JPH06200405A - Artificial wig - Google Patents
Artificial wigInfo
- Publication number
- JPH06200405A JPH06200405A JP3182146A JP18214691A JPH06200405A JP H06200405 A JPH06200405 A JP H06200405A JP 3182146 A JP3182146 A JP 3182146A JP 18214691 A JP18214691 A JP 18214691A JP H06200405 A JPH06200405 A JP H06200405A
- Authority
- JP
- Japan
- Prior art keywords
- group
- filament
- chemical
- hydrophilic
- artificial wig
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Paints Or Removers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、髪の毛の表面が親水性
化された人工鬘に関するものである。さらに詳しくは、
髪の毛の表面に親水性の単分子膜を形成したことを特徴
とする人工鬘に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an artificial wig in which the surface of hair is made hydrophilic. For more details,
The present invention relates to an artificial wig having a hydrophilic monomolecular film formed on the surface of hair.
【０００２】[0002]
【従来の技術】一般に人工鬘は、ナイロン、アクリル、
分散染料可染型ポリエステル、塩基性可染型ポリエステ
ル、レーヨン、アセテート等の化合繊繊維フィラメント
を用いて作られている。その他、人毛で作られたものも
ある。しかし人毛で作られたものは、高価であったり、
吸汗すると伸びてしまって髪型が崩れ易いという欠点が
ある。2. Description of the Related Art Generally, artificial wigs are made of nylon, acrylic,
It is made of synthetic fiber filaments such as disperse dye dyeable polyester, basic dyeable polyester, rayon and acetate. Others are made of human hair. However, those made of human hair are expensive,
It has the drawback that it grows up when sweating and the hairstyle tends to collapse.
【０００３】一方、化合繊繊維フィラメントで作られた
ものは、コストが安く型くずれしない等優れているが、
帯電し易かったり櫛の通りが悪い、あるいはむれるなど
欠点があった。On the other hand, the one made of the compound fiber filament is excellent in that it is inexpensive and does not lose its shape.
There were drawbacks such as easy charging, poor combing, and peeling.
【０００４】[0004]
【発明が解決しようとする課題】前記従来技術の化合繊
繊維フィラメントを用いた人工鬘の問題を改善するた
め、人工毛の表面を帯電防止処理する方法が用いられて
いるが、まだ満足できるものが無いのが現状である。In order to improve the problem of artificial wigs using the above-mentioned conventional synthetic fiber filaments, a method of antistatic treatment of the surface of artificial hair is used, but it is still satisfactory. There is no such thing.
【０００５】本発明は前記従来技術の課題を解決するた
め、耐久性に優れた所望の親水性を有する人工鬘を提供
することを目的とする。In order to solve the above-mentioned problems of the prior art, it is an object of the present invention to provide an artificial wig having excellent durability and desired hydrophilicity.
【０００６】[0006]
【課題を解決するための手段】前記目的を達成するた
め、本発明の人工鬘は、少なくとも髪の毛の部分が化合
繊繊維で構成された人工鬘において、前記少なくとも髪
の毛の部分の繊維表面が親水性基を含む化学吸着単分子
膜で覆われていることを特徴とする。In order to achieve the above object, the artificial wig of the present invention is an artificial wig in which at least a hair portion is composed of a synthetic fiber, and at least the fiber surface of the hair portion is hydrophilic. It is characterized by being covered with a chemisorption monomolecular film containing a group.
【０００７】前記構成においては、化学吸着単分子膜の
親水性基が、−ＯＨ、−ＣＯＯＨ、−ＮＨ2 、−Ｎ+ Ｒ
3 Ｘ- （ただし、Ｒはアルキル基、Ｘはハロゲン原子を
示す）、−ＮＯ2 、及び−ＳＯ3 Ｈ基から選ばれる少な
くとも一種の官能基であることが好ましい。In the above structure, the hydrophilic group of the chemisorption monolayer is --OH, --COOH, --NH 2 , --N + R.
3 X − (wherein R represents an alkyl group and X represents a halogen atom), —NO 2 and at least one functional group selected from —SO 3 H groups are preferable.
【０００８】また前記構成においては、吸着された化学
吸着単分子膜が、前記の化学式１（ただし、Ａは−Ｏ
Ｈ、−ＣＯＯＨ、−ＮＨ2 、−Ｎ+ Ｒ3 Ｘ- （Ｒはアル
キル基、Ｘはハロゲン原子を示す）、−ＮＯ2 、または
−ＳＯ3 Ｈ基、ｌは３０以下の自然数、Ｂは官能基であ
っても良いし無くてもよい）で示されことが好ましい。In the above structure, the adsorbed chemisorption monolayer is represented by the chemical formula 1 (where A is -O).
H, -COOH, -NH 2, -N + R 3 X - (R is an alkyl group, X represents a halogen atom), - NO 2, or -SO 3 H group, l is 30 or less natural number, B is It may or may not be a functional group).
【０００９】[0009]
【作用】前記した本発明の構成によれば、きわめて親水
性の高い官能基が化学吸着された分子を介して化学結合
で化合繊繊維フィラメント表面に固定されるため、帯電
しにくい。また、たとえフィラメントそのものが撥水性
であり全く吸汗性が無くても、汗はフィラメント表面を
濡らし表面全面に広がり蒸発していくので、蒸れにくく
型くずれしにくい。しかも、この単分子膜は、膜厚がナ
ノメーターレベルであるため、合成フィラメント本来の
弾力性を劣化させるおそれも無い。また、合成フィラメ
ント製の髪の毛の色調や光沢を妨げることもない。しか
もこの化学吸着単分子膜は、化合繊繊維フィラメントの
基材と共有結合によって化学結合しているので、耐久性
にも優れ、洗髪や、櫛やブラシで髪をとかすことなどに
よっては剥離しない。According to the above-mentioned constitution of the present invention, since the highly hydrophilic functional group is fixed to the surface of the chemical fiber filament by chemical bond through the chemically adsorbed molecule, it is difficult to be charged. Even if the filament itself is water-repellent and has no sweat absorption property, sweat wets the filament surface, spreads over the entire surface, and evaporates. Moreover, since this monomolecular film has a film thickness on the nanometer level, there is no fear of degrading the original elasticity of the synthetic filament. Further, it does not interfere with the color tone and gloss of the synthetic filament hair. In addition, since this chemically adsorbed monolayer is chemically bonded to the base material of the compound fiber filament by covalent bond, it has excellent durability and does not peel off when washing the hair or combing the hair with a comb or a brush.
【００１０】また前記、化学吸着単分子膜の親水性基
が、−ＯＨ、−ＣＯＯＨ、−ＮＨ2 、−Ｎ+ Ｒ3 Ｘ
- （ただし、Ｒはアルキル基、Ｘはハロゲン原子を示
す）、−ＮＯ 2 、及び−ＳＯ3 Ｈ基から選ばれる少なく
とも一種の官能基であるという本発明の好ましい構成に
よれば、より人毛に近似した感触の繊維表面とすること
ができる。Further, the hydrophilic group of the chemisorption monolayer
Is -OH, -COOH, -NH2, -N+R3X
-(However, R is an alkyl group and X is a halogen atom.
), -NO 2, And -SO3Less selected from H groups
In the preferred constitution of the present invention that both are one kind of functional group
According to this, the fiber surface should have a feel that more closely resembles human hair.
You can
【００１１】また前記化学式１に示す単分子膜であれ
ば、さらに人毛に近似した感触の繊維表面とすることが
できる。Further, the monomolecular film represented by the above chemical formula 1 can provide a fiber surface having a feeling similar to that of human hair.
【００１２】[0012]
【実施例】本発明においては、化合繊繊維フィラメント
として、ナイロン、アクリル、分散染料可染型ポリエス
テル、塩基性可染型ポリエステル、レーヨン、アセテー
ト等を使用することができる。たとえば、ナイロン、ア
クリル、塩基性可染型ポリエステル等のフィラメント表
面にクロロシリル基を分子末端に含む物質、たとえば、
Ａ−（Ｂ）l −ＳｉＸq Ｃｌ3-q （ただし、Ａはブロモ
基、ヨード基、シアノ基、チオシアノ基、クロロシリル
基、またはエステル結合を含む官能基、ｑは０または１
または２、ｌは３０以下の自然数、Ｂ官能基）を混ぜた
非水系溶媒に接触させ、前記フィラメント表面の水酸基
と前記クロロシリル基を分子末端に含む物質のクロロシ
リル基とを反応させて、前記物質を前記フィラメント表
面に析出させる工程と、非水系有機溶媒を用い前記表面
に残った余分なクロロシリル基を複数個含む物質を洗浄
除去した後、前記物質のブロモ基、ヨード基、シアノ
基、チオシアノ基、クロロシリル基、またはエステル結
合を含む官能基を化学反応させて−ＯＨ、−ＣＯＯＨ、
−ＮＨ2 、−Ｎ+ Ｒ3 Ｘ- （Ｘはハロゲン原子を示
す）、−ＮＯ2 、または−ＳＯ3 Ｈ基に変換させる工程
とにより親水性化学吸着単分子膜をフィラメント表面に
形成する。EXAMPLE In the present invention, as the compound fiber filament, nylon, acrylic, disperse dye dyeable polyester, basic dyeable polyester, rayon, acetate or the like can be used. For example, a substance containing a chlorosilyl group at the molecular end on the filament surface of nylon, acrylic, basic dyeable polyester, for example,
A- (B) l -SiX q Cl 3-q (where A is a bromo group, an iodo group, a cyano group, a thiocyano group, a chlorosilyl group, or a functional group containing an ester bond, and q is 0 or 1
Alternatively, 2, 1 is contacted with a non-aqueous solvent in which a natural number of 30 or less and a B functional group) is mixed, and the hydroxyl group on the surface of the filament is reacted with the chlorosilyl group of the substance containing the chlorosilyl group at the molecular end to give the substance. And a step of depositing on the surface of the filament, and after washing and removing a substance containing a plurality of excess chlorosilyl groups remaining on the surface using a non-aqueous organic solvent, a bromo group, an iodo group, a cyano group, and a thiocyano group of the substance. , A chlorosilyl group, or a functional group containing an ester bond is chemically reacted to -OH, -COOH,
-NH 2, -N + R 3 X - (X represents a halogen atom), - NO 2, or by a step of converting the -SO 3 H group to form a hydrophilic chemically adsorbed monomolecular film on the filament surface.
【００１３】本発明に関する人工鬘用合成フィラメント
を親水性化する方法には、化学吸着した単分子膜に親水
性機能を有する官能基として−ＯＨ、−ＣＯＯＨ、−Ｎ
Ｈ2、−Ｎ+ Ｒ3 Ｘ- （Ｒはアルキル基、Ｘはハロゲン
原子を示す）、−ＮＯ2 、または−ＳＯ3 Ｈ基等を導入
する方法がある。The method for making the synthetic filament for artificial wick hydrophilic according to the present invention includes -OH, -COOH, -N as a functional group having a hydrophilic function on the chemically adsorbed monomolecular film.
H 2, -N + R 3 X - (R is an alkyl group, X represents a halogen atom), - NO 2, or a method of introducing a -SO 3 H group.
【００１４】なお本発明は、頭部の髪の部分を全面的に
覆う鬘、同部分的に覆う鬘、ウィッグ、ヘアーピース、
ヘアーネット、もしくはこれらの裏地材、中地材などに
も広く応用できる。According to the present invention, a wig that entirely covers the hair portion of the head, a wig that partially covers the hair portion, a wig, a hair piece,
It can be widely applied to hair nets, lining materials, middle materials and the like.
【００１５】以下具体的実施例を順に説明する。 実施例１（−ＯＨ基の導入） まず、加工の終了したナイロン製合成フィラメント１１
を用意し（図１（ａ））、有機溶媒で洗浄した後、表面
をエステル結合（Ｒ−ＣＯ−ＯＣＨ2 −（Ｒは官能
基））を含む官能基及びクロロシラン基を含む物質を混
ぜた非水系の溶媒、例えば、ＣＨ3 ＯＯＣ（ＣＨ2 ）7
ＳｉＣｌ3 を用い、２wt％程度の濃度で溶かした８０wt
％ｎ−ヘキサデカン（トルエン、キシレン、ジシクロヘ
キシルでもよい）、１２wt％四塩化炭素、８wt％クロロ
ホルム溶液を調整し、前記ガラスを５時間程度浸漬する
と、ナイロンフィラメント表面にはイミノ基１２が多数
含まれているので、エステル結合及びクロロシラン基を
含む物質のＳｉＣｌ基と前記イミノ基が反応し脱塩酸反
応が生じフィラメント表面全面に亘り、下記式（化２）
で示す結合が生成され、エステル結合を含む単分子膜１
３がフィラメント表面と化学結合（共有結合）した状態
でおよそ２０オングストロームの膜厚で形成できた（図
１（ｂ））。Specific embodiments will be described below in order. Example 1 (Introduction of —OH group) First, a nylon-made synthetic filament 11 that has been processed.
Was prepared (FIG. 1 (a)), washed with an organic solvent, and then the surface was mixed with a substance containing a functional group containing an ester bond (R—CO—OCH 2 — (R is a functional group)) and a chlorosilane group. Non-aqueous solvent such as CH 3 OOC (CH 2 ) 7
80 wt% of SiCl 3 dissolved at a concentration of 2 wt%
% N-Hexadecane (toluene, xylene, dicyclohexyl may be used), 12 wt% carbon tetrachloride, 8 wt% chloroform solution were prepared, and when the glass was immersed for about 5 hours, a large number of imino groups 12 were contained on the surface of the nylon filament. Since the SiCl group of the substance containing an ester bond and a chlorosilane group reacts with the imino group to cause a dehydrochlorination reaction, the following formula (Formula 2)
The monolayer 1 containing an ester bond is formed by the bond shown in 1
3 was chemically bonded (covalently bonded) to the filament surface, and could be formed with a film thickness of about 20 Å (FIG. 1 (b)).
【００１６】[0016]
【化２】 [Chemical 2]
【００１７】次に、このフィラメント表面を数wt％のリ
チウムアルミニウムハイドライド（ＬｉＡｌＨ4 ）を含
むエーテル溶液中で室温下で２０分反応させて、末端を
親水性の水酸基に変換し、表面に下記式（化３）で表わ
される単分子膜１４を形成した（図１（ｃ））。Next, the surface of the filament is reacted in an ether solution containing several wt% of lithium aluminum hydride (LiAlH 4 ) at room temperature for 20 minutes to convert the terminal to a hydrophilic hydroxyl group, and the surface of the following formula A monomolecular film 14 represented by (Chemical Formula 3) was formed (FIG. 1C).
【００１８】[0018]
【化３】 [Chemical 3]
【００１９】最後に、この様にして得た親水性化された
フィラメントを用いて人工鬘を加工した。この単分子膜
１４はきわめて強固に表面に化学結合（共有結合）して
いるので洗濯しても全く剥離することがなかった。Finally, an artificial wig was processed using the hydrophilicized filaments thus obtained. Since this monomolecular film 14 was extremely strongly chemically bonded (covalently bonded) to the surface, it was not peeled off at all even when washed.
【００２０】なお、この実施例においては、合成フィラ
メントに吸着を行なったが、加工の終了した人工鬘の状
態で鬘全体に化学吸着膜を形成してもよい。また、他の
方法として、有機溶媒で洗浄した後、吸着試薬としてク
ロロシラン基を複数個持つ物質、例えば、ＳｉＣｌ
4 （ＳｉＨＣｌ3 、Ｃｌ3 ＳｉＯＳｉＣｌ3 やＣｌ3 Ｓ
ｉＯＳｉＣｌ2 ＯＳｉＣｌ3 でもよい）を用いて同様の
化学吸着を行なえば、下記式（化４）で示す結合が生成
され、ＯＨ基を多く含むシロキサン単分子膜が、繊維の
表面と化学結合（共有結合）した状態で、およそ３オン
グストロームの膜厚で形成できた。In this embodiment, the synthetic filament was adsorbed, but a chemically adsorbed film may be formed on the entire wick in the state of the artificial wig which has been processed. As another method, after washing with an organic solvent, a substance having a plurality of chlorosilane groups as an adsorption reagent, for example, SiCl
4 (SiHCl 3 , Cl 3 SiOSiCl 3 and Cl 3 S
iOSiCl 2 OSiCl 3 may also be used) to generate the bond represented by the following formula (Formula 4), and the siloxane monomolecular film containing a large amount of OH groups forms a chemical bond (covalent bond) with the surface of the fiber. In the bonded state, a film having a film thickness of approximately 3 Å could be formed.
【００２１】[0021]
【化４】 [Chemical 4]
【００２２】さらにまた、ＳｉＣｌ3 の化学吸着に浸漬
した後、有機溶剤で洗浄することなく、そのまま水分を
含まない雰囲気中で乾燥させても同様の効果が得られ
た。この場合には、下記式（化５）で表わされる単分子
膜を介してポリシランの薄膜がフィラメント表面に形成
されて同様の親水性が得られた。Furthermore, after soaking in the chemical adsorption of SiCl 3 , without washing with an organic solvent, the same effect can be obtained by drying in an atmosphere containing no water. In this case, a polysilane thin film was formed on the filament surface through the monomolecular film represented by the following formula (Formula 5), and the same hydrophilicity was obtained.
【００２３】[0023]
【化５】 [Chemical 5]
【００２４】実施例２（−ＣＯＯＨ基の導入） 例えば、ポリアクリルフィラメント２１を用意し（図２
（ａ））、よく洗浄した後、エステル結合（Ｒ−ＣＯ−
ＯＣＨ2 −（Ｒは官能基））をもつ官能基とクロロシラ
ン基を含む物質を混ぜた非水系の溶媒、例えば、ＣＨ3
ＯＯＣ（ＣＨ2）10ＳｉＣｌ3 を用い、２wt％程度の濃
度で溶かした８０wt％ｎ−ヘキサデカン（トルエン、キ
シレン、ジシクロヘキシルでもよい）、１２wt％四塩化
炭素、８wt％クロロホルム溶液を調整し、前記基板を５
時間程度浸漬すると、アクリルフィラメント表面には未
反応のカルボキシル基の水酸基２２が多数含まれている
ので、エステル結合及びクロロシラン基を含む物質のＳ
ｉＣｌ基と前記水酸基が反応し脱塩酸反応が生じ表面全
面に亘り、下記式（化６）の結合が生成され、エステル
結合を含む単分子膜２３がフィラメントの表面と化学結
合（共有結合）した状態でおよそ２０オングストローム
の膜厚で形成できた（図２（ｂ））。Example 2 (Introduction of --COOH group) For example, a polyacrylic filament 21 was prepared (see FIG. 2).
(A)), after thorough washing, ester bond (R-CO-
A non-aqueous solvent prepared by mixing a substance containing a chlorosilane group with a functional group having OCH 2 — (R is a functional group), for example, CH 3
The use OOC (CH 2) 10 SiCl 3 , 80wt% dissolved at a concentration of about 2 wt% n-hexadecane (toluene, xylene, or a dicyclohexyl), adjusted 12 wt% carbon tetrachloride, a 8 wt% chloroform solution, the substrate 5
After soaking for about an hour, many unreacted hydroxyl groups 22 of the carboxyl group are contained on the surface of the acrylic filament, so that S of the substance containing the ester bond and the chlorosilane group is contained.
The iCl group and the hydroxyl group react to cause a dehydrochlorination reaction, and a bond of the following formula (Formula 6) is generated over the entire surface, and the monomolecular film 23 containing an ester bond is chemically bonded (covalently bonded) to the surface of the filament. In this state, a film having a thickness of about 20 Å could be formed (FIG. 2 (b)).
【００２５】[0025]
【化６】 [Chemical 6]
【００２６】次に、この表面を塩酸（ＨＣｌ）の３６wt
％溶液中で６５℃で３０分反応させて、下記式化７に示
す末端に親水性のカルボキシル基を形成した。Next, the surface is covered with 36 wt% of hydrochloric acid (HCl).
% Solution at 65 ° C. for 30 minutes to form a hydrophilic carboxyl group at the terminal represented by the following formula (7).
【００２７】[0027]
【化７】 [Chemical 7]
【００２８】なお、この単分子膜２４（図２（ｃ））も
きわめて強固に表面に化学結合（共有結合）しているの
で全く剥離することがなかった。最後に、この様にして
得た親水性化されたフィラメントを用いて人工鬘を加工
した結果、雨天でも型くずれせず、晴天でも全く帯電し
ない人工鬘を製作できた。Since the monomolecular film 24 (FIG. 2 (c)) is also very strongly chemically bonded (covalently bonded) to the surface, it was not peeled at all. Finally, as a result of processing the artificial wig using the hydrophilicized filaments thus obtained, it was possible to manufacture an artificial wig that did not lose its shape even in rainy weather and was not electrically charged even in fine weather.
【００２９】実施例３（−ＮＨ2 基の導入） まず、ナイロンフィラメント３１を用意し（図３
（ａ））シアノ基及びクロロシラン基を含む物質を混ぜ
た非水系の溶媒、例えばＮＣ（ＣＨ2 ）17ＳｉＣｌ3を
用い、１wt％程度の濃度で溶かした８０wt％ｎ−ヘキサ
デカン（トルエン、キシレン、ジシクロヘキシルでもよ
い）、１２wt％四塩化炭素、８wt％クロロホルム溶液を
調整し、前記フィラメントを２時間程度浸漬すると、フ
ィラメント表面にはイミノ基３２が多数含まれているの
で、シアノ基を含む物質のＳｉＣｌ基と前記イミノ基が
反応し脱塩酸反応が生じ表面全面に亘り、下記式化８に
示す結合が生成され、シアノ基を含む単分子膜３３が表
面と化学結合（共有結合）した状態で形成できた（図３
（ｂ））。Example 3 (Introduction of --NH 2 Group) First, a nylon filament 31 was prepared (see FIG. 3).
(A) 80 wt% n-hexadecane (toluene, xylene, dissolved in a concentration of about 1 wt% using a nonaqueous solvent such as NC (CH 2 ) 17 SiCl 3 mixed with a substance containing a cyano group and a chlorosilane group, Dicyclohexyl may be used), 12 wt% carbon tetrachloride, 8 wt% chloroform solution is prepared, and when the filament is immersed for about 2 hours, a large number of imino groups 32 are contained on the filament surface. Group reacts with the imino group to cause a dehydrochlorination reaction, and a bond represented by the following formula 8 is generated over the entire surface to form a monomolecular film 33 containing a cyano group in a chemical bond (covalent bond) with the surface. Done (Fig. 3
(B)).
【００３０】[0030]
【化８】 [Chemical 8]
【００３１】次に、リチウムアルミニウムハイドライド
の溶解したエーテル（１０ｍｇ／ｍｌ）にプレートを浸
漬し、一晩反応させる。その後、溶液から取り出しエー
テル、続いてエーテルと同容量の１０wt％の塩酸を加え
る。その後、さらにトリエチルアミン溶液に入れて、２
時間反応を行わせた後、クロロホルム溶液で洗浄する
と、下記式化９で表わせる親水性の単分子膜を得た。な
お、この単分子膜３３（図３（ｃ））もきわめて強固に
フィラメント表面に化学結合（共有結合）しているので
全く剥離することがなかった。Next, the plate is immersed in ether (10 mg / ml) in which lithium aluminum hydride is dissolved, and the reaction is carried out overnight. Then, the solution was taken out of the solution, and ether was added thereto, followed by the same volume of 10 wt% hydrochloric acid as the ether. Then, add more to the triethylamine solution,
After allowing the reaction to proceed for a period of time, washing with a chloroform solution gave a hydrophilic monomolecular film represented by the following formula (9). The monomolecular film 33 (FIG. 3C) was also extremely strongly chemically bonded (covalently bonded) to the filament surface, so that it was not peeled at all.
【００３２】[0032]
【化９】 [Chemical 9]
【００３３】また、他の−ＮＨ2 基の導入実施例とし
て、次のようなものがある。まず、フィラメントをよく
水洗浄した後、ブロモ基またはヨード基とクロロシラン
基を含む物質を混ぜた非水系の溶媒、例えば、Ｂｒ（Ｃ
Ｈ2 ）17ＳｉＣｌ3を用い、１wt％程度の濃度で溶かし
た８０wt％ｎ−ヘキサデカン（トルエン、キシレン、ジ
シクロヘキシルでもよい）、１２wt％四塩化炭素、８wt
％クロロホルム溶液を調整し、前記フィラメントを２時
間程度浸漬すると、表面にはイミノ基が多数含まれてい
るので、ブロモ基を含む物質のＳｉＣｌ基と前記水酸基
が反応し脱塩酸反応が生じ表面全面に亘り、下記式化１
０の結合が生成され、ブロモ基を含む単分子膜が表面と
化学結合（共有結合）した状態で形成できた。Other examples of introduction of —NH 2 group are as follows. First, after thoroughly washing the filament with water, a non-aqueous solvent, such as Br (C), in which a substance containing a bromo group or an iodo group and a chlorosilane group is mixed.
H 2) with 17 SiCl 3, 80 wt% was dissolved at a concentration of about 1 wt% n-hexadecane (toluene, xylene, or a dicyclohexyl), 12 wt% carbon tetrachloride, 8 wt
% Chloroform solution and soaking the filament for about 2 hours, the surface contains a large number of imino groups, so the SiCl group of the substance containing the bromo group reacts with the hydroxyl group to cause dehydrochlorination reaction and the entire surface Formula 1 below
A bond of 0 was generated, and a monomolecular film containing a bromo group could be formed in a state of being chemically bonded (covalently bonded) to the surface.
【００３４】[0034]
【化１０】 [Chemical 10]
【００３５】次に、ナトリウムアミドの溶解したＮ，Ｎ
ジメチルホルムアミド溶液（８ｍｇ／ｍｌ）にフィラメ
ントを入れ一晩反応を行わせと、下記式化１０で表わせ
る単分子膜を得た。Next, dissolved N, N of sodium amide
The filament was placed in a dimethylformamide solution (8 mg / ml) and reacted overnight to obtain a monomolecular film represented by the following formula 10.
【００３６】[0036]
【化１１】 [Chemical 11]
【００３７】さらに、リチウムアルミニウムハイドライ
ドの溶解したエーテル（１０ｍｇ／ｍｌ）にプレートを
浸漬し、一晩反応させた後取り出し、空の容器に入れ
て、エーテル、続いてエーテルと同容量の１０wt％の塩
酸を加える。その後トリエチルアミン溶液に入れて、２
時間反応を行わせた後、クロロホルム溶液で洗浄する
と、下記式化１２で表わせる水に対する濡れ角度が６０
度の単分子膜を得た。Further, the plate was immersed in ether (10 mg / ml) in which lithium aluminum hydride was dissolved, reacted overnight, taken out, placed in an empty container, and then ether, and then 10 wt% of the same volume as ether. Add hydrochloric acid. Then add it to the triethylamine solution and
After reacting for a period of time and washing with a chloroform solution, the wetting angle to water represented by the following formula 12 is 60.
A monolayer film of a certain degree was obtained.
【００３８】[0038]
【化１２】 [Chemical 12]
【００３９】なお、この単分子膜もきわめて強固にフィ
ラメント表面に化学結合（共有結合）しているので全く
剥離することがなかった。最後に、この様にして得た親
水性化されたフィラメントを用いて人工鬘を加工した結
果、雨天でも型くずれせず、湿度の低い晴天でも全く帯
電しない人工鬘を製作できた。Since this monomolecular film was also extremely strongly chemically bonded (covalently bonded) to the filament surface, it was not peeled at all. Finally, as a result of processing the artificial wig using the hydrophilicized filament thus obtained, it was possible to manufacture an artificial wig that does not lose its shape even in rainy weather and does not become charged at all even in fine weather with low humidity.
【００４０】実施例４（−Ｎ+ Ｒ3 Ｘ- 基（Ｘはハロゲ
ン原子を示す）の導入） まず、塩基性可染型ポリエステルフィラメント４１を用
意し、一端にクロロシラン基及び他の一端にもクロロシ
ラン基を含む物質を混ぜた非水系の溶媒、例えば、Ｃｌ
Ｓｉ（ＣＨ3 ）2 （ＣＨ2 ）10ＳｉＣｌ3 を用い、２wt
％程度の濃度で溶かした８０wt％ｎ−ヘキサデカン（ト
ルエン、キシレン、ジシクロヘキシルでもよい）、１２
wt％四塩化炭素、８wt％クロロホルム溶液を調整し、前
記フィラメント表面４１を５時間程度浸漬すると、フィ
ラメント表面には水酸基４２が含まれているので、一端
にクロロシラン基及び他の一端にもクロロシラン基を含
む物質の一端のＳｉＣｌ基と前記水酸基が反応し脱塩酸
反応が生じフィラメント表面全面に亘り、下記式化１３
の結合が生成され、クロロシラン基を含む単分子膜４３
が表面と化学結合（共有結合）した状態で形成できた
（図４（ｂ））。Example 4 (Introduction of -N + R 3 X - Group (X represents a halogen atom)) First, a basic dyeable polyester filament 41 was prepared, and a chlorosilane group was provided at one end and also at the other end. A non-aqueous solvent mixed with a substance containing a chlorosilane group, for example, Cl
Si (CH 3 ) 2 (CH 2 ) 10 SiCl 3 was used, and 2 wt.
80 wt% n-hexadecane (toluene, xylene, dicyclohexyl may be used) dissolved in a concentration of about 12%, 12
When a wt% carbon tetrachloride, 8 wt% chloroform solution is prepared and the filament surface 41 is immersed for about 5 hours, a hydroxyl group 42 is contained on the filament surface, so that a chlorosilane group at one end and a chlorosilane group at the other end. The SiCl group at one end of the substance containing OH reacts with the hydroxyl group to cause a dehydrochlorination reaction, and the compound represented by the following formula 13
43 is formed and a monolayer 43 containing a chlorosilane group is formed.
Was chemically bonded to the surface (covalent bond) (FIG. 4 (b)).
【００４１】[0041]
【化１３】 [Chemical 13]
【００４２】そこで、１０wt％の（ＣＨ3 ）2 ＮＣ2 Ｈ
4 ＯＨのクロロホルム溶液にフィラメントを浸漬し脱塩
酸反応を生じさせた後、クロロホルムで洗浄すると、下
記式化１４で表わせる単分子膜４４が得られた（図４
（ｃ））。Therefore, 10 wt% of (CH 3 ) 2 NC 2 H
The filament was dipped in a chloroform solution of 4 OH to cause a dehydrochlorination reaction, and then washed with chloroform to obtain a monomolecular film 44 represented by the following formula 14 (FIG. 4).
(C)).
【００４３】[0043]
【化１４】 [Chemical 14]
【００４４】そこで、さらにハロゲン原子としてヨウ素
を含むＣＨ3 Ｉを溶解させたクロロホルム溶液に浸漬し
２時間還流すると、下記式化１５で示される４級アミノ
基を表面に有する水に対する濡れ性のきわめて高いフィ
ラメント４５が得られた（図４（ｄ））。Then, when further immersed in a chloroform solution in which CH 3 I containing iodine as a halogen atom is dissolved and refluxed for 2 hours, the wettability to water having a quaternary amino group represented by the following formula 15 on the surface is extremely high. A high filament 45 was obtained (FIG. 4 (d)).
【００４５】[0045]
【化１５】 [Chemical 15]
【００４６】最後に、この様にして得た親水性化された
フィラメントを用いて人工鬘を加工した結果、雨天でも
型くずれせず、晴天でも全く帯電しない人工鬘を製作で
きた。Finally, the thus-obtained hydrophilic filament was used to process the artificial wig, and as a result, it was possible to manufacture an artificial wig that would not lose its shape even in rainy weather and would not be charged at all even in fine weather.
【００４７】実施例５（−ＮＯ2 基の導入） まず、人工鬘用のナイロンフィラメントを用意し（図５
（ａ））、有機溶媒で洗浄した後、ブロモあるいはヨー
ド基及びクロロシラン基を含む物質を混ぜた非水系の溶
媒、例えば、下記式化１６を用いた。Example 5 (Introduction of --NO 2 group) First, a nylon filament for artificial wig was prepared (FIG. 5).
(A)) After washing with an organic solvent, a nonaqueous solvent in which a substance containing a bromo or iodo group and a chlorosilane group is mixed, for example, the following chemical formula 16 was used.
【００４８】[0048]
【化１６】 [Chemical 16]
【００４９】この化１６の化合物を２wt％程度の濃度で
溶かした８０wt％ｎ−ヘキサデカン（トルエン、キシレ
ン、ジシクロヘキシルでもよい）、１２wt％四塩化炭
素、８wt％クロロホルム溶液を調整し、前記フィラメン
ト表面５１を５時間程度浸漬すると、フィラメント表面
にはイミノ基（−ＮＨ）が多数含まれているので、ブロ
モ基を含む物質のＳｉＣｌ基と前記イミノ基５２が反応
し脱塩酸反応が生じ表面全面に亘り、下記式化１７に示
す結合が生成され、ブロモ基を含む単分子膜５３がフィ
ラメント表面と化学結合（共有結合）した状態でおよそ
２５オングストロームの膜厚で形成できた（図５
（ｂ））。80 wt% n-hexadecane (toluene, xylene, dicyclohexyl may be used), 12 wt% carbon tetrachloride, 8 wt% chloroform solution prepared by dissolving the compound of Chemical formula 16 at a concentration of about 2 wt% were prepared, and the filament surface 51 was prepared. When the filament is immersed for about 5 hours, the filament surface contains a large number of imino groups (-NH). Therefore, the SiCl group of the substance containing a bromo group reacts with the imino group 52 to cause a dehydrochlorination reaction, and the entire surface is covered. The bond shown in Formula 17 below was generated, and the monomolecular film 53 containing a bromo group could be formed with a film thickness of about 25 Å in a state of being chemically bonded (covalently bonded) to the filament surface (FIG. 5).
(B)).
【００５０】[0050]
【化１７】 [Chemical 17]
【００５１】次に、このフィラメント表面を５wt％Ａｇ
ＮＯ3 を含むアルカリ性水溶液中で８０℃、２時間反応
させると、下記式化１８で示される親水性の単分子膜５
４（図５（ｃ））が得られた。Next, the surface of this filament is coated with 5 wt% Ag.
When reacted at 80 ° C. for 2 hours in an alkaline aqueous solution containing NO 3, a hydrophilic monomolecular film 5 represented by the following formula 18 is obtained.
4 (FIG. 5 (c)) was obtained.
【００５２】[0052]
【化１８】 [Chemical 18]
【００５３】最後に、この様にして得た親水性化された
フィラメントを用いて人工鬘を加工した結果、雨天でも
型くずれせず、晴天でも全く帯電しない人工鬘を製作で
きた。Finally, as a result of processing the artificial wig using the thus-hydrophilized filament, it was possible to manufacture an artificial wig that did not lose its shape even in rainy weather and was not electrically charged even in fine weather.
【００５４】実施例６（−ＳＯ3 Ｈ基の導入） まず、人工鬘用のナイロンフィラメントを用意し（図６
（ａ））、有機溶媒で洗浄した後、チオシアノ基（−Ｓ
ＣＮ）及びクロロシラン基を含む物質を混ぜた非水系の
溶媒、例えば、ＮＣＳ（ＣＨ2 ）10ＳｉＣｌ3 を用い、
２wt％程度の濃度で溶かした８０wt％ｎ−ヘキサデカン
（トルエン、キシレン、ジシクロヘキシルでもよい）、
１２wt％四塩化炭素、８wt％クロロホルム溶液を調整
し、前記レンズ６１を５時間程度浸漬すると、表面には
イミノ基６２が多数含まれているので、チオシアノ基及
びクロロシラン基を含む物質のＳｉＣｌ基と前記イミノ
基が反応し脱塩酸反応が生じ表面全面に亘り、下記式化
１９で示される結合が生成され、チオシアノ基を含む単
分子膜６３がフィラメント表面と化学結合（共有結合）
した状態でおよそ２０オングストロームの膜厚で形成で
きた（図６（ｂ））。Example 6 (Introduction of --SO 3 H group) First, a nylon filament for artificial wig was prepared (FIG. 6).
(A)), after washing with an organic solvent, a thiocyano group (-S
CN) and a non-aqueous solvent mixed with a substance containing a chlorosilane group, for example NCS (CH 2 ) 10 SiCl 3 ,
80 wt% n-hexadecane dissolved in a concentration of about 2 wt% (toluene, xylene, dicyclohexyl may be used),
A 12 wt% carbon tetrachloride, 8 wt% chloroform solution was prepared, and when the lens 61 was immersed for about 5 hours, a large number of imino groups 62 were contained on the surface, so that a SiCl group of a substance containing a thiocyano group and a chlorosilane group was formed. The imino group reacts to cause a dehydrochlorination reaction, and a bond represented by the following formula 19 is generated over the entire surface, and the monomolecular film 63 containing a thiocyano group chemically bonds (covalent bond) with the filament surface.
In this state, a film having a thickness of about 20 Å could be formed (FIG. 6B).
【００５５】[0055]
【化１９】 [Chemical 19]
【００５６】次に、リチウムアルミニウムハイドライド
の溶解したエーテル（１０ｍｇ／ｍｌ）にフィラメント
を入れ、４時間反応させると、下記式化２０で示される
親水性の単分子膜６４（図６（ｃ））が得られた。Next, the filament was placed in ether (10 mg / ml) in which lithium aluminum hydride was dissolved and reacted for 4 hours, and a hydrophilic monomolecular film 64 represented by the following formula 20 was obtained (FIG. 6 (c)). was gotten.
【００５７】[0057]
【化２０】 [Chemical 20]
【００５８】次に、１０wt％の過酸化水素水と１０wt％
の酢酸が容量比で１対５の混合溶液中に入れ、４０℃か
ら５０℃の間で３０分反応させると、下記式化２１で示
される親水性の高い単分子膜６５（図６（ｄ））が得ら
れた。Next, 10 wt% hydrogen peroxide solution and 10 wt%
When the acetic acid of 1 was placed in a mixed solution having a volume ratio of 1: 5 and reacted at 40 ° C. to 50 ° C. for 30 minutes, a highly hydrophilic monomolecular film 65 represented by the following formula 21 (see FIG. 6 (d ))was gotten.
【００５９】[0059]
【化２１】 [Chemical 21]
【００６０】最後に、この様にして得た親水性化された
フィラメントを用いて人工鬘を加工した結果、雨天でも
型くずれせず、晴天でも全く帯電しない人工鬘を製作で
きた。Finally, as a result of processing the artificial wig using the hydrophilicized filaments thus obtained, it was possible to manufacture an artificial wig that did not lose its shape even in rainy weather and was not electrically charged even in fine weather.
【００６１】なお、あらかじめクロロシラン基を複数個
含む物質を混ぜた非水系の溶媒、例えば、ＳｉＣｌ4 を
用い、１wt％程度の濃度で溶かした８０wt％ｎ−ヘキサ
デカン（トルエン、キシレン、ジシクロヘキシルでもよ
い）、１２wt％四塩化炭素、８wt％クロロホルム溶液を
調整し、前記フィラメントを１時間程度浸漬し、その後
フレオン系溶剤で洗浄しさらに水洗すると、フィラメン
ト表面には水酸基やイミノ基が含まれているので、表面
に（ＨＯ）3 ＳｉＯ−が形成されて、表面に水酸基が並
んだ状態で多数形成される。この状態でもかなり親水性
が高いが、このＳｉＣｌ4 の化学吸着工程を行なった
後、さらに実施例１〜６をおこなえばシロキサンの単分
子膜を介して親水性の単分子膜をより高密度にフィラメ
ント表面に形成できる。It should be noted that 80 wt% n-hexadecane (toluene, xylene, dicyclohexyl may be used) prepared by mixing a substance containing a plurality of chlorosilane groups in advance with a non-aqueous solvent, for example, SiCl 4 , dissolved at a concentration of about 1 wt%. , 12 wt% carbon tetrachloride, 8 wt% chloroform solution was prepared, the filament was immersed for about 1 hour, then washed with a Freon solvent and further washed with water, because the filament surface contains hydroxyl groups and imino groups. It is (HO) 3 SiO- is formed on the surface, are formed a number in a state aligned hydroxyl on the surface. In this state, the hydrophilic monolayer is still highly hydrophilic, but after carrying out this SiCl 4 chemisorption step, Examples 1 to 6 are carried out to further increase the density of the hydrophilic monolayer through the siloxane monolayer. It can be formed on the filament surface.
【００６２】[0062]
【発明の効果】以上述べてきたように、本願発明の方法
を用いれば、人工鬘用の化合繊繊維フィラメント表面に
化学吸着された分子を介して親水基が化学結合（共有結
合）で固定されたフィラメントを作製できる。従って、
着用時汗をかいても、汗はフィラメント表面を濡らし表
面全面に広がるので蒸れることが無い。また、この膜
は、化学結合（共有結合）でフィラメント表面に固定さ
れているため剥離することもない。しかも、この単分子
膜は、膜厚がナノメーターレベルであるため、フィラメ
ント本来の弾力性や光沢を劣化させるおそれも無い。従
って、型くずれせず櫛通りのよい人工鬘を提供できる。As described above, according to the method of the present invention, the hydrophilic group is fixed by the chemical bond (covalent bond) via the molecule chemically adsorbed on the surface of the synthetic fiber filament for artificial wig. Filaments can be produced. Therefore,
Even if you sweat when you wear it, the sweat does not get damp because it wets the filament surface and spreads over the entire surface. Further, since this film is fixed on the filament surface by a chemical bond (covalent bond), it does not peel off. Moreover, since this monomolecular film has a film thickness on the nanometer level, there is no fear of deteriorating the elasticity and gloss inherent to the filament. Therefore, it is possible to provide an artificial wig that can be easily combed without losing its shape.
【図１】本発明の第１の実施例である人工鬘用ナイロン
フィラメント表面に親水性の単分子膜を形成する工程を
説明するために、フィラメント表面を分子レベルまで拡
大した工程断面図である。FIG. 1 is a process cross-sectional view in which a filament surface is enlarged to a molecular level in order to explain a process of forming a hydrophilic monomolecular film on a surface of a nylon filament for artificial wig according to a first embodiment of the present invention. .
【図２】本発明の第２の実施例である人工鬘用アクリル
フィラメント表面に親水性単分子膜を形成する工程を説
明するために、フィラメント表面を分子レベルまで拡大
した工程断面図である。FIG. 2 is a process cross-sectional view in which the filament surface is enlarged to a molecular level in order to explain the process of forming a hydrophilic monomolecular film on the surface of the acrylic filament for artificial wig according to the second embodiment of the present invention.
【図３】本発明の第３の実施例である人工鬘用ナイロン
フィラメントに親水性単分子膜を形成する工程を説明す
るために、フィラメント表面を分子レベルまで拡大した
工程断面図である。FIG. 3 is a process cross-sectional view in which the filament surface is enlarged to a molecular level in order to explain the process of forming a hydrophilic monomolecular film on the nylon filament for artificial wig according to the third embodiment of the present invention.
【図４】本発明の第４の実施例である人工鬘用塩基性可
染型ポリエステルフィラメント表面に親水性単分子膜を
形成する工程を説明するために、フィラメント表面を分
子レベルまで拡大した工程断面図である。FIG. 4 is a process of expanding a filament surface to a molecular level in order to explain a process of forming a hydrophilic monomolecular film on the surface of a basic dyeable polyester filament for artificial wig, which is a fourth embodiment of the present invention. FIG.
【図５】本発明の第５の実施例である人工鬘用ナイロン
フィラメント表面に親水性単分子膜を形成する工程を説
明するために、フィラメント表面を分子レベルまで拡大
した工程断面図である。FIG. 5 is a process cross-sectional view in which the filament surface is enlarged to a molecular level in order to explain the process of forming a hydrophilic monomolecular film on the surface of the nylon filament for artificial wig according to the fifth embodiment of the present invention.
【図６】本発明の第６の実施例である人工鬘用ナイロン
フィラメント表面に親水性単分子膜を形成する工程を説
明するために、フィラメント表面を分子レベルまで拡大
した工程断面図である。FIG. 6 is a process cross-sectional view in which the filament surface is enlarged to a molecular level in order to explain the process of forming a hydrophilic monomolecular film on the surface of a nylon filament for artificial wig according to the sixth embodiment of the present invention.
１１、３１、５１、６１ 人工鬘用ナイロンフィラメン
ト ２１ 人工鬘用アクリルフィラメント ４１ 人工鬘用塩基性可染型ポリエステル １２、３２、５２、６２ イミノ基 ２２、４２ 水酸基 １３、１４、１５、２３、２４、２５、３３、３４、４
３、４４、４５、５３、５４、６３、６４、６５ 単分
子膜11, 31, 51, 61 Nylon filament for artificial wig 21 Acrylic filament for artificial wig 41 Basic dyeable polyester for artificial wig 12, 32, 52, 62 Imino group 22, 42 Hydroxyl group 13, 14, 15, 23, 24 , 25, 33, 34, 4
3,44,45,53,54,63,64,65 Monolayer
Claims (3)
構成された人工鬘において、前記少なくとも髪の毛の部
分の繊維表面が親水性基を含む化学吸着単分子膜で覆わ
れていることを特徴とする人工鬘。1. An artificial wig in which at least a hair portion is composed of a compound fiber, wherein the fiber surface of at least the hair portion is covered with a chemisorption monomolecular film containing a hydrophilic group. Artificial wig.
Ｈ、−ＣＯＯＨ、−ＮＨ 2 、−Ｎ+ Ｒ3 Ｘ- （ただし、
Ｒはアルキル基、Ｘはハロゲン原子を示す）、−Ｎ
Ｏ2 、及び−ＳＯ3 Ｈ基から選ばれる少なくとも一種の
官能基である請求項１に記載の人口鬘。2. The hydrophilic group of the chemisorption monolayer is -O.
H, -COOH, -NH 2, -N+R3X-(However,
R is an alkyl group, X is a halogen atom), -N
O2, And -SO3At least one selected from H groups
The artificial wig according to claim 1, which is a functional group.
化学式１（ただし、Ａは−ＯＨ、−ＣＯＯＨ、−Ｎ
Ｈ2 、−Ｎ+ Ｒ3 Ｘ- （Ｒはアルキル基、Ｘはハロゲン
原子を示す）、−ＮＯ2 、または−ＳＯ3 Ｈ基、ｌは３
０以下の自然数、Ｂは官能基であっても良いし無くても
よい）で示されるものである請求項１または２に記載の
人口鬘。 【化１】 3. The adsorbed chemisorption monolayer is represented by the following chemical formula 1 (where A is --OH, --COOH, --N).
H 2, -N + R 3 X - (R represents an alkyl group, X is a halogen atom), - NO 2 or -SO 3 H group,, l 3
A natural number less than or equal to 0, and B may or may not be a functional group.) The population of claim 1 or 2. [Chemical 1]
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18214691A JP2921533B2 (en) | 1991-07-23 | 1991-07-23 | Artificial wig |
| EP19920104188 EP0508136B1 (en) | 1991-03-14 | 1992-03-11 | Surface-treated apparel material |
| DE69225743T DE69225743T2 (en) | 1991-03-14 | 1992-03-11 | Surface treated material for clothing |
| KR1019920004216A KR950004492B1 (en) | 1991-03-14 | 1992-03-14 | Surface treated apparel material |
| US08/165,569 US5474839A (en) | 1991-03-14 | 1993-12-13 | Surface-treated apparel material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18214691A JP2921533B2 (en) | 1991-07-23 | 1991-07-23 | Artificial wig |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06200405A true JPH06200405A (en) | 1994-07-19 |
| JP2921533B2 JP2921533B2 (en) | 1999-07-19 |
Family
ID=16113167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18214691A Expired - Lifetime JP2921533B2 (en) | 1991-03-14 | 1991-07-23 | Artificial wig |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2921533B2 (en) |
-
1991
- 1991-07-23 JP JP18214691A patent/JP2921533B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2921533B2 (en) | 1999-07-19 |
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