JPWO2007083672A1 - Fiber treatment agent, fiber treatment method, fiber and fabric treated with this fiber treatment agent - Google Patents
Fiber treatment agent, fiber treatment method, fiber and fabric treated with this fiber treatment agent Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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Abstract
本発明にかかる繊維処理剤は、繊維表面の処理を行う際に用いられる繊維処理剤であって、高分子成分であるＤＮＡ、ＤＮＡ金属塩又はＲＮＡと低分子成分であるデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドの少なくとも1種類（ＤＮＡ及び／又はＲＮＡ等という）と、反応基を有する反応性有機化合物または固着性を有する有機化合物とを含有している。この構成の繊維処理剤により処理を行うと、繊維処理を施した繊維を長期間使用等しても、ＤＮＡ等が取り除かれてしまうことがなく、ＤＮＡ等の有する特性を保つことができるので、耐久性が良く、保湿性、吸水性、吸湿性、制電性、ＵＶカット、創傷治療性、褥瘡予防及び回復並びに肌荒れ防止等を持続的に発現することができる。The fiber treatment agent according to the present invention is a fiber treatment agent used for treating a fiber surface, and is a high molecular component DNA, DNA metal salt or RNA, and a low molecular component deoxyoligonucleotide, deoxymono. It contains at least one kind of nucleotide, oligonucleotide, and mononucleotide (referred to as DNA and / or RNA) and a reactive organic compound having a reactive group or an organic compound having stickiness. When treated with the fiber treatment agent of this configuration, even if the fiber subjected to fiber treatment is used for a long period of time, DNA and the like are not removed, and the characteristics such as DNA can be maintained. Durability is good, and moisture retention, water absorption, moisture absorption, antistatic, UV cut, wound healing, pressure ulcer prevention and recovery, rough skin prevention and the like can be continuously expressed.
Description
本発明は、繊維処理剤、繊維処理方法、この繊維処理剤により処理された繊維および布帛に関する。 The present invention relates to a fiber treatment agent, a fiber treatment method, a fiber and a fabric treated with the fiber treatment agent.
従来、ブラウス、ドレスシャツ、パンツ、スカート、裏地、家具・車両等の座席のシートの表皮材等の繊維を用いた製品が市場に出回っている。
これら繊維製品は、各種用途の違いにより、材料となる繊維に要求される特性が異なっている。これら要求される特性としては、例えば、保湿性、吸水性、吸湿性、制電性等が挙げられる。
例えば、ブラウスの場合には、普段から着るものであるため、汗をかいたりすることが多い。そのため、吸湿性等が要求される。この吸湿性を満足するために、繊維は、種々のものが用いられている。このような用途に適する繊維材料としては、例えば、ナイロン、ポリエステル、アクリル、ポリウレタン等の合成繊維、綿、麻、羊毛等の天然繊維が挙げられ、これらの複合繊維も挙げられる。Conventionally, products using fibers such as skin materials for seats of blouses, dress shirts, pants, skirts, linings, furniture and vehicles, etc. have been on the market.
These fiber products have different characteristics required for the fibers used as a material due to differences in various applications. Examples of these required properties include moisture retention, water absorption, hygroscopicity, and antistatic properties.
For example, in the case of a blouse, since it is usually worn, it often sweats. Therefore, hygroscopicity is required. In order to satisfy this hygroscopicity, various types of fibers are used. Examples of the fiber material suitable for such applications include synthetic fibers such as nylon, polyester, acrylic, and polyurethane, and natural fibers such as cotton, hemp, and wool, and composite fibers thereof.
一方、これらの繊維材料に、特定の繊維処理剤により処理を施すことで、上記の特性を向上させたり、上記の特性の他に、特殊な特性を付与したりすることも試みられている。
このような特定の繊維処理剤としては、例えば、特許文献１に記載のように、架橋剤で処理することで得られた機能性蛋白質と、溶剤系樹脂又は水系樹脂を含む繊維処理材等が知られている。On the other hand, it has been tried to improve the above-mentioned characteristics by giving these fiber materials with a specific fiber treating agent, or to give special characteristics in addition to the above-mentioned characteristics.
As such a specific fiber treatment agent, for example, as described in Patent Document 1, a functional protein obtained by treatment with a crosslinking agent and a fiber treatment material containing a solvent-based resin or a water-based resin, etc. Are known.
しかしながら、特許文献１に記載の技術では、耐久性、保湿性、吸水性、吸湿性、制電性については、機能性蛋白質の特性として発現するものの、創傷治癒性なかんずく肌荒れ防止効果については弱いという問題がある。 However, in the technique described in Patent Document 1, although durability, moisture retention, water absorption, hygroscopicity, and antistatic properties are expressed as characteristics of functional proteins, the wound healing property, particularly, the rough skin prevention effect is weak. There's a problem.
本発明の目的は、耐久性が良く、保湿性、吸水性、吸湿性、制電性といった従来技術に加えて、創傷治癒性、褥瘡予防及び回復、肌荒れ防止並びにＵＶカットを持続的に発現することができる繊維処理剤、繊維処理方法、この繊維処理剤により処理された繊維および布帛を提供することにある。 The object of the present invention is excellent in durability and, in addition to conventional techniques such as moisture retention, water absorption, hygroscopicity, and antistatic, in addition to continuously exhibiting wound healing, pressure ulcer prevention and recovery, rough skin prevention and UV cut. An object of the present invention is to provide a fiber treatment agent, a fiber treatment method, a fiber and a fabric treated with the fiber treatment agent.
本発明の繊維処理剤は、繊維表面の処理を行う際に用いられる繊維処理剤であって、ＤＮＡ、ＤＮＡ金属塩（例えばＫ，Ｃａ，Ｎａ，Ｍｇ等）又はＲＮＡ、ＤＮＡ又はＲＮＡの酵素分解生成物又は加水分解生成物、該分解生成物から分離したデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチド（以下、これらをＤＮＡ及び／又はＲＮＡ等と呼ぶこともある）、或いは前記分解生成物又は前記化合物から選択された少なくとも1種の混合物を含有することを特徴とする。
本発明において、溶媒は繊維処理剤に使用できれば何でも良いが、安全性等から水が最も好ましい。The fiber treatment agent of the present invention is a fiber treatment agent used when treating a fiber surface, and is an enzyme degradation of DNA, DNA metal salt (eg, K, Ca, Na, Mg, etc.) or RNA, DNA or RNA. Products or hydrolysis products, deoxyoligonucleotides, deoxymononucleotides, oligonucleotides, mononucleotides (hereinafter sometimes referred to as DNA and / or RNA) separated from the degradation products, or the degradation products Or at least one mixture selected from the above-mentioned compounds.
In the present invention, any solvent can be used as long as it can be used for the fiber treatment agent, but water is most preferable from the viewpoint of safety.
このような本発明では、高分子の前記ＤＮＡ及び／又はＲＮＡ等を含むため、繊維に保湿性、吸水性、吸湿性、制電性、ＵＶカット効果といった機能を付与することができる。また、低分子のデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドを含むことにより経皮吸収し末梢血流の改善、細胞のＡＴＰ産生を通して、創傷治癒性、褥瘡予防及び回復、肌荒れ防止並びに紫外線の影響の軽減を即効的に発現する。 In the present invention, since the polymer DNA and / or RNA is included, the fiber can be provided with functions such as moisture retention, water absorption, hygroscopicity, antistatic property, and UV cut effect. In addition, low-molecular deoxyoligonucleotides, deoxymononucleotides, oligonucleotides, mononucleotides are absorbed percutaneously to improve peripheral blood flow, cell ATP production, wound healing, pressure ulcer prevention and recovery, rough skin prevention and Immediately expresses the reduction of the effects of ultraviolet rays.
更に、高分子の前記ＤＮＡ及び／又はＲＮＡ等は、皮膚に存在するＤＮＡ分解酵素（ヌクレア−ゼ）またはＲＮＡ分解酵素（リボヌクレアーゼ）により、徐々に分解して低分子のデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドとなることから、創傷治癒性、褥瘡予防及び回復、肌荒れ防止効果並びに紫外線の影響の軽減に持続性を付与することができる。これらの効果があることは、例えば特願２００５−１７２８０６で、デオキシオリゴヌクレオチドなどの分子量が比較的小さいので経皮的に吸収され易く、またそれらは経皮的に吸収されたとき細胞賦活作用及び血行促進作用を有することが知られている。又、最近の研究ではオリゴヌクレオチドを皮膚に塗り経皮吸収させることで、紫外線等に起因する皮膚がんの発生を予防できる事が報告されている（PNAS March 16,2004 vol.101 no.11 3933-3938）。 Furthermore, the high molecular weight DNA and / or RNA is gradually degraded by a DNA degrading enzyme (nuclease) or RNA degrading enzyme (ribonuclease) existing in the skin, so that low molecular deoxyoligonucleotides and deoxymononucleotides are obtained. Since it becomes an oligonucleotide or a mononucleotide, persistence can be imparted to wound healing, pressure ulcer prevention and recovery, rough skin prevention and reduction of the influence of ultraviolet rays. For example, in Japanese Patent Application No. 2005-172806, these effects are easily absorbed percutaneously because the molecular weight of deoxyoligonucleotide or the like is relatively small, and when they are absorbed percutaneously, It is known to have a blood circulation promoting action. In recent studies, it has been reported that the occurrence of skin cancer caused by ultraviolet rays can be prevented by applying an oligonucleotide to the skin and absorbing it percutaneously (PNAS March 16, 2004 vol.101 no.11). 3933-3938).
以下、本発明の繊維処理剤を構成する各成分について説明する。
ヌクレオプロテイン（プロタミン、ＤＮＡ及び／又はＲＮＡからなる）及びＤＮＡは、例えば、魚類の白子から抽出し、精製することにより得ることができる。前記魚類は、例えば、鮭、鱒、鰊及び鱈であり、とりわけ、鮭が好ましい。ＤＮＡについては以下に更に詳しく説明する。
本発明の製造原料であるＤＮＡは種々の態様のものでよく、例えば、二本鎖、一本鎖又は環状のＤＮＡであってよい。ＤＮＡの供給源は、動物、植物、微生物等の様々な生物である。水産加工上の廃棄物である、魚類特に鮭、鱒、鰊及び鱈の精巣（白子）は、とりわけＤＮＡを多く含むが、従来、資源として有効に利用されず、多くが廃棄されていた。それ故、廃棄物の資源化という観点から、これらの精巣由来のＤＮＡを利用することは望ましい。また、哺乳動物や鳥類、例えばウシ、ブタ、ニワトリ等の胸腺から得られるＤＮＡを使用することができる。更に、合成ＤＮＡもまた使用することができる。
ＲＮＡは、例えば、酵母から抽出し、精製することにより得ることができる。Hereinafter, each component which comprises the fiber treatment agent of this invention is demonstrated.
Nucleoprotein (consisting of protamine, DNA and / or RNA) and DNA can be obtained, for example, by extracting and purifying from fish larvae. Examples of the fish include salmon, salmon, salmon and salmon, and salmon is particularly preferable. DNA will be described in more detail below.
The DNA that is the production raw material of the present invention may have various forms, for example, double-stranded, single-stranded or circular DNA. The source of DNA is various organisms such as animals, plants, and microorganisms. Fish, particularly sharks, sharks, sharks, and shark testes (shirako), which are wastes from marine processing, contain a lot of DNA, but they have not been effectively used as resources, and many of them have been discarded. Therefore, it is desirable to use these testis-derived DNA from the viewpoint of recycling waste. In addition, DNA obtained from thymus of mammals and birds, for example, cows, pigs, chickens and the like can be used. In addition, synthetic DNA can also be used.
RNA can be obtained, for example, by extraction from yeast and purification.
ＤＮＡ及び／又はＲＮＡ等を構成する4種の塩基の一部もしくは全部が、他の官能基と反応したものであっても問題ない。そのようにすることで、後述する繊維処理剤の他の成分や繊維との相性を良くしたり、一部疎水基で前記塩基を変性したりすることで、より耐久性のある繊維処理剤を得ることができる。又、ＤＮＡは通常ポリマーであるが、繊維処理剤の溶媒として最も好ましい水に溶解しやすいよう、ＤＮＡの分子量を小さく、必要であればオリゴマーレベルの分子量まで小さくしたものを用いても良い。 There is no problem even if some or all of the four types of bases constituting DNA and / or RNA react with other functional groups. By doing so, it is possible to improve the compatibility with other components and fibers of the fiber treatment agent described later, or to modify the base with a part of the hydrophobic group, thereby making the fiber treatment agent more durable. Obtainable. Further, although DNA is usually a polymer, a DNA having a small molecular weight and, if necessary, a molecular weight at an oligomer level may be used so that it can be easily dissolved in water, which is the most preferable solvent for the fiber treatment agent.
本発明に用いる高分子のＤＮＡ及び／又はＲＮＡは、保湿性、吸水性、吸湿性、制電性といった機能と、徐々に分解してデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドとなり創傷治癒等の機能を発揮する両面性を持つためには、約１０μｍ以下、好ましくは１から10μｍの平均粒径が望ましい。 The high molecular weight DNA and / or RNA used in the present invention has functions such as moisture retention, water absorption, hygroscopicity, and antistatic, and gradually decomposes into deoxyoligonucleotides, deoxymononucleotides, oligonucleotides, and mononucleotides. In order to have double-sided properties that exhibit a function such as healing, an average particle size of about 10 μm or less, preferably 1 to 10 μm, is desirable.
本発明において、前述したＤＮＡ及び／又はＲＮＡ等とともに、他の成分を用いることにより、別の繊維処理剤とすることができる。このような本発明の別の繊維処理剤について以下に説明する。 In this invention, it can be set as another fiber processing agent by using another component with DNA and / or RNA which were mentioned above. Such another fiber treatment agent of the present invention will be described below.
本発明の別の繊維処理剤は、前述したＤＮＡ及び／又はＲＮＡ等と、反応基を有する反応性有機化合物または固着性を有する有機化合物と、を含有することを特徴とする。
このような本発明では、反応基を有する反応性有機化合物を含有することにより、洗濯や摩擦などによる繊維処理剤成分（主にＤＮＡ及び／又はＲＮＡ等）が剥がれることを抑制できる。Another fiber treatment agent of the present invention is characterized by containing the above-described DNA and / or RNA and the like, and a reactive organic compound having a reactive group or an organic compound having adhesiveness.
In such this invention, by containing the reactive organic compound which has a reactive group, it can suppress that the fiber processing agent component (mainly DNA and / or RNA etc.) by washing, friction, etc. peels.
本発明において、前記反応性有機化合物としては、（成分１）分子中に重合可能なビニル基を有する親水性化合物、（成分２）水酸基、カルボキシル基、アミノ基、スルホン酸基、リン酸基を含む単量体、（成分３）エポキシ基を有する親水性化合物、（成分４）アジリジン基を有する化合物として、これらの各成分１〜成分４のうちの少なくともいずれか１つ以上を含むことが好ましい。 In the present invention, the reactive organic compound includes (Component 1) a hydrophilic compound having a vinyl group polymerizable in the molecule, (Component 2) a hydroxyl group, a carboxyl group, an amino group, a sulfonic acid group, and a phosphoric acid group. It is preferable that at least any one of these components 1 to 4 is included as a monomer to be contained, (Component 3) a hydrophilic compound having an epoxy group, and (Component 4) a compound having an aziridine group. .
前記成分１の具体例は、ポリエチレングリコールジアクリレート、ポリエチレングリコールジメタクリレート、ビスフェノールＡポリエチレングリコールジアクリレート、ビスフェノールＡポリエチレングリコールジメタクリレート、ビスフェノールＳポリエチレングリコールジメタクリレート等である。 Specific examples of Component 1 are polyethylene glycol diacrylate, polyethylene glycol dimethacrylate, bisphenol A polyethylene glycol diacrylate, bisphenol A polyethylene glycol dimethacrylate, bisphenol S polyethylene glycol dimethacrylate, and the like.
前記成分２の具体例は、アクリル酸、メタクリル酸、マレイン酸、イタコン酸、アクリルアミド、メタクリルアミド、ビニルスルホン酸、ヒドロキシプロピルメタクリレート等である。
前記成分３の具体例は、ポリエチレングリコールジグリシジルエーテル等である。
前記成分４の具体例は、下記化学式（１）を有する化合物等である。Specific examples of the component 2 include acrylic acid, methacrylic acid, maleic acid, itaconic acid, acrylamide, methacrylamide, vinyl sulfonic acid, hydroxypropyl methacrylate and the like.
Specific examples of the component 3 include polyethylene glycol diglycidyl ether.
Specific examples of the component 4 include compounds having the following chemical formula (1).
このような本発明においては、前述したＤＮＡ及び／又はＲＮＡ等を適当な溶媒、例えば水溶液にしたものと、反応性有機化合物とを調製して繊維処理剤とする。
また、ＤＮＡ及び／又はＲＮＡ等と反応性有機化合物の他に、フィブロイン、セリシン、卵殻膜等の蛋白質、キトサン、セルロース等の多糖類を配合しても良い。これらを配合することで吸湿性の向上の効果が得られる。In the present invention, a fiber treatment agent is prepared by preparing the aforementioned DNA and / or RNA in an appropriate solvent, for example, an aqueous solution, and a reactive organic compound.
In addition to organic compounds reactive with DNA and / or RNA, proteins such as fibroin, sericin and eggshell membranes, and polysaccharides such as chitosan and cellulose may be blended. By blending these, the effect of improving hygroscopicity can be obtained.
このような本発明によれば、反応基を有する反応性有機化合物を含有することにより、繊維処理を施した繊維を長期間使用等しても、繊維からＤＮＡ及び／又はＲＮＡ等が取り除かれてしまうことが抑えられる。従って、洗濯耐久性や摩擦等でもＤＮＡ及び／又はＲＮＡ等が除去されず、保湿性、吸水性、吸湿性、制電性、創傷治療性、褥瘡予防及び回復並びに肌荒れ防止、ＵＶカット効果を持続的に発現することができる繊維処理剤とすることができる。 According to the present invention, by containing a reactive organic compound having a reactive group, DNA and / or RNA and the like are removed from the fiber even if the fiber subjected to fiber treatment is used for a long period of time. It is suppressed. Therefore, DNA and / or RNA is not removed by washing durability or friction, etc., and it maintains moisture retention, water absorption, hygroscopicity, antistatic, wound healing, pressure ulcer prevention and recovery, rough skin prevention, and UV cut effect It can be set as the fiber processing agent which can express expressly.
本発明においては、該繊維処理剤の全量に対して、前記ＤＮＡ及び／又はＲＮＡ等が０．１〜１０質量％含まれ、前記反応性有機化合物が１〜２０質量％含まれていることが好ましい。より好ましくは、前記ＤＮＡ及び／又はＲＮＡが０．２〜５質量％含まれ、前記反応性有機化合物が２〜１０質量％含まれているものとする。 In this invention, 0.1-10 mass% of said DNA and / or RNA, etc. are contained with respect to the whole quantity of this fiber treatment agent, and 1-20 mass% of said reactive organic compounds are contained. preferable. More preferably, the DNA and / or RNA is contained in an amount of 0.2 to 5% by mass, and the reactive organic compound is contained in an amount of 2 to 10% by mass.
ここで、前記ＤＮＡ及び／又はＲＮＡ等が０．１質量％未満であり、前記反応性有機化合物が１質量％未満であると、保湿性等の効果が不十分になる。また、ＤＮＡ及び／又はＲＮＡ等が１０質量％を超え、前記反応性有機化合物が２０質量％を超えると、処理される繊維が固くなる場合がある。 Here, if the DNA and / or RNA is less than 0.1% by mass and the reactive organic compound is less than 1% by mass, effects such as moisture retention become insufficient. Moreover, when DNA and / or RNA etc. exceed 10 mass% and the said reactive organic compound exceeds 20 mass%, the fiber processed may become hard.
本発明の別の繊維処理剤は、前述したＤＮＡ及び／又はＲＮＡ等と、固着性を有する有機化合物と、を含有することを特徴とする。
このような本発明では、固着性を有する有機化合物を含有するため、洗濯や摩擦などによる繊維処理剤成分（主にＤＮＡ）が剥がれることを抑制できる。Another fiber treatment agent of the present invention is characterized by containing the above-described DNA and / or RNA and the like and an organic compound having adhesiveness.
In such this invention, since it contains the organic compound which has adhesiveness, it can suppress that the fiber processing agent component (mainly DNA) by washing | cleaning, friction, etc. peels.
本発明において、前記固着性を有する有機化合物は、いわゆる接着性樹脂としての機能をもち、繊維処理剤の有効成分(主にＤＮＡ及び／又はＲＮＡ等)を繊維に固着させる事が出来れば特に制限はない。
例えば、前述の成分１〜成分４、成分５（イソシアネート及び／又はその前駆体を有する化合物）、アクリル系樹脂、ポリウレタン系樹脂、シリコン系樹脂、シリコン含有アクリル系樹脂の少なくとも一つから選ばれる接着性樹脂であることが好ましい。In the present invention, the organic compound having an adhesive property has a function as a so-called adhesive resin, and is particularly limited as long as an active ingredient (mainly DNA and / or RNA) of the fiber treatment agent can be fixed to the fiber. There is no.
For example, an adhesion selected from at least one of the above-described components 1 to 4, component 5 (compound having isocyanate and / or its precursor), acrylic resin, polyurethane resin, silicon resin, and silicon-containing acrylic resin. Preferably, it is a functional resin.
前記成分１〜成分４は、先に反応性有機化合物として説明した成分１〜成分４と同じであるので、説明を省略する。
前記成分５のうち、イソシアネート基を有する化合物の具体例としては、化学式（ｉ）および（ii）に示されるヘキサメチレンジイソシアネートおよび１，３，５−トリイソシアネート−ｎ−ペンタン等を挙げることができる。Since Component 1 to Component 4 are the same as Component 1 to Component 4 described above as the reactive organic compound, description thereof will be omitted.
Specific examples of the compound having an isocyanate group among the components 5 include hexamethylene diisocyanate and 1,3,5-triisocyanate-n-pentane represented by chemical formulas (i) and (ii). .
また、成分５のうち、イソシアネート基の前駆体を有する化合物の具体例としては、ヘキサメチレンジイソシアネートの前駆体および１，３，５−トリイソシアネート−ｎ−ペンタンの前駆体を挙げることができる。このうち、ヘキサメチレンジイソシアネートの前駆体としては、化学式（iii）および（iv）に示す１，６−ジ（メチルカルバモイル）−ｎ−ヘキサン、１，６−ジ（フェニルカルバモイル）−ｎ−ヘキサンが挙げられる。また、１，３，５−トリイソシアネート−ｎ−ペンタンの前駆体として、化学式（ｖ）に示す化合物を挙げることができる。 Moreover, as a specific example of the compound which has the precursor of an isocyanate group among the components 5, the precursor of hexamethylene diisocyanate and the precursor of 1,3,5-triisocyanate-n-pentane can be mentioned. Among these, as precursors of hexamethylene diisocyanate, 1,6-di (methylcarbamoyl) -n-hexane and 1,6-di (phenylcarbamoyl) -n-hexane represented by chemical formulas (iii) and (iv) are exemplified. Can be mentioned. Moreover, the compound shown to Chemical formula (v) can be mentioned as a precursor of 1,3,5-triisocyanate-n-pentane.
又、他の成分５としては、エーテル系、エステル系、またはカーボネート系のポリウレタンの末端部アミノ基が、メトキシカルボニル基，エトキシカルボニル基，フェノキシカルボニル基，等で化学修飾された構造のカーバメート基を有する、ポリマーまたはオリゴマー（例；第一工業製薬株式会社製のエラストロン（登録商標）またはスーパーフレックス（登録商標））、等も用いることができる。
なお、イソシアネートの修飾基を有する改質剤を用いる場合には、繊維加工における加熱時の修飾基脱離性を高める目的で、炭酸水素ナトリウム等の弱アルカリ塩、および／または有機錫あるいは有機鉛系の触媒を併用しても良い。The other component 5 includes a carbamate group having a structure in which the terminal amino group of an ether, ester, or carbonate polyurethane is chemically modified with a methoxycarbonyl group, an ethoxycarbonyl group, a phenoxycarbonyl group, or the like. A polymer or an oligomer (eg, Elastolon (registered trademark) or Superflex (registered trademark)) manufactured by Daiichi Kogyo Seiyaku Co., Ltd., etc.
When a modifier having an isocyanate modification group is used, a weak alkali salt such as sodium hydrogen carbonate and / or organic tin or organic lead is used for the purpose of enhancing the detachability of the modification group during heating in fiber processing. System catalysts may be used in combination.
本発明の繊維処理剤において、前記固着性を有する有機化合物は、ワックス、シリコン等の親油性化合物および／またはエーテル、アクリル、ウレタン、アミド、エステル等の基を含む高分子化合物としてもよい。
ここで、固着性を有する有機化合物は、反応性はないが、それ自体が適度な親油性または親水性を有し、繊維表面に固着する有機化合物であり、繊維、織物用の柔軟剤、平滑仕上剤、帯電防止剤等に用いられる有機化合物である。具体的には、親油性化合物としては、ワックス、シリコンのほかに、中性油脂、鉱物油および動物蝋等を挙げることができ、また、高分子化合物としては、アクリル系樹脂、ポリウレタン系樹脂、シリコン含有アクリル系樹脂等を挙げることができる。In the fiber treatment agent of the present invention, the organic compound having the sticking property may be a lipophilic compound such as wax and silicon and / or a polymer compound containing a group such as ether, acrylic, urethane, amide, and ester.
Here, the organic compound having adhesiveness is not reactive, but has an appropriate lipophilicity or hydrophilicity per se, and is an organic compound that adheres to the fiber surface. Organic compounds used for finishing agents, antistatic agents and the like. Specifically, examples of the lipophilic compound include neutral oils, mineral oils and animal waxes in addition to wax and silicon, and examples of the polymer compound include acrylic resins, polyurethane resins, Examples thereof include silicon-containing acrylic resins.
本発明によれば、前述したＤＮＡ及び／又はＲＮＡ等をこのような親油性化合物および／または高分子化合物が繊維表面に固着し、繊維内に浸漬されたＤＮＡ及び／又はＲＮＡ等の繊維外への溶出を妨げることができる。このため、前述した反応性有機化合物と同様、繊維処理を施した繊維を長期間使用等してもＤＮＡ及び／又はＲＮＡ等が取り除かれてしまうことを防ぐことができる。 According to the present invention, the above-described lipophilic compound and / or polymer compound adheres to the surface of the fiber such as DNA and / or RNA described above, and out of the fiber such as DNA and / or RNA immersed in the fiber. Can be prevented. For this reason, like the above-mentioned reactive organic compound, it can prevent that DNA and / or RNA etc. are removed even if the fiber which performed fiber treatment is used for a long period of time.
前述した反応性有機化合物あるいは固着性を有する有機化合物によるＤＮＡ及び／又はＲＮＡ等の定着のほか、マイクロカプセル等の機械的手段による定着を図ってもよい。
本発明において、前述したＤＮＡ及び／又はＲＮＡ等は、より洗濯耐久性等を向上させるために、マイクロカプセルの中に、固体状及び／又は溶媒に溶解させて含ませても良い。
このようにすることで、特に水に溶解しやすいＤＮＡ及び／又はＲＮＡ等が繊維外に溶出することを防げるため、耐洗濯耐久性に優れる。In addition to the fixation of DNA and / or RNA by the above-mentioned reactive organic compound or organic compound having adhesiveness, fixation by mechanical means such as microcapsules may be achieved.
In the present invention, the above-described DNA and / or RNA may be contained in a microcapsule in a solid state and / or dissolved in a solvent in order to further improve washing durability and the like.
By doing in this way, it can prevent especially DNA and / or RNA etc. which are easy to melt | dissolve in water to elute out of a fiber, Therefore It is excellent in washing-proof durability.
ＤＮＡ及び／又はＲＮＡ等をマイクロカプセルに含ませるには、種々の方法によりカプセル化できるが、代表として以下１）〜３）の方法を挙げる。 In order to include DNA and / or RNA in a microcapsule, they can be encapsulated by various methods, but representative examples include the methods 1) to 3) below.
１）ＤＮＡ及び／又はＲＮＡ等の粉体を水不溶性の（メタ）アクリル系またはポリウレタン系樹脂で皮膜する方法
ＤＮＡ及び／又はＲＮＡ等（平均粒径：１０μｍ以下）を、水不溶性の（メタ）アクリルモノマー（例；アクリル酸エチル，アクリル酸ブチル，メタクリル酸メチル，アクリル酸，等の単体または混合物）に浸漬し、この混合物を水に分散させる。分散性を高める為に界面活性剤等を添加しても良い。重合開始剤を添加した後に加熱、または紫外線を照射する事で（メタ）アクリルモノマーを重合させ、水不溶性のカプセルを製造する。（メタ）アクリルモノマーの代わりに水不溶性の熱硬化型ポリウレタン樹脂を用いても良い。1) Method of coating powder of DNA and / or RNA with water-insoluble (meth) acrylic or polyurethane resin DNA and / or RNA (average particle size: 10 μm or less) is water-insoluble (meth) It is immersed in an acrylic monomer (eg, simple substance or mixture of ethyl acrylate, butyl acrylate, methyl methacrylate, acrylic acid, etc.), and this mixture is dispersed in water. A surfactant or the like may be added to improve dispersibility. After adding the polymerization initiator, the (meth) acrylic monomer is polymerized by heating or irradiating with ultraviolet rays to produce a water-insoluble capsule. A water-insoluble thermosetting polyurethane resin may be used in place of the (meth) acrylic monomer.
２）ＤＮＡ及び／又はＲＮＡ等水溶液を無機カプセル内に封入する方法
ＤＮＡ及び／又はＲＮＡ等の水溶液に、水溶性（メタ）アクリルモノマー（例；アクリル酸ソーダ塩，（メタ）アクリル酸−２−ヒドロキシエチル，アクリル酸，等の単体または混合物）および重合開始剤を添加し、この水溶液を、細孔を持つシリカゲルまたはゼオライト微粒子に含浸させ、更に水または水／アルコール混合液に分散した後、加熱または紫外線を照射する事で、無機物担持カプセルを製造する。2) Method of enclosing an aqueous solution such as DNA and / or RNA in an inorganic capsule In an aqueous solution such as DNA and / or RNA, a water-soluble (meth) acrylic monomer (eg, sodium acrylate salt, (meth) acrylic acid-2- Hydroxyethyl, acrylic acid, etc. alone or in mixture) and a polymerization initiator are added, this aqueous solution is impregnated into fine silica gel or zeolite fine particles, further dispersed in water or a water / alcohol mixture, and then heated. Or an inorganic substance carrying capsule is manufactured by irradiating with ultraviolet rays.
３）ＤＮＡ及び／又はＲＮＡ等をゼラチンと共にカプセル化する方法
ゼラチンおよびＤＮＡ及び／又はＲＮＡ等（粉体または水溶液）を含む温水（５０〜６０℃）を、同温で疎水性有機溶媒中に分散した後に冷却し、次いで溶媒系にイソプロパノールを滴下することで固化し、濾過後アルデヒドに浸すことで硬化する。3) Method for encapsulating DNA and / or RNA together with gelatin Disperse warm water (50-60 ° C) containing gelatin and DNA and / or RNA (powder or aqueous solution) in a hydrophobic organic solvent at the same temperature. Then, it is cooled, then solidified by adding dropwise isopropanol to the solvent system, and cured by immersion in aldehyde after filtration.
以上に述べた本発明の各繊維処理剤に対し、これを既存の繊維材料に適用することで、本発明の繊維が得られる。
本発明の繊維は、前述した本発明の繊維処理剤により処理されたことを特徴とする。
ここで、繊維としては、例えば、ナイロン、ポリエステル、アクリル、ポリウレタン等の合成繊維、綿、麻、羊毛等の天然繊維が挙げられ、これらの複合繊維も挙げられる。
また、繊維処理剤の処理方法としては、任意の処理方法でよいが、例えば浸漬法、パディング法等を使用できる。浸漬法としては、室温静置法、加熱撹拌法等がある。パディング法としては、パッドドライ法、パッドスチーム法等があるが、反応性有機化合物の場合は、いずれの方法を使用してもよい。The fiber of the present invention can be obtained by applying the fiber treatment agent of the present invention described above to an existing fiber material.
The fiber of the present invention is characterized by being treated with the fiber treatment agent of the present invention described above.
Here, examples of the fiber include synthetic fibers such as nylon, polyester, acrylic, and polyurethane, and natural fibers such as cotton, hemp, and wool, and also include these composite fibers.
Moreover, as a processing method of a fiber processing agent, although arbitrary processing methods may be sufficient, the immersion method, the padding method, etc. can be used, for example. Examples of the dipping method include a room temperature standing method and a heating and stirring method. The padding method includes a pad dry method and a pad steam method, and any method may be used in the case of a reactive organic compound.
更に、公知の電子線、放射線照射装置を用いて、本発明の繊維処理剤を塗布又は含浸させた繊維に、電子線又は放射線を照射させても良い。反応性有機化合物や固着性を有する有機化合物が架橋することで、より強固な皮膜を繊維上に生成することができ、更には、繊維表面に発生したラジカルを起点に架橋することで繊維材料にＤＮＡ及び／又はＲＮＡ等を直接化学結合させることができる。
これらによれば、前述の繊維処理剤により処理されていることにより、耐久性が良く、保湿性、吸水性、吸湿性、制電性、創傷治療性、褥瘡予防及び回復並びに肌荒れ防止、ＵＶカット効果を持続的に発現する繊維とすることができる。Furthermore, you may irradiate an electron beam or a radiation to the fiber which apply | coated or impregnated the fiber treatment agent of this invention using a well-known electron beam and a radiation irradiation apparatus. A reactive organic compound or an organic compound having adhesiveness can be cross-linked to produce a stronger film on the fiber, and further to the fiber material by cross-linking starting from radicals generated on the fiber surface. DNA and / or RNA can be directly chemically bonded.
According to these, by being treated with the above-mentioned fiber treatment agent, durability is good, moisture retention, water absorption, moisture absorption, antistatic, wound healing, pressure ulcer prevention and recovery, rough skin prevention, UV cut It can be set as the fiber which expresses an effect continuously.
このような本発明の繊維を用いることで、本発明の布帛が得られる。
本発明の布帛は、前述した本発明の繊維を２０重量％以上含んで成り、織物，編物，または不織布を有することを特徴とする。
このような布帛においても、前述した繊維あるいは繊維処理剤で説明した各効果を得ることができる。By using such a fiber of the present invention, the fabric of the present invention is obtained.
The fabric of the present invention comprises 20% by weight or more of the fiber of the present invention described above, and has a woven fabric, a knitted fabric, or a nonwoven fabric.
Also in such a fabric, each effect demonstrated with the fiber or fiber processing agent mentioned above can be acquired.
Ｐ…ピーク P ... Peak
以下、実施例および比較例を挙げて、本発明をより具体的に説明する。
［実施例１］
（１-１）抽出、精製したＤＮＡの製造方法：鮭の白子より白子抽出物を以下のように精製した。
１）鮭白子の前処理
鮭白子１０００ｇをとり、血抜き及び水洗を行った。水切りした後３００ｍｌの水を加え、磨砕、攪拌して懸濁液を得た。
２）粉化処理
次に、この懸濁液を濾過し白子の皮等の固形分を取り除いた後、スプレードライヤーで噴霧乾燥し、粉状の物質を得た。Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples.
[Example 1]
(1-1) Method for producing extracted and purified DNA: Shiroko extract was purified from salmon mushroom as follows.
1) Pre-treatment of white silkworm 1000g white silkworm was taken, and blood-bleeding and water washing were performed. After draining, 300 ml of water was added, ground and stirred to obtain a suspension.
2) Powdering treatment Next, the suspension was filtered to remove solids such as white skin, and then spray-dried with a spray dryer to obtain a powdery substance.
３）洗浄及び回収
この粉状の物質をエタノール洗浄して、エタノール可溶物と水分を除き、減圧乾燥し、粉末状物として、白子抽出物１８０ｇを得た。
かくして得られた白子抽出物は淡黄色の粉末であって、その化学的、物理的性質を以下に示す。
核酸含有量： ２５〜５０％
タンパク質含有量： ２５〜６０％
灰分含有量： ５〜１５％
ニンヒドリン反応： 陽性3) Washing and recovery This powdery substance was washed with ethanol to remove ethanol-soluble substances and moisture and dried under reduced pressure to obtain 180 g of a white child extract as a powdery substance.
The white extract thus obtained is a pale yellow powder, and its chemical and physical properties are shown below.
Nucleic acid content: 25-50%
Protein content: 25-60%
Ash content: 5-15%
Ninhydrin reaction: positive
（１−２）オリゴヌクレオチドの製造方法
鮭白子由来のＤＮＡに対して、食品添加物として認可されているヌクレアーゼ［例えば、酵素製剤ヌクレアーゼ「アマノ」（天野製薬社製）］を用いて限定分解を行った。産生したモノヌクレオチドとオリゴヌクレオチドを電気泳動装置で分析して最適条件を決定した。 具体的には、６５℃前後に調整した温水に原料として粉末状ＤＮＡ−Ｎａ塩を用い、撹拌後、更に７０℃に加温し、原料に対してヌクレアーゼ０．２５％を加えて３時間反応させた。次に、８５℃で１０分間加熱してヌクレアーゼを失活させた後、遠心分離し、上澄み液にスプレードライ法を適用して、オリゴヌクレオチドの乾燥粉末を得た。(1-2) Oligonucleotide production method Restricted degradation using nuclease [for example, enzyme preparation nuclease “Amano” (manufactured by Amano Pharmaceutical Co., Ltd.]], which is approved as a food additive, for DNA derived from coconut candy. went. The produced mononucleotide and oligonucleotide were analyzed with an electrophoresis apparatus to determine the optimum conditions. Specifically, using powdered DNA-Na salt as raw material in warm water adjusted to around 65 ° C., after stirring, further heating to 70 ° C., adding nuclease 0.25% to the raw material, and reacting for 3 hours I let you. Next, the nuclease was inactivated by heating at 85 ° C. for 10 minutes, followed by centrifugation, and a spray-drying method was applied to the supernatant to obtain a dried oligonucleotide powder.
（１−３）オリゴヌクレオチドの分析
６５℃前後に調整した温水に原料として鮭白子由来の粉末状ＤＮＡ−Ｎａ塩を投入し、撹拌後、更に７０℃に加温し、原料に対して酵素製剤ヌクレアーゼ「アマノ」（天野製薬社製）を０．０５％加えて３時間反応させた。次に、８５℃で１０分間加熱してヌクレアーゼを失活させた後、ＨＰＬＣ（高速液体クロマトグラフィ）で分析した。その結果を図１に示す。図１に示される通り、矢印Ｐで示されるピーク２６以後がオリゴヌクレオチドの吸収であり、実施例１では３１％がオリゴヌクレオチドの分画であった。(1-3) Analysis of oligonucleotides Powdered DNA-Na salt derived from white coconut is added as raw material to warm water adjusted to around 65 ° C., stirred, and further heated to 70 ° C. Nuclease “Amano” (Amano Pharmaceutical Co., Ltd.) was added at 0.05% and reacted for 3 hours. Next, the nuclease was inactivated by heating at 85 ° C. for 10 minutes, and then analyzed by HPLC (high performance liquid chromatography). The result is shown in FIG. As shown in FIG. 1, the absorption after the peak 26 indicated by the arrow P is the absorption of the oligonucleotide, and in Example 1, 31% was the fraction of the oligonucleotide.
（２）繊維処理剤の製造方法
前記（１）で得た鮭白子より抽出精製したＤＮＡ及びオリゴヌクレオチド（５ｗｔ％）の水溶液と、修飾イソシアネート系反応性改質剤として、第一工業製薬株式会社製のエラストロン（登録商標）Ｆ−２９、および触媒類を以下の配合比で混合した。
＜成分＞ ＜重量％＞
ａ-1）ＤＮＡ-Ｎａ塩（５ｗｔ％）水溶液 ： 1０．００
ａ-2）オリゴヌクレオチド（５ｗｔ％）水溶液 ： 1０．００
ｂ）エラストロン（登録商標）Ｆ−２９ ： ６．６７
（ポリウレタン純分：１５ｗｔ％）
ｃ）炭酸水素ナトリウム ： ０．０６
ｄ）エラストロン（登録商標）ＣＡＴ−２１ ： ０．６０
ｅ）水 ： ７２．６７(2) Manufacturing method of fiber treating agent Daiichi Kogyo Seiyaku Co., Ltd. as an aqueous solution of DNA and oligonucleotide (5 wt%) extracted and purified from the silkworm obtained in (1) above and a modified isocyanate-based reactive modifier Elastron (registered trademark) F-29 manufactured by the company and catalysts were mixed in the following blending ratio.
<Ingredient><Wt%>
a-1) DNA-Na salt (5 wt%) aqueous solution: 10.00
a-2) Oligonucleotide (5 wt%) aqueous solution: 10.00
b) Elastron (registered trademark) F-29: 6.67
(Pure polyurethane: 15wt%)
c) Sodium bicarbonate: 0.06
d) Elastron (registered trademark) CAT-21: 0.60
e) Water: 72.67
（３）繊維処理剤での繊維を処理する方法
２０ｃｍ四方サイズの白色ニット生地（ポリエステル１００％、目付２００ｇ／ｍ2）を基布として、この基布を上記配合の繊維処理剤に浸漬させた。処理後、ロール間圧力が４．０ｋｇ／ｃｍ2のマングル（一方が金属ロール、他方がゴムロールで構成された２本のロール間に対象の布を挿入し、水分を絞り出す装置）で絞り（絞り率：１２４％）、市販の熱風乾燥機で温度を１００℃にて５分間乾燥させ、次いで１７０℃にて２分間加熱した。
加工生地を「ＪＩＳ Ｌ０２１７ １０３法」に準拠した方法で１度洗濯し、熱風乾燥機で１００℃にて５分間乾燥させ、繊維布帛（実施例１）を得た。(3) Method of treating fibers with fiber treatment agent Using a white knitted fabric of 20 cm square size (100% polyester, basis weight 200 g / m 2 ) as a base fabric, the base fabric was immersed in the fiber treatment agent having the above composition. . After the treatment, a mangle with a pressure between the rolls of 4.0 kg / cm 2 (a device that inserts the target cloth between two rolls, one of which is a metal roll and the other is a rubber roll, and squeezes out moisture) (Rate: 124%), the temperature was dried at 100 ° C. for 5 minutes with a commercially available hot air dryer, and then heated at 170 ° C. for 2 minutes.
The processed fabric was washed once by a method according to “JIS L0217 103 method” and dried at 100 ° C. for 5 minutes by a hot air dryer to obtain a fiber fabric (Example 1).
［比較例１］
上記実施例と同一の生地を基布とし、上記実施例１における繊維処理剤の配合から、ａ）のＤＮＡ-Ｎａ塩水溶液：１０．０ｗｔ％及びオリゴヌクレオチド（５ｗｔ％）水溶液
：1０．００ｗｔ％を、水：２０．０ｗｔ％に代えた繊維処理剤を用いた以外は、上記実
施例と同一の条件で加工して、比較例の繊維布帛（比較例１）を得た。
上記実施例および比較例で得た繊維布帛を、「ＪＩＳ Ｌ０２１７ １０３法」に準拠した方法で１０回洗濯した後、熱風乾燥機で１００℃にて５分間乾燥させた。[Comparative Example 1]
Based on the same fabric as in the above Example, the fiber treatment agent formulation in Example 1 above was used, and a) DNA-Na salt aqueous solution: 10.0 wt% and oligonucleotide (5 wt%) aqueous solution: 10.00 wt% Was processed under the same conditions as in the above example except that the fiber treatment agent was used in place of water: 20.0 wt% to obtain a fiber fabric of Comparative Example (Comparative Example 1).
The fiber fabrics obtained in the above examples and comparative examples were washed 10 times by a method based on “JIS L0217 103 method” and then dried at 100 ° C. for 5 minutes by a hot air dryer.
［実施例２及び比較例２］
実施例１および比較例１の方法で得られた繊維布帛を各々の１０回洗濯後の繊維布帛したものをそれぞれ実施例２および比較例２とし、計４種につき、以下の試験を行った。
１）吸湿性試験
２）吸水速度
３）摩擦帯電圧
１）から３）の評価の結果を表１に示す。[Example 2 and Comparative Example 2]
The fiber fabrics obtained by the method of Example 1 and Comparative Example 1 were each subjected to 10 times of laundering and designated as Example 2 and Comparative Example 2, respectively, and the following tests were conducted on a total of four types.
1) Hygroscopicity test 2) Water absorption speed 3) Friction voltage 1) to 3) are shown in Table 1.
４）着用後の人肌の柔軟性および弾性（回復率）試験
前記した実施例１及び比較例１で得られた繊維布帛について、下記の方法により、「肌の柔軟性及び弾性（回復率）」を確認し、比較・評価した。肌の柔軟性及び弾性評価の結果を、表２に示す。4) Softness and elasticity (recovery rate) test of human skin after wearing About the fiber fabric obtained in Example 1 and Comparative Example 1 described above, “softness and elasticity (recovery rate) of skin” by the following method. ”Was confirmed and compared and evaluated. The results of skin softness and elasticity evaluation are shown in Table 2.
肌の柔軟性及び弾性（回復率）：
肌の柔軟性及び弾性（回復率）は、キュートメーター（ＭＰＡ５８０：（株）インテグラル製）を用いて、吸引時、吸引後の肌高さを測定することにより評価した。ここで、吸引前と吸引時の肌高さの差が引っ張り高さ（Ａ）であり、肌の柔軟性を示す指標となる。また、吸引時と吸引後の肌高さの差をＢとすると、ＢとＡの比が肌の弾性（回復率）となり、完全に回復する場合、Ｂ／Ａ＝１となる。Skin softness and elasticity (recovery rate):
The softness and elasticity (recovery rate) of the skin were evaluated by measuring the skin height after suction using a cutometer (MPA580: manufactured by Integral Co., Ltd.). Here, the difference in skin height before and during suction is the tensile height (A), which is an index indicating the flexibility of the skin. Further, if the difference in skin height during suction and after suction is B, the ratio of B and A becomes the elasticity (recovery rate) of the skin, and B / A = 1 when fully recovered.
また、以下の手順により、人の前腕部に試験布帛を接触させた後、各々の部位の皮膚柔軟性及び弾性（回復率）を評価した。
（ｉ）市販の粘着テープを被験者の前腕部の肌に貼り、剥がした後、アセトン／エーテル液で肌荒れを形成させる。
（ii）被験者の前腕部試験部位について、吸引前と吸引時の肌高さの差（Ａ）及び吸引時と吸引後の肌高さの差（Ｂ）を測定する（測定部位の試験前状態の確認）。
（iii）被験者の試験部位に試験布帛（約１ｃｍ×１ｃｍ）を固定し、約８時間、連続
的に皮膚に接触させる。
（iv）上記（iii）を１６日間、毎日繰り返す。
（ｖ）１６日後、キュートメーターを用いて再び測定を行い、試験後（１６日）と試験前（０日）の比率（試験後／試験前）を算出した。同一の繊維布帛につき各ｎ＝５の平均値を算出した。Moreover, after making a test fabric contact a person's forearm part with the following procedures, the skin softness | flexibility and elasticity (recovery rate) of each site | part were evaluated.
(I) A commercially available adhesive tape is applied to the skin of the subject's forearm, peeled off, and then roughened with an acetone / ether solution.
(Ii) For the subject's forearm test site, the skin height difference (A) before and after suction and the skin height difference (B) between and after suction (B) Confirmation).
(Iii) A test fabric (about 1 cm × 1 cm) is fixed to the test site of the subject, and is continuously brought into contact with the skin for about 8 hours.
(Iv) Repeat (iii) above for 16 days every day.
(V) After 16 days, measurement was again performed using a cutometer, and the ratio (after test / before test) between after test (16 days) and before test (0 days) was calculated. Each n = 5 average value was calculated for the same fiber fabric.
実施例１，２及び比較例１，２の試験布帛（約１０ｃｍ×１０ｃｍ）を、ヒト上腕に固定し、１時間後に、レーザードップラー計（オーエーエス株式会社製ＣＤＦ２０００）で血流量を測定した。試験結果の判定は、下記判定基準で行った。
＋＋：試験布帛の固定前に比べ血流量が極めて増加した（著効）
＋ ：試験布帛の固定前に比べ血流量が増加した（有効）
± ：試験布帛の固定前に比べ血流量がやや増加した（やや有効）
− ：試験布帛の固定前に比べ血流量が同等以下であった（無効）
結果を表３に示す。The test fabrics of Examples 1 and 2 and Comparative Examples 1 and 2 (about 10 cm × 10 cm) were fixed to the human upper arm, and after 1 hour, the blood flow was measured with a laser Doppler meter (CDF2000 manufactured by OSS Corporation). The test results were determined according to the following criteria.
++: The blood flow increased significantly compared to before the test fabric was fixed (high effect)
+: Blood flow increased compared to before fixation of test fabric (effective)
±: The blood flow increased slightly compared to before the test fabric was fixed (slightly effective)
−: The blood flow was equal to or less than before fixation of the test fabric (invalid)
The results are shown in Table 3.
血流量測定試験の評価は＋＋［試験布帛の固定前に比べ血流量が極めて増加した（著効）］であるのに対して、比較例の製剤の血流量測定試験の評価は±［試験布帛の固定前に比べ血流量がやや増加した（やや有効）］で有意差があり、ヒトの皮膚から浸透して血流量を著しく増加させることは明らかである。 The evaluation of the blood flow measurement test is ++ [the blood flow is extremely increased compared to before fixing the test fabric (highly effective)], whereas the evaluation of the blood flow measurement test of the comparative preparation is ± [test fabric. There is a significant difference in blood flow slightly increased (somewhat effective) compared to before fixation, and it is clear that it permeates from human skin and significantly increases blood flow.
［実施例３］
（１）繊維処理剤の調整方法
実施例１で得た鮭白子より抽出したＤＮＡ−Ｎａと反応性有機化合物とを配合して繊維処理剤を調整した。
繊維処理剤の各成分の濃度は以下の通り。
ＤＮＡ−Ｎａ水溶液（１０ｗｔ％） ： １０．０ｗｔ％
反応性有機化合物（化学式Ａ） ： ５．０ｗｔ％
反応性有機化合物（化学式Ｂ） ： ０．５％
水 ： ８４．５ｗｔ％[Example 3]
(1) Method for adjusting fiber treating agent A fiber treating agent was prepared by blending DNA-Na extracted from the milk powder obtained in Example 1 and a reactive organic compound.
The concentration of each component of the fiber treatment agent is as follows.
DNA-Na aqueous solution (10 wt%): 10.0 wt%
Reactive organic compound (Chemical formula A): 5.0 wt%
Reactive organic compound (chemical formula B): 0.5%
Water: 84.5wt%
（２）繊維処理剤で繊維を処理する方法
前項の繊維処理剤を２０ｃｍ四方サイズの綿ニット（目付１８４ｇ／ｍ２）に含浸させた後、０．４Ｍｐａのマングルで絞った（絞り率１００％）。この後、熱風乾燥機で５０℃で２０分間予備乾燥させた後、１１０℃で３０分加熱した。加工生地を「ＪＩＳ Ｌ０２１７ １０３法」に準じた方法で１度洗濯した後、乾燥させて繊維布帛を得た。(2) Method of treating fibers with fiber treatment agent After impregnating the fiber treatment agent of the previous item into a 20 cm square size cotton knit (weight per unit area 184 g / m 2 ), the fiber treatment agent was squeezed with a 0.4 Mpa mangle (squeezing rate 100%) ). Thereafter, it was pre-dried at 50 ° C. for 20 minutes with a hot air dryer, and then heated at 110 ° C. for 30 minutes. The processed fabric was washed once by a method according to “JIS L0217 103 method” and then dried to obtain a fiber fabric.
［実施例４］
（１）マイクロカプセルの作製方法
実施例１で得た鮭白子より抽出したＤＮＡ−Ｎａをメチルアルコールに溶解させた後、多孔質シリカ（平均粒径３μｍ、比表面積２５０ｍ２／ｇ）を加えて攪拌した。懸濁液をエバポレーターに移し、攪拌したまま系内を減圧して多孔質シリカの細孔内を脱気しＤＮＡ−Ｎａを含浸させた。その後、４０℃に昇温して徐々に溶媒を留去しＤＮＡ−Ｎａを内包した多孔質シリカのマイクロカプセルを作製した。[Example 4]
(1) Microcapsule production method After dissolving DNA-Na extracted from the milk powder obtained in Example 1 in methyl alcohol, porous silica (average particle size 3 μm, specific surface area 250 m 2 / g) was added. Stir. The suspension was transferred to an evaporator, and the inside of the system was decompressed with stirring to deaerate the pores of the porous silica, and impregnated with DNA-Na. Thereafter, the temperature was raised to 40 ° C., and the solvent was gradually distilled off to prepare microcapsules of porous silica encapsulating DNA-Na.
（２）繊維処理剤の調整方法
前項で調整した５ｗｔ％ＤＮＡ−Ｎａ含有マイクロカプセルを２０ｗｔ％用い、水を７４．５ｗｔ％にした以外は、前述した実施例３（１）と同様の方法で繊維処理剤を調整した。
（３）繊維処理剤で繊維を処理する方法
前項で調整した繊維処理剤を用い、実施例３と同様の方法で、綿ニットを処理した。絞り率は１００％であった。(2) Preparation method of fiber treatment agent The same method as in Example 3 (1) described above except that 20 wt% of the 5 wt% DNA-Na-containing microcapsule prepared in the previous section was used and water was changed to 74.5 wt%. The fiber treatment agent was adjusted.
(3) Method of treating fiber with fiber treating agent Cotton knit was treated in the same manner as in Example 3 using the fiber treating agent prepared in the previous section. The aperture ratio was 100%.
［実施例５］
（１）繊維処理剤の調整法
反応性有機化合物（化学式Ｂ）を使用せず、水を８５．０％とした以外は、実施例３（１）と同様の方法で繊維処理剤を調整した。
（２）繊維処理剤で繊維を処理する方法
前項の繊維処理剤を２０ｃｍ四方サイズの綿ニット（目付１８４ｇ／ｍ２）に含浸させた後，０．４Ｍｐａのマングルで絞った（絞り率１００％）。この綿ニットに照射線量が５０ｋＧｙとなるように電子線を照射し、その後４０℃で２０分維持した。そして、加工生地を「ＪＩＳ Ｌ０２１７ １０３法」に準じた方法で１度洗濯した後、乾燥させて繊維布帛を得た。[Example 5]
(1) Preparation method of fiber treatment agent A fiber treatment agent was prepared in the same manner as in Example 3 (1) except that the reactive organic compound (Chemical Formula B) was not used and water was changed to 85.0%. .
(2) Method of treating fiber with fiber treatment agent After impregnating the fiber treatment agent of the previous section into a 20 cm square size cotton knit (weight per unit area: 184 g / m 2 ), the fiber treatment agent was squeezed with a 0.4 Mpa mangle (squeezing rate 100%) ). This cotton knit was irradiated with an electron beam so that the irradiation dose was 50 kGy, and then maintained at 40 ° C. for 20 minutes. The processed fabric was washed once by a method according to “JIS L0217 103 method” and then dried to obtain a fiber fabric.
［比較例３］
（１）繊維処理剤の調整法
反応性有機化合物（化学式ＡおよびＢ）を使用せず、水を９０．０％とした以外は、実施例３（１）と同様の方法で繊維処理剤を調整した。
（２）繊維処理剤で繊維を処理する方法
前項で調整した繊維処理剤を用い、実施例３（２）と同様の方法で、綿ニットを処理した。絞り率は９５％であった。[Comparative Example 3]
(1) Preparation method of fiber treatment agent The fiber treatment agent was prepared in the same manner as in Example 3 (1) except that the reactive organic compounds (chemical formulas A and B) were not used and water was changed to 90.0%. It was adjusted.
(2) Method of treating fiber with fiber treating agent Cotton knit was treated in the same manner as in Example 3 (2) using the fiber treating agent prepared in the previous section. The drawing rate was 95%.
［測定手順］
実施例１、３、４、５および比較例１で得られた繊維布帛上のＤＮＡ−Ｎａ量を測定した。この際、繊維布帛上のＤＮＡ−Ｎａ量の定量は下記の方法で行った。
ＤＮＡ−Ｎａを加工した繊維布帛１ｇを切り取り、１ｍｏｌ／Ｌの塩酸で１００℃、１時間処理してＤＮＡを加水分解させる。
ＤＮＡ成分の溶出した水溶液を採取し、２６０ｎｍの波長の吸光度を測定する。
そして、別途調整した標準溶液の吸光度から作成した検量線から水溶液中のＤＮＡ濃度を求め、繊維布帛上にあったＤＮＡ量を計算する。
ここで、ＤＮＡ量（ｗｔ％）＝ＤＮＡ重量／加工後の生地重量、とする。
これらの処理の結果を表４に示す。[Measurement procedure]
The amount of DNA-Na on the fiber fabrics obtained in Examples 1, 3, 4, 5 and Comparative Example 1 was measured. At this time, the amount of DNA-Na on the fiber fabric was quantified by the following method.
1 g of fiber fabric processed with DNA-Na is cut out and treated with 1 mol / L hydrochloric acid at 100 ° C. for 1 hour to hydrolyze DNA.
An aqueous solution in which the DNA component is eluted is collected, and the absorbance at a wavelength of 260 nm is measured.
Then, the DNA concentration in the aqueous solution is obtained from a calibration curve prepared from the absorbance of the standard solution separately prepared, and the amount of DNA on the fiber fabric is calculated.
Here, the amount of DNA (wt%) = DNA weight / dough weight after processing.
Table 4 shows the results of these treatments.
本発明によれば、耐久性が良く、保湿性、吸水性、吸湿性、制電性、創傷治療性、ＵＶカット性、褥瘡予防及び回復並びに肌荒れ防止を持続的に発現することができる繊維処理剤、繊維処理方法、この繊維処理剤により処理された繊維および布帛を提供することができる。 According to the present invention, the fiber treatment has good durability and can continuously express moisture retention, water absorption, moisture absorption, antistatic, wound healing, UV cut property, pressure ulcer prevention and recovery, and rough skin prevention. Agent, fiber treatment method, fiber and fabric treated with the fiber treatment agent can be provided.
本発明は、ブラウス、ドレスシャツ、パンツ、スカート、裏地、家具・車両等の座席のシートの表皮材等の繊維に利用することができる。 INDUSTRIAL APPLICABILITY The present invention can be used for a fiber such as a skin material of a seat of a blouse, a dress shirt, pants, a skirt, a lining, furniture, a vehicle or the like.
Claims (12)
ＤＮＡ、ＤＮＡ金属塩又はＲＮＡ、ＤＮＡ又はＲＮＡの酵素分解生成物又は加水分解生成物、該分解生成物から分離したデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチド、或いは前記分解生成物又は前記化合物から選択された少なくとも1種の混合物を含有することを特徴とする繊維処理剤。A fiber treatment agent used when treating the fiber surface,
DNA, DNA metal salt or RNA, enzymatic degradation product or hydrolysis product of DNA or RNA, deoxyoligonucleotide, deoxymononucleotide, oligonucleotide, mononucleotide separated from the degradation product, or the degradation product or the above A fiber treatment agent comprising at least one mixture selected from compounds.
ＤＮＡ、ＤＮＡ金属塩又はＲＮＡ、ＤＮＡ又はＲＮＡの酵素分解生成物又は加水分解生成物、該分解生成物から分離したデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドと、反応基を有する反応性有機化合物とを含有することを特徴とする繊維処理剤。A fiber treatment agent used when treating the fiber surface,
DNA, DNA metal salt or RNA, enzymatic degradation product or hydrolysis product of DNA or RNA, deoxyoligonucleotide, deoxymononucleotide, oligonucleotide, mononucleotide separated from the degradation product, and reactivity having a reactive group A fiber treatment agent comprising an organic compound.
ＤＮＡ、ＤＮＡ金属塩又はＲＮＡ、ＤＮＡ又はＲＮＡの酵素分解生成物又は加水分解生成物、該分解生成物から分離したデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドと、固着性を有する有機化合物とを含有することを特徴とする繊維処理剤。A fiber treatment agent used when treating the fiber surface,
DNA, DNA metal salt or RNA, enzymatic degradation product or hydrolysis product of DNA or RNA, deoxyoligonucleotide, deoxymononucleotide, oligonucleotide, mononucleotide separated from the degradation product, and organic compound having adhesiveness A fiber treatment agent characterized by comprising:
前記反応性有機化合物は、（成分１）分子中に重合可能なビニル基を有する親水性化合物、（成分２）水酸基、カルボキシル基、アミノ基、スルホン酸基、リン酸基を含む単量体、（成分３）エポキシ基を有する親水性化合物、（成分４）アジリジン基を有する化合物として、これらの成分１〜成分４のうち少なくともいずれか１つ以上を含むことを特徴とする繊維処理剤。The fiber treatment agent according to claim 2,
The reactive organic compound includes (Component 1) a hydrophilic compound having a polymerizable vinyl group in the molecule, (Component 2) a monomer containing a hydroxyl group, a carboxyl group, an amino group, a sulfonic acid group, and a phosphate group, (Component 3) A hydrophilic compound having an epoxy group and (Component 4) a compound having an aziridine group, at least one of these components 1 to 4 is included, and a fiber treatment agent characterized by comprising:
該繊維処理剤の全量に対して、前記ＤＮＡ、ＤＮＡ金属塩又はＲＮＡ、ＤＮＡ又はＲＮＡの酵素分解生成物又は加水分解生成物、該分解生成物から分離したデオキシオリゴヌクレオチド、デオキシモノヌクレオチド、オリゴヌクレオチド、モノヌクレオチドは、０．１〜１０質量％含まれ、前記反応性有機化合物は、１〜２０質量％含まれていることを特徴とする繊維処理剤。In the fiber treatment agent according to claim 2 or 4,
The DNA, DNA metal salt or RNA, enzymatic degradation product or hydrolysis product of DNA or RNA, deoxyoligonucleotide, deoxymononucleotide, oligonucleotide separated from the degradation product with respect to the total amount of the fiber treatment agent The fiber treatment agent, wherein 0.1 to 10% by mass of mononucleotide is contained and 1 to 20% by mass of the reactive organic compound is contained.
前記固着性を有する有機化合物は、（成分１）分子中に重合可能なビニル基を有する親水性化合物、（成分２）水酸基、カルボキシル基、アミノ基、スルホン酸基、リン酸基を含む単量体、（成分３）エポキシ基を有する親水性化合物、（成分４）アジリジン基を有する化合物、（成分５）イソシアネート基またはその前駆体を有する化合物、として、これらの成分１〜成分５のうち少なくともいずれか１つ以上を含むことを特徴とする繊維処理剤。In the fiber treatment agent of Claim 3,
The organic compound having adhesiveness is (Component 1) a hydrophilic compound having a vinyl group polymerizable in the molecule, (Component 2) a single amount containing a hydroxyl group, a carboxyl group, an amino group, a sulfonic acid group, and a phosphoric acid group. Body, (component 3) hydrophilic compound having an epoxy group, (component 4) a compound having an aziridine group, (component 5) a compound having an isocyanate group or a precursor thereof, at least of these components 1 to 5 Any one or more, The fiber processing agent characterized by the above-mentioned.
前記固着性を有する有機化合物は、アクリル系樹脂、ポリウレタン系樹脂、シリコン系樹脂、シリコン含有アクリル系樹脂の少なくとも一つから選ばれる接着性樹脂であることを特徴とする繊維処理剤。In the fiber treatment agent of Claim 3,
The fiber treatment agent, wherein the organic compound having adhesiveness is an adhesive resin selected from at least one of an acrylic resin, a polyurethane resin, a silicon resin, and a silicon-containing acrylic resin.
前記固着性を有する有機化合物は、ワックス、シリコン等の親油性化合物および／またはエーテル、アクリル、ウレタン、アミド、エステル等の基を含む高分子化合物であることを特徴とする繊維処理剤。In the fiber treatment agent of Claim 3,
The fiber treatment agent, wherein the organic compound having the sticking property is a lipophilic compound such as wax and silicon and / or a polymer compound containing groups such as ether, acrylic, urethane, amide, and ester.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006013246 | 2006-01-20 | ||
| JP2006013246 | 2006-01-20 | ||
| PCT/JP2007/050613 WO2007083672A1 (en) | 2006-01-20 | 2007-01-17 | Fiber-treating agent, fiber-treating method, fiber and cloth treated with the fiber-treating agent |
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| Publication Number | Publication Date |
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| JPWO2007083672A1 true JPWO2007083672A1 (en) | 2009-06-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| JP2007554927A Pending JPWO2007083672A1 (en) | 2006-01-20 | 2007-01-17 | Fiber treatment agent, fiber treatment method, fiber and fabric treated with this fiber treatment agent |
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| Country | Link |
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| JP (1) | JPWO2007083672A1 (en) |
| KR (1) | KR20080083665A (en) |
| CN (1) | CN101370977A (en) |
| TW (1) | TW200736449A (en) |
| WO (1) | WO2007083672A1 (en) |
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| JP5571557B2 (en) * | 2008-08-11 | 2014-08-13 | 倉敷紡績株式会社 | Method for producing spun yarn |
| TWI446868B (en) * | 2010-07-26 | 2014-08-01 | Hung Jung Liu | A method of planting parts |
| CN102352562A (en) * | 2011-07-29 | 2012-02-15 | 苏州卡奇特纺织有限公司 | Antistatic agent for wool acrylic fabric |
| CN102352563A (en) * | 2011-07-29 | 2012-02-15 | 苏州卡奇特纺织有限公司 | Antistatic agent for cotton fabrics |
| JP7008438B2 (en) * | 2017-07-14 | 2022-02-10 | 信越化学工業株式会社 | Functional agent-containing fiber and its manufacturing method |
| CN112220961B (en) * | 2020-09-14 | 2022-11-04 | 株洲千金药业股份有限公司 | Mattress-proof deodorization chip, puerpera pad and preparation method of mattress-proof deodorization chip |
| CN116005361B (en) * | 2022-12-29 | 2023-07-21 | 东莞盛翔新材料技术有限公司 | Preparation method of cellulose-collagen composite nanofiber membrane |
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| DE69730042T2 (en) * | 1996-04-19 | 2005-07-21 | Idemitsu Kosan Co., Ltd. | Composition and method for treating fibers |
| JP2000270879A (en) * | 1999-03-26 | 2000-10-03 | Mitsubishi Rayon Co Ltd | Nucleic acid-immobilized gel-holding fiber, arranged body of the fiber and section thereof |
| JP2002071693A (en) * | 2000-09-05 | 2002-03-12 | Mitsubishi Rayon Co Ltd | Method of manufacturing nucleic acid bonded fiber |
| JP4752041B2 (en) * | 2004-02-12 | 2011-08-17 | 独立行政法人 国立印刷局 | Anti-counterfeit paper, method for manufacturing the paper, and method for identifying the paper |
-
2007
- 2007-01-17 KR KR1020087017321A patent/KR20080083665A/en not_active Application Discontinuation
- 2007-01-17 WO PCT/JP2007/050613 patent/WO2007083672A1/en active Application Filing
- 2007-01-17 JP JP2007554927A patent/JPWO2007083672A1/en active Pending
- 2007-01-17 CN CNA2007800024023A patent/CN101370977A/en active Pending
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| Publication number | Publication date |
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| KR20080083665A (en) | 2008-09-18 |
| TW200736449A (en) | 2007-10-01 |
| WO2007083672A1 (en) | 2007-07-26 |
| CN101370977A (en) | 2009-02-18 |
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