. Lower polyhydric alcohols, ketones, aldehydes, ethers, amines, lower fatty acids, and other hydrophilic substances capable of dissolving the above surfactants can be freely selected from a very wide range of substances. it can.

Specific examples of the water-soluble solvent include alcohols such as methanol, ethanol, propanol, isopropanol, and benzyl alcohol, glycerin, ethylene glycol, diethylene glycol, triethylene glycol, hexanediol 2.5 and 2.3.
Polyhydric alcohols (molecular weight 60 to 2000) such as butylene glycol, heptanediol, 2.4 hexylene glycol, 1.5 pentanediol, 1.4 butanediol, propylene glycol, 1.3 butylene glycol, dipropylene glycol, and acetone , Acetonylacetone, ketones such as diacetone alcohol, formaldehyde, aldehydes such as acetaldehyde, ethylene oxide, dioxane, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether,
Ethylene glycol monopropyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, ethylene glycol monoisobutyl ether, diethylene glycol monomethyl ether, ethylene glycol monopropyl ether (monoisopropyl ether), dimethylene glycol monoethyl ether, dimethylene glycol monomethyl ether , Dimethylene glycol monobutyl ether, dimethylene glycol diethyl ether, ethoxy triglycol, monopropylene glycol methyl ether, dipropylene glycol methyl ether, tripropylene glycol monomethyl ether, ethylene glycol monomethyl ether acetate, diethylene glycol monomethyl ether acetate, acetic acid Ethers such as ethylene glycol monoethyl ether, monoethanolamine, diethanolamine, triethanolamine, positive butylamine, ethylenediamine, propylenediamine, ethylamine, pyridine, amines such as cyclohexylamine,
Formic acid, acetic acid, butyric acid, lower fatty acids such as lactic acid, etc., are selected from methoxyglycol acetate, methyl lactate, ethyl lactate, acetonitrile, tetrahydrofuran, furfuryl alcohol and the like. One type may be used, and in some cases, the solubility of the surfactant can be freely changed by mixing two or more types of water-soluble solvents, which is very convenient. The content of the water-soluble solvent in the first agent or the second agent is 0.1 to 50.0% by weight, preferably 1.0 to 10.0% by weight.

As for the oil component, almost all of the commonly used oil classifications, from non-polar oils to polar oils such as silicone oils, hydrocarbon oils and ester oils, can be emulsified. Specific examples include silicone oils such as dimethylpolysiloxane, methylphenylpolysiloxane, diphenylpolysiloxane, and methylhydrogenpolysiloxane, liquid paraffin, squalane, terpene-based hydrocarbons, other synthetic hydrocarbon oils, and linear oils. Or branched alcohol esters of linear or branched fatty acids such as glycerin esters of branched fatty acids, for example glyceryl-tri-2-ethylhexanoate, glyceryl-tri-isostearate, for example trimethylolpropane-tri-2-ethylhexano Ester, pentaerythritol-tetra-2-ethylhexanoate, and other ester oils such as 2-ethylhexylic acid ester of glycerin-sorbitan condensate and hexadecyl adipate. Only one type of these oil components may be selected and used, or two or more types may be used in combination if necessary. The blending amount of the oil component is 1.0 to 80.0% by weight, preferably 5.0 to 20.0% by weight in the first agent or the second agent.

Regarding the quantitative relationship of the oil-in-water emulsion in the present invention, the composition of the oil-in-water emulsion in the first step is such that the oil content is 1 to 90 parts, and the water-soluble solvent is 1 to 90 parts.
Parts, hydrophilic nonionic surfactant in the range of 0.2 to 10 parts. Next, in the second stage, the emulsions 5-95
Parts are diluted with 95 to 5 parts of an aqueous phase component to prepare a stable oil-in-water emulsion. The details of the method for producing an oil-in-water emulsion are described in JP-B-57-292.
No. 13 has been described.

The oil-in-water emulsion of the present invention comprises the first
By using at least one of the second agent and the second agent, it is possible to prevent dripping after mixing the two agents. Particularly when the oil-in-water emulsion of the present invention is used as the first agent, the first agent is prepared by adding an oxidizing dye to a water-soluble solvent in the first step of the oil-in-water emulsion. By doing so, the dispersibility of the oxidation dye in the system becomes very good, and the time required for the manufacturing process can be easily shortened.

Examples of the oxidation dye contained in the first agent include p-phenylenediamine, p-toluylenediamine,
N-methyl-p-phenylenediamine, N, N-dimethyl-p-phenylenediamine, N, N-diethyl-2methyl-p-phenylenediamine, N-ethyl-N- (hydroxyethyl) -p-phenylenediamine, Chlor-
p-phenylenediamine, N, N-bis- (2-hydroxyethyl) -p-phenylenediamine, methoxy-p
-Phenylenediamine, 2,6-dichloro-p-phenylenediamine, 2-chloro-6-bromo-p-phenylenediamine, 2-chloro-6-methyl-p-phenylenediamine, 6-methoxy-3-methyl-p -Phenylenediamine, 2,5-diaminoanisole, N- (2-hydroxypropyl) -p-phenylenediamine, N-2
- one or several NH _2, such as methoxy ethyl -p- phenylenediamine - group, NHR ¹ - groups or N (R ¹⁾ ₂ -
A group, (R ¹ represents an alkyl group having 1 to 4 carbon atoms or a hydroxyalkyl group), p-diamines; 2,
5-diaminopyridine derivative; para-aminophenol,
2-methyl-4-aminophenol, 3-methyl-4-
Aminophenol, 2-chloro-4-aminophenol, 3-chloro-4-aminophenol, 2,6-dimethyl-4-aminophenol-3,5-dimethyl-4-
Aminophenol, 2,3-dimethyl-4-aminophenol, 2,5-dimethyl-4-aminophenol, 2,
P of 4-diaminophenol, 5-aminosalicylic acid, etc.
-Aminophenols, o-aminophenols, o-
Phenylenediamines, α-naphthol, o-cresol, m-cresol, 2,6-dimethylphenol,
2,5-dimethylphenol, 3,4-dimethylphenol, 3,5-dimethylphenol, benzcatechin,
Pyrogallol, 1,5-dihydroxynaphthalene, 1,
7-dihydroxynaphthalene, 5-amino-2-methylphenol, hydroquinone, 2,4-diaminoanisole, m-toluylenediamine, 4-aminophenol,
Resorcin, resorcin monomethyl ether, m-phenylenediamine, 1-phenyl-3-methyl-5-pyrazolone, 1-phenyl-3-amino-5-pyrazolone,
1-phenyl-3,5-dimethyl-pyrazolidine, 1-
Methyl-7-dimethyl-amino-4-hydroxy-2-
Quinolone, m-aminophenol, 4-chlororesorcin, 2-methylresorcin, 2,4-diaminophenoxyethanol, 3,5-diamino-trifluoromethylbenzene, 2,4-diamino-fluorobenzene, 3,5-
Diamino-fluorobenzene, 2,4-diamino-6-hydroxypyrimidine, 2,4,6-triaminopyrimidine, 2-amino-4,6-dihydroxypyrimidine, 4
-Amino-2,6-dihydroxypyrimidine, 4,6-
Examples thereof include diamino-2-hydroxypyrimidine and 2,6-diaminopyrimidine. The blending amount of these oxidation dyes is 0.1 to 10.0% by weight in the first agent.

The second agent in the oxidative hair dye according to the present invention contains an oxidant which reacts with the oxidative dye in the first agent to develop a color of the oxidative dye. When the oil-in-water emulsion of the present invention is used as the second agent, the second agent may be prepared by previously adding an oxidizing agent to water in the second step of producing the oil-in-water emulsion.

Examples of such oxidizing agents include hydrogen peroxide, persulfates, percarbonates and the like. The content of these oxidizing agents is 0.1 to 10.0% by weight in the oxidative hair dye.
It is.

The mixing ratio of the first agent and the second agent is the first
There is no particular limitation as long as the effect of the main agent contained in the agent is not impaired. In the present invention, one or both of the first agent and the second agent, other components used in a usual oxidative hair dye, for example, perfumes, pH adjusters, alcohols such as aromatic alcohols and polyhydric alcohols, and cations. Surfactant,
A moisturizer, an antiseptic, an anti-UV agent, a sequestering agent, a reducing agent and the like can be appropriately added within a range that does not impair the effects of the present invention.

[0041]

Next, the present invention will be described in more detail by way of examples. Note that the present invention is not limited by this. The compounding amount is% by weight.

Examples 1 to 3 and Comparative Examples 1 to 3 In addition to the combinations shown in Table 1, ammonia water (28
%), 3.0% by weight, an appropriate amount of fragrance, and the balance of ion-exchanged water were added to prepare the first oxidative hair dye. The manufacturing methods of Examples 1 to 3 and Comparative Example 3 at this time are as follows.

(1) Manufacturing method of Examples 1 to 3 (first agent) First, a hydrophilic nonionic surfactant was added to a water-soluble solvent to prepare 5
Heat and dissolve at 0-55 ° C. Cool it to 40 ° C,
Add dye and stabilizer and dissolve. Oil phase is 50 to 5
The temperature is adjusted to 5 ° C., and the oil phase is gradually stirred and added to the water-soluble solvent phase for emulsification to obtain a gel or an oil-in-water emulsion. This is further diluted with an aqueous phase and cooled to 25-30 ° C by stirring to obtain a stable gel or oil-in-water emulsion.

(2) Method for producing Comparative Example 3 (first agent) A hydrophilic nonionic surfactant and a water-soluble solvent are dissolved in water heated to 70 to 80 ° C. The oil phase is also adjusted to 70 to 80 ° C., and the mixture is gradually added to the aqueous phase with stirring to emulsify.
The dye and stabilizer are previously dissolved in water heated to 35 to 40 ° C. After gradually cooling the emulsified phase to 40 ° C., the dye parts are added and stirred to obtain an oil-in-water emulsion.

Using each of the obtained first agents and the second agent having the formulation shown in Table 2, the temperature stability and the dryness and the feeling of dryness when applied to the hair when applied to hair were measured according to the following methods and standards. The sex and sagging after application were evaluated. Table 3 shows the results.

(1) Evaluation of Temperature Stability <Evaluation Method> Each sample was stored at 50 ° C. for 1 month and then visually observed.

<Evaluation Criteria> A: No change. ◯: The viscosity was slightly lowered. Δ: Slightly separated. X: Separated.

(2) Evaluation of dry feeling after drying hair <Evaluation method> Evaluation panel evaluated the dry feeling after drying hair when a series of hair dyeing operations were performed using each sample.

<Evaluation Criteria> ⊚: Smooth and non-drying. ○: Not dry. Δ: Somewhat dry. X: Remarkably dry.

(3) Evaluation of operability <Evaluation method> Each sample was applied to hair by a special panel for evaluation, and its operability was evaluated.

<Evaluation Criteria> A: Good adhesion to hair and easy spreading. ○: Easy to extend. Δ: The spread is poor. X: Poor adhesion to hair and difficult to apply.

(4) Evaluation of sagging <Evaluation method> Each sample was applied to hair by a special evaluation panel, and sagging was evaluated.

<Evaluation Criteria> ⊚: Viscosity does not decrease and does not drop at all. ◯: Does not drip. Δ: Some dripping is seen. X: Viscosity is lowered, and it drops.

[0054]

[Table 1] ─────────────────────────────────── Examples Examples Comparative examples Blended ingredients ───── ────────────── 1 2 3 1 2 3 ─────────────────────────────── ───── Polyoxyethylene (40 mol) Cetyl ether 2.0 − 2.0 − − 2.0 Polyoxyethylene (20 mol) Cetyl ether − 2.0 − − − − Polyoxypropylene (12 mol) Lauryl ether 2.0 1.0 2.0 − − 2.0 Polyoxyethylene (5 mol) cetyl ether 2.0 1.0 2.0 − − 2.0 Polyoxilanoline alcohol derivative − 2.0 − − − − Ethylene glycol 200 5.0 − 5.0 − − 5.0 Dipropylene glycol 5.0 − − − − 5.0 Propylene glycol − 1.0 − − 5.0-KOH ---- 0.4-Dimethyl poly Roxane (20cs) 75.0 − 55.0 − − 75.0 Squalane − 20.0 − − − − Deodorized lanolin − 40.0 − − − − Purified petrolatum − 1.0 − − − − Beeswax − 2.0 − − − − Hexadecyl adipate − 24.0 − − − − − Stearic acid − − − − 8.0 − Stearyl alcohol − − − − 4.0 − Butyl stearate − − − − 6.0 − Paraphenylenediamine 1.0 1.0 1.0 1.0 1.0 1.0 L-Ascorbic acid 0.5 0.5 0.5 0.5 0.5 0.5 EDTA salt 0.2 0.2 0.2 0.2 0.2 0.2 ───────────────────────────────────

[0055]

[Table 2] ───────────────────────────────── Formulation of the second agent ─────── ─────────────────────────── (1) Liquid paraffin 1.0 wt% (2) Stearyl alcohol 3.0 (3) Polyoxyethylene (20) Cetyl ether 0.5 (4) Sodium lauryl sulphate 1.0 (5) Hydrogen peroxide solution (30%) 20.0 (6) Methylparaben proper amount (7) Sodium sulphate proper amount (8) Phosphate buffer pH 3 Adjust (9) Ion-exchanged water Residual ──────────────────────────────────

(Production method) (9) is heated to dissolve (6). (1) to (4) melted by heating are gradually added thereto and cooled. Further, (5), (7) and (8) are added.

[0057]

[Table 3] ──────────────────────────────── Examples Examples Comparative examples Evaluation ───────── ────────── 1 2 3 1 2 3 3 ──────────────────────────────── Temperature stability ◎ ◎ ◎ ◎ ○ ○ × Feeling dry after drying hair ◎ ◎ ◎ ◎ × △ ○ Operability ◎ ◎ ◎ △ ○ △ Dripping after application ◎ ◎ ◎ × × △ △ ──────────── ─────────────────────

As is clear from the results of Table 3, the product of the present invention was an excellent oxidative hair dye as compared with the comparative product. next,
A formulation example of the first agent according to the present invention will be given.

Example 4 (1) Ethylene glycol 200 5.0% by weight (2) Dipropylene glycol 5.0 (3) Polyoxyethylene (40 mol addition) Cetyl ether 2.0 (4) Polyoxypropylene (12 Lauryl ether 2.0 (5) Polyoxyethylene (5 mol addition) Cetyl ether 2.0 (6) Dimethyl polysiloxane (20cs) 75.0 (7) Collagen hydrolyzate 0.1 (8) Carboxy Vinyl polymer 0.5 (9) Perfume proper amount (10) L-ascorbic acid 0.5 (11) EDTA salt 0.2 (12) Paraphenylenediamine 1.0 (13) Ammonia water (28%) 5.0 ( 14) Ion-exchanged water balance (Production method) (3), (4), (5) and (9) are dissolved in (1) and (2), heated to 70 ° C and cooled to RT, (7) , (10), (11) and (12) are dissolved, then (6) is added and emulsified by a homomixer treatment. Next, (13) and (14) in which (8) was dissolved were added to the emulsion to obtain an oil-in-water type hair dye.

Example 5 (1) Ethylene glycol 200 5.0% by weight (2) Dipropylene glycol 5.0 (3) Polyoxyethylene (40 mol addition) Cetyl ether 2.0 (4) Polyoxypropylene (12 Lauryl ether 2.0 (5) Polyoxyethylene (5 mol addition) Cetyl ether 2.0 (6) Dimethylpolysilixane 75.0 (7) Amino-modified silicone 0.5-1.0 (Shin-Etsu Chemical) Industrial Co., Ltd .: APS-10-DMS) (8) Perfume proper amount (9) L-ascorbic acid 0.5 (10) EDTA salt 0.2 (11) Paraphenylenediamine 1.0 (12) Ammonia water (28% ) 8.0 (13) Ion-exchanged water balance (Production method) (3), (4), (5) and (8) are dissolved in (1) and (2), heated to 70 ° C and cooled to RT. Then, after dissolving (7), (9), (10) and (11), (6) is added and emulsified by homomixer treatment. Next, by adding (12), (13) to the emulsion,
An oil-in-water type hair dye was obtained.

Example 6 (1) Propylene glycol 7.0 wt% (2) Polyoxilanoline alcohol derivative 2.0 (30 mol addition) (3) Polyoxyethylene (20 mol addition) cetyl ether 2.0 (4 ) Polyoxypropylene (12 mol addition) Lauryl ether 1.0 (5) Polyoxyethylene (5 mol addition) Cetyl ether 1.0 (6) Squalane 20.0 (7) Deodorized lanolin 40.0 (8) Purified petrolatum 1.0 (9) Beeswax 2.0 (10) Hexadecyl adipate 24.0 (11) Collagen hydrolyzate 0.1 (12) Perfume proper amount (13) L-ascorbic acid 0.5 (14) EDTA salt 0.2 (15) Paraphenylenediamine 1.0 (16) Ammonia water (28%) 5.0 (17) Ion-exchanged water balance (Production method) (2), (3), (4), (1) And heat to dissolve at 50 ° C. On the other hand, after dissolving (6), (7), (8), (9), and (10) at 70 ° C, (12) was added to adjust the temperature to 50 ° C and stirring was continued. While gradually adding to (1), emulsify by homomixer treatment. Next, in the emulsion (11), (14), (15), (1
An oil-in-water type hair dye was obtained by adding (17) in which 6) was dissolved.

[0062]

As described above, the oxidative hair dye of the present invention is excellent in temperature stability, has good adhesion to hair, is easy to spread, and is free from sagging due to a decrease in viscosity after application. The hair has a smooth texture and is dry and dry.

Claims (2)

[Claims] 1. A two-component oxidative hair dye, which comprises a first agent containing an oxidative dye and a second agent containing an oxidant and is mixed immediately before use, wherein the first agent and / or Alternatively, the second agent adds the hydrophilic nonionic surfactant to the water-soluble solvent as the first step, and then adds the oil phase to this to prepare an oil-in-water emulsion, and the second step An oxidative hair dye, comprising an oil-in-water emulsion obtained by adding water to the emulsion. 2. A method for producing a two-pack type oxidative hair dye, which comprises a first agent containing an oxidative dye and a second agent containing an oxidant, and is mixed immediately before use. As a first step, the method for producing an agent comprises adding an oxidation dye and a hydrophilic nonionic surfactant in a water-soluble solvent, and then adding an oil phase to the oil-in-water emulsion to prepare an oil-in-water emulsion. A method for producing an oxidative hair dye, which is carried out by adding water to the emulsion in two steps.