JP4703090B2 - Hair treatment composition and method for producing the same - Google Patents

Description

【００３８】
＜実施例１〜３、比較例１〜３＞
実施例１ないし３および比較例１ないし３の第１剤および第２剤の組成と、評価基準１による臭気についての評価と、評価基準３による髪の傷みについての評価とを、図６に示した。図６において、各成分は、図１に示した工程に従って、毛髪染毛剤組成物第１剤および第２剤の試料として調製された。
【００３９】
なお、実施例中、「非イオン系可溶化剤」とあるのは、日光ケミカルズ株式会社製「ＢＣシリーズ」として購入可能なポリオキシエチレンセチルエーテルを用いた。代替品としては、同社「ＢＳシリーズ」のポリオキシエチレンステアリルエーテルや、日本エマルジョン株式会社、「ＥＭＡＬＥＸ ６００シリーズ」などがある。また、「加水分解シルク液」としては、成和化成株式会社製「Ｐｒｏｍｏｉｓ ＳＩＬＫ−１０００」を用いた。更に、香料としては、天然精油として、オレンジ、レモン、ベルガモット、マンダリンからそれぞれ抽出した成分を、２：１：１：２の割合で混合したものを用いた。これらのうち、非イオン系可溶化剤については、後述する実施例４、５、比較例４ないし６でも同様である。また、加水分解シルク液と香料については、全実施例および全比較例においても、同じものを用いた。
【００４０】
ついで、第１剤および第２剤をそれぞれ重量比１：２の割合で混合した。図６中（混合）とあるのは、この混合状態を示す。混合したものを、長さ２０ｃｍ、重量１５ｇの未処理毛に塗布し、３０分放置、次いで水洗後、ドライヤーにて乾燥した。評価基準３の引っ張り強度は、この状態で測定した。
【００４１】
図に示したように、実施例１ないし３では、パネラは、第１剤、第２剤、および両剤を混合した場合でも、全く臭気を感じることがなかった。また、実施例の組成物で処理を受けた毛髪の引張り強度は、いずれも３３キログラム以上あり、ダメージは小さかった。これに対して比較例では、いずれも第１剤および両剤を混合した場合には、僅かに刺激臭があるか（比較例１）あるいは強い臭気が感じられた。また、引張り強度は、３０キログラム以下となった。
【００４２】
＜実施例４，５、比較例４〜６＞
実施例４，５および比較例４ないし６の第１剤および第２剤の組成と、評価基準１による臭気についての評価と、評価基準３による髪の傷みについての評価とを、図７に示した。図７において、各成分は、図１に示した工程に従って、毛髪脱色剤組成物第１剤および第２剤の試料として調製された。
【００４３】
ついで、第１剤および第２剤をそれぞれ重量比１：２の割合で混合した。図７中（混合）とあるのは、この混合状態を示す。混合したものを、長さ２０ｃｍ、重量１５ｇの未処理毛に塗布し、３０分放置、次いで水洗後、ドライヤーにて乾燥した。評価基準３の引っ張り強度は、この状態で測定した。
【００４４】
図に示したように、実施例４，５では、パネラは、第１剤、第２剤、および両剤を混合した場合でも、全く臭気を感じることがなかった。また、実施例の組成物で処理を受けた毛髪の引張り強度は、いずれも３４キログラム以上あり、ダメージは小さかった。これに対して比較例では、いずれも第１剤および両剤を混合した場合には、強い臭気が感じられた。また、引張り強度は、２９キログラム以下となった。
【００４５】
＜実施例６〜８、比較例７〜９＞
実施例６ないし８および比較例７ないし９の第１剤および第２剤の組成と、評価基準１による臭気についての評価と、評価基準３による髪の傷みについての評価とを、図８に示した。図８において、各成分は、図１に示した工程に従って、パーマネントウェーブ用組成物第１剤および第２剤の試料として調製された。
【００４６】
なお、実施例６ないし８、および比較例７ないし９で用いた非イオン系可溶化剤は、日光ケミカルズ株式会社製、「ＣＯ（またはＨＣＯ）シリーズ」として購入可能なポリオキシエチレンヒマシ油（または硬化ヒマシ油）を用いた。代替品としては、同社製「ＰＢＣ（またはＰＥＮ）シリーズ」のポリオキシエチレンポリオキシプロピレンアルキルエーテルなどがある。
【００４７】
ついで、長さ２０ｃｍ、重量１５ｇの未処理毛を直径１３ｍｍのロッドに巻き、図８に示したパーマネントウェーブ用第１剤に１０分浸積、次いで水洗後、前記パーマネントウェーブ用第２剤に１０分間浸積、水洗し、ドライヤーにて乾燥した。評価基準３の引っ張り強度は、この状態で測定した。
【００４８】
図に示したように、実施例６ないし８では、パネラは、第１剤、第２剤、および使用中、使用後においても、全く臭気を感じることがなかった。また、実施例の組成物で処理を受けた毛髪の引張り強度は、いずれも３４キログラム以上あり、ダメージは小さかった。これに対して比較例では、いずれも第１剤単独および使用中、使用後において、強い臭気が感じられた。また、引張り強度は、２５キログラム以下となった。
【００４９】
次に、上述した実施例１ないし８について、評価基準２により臭気を評価した結果を図９に示す。なお、図中、第１実施例と第６実施例を除いて、第２剤の表示がないが、第２実施例ないし第５実施例については、第２剤は、第１実施例と同一であり、第７，第８実施例については、第６実施例と同一なので、それぞれ結果の表示を省略した。また、上述した比較例１ないし９についても、同様に測定した結果を、図１０に示した。
【００５０】
実施例１ないし８については、図９に示したように、アンモニア、アミン類、硫化水素、メルカプタンのいずれについても、ほとんど検出されないか、あるいは極めて微量であり、これらの成分に基づく不快臭は、ほとんど存在しないことが分かる。他方、図１０に示した比較例では、アンモニアが３０ｐｐｍ以上（使用した検知管の検知上の上限を越える量）アミン類が１００ｐｐｍ以上（使用した検知管の検知上の上限を越える量）、メルカプタンが比較例１の混合したものと比較例８の第１剤を除いて、４ｐｐｍ以上検出されており、使用者はかなり強い不快臭を感じることが分かる。
【００５１】
【発明の効果】
以上詳述したように本発明の毛髪処理剤組成物によれば、組成物自体に不快な臭いがない。従って、使用者は不快臭に悩まされることなく、各種の毛髪処理剤組成物を使用することができる。また、本発明の毛髪処理剤組成物の製造方法によれば、簡易な工程で、使用時の不快臭がない毛髪処理剤組成物を得ることができる。
【図面の簡単な説明】
【図１】 本発明の実施の形態としての毛髪処理剤組成物を製造する工程を示す工程図である。
【図２】 代表的な検知管の外観を示す説明図である。
【図３】 実施の形態における評価基準２の手法での臭気の測定手法を示す説明図である。
【図４】 実施例の毛髪処理剤組成物を構成する各剤について、アンモニア、アミン類、硫化水素、メルカプタンの４種類について、その含有量を測定した結果を示す説明図である。
【図５】 実施例の毛髪処理剤組成物を構成するその他の剤について、アンモニア、アミン類、硫化水素、メルカプタンの４種類について、その含有量を測定した結果を示す説明図である。
【図６】 実施例１ないし３および比較例１ないし３についての評価基準１および３による結果を示す説明図である。
【図７】 実施例４，５および比較例４ないし６についての評価基準１および３による結果を示す説明図である。
【図８】 実施例６ないし８および比較例７ないし９についての評価基準１および３による結果を示す説明図である。
【図９】 実施例１ないし８について、評価基準２による結果を示す説明図である。
【図１０】 比較例１ないし９について、評価基準２による結果を示す説明図である。
【符号の説明】
１００…デシケータ
１０５…ねじ口
１１０…シャーレ
１２０…検知管式気体測定器
１３０…ハンドル
１５０…検知管[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a hair treatment composition, and more particularly to a hair treatment composition comprising a plurality of agents constituting the hair treatment agent and a method for producing the same.
[0002]
[Prior art]
Cosmetic compositions used for the treatment of human keratinous materials such as hair, body hair or skin are generally known to contain at least one alkaline agent for bringing the pH of the composition to a value of 5-13. ing. In the case of a composition having a basic pH, the role of the alkaline agent varies depending on the type of the composition. In the case of a composition using aqueous hydrogen peroxide as the oxidizing agent, it is necessary to have a basic pH in order to decompose the aqueous hydrogen peroxide. In general, in the case of a composition for treating hair, it is possible to expand the hair cuticle by making the pH basic, thereby facilitating the treatment agent to enter the hair. These two effects are that if the composition is a hair removal agent, a hair dyeing or bleaching composition, a skin dyeing or bleaching composition or a permanent wave or straightening hair composition for straightening, It occurs individually or simultaneously in many applications of cosmetic compositions.
[0003]
[Problems to be solved by the invention]
Alkaline agents commonly used in hair treatment compositions in the current art, such as hair dyes, hair bleaching agents and permanent wave compositions, are aqueous ammonia or ammonium carbonates such as ammonium carbonate and ammonium bicarbonate. It has a pungent odor like salt. For this reason, there was a problem that the user of this type of hair treatment composition may feel uncomfortable in use. For example, aqueous ammonia has a strong pungent odor that makes it difficult to breathe. This is particularly annoying for users of permanent wave, dyeing or bleaching compositions. Furthermore, ammonium salts such as ammonium carbonate also have an irritating odor, although not as much as ammonia. Further, these ammonium salts often require a considerable amount in order to achieve a relatively high basic pH, and as a result, the irritating odor as a composition cannot be reduced.
[0004]
Also in the base, what is currently generally used has emitted some base odor. There was also a base with high irritation to the skin. Conventionally, it has been considered that such irritating odors are unavoidable for hair treatment compositions, and measures such as mitigating irritation have been taken by adding fragrant ingredients and flavoring agents. It wasn't too much. An object of the present invention is to fundamentally solve problems such as an irritating odor in such a hair treatment composition.
[0005]
[Means for solving the problems and their functions and effects]
As a result of intensive research, the present inventor has found that in a hair treatment composition comprising a plurality of agents constituting the hair treatment agent, each of the plurality of agents has a proportion of a predetermined component that stimulates olfaction in terms of odor. It was found that an odorless hair treatment composition with little damage to the hair could be obtained by setting it below the detection limit, and the present invention was completed.
[0006]
  That is, the hair treatment composition of the present invention is
1st and 2ndMade of medicineUsed for hair dyeingA hair treatment composition comprising:
  AboveThe first agent is, (A) alkaline agent, (B) base, (C) including reducing agentThe second agent includes (B) a base,
  The (A) alkali agent is monoethanolamine,The alkali agent (A) in the first agentThe blending amount is 1 to 10% by weight,
  The base (B) is at least one dyeing compound selected from the group consisting of an oxidative dye intermediate, a coupler and a direct dye as an active agent;An oxidizing agent that acts on the staining compound, the first agent includes at least the staining compound, and the second agent includes at least the oxidizing agent,
  (C) the reducing agent is sodium sulfite and / or ascorbic acid,(C) the reducing agent in the first agentThe blending amount is 0.1 to 5% by weight,
  Above1st and 2ndNone of the agents contain a fragrant ingredient and a flavoring agent,
  Above1st and 2ndWhen 1 gram of each agent is left alone in a 3 liter desiccator for 3 hours and then a predetermined component that stimulates olfaction is detected using a detector tube,
    ammonia:1ppm or less,
    Amines:0.5ppm or less,
    Hydrogen sulfide: 0.05 ppm or less,
    Mercaptans: 0.05ppm or less
And
  In useThe first and second agents areWhen 1 gram of the mixed agent is left in a 3 liter desiccator for 3 hours and then a predetermined component that stimulates olfaction is detected using a detector tube,
    Ammonia: 1 ppm or less,
    Amines: 0.75 ppm or less,
    Hydrogen sulfide: 0.05 ppm or less,
    Mercaptan: 0.05 ppm or less
And
  The gist is that it is used for dyeing hair. For this reason, the hair treatment composition of the present invention does not have an unpleasant smell even when used, and can be used comfortably.
[0007]
  In addition, the method for producing the hair treatment composition of the present invention comprises:
  1st and 2ndConsisting ofFor hair dyeingA method for producing a hair treatment composition comprising:
  (A)Prepare monoethanolamine as an alkaline agent,
  (B)As a base, as an active agent, at least one dyeing compound selected from the group consisting of an oxidative dye intermediate, a coupler and a direct dye;Preparing an oxidizing agent that acts on the staining compound;
  (C)Prepare sodium sulfite and / or ascorbic acid as a reducing agent,
  AboveFirstThe agent includes (A) the alkali agent, (B) base, and (C) the reducing agent.And (B) at least the staining compound as a base,
The former second agent (B) contains at least the oxidizing agent as a base,
Said first agent1 to 10% by weight of monoethanolamine in the above,First agentThe amount of sodium sulfite and / or ascorbic acid is adjusted to 0.1 to 5% by weight in
Above1st and 2ndIn any of these agents, no fragrance ingredients and flavoring agents are blended,
  Above1st and 2ndWhen 1 gram of each agent is left alone in a 3 liter desiccator for 3 hours and then a predetermined component that stimulates olfaction is detected using a detector tube,
    ammonia:1ppm or less,
    Amines:0.5ppm or less,
    Hydrogen sulfide: 0.05 ppm or less,
    Mercaptans: 0.05ppm or less
Make sure
By storing the prepared first and second agents in a predetermined container so as to be used for hair dyeing,
  In useThe first and second agentsmixtureShiWhen 1 gram of the agent in a fresh state is left in a 3 liter desiccator for 3 hours and a predetermined component that stimulates olfaction is detected using a detector tube,
    Ammonia: 1 ppm or less,
    Amines: 0.75 ppm or less,
    Hydrogen sulfide: 0.05 ppm or less,
    Mercaptan: 0.05 ppm or less
To be
  Is the gist.
[0008]
According to the method for producing a hair treatment composition of the present invention, it is possible to produce a hair treatment composition that does not give an unpleasant odor perception to the user in a simple process.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the hair treatment composition of the present invention will be described in detail. When practicing the hair treatment composition of the present invention, each of the plurality of agents is prepared such that the ratio of the predetermined component that stimulates olfaction is not more than the perception limit on olfaction. At this time, a component having a fragrance and a flavoring agent may not be added to any of the plurality of agents. The flavoring agent is intended to impart some fragrance to the composition, and can include fragrances such as natural fragrances and synthetic fragrances. In addition, the predetermined component that stimulates olfaction includes at least ammonia, amines, hydrogen sulfide, and mercaptan. This is because these components make the user sense an unpleasant smell. Moreover, as a some agent, (A) Alkaline agent, (BGroupAn agent, (C) a reducing agent, etc. can be considered. It is more preferable that these plural agents do not emit an unpleasant odor that stimulates olfaction by mixing (A) an alkali agent, (B) base, and (C) a reducing agent during use.
[0010]
Among the plurality of agents, as the alkaline agent of component (A), monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, 2-amino-2-methyl-1-propanol and 2-amino-2-methyl- Examples thereof include organic amines such as 1,3-propanediol, basic amino acids such as arginine, and inorganic alkalizing agents such as sodium carbonate and sodium hydroxide. Of these, monoethanolamine is particularly preferable.
[0011]
The alkali agent of component (A) can be used alone or in combination of two or more, and the blending amount is preferably 0.5 to 20% by weight, particularly preferably 1 to 15% by weight in the total composition. is there. This is because if the amount is too small, the effect of swelling the hair is inferior, and if it is too large, the action of the reducing agent and the oxidizing agent is hindered, and hair damage and skin irritation increase.
[0012]
Among these agents, (B) base includes oil agent, activator, thickener,Agent, hairAll the bases which can be generally used at present, such as a hair protecting agent, a plant extract and a stabilizing agent, can be mentioned. Among these, specific examples of agents satisfying the above conditions will be described in detail in the following “Examples”, but conversely, those having a low degree of purification and having some base odor are excluded. For example, oleyl alcohol, oleic acid and oil agents, activators and the like synthesized therefrom are bases having a specific odor and are not used as the base of the present invention.
[0013]
The base of the component (B) is not particularly limited, and is preferably a highly purified and carefully selected material, and particularly preferably deodorized and purified.
[0014]
(B) As a base, it can be used alone or in combination depending on the intended use and dosage form of the composition, and the blending amount thereof can be added within a range not impairing the effect of the composition. There is no particular limitation.
[0015]
Component (C) reducing agents include cysteine or derivatives thereof, mercaptocarboxylic acids such as thiomalic acid, mercapto alcohols such as thioglycerol, mercaptocarboxylic esters such as glycerol monothioglycolate, cysteamine, cysteine amide, etc. Examples thereof include mercapto compounds, sulfites such as sulfurous acid and sodium sulfite, bisulfites such as sodium hydrogensulfite, ascorbic acid and derivatives thereof.
[0016]
As the reducing agent of component (C), sulfite, bisulfite, ascorbic acid or a derivative thereof is particularly preferable.
[0017]
A reducing agent can be used 1 type or in combination of 2 or more types, As for the compounding quantity, 0.1-20 weight% is preferable in the whole composition, Most preferably, it is 0.5-15 weight%. This is because if the amount is too small, the stability of the composition and the treatment effect on the hair will be inferior, and if it is too large, damage to the hair and irritation to the skin will increase.
[0018]
The hair treatment composition of the present invention may contain an active agent. Examples of the active agent used in the hair treatment composition include oxidative dye intermediates, couplers, and dye compounds selected from the group consisting of direct dyes.
[0019]
Examples of the oxidative dye intermediate that is an active agent include phenylenediamines, aminophenols, diaminopyridines, and salts thereof. Among these, p-phenylenediamine, p-toluylenediamine, N, N-bis (2-hydroxyethyl) -p-phenylenediamine, 2- (2′-hydroxyethyl) -p-phenylenediamine, N-phenyl- p-phenylenediamine, 4,4′-diaminodiphenylamine, 2-chloro-p-phenylenediamine, N, N-dimethyl-p-phenylenediamine, p-aminophenol, o-aminophenol, p-methylaminophenol, 2 , 6-Dichloro-p-phenylenediamine, p-aminophenylsulfamic acid, 2,5-diaminopyridine and salts thereof are preferred from the viewpoint of effect and hair dyeing power.
[0020]
The oxidation dye intermediate can be used singly or in combination of two or more, and the blending amount is preferably 0.01 to 15% by weight, particularly preferably 0.1 to 10% by weight.
[0021]
Couplers that are active agents include resorcin, pyrogallol, catechol, m-aminophenol, m-phenylenediamine, 2,4-diaminophenol, 1,2,4-benzenetriol, toluene-3,4-diamine, toluene- 2,4-diamine, hydroquinone, α-naphthol, 2,6-diaminopyridine, 3,3′-iminodiphenol, 1,5-dihydroxynaphthalene, 5-amino-o-cresol, diphenylamine, p-methylaminophenol Phloroglucin, 2,4-diaminophenoxyethanol, tannic acid, gallic acid, ethyl gallate, methyl gallate, propyl gallate, pentaploid, 1-methoxy-2-amino-4- (2-hydroxyethyl) aminobenzene, 5 -(2-hydroxyamino) -2-me Le phenols and their salts and the like, other "quasi-drug material Standard" (issued June 1991, Yakujinipposha) as appropriate those listed in, can be used.
[0022]
Couplers can be used alone or in combination of two or more, and the blending amount is preferably 0.01 to 10% by weight, particularly preferably 0.1 to 5% by weight.
[0023]
Examples of direct dyes that are active agents include known dyes such as nitro dyes, basic dyes, tar dyes, and natural dyes. Among these, nitro dyes, azo dyes, nitroso dyes, triphenylmethane dyes, xanthene dyes, quinoline dyes, anthraquinone dyes or indigo dyes are preferable from the viewpoint of stability and effect.
[0024]
Direct dyes can be used singly or in combination of two or more, and the blending amount is preferably 0.001 to 15% by weight, particularly preferably 0.01 to 10% by weight.
[0025]
Next, an embodiment of a method for producing a hair treatment composition will be described. In the production method of the present invention, for each of the plurality of agents, the ratio of the predetermined component that stimulates olfaction selects an agent that is not more than the perception limit on olfaction, but at this time, the selection is as a predetermined component that stimulates olfaction, Any of ammonia, amines, hydrogen sulfide, and mercaptans may be performed under the condition that it is below the odor perception limit. Moreover, although a some agent is prepared and this is accommodated in a predetermined container, this process can be performed as follows. That is, in the preparation of the drug, a plurality of agents are classified into an oil phase that is an oil-soluble component, an aqueous phase that is a water-soluble component, and an additive phase that is an unstable component at a high temperature, and a step of weighing. A step of heating and dissolving the components of the oil phase and the aqueous phase, a step of adding and emulsifying the aqueous phase that has reached a predetermined temperature, respectively, and cooling the emulsified mixture to a predetermined temperature or less. And the step of adding the components of the additive phase to the emulsified mixture at a low temperature.
[0026]
【Example】
Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited thereto. In addition, a compounding quantity shows weight%. First, the manufacturing method of the hair-treatment agent composition in an Example is demonstrated. FIG. 1 is a process diagram showing a production process of a hair treatment composition in Examples. As shown, the compositions of the examples are
Step S10: A hair treatment composition is manufactured from three types of agents (A) alkaline agent, (B) base, and (C) reducing agent. A step of selecting an agent whose ratio is below the odor perception limit,
Step S20: (A) (B) (C) each agent is classified into an oil phase that is an oil-soluble component, an aqueous phase that is a water-soluble component, and an additive phase that is an unstable component at high temperatures, Weighing,
Step S30: a step of heating and dissolving the components of the oil phase and the water phase,
Step S40: A step of adding an aqueous phase that has become a predetermined temperature or more to the oil phase and emulsifying and mixing,
Step S50: a step of cooling the emulsified mixture below a predetermined temperature and then adding the components of the additive phase to the emulsified mixture at a low temperature.
Step S60: A step of storing the emulsified mixture to which the components of the additive phase are added in a predetermined container.
It is manufactured by a manufacturing process consisting of
[0027]
Examples of the hair treatment composition obtained in such a process include hair coloring agents, hair bleaching agents, and permanent agents. Of the above production steps, each step except step S10 is a known one, so the description thereof will be omitted, and step S10, that is, three types of agents (A) alkaline agent, (B) base, and (C) reducing agent will be omitted. Will be described in more detail with respect to the step of selecting an agent in which the ratio of the predetermined component that stimulates olfaction is not more than the perception limit on olfaction. As predetermined components for stimulating the sense of smell contained in each of these agents, four types of ammonia, amines, hydrogen sulfide, and mercaptans are taken up. These components are representative as odor components that can be contained in the hair treatment composition, particularly as odor components that cause discomfort to the user. Since these components give the user unpleasant feeling even when the content ratio is on the order of ppm, a detection tube was used for the detection.
[0028]
The detector tube contains a substance that reacts only with a specific component and changes its hue, and its typical form is shown in FIG. The detection tube 150 has a detectable substance and a concentration range for each tube type. For example, in the detector tube made by Gastec Co., Ltd., detector tube / ammonia 3L, the measurement range is 0.5 to 78 ppm, the detection limit is 0.2 ppm, and the color change is pink to yellow. The detection tube 150 also has a suction time for sucking the gas. For example, in the case of ammonia 3L, the number of suctions is two (100 milliliters), and the time from suction to detection is 60 seconds. . The detector tube can specify the concentration of the substance by reading the area where the color has changed after the elapse of this time.
[0029]
In order to capture the measurement object into the detection tube 150, as shown in FIG.
(1) Take 1 gram of a measurement object as a sample SMP in a petri dish 110 with a diameter of 30 mm and a depth of 15 mm, and arrange the surface as flat as possible.
(2) Place the petri dish 110 in a glass screw port desiccator 100 with a capacity of 3 liters, seal it,
(3) After being left in this state for 3 hours and the objects to be detected are uniformly dispersed in the desiccator 100, the detector tube type gas measuring device 120 is connected to the desiccator screw port 105, and the handle 130 is operated to measure the measurement gas. Aspirate,
This method is used.
[0030]
In step S10, for each agent, ammonia, amines, hydrogen sulfide andBimeSelection is made by measuring the concentration of lucaptan using a dedicated detector tube. The odor to be measured and the detector tube type are as follows.
・ Ammonia: 3L ammonia detector tube manufactured by Gastec
Measurement range, 0.5-78ppm
Detection limit, 0.2ppm
Number of aspirations 2 times, aspiration volume 100 ml / time
Suction time 60 seconds
・ Amines: 180L amine detector tube manufactured by Gastec
Measuring range, 0.5-10ppm
Detection limit, 0.1ppm
Number of aspirations 1 time, aspiration volume 100 ml / time
Suction time 60 seconds
-Hydrogen sulfide: 4LT hydrogen sulfide detector tube manufactured by Gastec
Measurement range, 0.1-4ppm
Detection limit, 0.05ppm
Number of aspirations 2 times, aspiration volume 100 ml / time
Suction time 60 seconds
・ MeLUCAPTAN: 70L mercaptans detector tube manufactured by GASTECH
Measurement range, 0.1-8.0ppm
Detection limit, 0.05ppm
Number of aspirations 4 times, aspiration volume 100 ml / time
Suction time 90 seconds
Under such conditions, the odor concentration of each agent to be measured was measured in ppm. In addition, about amines, the Gastec company make and 180 amine detector tube (measurement range, 5-100 ppm) were used as needed. This detector tube has the same measurement conditions as the 180L amine detector tube manufactured by the same company.
[0031]
FIG. 4 and FIG. 5 explain the results of testing the contents of each of these agents, using ammonia, amines, hydrogen sulfide, and mercaptan among the components that stimulate olfaction using a detection tube. FIG. Except for “50% ammonium thioglycolate solution” and “reagent special grade 25% aqueous ammonia”, the concentrations of the agents shown in the figure are all below the odor detection limit for ammonia, amines, hydrogen sulfide, and mercaptans. It was. Therefore, at least these two agents are not selected for each of the agents (A), (B), and (C). In the leftmost column in the figure, each component corresponds to one of three types of agents (A) alkaline agent, (B) base, and (C) reducing agent.
[0032]
Through the steps described above, the agents (A), (B), and (C) are selected, and the hair treatment composition is manufactured through all the steps shown in FIG. Then, next, although the Example of the composition obtained at this process is described, each evaluation method used by the present Example is demonstrated prior to description of each agent of an Example.
[0033]
<Evaluation criteria 1>
[Odor] By professional panelists (10 persons), before use (when mixing 1st agent, 2nd agent and / or 1st agent, 2nd agent), in use, regarding hair dye, hair bleach and permanent agent The odor felt by each panel after use was evaluated according to the following criteria.
◎ ・ ・ ・ No odor at all
○ ・ ・ ・ No odor
△ ・ ・ ・ Slight irritating odor or base odor
× ・ ・ ・ I feel a strong irritating odor or base odor
[0034]
<Evaluation criteria 2>
Measurement with a detector tube: The measurement with a detector tube is in principle the same as the above measurement performed for each agent (repost).
(1) One gram of a measurement object is taken as a sample SMP in a petri dish 110 having a diameter of 30 mm and a depth of 15 mm, and the surface thereof is adjusted as flat as possible.
(2) The petri dish 110 is placed in a glass screw port desiccator 100 having an internal volume of 3 liters and sealed.
(3) After being left in this state for 3 hours and the objects to be detected are uniformly dispersed in the desiccator 100, the detector tube type gas measuring device 120 is connected to the desiccator screw port 105, and the handle 130 is operated to measure the measurement gas. Sucking in ammonia, amines, hydrogen sulfide andBimeThe concentration of lucaptan is measured using a dedicated detector tube.
[0035]
The odor to be measured and detector tube type are as follows (repost).
・ Ammonia: 3L ammonia detector tube manufactured by Gastec
Measurement range, 0.5-78ppm
Detection limit, 0.2ppm
Number of aspirations 2 times, aspiration volume 100 ml / time
Suction time 60 seconds
・ Amines: 180L amine detector tube manufactured by Gastec
Measuring range, 0.5-10ppm
Detection limit, 0.1ppm
Number of aspirations 1 time, aspiration volume 100 ml / time
Suction time 60 seconds
-Hydrogen sulfide: 4LT hydrogen sulfide detector tube manufactured by Gastec
Measurement range, 0.1-4ppm
Detection limit, 0.05ppm
Number of aspirations 2 times, aspiration volume 100 ml / time
Suction time 60 seconds
・ MeLUCAPTAN: 70L mercaptans detector tube manufactured by GASTECH
Measurement range, 0.1-8.0ppm
Detection limit, 0.05ppm
Number of aspirations 4 times, aspiration volume 100 ml / time
Suction time 90 seconds
Under such conditions, the concentration of the odor to be measured was measured in ppm.
[0036]
<Evaluation criteria 3>
[Hair damage] Collect 30 hairs from each hair bundle that has been treated with a hair dye, a depigmenting agent and a permanent wave, and fix both ends of 5 cm and 6 cm from the tip of the hair with 1 cm wide glass fiber tape, Break the hair at the 5 cm and 6 cm portions from the hair tip, measure the hair diameter with a micrometer, measure the break weight with a rheometer, and pull the hair according to the following formula (1). The strength was determined.
[0037]
[Expression 1]

[0038]
<Examples 1-3, Comparative Examples 1-3>
FIG. 6 shows the compositions of the first agent and the second agent of Examples 1 to 3 and Comparative Examples 1 to 3, evaluation of odor based on Evaluation Criteria 1, and evaluation of hair damage based on Evaluation Criteria 3. It was. In FIG. 6, each component was prepared as a sample of the hair dye composition first agent and second agent according to the process shown in FIG.
[0039]
In the examples, “nonionic solubilizer” used was polyoxyethylene cetyl ether which can be purchased as “BC series” manufactured by Nikko Chemicals Co., Ltd. Alternatives include the company's “BS Series” polyoxyethylene stearyl ether, Japan Emulsion Co., Ltd., and “EMALEX 600 Series”. In addition, “Promois SILK-1000” manufactured by Seiwa Kasei Co., Ltd. was used as the “hydrolyzed silk solution”. Furthermore, as a fragrance | flavor, what mixed each component extracted from orange, lemon, bergamot, and mandarin as a natural essential oil was used in the ratio of 2: 1: 1: 2. Among these, the nonionic solubilizer is the same in Examples 4 and 5 and Comparative Examples 4 to 6 described later. Moreover, about the hydrolysis silk liquid and the fragrance | flavor, the same thing was used also in all the Examples and all the comparative examples.
[0040]
Next, the first agent and the second agent were mixed at a weight ratio of 1: 2. In FIG. 6, (mixed) indicates this mixed state. The mixture was applied to untreated hair having a length of 20 cm and a weight of 15 g, left for 30 minutes, then washed with water and dried with a dryer. The tensile strength of Evaluation Criteria 3 was measured in this state.
[0041]
As shown in the figure, in Examples 1 to 3, the panelists did not feel any odor even when the first agent, the second agent, and both agents were mixed. Moreover, the tensile strength of the hair which received the process with the composition of the Example was all 33 kilograms or more, and the damage was small. On the other hand, in the comparative examples, when both the first agent and both agents were mixed, there was a slight irritating odor (Comparative Example 1) or a strong odor was felt. Moreover, the tensile strength was 30 kg or less.
[0042]
<Examples 4 and 5 and Comparative Examples 4 to 6>
FIG. 7 shows the compositions of the first agent and the second agent of Examples 4 and 5 and Comparative Examples 4 to 6, the evaluation of odor based on Evaluation Standard 1, and the evaluation of hair damage based on Evaluation Standard 3. It was. In FIG. 7, each component was prepared as a sample of the hair bleaching agent composition first agent and second agent according to the process shown in FIG.
[0043]
Next, the first agent and the second agent were mixed at a weight ratio of 1: 2. In FIG. 7, (mixed) indicates this mixed state. The mixture was applied to untreated hair having a length of 20 cm and a weight of 15 g, left for 30 minutes, then washed with water and dried with a dryer. The tensile strength of Evaluation Criteria 3 was measured in this state.
[0044]
As shown in the figure, in Examples 4 and 5, the panelists did not feel any odor even when the first agent, the second agent, and both agents were mixed. Moreover, the tensile strength of the hair which received the process with the composition of the Example was all 34 kilograms or more, and the damage was small. On the other hand, in the comparative examples, when both the first agent and both agents were mixed, a strong odor was felt. Further, the tensile strength was 29 kilograms or less.
[0045]
<Examples 6-8, Comparative Examples 7-9>
FIG. 8 shows the compositions of the first agent and the second agent of Examples 6 to 8 and Comparative Examples 7 to 9, the evaluation of odor by Evaluation Criteria 1, and the evaluation of hair damage by Evaluation Criteria 3. It was. In FIG. 8, each component was prepared as a sample of the permanent wave composition first agent and second agent according to the process shown in FIG. 1.
[0046]
The nonionic solubilizers used in Examples 6 to 8 and Comparative Examples 7 to 9 are polyoxyethylene castor oils (or “CO (or HCO) series”) manufactured by Nikko Chemicals Co., Ltd. (or Hardened castor oil). As an alternative, there is polyoxyethylene polyoxypropylene alkyl ether of “PBC (or PEN) series” manufactured by the same company.
[0047]
Next, untreated hair having a length of 20 cm and a weight of 15 g is wound on a rod having a diameter of 13 mm, immersed in the first permanent wave agent shown in FIG. 8 for 10 minutes, then washed with water, and then 10% in the second agent for permanent wave. Soaking for a minute, washing with water and drying with a dryer. The tensile strength of Evaluation Criteria 3 was measured in this state.
[0048]
As shown in the figure, in Examples 6 to 8, the panelists did not feel any odor during the first agent, the second agent, and during and after use. Moreover, the tensile strength of the hair which received the process with the composition of the Example was all 34 kilograms or more, and the damage was small. On the other hand, in the comparative examples, a strong odor was felt in the first agent alone, during use, and after use. Moreover, the tensile strength was 25 kilograms or less.
[0049]
Next, FIG. 9 shows the results of evaluating the odor according to Evaluation Criteria 2 for Examples 1 to 8 described above. In the figure, except for the first and sixth examples, there is no indication of the second agent, but for the second to fifth examples, the second agent is the same as the first example. Since the seventh and eighth examples are the same as the sixth example, display of the results is omitted. Further, the results of measurement in the same manner for Comparative Examples 1 to 9 described above are shown in FIG.
[0050]
For Examples 1 to 8, as shown in FIG. 9, ammonia, amines, hydrogen sulfide, and mercaptans are hardly detected or very small amounts, and unpleasant odors based on these components are It turns out that there is hardly any. On the other hand, in the comparative example shown in FIG. 10, ammonia is 30 ppm or more (amount exceeding the detection upper limit of the detection tube used), amines is 100 ppm or more (amount exceeding the detection upper limit of the detection tube used), mercaptan However, 4 ppm or more was detected except for the mixture of Comparative Example 1 and the first agent of Comparative Example 8, indicating that the user feels a very strong unpleasant odor.
[0051]
【The invention's effect】
As described in detail above, according to the hair treatment composition of the present invention, the composition itself has no unpleasant odor. Therefore, the user can use various hair treatment compositions without suffering from an unpleasant odor. Moreover, according to the manufacturing method of the hair-treatment agent composition of this invention, the hair-treatment agent composition without an unpleasant odor at the time of use can be obtained with a simple process.
[Brief description of the drawings]
FIG. 1 is a process diagram showing a process for producing a hair treatment composition as an embodiment of the present invention.
FIG. 2 is an explanatory view showing the appearance of a typical detector tube.
FIG. 3 is an explanatory diagram showing a method for measuring odor by the method of Evaluation Criteria 2 in the embodiment.
FIG. 4 is an explanatory diagram showing the results of measuring the contents of four types of ammonia, amines, hydrogen sulfide, and mercaptan for each agent constituting the hair treatment composition of Examples.
FIG. 5 is an explanatory view showing the results of measuring the contents of four types of ammonia, amines, hydrogen sulfide, and mercaptan for other agents constituting the hair treatment composition of Examples.
FIG. 6 is an explanatory diagram showing results according to evaluation criteria 1 and 3 for Examples 1 to 3 and Comparative Examples 1 to 3.
7 is an explanatory diagram showing the results of evaluation criteria 1 and 3 for Examples 4 and 5 and Comparative Examples 4 to 6. FIG.
FIG. 8 is an explanatory diagram showing results according to evaluation criteria 1 and 3 for Examples 6 to 8 and Comparative Examples 7 to 9.
FIG. 9 is an explanatory diagram showing results according to evaluation criteria 2 for Examples 1 to 8.
FIG. 10 is an explanatory diagram showing the results of evaluation criteria 2 for Comparative Examples 1 to 9.
[Explanation of symbols]
100 ... desiccator
105 ... Screw port
110 ... Petri dish
120 ... Detector tube type gas measuring device
130 ... handle
150 ... Detector tube

Claims (4)

A hair treatment composition comprising first and second agents and used for hair dyeing ,
The first agent includes (A) an alkali agent, (B) a base, and (C) a reducing agent, and the second agent includes (B) a base,
The alkali agent (A) is monoethanolamine, and the blending amount of the alkali agent (A) in the first agent is 1 to 10% by weight,
The base (B) includes, as an active agent, at least one dyeing compound selected from the group consisting of an oxidative dye intermediate, a coupler, and a direct dye; and an oxidant that acts on the dyeing compound, One agent contains at least the staining compound, the second agent contains at least the oxidizing agent,
The (C) reducing agent is sodium sulfite and / or ascorbic acid, and the blending amount of the (C) reducing agent in the first agent is 0.1 to 5% by weight,
Neither the first agent nor the second agent contains a fragrance component and a flavoring agent,
When the first and second agents are alone and 1 gram of each agent is left in a 3 liter desiccator for 3 hours, and then a predetermined component that stimulates olfaction is detected using a detector tube,
Ammonia: 1 ppm or less,
Amines: 0.5 ppm or less,
Hydrogen sulfide: 0.05 ppm or less,
Mercaptans: 0. 05 ppm or less,
When 1 gram of the agent mixed with the first and second agents in use is left in a 3 liter desiccator for 3 hours, and then a predetermined component that stimulates odor is detected using a detector tube,
Ammonia: 1 ppm or less,
Amines: 0.75 ppm or less,
Hydrogen sulfide: 0.05 ppm or less,
Mercaptan: A hair treatment composition that is 0.05 ppm or less. A hair treatment composition according to claim 1,
A hair treatment composition wherein the pH of the composition is in the range of 5 to 13. A method for producing a hair treatment composition for hair dye comprising the first and second agents,
(A) Prepare monoethanolamine as an alkaline agent,
(B) As a base, as an active agent , preparing at least one dyeing compound selected from the group consisting of an oxidative dye intermediate, a coupler and a direct dye, and an oxidant acting on the dyeing compound,
(C) preparing sodium sulfite and / or ascorbic acid as a reducing agent,
The first agent comprises (A) the alkali agent, (B) base, (C) a reducing agent only contains, and (B) at least the dye compound as a base,
The former second agent (B) contains at least the oxidizing agent as a base,
The amount of monoethanolamine in the first agent is adjusted to 1 to 10% by weight, the amount of sodium sulfite and / or ascorbic acid in the first agent is adjusted to 0.1 to 5% by weight,
Neither the first agent nor the second agent is blended with a fragrant component and a flavoring agent,
When the first and second agents are alone and 1 gram of each agent is left in a 3 liter desiccator for 3 hours, and then a predetermined component that stimulates olfaction is detected using a detector tube,
Ammonia: 1 ppm or less,
Amines: 0.5 ppm or less,
Hydrogen sulfide: 0.05 ppm or less,
Mercaptans: 0. Make sure that is 0 5ppm or less,
By storing the prepared first and second agents in a predetermined container so as to be used for hair dyeing,
When 1 gram of the agent mixed with the first and second agents at the time of use is left in a 3 liter desiccator for 3 hours and then a predetermined component that stimulates odor is detected using a detector tube,
Ammonia: 1 ppm or less,
Amines: 0.75 ppm or less,
Hydrogen sulfide: 0.05 ppm or less,
Mercaptan: 0.05 ppm or less
A method for producing a hair treatment composition. A method for producing a hair treatment composition according to claim 3,
The preparation of the first and second agents is as follows:
Classifying the selected first and second agents into an oil phase that is an oil-soluble component, an aqueous phase that is a water-soluble component, and an additive phase that is an unstable component at high temperatures, and weighing ,
A step of heating and dissolving the components of the oil phase and the aqueous phase,
A step of adding and emulsifying and mixing the aqueous phase, which has reached a predetermined temperature or more, to the oil phase,
A step of cooling the emulsified mixture to a predetermined temperature or lower and then adding the components of the additive phase to the emulsified mixture at a low temperature.

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