JP4883964B2 - Hair cosmetics - Google Patents

Hair cosmetics Download PDF

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JP4883964B2
JP4883964B2 JP2005264012A JP2005264012A JP4883964B2 JP 4883964 B2 JP4883964 B2 JP 4883964B2 JP 2005264012 A JP2005264012 A JP 2005264012A JP 2005264012 A JP2005264012 A JP 2005264012A JP 4883964 B2 JP4883964 B2 JP 4883964B2
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hair
agent
acid
treatment method
hair treatment
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JP2007077037A (en
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和久 福原
雅規 高井
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Kao Corp
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/04—Preparations for permanent waving or straightening the hair
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24—Phosphorous; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585—Organosilicon compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/95—Involves in-situ formation or cross-linking of polymers

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Cosmetics (AREA)

Description

本発明は、毛髪にハリ・コシを付与する毛髪化粧料及び毛髪処理方法に関する。   The present invention relates to a hair cosmetic and a hair treatment method for imparting firmness and firmness to hair.

従来、毛髪の内部に物質を浸透させて毛髪の物性や外観、感触を改質する方法として毛髪成分と類似したコラーゲン、ケラチン等の分解物及び誘導体を補充する方法が提案されているが、未だ十分な効果とはいえない。   Conventionally, a method of replenishing degradation products and derivatives of collagen, keratin, etc. similar to hair components has been proposed as a method for improving the physical properties, appearance, and feel of hair by infiltrating substances into the hair, but it has not yet been proposed. It is not a sufficient effect.

一方、アルカリ処理した毛髪に、アルキルトリアルコキシシランを用いて、毛髪を強化する技術が知られている（例えば、特許文献１参照）。また、有機ケイ素化合物等を用い部分的又は全体的に加水分解し、部分的又は全体的に重合させることで得られる有機ケイ素化合物を、爪、毛髪等のケラチン物質に適用することで、ケラチン物質を保護および強化するための方法も提案されている（例えば、特許文献２及び３参照）。   On the other hand, a technique for strengthening hair using alkyltrialkoxysilane on alkali-treated hair is known (see, for example, Patent Document 1). Further, by applying an organosilicon compound obtained by partial or total hydrolysis using an organosilicon compound or the like and partial or total polymerization to a keratin material such as a nail or hair, a keratin material A method for protecting and strengthening is also proposed (see, for example, Patent Documents 2 and 3).

しかしながら、これらの技術では、有機ケイ素化合物は、ケラチン表面にのみ存在するものであるため、洗浄により効果が無くなったり、ケラチン表面の感触が本来の感触でなくなったりするという問題を有する。
特開昭61-7号公報 特表2000-510167号公報 特開2002-97114号公報 However, in these techniques, since the organosilicon compound exists only on the keratin surface, there is a problem that the effect is lost by washing, or the feel of the keratin surface is not the original feel.
JP 61-7 Special Table 2000-510167 JP 2002-97114 A

本発明は、毛髪繊維、特にハリ・コシがない毛髪（化学処理等で損傷した毛髪、欧米人や高齢者の細い毛髪等）に対し、優れたハリ・コシを付与することができる毛髪化粧料及び毛髪処理方法を提供することを目的とする。ここで、ハリ・コシを付与するとは、毛髪弾性を向上させることをいう。   The present invention is a hair cosmetic that can impart excellent firmness and firmness to hair fibers, particularly hair that has no firmness and firmness (hair damaged by chemical treatment, etc., thin hair of Westerners and elderly people, etc.) And an object of the present invention is to provide a hair treatment method. Here, giving firmness and elasticity means improving hair elasticity.

本発明者は、酸（カルボン酸を除く）の共存下でアルコキシシランの加水分解を行い、生成したシラノール化合物を適度な時間内に毛髪に塗布することにより、シラノール化合物を毛髪に浸透させ、かつ毛髪内部で重合させることができ、毛髪に優れたハリ・コシを付与できることを見出した。この技術によれば、毛髪内でシラノール化合物を重合し、毛髪内部から毛髪の改質を行うことができるため、従来の有機ケイ素化合物を用いて毛髪表面に被膜を形成させ毛髪を強化及び保護する技術に比べ、明らかに毛髪改質効果、感触及び持続性に優れている。   The present inventor hydrolyzes alkoxysilane in the presence of an acid (excluding carboxylic acid), and by applying the produced silanol compound to the hair within an appropriate time, the silanol compound penetrates into the hair, and It has been found that it can be polymerized inside the hair and can impart excellent elasticity and firmness to the hair. According to this technology, the silanol compound can be polymerized in the hair and the hair can be modified from the inside of the hair, so that a conventional organic silicon compound is used to form a film on the hair surface to strengthen and protect the hair. Compared with technology, it is clearly superior in hair modification effect, feel and sustainability.

本発明は、第一の態様として、次の一般式(1)で表されるアルコキシシラン（以下「アルコキシシラン(1)」という）を含有する第１剤と、酸（カルボン酸を除く）及び水を含有しpH1.5〜４である第２剤とからなる毛髪化粧料、第二の態様として、アルコキシシラン(1)、酸（カルボン酸を除く）及び水を配合してなり、pH２〜４である毛髪化粧料を提供するものである。   The present invention provides, as a first aspect, a first agent containing an alkoxysilane represented by the following general formula (1) (hereinafter referred to as “alkoxysilane (1)”), an acid (excluding carboxylic acid), and A hair cosmetic comprising a second agent containing water and having a pH of 1.5 to 4, as a second embodiment, comprising an alkoxysilane (1), an acid (excluding carboxylic acid) and water, and having a pH of 2 4 is provided.

Ｒ1 pＳｉ(ＯＲ2)4-p (1) R 1 p Si (OR 2 ) 4-p (1)

〔式中、Ｒ1及びＲ2は、炭素数１〜６の直鎖若しくは分岐鎖のアルキル基又は炭素数２〜６の直鎖若しくは分岐鎖のアルケニル基を示し、ｐ個のＲ1及び（４−ｐ）個のＲ2は同一でも異なってもよい。ｐは０〜３の整数を示す。〕 [Wherein, R 1 and R 2 represent a linear or branched alkyl group having 1 to 6 carbon atoms or a linear or branched alkenyl group having 2 to 6 carbon atoms, and p R 1 and ( 4-p) R 2 may be the same or different. p shows the integer of 0-3. ]

また本発明は、上記第一の態様の毛髪化粧料における第１剤と第２剤とを混合して得られる混合物、又は第二の態様の毛髪化粧料を毛髪に塗布し、アルコキシシラン(1)の加水分解で生成する次の一般式(2)で表されるシラノール化合物を毛髪に浸透させる毛髪処理方法を提供するものである。   In addition, the present invention applies a mixture obtained by mixing the first agent and the second agent in the hair cosmetic composition of the first aspect or the hair cosmetic composition of the second aspect to the hair, and alkoxysilane (1 The present invention provides a hair treatment method in which the silanol compound represented by the following general formula (2) generated by hydrolysis of

Ｒ1 pＳｉ(ＯＨ)n(ＯＲ2)4-p-n (2) R 1 p Si (OH) n (OR 2 ) 4-pn (2)

〔式中、Ｒ1、Ｒ2及びｐは前記と同じ意味を示し、ｎは１以上（４−ｐ）以下の整数を示す。ｐ個のＲ1及び（４−ｐ−ｎ）個のＲ2は同一でも異なってもよい。〕 [Wherein R 1 , R 2 and p represent the same meaning as described above, and n represents an integer of 1 or more and (4-p) or less. p R 1 and (4-p−n) R 2 may be the same or different. ]

本発明によれば、アルコキシシランの加水分解で生成したシラノール化合物を毛髪に浸透させ、かつ毛髪内部で重合させることができるため、毛髪直径が増加する。その結果として、毛髪、特に、ハリ・コシがない毛髪（損傷毛、細い毛髪等）に対し、優れたハリ・コシを付与することができる。更に、毛髪のまとまり性向上効果や、くせ毛の矯正効果も得られる。また、その効果はシャンプーを繰り返しても持続する。   According to the present invention, since the silanol compound produced by hydrolysis of alkoxysilane can be penetrated into the hair and polymerized inside the hair, the hair diameter is increased. As a result, excellent firmness and firmness can be imparted to hair, particularly hair that does not have firmness and firmness (damaged hair, fine hair, etc.). Furthermore, the effect of improving the cohesiveness of the hair and the effect of correcting the comb hair are also obtained. In addition, the effect persists even after repeated shampooing.

本発明の毛髪処理方法における「毛髪処理」とは、毛髪をハリ・コシやまとまりのある髪質に改質することをいう。   “Hair treatment” in the hair treatment method of the present invention refers to modifying the hair into a firm, firm, and coherent hair quality.

〔アルコキシシラン(1)〕
一般式(1)中のＲ1及びＲ2において、アルキル基としては、メチル基、エチル基、プロピル基、ブチル基、イソプロピル基、イソブチル基、t-ブチル基等が挙げられ、アルケニル基としては、ビニル基、アリル基等が挙げられる。特に、Ｒ2としては、加水分解により生じる副生成物の安全性、加水分解反応の反応性等の点から、エチル基が好ましい。 [Alkoxysilane (1)]
In R 1 and R 2 in the general formula (1), examples of the alkyl group include a methyl group, an ethyl group, a propyl group, a butyl group, an isopropyl group, an isobutyl group, and a t-butyl group. , Vinyl group, allyl group and the like. In particular, R 2 is preferably an ethyl group from the viewpoint of safety of by-products generated by hydrolysis, reactivity of hydrolysis reaction, and the like.

アルコキシシラン(1)は、本発明の毛髪化粧料が二剤式の場合には、水を含有しない第１剤に配合され、水を含有する第２剤と混合後、加水分解によって水溶性のシラノール化合物(2)となり、毛髪内への浸透が可能になる。生成するシラノール化合物(2)の物性、毛髪内への浸透性の点から、一般式(1)中のｐは０〜２が好ましい。アルコキシシラン(1)としては、テトラメトキシシラン、テトラエトキシシラン、アルキル（炭素数１〜６）トリメトキシシラン、アルキル（炭素数１〜６）トリエトキシシラン、ジアルキル（炭素数１〜６）ジエトキシシラン等が挙げられる。   When the hair cosmetic composition of the present invention is a two-component type, the alkoxysilane (1) is blended with the first agent not containing water, mixed with the second agent containing water, and then water-soluble by hydrolysis. It becomes a silanol compound (2) and can penetrate into the hair. From the viewpoint of physical properties of the silanol compound (2) to be produced and penetrability into hair, p in the general formula (1) is preferably 0-2. Examples of the alkoxysilane (1) include tetramethoxysilane, tetraethoxysilane, alkyl (1 to 6 carbon atoms) trimethoxysilane, alkyl (1 to 6 carbon atoms) triethoxysilane, and dialkyl (1 to 6 carbon atoms) diethoxy. Silane etc. are mentioned.

アルコキシシラン(1)の含有量は、架橋反応による反応性の点から、本発明の毛髪化粧料中（二剤式の場合には第１剤と第２剤を合わせた全組成中；以下同じ）の４重量％以上、特に12重量％以上が好ましく、また82重量％以下、特に58重量％以下が好ましい。また、第１剤中のアルコキシシラン(1)の含有量は、保存安定性の点から、70〜100重量％、更には80〜100重量％、特に90〜100重量％が好ましい。   The content of alkoxysilane (1) is in the hair cosmetic composition of the present invention from the point of reactivity due to the crosslinking reaction (in the case of two-component type, in the total composition of the first agent and the second agent; the same applies hereinafter) 4% by weight or more, particularly 12% by weight or more, and preferably 82% by weight or less, particularly preferably 58% by weight or less. Further, the content of the alkoxysilane (1) in the first agent is preferably 70 to 100% by weight, more preferably 80 to 100% by weight, and particularly preferably 90 to 100% by weight from the viewpoint of storage stability.

〔酸（カルボン酸を除く）〕
本発明では、酸としてカルボン酸以外の酸が使用される。かかる酸としては、塩酸、硫酸、硝酸、リン酸等の無機酸類、メタンスルホン酸、パラトルエンスルホン酸等の有機スルホン酸類、ラウリル硫酸等のアルキル硫酸類、モノラウリルリン酸等のアルキルリン酸類が例示される。これらの中で無機酸類が好ましく、なかでもpH調整が容易な点から、リン酸が好ましい。 [Acid (excluding carboxylic acid)]
In the present invention, an acid other than a carboxylic acid is used as the acid. Examples of such acids include inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid, organic sulfonic acids such as methanesulfonic acid and paratoluenesulfonic acid, alkyl sulfuric acids such as lauryl sulfuric acid, and alkyl phosphoric acids such as monolauryl phosphoric acid. Illustrated. Among these, inorganic acids are preferable, and phosphoric acid is particularly preferable from the viewpoint of easy pH adjustment.

酸は、本発明の毛髪化粧料が二剤式の場合には、第１剤に配合されるアルコキシシラン(1)とは別個に第２剤に配合することが溶解性、保存安定性の点から好ましい。酸は、第２剤又は全組成のpHが別途規定する範囲内となる量が使用される。酸の含有量は、酸の種類や緩衝系によって大きく異なるため、一律に規定することはできない。比較的低濃度の酸を用いてアルコキシシランの加水分解に長時間をかけてシラノール化合物を生成させた場合は、生成したシラノール化合物が比較的安定であるため毛髪に浸透しやすく処理効果が高い。この場合の適切な濃度としては、塩酸を単体で用いる場合、本発明の毛髪化粧料中に、純分として0.001〜0.01重量％が好ましく、リン酸を単体で用いる場合、純分として0.001〜0.01重量％が好ましい。一方、比較的高濃度の酸を用いてアルコキシシランの加水分解を比較的短時間で完了させ処理を簡便に行う場合には、生成したシラノール化合物が重合する前に毛髪に浸透するように、シラノール化合物が生成した後直ぐ（10分以内）に毛髪に塗布すると良い。この場合の酸の濃度は、塩酸を単体で用いる場合、本発明の毛髪化粧料中に、純分として0.01〜0.05重量％が好ましく、リン酸を単体で用いる場合、純分として0.01〜0.5重量％が好ましく、リン酸緩衝系の場合、リン酸の純分として0.2〜２重量％が好ましい。   In the case where the hair cosmetic composition of the present invention is a two-component type, the acid may be blended in the second agent separately from the alkoxysilane (1) blended in the first agent, in terms of solubility and storage stability. To preferred. The acid is used in such an amount that the pH of the second agent or the total composition falls within a separately specified range. Since the acid content varies greatly depending on the type of acid and the buffer system, it cannot be defined uniformly. When a silanol compound is produced by taking a long time to hydrolyze alkoxysilane using a relatively low concentration of acid, the produced silanol compound is relatively stable, so that it easily penetrates into hair and has a high treatment effect. As an appropriate concentration in this case, when hydrochloric acid is used alone, the hair cosmetic composition of the present invention preferably has a pure content of 0.001 to 0.01% by weight, and when phosphoric acid is used alone, 0.001 to 0.01 as a pure component. % By weight is preferred. On the other hand, when the hydrolysis of alkoxysilane is completed in a relatively short time using a relatively high concentration of acid and the treatment is carried out easily, the silanol compound is allowed to penetrate into the hair before polymerization. It may be applied to the hair as soon as the compound is formed (within 10 minutes). The concentration of the acid in this case is preferably 0.01 to 0.05% by weight as a pure component in the hair cosmetic composition of the present invention when hydrochloric acid is used alone, and 0.01 to 0.5% as a pure component when phosphoric acid is used alone. %, And in the case of a phosphate buffer system, 0.2 to 2% by weight is preferable as a pure content of phosphoric acid.

〔水〕
水は、本発明の毛髪化粧料が二剤式の場合には、第１剤に配合されるアルコキシシラン(1)とは別個に、第２剤に配合され、その含有量は、毛髪を十分に膨潤させ、加水分解で生成するシラノール化合物(2)を毛髪へ十分浸透させる観点から、本発明の毛髪化粧料中の20〜95重量％、特に30〜86重量％が好ましい。 〔water〕
When the hair cosmetic composition of the present invention is a two-component type, water is blended in the second agent separately from the alkoxysilane (1) blended in the first agent, and its content is sufficient for the hair. From the viewpoint of allowing the silanol compound (2) produced by hydrolysis to sufficiently penetrate into the hair, 20 to 95% by weight, particularly 30 to 86% by weight in the hair cosmetic composition of the present invention is preferred.

〔pH〕
本発明の毛髪化粧料は、アルコキシシラン(1)を加水分解させ、シラノール化合物(2)を生成させる必要性、及びシラノール化合物(2)を毛髪内に浸透させて毛髪内で重合反応をさせるために、重合反応を遅らせる必要がある。このために本発明の毛髪化粧料のpH（20℃）は２〜４に調整されるが、2.5〜４、特に2.5〜3.5が好ましい。なお、本発明の毛髪化粧料（二剤式の場合は混合後）は、上記pH範囲において緩衝能を有することが好ましく、特に、酸としてリン酸を用い、これにアルカリ金属水酸化物（水酸化ナトリウム等）を添加することにより、リン酸緩衝系とすることが最も好ましい。二剤式の場合には第２剤のpH（20℃）が1.5〜４に調整されるが、1.5〜3.5、特に２〜3.5が好ましい。緩衝系とする場合には、第２剤を緩衝系とすることが好ましい。 [PH]
The hair cosmetic composition of the present invention is required to hydrolyze the alkoxysilane (1) to produce the silanol compound (2), and to allow the silanol compound (2) to penetrate into the hair and cause a polymerization reaction in the hair. In addition, it is necessary to delay the polymerization reaction. For this purpose, the pH (20 ° C.) of the hair cosmetic composition of the present invention is adjusted to 2 to 4, preferably 2.5 to 4, particularly 2.5 to 3.5. The hair cosmetic composition of the present invention (after mixing in the case of the two-component type) preferably has a buffering capacity in the above pH range, and in particular, phosphoric acid is used as the acid, and an alkali metal hydroxide (water) It is most preferable to add a phosphate buffer system by adding sodium oxide or the like. In the case of the two-component type, the pH (20 ° C.) of the second agent is adjusted to 1.5 to 4, but 1.5 to 3.5, particularly 2 to 3.5 is preferable. When a buffer system is used, it is preferable that the second agent is a buffer system.

〔その他の成分〕
また、シラノール化合物(2)を溶解する目的で、メタノール、エタノール等の炭素数１〜３の低級１級アルコール、グリセリン等の水溶性有機溶剤を使用することもできるが、その量が多すぎると、本発明の毛髪化粧料を毛髪に塗布した際に、毛髪が十分に膨潤せず、シラノール化合物(2)が十分に浸透し難くなる。そのため、水溶性有機溶剤の使用量は、本発明の毛髪化粧料中の35重量％以下、特に20重量％以下とすることが好ましい。なお、これ以外に、アルコキシシラン(1)の加水分解後の毛髪化粧料には、副生物としてのＲ2ＯＨが含有されることになる。 [Other ingredients]
In addition, for the purpose of dissolving the silanol compound (2), a water-soluble organic solvent such as methanol or ethanol having 1 to 3 carbon atoms such as lower primary alcohol or glycerin can be used. When the hair cosmetic composition of the present invention is applied to hair, the hair does not swell sufficiently, and the silanol compound (2) does not sufficiently penetrate. Therefore, the amount of the water-soluble organic solvent used is preferably 35% by weight or less, particularly 20% by weight or less in the hair cosmetic composition of the present invention. In addition to this, the hair cosmetic material after hydrolysis of the alkoxysilane (1) contains R 2 OH as a by-product.

本発明の毛髪化粧料には、その他、界面活性剤、油剤、シリコーン誘導体、カチオン性ポリマー、保湿剤、粘度調整剤、香料、色素、紫外線吸収剤、酸化防止剤、抗菌剤、防腐剤等を、目的に応じて適宜配合することができる。   The hair cosmetic composition of the present invention includes surfactants, oil agents, silicone derivatives, cationic polymers, humectants, viscosity modifiers, fragrances, pigments, UV absorbers, antioxidants, antibacterial agents, preservatives, etc. Depending on the purpose, it can be blended appropriately.

〔毛髪化粧料の形態〕
本発明の毛髪化粧料の形態は、長期間安定である点から、好適には、アルコキシシラン(1)を含有する第１剤と、酸（カルボン酸を除く）及び水を含有しpH1.5〜４である第２剤からなるものであるが、使用直前にアルコキシシラン(1)、酸（カルボン酸を除く）及び水、並びにその他任意成分を混合し、pHを２〜４とすることによって調製されたものであってもよい。 [Form of hair cosmetic]
The form of the hair cosmetic composition of the present invention preferably contains a first agent containing alkoxysilane (1), an acid (excluding carboxylic acid), and water, and has a pH of 1.5. It consists of the second agent that is ~ 4, but by mixing the alkoxysilane (1), acid (excluding carboxylic acid) and water and other optional components immediately before use, and adjusting the pH to 2-4 It may be prepared.

本発明の毛髪化粧料を、使用直前にアルコキシシラン(1)、酸及び水、並びにその他任意成分を混合することによって調製する場合、混合する順序は、特に限定されないが、加水分解によって生成したシラノール化合物(2)は、即座に重合反応を開始するので、これを抑制するため、酸と水を混合した後にアルコキシシラン(1)を混合することが好ましい。   When the hair cosmetic composition of the present invention is prepared by mixing alkoxysilane (1), acid and water, and other optional components immediately before use, the mixing order is not particularly limited, but silanol produced by hydrolysis Since the compound (2) starts a polymerization reaction immediately, in order to suppress this, it is preferable to mix the alkoxysilane (1) after mixing the acid and water.

本発明の二剤式毛髪化粧料の第１剤及び第２剤を使用直前に混合することにより、又はアルコキシシラン(1)、酸及び水、並びにその他任意成分を混合することにより、アルコキシシラン(1)は、加水分解によって水溶性のシラノール化合物(2)となり、毛髪内への浸透が可能になる。シラノール化合物(2)の物性、毛髪内への浸透性の点から、一般式(2)中のｐは０〜２が好ましく、ｎは２〜４が好ましく、（４−ｐ−ｎ）は０が好ましい。また、シラノール化合物(2)の分子量は、毛髪内への浸透のし易さから、300以下、特に90〜200が好ましい。   By mixing the first and second agents of the two-component hair cosmetic of the present invention immediately before use, or by mixing alkoxysilane (1), acid and water, and other optional components, 1) becomes a water-soluble silanol compound (2) by hydrolysis and can penetrate into the hair. From the viewpoint of the physical properties of the silanol compound (2) and the penetrability into hair, p in the general formula (2) is preferably 0 to 2, n is preferably 2 to 4, and (4-pn) is 0. Is preferred. Further, the molecular weight of the silanol compound (2) is preferably 300 or less, particularly preferably 90 to 200, from the viewpoint of easy penetration into hair.

〔毛髪処理方法〕
本発明の毛髪化粧料を用いて毛髪を処理するには、本発明の二剤式毛髪化粧料の第１剤及び第２剤を使用直前に混合後、又はアルコキシシラン(1)、酸（カルボン酸を除く）及び水、並びにその他任意成分を使用直前に混合後、振とう攪拌して、目視で混合溶液が均一な１相になったことを確認した後に、得られた混合物を毛髪に塗布するのが好ましい。第１剤と第２剤の混合割合（第１剤／第２剤の重量比）は、好ましくは80／20〜１／99、更に好ましくは60／40〜20／80である。混合直後はお互いに相溶しない状態であったのが、振とう攪拌を継続するうちに均一な１相となることで、アルコキシシラン(1)が加水分解し、シラノール化合物(2)が生成したことを確認することができる。 [Hair treatment method]
In order to treat the hair using the hair cosmetic composition of the present invention, the first agent and the second agent of the two-component hair cosmetic composition of the present invention are mixed immediately before use, or after alkoxysilane (1), acid (carvone) (Excluding acid) and water, and other optional components are mixed immediately before use, shaken and stirred, and after confirming that the mixed solution has become a uniform single phase by visual observation, apply the resulting mixture to the hair It is preferable to do this. The mixing ratio of the first agent and the second agent (weight ratio of the first agent / second agent) is preferably 80/20 to 1/99, more preferably 60/40 to 20/80. Immediately after mixing, they were incompatible with each other, but by continuing to be shaken and stirred, it became a uniform single phase, so that alkoxysilane (1) was hydrolyzed and silanol compound (2) was produced. I can confirm that.

得られた混合物を放置すれば、シラノール化合物(2)の重合反応が進むので、３時間以内、更には30分以内、特に15分以内に、得られた混合物を毛髪に塗布することが好ましい。これにより、シラノール化合物(2)を毛髪内に浸透させることができる。塗布する毛髪は、濡れていてもよく、乾いていてもよい。乾燥した毛髪１ｇに対して、前記混合物を、0.5〜３ｇ塗布することが好ましい。塗布する対象は、人の頭髪であってもよく、かつら等の毛髪であってもよい。   If the resulting mixture is allowed to stand, the polymerization reaction of the silanol compound (2) proceeds, so it is preferable to apply the obtained mixture to the hair within 3 hours, further within 30 minutes, particularly within 15 minutes. This allows the silanol compound (2) to penetrate into the hair. The hair to be applied may be wet or dry. It is preferable to apply 0.5 to 3 g of the mixture to 1 g of dried hair. The target to be applied may be human hair or hair such as a wig.

シラノール化合物(2)を毛髪に十分に浸透させるために、毛髪に塗布しておく時間は、15〜90分、特に20〜60分が好ましい。塗布後一定時間放置することで、シラノール化合物(2)の浸透及び重合反応を進める。この際、毛髪の塗布部を40〜90℃、好ましくは40〜60℃に加温してもよい。場合によっては酸、塩基などを毛髪に塗布し、シラノール化合物(2)の重合反応を促進してもよい。重合反応後に毛髪表面に付着しているシラノール化合物、及びその重合物は、毛髪乾燥後に被膜となり、毛髪感触の悪化を引き起こす原因になるため、シャンプー等で十分に除去することが好ましい。   In order to allow the silanol compound (2) to sufficiently permeate into the hair, the time applied to the hair is preferably 15 to 90 minutes, particularly preferably 20 to 60 minutes. By allowing it to stand for a certain period of time after coating, the penetration and polymerization reaction of the silanol compound (2) proceeds. Under the present circumstances, you may heat the application part of hair to 40-90 degreeC, Preferably it is 40-60 degreeC. In some cases, an acid, a base, or the like may be applied to the hair to accelerate the polymerization reaction of the silanol compound (2). Since the silanol compound adhering to the hair surface after the polymerization reaction and the polymer thereof become a film after drying the hair and cause deterioration of the hair feel, it is preferably removed sufficiently with a shampoo or the like.

実施例１〜８及び比較例１〜６
メチルトリエトキシシランからなる第１剤と、各種の酸及び水を含有する第２剤を混合して表１に示す毛髪化粧料を調製し、加水分解時間、ポリシロキサン収着量、ハリ・コシ感、まとまり感について評価を行った。この結果を表１に併せて示す。 Examples 1-8 and Comparative Examples 1-6
A hair cosmetic shown in Table 1 is prepared by mixing a first agent composed of methyltriethoxysilane and a second agent containing various acids and water, and the hydrolysis time, polysiloxane sorption amount, elasticity Evaluation was made on feeling and unity. The results are also shown in Table 1.

＜毛髪処理方法＞
一人の欧米人から採取した化学処理履歴のない毛髪を用いて、６ｇの毛束を作製した。次いで、この毛束に表１に示す毛髪化粧料10ｇをむらなく塗布した後、ラップで包み、48℃のオーブン中で30分静置した。その後、余分な毛髪化粧料をタオルでふき取り、pH３の10重量％リンゴ酸−水酸化ナトリウム緩衝液中で15分間室温（23℃）にて放置し、毛髪内のシラノール化合物を重合した。その後、以下に示す組成のシャンプー及びヘアリンスで処理してから乾燥した。
なお、各毛髪化粧料は、第１剤と第２剤を混合し、マグネチックスターラーにより外観が透明になるまで（すなわち加水分解が完了するまで）連続攪拌を行った後、10分以内に毛髪に塗布した。 <Hair treatment method>
A hair bundle of 6 g was prepared using hair with no chemical treatment history collected from one Westerner. Next, 10 g of the hair cosmetic shown in Table 1 was uniformly applied to the hair bundle, and then wrapped in a wrap and allowed to stand in an oven at 48 ° C. for 30 minutes. Thereafter, excess hair cosmetic was wiped off with a towel and left in a 10 wt% malic acid-sodium hydroxide buffer solution of pH 3 for 15 minutes at room temperature (23 ° C.) to polymerize the silanol compound in the hair. Then, it processed with the shampoo and hair rinse of the composition shown below, and dried.
Each hair cosmetic mixes the first agent and the second agent, and after continuous stirring with a magnetic stirrer until the appearance becomes transparent (that is, until hydrolysis is completed), the hair is within 10 minutes. It was applied to.

・シャンプー
（重量％）
ポリオキシエチレン(2.5)ラウリルエーテル硫酸
ナトリウム（25重量％水溶液） 62.00
ラウリン酸ジエタノールアミド 2.28
エデト酸二ナトリウム 0.10
安息香酸ナトリウム 0.50
オキシベンゾン 0.03
リン酸（75重量％水溶液） 0.10
ジブチルヒドロキシトルエン 0.01
塩化ナトリウム 0.80
赤色106号 0.00012
香料 0.26
精製水 バランス ·shampoo
(weight%)
Polyoxyethylene (2.5) sodium lauryl ether sulfate (25% by weight aqueous solution) 62.00
Lauric acid diethanolamide 2.28
Edetate disodium 0.10
Sodium benzoate 0.50
Oxybenzone 0.03
Phosphoric acid (75 wt% aqueous solution) 0.10
Dibutylhydroxytoluene 0.01
Sodium chloride 0.80
Red No. 106 0.00012
Fragrance 0.26
Purified water balance

・ヘアリンス
（重量％）
塩化ステアリルトリメチルアンモニウム（28重量％水溶液） 3.0
セタノール 3.0
プロピレングリコール 3.0
メチルパラベン 0.1
精製水 バランス ・ Hair rinse
(weight%)
Stearyltrimethylammonium chloride (28 wt% aqueous solution) 3.0
Cetanol 3.0
Propylene glycol 3.0
Methylparaben 0.1
Purified water balance

＜加水分解時間＞
第１剤と第２剤を混合し、マグネチックスターラーにより外観が透明になるまでの時間を加水分解時間とした。 <Hydrolysis time>
The first agent and the second agent were mixed, and the time until the appearance became transparent with a magnetic stirrer was defined as the hydrolysis time.

＜毛髪へのポリシロキサン収着量＞
毛髪へのポリシロキサン収着量評価には「ICP（誘導結合プラズマ）発光分析装置（堀場製作所，JY238ULTRACE）」を用いた。ポリシロキサン収着量は、灰化／アルカリ溶融／ICP法を用いて測定したケイ素元素の量に基づき、ポリシロキサン（ＣＨ3ＳｉＯ1.5）の量に換算して求めた。
試料0.1ｇを白金坩堝に採取し、ヒーターで煙が出なくなるまで炭化後、550℃の電気炉に２時間入れ灰化させる。冷却後、残った灰分上にアルカリ融剤（Ｎａ2ＣＯ3：Ｈ3ＢＯ3＝５：２）１ｇを加え、950℃電気炉30分でアルカリ溶融し、冷却後、６Ｎ塩酸４mLで溶解して純水で50mLにメスアップしたものを試料溶液とした。吸収波長251.612nm、積分時間３秒で３回測定し、その平均値から、検量線を使用してケイ素元素量を求めた。毛髪へのポリシロキサン収着量の計算法は次のとおりである（式中、「2.4」はケイ素元素量からメチルポリシロキサン量への換算係数）。 <Polysiloxane sorption amount on hair>
An ICP (inductively coupled plasma) emission spectrometer (Horiba, JY238ULTRACE) was used to evaluate the amount of polysiloxane sorbed onto the hair. The polysiloxane sorption amount was determined by converting to the amount of polysiloxane (CH 3 SiO 1.5 ) based on the amount of silicon element measured using ashing / alkaline melting / ICP method.
0.1 g of sample is collected in a platinum crucible, carbonized until no smoke is produced with a heater, and then placed in an electric furnace at 550 ° C. for 2 hours for ashing. After cooling, add 1 g of alkaline flux (Na 2 CO 3 : H 3 BO 3 = 5: 2) on the remaining ash, melt in alkali at 950 ° C. for 30 minutes, cool and dissolve in 4 mL of 6N hydrochloric acid. The sample solution was made up to 50 mL with pure water. Measurement was performed three times at an absorption wavelength of 251.512 nm and an integration time of 3 seconds, and the amount of silicon element was determined from the average value using a calibration curve. The calculation method of the amount of polysiloxane sorbed on the hair is as follows (wherein “2.4” is a conversion factor from the amount of silicon element to the amount of methylpolysiloxane).

ポリシロキサン収着量（％）＝〔ケイ素元素量（mg）／毛髪重量（ｇ）〕×0.1×2.4   Polysiloxane sorption amount (%) = [silicon element amount (mg) / hair weight (g)] × 0.1 × 2.4

＜ハリ・コシ感及びまとまり感＞
５名の専門パネラーにより、「毛髪のハリ・コシ向上感」、及び「毛髪のまとまり感」について、下記基準に従って評価し、その合計値を示した。 <Harness, stiffness, and unity>
Five professional panelists evaluated “feeling of firmness and firmness of hair” and “feeling of unity hair” according to the following criteria, and indicated the total value.

・毛髪のハリ・コシ向上感
（未処理毛と比較して、処理毛の方にハリ・コシ感を）
２：感じる
１：やや感じる
０：変わらない ・ Harness and firmness of hair (feels firmness and firmness on treated hair compared to untreated hair)
2: Feel 1: Feel slightly 0: Not change

・毛髪のまとまり感
（未処理毛と比較して、処理毛の方にまとまり感を）
２：感じる
１：やや感じる
０：変わらない ・ A sense of unity of hair (a sense of unity towards treated hair compared to untreated hair)
2: Feel 1: Feel slightly 0: Not change

Claims (8)

次の一般式(1)
Ｒ 1 p Ｓｉ(ＯＲ 2 ) 4-p (1)
〔式中、Ｒ 1 及びＲ 2 は、炭素数１〜６の直鎖若しくは分岐鎖のアルキル基又は炭素数２〜６の直鎖若しくは分岐鎖のアルケニル基を示し、ｐ個のＲ 1 及び（４−ｐ）個のＲ 2 は同一でも異なってもよい。ｐは０〜３の整数を示す。〕
で表されるアルコキシシランを、第１剤と第２剤を合わせた全組成を基準として12〜82重量％含有する第１剤と、酸（カルボン酸を除く）及び水を含有しpH1.5〜４である第２剤とを混合し、目視で混合溶液が均一な１相になったことを確認した後３時間以内に、得られたpH２〜４の混合物を毛髪に塗布し、一般式(1)で表されるアルコキシシランの加水分解で生成する次の一般式(2)
Ｒ1 pＳｉ(ＯＨ)n(ＯＲ2)4-p-n (2)
〔式中、Ｒ1、Ｒ2及びｐは前記と同じ意味を示し、ｎは１以上（４−ｐ）以下の整数を示す。ｐ個のＲ1及び（４−ｐ−ｎ）個のＲ2は同一でも異なってもよい。〕
で表されるシラノール化合物を毛髪に浸透させる毛髪処理方法。 The following general formula (1)
R 1 p Si (OR 2 ) 4-p (1)
[Wherein, R 1 and R 2 represent a linear or branched alkyl group having 1 to 6 carbon atoms or a linear or branched alkenyl group having 2 to 6 carbon atoms, and p R 1 and ( 4-p) R 2 may be the same or different. p shows the integer of 0-3. ]
A first agent containing 12 to 82% by weight of the alkoxysilane represented by the formula (1) and the second agent, based on the total composition of the first agent and the second agent, an acid (excluding carboxylic acid) and water, and a pH of 1.5 mixing the second agent is to 4, applied within 3 hours after the mixed solution was confirmed to have become uniform one phase visually the resulting mixture of pH2~4 the hair, generally The following general formula (2) generated by hydrolysis of the alkoxysilane represented by the formula (1)
R 1 p Si (OH) n (OR 2 ) 4-pn (2)
[Wherein R 1 , R 2 and p represent the same meaning as described above, and n represents an integer of 1 or more and (4-p) or less. p R 1 and (4-p−n) R 2 may be the same or different. ]
A hair treatment method for allowing the silanol compound represented by formula to penetrate into the hair. 第１剤と第２剤の混合物を毛髪に塗布した後、15〜90分放置して一般式(2)で表されるシラノール化合物を毛髪に浸透させる請求項１記載の毛髪処理方法。The hair treatment method according to claim 1, wherein after the mixture of the first agent and the second agent is applied to the hair, the hair is allowed to stand for 15 to 90 minutes to allow the silanol compound represented by the general formula (2) to penetrate into the hair. 第１剤と第２剤の混合物を毛髪に塗布した後、塗布部を加温する、請求項１又は２記載の毛髪処理方法。 The hair treatment method according to claim 1 or 2 , wherein the application part is heated after the mixture of the first agent and the second agent is applied to the hair. 第１剤と第２剤を合わせた全組成中の水の含有量が、20〜95重量％である請求項１〜３のいずれかに記載の毛髪処理方法。 The hair treatment method according to any one of claims 1 to 3 , wherein the content of water in the total composition of the first agent and the second agent is 20 to 95% by weight. 第１剤と第２剤の混合割合（第１剤／第２剤の重量比）が、80／20〜１／99である請求項１〜４のいずれかに記載の毛髪処理方法。The hair treatment method according to any one of claims 1 to 4, wherein a mixing ratio of the first agent and the second agent (weight ratio of the first agent / second agent) is 80/20 to 1/99. 酸が、無機酸である請求項１〜５のいずれかに記載の毛髪処理方法。 The hair treatment method according to any one of claims 1 to 5 , wherein the acid is an inorganic acid. 無機酸が、リン酸である請求項６記載の毛髪処理方法。 The hair treatment method according to claim 6 , wherein the inorganic acid is phosphoric acid. 第１剤と第２剤の混合物が緩衝能を有するものである請求項１〜７のいずれかに記載の毛髪処理方法。 The hair treatment method according to any one of claims 1 to 7 , wherein the mixture of the first agent and the second agent has a buffering capacity.
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