JP2019019443A - Functional fiber and method for producing the same - Google Patents
Functional fiber and method for producing the same Download PDFInfo
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- JP2019019443A JP2019019443A JP2018134061A JP2018134061A JP2019019443A JP 2019019443 A JP2019019443 A JP 2019019443A JP 2018134061 A JP2018134061 A JP 2018134061A JP 2018134061 A JP2018134061 A JP 2018134061A JP 2019019443 A JP2019019443 A JP 2019019443A
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- fiber
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- weight
- treatment liquid
- component
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Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Description
本発明は、機能性繊維に関し、さらに詳しくは、洗濯後も防ダニおよび防カビの少なくとも一方の機能を有する成分を含有する繊維に関するものである。 The present invention relates to a functional fiber, and more particularly to a fiber containing a component having at least one function of anti-mite and anti-mold even after washing.
従来、綿やポリエステル等の繊維に防ダニや防カビ等の機能を与えるために、繊維と防ダニ剤や防カビ剤とを混合することが行われている。 Conventionally, in order to provide fibers such as cotton and polyester with functions such as anti-mite and anti-mold, mixing of fibers with anti-mite and anti-mold agents has been performed.
しかし、単に繊維と防ダニ剤等とを混合するだけでは、製品に加工した後の洗濯や時間の経過と共に防ダニ剤等の揮散や脱落が起こり、防ダニ機能等が低下するという問題がある。 However, simply mixing the fiber and the mite-proofing agent has the problem that the mite-proofing agent will volatilize or fall off with the lapse of time after washing or after processing into a product, and the mite-proofing function will decrease. .
そこで、上記の問題の改善にあたり、特許文献１には防ダニ剤を樹脂バインダーによって繊維表面に固着させた繊維が開示されている。 Therefore, in order to improve the above problem, Patent Document 1 discloses a fiber in which an acaricide is fixed to a fiber surface with a resin binder.
上記の特許文献１に記載された発明は、従来のものよりも洗濯耐久性を持った防ダニ繊維とすることができるが、洗濯耐久性の点で、まだまだ満足のいくものではない。 The invention described in the above-mentioned Patent Document 1 can be a tick-proof fiber having washing durability more than the conventional one, but is still not satisfactory in terms of washing durability.
したがって、本発明は、このような背景下において、従来よりも洗濯耐久性を持った機能性繊維および、その製造方法の提供を目的とするものである。 Therefore, the present invention aims to provide a functional fiber having durability for washing more than that in the past and a method for producing the same, in such a background.
本発明者らは、従来よりも、洗濯耐久性を有する機能性繊維を得るため鋭意研究を重ねた。その結果、本発明者らは、繊維と防ダニおよび防カビの少なくとも一方の機能を有する成分を含んだ処理液とを接触させた後の乾燥温度および乾燥時間を特定範囲にすることにより所期の目的が達成できることを見いだし、本発明に到達した。 The inventors of the present invention have made extensive studies in order to obtain functional fibers having washing durability. As a result, the present inventors set the drying temperature and drying time after bringing the fibers into contact with the treatment liquid containing a component having at least one of the function of anti-mite and anti-fungus within a specific range. The present invention has been achieved by finding that the above-described object can be achieved.
すなわち本発明は、防ダニおよび防カビの少なくとも一方の機能を有する成分を含有する繊維であって、ＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯処理を１０回繰り返した後の上記成分の合計含有量が繊維重量あたり０．０１重量％以上であることを特徴とする機能性繊維を第１の要旨とする。 That is, the present invention is a fiber containing a component having at least one function of anti-mite and fungus, and the total content of the above-described components after the washing treatment is repeated 10 times according to the G method described in JIS L 1096 A first aspect is a functional fiber characterized in that the amount is 0.01% by weight or more per fiber weight.
また、上記第１の要旨の機能性繊維を製造する方法であって、繊維と防ダニおよび防カビの少なくとも一方の機能を有する成分を含有する処理液とを接触させる工程と、上記処理液と接触した繊維を１００〜１９０℃、０．５〜６０分間乾燥する工程とを有することを特徴とする機能性繊維の製造方法を第２の要旨とする。 Moreover, it is a method for producing the functional fiber according to the first aspect, the step of bringing the fiber into contact with a treatment liquid containing a component having at least one function of anti-mite and fungus, and the treatment liquid, The second gist is a method for producing a functional fiber, comprising the step of drying the contacted fiber at 100 to 190 ° C. for 0.5 to 60 minutes.
本発明は、ＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯処理を１０回繰り返した後の防ダニおよび防カビの少なくとも一方の機能を有する成分の合計含有量が繊維重量あたり０．０１重量％以上の繊維であるため、洗濯耐久性を有する機能性繊維とすることができる。 In the present invention, the total content of components having at least one function of anti-mite and anti-mold after the washing treatment is repeated 10 times according to method G described in JIS L 1096 is 0.01% by weight or more per fiber weight. Therefore, a functional fiber having durability for washing can be obtained.
また、ＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯処理を１０回繰り返した後において、ＪＩＳ Ｌ １９２０記載の侵入阻止法に準じて測定するダニの忌避率が３０％以上である繊維であると、より防ダニ機能を有する機能性繊維とすることができる。 Further, after the washing treatment is repeated 10 times according to the G method described in JIS L 1096, the tick repellent rate measured according to the intrusion prevention method described in JIS L 1920 is 30% or more, It can be set as the functional fiber which has a tick-proof function more.
そして、ＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯処理を１０回繰り返した後において、ＪＩＳ Ｌ １９２１記載の吸収法に準じアオカビを用いて測定する抗カビ活性値が２以上であると、より防カビ機能を有する機能性繊維とすることができる。 And after repeating a washing process 10 times according to G method of JIS L 1096, when the anti-fungal activity value measured using blue mold according to the absorption method of JIS L 1921 is 2 or more, it is more It can be set as the functional fiber which has a mold function.
上記繊維が合成繊維であると、より洗濯耐久性を有する機能性繊維とすることができる。 When the fiber is a synthetic fiber, it can be a functional fiber having more washing durability.
上記繊維の形状が綿状または布帛であると、より洗濯耐久性を有する機能性繊維とすることができる。 When the shape of the fiber is cotton or fabric, a functional fiber having more washing durability can be obtained.
さらに、上記防ダニ機能を有する成分がジカルボン酸エステル系化合物、有機ヨード系化合物、ピレスロイド系化合物、芳香族ケトン系化合物、芳香族カルボン酸系化合物、芳香族エステル系化合物およびフェノール系化合物からなる群から選ばれる少なくとも一つであると、より防ダニ機能を有する繊維とすることができる。 Further, the group having the above-mentioned acaricidal function is composed of a dicarboxylic acid ester compound, an organic iodine compound, a pyrethroid compound, an aromatic ketone compound, an aromatic carboxylic acid compound, an aromatic ester compound, and a phenol compound. If it is at least one selected from the above, it can be made a fiber having a more anti-mite function.
そして、上記繊維が親水性ポリマーを含有すると、防ダニおよび防カビの少なくとも一方の機能を有する成分をより繊維に含有させることができる。 And when the said fiber contains a hydrophilic polymer, the component which has at least one function of a tick prevention and a mold prevention can be made to contain in a fiber more.
また、上記親水性ポリマーを含有する繊維において、さらに浸透促進剤を含有すると防ダニおよび防カビの少なくとも一方の機能を有する成分をより一層繊維に含有させることができる。 Further, in the fiber containing the hydrophilic polymer, when a penetration accelerator is further contained, a component having at least one of an anti-mite function and an anti-mold function can be further contained in the fiber.
上記機能性繊維を製造する方法であって、繊維と防ダニおよび防カビの少なくとも一方の機能を有する成分を含有する処理液とを接触させる工程、上記処理液と接触した繊維を１００〜１９０℃、０．５〜６０分間乾燥する工程を有する繊維の製造方法であると、得られる繊維を、洗濯耐久性を有する機能性繊維とすることができる。 A method for producing the functional fiber, the step of bringing the fiber into contact with a treatment liquid containing a component having at least one function of mite and fungus, and the fiber in contact with the treatment liquid at 100 to 190 ° C. When the fiber production method has a step of drying for 0.5 to 60 minutes, the resulting fiber can be a functional fiber having washing durability.
上記の繊維と防ダニおよび防カビの少なくとも一方の機能を有する成分を含有する処理液とを接触させる工程が、繊維と防ダニおよび防カビの少なくとも一方の機能を有する成分を含有する処理液とを接触させ、接触させた繊維の絞り率を０〜１２０重量％に調整する工程であると、得られる繊維を、より洗濯耐久性を有する機能性繊維とすることができる。 The step of bringing the fiber into contact with a treatment liquid containing a component having at least one function of mite and fungus is a treatment liquid containing a fiber and a component having at least one function of mite and fungus. When the step of adjusting the squeezing rate of the contacted fiber to 0 to 120% by weight is made, the resulting fiber can be made into a functional fiber having more washing durability.
本発明の実施の形態について詳細に説明する。
本発明は、ＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯処理を１０回繰り返した後の防ダニおよび防カビの少なくとも一方の機能を有する成分の合計含有量が繊維重量あたり０．０１重量％以上の機能性繊維である。
Embodiments of the present invention will be described in detail.
In the present invention, the total content of components having at least one function of anti-mite and anti-mold after the washing treatment is repeated 10 times according to method G described in JIS L 1096 is 0.01% by weight or more per fiber weight. Functional fiber.
本発明において、機能性繊維とは、例えば、防ダニ、撥水、撥油、防汚、親水、防しわ、防縮、風合い、柔軟、縫製性向上、平滑、スリップ防止、つや出し、つや消し、消臭、起毛、難燃、帯電防止、抗菌、抗生物等の機能を少なくとも一つ有する繊維を意味する。 In the present invention, functional fibers are, for example, mite-proof, water-repellent, oil-repellent, anti-fouling, hydrophilic, anti-wrinkle, anti-shrink, texture, softness, improved sewing, smoothness, anti-slip, gloss, matte, deodorant It means a fiber having at least one function such as raising, flame retardant, antistatic, antibacterial and antibiotics.
つぎに本発明の繊維について説明する。 Next, the fiber of the present invention will be described.
＜繊維＞
本発明の繊維の種類としては、特に限定されず、例えば、綿、麻等の植物繊維、絹、羊毛等の動物繊維等の天然繊維、ポリエステル繊維、アクリル繊維、アクリル系繊維、ナイロン繊維、ビニロン繊維、ポリプロピレン繊維、ポリ塩化ビニル繊維、ポリエチレン繊維、ビニリデン繊維、ポリウレタン繊維、アラミド繊維、ポリアリレート系繊維、ポリ−パラフェニレンベンゾビスオキサゾール繊維、エチレンビニルアルコール繊維、アクリレート系繊維、ポリ乳酸等の合成繊維、アセテート繊維、トリアセテート繊維、プロミックス等の半合成繊維、レーヨン繊維、ポリノジック繊維、キュプラ繊維、リヨセル繊維等の再生繊維、ガラス繊維、金属繊維、炭素繊維等の無機繊維等の化学繊維を用いることができる。なかでも合成繊維が好ましく、より好ましくはポリエステル繊維である。また、これらの繊維は、２種類以上を交撚、混紡、混繊、交織等されていてもよい。
<Fiber>
The type of fiber of the present invention is not particularly limited. For example, natural fibers such as plant fibers such as cotton and hemp, animal fibers such as silk and wool, polyester fibers, acrylic fibers, acrylic fibers, nylon fibers, and vinylon. Synthesis of fiber, polypropylene fiber, polyvinyl chloride fiber, polyethylene fiber, vinylidene fiber, polyurethane fiber, aramid fiber, polyarylate fiber, poly-paraphenylenebenzobisoxazole fiber, ethylene vinyl alcohol fiber, acrylate fiber, polylactic acid, etc. Semi-synthetic fibers such as fiber, acetate fiber, triacetate fiber, promix, etc., recycled fiber such as rayon fiber, polynosic fiber, cupra fiber, lyocell fiber, etc., chemical fiber such as inorganic fiber such as glass fiber, metal fiber, carbon fiber, etc. be able to. Of these, synthetic fibers are preferable, and polyester fibers are more preferable. In addition, these fibers may be knitted, blended, blended, or woven in two or more types.
本発明の好適な繊維である合成繊維は、スパン、フィラメントのいずれでもよく、また、繊維の断面形状は、特に限定されず、丸形、三角、中空、六角、扁平等のいずれの断面形状であってもよい。さらに、合成繊維の太さは、通常１０００デシテックス以下、好ましくは５００デシテックス以下、より好ましくは２００デシテックス以下である。 The synthetic fiber, which is a preferred fiber of the present invention, may be either a span or a filament, and the cross-sectional shape of the fiber is not particularly limited, and may be any cross-sectional shape such as round, triangular, hollow, hexagonal, flat, etc. There may be. Furthermore, the thickness of the synthetic fiber is usually 1000 dtex or less, preferably 500 dtex or less, more preferably 200 dtex or less.
また、上記繊維の形状は、特に限定されず、例えば、綿状、布帛、編物、不織布および糸等があげられる。なかでも寝具の中綿、クッション材等に用いる綿状または布帛が好ましい。 Moreover, the shape of the said fiber is not specifically limited, For example, cotton shape, a fabric, a knitted fabric, a nonwoven fabric, a thread | yarn etc. are mention | raise | lifted. Of these, cotton-like or cloth used for fillings, cushioning materials and the like of bedding is preferable.
＜処理剤組成物＞
本発明で用いる防ダニ機能を有する成分、防カビ機能を有する成分は、通常、上記成分と任意成分とを含有する処理剤組成物として用いられる。そして、この処理剤組成物は、通常、水等の溶媒に分散もしくは溶解させた処理液として繊維の処理に供せられる。以下、処理剤組成物に含まれる各成分について説明する。まず、本発明で用いる防ダニ機能を有する成分について説明する。
<Treatment agent composition>
The component having an anti-mite function and the component having an anti-fungal function used in the present invention are usually used as a treating agent composition containing the above components and optional components. And this processing agent composition is normally used for the process of a fiber as a processing liquid disperse | distributed or dissolved in solvents, such as water. Hereinafter, each component contained in the treating agent composition will be described. First, components having an anti-mite function used in the present invention will be described.
〔防ダニ機能を有する成分〕
上記防ダニ機能を有する成分としては、例えば、セバシン酸ジブチル、セバシン酸ジイソプロピル、ドデカン二酸ジブチル等のジカルボン酸エステル系化合物、３−ヨード−２−プロピニルブチルカーバメート等の有機ヨード系化合物、フェノトリン等のピレスロイド系化合物、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテル、ベンゾイン、ベンゾイル安息香酸メチル、ヒドロキシメトキシベンゾフェノン、２−ヒドロキシベンゾフェノン等の芳香族ケトン系化合物、サリチル酸ベンジル、パラオキシ安息香酸ブチル、サリチル酸フェニル、安息香酸ベンジル、安息香酸フェニル等の芳香族エステル系化合物、イソプロピルメチルフェノール等のフェノール系化合物等があげられる。これらの化合物は、単独で、もしくは２種類以上併せて用いることができる。これらのなかでも、ジカルボン酸エステル系化合物および有機ヨード系化合物が好ましく、より好ましくはセバシン酸ジブチル、３−ヨード−２−プロピニルブチルカーバメートであり、特には、セバシン酸ジブチルと３−ヨード−２−プロピニルブチルカーバメートとを併用することが好ましい。
[Ingredients having anti-mite function]
Examples of the component having an anti-mite function include dicarboxylic acid ester compounds such as dibutyl sebacate, diisopropyl sebacate and dibutyl dodecanedioate, organic iodo compounds such as 3-iodo-2-propynyl butyl carbamate, phenothrin and the like. Pyrethroid compounds, benzoin ethyl ether, benzoin isopropyl ether, benzoin, aromatic ketone compounds such as methyl benzoylbenzoate, hydroxymethoxybenzophenone, 2-hydroxybenzophenone, benzyl salicylate, butyl paraoxybenzoate, phenyl salicylate, benzyl benzoate And aromatic ester compounds such as phenyl benzoate, and phenol compounds such as isopropylmethylphenol. These compounds can be used alone or in combination of two or more. Among these, dicarboxylic acid ester compounds and organic iodo compounds are preferable, more preferably dibutyl sebacate and 3-iodo-2-propynylbutyl carbamate, and particularly dibutyl sebacate and 3-iodo-2- It is preferable to use propynylbutyl carbamate in combination.
処理剤組成物における防ダニ機能を有する成分の含有量は、通常、１０〜９０重量％、好ましくは１５〜８０重量％、特に好ましくは２０〜７０重量％である。防ダニ機能を有する成分の含有量が低すぎると、充分な防ダニ機能が得られない傾向があり、防ダニ機能を有する成分の含有量が多すぎると、処理液とした際の溶解性に劣る傾向がある。 Content of the component which has an anti-mite function in a processing agent composition is 10 to 90 weight% normally, Preferably it is 15 to 80 weight%, Most preferably, it is 20 to 70 weight%. If the content of the component having an anti-mite function is too low, there is a tendency that sufficient anti-mite function is not obtained, and if the content of the component having an anti-mite function is too much, the solubility when used as a treatment liquid is increased. There is a tendency to be inferior.
〔防カビ機能を有する成分〕
上記防カビ機能を有する成分としては、例えば、３−ヨード−２−プロピニルブチルカーバメート等の有機ヨード系化合物、２−クロロ−６−トリクロロメチルピリジン、２−クロロ−４−トリクロロメチル−６−メトキシピリジン、２−クロロ−４−トリクロロメチル−６−（２−フリルメトキシ）ピリジン、ジ（４−クロロフェニル）ピリジルメタノール、２，３，５−トリクロロ−４−（ｎ−プロピルスルフォニル）ピリジン、ジンクピリチオン等のピリジン系化合物等があげられる。これらの化合物は、単独で、もしくは２種類以上併せて用いることができる。これらのなかでも、有機ヨード系化合物が好ましく、特に好ましくは３−ヨード−２−プロピニルブチルカーバメートである。
[Ingredients having antifungal function]
Examples of the component having an antifungal function include organic iodine compounds such as 3-iodo-2-propynylbutylcarbamate, 2-chloro-6-trichloromethylpyridine, 2-chloro-4-trichloromethyl-6-methoxy. Pyridine, 2-chloro-4-trichloromethyl-6- (2-furylmethoxy) pyridine, di (4-chlorophenyl) pyridylmethanol, 2,3,5-trichloro-4- (n-propylsulfonyl) pyridine, zinc pyrithione, etc. And pyridine compounds. These compounds can be used alone or in combination of two or more. Among these, an organic iodo compound is preferable, and 3-iodo-2-propynylbutyl carbamate is particularly preferable.
処理剤組成物における防カビ機能を有する成分の含有量は、通常、１０〜９０重量％、好ましくは１５〜８０重量％、特に好ましくは２０〜７０重量％である。防カビ機能を有する成分の含有量が低すぎると、充分な防カビ機能が得られない傾向があり、防カビ機能を有する成分の含有量が多すぎると、処理液とした際の溶解性に劣る傾向がある。 The content of the component having an antifungal function in the treatment composition is usually 10 to 90% by weight, preferably 15 to 80% by weight, and particularly preferably 20 to 70% by weight. If the content of the component having an antifungal function is too low, there is a tendency that a sufficient antifungal function is not obtained, and if the content of the component having an antifungal function is too large, the solubility when used as a treatment liquid is increased. There is a tendency to be inferior.
〔界面活性剤〕
上記防ダニおよび防カビの少なくとも一方の機能を有する成分（以下、「機能性成分」と称する。）を含む処理剤組成物は、前述のとおり、通常、水等の溶媒に分散もしくは溶解させた処理液として用いるが、上記機能性成分の多くは、疎水性物質である。そのため、溶媒への分散性を高めるため処理剤組成物に界面活性剤を配合することが好ましい。
[Surfactant]
As described above, the treatment agent composition containing a component having the function of at least one of the above-mentioned mite-proofing and mold-proofing (hereinafter referred to as “functional component”) is usually dispersed or dissolved in a solvent such as water. Although used as a treatment liquid, many of the functional components are hydrophobic substances. Therefore, it is preferable to add a surfactant to the treating agent composition in order to improve the dispersibility in a solvent.
上記界面活性剤としては、アニオン界面活性剤、カチオン界面活性剤、両性イオン界面活性剤等のイオン性界面活性剤、非イオン性界面活性剤があげられる。 Examples of the surfactant include ionic surfactants such as anionic surfactants, cationic surfactants, and zwitterionic surfactants, and nonionic surfactants.
上記アニオン界面活性剤としては、例えば、脂肪酸石鹸、ポリオキシエチレン（以下、「ＰＯＥ」と称する。）アルキルエーテルカルボン酸塩等のカルボン酸塩類、アルキルベンゼンスルホン酸塩、アルキルナフタレンスルホン酸塩、スルホコハク酸塩、ＰＯＥアルキルスルホコハク酸塩等のスルホン酸塩類、アルキル硫酸塩、ＰＯＥアルキルアリルエーテル硫酸塩等の硫酸エステル類、ＰＯＥアルキルアリルエーテルリン酸塩等のリン酸エステル類等があげられる。 Examples of the anionic surfactant include fatty acid soaps, carboxylates such as polyoxyethylene (hereinafter referred to as “POE”) alkyl ether carboxylates, alkylbenzene sulfonates, alkylnaphthalene sulfonates, and sulfosuccinic acids. Salts, sulfonates such as POE alkyl sulfosuccinate, sulfates such as alkyl sulfates and POE alkyl allyl ether sulfates, phosphate esters such as POE alkyl allyl ether phosphates, and the like.
上記カチオン界面活性剤としては、例えば、脂肪族アミン塩、脂肪族４級アンモニウム塩、塩化ベンザルコニウム塩等があげられる。 Examples of the cationic surfactant include aliphatic amine salts, aliphatic quaternary ammonium salts, benzalkonium chloride salts, and the like.
上記両性イオン界面活性剤としては、例えば、カルボキシベタイン等があげられる。 Examples of the zwitterionic surfactant include carboxybetaine.
上記非イオン性界面活性剤としては、例えば、ＰＯＥアルキルエーテル、ＰＯＥアルキル多環エーテル、ＰＯＥ多環フェニルエーテル、ＰＯＥラノリン誘導体等のＰＯＥ付加型エーテル類、ＰＯＥグリセリン脂肪酸エステル、ＰＯＥヒマシ油エーテル、ＰＯＥ硬化ヒマシ油エーテル、ＰＯＥソルビタン脂肪酸エステル等のＰＯＥ付加型エステルエーテル類、ＰＯＥ脂肪酸エステル、ポリグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル、プロピレングリコール脂肪酸エステル、しょ糖脂肪酸エステル等のエステル類等があげられる。 Examples of the nonionic surfactant include POE addition ethers such as POE alkyl ether, POE alkyl polycyclic ether, POE polycyclic phenyl ether, POE lanolin derivative, POE glycerin fatty acid ester, POE castor oil ether, POE. POE addition-type ester ethers such as hydrogenated castor oil ether and POE sorbitan fatty acid ester, esters such as POE fatty acid ester, polyglycerin fatty acid ester, sorbitan fatty acid ester, propylene glycol fatty acid ester, and sucrose fatty acid ester.
上記界面活性剤のなかでも、上記機能性成分に対して、少量の界面活性剤量で乳化安定性が高く、皮膚刺激が少なく、安全性に優れている点で、非イオン性界面活性剤が好ましく、より好ましくはＰＯＥ付加型エーテル類およびＰＯＥ付加型エステルエーテル類であり、特に好ましくはＰＯＥ多環フェニルエーテル、ＰＯＥヒマシ油エーテル、ＰＯＥ硬化ヒマシ油エーテル、ＰＯＥソルビタン脂肪酸エステルである。また、上記界面活性剤は、単独でもしくは２種以上併せて用いることができる。 Among the above surfactants, the nonionic surfactant is a non-ionic surfactant in that it has high emulsification stability with a small amount of surfactant, less skin irritation, and excellent safety with respect to the functional component. POE addition-type ethers and POE addition-type ester ethers are preferable, and POE polycyclic phenyl ether, POE castor oil ether, POE hydrogenated castor oil ether, and POE sorbitan fatty acid ester are particularly preferable. Moreover, the said surfactant can be used individually or in combination of 2 or more types.
処理剤組成物における界面活性剤の含有量は、通常、１０〜９０重量％、好ましくは２０〜８５重量％、特に好ましくは３０〜８０重量％である。界面活性剤の含有量が低すぎると、処理液中で機能性成分が分離しやすくなる傾向があり、界面活性剤の含有量が多すぎると、機能性成分を含有させた後の繊維に汚れが付着しやすくなる傾向がある。また、界面活性剤の含有量が多すぎると、処理剤組成物における機能性成分の割合が相対的に少なくなるため、処理剤組成物の必要量が増えコスト高になる傾向があり、さらに処理液調製時の撹拌の際に泡立ちによりハンドリングが悪化する傾向がある。 The content of the surfactant in the treatment agent composition is usually 10 to 90% by weight, preferably 20 to 85% by weight, particularly preferably 30 to 80% by weight. If the surfactant content is too low, the functional components tend to be separated in the treatment liquid, and if the surfactant content is too high, the fibers after the functional components are contained are stained. Tends to adhere. In addition, if the surfactant content is too high, the proportion of the functional component in the treatment composition is relatively small, and therefore the necessary amount of the treatment composition tends to increase and the cost tends to increase. There is a tendency for handling to deteriorate due to foaming during stirring during liquid preparation.
また、機能性成分と界面活性剤の配合割合は、機能性成分１００重量部に対し、界面活性剤が１０〜９００重量部、好ましくは１５〜４００重量部、特に好ましくは２０〜２００重量部である。 The mixing ratio of the functional component and the surfactant is 10 to 900 parts by weight, preferably 15 to 400 parts by weight, particularly preferably 20 to 200 parts by weight, based on 100 parts by weight of the functional component. is there.
〔親水性ポリマー〕
本発明で用いる処理剤組成物には、繊維に機能性成分をより多く含有させるために、親水性ポリマーを配合することが好ましい。
[Hydrophilic polymer]
In the treatment agent composition used in the present invention, a hydrophilic polymer is preferably blended so that the fiber contains more functional components.
上記親水性ポリマーとしては、例えば、ポリアクリル酸ナトリウム等のアクリル酸系ポリマー、ヒドロキシエチルセルロース、ヒドロキシメチルセルロース、ヒドロキシプロピルセルロース、カルボキシメチルセルロース、メチルセルロース等のセルロース誘導体、ローカストビーンガム、グアガム、ペクチン、ジェランガム、キサンタンガム、プルラン、カラギーナン、デキストラン、アルギン酸ナトリウム等の多糖類等があげられる。これらは単独でもしくは２種以上併せて用いることができる。これらのなかでも好ましくはアクリル酸系ポリマーおよび多糖類であり、特に好ましくはポリアクリル酸ナトリウム、キサンタンガムである。 Examples of the hydrophilic polymer include acrylic acid-based polymers such as sodium polyacrylate, cellulose derivatives such as hydroxyethyl cellulose, hydroxymethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, and methyl cellulose, locust bean gum, guar gum, pectin, gellan gum, and xanthan gum. And polysaccharides such as pullulan, carrageenan, dextran, and sodium alginate. These may be used alone or in combination of two or more. Of these, acrylic acid polymers and polysaccharides are preferable, and sodium polyacrylate and xanthan gum are particularly preferable.
処理剤組成物における親水性ポリマーの含有量は、通常、０．５〜２０重量％、好ましくは１〜１０重量％、特に好ましくは２〜５重量％である。親水性ポリマーの含有量が低すぎると、効果が充分に得られない傾向があり、親水性ポリマーの含有量が高すぎると機能性成分を含有させた後の繊維の生地の風合いを損ねる傾向がある。 The content of the hydrophilic polymer in the treatment agent composition is usually 0.5 to 20% by weight, preferably 1 to 10% by weight, particularly preferably 2 to 5% by weight. If the content of the hydrophilic polymer is too low, the effect tends not to be sufficiently obtained, and if the content of the hydrophilic polymer is too high, the texture of the fiber fabric after containing the functional component tends to be impaired. is there.
また、機能性成分と親水性ポリマーの配合割合は、機能性成分１００重量部に対し、親水性ポリマー０．１〜５０重量部が好ましく、さらに好ましくは０．５〜２０重量部、特に好ましくは１〜５重量部である。 Further, the blending ratio of the functional component and the hydrophilic polymer is preferably 0.1 to 50 parts by weight, more preferably 0.5 to 20 parts by weight, particularly preferably 100 parts by weight of the functional component. 1 to 5 parts by weight.
親水性ポリマーの効果の理由については、定かではないが、親水性ポリマーの保湿効果により、後記で説明する乾燥工程における水の蒸発を緩やかにし、機能性成分と水との共沸を抑制するため、あるいは親水性ポリマーと機能性成分との間に水素結合等の相互作用があり、物理的に機能性成分の気化を抑制しているためと推察される。 The reason for the effect of the hydrophilic polymer is not clear, but due to the moisturizing effect of the hydrophilic polymer, the evaporation of water in the drying process described later is moderated, and the azeotropy of the functional component and water is suppressed. Alternatively, it is presumed that there is an interaction such as hydrogen bonding between the hydrophilic polymer and the functional component, and the vaporization of the functional component is physically suppressed.
〔浸透促進剤〕
また、上記処理剤組成物に親水性ポリマーを配合する場合は、さらに浸透促進剤を配合することが好ましい。親水性ポリマーと浸透促進剤とを併用することにより、機能性成分の繊維への含有量をより増加させることができる。
[Penetration enhancer]
Moreover, when mix | blending a hydrophilic polymer with the said processing agent composition, it is preferable to mix | blend a penetration enhancer further. By using a hydrophilic polymer and a penetration enhancer in combination, the content of the functional component in the fiber can be further increased.
上記浸透促進剤としては、安息香酸、安息香酸メチル、安息香酸エチル、安息香酸プロピル、安息香酸ブチル、安息香酸ベンジル、安息香酸フェニル等の安息香酸化合物、ｏ−フェニルフェノール、サリチル酸フェニル、１，３，５−トリクロロベンゼン、アニソール、グアヤコール、フタルイミド等の芳香族化合物があげられる。これらは単独でもしくは２種以上併せて用いることができる。これらのなかでも、安息香酸化合物が好ましく、安息香酸および安息香酸ベンジルがより好ましい。なお、上記の浸透促進剤として記載されている化合物を防ダニ機能を有する成分として用いる場合は、浸透促進剤に含めないものとする。 Examples of the penetration enhancer include benzoic acid compounds such as benzoic acid, methyl benzoate, ethyl benzoate, propyl benzoate, butyl benzoate, benzyl benzoate, phenyl benzoate, o-phenylphenol, phenyl salicylate, 1,3 , 5-trichlorobenzene, anisole, guaiacol, phthalimide and the like. These may be used alone or in combination of two or more. Among these, benzoic acid compounds are preferable, and benzoic acid and benzyl benzoate are more preferable. In addition, when using the compound described as said penetration enhancer as a component which has a tick prevention function, it shall not be included in a penetration enhancer.
処理剤組成物における浸透促進剤の含有量は、通常、１〜５０重量％、好ましくは５〜３０重量％、特に好ましくは１０〜２０重量％である。浸透促進剤の含有量が低すぎると、効果が減退する傾向があり、浸透促進剤の含有量が多すぎるとコストが高くなる傾向があり、また、機能性成分を含有させた後の繊維の生地の風合いを損ねる傾向がある。 The content of the penetration enhancer in the treatment agent composition is usually 1 to 50% by weight, preferably 5 to 30% by weight, particularly preferably 10 to 20% by weight. If the content of the penetration enhancer is too low, the effect tends to decrease, and if the content of the penetration enhancer is too large, the cost tends to increase, and the fiber after the functional component is contained There is a tendency to damage the texture of the fabric.
また、機能性成分と浸透促進剤の配合割合は、機能性成分１００重量部に対し、浸透促進剤が１〜５００重量部、好ましくは１０〜２００重量部、特に好ましくは２０〜１００重量部である。 The blending ratio of the functional component and the penetration enhancer is 1 to 500 parts by weight, preferably 10 to 200 parts by weight, particularly preferably 20 to 100 parts by weight, based on 100 parts by weight of the functional component. is there.
さらに、上記処理剤組成物には、本発明の効果を阻害しない範囲で、必要に応じて、溶剤、香料、着色料、防腐剤、殺虫剤等の任意成分を配合してもよい。 Furthermore, you may mix | blend arbitrary components, such as a solvent, a fragrance | flavor, a coloring agent, an antiseptic | preservative, and an insecticide, with the said processing agent composition in the range which does not inhibit the effect of this invention.
上記溶剤としては、例えば、エタノール、フェノキシエタノール、プロピレングリコール、１，３−ブチレングリコール、フェニルジグリコール、ソルビトール等があげられる。 Examples of the solvent include ethanol, phenoxyethanol, propylene glycol, 1,3-butylene glycol, phenyl diglycol, sorbitol, and the like.
本発明で用いる処理剤組成物は、上記機能性成分、必要に応じて界面活性剤、親水性ポリマー、浸透促進剤および、その他の任意成分をミキサー等で均一に混合することにより得ることができる。 The treatment agent composition used in the present invention can be obtained by uniformly mixing the functional component, if necessary, a surfactant, a hydrophilic polymer, a penetration enhancer, and other optional components with a mixer or the like. .
＜処理液＞
上記処理剤組成物は、通常、下記の溶媒に分散もしくは溶解させ処理液とした状態で用いられる。なお、上記処理剤組成物の各成分は、上記処理液とする前に、全て混合しておいてもよいし、溶媒中に各成分を同時、もしくは順次添加して混合してもよい。また、任意の成分を溶媒に分散もしくは溶解させた溶液同士を混合して処理液としてもよい。
<Processing liquid>
The treatment agent composition is usually used in a state of being treated or dispersed in the following solvent. In addition, each component of the said processing agent composition may be all mixed before making it into the said processing liquid, and you may add each component in a solvent simultaneously or sequentially, and may mix. Alternatively, a solution obtained by dispersing or dissolving an arbitrary component in a solvent may be mixed to obtain a treatment liquid.
上記、処理剤組成物を分散もしくは溶解させる溶媒としては、通常、水が用いられる。また、必要に応じて、メタノール、エタノール、プロパノール等の炭素数１〜４の低級アルコールを用いてもよい。これらは、単独でもしくは２種類以上併せて用いることができる。 As the solvent for dispersing or dissolving the treatment agent composition, water is usually used. Moreover, you may use C1-C4 lower alcohols, such as methanol, ethanol, and propanol, as needed. These can be used alone or in combination of two or more.
処理液における処理剤組成物の含有量は、機能性成分や用いる繊維によっても異なるが、通常０．５〜５０重量％であり、好ましくは０．５〜２０重量％である。 Although content of the processing agent composition in a processing liquid changes with functional components and the fiber to be used, it is 0.5-50 weight% normally, Preferably it is 0.5-20 weight%.
上記処理液の調製方法としては、特に制限はなく、公知一般の方法を採用することができる。例えば、上記溶媒と処理剤組成物とを配合し、ミキサー等で撹拌しながら必要に応じて加熱することにより処理液を得ることができる。 There is no restriction | limiting in particular as a preparation method of the said processing liquid, A well-known general method is employable. For example, the treatment liquid can be obtained by blending the solvent and the treatment agent composition and heating as necessary while stirring with a mixer or the like.
上記処理液調製のために加熱する場合、その処理液の温度は、通常２５〜９０℃であり、好ましくは３０〜８５℃である。処理液の温度が高すぎると機能性成分が蒸発・昇華する傾向があり、温度が低すぎると処理剤組成物が溶解しにくくなる傾向がある。 When heating for the preparation of the treatment liquid, the temperature of the treatment liquid is usually 25 to 90 ° C, preferably 30 to 85 ° C. If the temperature of the treatment liquid is too high, the functional component tends to evaporate and sublime, and if the temperature is too low, the treatment composition tends to be difficult to dissolve.
また、加熱時間は、処理剤組成物の各成分が溶解できればよく、通常１２０分間以下、好ましくは２０〜４０分間である。 Moreover, the heating time should just melt | dissolve each component of a processing agent composition, and is 120 minutes or less normally, Preferably it is 20 to 40 minutes.
上記加熱方法としては、特に制限はなく、蒸気や電気ヒーター等の公知の方法を用いることができる。 There is no restriction | limiting in particular as said heating method, Well-known methods, such as a vapor | steam and an electric heater, can be used.
このようにして、本発明で用いる機能性成分を含有する処理液を調製することができる。次に、上記の処理液を用い本発明の機能性成分を含有する繊維を製造する方法について詳細に説明する。 Thus, the process liquid containing the functional component used by this invention can be prepared. Next, a method for producing a fiber containing the functional component of the present invention using the above treatment liquid will be described in detail.
＜機能性繊維の製造方法＞
本発明の機能性成分を含有する繊維は、繊維と機能性成分を含有する処理液とを接触させる工程、上記処理液と接触した繊維を１００〜１９０℃、０．５〜６０分間乾燥する工程を経ることにより得ることができる。以下、各工程について詳述する。
<Method for producing functional fiber>
The fiber containing the functional component of the present invention is a step of bringing the fiber and the treatment liquid containing the functional component into contact, and a step of drying the fiber in contact with the treatment liquid at 100 to 190 ° C. for 0.5 to 60 minutes. It can obtain by going through. Hereinafter, each process is explained in full detail.
上記繊維と機能性成分を含有する処理液とを接触させる方法としては、特に限定されないが、例えば、ローラー塗布、浸漬、シャワー、スプレー、ディッピング等の方法があげられる。なかでも繊維の形状が布帛である場合は、浸漬が好ましく、繊維の形状が綿状である場合は、スプレーが好ましい。 The method for bringing the fiber into contact with the treatment liquid containing the functional component is not particularly limited, and examples thereof include roller coating, dipping, showering, spraying, and dipping. In particular, when the fiber shape is a fabric, dipping is preferable, and when the fiber shape is cotton, spray is preferable.
以下、好適な接触方法である浸漬とスプレーを例にとって説明する。まず接触方法が浸漬の場合について説明する。 In the following, description will be given by taking dipping and spraying, which are preferable contact methods, as an example. First, the case where the contact method is immersion will be described.
繊維に処理液を浸漬させる際の処理液の温度は、通常１０〜６０℃、好ましくは１５〜５０℃、より好ましくは２０〜４０℃である。処理液の温度が低すぎると、充分な量の機能性成分を繊維に含有させることができなくなる傾向があり、処理液の温度が高すぎると、機能性成分が蒸発または昇華しやすくなる傾向がある。 The temperature of the treatment liquid at the time of immersing the treatment liquid in the fiber is usually 10 to 60 ° C, preferably 15 to 50 ° C, more preferably 20 to 40 ° C. If the temperature of the treatment liquid is too low, there is a tendency that a sufficient amount of the functional component cannot be contained in the fiber. If the temperature of the treatment liquid is too high, the functional component tends to evaporate or sublimate. is there.
処理液に浸漬することにより機能性成分を含んだ処理液含有繊維は、絞り率を調整することが好ましい。すなわち、処理液含有繊維の絞り率を特定の範囲に調整することにより、機能性成分の含有率を多くすることができ、より洗濯耐久性を有する機能性繊維とすることができる。絞り率を調整する方法としては、特に限定されず、エアー脱水、遠心脱水、マングル脱水、自然乾燥等を用いることができる。なかでもマングル脱水が好ましい。 It is preferable to adjust the drawing ratio of the treatment liquid-containing fiber containing the functional component by dipping in the treatment liquid. That is, by adjusting the drawing rate of the treatment liquid-containing fiber to a specific range, the content rate of the functional component can be increased, and the functional fiber having more washing durability can be obtained. The method for adjusting the drawing ratio is not particularly limited, and air dehydration, centrifugal dehydration, mangle dehydration, natural drying, and the like can be used. Of these, mangle dehydration is preferred.
上記絞り率調整後の繊維の絞り率は、通常０〜１２０重量％、好ましくは３０〜１１０重量％、より好ましくは５０〜１００重量％である。絞り率が上記範囲外であると充分な量の機能性成分を繊維に含有させることができなくなる傾向がある。上記の理由として、水分が少なすぎる場合は、機能性成分が繊維内部に移行する前に蒸発するためと推察される。また、水分が多すぎる場合は、気化熱により繊維の温度が充分に上がらない、あるいは機能性成分の濃度が希薄化することで繊維外からの内部への濃度勾配差による移動が起こらないためと推察される。 The draw ratio of the fiber after adjusting the draw ratio is usually 0 to 120% by weight, preferably 30 to 110% by weight, and more preferably 50 to 100% by weight. When the drawing ratio is outside the above range, there is a tendency that a sufficient amount of the functional component cannot be contained in the fiber. As the above reason, it is presumed that when the water content is too small, the functional component evaporates before moving into the fiber. Also, if there is too much moisture, the temperature of the fiber will not rise sufficiently due to the heat of vaporization, or the concentration of the functional component will dilute and movement due to the concentration gradient difference from the outside of the fiber will not occur. Inferred.
なお、本発明において絞り率とは、処理液と接触前の繊維の重量に対する、処理液と接触後の繊維が有する処理液重量の割合をいい、具体的には、下記の式（１）により求めることができる。
［式］
絞り率（重量％）＝｛（処理液と接触後の繊維の重量−処理液と接触前の繊維の重量）／処理液と接触前の繊維の重量｝×１００ ・・・（１）
In the present invention, the squeezing ratio refers to the ratio of the weight of the treatment liquid possessed by the fiber after contact with the treatment liquid to the weight of the fiber before contact with the treatment liquid, and specifically by the following formula (1). Can be sought.
[formula]
Drawing ratio (% by weight) = {(weight of fiber after contact with treatment liquid−weight of fiber before contact with treatment liquid) / weight of fiber before contact with treatment liquid} × 100 (1)
次に接触方法がスプレーの場合について説明する。 Next, the case where the contact method is spray will be described.
処理液を繊維にスプレーする際の処理液の噴霧量は、通常、繊維重量の５〜５０重量％であり、好ましくは５〜４０重量％、特に好ましくは５〜３０重量％である。処理液の噴霧量が少なすぎても多すぎても、充分な量の機能性成分を繊維に含有させることができなくなる傾向がある。 The spray amount of the treatment liquid when the treatment liquid is sprayed on the fibers is usually 5 to 50% by weight, preferably 5 to 40% by weight, and particularly preferably 5 to 30% by weight of the fiber weight. If the spray amount of the treatment liquid is too small or too large, there is a tendency that a sufficient amount of the functional component cannot be contained in the fiber.
上記処理液を繊維にスプレーする際の処理液の温度は、通常１０〜６０℃、好ましくは３０〜５０℃である。処理液の温度が低すぎると、粘度が高くなり作業性が悪くなる傾向があり、処理液の温度が高すぎると機能性成分が蒸発・昇華する傾向がある。 The temperature of the treatment liquid when the treatment liquid is sprayed on the fibers is usually 10 to 60 ° C, preferably 30 to 50 ° C. If the temperature of the treatment liquid is too low, the viscosity tends to be high and workability tends to be poor. If the temperature of the treatment liquid is too high, the functional component tends to evaporate and sublime.
上記では、浸漬およびスプレーによる接触方法の例を説明したが、上記の他の接触方法であっても適宜上記の条件に準じて、繊維と処理液とを接触させることにより、浸漬またはスプレーの場合と同様の機能を有する繊維とすることができる。 In the above, the example of the contact method by dipping and spraying has been described. However, even in the case of the other contact methods described above, by appropriately contacting the fiber and the treatment liquid according to the above conditions, in the case of dipping or spraying It can be set as the fiber which has the function similar to.
次に上記処理液と接触した後の繊維は、その後乾燥工程に供される。この乾燥工程において、特定範囲の温度および時間で乾燥することが本発明の製造方法の特徴である。繊維を特定範囲の温度および時間で乾燥させることにより、洗濯耐久性を有する機能性繊維とすることができる。 Next, the fiber after coming into contact with the treatment liquid is then subjected to a drying step. In this drying step, it is a feature of the production method of the present invention to dry at a specific range of temperature and time. By drying the fiber at a specific range of temperature and time, a functional fiber having washing durability can be obtained.
上記乾燥温度としては、通常１００〜１９０℃、好ましくは１３０〜１８５℃より好ましくは１４０〜１８０℃である。乾燥温度が低すぎると洗濯耐久性に劣る傾向があり、乾燥温度が高すぎると機能性成分の含有量が少なくなり、また、繊維が劣化する傾向がある。 As said drying temperature, it is 100-190 degreeC normally, Preferably it is 130-185 degreeC, More preferably, it is 140-180 degreeC. If the drying temperature is too low, the washing durability tends to be inferior. If the drying temperature is too high, the content of the functional component tends to decrease, and the fibers tend to deteriorate.
また、処理剤組成物に親水性ポリマーおよび浸透促進剤を配合する場合の乾燥温度は、１７０〜１９０℃が好ましい。浸透促進剤がその効果を奏するには１７０℃以上の温度が必要であるが、機能性成分は熱に弱く蒸発・昇華しやすいため１７０℃以上の温度を加えると、機能性成分の繊維への含有量は減少する。しかし、親水性ポリマーと浸透促進剤とを併用することにより、親水性ポリマーが機能性成分の気化を防ぎ、さらに浸透促進剤の機能により、機能性成分の繊維への含有量を増加させることができる。 Moreover, as for the drying temperature in the case of mix | blending a hydrophilic polymer and a penetration enhancer with a processing agent composition, 170-190 degreeC is preferable. A temperature of 170 ° C. or higher is necessary for the penetration enhancer to exert its effect. However, when the functional component is weak against heat and easily evaporates and sublimates, if a temperature of 170 ° C. or higher is applied, the functional component is added to the fiber The content is reduced. However, when a hydrophilic polymer and a penetration enhancer are used in combination, the hydrophilic polymer prevents vaporization of the functional component, and the function of the penetration enhancer further increases the content of the functional component in the fiber. it can.
上記乾燥時間は、通常０．５〜６０分間、好ましくは１〜３０分間、より好ましくは１〜２０分間である。乾燥時間が短すぎると洗濯耐久性に劣る傾向があり、乾燥時間が長すぎると機能性成分の含有量が少なくなる傾向があり、また、作業時間がかかりすぎるため実用的ではない。 The drying time is usually 0.5 to 60 minutes, preferably 1 to 30 minutes, more preferably 1 to 20 minutes. If the drying time is too short, the washing durability tends to be inferior, and if the drying time is too long, the content of the functional component tends to decrease, and it takes too much work time, which is not practical.
なかでも、繊維の形状が綿状である場合の乾燥時間は、１〜６０分間が好ましく、より好ましくは１〜２０分間、特に好ましくは１〜１５分間である。 Especially, the drying time when the fiber shape is cottony is preferably 1 to 60 minutes, more preferably 1 to 20 minutes, and particularly preferably 1 to 15 minutes.
また、繊維の形状が布帛である場合の乾燥時間は、１〜５分間が好ましく、より好ましくは１〜３分間、特に好ましくは１〜２分間である。 The drying time when the fiber shape is a fabric is preferably 1 to 5 minutes, more preferably 1 to 3 minutes, and particularly preferably 1 to 2 minutes.
上記乾燥方法としては、特に限定されず、熱風乾燥、シリンダー乾燥、オーブン等を用いることができる。 It does not specifically limit as said drying method, Hot air drying, cylinder drying, oven, etc. can be used.
上記乾燥温度および時間で繊維を乾燥させることによって、繊維に機能性成分を強固に吸着させることができ、洗濯耐久性を有する機能性繊維とすることができる。 By drying the fiber at the above drying temperature and time, the functional component can be firmly adsorbed to the fiber, and a functional fiber having washing durability can be obtained.
一般的に常温下の繊維、特に合成繊維は密度が高いため、単に機能性成分を含有する処理液と繊維とを接触させるだけでは繊維内部に機能性成分が浸透することはなく、洗濯によって容易に脱落する。それに対し、本発明の製造方法で機能性成分を付着させ、加熱することにより、繊維分子の熱運動により生じた分子間隙に機能性成分を浸透させることが可能になる。したがって、内部に導入された機能性成分は繊維と強く固着し洗濯後も残留すると考えられる。 In general, fibers at room temperature, especially synthetic fibers, have a high density, so simply contacting the treatment liquid containing the functional ingredients with the fibers does not allow the functional ingredients to penetrate inside the fibers, and it is easy to wash. Fall off. On the other hand, by attaching the functional component by the production method of the present invention and heating, it becomes possible to penetrate the functional component into the molecular gap generated by the thermal motion of the fiber molecule. Therefore, it is considered that the functional component introduced into the inside strongly adheres to the fiber and remains after washing.
このようにして、本発明の機能性成分を含有する繊維を得ることができる。 Thus, the fiber containing the functional component of the present invention can be obtained.
＜機能性繊維＞
上記製造方法によって得られた機能性成分を含有する繊維は、機能性成分を機能性繊維重量あたり、通常１〜１５重量％、好ましくは１〜１０重量％含有する。
<Functional fiber>
The fiber containing the functional component obtained by the above production method usually contains 1 to 15% by weight, preferably 1 to 10% by weight of the functional component per weight of the functional fiber.
なお、本発明において、機能性繊維重量あたりの機能性成分の含有量とは、繊維の公定水分率における機能性成分の含有量を意味する。 In addition, in this invention, content of the functional component per functional fiber weight means content of the functional component in the official moisture content of a fiber.
本発明において機能性繊維重量あたりの機能性成分の含有量は、つぎのようにして測定することができる。機能性繊維１ｇを５ｍｍ角に裁断し、２０ｍＬのクロロホルムを加える。つぎに、この繊維入りの溶液を静置状態で超音波処理を３時間行い、機能性成分を抽出し、これを試料とする。この試料をガスクロマトグラフにより分析することにより、繊維重量あたりの機能性成分の含有量を測定することができる。 In the present invention, the content of the functional component per functional fiber weight can be measured as follows. 1 g of functional fiber is cut into 5 mm square, and 20 mL of chloroform is added. Next, this solution containing fibers is subjected to ultrasonic treatment for 3 hours in a stationary state to extract functional components, which are used as samples. By analyzing this sample with a gas chromatograph, the content of the functional component per fiber weight can be measured.
本発明においては、ＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯処理を１０回繰り返した後の機能性成分の合計含有量が、機能性繊維重量あたり０．０１重量％以上である。より好ましくは０．０５重量％以上であり、特に好ましくは０．１重量％以上、殊に好ましくは０．２重量％以上である。機能性成分の含有量が少なすぎると機能性が充分でなくなる。なお、洗濯１０回後の機能性成分の合計含有量の上限は、通常、機能性繊維重量あたり５重量％である。 In the present invention, the total content of the functional components after repeating the washing treatment 10 times in accordance with the method G described in JIS L 1096 is 0.01% by weight or more per functional fiber weight. More preferably, it is 0.05 weight% or more, Most preferably, it is 0.1 weight% or more, Most preferably, it is 0.2 weight% or more. If the content of the functional component is too small, the functionality becomes insufficient. In addition, the upper limit of the total content of functional components after 10 washings is usually 5% by weight per functional fiber weight.
また、本発明においては、上記洗濯処理を１０回行った後の機能性成分の脱落率は、通常９９重量％以下、好ましくは９７重量％以下、特に好ましくは９５重量％以下である。機能性成分の脱落率が多すぎる場合は、機能性が充分ではなくなる傾向がある。 In the present invention, the dropout rate of the functional component after the washing treatment is performed 10 times is usually 99% by weight or less, preferably 97% by weight or less, and particularly preferably 95% by weight or less. When the dropout rate of the functional component is too large, the functionality tends to be insufficient.
なお、上記脱落率とは、洗濯処理直前の機能性繊維重量あたりの機能性成分の含有量に対する、洗濯処理を１０回行った後の機能性繊維重量あたりの機能性成分の含有量の割合を１００から引いた数値をいい、具体的には、下記の式（２）により求めることができる。
［式］
脱落率（重量％）＝１００−（洗濯処理を１０回行った後の機能性繊維重量あたりの機能性成分の含有量／洗濯処理直前の機能性繊維重量あたりの機能性成分の含有量×１００） ・・・（２）
The drop-off rate is the ratio of the functional component content per functional fiber weight after the washing treatment is performed 10 times with respect to the functional component content per functional fiber weight immediately before the washing treatment. A numerical value subtracted from 100 can be obtained, and specifically, can be obtained by the following equation (2).
[formula]
Drop-off rate (% by weight) = 100− (functional component content per functional fiber weight after 10 washing treatments / functional component content per functional fiber weight immediately before washing treatment × 100 (2)
また、本発明の機能性繊維が防ダニ機能を有する成分を含有する場合は、上記洗濯処理を１０回繰り返した後のダニの忌避率が、３０％以上であることが好ましい。洗濯処理後のダニの忌避率が上記の数値を満たす場合、より洗濯耐久性を有する機能性繊維とすることができる。 Moreover, when the functional fiber of this invention contains the component which has a tick prevention function, it is preferable that the repelling rate of a tick after repeating the said washing process 10 times is 30% or more. When the repelling rate of ticks after the washing treatment satisfies the above numerical value, it can be a functional fiber having more washing durability.
上記ダニの忌避率は、通常３０％以上であり、好ましくは４０％以上、より好ましくは５０％以上である。なお、ダニの忌避率の上限は、通常１００％である。 The repellent rate of the mites is usually 30% or more, preferably 40% or more, more preferably 50% or more. The upper limit of the mite repellent rate is usually 100%.
なお、本発明においてダニの忌避率とは、ＪＩＳ Ｌ １９２０記載の侵入阻止法に準じて測定される値である。 In the present invention, the mite repellent rate is a value measured according to the intrusion prevention method described in JIS L 1920.
また、本発明の機能性繊維が防カビ機能を有する成分を含有する場合は、上記洗濯処理を１０回繰り返した後の抗カビ活性値が、通常２以上であり、好ましくは３以上、より好ましくは４以上である。なお、抗カビ活性値の上限は、通常５である。 In addition, when the functional fiber of the present invention contains a component having an antifungal function, the antifungal activity value after repeating the above washing treatment 10 times is usually 2 or more, preferably 3 or more, more preferably Is 4 or more. The upper limit of the antifungal activity value is usually 5.
本発明において抗カビ活性値とは、ＪＩＳ Ｌ １９２１（２０１５）記載の吸収法にに準じアオカビを用いて測定する方法により得られる値である。 In the present invention, the antifungal activity value is a value obtained by a method of measuring using blue mold according to the absorption method described in JIS L 1921 (2015).
本発明の機能性繊維は、洗濯を１０回した後においても機能性成分の含有量を高くすることができるため、洗濯耐久性を有する機能性繊維とすることができる。特に布団の中綿、布団カバー、枕カバー、側地、シーツ、ソファーカバー等に有用である。 Since the functional fiber of the present invention can increase the content of the functional component even after washing 10 times, it can be a functional fiber having washing durability. It is particularly useful for blankets, duvet covers, pillow covers, side covers, sheets and sofa covers.
以下、実施例をあげて本発明をさらに具体的に説明するが、本発明はその要旨を超えない限り、実施例の記載に限定されるものではない。
なお、例中「部」、「％」とあるのは、重量基準を意味する。
EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to the description of the examples unless it exceeds the gist.
In the examples, “parts” and “%” mean weight basis.
実施例に先立って以下の機能性成分および界面活性剤を準備した。
〔防ダニ機能を有する成分〕
・安息香酸フェニル
・ベンゾイル安息香酸メチル
・セバシン酸ジエチル
・ヒドロキシメトキシベンゾフェノン
・セバシン酸ジメチル
・安息香酸ベンジル
・イソプロピルメチルフェノール
・フェノトリン
・ベンゾインイソプロピルエーテル
・ベンゾイン
・ベンゾインエチルエーテル
・セバシン酸ジイソプロピル
・ベンジルサリチレート
・サリチル酸フェニル
・ヒドロキシ安息香酸ブチル
・ヒドロキシベンゾフェノン
・セバシン酸ジブチル（以下、「ＤＢＳ」と称する）
・３−ヨード−２−プロピニルブチルカーバメート（以下、「ＩＰＢＣ」と称する）
〔防カビ機能を有する成分〕
・ＩＰＢＣ
〔界面活性剤〕
・ポリオキシアルキレンポリスチルフェニルエーテル（日本乳化剤社製、Ｎ−２６０７）
・ポリオキシエチレン硬化ひまし油エーテル（日本乳化剤社製、Ｎ−１５２０ＨＣ）
Prior to the examples, the following functional components and surfactants were prepared.
[Ingredients having anti-mite function]
・ Phenylbenzoate ・ Methyl benzoylbenzoate ・ Diethyl sebacate ・ Hydroxymethoxybenzophenone ・ Dimethyl sebacate ・ Benzyl benzoate ・ Isopropylmethylphenol ・ Phenothrin ・ Benzoin isopropyl ether ・ Benzoin ・ Benzoin ethyl ether ・ Diisopropyl sebacate ・ Benzyl salicylate・ Phenyl salicylate ・ Butyl hydroxybenzoate ・ Hydroxybenzophenone ・ Dibutyl sebacate (hereinafter referred to as “DBS”)
3-iodo-2-propynyl butyl carbamate (hereinafter referred to as “IPBC”)
[Ingredients having antifungal function]
・ IPBC
[Surfactant]
・ Polyoxyalkylene polystilphenyl ether (N-2607, manufactured by Nippon Emulsifier Co., Ltd.)
・ Polyoxyethylene hydrogenated castor oil ether (N-1520HC, manufactured by Nippon Emulsifier Co., Ltd.)
＜実施例１＞
安息香酸フェニル５０部およびポリオキシアルキレンポリスチルフェニルエーテル２０部、ポリオキシエチレン硬化ひまし油エーテル１２．５部、溶剤としてフェニルジグリコール１７．５部を混合し処理剤組成物を調製した。この処理剤組成物の含有量が処理液中２０％となるように水と混合し、処理液を調製した。その後処理液に繊維（色染社製、試験用繊維ダブルピケ〔ポリエステル系繊維〕）を浸漬し、マングルにて処理液含有繊維の絞り率を調整した。この際、処理液含有繊維の絞り率を７０％になるようにした（繊維重量に対し安息香酸フェニル７％）。次に、絞り率を調整した繊維を連続染色機（ピンテンター）にて１５０℃で１分間乾燥し機能性成分を含有する繊維を得た。
<Example 1>
A treating agent composition was prepared by mixing 50 parts of phenyl benzoate, 20 parts of polyoxyalkylene polystilphenyl ether, 12.5 parts of polyoxyethylene hydrogenated castor oil ether, and 17.5 parts of phenyl diglycol as a solvent. A treatment liquid was prepared by mixing with water so that the content of the treatment composition was 20% in the treatment liquid. Thereafter, a fiber (manufactured by Color dyeing Co., Ltd., test fiber double picket [polyester fiber]) was immersed in the treatment liquid, and the drawing ratio of the treatment liquid-containing fiber was adjusted with a mangle. At this time, the drawing ratio of the treatment liquid-containing fiber was set to 70% (phenyl benzoate 7% with respect to the fiber weight). Next, the fiber having the adjusted drawing ratio was dried at 150 ° C. for 1 minute by a continuous dyeing machine (pin tenter) to obtain a fiber containing a functional component.
＜実施例２〜３２＞
実施例１において防ダニ機能を有する成分、処理液中の処理剤組成物含有量、絞り後の含有量、乾燥温度および乾燥時間を後記の表１のように変更した以外は、実施例１と同様にして実施例２〜３２の機能性成分を含有する繊維を得た。
<Examples 2-32>
Example 1 except that the components having an anti-mite function in Example 1, the content of the treatment agent composition in the treatment liquid, the content after squeezing, the drying temperature and the drying time were changed as shown in Table 1 below. Similarly, the fiber containing the functional component of Examples 2-32 was obtained.
得られた上記繊維をＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯を１０回した後の繊維に残存する機能性成分の合計含有量およびダニ忌避率を以下の評価方法により評価した。その結果を後記表１に示す。 The total amount of functional components remaining in the fiber and the mite repellent rate after the laundry was washed 10 times according to the G method described in JIS L 1096 were evaluated by the following evaluation methods. The results are shown in Table 1 below.
〔機能性成分の含有量〕
繊維に付着、および内部浸透している機能性成分の合計含有量は、以下の測定方法で定量した。
（ｉ）試料溶液Ａの調製
機能性繊維１ｇを５ｍｍ角に裁断し、そこに２０ｍＬのクロロホルムを加えた。この繊維入りの溶液を静置状態で超音波処理を３時間行い、機能性成分を抽出し、この抽出液を試料溶液Ａとした。
（ｉｉ）標準試料溶液Ｂの調製
標準物質として各実施例で用いた機能性成分５００ｍｇをクロロホルムに溶解させ、全量を１００ｍＬとし、さらにこの溶液をクロロホルムで５倍希釈を行い、標準試料溶液Ｂとした（標準物質濃度：１００ｍｇ／１００ｍＬ）。
（ｉｉｉ）内部標準液Ｃの調製
内部標準物質としてフタル酸ジイソブチル５００ｍｇをクロロホルムに溶解させ、全量を１００ｍＬとし、これを内部標準液Ｃとした。
（ｉｖ）試料溶液Ｄおよび標準溶液Ｅの調製
上記試料溶液Ａ２０ｍＬに上記内部標準液Ｃ５ｍＬを添加し、試料溶液Ｄとした。また、上記標準試料溶液Ｂ２０ｍＬに上記内部標準液Ｃ５ｍＬを添加し、標準溶液Ｅとした。（ｖ）試料溶液Ｄおよび標準溶液Ｅの測定
試料溶液および標準溶液をガスクロマトグラフにより分析を行った。得られたクロマトグラムから、標準物質と内部標準物質とのピーク面積比を求め、各機能性成分を定量した。
[Content of functional ingredients]
The total content of functional components adhering to the fiber and penetrating inside was quantified by the following measuring method.
(I) Preparation of sample solution A 1 g of functional fibers were cut into 5 mm square, and 20 mL of chloroform was added thereto. This fiber-containing solution was subjected to ultrasonic treatment for 3 hours in a stationary state to extract functional components, and this extract was used as sample solution A.
(Ii) Preparation of standard sample solution B 500 mg of the functional component used in each example as a standard substance was dissolved in chloroform to make a total volume of 100 mL, and this solution was further diluted 5-fold with chloroform. (Standard substance concentration: 100 mg / 100 mL).
(Iii) Preparation of internal standard solution C As an internal standard substance, 500 mg of diisobutyl phthalate was dissolved in chloroform to make a total volume of 100 mL.
(Iv) Preparation of sample solution D and standard solution E Sample solution D was prepared by adding 5 mL of the internal standard solution C to 20 mL of the sample solution A. Further, 5 mL of the internal standard solution C was added to 20 mL of the standard sample solution B to obtain a standard solution E. (V) Measurement of sample solution D and standard solution E The sample solution and the standard solution were analyzed by gas chromatography. From the obtained chromatogram, the peak area ratio between the standard substance and the internal standard substance was determined, and each functional component was quantified.
［ガスクロマトグラフ測定条件］
使用機器 ：ＧＣ−２０１４［島津製作所社製］
検出機 ：ＦＩＤ
使用カラム ：Ｒｔｘ−２００（３０ｍ）［ＧＬサイエンス社製］
カラム温度 ：２４０℃
キャリアガス流量：１．４５ｍＬ／分
注入量 ：１μＬ
[Gas chromatograph measurement conditions]
Equipment used: GC-2014 [manufactured by Shimadzu Corporation]
Detector: FID
Column used: Rtx-200 (30 m) [manufactured by GL Sciences]
Column temperature: 240 ° C
Carrier gas flow rate: 1.45 mL / min Injection volume: 1 μL
〔ダニ忌避率の評価〕
ＪＩＳ Ｌ １９２０記載の侵入阻止法に準じてダニ忌避率の評価を行った。
[Evaluation of tick repellency]
The mite repellent rate was evaluated according to the intrusion prevention method described in JIS L 1920.
上記の結果から、実施例１〜３２において洗濯１０回後の機能性成分の含有量が機能性繊維重量あたり０．０１％以上であり、洗濯耐久性を有する機能性繊維とすることができた。 From the above results, in Examples 1 to 32, the content of the functional component after 10 washes was 0.01% or more per functional fiber weight, and it was possible to obtain functional fibers having washing durability. .
次に実施例３３〜４９、比較例１〜６に先立って、下記の処理剤組成物Ｉを調製した。 Next, prior to Examples 33 to 49 and Comparative Examples 1 to 6, the following treating agent composition I was prepared.
〔処理剤組成物Ｉの調製〕
ＩＰＢＣ２０部、ポリオキシエチレン硬化ひまし油エーテル６部およびポリオキシアルキレンポリスチルフェニルエーテル２９部、溶剤としてフェニルジグリコール４５部を混合し処理剤組成物Ｉを得た。
[Preparation of treatment composition I]
A treating agent composition I was obtained by mixing 20 parts of IPBC, 6 parts of polyoxyethylene hydrogenated castor oil ether, 29 parts of polyoxyalkylene polystilphenyl ether, and 45 parts of phenyl diglycol as a solvent.
＜実施例３３＞
上記処理剤組成物Ｉの含有量が処理液中１％となるように水と混合し、処理液とした。次に、繊維（色染社製、試験用繊維ダブルピケ〔ポリエステル系繊維〕）を処理液に浸漬し、マングルにて処理液含有繊維の絞り率を調整した。この際、処理液含有繊維の絞り率が１００％となるようにした（繊維重量に対しＩＰＢＣ０．２％）。次に、上記の繊維を連続染色機（ピンテンター）にて１５０℃で１分間乾燥し機能性成分を含有する繊維を得た。得られた機能性成分を含有する繊維の、洗濯１０回後の機能性成分の含有量を実施例１と同様にして評価した。結果を下記の表２に示す。
<Example 33>
It mixed with water so that content of the said processing agent composition I might be 1% in a processing liquid, and it was set as the processing liquid. Next, a fiber (manufactured by Color Dyeing Co., Ltd., test fiber double picket [polyester fiber]) was immersed in the treatment liquid, and the drawing ratio of the treatment liquid-containing fiber was adjusted with a mangle. At this time, the drawing ratio of the treatment liquid-containing fiber was set to 100% (IPBC 0.2% with respect to the fiber weight). Next, the above fiber was dried at 150 ° C. for 1 minute by a continuous dyeing machine (pin tenter) to obtain a fiber containing a functional component. The content of the functional component after 10 washings of the fiber containing the functional component was evaluated in the same manner as in Example 1. The results are shown in Table 2 below.
＜実施例３４〜４９、比較例１〜６＞
上記実施例３３において、処理液中の処理剤組成物含有量、絞り率、乾燥温度、乾燥時間および絞り後の含有量を下記表２のように変更した以外は、実施例３３と同様にして実施例３４〜４９および比較例１〜６の機能性成分を含有する繊維を得た。なお、実施例３４、３８および比較例１、２では、マングルによる絞り率の調整は行わず、自然乾燥により絞り率を調整した。得られた機能性成分を有する繊維の、洗濯１０回後の機能性成分の含有量を実施例１と同様にして評価した。結果を下記の表２に示す。
<Examples 34 to 49, Comparative Examples 1 to 6>
In Example 33, the treatment agent composition content, the drawing ratio, the drying temperature, the drying time, and the content after drawing in the treatment liquid were changed as shown in Table 2 below, in the same manner as in Example 33. Fibers containing the functional components of Examples 34 to 49 and Comparative Examples 1 to 6 were obtained. In Examples 34 and 38 and Comparative Examples 1 and 2, the drawing rate was not adjusted by mangle, but the drawing rate was adjusted by natural drying. The content of the functional component after 10 washings of the obtained fiber having the functional component was evaluated in the same manner as in Example 1. The results are shown in Table 2 below.
実施例３３〜４９の繊維は、洗濯１０回後も機能性成分の含有量が機能性繊維重量あたり０．０１％以上であった。それに対し、比較例１〜６の繊維は、洗濯１０回後の機能性成分の含有量が機能性繊維重量あたり０．０１％未満であった。 In the fibers of Examples 33 to 49, the content of the functional component was 0.01% or more per functional fiber weight even after 10 washes. On the other hand, in the fibers of Comparative Examples 1 to 6, the content of the functional component after 10 washings was less than 0.01% per functional fiber weight.
次に実施例５０〜６７、比較例７〜１１に先立って、下記の処理剤組成物ＩＩを調製した。 Next, prior to Examples 50 to 67 and Comparative Examples 7 to 11, the following treatment agent composition II was prepared.
〔処理剤組成物ＩＩの調製〕
ＤＢＳ６０部、ポリオキシエチレン硬化ひまし油エーテル６部、ポリオキシアルキレンポリスチルフェニルエーテル３４部とを混合し処理剤組成物ＩＩを得た。
[Preparation of Treatment Agent Composition II]
60 parts of DBS, 6 parts of polyoxyethylene hydrogenated castor oil ether, and 34 parts of polyoxyalkylene polystilphenyl ether were mixed to obtain a treating agent composition II.
＜実施例５０＞
上記処理剤組成物ＩＩの含有量が処理液中２％となるように水と混合し、処理液とした。次に、繊維（色染社製、試験用繊維ダブルピケ〔ポリエステル系繊維〕）を処理液に浸漬し、マングルにて処理液含有繊維の絞り率を調整した。この際、処理液含有繊維の絞り率が１００％となるようにした（繊維重量に対しＤＢＳ０．２％）。次に、上記の繊維を連続染色機（ピンテンター）にて１５０℃で１分間乾燥し機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維の、洗濯１０回後の機能性成分の含有量を実施例１と同様にして評価した。結果を下記の表３に示す。
<Example 50>
It mixed with water so that content of the said processing agent composition II might be 2% in a processing liquid, and it was set as the processing liquid. Next, a fiber (manufactured by Color Dyeing Co., Ltd., test fiber double picket [polyester fiber]) was immersed in the treatment liquid, and the drawing ratio of the treatment liquid-containing fiber was adjusted with a mangle. At this time, the drawing rate of the treatment liquid-containing fiber was set to 100% (DBS 0.2% with respect to the fiber weight). Next, the above fiber was dried at 150 ° C. for 1 minute by a continuous dyeing machine (pin tenter) to obtain a fiber containing a functional component. The content of the functional component after 10 washings of the obtained fiber having the functional component was evaluated in the same manner as in Example 1. The results are shown in Table 3 below.
＜実施例５１〜６７、比較例７〜１１＞
上記実施例５０において、処理液中の処理剤組成物含有量、絞り率、乾燥温度および乾燥時間を下記表３のように変更した以外は、実施例５０と同様にして実施例５１〜６７および比較例７〜１１の機能性成分を含有する繊維を得た。なお、実施例５４、５５および比較例７では、マングルによる絞り率の調整は行わず、自然乾燥により絞り率を調整した。得られた機能性成分を有する繊維の、洗濯１０回後の機能性成分の含有量を実施例１と同様にして評価した。結果を下記の表３に示す。
<Examples 51 to 67, Comparative Examples 7 to 11>
In Example 50 described above, Examples 51 to 67 and Example 51 to 67 were performed in the same manner as in Example 50 except that the treatment agent composition content, the drawing ratio, the drying temperature, and the drying time in the treatment liquid were changed as shown in Table 3 below. Fibers containing the functional components of Comparative Examples 7 to 11 were obtained. In Examples 54 and 55 and Comparative Example 7, the drawing rate was not adjusted by mangle, but the drawing rate was adjusted by natural drying. The content of the functional component after 10 washings of the obtained fiber having the functional component was evaluated in the same manner as in Example 1. The results are shown in Table 3 below.
実施例５０〜６７の繊維は、洗濯１０回後も機能性成分の含有量が機能性繊維重量あたり０．０１％以上であった。それに対し、比較例７〜１１の繊維は、洗濯１０回後の機能性成分の含有量が機能性繊維重量あたり０．０１％未満であった。 In the fibers of Examples 50 to 67, the content of the functional component was 0.01% or more per functional fiber weight even after 10 washes. On the other hand, in the fibers of Comparative Examples 7 to 11, the content of the functional component after 10 washings was less than 0.01% per functional fiber weight.
次に、実施例６８〜７６に先立って、下記の処理剤組成物Ａ〜Ｃおよび親水性ポリマー分散液ａ、ｂを調製した。 Next, prior to Examples 68 to 76, the following treatment agent compositions A to C and hydrophilic polymer dispersions a and b were prepared.
〔処理剤組成物Ａの調製〕
ＤＢＳ４５部、ＩＰＢＣ２０部とポリオキシエチレン硬化ひまし油エーテル６部、ポリオキシアルキレンポリスチルフェニルエーテル２９部とを混合し処理剤組成物Ａを得た。
[Preparation of treating agent composition A]
45 parts of DBS, 20 parts of IPBC, 6 parts of polyoxyethylene hydrogenated castor oil ether, and 29 parts of polyoxyalkylene polystilphenyl ether were mixed to obtain a treating agent composition A.
〔処理剤組成物Ｂの調製〕
上記処理剤組成物Ａ８３．３部と浸透促進剤として安息香酸１６．７部とを混合し、処理剤組成物Ｂを得た。
[Preparation of treating agent composition B]
83.3 parts of the treatment agent composition A and 16.7 parts of benzoic acid as a penetration enhancer were mixed to obtain treatment agent composition B.
〔処理剤組成物Ｃの調製〕
上記処理剤組成物Ａ８３．３部と浸透促進剤として安息香酸ベンジル１６．７部とを混合し、処理剤組成物Ｃを得た。
[Preparation of treating agent composition C]
The above-mentioned treating agent composition A 83.3 parts and 16.7 parts of benzyl benzoate as a penetration enhancer were mixed to obtain treating agent composition C.
〔親水性ポリマー分散液ａ〕
親水性ポリマーとしてキサンタンガム１００部と溶剤として１，３−ブチレングリコール１００部とを混合し、親水性ポリマー分散剤を得た。次に、親水性ポリマー分散剤０．３７５部、イオン交換水９９．６２５部を８０℃で１５分間加温・撹拌し、親水性ポリマー分散液ａを得た。
[Hydrophilic polymer dispersion a]
100 parts of xanthan gum as a hydrophilic polymer and 100 parts of 1,3-butylene glycol as a solvent were mixed to obtain a hydrophilic polymer dispersant. Next, 0.375 parts of the hydrophilic polymer dispersant and 99.625 parts of ion-exchanged water were heated and stirred at 80 ° C. for 15 minutes to obtain a hydrophilic polymer dispersion a.
〔親水性ポリマー分散液ｂ〕
親水性ポリマーとしてポリアクリル酸Ｎａ１００部と溶剤として１，３−ブチレングリコール１００部とを混合し、親水性ポリマー分散剤を得た。次に、親水性ポリマー分散剤０．７５部、イオン交換水９９．２５部を８０℃で１５分間加温・撹拌し、親水性ポリマー分散液ｂを得た。
[Hydrophilic polymer dispersion b]
100 parts of polyacrylic acid Na as a hydrophilic polymer and 100 parts of 1,3-butylene glycol as a solvent were mixed to obtain a hydrophilic polymer dispersant. Next, 0.75 parts of a hydrophilic polymer dispersant and 99.25 parts of ion exchange water were heated and stirred at 80 ° C. for 15 minutes to obtain a hydrophilic polymer dispersion b.
上記処理剤組成物Ａ〜Ｃおよび親水性ポリマー分散液ａ、ｂを用いて下記の処理液Ｉ〜ＶＩを調製した。 The following treatment liquids I to VI were prepared using the treatment agent compositions A to C and the hydrophilic polymer dispersions a and b.
〔処理液Ｉの調製〕
処理剤組成物Ａ６．２５部、イオン交換水９３．７５部を混合し、処理液Ｉを得た。
[Preparation of Treatment Solution I]
6.25 parts of treating agent composition A and 93.75 parts of ion-exchanged water were mixed to obtain a treatment liquid I.
〔処理液ＩＩの調製〕
処理剤組成物Ａ６．２５部、親水性ポリマー分散液ａ９３．７５部を混合し、処理液ＩＩを得た。
[Preparation of Treatment Solution II]
6.25 parts of treatment agent composition A and 93.75 parts of hydrophilic polymer dispersion a were mixed to obtain treatment liquid II.
〔処理液ＩＩＩ〕
処理剤組成物Ａ６．２５部、親水性ポリマー分散液ｂ９３．７５部を混合し、処理液ＩＩＩを得た。
[Treatment liquid III]
6.25 parts of treatment agent composition A and 93.75 parts of hydrophilic polymer dispersion b were mixed to obtain treatment liquid III.
〔処理液ＩＶ〕
処理剤組成物Ｂ１２部と親水性ポリマー分散液ａ８８部とを混合し、処理液ＩＶを得た。
[Treatment solution IV]
Treatment agent composition B12 part and hydrophilic polymer dispersion liquid a88 part were mixed, processing liquid IV was obtained.
〔処理液Ｖ〕
処理剤組成物Ｃ１２部と親水性ポリマー分散液ａ８８部とを混合し、処理液Ｖを得た。
[Treatment solution V]
A treating solution V was obtained by mixing 12 parts of the treating agent composition C and 88 parts of the hydrophilic polymer dispersion a.
〔処理液ＶＩ〕
処理剤組成物Ｃ１２部と親水性ポリマー分散液ｂ８８部とを混合し、処理液ＶＩを得た。
[Treatment solution VI]
A treating liquid VI was obtained by mixing 12 parts of the treating agent composition C and 88 parts of the hydrophilic polymer dispersion b.
＜実施例６８＞
上記処理液Ｉに繊維（色染社製、試験用繊維ダブルピケ〔ポリエステル系繊維〕）を浸漬し、マングルにて処理液含有繊維の絞り率を調整した。この際、処理液含有繊維の絞り率が８０％になるようにした（繊維重量に対しＤＢＳ２．２５％、ＩＰＢＣ１％）。次に、絞り率を調整した繊維を連続染色機（ピンテンター）にて１６０℃で１分間乾燥し機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維の、洗濯１０回後の機能性成分の含有量を実施例１と同様にして評価した。結果を下記の表４に示す。
<Example 68>
Fibers (manufactured by Color Dyeing Co., Ltd., test fiber double picket [polyester fiber]) were immersed in the treatment liquid I, and the drawing ratio of the treatment liquid-containing fibers was adjusted with a mangle. At this time, the drawing ratio of the treatment liquid-containing fiber was set to 80% (DBS 2.25%, IPBC 1% with respect to the fiber weight). Next, the fiber with the adjusted drawing ratio was dried with a continuous dyeing machine (pin tenter) at 160 ° C. for 1 minute to obtain a fiber containing a functional component. The content of the functional component after 10 washings of the obtained fiber having the functional component was evaluated in the same manner as in Example 1. The results are shown in Table 4 below.
＜実施例６９〜７６＞
実施例６８において、用いる処理液および乾燥温度を下記の表４のように変更した以外は、実施例６８と同様にして実施例６９〜７６の機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維を実施例６８と同様にして評価した。それらの結果を下記の表４に示す。
<Examples 69 to 76>
In Example 68, fibers containing functional components of Examples 69 to 76 were obtained in the same manner as in Example 68 except that the treatment liquid used and the drying temperature were changed as shown in Table 4 below. The obtained fiber having a functional component was evaluated in the same manner as in Example 68. The results are shown in Table 4 below.
親水性ポリマーを配合した実施例６９、７０は、親水性ポリマーを配合していない実施例６８と比較して洗濯１０回後の機能性成分の含有量が高かった。また、親水性ポリマーと浸透促進剤を配合した実施例７１〜７６は、実施例６８と比較して洗濯１０回後の機能性成分の含有量が高かった。 In Examples 69 and 70 in which the hydrophilic polymer was blended, the content of the functional component after 10 washes was higher than in Example 68 in which the hydrophilic polymer was not blended. Moreover, Examples 71-76 which mix | blended the hydrophilic polymer and the penetration enhancer had a high content of the functional component after 10 washings compared with Example 68.
実施例７７、７８に先立って下記の処理剤組成物Ｄ、Ｅを調製した。 Prior to Examples 77 and 78, the following treating agent compositions D and E were prepared.
〔処理剤組成物Ｄの調製〕
ＤＢＳ４５部とＩＰＢＣ２０部、ポリオキシエチレン硬化ひまし油エーテル６部、ポリオキシアルキレンポリスチルフェニルエーテル２９部とを混合し処理剤組成物Ｄを得た。
[Preparation of treating agent composition D]
45 parts of DBS, 20 parts of IPBC, 6 parts of polyoxyethylene hydrogenated castor oil ether and 29 parts of polyoxyalkylene polystilphenyl ether were mixed to obtain a treating agent composition D.
〔処理剤組成物Ｅの調製〕
上記処理剤組成物Ｄ９１部と浸透促進剤として安息香酸ベンジル９部とを混合し、処理剤組成物Ｅを得た。
[Preparation of treating agent composition E]
A treating agent composition E was obtained by mixing 91 parts of the treating agent composition D and 9 parts of benzyl benzoate as a penetration enhancer.
上記処理剤組成物Ｄ、Ｅおよび前記親水性ポリマー分散液ａを用いて下記の処理液ＶＩＩ、ＶＩＩＩを調製した。 The following treatment liquids VII and VIII were prepared using the treatment agent compositions D and E and the hydrophilic polymer dispersion liquid a.
〔処理液ＶＩＩの調製〕
処理剤組成物Ｄ１２．５部とイオン交換水８７．５部とを混合し、処理液ＶＩＩを得た。
[Preparation of Treatment Solution VII]
Processing agent composition D12.5 part and ion-exchange water 87.5 parts were mixed, and the processing liquid VII was obtained.
〔処理液ＶＩＩＩの調製〕
処理剤組成物Ｅ１３．８部と親水性ポリマー分散液ａ８６．２部とを混合し、処理液ＶＩＩＩを得た。
[Preparation of treatment liquid VIII]
Treatment agent composition E13.8 parts and hydrophilic polymer dispersion a86.2 parts were mixed to obtain treatment liquid VIII.
＜実施例７７＞
上記処理液ＶＩＩに繊維（色染社製、試験用繊維ダブルピケ〔ポリエステル系繊維〕）を浸漬し、マングルにて処理液含有繊維の絞り率を調整した。この際、処理液含有繊維の絞り率が８０％になるようにした（繊維重量に対し、ＤＢＳ４．５％、ＩＰＢＣ２％）。次に、絞り率を調整した繊維を連続染色機（ピンテンター）にて１６０℃で１分間乾燥し機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維を実施例１と同様にして評価した。結果を下記の表５に示す。
<Example 77>
A fiber (manufactured by Color dyeing Co., Ltd., test fiber double picket [polyester fiber]) was immersed in the treatment liquid VII, and the drawing ratio of the treatment liquid-containing fiber was adjusted with a mangle. At this time, the drawing ratio of the treatment liquid-containing fiber was set to 80% (DBS 4.5%, IPBC 2% with respect to the fiber weight). Next, the fiber with the adjusted drawing ratio was dried with a continuous dyeing machine (pin tenter) at 160 ° C. for 1 minute to obtain a fiber containing a functional component. The obtained fiber having a functional component was evaluated in the same manner as in Example 1. The results are shown in Table 5 below.
＜実施例７８＞
前記処理液ＶＩＩＩに繊維（色染社製、試験用繊維ダブルピケ〔ポリエステル系繊維〕）を浸漬し、マングルにて処理液含有繊維の絞り率を調整した。この際、処理液含有繊維の絞り率が８０％になるようにした（繊維重量に対し、ＤＢＳ４．５％、ＩＰＢＣ２％）。次に、絞り率を調整した繊維を連続染色機（ピンテンター）にて１７０℃で１分間乾燥し機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維を実施例１と同様にして評価した。結果を下記の表５に示す。
<Example 78>
Fibers (manufactured by Color dyeing Co., Ltd., test fiber double picket [polyester fiber]) were immersed in the treatment liquid VIII, and the drawing ratio of the treatment liquid-containing fibers was adjusted with a mangle. At this time, the drawing ratio of the treatment liquid-containing fiber was set to 80% (DBS 4.5%, IPBC 2% with respect to the fiber weight). Next, the fiber with the adjusted drawing ratio was dried with a continuous dyeing machine (pin tenter) at 170 ° C. for 1 minute to obtain a fiber containing a functional component. The obtained fiber having a functional component was evaluated in the same manner as in Example 1. The results are shown in Table 5 below.
上記の結果から浸透促進剤と親水性ポリマーとを併用した実施例７８は、浸透促進剤と親水性ポリマーを用いない実施例７７よりも機能性成分の含有量とダニ忌避率が高かった。 From the above results, Example 78 in which a penetration enhancer and a hydrophilic polymer were used in combination had a higher functional component content and mite repellency than Example 77 in which a penetration enhancer and a hydrophilic polymer were not used.
＜実施例７９＞
ＤＢＳ６５部、ポリオキシエチレン硬化ひまし油エーテル６部、ポリオキシアルキレンポリスチルフェニルエーテル２９部を混合し処理剤組成物を得た。この処理剤組成物の含有量が処理液中２０％となるように水と混合し、処理液を調製した。次に繊維としてポリエステル綿を用い、繊維重量の１０％の処理液を繊維にスプレーした。この処理液を含有する繊維を１５０℃、２分間オーブンで乾燥し、実施例７９の機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維を実施例１と同様にして評価した。結果を下記の表６に示す。
<Example 79>
65 parts of DBS, 6 parts of polyoxyethylene hydrogenated castor oil ether and 29 parts of polyoxyalkylene polystilphenyl ether were mixed to obtain a treating agent composition. A treatment liquid was prepared by mixing with water so that the content of the treatment composition was 20% in the treatment liquid. Next, polyester cotton was used as the fiber, and a treatment liquid having a fiber weight of 10% was sprayed onto the fiber. The fiber containing the treatment liquid was dried in an oven at 150 ° C. for 2 minutes to obtain a fiber containing the functional component of Example 79. The obtained fiber having a functional component was evaluated in the same manner as in Example 1. The results are shown in Table 6 below.
＜実施例８０〜８２、比較例１２、１３＞
実施例７９において乾燥温度および乾燥時間を下記表６のように変更した以外は、実施例７９と同様にして実施例８０〜８２、比較例１２、１３の機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維を実施例７９と同様にして評価した。結果を下記の表６に示す。
<Examples 80 to 82, Comparative Examples 12 and 13>
A fiber containing functional components of Examples 80 to 82 and Comparative Examples 12 and 13 was obtained in the same manner as in Example 79 except that the drying temperature and drying time were changed as shown in Table 6 below. . The obtained fiber having a functional component was evaluated in the same manner as in Example 79. The results are shown in Table 6 below.
＜実施例８３＞
ＩＰＢＣ２０部、溶剤としてフェニルジグリコール４５部、ポリオキシエチレン硬化ひまし油エーテル６部、ポリオキシアルキレンポリスチルフェニルエーテル２９部を混合し処理剤組成物を得た。この処理剤組成物の含有量が処理液中２０％となるように水と混合し、処理液を調製した。次に繊維としてポリエステル綿を用い、繊維重量の１０％の処理液を繊維にスプレーした。この処理液を含有する繊維を１５０℃、２分間オーブンで乾燥し、実施例８３の機能性成分を含有する繊維を得た。得られた機能性成分を有する繊維を実施例７９と同様にして評価した。結果を下記の表６に示す。
<Example 83>
20 parts of IPBC, 45 parts of phenyldiglycol as a solvent, 6 parts of polyoxyethylene hydrogenated castor oil ether and 29 parts of polyoxyalkylene polystilphenyl ether were mixed to obtain a treating agent composition. A treatment liquid was prepared by mixing with water so that the content of the treatment composition was 20% in the treatment liquid. Next, polyester cotton was used as the fiber, and a treatment liquid having a fiber weight of 10% was sprayed onto the fiber. The fiber containing the treatment liquid was dried in an oven at 150 ° C. for 2 minutes to obtain a fiber containing the functional component of Example 83. The obtained fiber having a functional component was evaluated in the same manner as in Example 79. The results are shown in Table 6 below.
＜実施例８４〜８６、比較例１４、１５＞
実施例８３において乾燥温度および乾燥時間を下記表６のように変更した以外は、実施例８３と同様にして実施例８４〜８６、比較例１４、１５の機能性成分を含有する繊維を得た。得られた機能性成分を含有する繊維を実施例７９と同様にして評価した。結果を下記の表６に示す。
<Examples 84 to 86, Comparative Examples 14 and 15>
A fiber containing the functional components of Examples 84 to 86 and Comparative Examples 14 and 15 was obtained in the same manner as in Example 83 except that the drying temperature and drying time were changed as shown in Table 6 below in Example 83. . The fiber containing the obtained functional component was evaluated in the same manner as in Example 79. The results are shown in Table 6 below.
上記の表６に示すように実施例７９〜８６の繊維は、洗濯後でも機能性成分の含有量が０．０１％以上であり、さらにダニ忌避率も３０％以上であった。一方、比較例１２〜１５の繊維は、洗濯後の機能性成分の含有量が０．０１％未満であり、ダニ忌避率も３０％未満であった。 As shown in Table 6 above, the fibers of Examples 79 to 86 had a functional component content of 0.01% or more after washing and a mite repellent rate of 30% or more. On the other hand, the fibers of Comparative Examples 12 to 15 had a functional component content of less than 0.01% after washing and a tick repellent rate of less than 30%.
また、前記実施例４０、４５および比較例４、６の機能性成分を含有する繊維をＪＩＳ Ｌ １０９６記載のＧ法に準じて洗濯を１０回行い、洗濯後の抗カビ活性値を、以下の評価方法により評価した。 Further, the fibers containing the functional components of Examples 40 and 45 and Comparative Examples 4 and 6 were washed 10 times according to the G method described in JIS L 1096, and the antifungal activity value after washing was determined as follows. It evaluated by the evaluation method.
〔抗カビ活性値の評価〕
ＪＩＳ Ｌ １９２１（２０１５）の記載の吸収法に準じ、アオカビを用いて求めた抗カビ活性値を、下記の評価基準に基づいて評価した。
［評価基準］
Ａ：抗カビ活性値 ３．０以上（強い効果がある）
Ｂ：抗カビ活性値 ２．０以上、３．０未満（効果がある）
Ｃ：抗カビ活性値 １．０以上、２．０未満（弱い効果がある）
Ｄ：抗カビ活性値 １．０未満（効果が認められない）
[Evaluation of antifungal activity value]
In accordance with the absorption method described in JIS L 1921 (2015), the antifungal activity value determined using blue mold was evaluated based on the following evaluation criteria.
[Evaluation criteria]
A: Antifungal activity value of 3.0 or more (strong effect)
B: Antifungal activity value 2.0 or more and less than 3.0 (effective)
C: Antifungal activity value 1.0 or more and less than 2.0 (has a weak effect)
D: Antifungal activity value less than 1.0 (effect is not recognized)
上記の表７に示すように実施例４０、４５の繊維は、洗濯後でも機能性成分の含有量が０．０１％以上であった。また、抗カビ活性値の評価も、実施例４０が２．５であり、実施例４５が４．１と洗濯１０回後においても抗カビ活性を有していた。一方、比較例４、６の繊維は、洗濯後の機能性成分の含有量が０．０１％未満であり、さらには、抗カビ活性も弱いものであった。 As shown in Table 7 above, the fibers of Examples 40 and 45 had a functional component content of 0.01% or more even after washing. In addition, the antifungal activity value was 2.5 for Example 40 and 4.1 for Example 45, which had antifungal activity even after 10 washes. On the other hand, in the fibers of Comparative Examples 4 and 6, the content of the functional component after washing was less than 0.01%, and the antifungal activity was also weak.
本発明の繊維は、洗濯を１０回した後においても機能性成分の含有量を高くすることができるため、洗濯耐久性を有する防ダニ繊維とすることができる。特に布団の中綿、布団カバー、枕カバー、側地、シーツ、ソファーカバー等に有用である。 Since the fiber of the present invention can increase the content of the functional component even after washing 10 times, it can be a tick-proof fiber having washing durability. It is particularly useful for blankets, duvet covers, pillow covers, side covers, sheets and sofa covers.
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