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JP6503166B2 - Emulsifiable aerosol composition containing an oxidizing agent - Google Patents
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JP6503166B2 - Emulsifiable aerosol composition containing an oxidizing agent - Google Patents

Emulsifiable aerosol composition containing an oxidizing agent Download PDF

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JP6503166B2
JP6503166B2 JP2014168194A JP2014168194A JP6503166B2 JP 6503166 B2 JP6503166 B2 JP 6503166B2 JP 2014168194 A JP2014168194 A JP 2014168194A JP 2014168194 A JP2014168194 A JP 2014168194A JP 6503166 B2 JP6503166 B2 JP 6503166B2
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伸二 大島
伸二 大島
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Dariya Co Ltd
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Description

本発明は、染毛剤で用いられる酸化剤を含有する乳化型エアゾール組成物に関するものである。 The present invention relates to an emulsified aerosol composition containing an oxidizing agent used in a hair dye.

染毛剤としては、染毛剤、脱染剤、脱色剤、脱染・脱色剤などが知られており、2種類以上の剤を用時混合して調合される。染毛剤は一般的に第2剤として、毛髪の色を変化させるために酸化染料を毛髪中で化学反応(酸化重合)させ、色素を形成し毛髪内部に固定させたり、毛髪自身が持つメラニン色素を酸化反応によって分解して、毛髪を明るく見せる目的として、酸化剤含有組成物を用いてきた。 As a hair dye, a hair dye, a decoloring agent, a decoloring agent, a decoloring agent, a decoloring agent, etc. are known, and two or more types of agents are mixed and mixed at the time of use. A hair dye is generally used as a second agent, which chemically reacts (oxidatively polymerizes) an oxidation dye in the hair to change the color of the hair, forms a dye and fixes it inside the hair, or melanin of the hair itself Oxidizing agent containing compositions have been used for the purpose of decomposing the pigment by an oxidation reaction to make the hair appear brighter.

酸化剤含有組成物には酸化剤として過酸化水素が用いられる。過酸化水素は、不安定で酸素を放出して分解しやすく、この分解を抑えるため安定化剤として、フェナセチン、1−ヒドロキシエタン−1,1−ジホスホン酸、スズ酸ナトリウム、アセトアニリドなどが用いられる。(例えば特許文献1) In the oxidizing agent-containing composition, hydrogen peroxide is used as an oxidizing agent. Hydrogen peroxide is unstable and easily released oxygen and decomposed. As a stabilizer to suppress this decomposition, phenacetin, 1-hydroxyethane-1,1-diphosphonic acid, sodium stannate, acetanilide, etc. are used . (For example, Patent Document 1)

また、酸化剤含有エアゾール組成物は、当該組成物中に含まれている過酸化水素が、温度、pH、内容物の成分、容器内の金属粉、微生物等によって容易に分解するため、容器が膨張する危険性を有している。特にエアゾール製剤の場合には一般のプラスチック容器等とは異なり完全な密封状態となるため、過酸化水素の分解によって発生する酸素が容器内の内圧上昇をもたらし、内容物の吐出量が設定値より多くなり、製剤としての染毛性・脱色性に影響が出る可能性がある。(特許文献2) In addition, since the oxidizing agent-containing aerosol composition is easily decomposed by the temperature, pH, components of contents, metal powder in the container, microorganisms, etc., the hydrogen peroxide contained in the composition is There is a risk of swelling. Especially in the case of an aerosol preparation, unlike a general plastic container etc., since it is completely sealed, oxygen generated by the decomposition of hydrogen peroxide causes an increase in the internal pressure in the container, and the discharge amount of the contents It may increase and may affect the hair dyeability and decolorization as a preparation. (Patent Document 2)

また、エアゾール組成物で現在の市場で最も広く用いられている噴射剤は、LPGやDME等である。しかし、LPGやDME等を噴射剤として用いた場合には、使用環境が低温の時には、好適な泡沫状態の吐出物を得ることができず、また、使用環境が高温の時には、吐出された泡は嵩比重が極度に小さいものになる等、泡沫状態が使用環境によって大きく変化してしまうという欠点がある。(特許文献3) Also, the most widely used propellants in the current market for aerosol compositions are LPG, DME, etc. However, when LPG, DME, etc. are used as the propellant, it is not possible to obtain a suitable foam-like discharge when the use environment is low temperature, and when the use environment is high temperature, the discharged foam is used. Has a disadvantage that the foam state changes greatly depending on the use environment, such as extremely low bulk density. (Patent Document 3)

特開平7−258045JP-A-7-2558045 特開平8−301740JP-A-8-301740 特開2011−37772JP 2011-37772

特許文献1および2の記載内容では、過酸化水素の安定化を目的としているため、エアゾール製剤化した際には低温では好適な泡沫状態の吐出物を得ることができない。また、乳化組成物をエアゾール製剤化する際に、油剤が活性剤の発泡性を阻害し、好適な泡沫状態を得ることが困難である。 In the contents of Patent Documents 1 and 2, the purpose is to stabilize hydrogen peroxide, and therefore, when formulated into an aerosol, it is not possible to obtain a suitable foam-like discharge at low temperatures. In addition, when the emulsion composition is formulated into an aerosol, it is difficult for the oil to inhibit foaming of the active agent and to obtain a suitable foam state.

さらに、過酸化水素の安定化剤としてフェナセチンが知られているが、フェナセチンは、腎障害や腎盂、膀胱腫瘍の発生リスクがあるため、特許文献1および2に関しては、特許技術を行使し、エアゾール製剤化することは困難である。 Furthermore, although phenacetin is known as a stabilizer for hydrogen peroxide, phenacetin exerts patented technology with respect to Patent Documents 1 and 2 because of the risk of developing renal failure, renal pelvis and bladder tumor. It is difficult to formulate.

特許文献3に関しては、低温では好適な泡沫状態の吐出物を得ることが出来るが、過酸化水素を含有した際の安定性は考慮されていない。 With regard to Patent Document 3, although a suitable foam-like discharge can be obtained at low temperatures, the stability when hydrogen peroxide is contained is not considered.

また、従来の技術では、過酸化水素の分解を抑制することが十分でなく、特に夏場の高温になる車内や、海外などへの運搬に用いられるコンテナ中で高温条件下に長時間さらされた場合、過酸化水素の安定性が低下する問題があった。 Moreover, in the prior art, it is not enough to suppress the decomposition of hydrogen peroxide, and it has been exposed to high temperature conditions for a long time especially in the container which is used for transportation in the car and overseas etc. In the case, there was a problem that the stability of hydrogen peroxide was reduced.

また、低温時の好適な泡沫状態の吐出物を得るために発泡性を良くしてしまうと、常温での吐出物の嵩比重が極度に小さいものになるため、染毛性や明度を損なう問題があった。 In addition, if the foamability is improved to obtain a suitable foam-like discharge at low temperature, the bulk specific gravity of the discharge at normal temperature becomes extremely small, and thus the problem of impairing the hair coloring and lightness was there.

本発明は、上記問題を解決するため鋭意検討した結果、(A)過酸化水素、(B)POEラウリルエーテルおよびPOEアルキル(12〜14)エーテルから選ばれる1種または2種以上、(C)アルカリ金属の水酸化物、(D)1−ヒドロキシエタン−1,1−ジホスホン酸を含有するエアゾール原液と、(E)噴射剤を含有し、エアゾール原液がpH4.5以下であることを特徴とする酸化剤を含有する乳化型エアゾール組成物を提供することによって本発明を完成させるに至った。 MEANS TO SOLVE THE PROBLEM As a result of earnestly examining this invention, in order to solve the said problem, 1 type, 2 or more types chosen from (A) hydrogen peroxide, (B) POE lauryl ether, and POE alkyl (12-14) ether, (C) An aerosol stock solution containing an alkali metal hydroxide, (D) 1-hydroxyethane-1,1-diphosphonic acid, and (E) a propellant, the aerosol stock solution having a pH of 4.5 or less The present invention has been accomplished by providing an emulsified aerosol composition containing an oxidizing agent.

本発明は、保管条件や運搬条件を考慮する必要がなく、高温条件下に長時間さらされても、過酸化水素の安定性に優れた酸化剤を含有する乳化型エアゾール組成物であり、なおかつ低温時の使用にも発泡性を損なうことなく使用できる酸化剤を含有する乳化型エアゾール組成物を提供することができる。 The present invention is an emulsion type aerosol composition containing an oxidizing agent excellent in hydrogen peroxide stability even when exposed to high temperature conditions without having to consider storage conditions and transport conditions, and It is possible to provide an emulsified aerosol composition containing an oxidizing agent that can be used at low temperatures without impairing the foamability.

本発明は、アルカリ剤を含有する第1剤と用時混合して使用される酸化剤を含有する乳化型エアゾール組成物であって、(A)過酸化水素、(B)POEラウリルエーテルおよびPOEアルキル(12〜14)エーテルから選ばれる1種または2種以上、(C)アルカリ金属の水酸化物、(D)1−ヒドロキシエタン−1,1−ジホスホン酸を含有するエアゾール原液と、(E)噴射剤を含有し、エアゾール原液がpH4.5以下であることを特徴とする酸化剤を含有する乳化型エアゾール組成物である。 The present invention is an emulsion type aerosol composition containing an oxidizing agent which is used by being mixed with a first agent containing an alkaline agent at the time, which comprises (A) hydrogen peroxide, (B) POE lauryl ether and POE. (E) an aerosol stock solution containing one or more selected from alkyl (12 to 14) ethers, (C) hydroxides of alkali metals, (D) 1-hydroxyethane-1,1-diphosphonic acid; 2.) An emulsifying aerosol composition containing an oxidant, which contains a propellant, and the aerosol stock solution has a pH of 4.5 or less.

本発明による酸化剤を含有する乳化型エアゾール組成物は(A)過酸化水素を含有する。(A)過酸化水素はアルカリ剤を含有する第1剤中に含有する酸化染料を毛髪中で化学反応(酸化重合)させ、色素を形成し毛髪内部に固定させ毛髪の染毛を行ったり、毛髪自身が持つメラニン色素を酸化反応によって分解して、毛髪を明るく見せることができる。 The emulsified aerosol composition containing the oxidizing agent according to the present invention contains (A) hydrogen peroxide. (A) Hydrogen peroxide chemically reacts (oxidatively polymerizes) an oxidation dye contained in the first agent containing an alkali agent in the hair to form a pigment and fix it inside the hair to dye the hair, The melanin pigment possessed by the hair itself can be decomposed by an oxidation reaction to make the hair appear bright.

本発明に用いられる前記(A)成分の含有量は、特に限定されないが、1〜6重量%が好ましい。前記(A)成分が1重量%未満の場合、酸化染料を十分に酸化重合することができないか、メラニンを十分に分解することができない恐れがある。また、前記(A)成分の含有量が6重量%を超える場合、毛髪に負担がかかり毛髪を損傷する恐れがある。なお、本発明において他の成分についての含有量を示す値は、特段の断りがない限り重量%とする。 Although content of the said (A) component used for this invention is not specifically limited, 1 to 6 weight% is preferable. When the amount of the component (A) is less than 1% by weight, there is a possibility that the oxidation dye can not be sufficiently oxidatively polymerized or the melanin can not be sufficiently decomposed. Moreover, when content of the said (A) component exceeds 6 weight%, there is a possibility that a load may be applied to hair, and hair may be damaged. In the present invention, values indicating the contents of other components are weight% unless otherwise specified.

本発明に用いられる前記(A)成分の残存率が経時的に低下していくと、酸化染料を十分に酸化重合することができないか、メラニンを十分に分解することができず、適正な染毛性または明度を得ることが出来ない恐れがある。 When the residual rate of the component (A) used in the present invention decreases with time, the oxidation dye can not be sufficiently oxidized and polymerized, or the melanin can not be sufficiently degraded, and appropriate dyeing can not be performed. There is a possibility that hairiness or lightness can not be obtained.

本発明に用いられる前記(B)成分は、エアゾール原液の発泡性を向上させる観点から、(B)POEラウリルエーテルおよびPOEアルキル(12〜14)エーテルから選ばれる1種または2種以上を含有することが好ましい。また、前記(B)成分は他の非イオン性界面活性剤とは違い、低温での発泡性に特筆すべき効果がある。 The component (B) used in the present invention contains one or more selected from (B) POE lauryl ether and POE alkyl (12 to 14) ether from the viewpoint of improving the foamability of the aerosol stock solution. Is preferred. Further, unlike the other nonionic surfactants, the component (B) has a remarkable effect on the foaming property at a low temperature.

本発明に用いられる前記(B)成分は、POEラウリルエーテルまたはPOEアルキル(12〜14)エーテルであれば、特に限定されないが、ポリオキシエチレン基の平均付加モル数が2〜15であることが好ましい。より好ましくは2〜9の範囲である。ポリオキシエチレン基の平均付加モル数が15より大きいと、5℃条件下での発泡性が悪くなる恐れがある。 The component (B) used in the present invention is not particularly limited as long as it is POE lauryl ether or POE alkyl (12 to 14) ether, but the average addition mole number of polyoxyethylene group is 2 to 15 preferable. More preferably, it is in the range of 2-9. If the average added mole number of the polyoxyethylene group is more than 15, the foamability at 5 ° C. may be deteriorated.

本発明に用いられる前記(B)成分の含有量は、特に限定されないが、1〜3%が好ましい。より好ましくは1.5〜2.5%の範囲である。前記(B)成分が1%未満の場合、十分な発泡性が得られず、液ダレする恐れがある。3%を超える場合、泡が使用時に頭髪内部に浸透しにくくなり、適正な染毛性または明度を得ることが出来ない恐れがある。 Although content of the said (B) component used for this invention is not specifically limited, 1 to 3% is preferable. More preferably, it is 1.5 to 2.5% of range. When the component (B) is less than 1%, sufficient foamability can not be obtained, and there is a risk of dripping. If it exceeds 3%, bubbles may not penetrate into the hair at the time of use, and there is a possibility that the proper hair dyeability or lightness can not be obtained.

本発明に用いられる前記(C)成分は、pH調整剤として用いられ、前記(A)成分の安定性を向上する特筆すべき効果がある。 The component (C) used in the present invention is used as a pH adjuster, and has a remarkable effect of improving the stability of the component (A).

本発明に用いられる前記(C)成分は、特に限定されないが、水酸化リチウム、水酸化ナトリウム、水酸化カリウム、水酸化ルビジウム、水酸化セシウムを用いることができ、前記(C)成分は1種または2種以上を含有してもよい。その中でも前記(C)成分は、過酸化水素の安定性の観点から水酸化ナトリウム、水酸化カリウムが好ましい。より好ましくは、水酸化カリウムである。 The component (C) used in the present invention is not particularly limited, and lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide can be used, and the component (C) is one type. Or you may contain 2 or more types. Among them, the component (C) is preferably sodium hydroxide or potassium hydroxide from the viewpoint of the stability of hydrogen peroxide. More preferably, it is potassium hydroxide.

本発明に用いられる前記(C)成分の含有量は、特に限定されないが、0.004〜1%が好ましい。より好ましくは0.02〜0.5%の範囲である。前記(C)成分が0.004%未満の場合、pH調整作用が十分に得られず、前記(A)成分を安定化することができない恐れがある。1%を超える場合、これ以上のpH調整作用を得ることはできず、製剤の安定性に悪影響を及ぼす恐れがある。 Although content of the said (C) component used for this invention is not specifically limited, 0.004 to 1% is preferable. More preferably, it is in the range of 0.02 to 0.5%. When the amount of the component (C) is less than 0.004%, the pH adjusting action may not be sufficiently obtained, and the component (A) may not be stabilized. If it exceeds 1%, no further pH adjustment action can be obtained, which may adversely affect the stability of the preparation.

本発明に用いられる前記(D)成分は、前記(A)成分の安定化剤として優れた金属封鎖作用、pH調整作用および前記(A)成分の安定性向上の効果がある。 The component (D) used in the present invention has an excellent sequestering action as a stabilizer for the component (A), a pH adjusting action, and an effect of improving the stability of the component (A).

本発明に用いられる前記(D)成分の含有量は、特に限定されないが、0.01〜2%が好ましい。より好ましくは0.05〜1%の範囲である。前記(D)成分が0.01%未満の場合、pH調整作用が十分に得られず、前記(A)成分を安定化することができない恐れがある。2%を超える場合、これ以上の金属封鎖作用やpH調整作用を得ることはできず、かえって製剤の安定性に悪影響を及ぼす恐れがある。 Although content of the said (D) component used for this invention is not specifically limited, 0.01 to 2% is preferable. More preferably, it is in the range of 0.05 to 1%. When the amount of the component (D) is less than 0.01%, the pH adjusting action may not be sufficiently obtained, and the component (A) may not be stabilized. If it exceeds 2%, no further sequestering action or pH adjustment action can be obtained, which may adversely affect the stability of the preparation.

本発明に用いられる前記(E)成分は、エアゾール原液を液ダレすることなく、安定した泡沫を得ることができる。 The component (E) used in the present invention can obtain stable foam without dripping the aerosol stock solution.

本発明に用いられる前記(E)成分は、特に限定されないが、LPG、ジメチルエーテル等の液化ガス、炭酸ガス、窒素ガス等の圧縮ガスを用いることができ、前記(E)成分は1種または2種以上を含有してもよい。その中でも前記(E)成分は、製剤の安定した吐出量を維持できる観点から、液化ガスが好ましい。 The component (E) used in the present invention is not particularly limited, and liquefied gas such as LPG and dimethyl ether, compressed gas such as carbon dioxide gas and nitrogen gas can be used, and the component (E) is one or two. It may contain more than species. Among them, the component (E) is preferably liquefied gas from the viewpoint of maintaining a stable discharge amount of the preparation.

本発明に用いられる前記(E)成分は、初期内圧が20℃で0.2〜0.5MPaの範囲がよい。液化ガスは組成を変えることにより任意の初期内圧に調整できる。 The component (E) used in the present invention preferably has an initial internal pressure in the range of 0.2 to 0.5 MPa at 20 ° C. The liquefied gas can be adjusted to any initial internal pressure by changing the composition.

前記(A)〜(D)成分を含有するエアゾール原液と前記(E)成分との重量比は、エアゾール原液:噴射剤=88:12〜97:3が好ましい。より好ましくは、エアゾール原液:噴射剤=90:10〜95:5の範囲である。前記(E)成分の重量比がエアゾール原液:噴射剤=97:3未満の場合、5℃条件下での発泡性を損なう恐れがある。また、前記(E)成分の重量比がエアゾール原液:噴射剤=88:12を超える場合、吐出物の嵩比重が小さいものになり、本来使用する目的の効果が得られない、すなわち適正な染毛性または明度を得ることが出来ない恐れがある。 As for the weight ratio of the aerosol undiluted | stock solution containing the said (A)-(D) component, and the said (E) component, aerosol undiluted | stock solution: propellant = 88:12-97: 3 are preferable. More preferably, it is the range of aerosol undiluted | stock solution: propellant = 90: 10-95: 5. If the weight ratio of the component (E) is less than 97: 3 for the aerosol stock solution: propellant, the foamability at 5 ° C. may be impaired. In addition, when the weight ratio of the component (E) exceeds aerosol stock solution: propellant = 88: 12, the bulk specific gravity of the discharge becomes small, and the intended effect to be originally used can not be obtained, that is, proper dyeing There is a possibility that hairiness or lightness can not be obtained.

本発明による酸化剤を含有する乳化型エアゾール組成物はpH4.5以下が好ましい。
pH4.5を超える場合、前記(A)成分を安定化することができず、容器内の内圧上昇をもたらし、内容物の吐出量が設定値より多くなり、適正な染毛性または明度を得ることが出来ない恐れがある。
The emulsified aerosol composition containing the oxidizing agent according to the present invention preferably has a pH of 4.5 or less.
When the pH is higher than 4.5, the component (A) can not be stabilized, resulting in an increase in internal pressure in the container, and the discharge amount of the content becomes larger than the set value to obtain appropriate hair dyeing properties or lightness. There is a fear that you can not do it.

本発明の酸化剤を含有する乳化型エアゾール組成物は、その他の化粧料等に通常用いられる原料を、本発明の効果を損なわない範囲内で適宜配合してもよい。油剤、溶剤、非イオン性界面活性剤、陰イオン性界面活性剤、陽イオン性界面活性剤、両性界面活性剤、保湿剤、水溶性高分子、抗酸化剤、紫外線吸収剤、キレート剤、防腐剤、抗菌剤、着色剤、香料、ビタミン類、植物抽出液等を用いることができ、これらは1種または2種以上を含有してもよい。 The emulsion-type aerosol composition containing the oxidizing agent of the present invention may be appropriately blended with other raw materials usually used for cosmetics and the like within the range in which the effects of the present invention are not impaired. Oils, solvents, nonionic surfactants, anionic surfactants, cationic surfactants, amphoteric surfactants, moisturizers, water soluble polymers, antioxidants, UV absorbers, chelating agents, preservatives An agent, an antibacterial agent, a coloring agent, a fragrance, vitamins, a plant extract and the like can be used, and these may contain one or more kinds.

以下に、実施例および比較例をあげて、本発明をより詳細に説明する。本発明はこれにより制限されるものではない。 Hereinafter, the present invention will be described in more detail by way of examples and comparative examples. The present invention is not limited thereby.

本明細書に示す評価試験において、酸化剤を含有する乳化型エアゾール組成物に含まれる成分およびその含有量を種々変更しながら実施した各種の実験結果を以下に示す。 In the evaluation test shown in the present specification, various experimental results carried out while variously changing the components contained in the emulsified aerosol composition containing an oxidizing agent and the content thereof are shown below.

本明細書に示す評価試験において、「(A)過酸化水素の安定性」、「毛髪の染毛性」、「毛髪の明度」および「5℃条件下での発泡性」について評価した。 In the evaluation test shown in this specification, it evaluated about "(A) stability of hydrogen peroxide", "hair dyeability", "brightness of hair", and "foamability under 5 degreeC conditions."

本明細書に示す評価試験において、「(A)過酸化水素の安定性」は得られた酸化剤を含有する乳化型エアゾール組成物を40℃条件下で3ヵ月間保存した後、(A)過酸化水素の残存率を測定した。(A)過酸化水素の定量方法は、酸化還元滴定法を用いた。 In the evaluation test shown in the present specification, “(A) Stability of hydrogen peroxide” is the result of storing the obtained emulsified aerosol composition containing an oxidizing agent at 40 ° C. for 3 months, (A) The residual rate of hydrogen peroxide was measured. (A) The determination method of hydrogen peroxide used the oxidation-reduction titration method.

本明細書に示す評価試験において、「毛髪の染毛性」および「毛髪の明度」は得られた酸化剤を含有する乳化型エアゾール組成物をポリエチレン製内袋付き金属製の密閉容器に充填し、40℃条件下で3ヵ月間保存した酸化剤を含有する乳化型エアゾール組成物と染毛試験当日に調製した酸化剤を含有する乳化型エアゾール組成物とを用いて同時に染毛し比較評価した。 In the evaluation test shown in the present specification, “hair dyeability” and “hairness of hair” are obtained by filling the obtained emulsion-containing aerosol composition containing an oxidizing agent into a metal closed container with a polyethylene inner bag. At the same time, using an emulsion-type aerosol composition containing an oxidizing agent stored for 3 months under 40 ° C. and an emulsion-type aerosol composition containing an oxidizing agent prepared on the day of the hair dyeing test .

「毛髪の染毛性」、「毛髪の明度」および評価で用いた「アルカリ剤を含有する脱色剤」および「アルカリ剤と酸化染料を含有する染毛剤」の成分および含有量は後述する。「アルカリ剤を含有する脱色剤」および「アルカリ剤と酸化染料を含有する染毛剤」と同量比で混合し、得られた染毛剤組成物を25℃条件下で、毛髪試験用ドール(株式会社ビューラックス社製「カットマネキンNO.775N」)の毛髪全体に120gを塗布し20分間放置後、洗い流す染毛操作を行ない、乾かした毛髪を目視で確認して評価した。 The components and contents of the "coloring property of hair", the "brightness of hair" and the "decoloring agent containing an alkali agent" and the "hair coloring agent containing an alkali agent and an oxidation dye" used in the evaluation will be described later. The hair dye composition for hair test is obtained by mixing the hair dye composition obtained under the conditions of 25 ° C. by mixing in the same proportions as “the decolorizing agent containing an alkaline agent” and the “hair containing an alkaline agent and an oxidation dye”. After applying 120 g to the entire hair of “Cut Mannequin No. 775 N” (Burelux Co., Ltd.) and leaving it for 20 minutes, a hair dyeing operation to wash off was performed, and the dried hair was visually confirmed and evaluated.

本明細書に示す評価試験において、「5℃条件下での発泡性」は得られた酸化剤を含有する乳化型エアゾール組成物を5℃条件下で24時間保存した後、取り出してすぐに手の上に吐出し、製剤の発泡性を目視にて評価した。 In the evaluation test shown in the present specification, “foamability under 5 ° C. conditions” means that the obtained emulsified aerosol composition containing an oxidizing agent is stored under 5 ° C. conditions for 24 hours and then taken out immediately after removal. And the foamability of the preparation was evaluated visually.

「過酸化水素の残存率」の評価基準
40℃条件下で3ヵ月間保存での過酸化水素の残存率
◎:99%以上
○:96%以上99%未満
△:94%以上96%未満
×:94%未満
Evaluation criteria of "Percentage of residual hydrogen peroxide" Residual ratio of hydrogen peroxide after storage for 3 months under 40 ° C condition ◎: 99% or more ○: 96% or more and less than 99% Δ: 94% or more and less than 96% × Less than 94%

「毛髪の染毛性」または「毛髪の明度」の評価基準
◎:染毛性または明度に全く変化なし。
○:染毛性または明度に変化があるが問題ない程度。
△:染毛性または明度に変化がある。
×:染毛性または明度に明らかに異なる変化がある。
Evaluation criteria of "hair dyeability" or "hair lightness" :: no change in dyeability or lightness.
:: A degree of change in hair dyeability or lightness but no problem.
Δ: change in hair dyeability or lightness
X: There are distinctly different changes in hair dyeability or lightness.

「5℃条件下での発泡性」の評価基準
◎:泡を形成する。
○:泡を形成し、しばらく泡を保つ。
△:泡を形成するが、すぐに崩れる。
×:泡を形成しない。
Evaluation criteria of "foamability under 5 ° C. conditions" :: foam is formed.
○: Form bubbles and keep bubbles for a while.
Δ: Foam is formed but collapses immediately.
X: Does not form a bubble.

調製方法
(B)成分、その他の油性成分、活性剤等および精製水を80℃以上にて混合乳化する。乳化後、冷却し、35℃の時点で、(A)成分、(C)成分および(D)成分を混合し、エアゾール原液を得る。前記エアゾール原液を、(E)成分と混合し、酸化剤を含有する乳化型エアゾール組成物を得る。
Preparation method (B) Component, other oil component, activator, etc. and purified water are mixed and emulsified at 80 ° C. or higher. After emulsification, the mixture is cooled, and at 35 ° C., components (A), (C) and (D) are mixed to obtain an aerosol stock solution. The aerosol stock solution is mixed with the component (E) to obtain an emulsified aerosol composition containing an oxidizing agent.

表1はアルカリ剤と酸化染料を含有する染毛剤第1剤の成分と含有量を示す。この染毛剤第1剤と得られた酸化剤を含有する乳化型エアゾール組成物を「染毛剤第1剤:酸化剤を含有する乳化型エアゾール組成物(第2剤)=1:1」の混合比で混合し、これを用いて「毛髪の染毛性」を評価した。 Table 1 shows the components and contents of the first hair dye containing an alkaline agent and an oxidation dye. The emulsion-type aerosol composition containing the hair dye first agent and the obtained oxidizing agent was prepared as follows: "hair dye first agent: emulsion-type aerosol composition (second agent) = 1: 1 containing an oxidant" The mixture was mixed at a mixing ratio of 1, and the "hair-dyeing property" was evaluated using this.

Figure 0006503166
Figure 0006503166

表2はアルカリ剤を含有する脱色剤第1剤の成分と含有量を示す。この脱色剤第1剤と得られた酸化剤を含有する乳化型エアゾール組成物を「脱色剤第1剤:酸化剤を含有する乳化型エアゾール組成物(第2剤)=1:1」の混合比で混合し、これを用いて「毛髪の明度」を評価した。 Table 2 shows the components and contents of the first decoloring agent containing an alkaline agent. The emulsified aerosol composition containing the first decolorizing agent and the obtained oxidizing agent is mixed with "decoloring agent first agent: emulsified aerosol composition containing oxidizing agent (second agent) = 1: 1". The ratio was mixed and this was used to evaluate the "brightness of hair".

Figure 0006503166
Figure 0006503166

Figure 0006503166
Figure 0006503166

Figure 0006503166
Figure 0006503166

比較例1は非イオン界面活性剤を含有せず評価した。また、比較例2〜5は、界面活性剤の種類を変えて評価した。 Comparative Example 1 was evaluated without containing a nonionic surfactant. Moreover, Comparative Examples 2 to 5 were evaluated by changing the type of surfactant.

比較例1、2は毛髪の染毛性または明度に変化が見られた。さらに、5℃条件下での良好な発泡性は得られなかった。また、比較例3、5は、過酸化水素の残存率が良好ではなく、毛髪の染毛性または明度に変化が見られた。さらに、5℃条件下での良好な発泡性は得られなかった。比較例4は、過酸化水素の残存率が良好ではなく、毛髪の染毛性または明度に変化が見られた。 In Comparative Examples 1 and 2, changes were observed in the hair dyeability or lightness of the hair. Furthermore, good foamability under 5 ° C. conditions was not obtained. In addition, in Comparative Examples 3 and 5, the residual ratio of hydrogen peroxide was not good, and a change in hair dyeability or lightness was observed. Furthermore, good foamability under 5 ° C. conditions was not obtained. In Comparative Example 4, the residual rate of hydrogen peroxide was not good, and a change in hair dyeability or lightness was observed.

実施例1〜15は全て良好であった。(B)成分が3.0重量%より多くなると、毛髪の染毛性または明度に変化が見られる恐れがある。1.0重量より少なくなると5℃条件下での発泡性が悪くなる恐れがある。 Examples 1-15 were all good. When the amount of the component (B) is more than 3.0% by weight, a change in hair dyeability or lightness may be observed. If it is less than 1.0 weight, the foamability at 5 ° C. may be deteriorated.

Figure 0006503166
Figure 0006503166

比較例6は、(C)成分を含有せずアルカリ土類金属の水酸化物である水酸化カルシウムを含有した酸化剤を含有する乳化型エアゾール組成物について評価した。この結果、(A)成分の残存率が良好ではなかった。 The comparative example 6 evaluated about the emulsion type aerosol composition which does not contain (C) component but contains the oxidizing agent containing calcium hydroxide which is a hydroxide of alkaline-earth metal. As a result, the remaining rate of the component (A) was not good.

また、比較例7は(D)成分を含有せず、従来技術であるクエン酸をpH調整剤として用いて評価し、比較例8は(C)成分を含有せず、従来技術からあるクエン酸ナトリウムをpH調整剤として用いて評価した。この結果、(A)成分の残存率は良好ではなかった。 Moreover, Comparative Example 7 does not contain the component (D) and is evaluated using citric acid which is the prior art as a pH adjuster, and Comparative Example 8 does not contain the component (C) and citric acid which is different from the prior art It evaluated using sodium as a pH adjuster. As a result, the remaining rate of the component (A) was not good.

比較例9は、従来技術である(A)成分の安定化剤であるスズ酸ナトリウムを含有し、さらに、比較例10ではクエン酸およびクエン酸ナトリウムを用いて実施例1と同じpHに調整して評価した。この結果、(A)成分の残存率は良好ではなかった。 Comparative Example 9 contains sodium stannate which is a stabilizer of the component (A), which is the prior art, and in Comparative Example 10, the same pH as Example 1 is adjusted using citric acid and sodium citrate. It evaluated. As a result, the remaining rate of the component (A) was not good.

実施例16〜20の結果から、(C)成分の種類を変えたとしても良好であった。また、実施例16および17の結果から、(C)成分は、水酸化ナトリウム、水酸化カリウムが良好であり、特に水酸化カリウムは良好であった。 From the results of Examples 16 to 20, it was good even if the type of the component (C) was changed. From the results of Examples 16 and 17, the component (C) was good for sodium hydroxide and potassium hydroxide, and particularly good for potassium hydroxide.

Figure 0006503166
Figure 0006503166

Figure 0006503166
Figure 0006503166

実施例21〜31は全て良好であった。(C)成分は、酸化剤を含有する乳化型エアゾール組成物中に含有されていればよいが、好ましくは0.004〜1重量%、より好ましくは0.02〜0.5重量%が良好であった。さらに(D)成分は酸化剤を含有する乳化型エアゾール組成物中に含有されていれば良いが、好ましくは0.01〜2重量%、より好ましくは0.05〜1重量%が良好であった。また、酸化剤を含有する乳化型エアゾール組成物のpHは4.5以下が良く、特に3.5以下が良好であった。 Examples 21 to 31 were all good. The component (C) may be contained in an emulsion type aerosol composition containing an oxidizing agent, but preferably 0.004 to 1% by weight, more preferably 0.02 to 0.5% by weight. Met. Furthermore, the component (D) may be contained in the emulsified aerosol composition containing an oxidizing agent, but preferably 0.01 to 2% by weight, more preferably 0.05 to 1% by weight. The In addition, the pH of the emulsion type aerosol composition containing an oxidizing agent is preferably 4.5 or less, and particularly preferably 3.5 or less.

比較例11は、酸化剤を含有する乳化型エアゾール組成物のpHを7.0として評価した。その結果、過酸化水素の残存率が良好ではなく、毛髪の染毛性または明度に変化が見られた。 The comparative example 11 evaluated the pH of the emulsion type aerosol composition containing an oxidizing agent as 7.0. As a result, the residual ratio of hydrogen peroxide was not good, and a change in hair dyeability or lightness was observed.

Figure 0006503166
Figure 0006503166

実施例32〜36は全て良好であった。特にエアゾール原液:噴射剤=90:10〜95:5が良好であった。 Examples 32-36 were all good. In particular, the aerosol stock solution: propellant = 90: 10 to 95: 5 was good.

本発明は、染毛剤で用いられる酸化剤を含有する乳化型エアゾール組成物に関するものである。さらに詳しくは低温時にも発泡性が失わず、なおかつ高温条件下で長時間保存されても安定な酸化剤を含有する乳化型エアゾール組成物を提供できる。 The present invention relates to an emulsified aerosol composition containing an oxidizing agent used in a hair dye. More specifically, it is possible to provide an emulsified aerosol composition containing an oxidizing agent which does not lose foaming even at low temperatures and which is stable even when stored for a long time under high temperature conditions.

Claims (1)

アルカリ剤を含有する第1剤と混合して使用され、酸化剤を含有する乳化型エアゾール組成物であって、(A)過酸化水素、(B)POEラウリルエーテルおよびPOEアルキル(12〜14)エーテルから選ばれる1種または2種以上、(C)水酸化カリウム、(D)1−ヒドロキシエタン−1、1−ジホスホン酸を含有し、前記(B)成分のポリオキシエチレン基の平均付加モル数が2〜15の範囲であり、前記(B)成分の含有量が1.5〜2.5重量%であり、前記(C)成分の含有量が0.02〜1重量%であり、前記(D)成分の含有量が0.05〜1重量%であるエアゾール原液と、(E)噴射剤を含有し、エアゾール原液がpH4.5以下であり、前記エアゾール原液と(E)噴射剤を、エアゾール原液:噴射剤=90:10〜95:5(重量比)の比率で含有することを特徴とする酸化剤を含有する乳化型エアゾール組成物。 An emulsion type aerosol composition containing an oxidizing agent, which is used in combination with a first agent containing an alkaline agent, which is (A) hydrogen peroxide, (B) POE lauryl ether and POE alkyl (12 to 14) 1 or 2 types selected from ethers, (C) potassium hydroxide , (D) 1-hydroxyethane-1, 1-diphosphonic acid, and the average addition mole of the polyoxyethylene group of the component (B) The number is in the range of 2 to 15, the content of the component (B) is 1.5 to 2.5% by weight, and the content of the component (C) is 0.02 to 1% by weight, The aerosol undiluted | stock solution whose content of the said (D) component is 0.05 to 1 weight%, and (E) propellant are included, aerosol undiluted | stock solution is pH 4.5 or less, and the said aerosol undiluted | stock solution and (E) propellant The aerosol stock solution: propellant = 90: 1 95: 5-emulsifying aerosol composition containing an oxidizing agent characterized in that it contains a ratio (by weight).
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