JP5489425B2 - Method for producing acidic hair dye composition - Google Patents

Description

  The present invention relates to a novel method for producing an acidic hair dye composition used for an acidic hair dye for dyeing hair.

  When the hair dye is a liquid having a low viscosity, the hair dye falls on the scalp and the face and the scalp and the face become dirty. Therefore, the hair dye needs to have a certain degree of viscosity. Therefore, in general acid hair dye compositions, anionic polymers are used as thickeners for improving operability. Since this anionic polymer dissociates in an acidic environment and generates sodium ions to inhibit dyeing, it is usually dissolved in purified water and neutralized with an alkali agent when swollen (see Patent Document 1).

  However, when an anionic polymer is used as a thickener, there is a problem that the dyeability is lowered due to the added alkali agent. That is, an acidic dye is used for the acidic hair dye, and the acidic dye improves the dyeability in the acidic region, but when an alkaline agent is added, the pH rises and the dyeability on the hair is impaired.

Therefore, there has been a need for a technique for producing an acidic hair dye composition that exhibits excellent operability without impairing the dyeability of an acidic dye while using an anionic polymer.
JP 2002-179538 A

  The present invention has been made in response to such conventional circumstances and recent trends, and is a method for producing an acidic hair dye composition having good operability and significantly improved dyeability without blending an alkaline agent. The purpose is to provide.

  In order to solve the above problems, the present inventors have conducted research, and as a result, an acidic hair dye excellent in operability and dyeability by dissolving an anionic polymer in an organic solvent and then adding purified water or the like. It was found that a composition was obtained. Based on this knowledge, the present inventors have further studied and completed the present invention.

That is, the present invention is as follows.
Item 1. A method for producing an acidic hair dye composition, comprising the following steps:
(1) A method comprising a step of dissolving an anionic polymer in an organic solvent, and (2) a step of mixing purified water, an acid and an acid dye into the solution obtained in step (1).
Item 2. Item 2. The method according to Item 1, wherein the anionic polymer is at least one selected from the group consisting of alkyl-modified carboxyvinyl polymer, carboxyvinyl polymer, polyacrylic acid or a salt thereof.
Item 3. Item 3. The method according to Item 1 or 2, wherein the amount of the anionic polymer is 0.01 to 10% by weight.
Item 4. Item 4. The method according to any one of Items 1 to 3, wherein the organic solvent is one or more alcohols.
Item 5. The acidic hair dye composition obtained by the method in any one of claim | item 1 -4.

  In the present invention, the anionic polymer is dissolved in an organic solvent, and then purified water and the like are blended, so that the viscosity is stable over a long period of time, the operability is improved, the dyeing property is improved, and a high conditioning effect is obtained. It became possible to obtain the acidic hair dye composition which has. In the conventional production method, when the carboxyvinyl polymer is dissolved in water and acidified after neutralization with an alkali agent, dissociation occurs and sodium ions are generated, which inhibits the dyeing property. According to the production method of the present invention, such dissociation does not occur and there is an advantage that the dyeing property is remarkably improved.

The process in the manufacturing method of the acidic hair dye composition of this invention is demonstrated in detail below.
<Step (1)>
Step (1) is a step of dissolving an anionic polymer in an organic solvent.

  The anionic polymer blended in the step (1) of the present invention is not particularly limited as long as it is used for imparting thickening of hair dyes. For example, alkyl-modified carboxyvinyl polymer, carboxyvinyl polymer, polyacrylic Examples include acids or salts thereof. Of these, carboxyvinyl polymer is preferably exemplified.

  These can be easily obtained commercially, and examples thereof are: As carboxyvinyl polymer, for example, Carbopol 934, 940, 941 (both manufactured by Goodrich), Akpec HV-505 (Sumitomo) Seika Chemical Co., Ltd.), Hibiswako 104, 105 (both manufactured by Wako Pure Chemical Industries, Ltd.) and the like, and alkyl-modified carboxyvinyl polymers include PEMULEN TR-1, PEMULEN TR-2 (manufactured by Goodrich), etc. Is mentioned.

  In the acidic hair dye composition of the present invention, these anionic polymers are blended in an amount of 0.01 to 10% by weight, preferably 0.1 to 6.0% by weight, based on the total composition finally obtained. A blending amount in the range of 0.01 to 10% by weight is preferable because viscosity stability is sufficient and operability is good.

  The organic solvent for dissolving the anionic polymer is not particularly limited, and aromatic alcohol, lower alcohol, polyhydric alcohol and the like can be used. For example, aromatic alcohols include benzyl alcohol, phenylpropanol, 2-phenylethyl alcohol, dimethylbenzyl carbinol, α-methylbenzyl alcohol, phenethyl alcohol, 2-benzyloxyethanol, phenoxyethanol, p-anisyl alcohol, 2- Examples of the lower (1-5) alcohol include ethyl alcohol, isopropyl alcohol, and butyl alcohol. Examples of the polyhydric alcohol include ethylene glycol, propylene glycol, 1 , 3-butylene glycol, isoprene glycol, glycerin, diglycerin, dipropylene glycol, polyethylene glycol, polypropylene glycol and the like. Further, N-alkylpyrrolidones such as N-methylpyrrolidone may be used. Of these, benzyl alcohol, ethanol, N-methylpyrrolidone and the like are preferred.

  One or more of these organic solvents are blended so as to be 1 to 50% by weight, preferably 5 to 40% by weight, based on the entire acidic hair dye composition. A blending amount in the range of 1 to 50% by weight is preferable because a sufficient dyeing effect is exhibited.

  In the step (1), a preferable combination of an organic solvent and an anionic polymer is a combination of benzyl alcohol and / or ethanol and carboxyvinyl polymer; or at least one selected from benzyl alcohol, ethanol and N-methylpyrrolidone Combinations of carboxyvinyl polymer and the like can be mentioned, and more preferable examples include benzyl alcohol and a combination of benzyl alcohol and carboxyvinyl polymer. When benzyl alcohol and benzyl alcohol are used in combination as an organic solvent, benzyl alcohol: ethanol is usually blended at a ratio of about 1: 5 to 5: 1.

  Moreover, it is preferable to mix | blend the weight ratio of an organic solvent and anionic polymer so that a polymer may be 0.5-30.0 with respect to the organic solvent 100, More preferably, it will be 2.0-20.0. Blend as follows.

  The organic solvent in which the anionic polymer is thus obtained is used for the next step as it is.

<Step (2)>
Step (2) is a step of mixing purified water, acid and dye into the solution obtained in step (1).

  In the step (2) of the present invention, the acid blended in the acidic hair dye composition is not particularly limited as long as it is an acid used in the acidic hair dye composition. For example, lactic acid, citric acid, glycol Examples thereof include organic acids such as acid, tartaric acid, levulinic acid, malic acid and acetic acid, and inorganic acids such as phosphoric acid and hydrochloric acid, and the blending amount is such that the pH of the composition is 1.5 to 4.0, preferably pH 2.5. It mix | blends so that it may become a strongly acidic area | region of -3.0. If it is lower than 1.5, it is not preferable from the viewpoint of dye stability and skin irritation, and if it is higher than 4.0, sufficient dyeing power cannot be obtained, so that the pH is 1.5 to 4.0. preferable.

  The acidic dye blended in the acidic hair dye composition of the present invention is preferably a dye that is permitted to be used for coloring pharmaceuticals, quasi-drugs, and cosmetics that do not show harmful effects on the human body, Legal dyes listed in “Ministerial Ordinance for Determining Tar Color that can be Used for Pharmaceuticals” are extremely effective, and one or more of these can be blended.

  More specifically, those used as hair dyes as acid dyes can be used in a wide range. Particularly preferred are triphenylmethane dyes such as Blue No. 1, azo dyes such as Daidai No. 205, Examples include quinoline dyes such as yellow No. 203, xanthine dyes such as red No. 106, indigo dyes such as blue No. 2, anthraquinone dyes such as purple No. 401, and nitro dyes such as yellow No. 403 (1).

  Although it will not specifically limit if it is the compounding quantity currently mix | blended normally as a compounding quantity of the said dye, For example, 0.1-5 weight% with respect to the whole acidic hair dye composition, Preferably it is 0.15-3. It is preferable to blend in an amount of% by weight.

  In step (2), the order and procedure for blending purified water, acid and acid dye are not particularly limited, and they may be blended all at the same time. In addition, purified water is blended first, and then acid and acid dye are blended. May be blended in order.

<Others>
In the production method of the present invention, the acidic hair dye composition obtained by the steps (1) and (2) described above does not interfere with the effects of the present invention in addition to the above components, as well as other components usually used in acidic hair dyes. As long as it is possible, it can mix | blend suitably. When mix | blending another component, it is preferable to mix | blend after the said process (1) and (2).

  Examples of components that can be blended include solubilizers other than the above organic solvents, dispersants, thickeners, chondroitin sulfate, hyaluronate, diglycerin, sorbitol, maltitol, pyrrolidone carboxylic acid, lactose, oligosaccharides Etc. can be mix | blended with this invention acidic hair dye composition.

  Further, for example, oily components such as lanolin, squalane, liquid paraffin, petrolatum, higher fatty acid, triglyceride, ester oil and the like can be blended.

  In addition, if necessary, in the production method of the present invention, in addition to the above components, silicones, animal and plant extracts, ultraviolet absorbers, bactericides, oxidizing agents, as long as the effects, stability, and pH of the hair dye are not impaired. Inhibitors, preservatives, chelating agents, fragrances and the like can also be blended.

  In the production method of the present invention, it is not always necessary to use an alkali agent as a neutralizing agent. Rather, it is preferable not to add an alkali agent because dyeing properties are improved. Therefore, in a preferred embodiment of the present invention, an alkali agent in an amount exceeding the range that does not affect the dyeing property and pH is not added.

  The acidic hair dye composition obtained by the production method of the present invention is excellent in operability and has a viscosity that does not cause dripping when applied to the hair. Specifically, the viscosity of the composition obtained by the present invention is usually 5000 mPa · s to 35000 mPa · s, preferably 8000 mPa · s to 25000 mPa · s. Here, the viscosity is measured after a No. 6 rotor is rotated at 20 rpm for 5 minutes at 20 ° C. using a B-type viscometer (manufactured by BROOKFIELD).

  The present invention also includes an acidic hair dye composition obtained by the above production method.

  The acidic hair dye composition obtained by the present invention can be used in any form in which the acidic hair dye composition can be generally used. For example, forms such as semi-permanent hair dye, temporary hair dye, hair dye for gray hair dye, hair dye dye, hair dye for rinsing and hair dyeing can be taken.

  The acidic hair dye composition obtained by the present invention can be obtained by a method similar to that of conventional acidic hair dyes, for example, an applicator (a method of applying directly to the hair from a container) or a brush application (a method of applying to the hair by brush). It can be used for formulas, combs, brushing (combing, applying hair dye to brushes, and applying). Such a dosage form can be appropriately prepared according to the desired form of use. For example, it can be prepared in the form of liquid, cream, gel, spray, mousse, stick and the like.

  The present invention will be described more specifically with reference to the following examples. However, the present invention is not limited to these examples.

[Evaluation method]
Production of acidic hair dye composition (Examples 1 to 7)
Dissolve carboxyvinyl polymer (Apeck HV-505, manufactured by Sumitomo Seika Co., Ltd.) in benzyl alcohol and ethanol, and then add purified water, acid (lactic acid, citric acid or glycolic acid) and dye (purple 401). Thus, an acidic hair dye composition was obtained. The amount of each component is shown in Table 1. In addition, pH of each hair dye composition was adjusted to pH 2.5-3.0.
( Comparative Example 7 )
Dissolve carboxyvinyl polymer (Apeck HV-505, manufactured by Sumitomo Seika Co., Ltd.) in benzyl alcohol and ethanol, and then add purified water, acid (lactic acid, citric acid or glycolic acid) and dye (purple 401). Finally, an acidic hair dye composition was obtained by adding sodium hydroxide. The amount of each component is shown in Table 1. In addition, pH of the hair dye composition was adjusted to pH 2.5-3.0.

(Comparative Examples 1-3)
Carboxyvinyl polymer (Appec HV-505, manufactured by Sumitomo Seika Co., Ltd.) is dispersed in purified water, and an alkali agent (sodium hydroxide, 2-amino-2-methyl-1-propanol (AMP), or monoethanolamine is dispersed therein. ) And neutralized to dissolve. Thereafter, lactic acid and a dye (purple No. 401) were added, and then benzyl alcohol and ethanol were added to obtain an acidic hair dye composition. The amount of each component is shown in Table 2. In addition, pH of each hair dye composition was adjusted to pH 2.5-3.0.
(Comparative Examples 4-5)
Purified water, lactic acid and a dye (purple No. 401) were added to benzyl alcohol and ethanol, and sodium hydroxide was then added in Comparative Example 4. The amount of each component is shown in Table 2. In addition, pH of each hair dye composition was adjusted to pH 2.5-3.0.
(Comparative Example 6)
In Comparative Example 6, the compounding components are the same as those in Comparative Example 1, but the production method is different. In the production method of Comparative Example 6, carboxyvinyl polymer (Apeck HV-505, manufactured by Sumitomo Seika Co., Ltd.) is dispersed and dissolved in purified water, and then benzyl alcohol and ethanol, acid (lactic acid, citric acid or glycolic acid) and A dye (purple 401) was added, and finally sodium hydroxide was added to obtain an acidic hair dye composition. The amount of each component is shown in Table 2. In addition, pH of the hair dye composition was adjusted to pH 2.5-3.0.

Test example
Dyeing power test 5 g of each of Examples 1 to 7 and Comparative Examples 1 to 7 was applied to a yak hair bundle (10 cm to 1 g manufactured by Staffus Co., Ltd.), left at 45 ° C. for 15 minutes, and then shampooed. Wash with hair and dry. At this time, operability and dyeing property were evaluated by 10 expert panelists.
(Dyeing property)
◎: Very good dyeability ○: Good dyeability
A: Not dripping down (very easy to apply)
○: Almost no dripping (easy to apply)
△: not dripping very much (slightly difficult to paint)
×: Easy to sag (hard to paint)
The results of dyeability and operability are shown in Tables 1-2 and FIGS.
Viscosity The viscosity of each composition (final product) was measured using a B-type viscometer (BROOKFIELD, 20 ° C., No. 6 rotor, 5 minutes, 20 rpm).

[result]
In Comparative Example 1-3 in which the carboxyvinyl polymer was dispersed in purified water and neutralized with an alkali agent (sodium hydroxide), the dyeing result was poor. However, when no alkali agent is added in the conventional method, the operability (dripping) is deteriorated although the dyeing property is improved (Comparative Example 5). Moreover, in Comparative Examples 4 and 5 to which no carboxyvinyl polymer was added, sufficient viscosity was not obtained, and operability was very poor.

Furthermore, in Comparative Example 7 , sodium hydroxide was added at the end in addition to the method procedure according to the present invention. When the results of Example 1-7 and Comparative Example 7 were compared, in the method of the present invention, alkali was added. It turned out that it is not preferable to add an agent because the dyeing property is rather inferior.

  The viscosity is a viscosity that does not cause any problem in operability in any of the examples, and is not shown in the table. However, the viscosity change rate (the acidic hair dye composition of the examples is 3 in a 45 ° C. constant temperature bath). Stored for months, using a B-type viscometer (20 ° C., No. 6, rotor, 20 rpm, 5 minutes later), formula: viscosity change rate = (viscosity before storage−viscosity after storage) / viscosity before storage × 100 It was found that the stability was between 13 and 21 in any of the examples.

  From the above, it was shown that by the method of the present invention, an acidic hair dye composition having a stable viscosity over a long period of time and excellent in both operability and dyeability can be obtained.

FIG. 1 is a photograph showing the dyeability of Example 1-4. FIG. 2 is a photograph showing the dyeing properties of Example 5-7 and Comparative Example 7 . FIG. 3 is a photograph showing the dyeing properties of Comparative Example 1-4. FIG. 4 is a photograph showing the dyeing properties of Comparative Example 5-6.

Claims (3)

A method for producing an acidic hair dye composition not containing an alkali agent, comprising the following steps:
(1) At least one anionic polymer selected from the group consisting of an alkyl-modified carboxyvinyl polymer, carboxyvinyl polymer, polyacrylic acid or a salt thereof in an organic solvent is used in an amount of 4 to 4 in the acidic hair dye composition. A method comprising dissolving 6% by weight, and (2) thereafter, mixing purified water, an acid and an acid dye into the solution obtained in step (1). The method of claim 1 , wherein the organic solvent is one or more alcohols. The acidic hair dye composition which does not mix | blend an alkaline agent obtained by the method of Claim 1 or 2 .

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