JP4223356B2 - Elastic fiber treatment agent and elastic fiber - Google Patents
Elastic fiber treatment agent and elastic fiber Download PDFInfo
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- JP4223356B2 JP4223356B2 JP2003311991A JP2003311991A JP4223356B2 JP 4223356 B2 JP4223356 B2 JP 4223356B2 JP 2003311991 A JP2003311991 A JP 2003311991A JP 2003311991 A JP2003311991 A JP 2003311991A JP 4223356 B2 JP4223356 B2 JP 4223356B2
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本発明は弾性繊維用処理剤に関する。詳しくは、該処理剤を弾性繊維に付与することで、解舒性、制電性、チーズ捲形状、平滑性に優れた弾性繊維が得られ、弾性繊維と綿糸を用いた編物や織物において、綿糸がこすれて生じた風綿の吸着が少なく編織の工程での弾性繊維の糸切れが起こらなくなるような弾性繊維用処理剤及び該処理剤を用いて処理された弾性繊維に関する。 The present invention relates to a treatment agent for elastic fibers. Specifically, by applying the treatment agent to the elastic fiber, an elastic fiber excellent in unwinding property, antistatic property, cheese wrinkle shape, and smoothness is obtained. In a knitted fabric or a woven fabric using elastic fiber and cotton yarn, The present invention relates to a treatment agent for elastic fibers that causes little absorption of cotton fluff generated by rubbing cotton yarn and prevents yarn breakage of elastic fibers in the knitting process, and an elastic fiber treated with the treatment agent.
従来から、弾性繊維の処理剤として、いくつかの提案がなされている。特開平１０−３１０９７９号公報、特公平６−１５７４５号公報、特公昭４０−５５５７号公報、特公昭３７−４５８６号公報には膠着防止剤として、高級脂肪酸の金属塩を処理剤に用いる方法が記載されている。特開平９−７８４６０号公報、特開平８−７４１７９号公報、特公昭４２−８４３８号公報には膠着防止剤として、シリコーン樹脂を処理剤に用いる方法が記載されている。特開平１１−２２９２７７号公報には膠着防止剤として、アルキルリン酸エステル化合物を処理剤に用いる方法が記載されている。特表２００１−５０９８４７号公報、特開平１−２９８２５９号公報には、膠着性の少ない弾性繊維を得るため、溶融したポリウレタンポリマー中にステアリン酸エチレンビスアミド等の高級脂肪酸アミドを分散混合して紡糸する方法が記載されている。特開平１１−６１６５１号公報には制電剤として、有機スルホン酸化合物、有機硫酸化合物を処理剤に用いる方法が記載されている。特開平９−４９１６７号公報、特開平７−１７３７７０号公報には制電剤として、アルキルホスフェート金属塩とアルキルホスフェートアミン塩を処理剤に用いる方法が記載されている。特開平１１−０１２９５０号公報には弾性繊維に良好なチーズ捲形状を付与する処理剤としてシリコーンオイル、カルボキシアミド変性シリコーン、高級脂肪酸マグネシウム塩からなる処理剤が記載されている。 Conventionally, several proposals have been made as treatment agents for elastic fibers. JP-A-10-310979, JP-B-6-15745, JP-B-40-5557, JP-B37-4586 discloses a method using a metal salt of a higher fatty acid as a processing agent as an anti-sticking agent. Are listed. Japanese Patent Application Laid-Open No. 9-78460, Japanese Patent Application Laid-Open No. 8-74179, and Japanese Patent Publication No. 42-8438 describe a method of using a silicone resin as a treatment agent as an anti-sticking agent. Japanese Patent Application Laid-Open No. 11-229277 describes a method using an alkyl phosphate ester compound as a treating agent as an anti-sticking agent. In JP-T-2001-509847 and JP-A-1-298259, in order to obtain an elastic fiber with low adhesiveness, a higher fatty acid amide such as ethylene bisamide stearate is dispersed and mixed in a melted polyurethane polymer and spun. A method is described. Japanese Patent Application Laid-Open No. 11-61651 describes a method in which an organic sulfonic acid compound or an organic sulfuric acid compound is used as a treatment agent as an antistatic agent. Japanese Patent Application Laid-Open Nos. 9-49167 and 7-173770 describe a method of using an alkyl phosphate metal salt and an alkyl phosphate amine salt as treatment agents as antistatic agents. Japanese Patent Application Laid-Open No. 11-012950 discloses a treatment agent comprising silicone oil, a carboxyamide-modified silicone, and a higher fatty acid magnesium salt as a treatment agent for imparting a good cheese cake shape to elastic fibers.
弾性繊維用処理剤は、シリコーン油、鉱物油およびエステル油などの疎水性のベース成分を用いているため、制電性が不十分である。チーズ解舒性については、繊維間の膠着性が強いと、チーズ解舒性が悪くなる。チーズ捲形状については、繊維間摩擦が悪くなると、チーズ捲形状が悪くなる。加工工程での操業性安定化には、平滑性が必要である。弾性繊維と綿糸を交編する場合、風綿が弾性繊維に吸着して吸糸口に詰まり、吸糸口で糸切れが起こるため、たびたび清掃しなければいけない問題がある。本発明は弾性繊維に付与することで、制電性、解舒性、チーズ捲形状、平滑性に優れた弾性繊維が得られ、弾性繊維と綿糸の交編時に風綿吸着が少なく、細物弾性繊維と綿糸の高速編織加工が可能となる弾性繊維用処理剤及び該処理剤を用いて処理された弾性繊維を提供することを目的とする。 Since the treatment agent for elastic fibers uses hydrophobic base components such as silicone oil, mineral oil and ester oil, the antistatic property is insufficient. As for the cheese unwinding property, if the sticking property between fibers is strong, the cheese unwinding property is deteriorated. About cheese basket shape, when the friction between fibers worsens, cheese bowl shape will worsen. Smoothness is required to stabilize operability in the processing process. In the case of knitting elastic fibers and cotton yarns, there is a problem that the cotton must be cleaned frequently because the cotton is adsorbed to the elastic fibers and clogs the yarn suction port, causing yarn breakage at the yarn suction port. By applying to the elastic fiber, the present invention provides an elastic fiber excellent in antistatic property, unwinding property, cheese wrinkle shape, and smoothness. It is an object of the present invention to provide an elastic fiber treatment agent capable of high-speed knitting of elastic fibers and cotton yarn, and an elastic fiber treated with the treatment agent.
本発明は、Ｎ，Ｎ′−置換脂肪酸ビスアミド、Ｎ，Ｎ′−置換脂肪族ジアミド、Ｎ−置換脂肪酸アミドの平均粒子径を０．０１〜２０μｍの範囲に制御することにより、膠着防止性を向上させるとともに、その処理剤中での分散安定性を改善し、更には弾性糸に制電性、チーズ捲形状、平滑性、綿糸との交編時の風綿吸着防止の効果を付与できることを見出したものである。本発明は、平均粒子径が０．０１〜２０μｍである下記式１で表される化合物、平均粒子径が０．０１〜２０μｍである下記式２で表される化合物、平均粒子径が０．０１〜２０μｍである下記式３で表される化合物より選ばれる少なくとも一種以上を０．０１〜２０重量部使用し、ベース成分としてシリコーン油、鉱物油及びエステル油より選ばれる少なくとも一種以上を８０〜９９．９９重量部使用して構成される弾性繊維用処理剤である。
Ｒ１−Ｃ（Ｏ）−ＮＨ−Ｒ３−ＮＨ−Ｃ（Ｏ）−Ｒ２ （式１）
Ｒ４−ＮＨ−Ｃ（Ｏ）−Ｒ５−Ｃ（Ｏ）−ＮＨ−Ｒ６ （式２）
Ｒ７−ＮＨ−Ｃ（Ｏ）−Ｒ８ （式３）
（式１、式２、式３において、Ｒ１、Ｒ２、Ｒ４、Ｒ６、Ｒ７、Ｒ８は有機基を表し、Ｒ３、Ｒ５は炭素数１〜１０の脂肪族炭化水素基、置換基を有してもよい芳香族炭化水素基を表す。）
The present invention provides anti-sticking property by controlling the average particle size of N, N′-substituted fatty acid bisamide, N, N′-substituted aliphatic diamide, and N-substituted fatty acid amide within a range of 0.01 to 20 μm. In addition to improving the dispersion stability in the treatment agent, it is also possible to impart antistatic properties, cheese wrinkle shape, smoothness to the elastic yarn, and the effect of preventing fluff adsorption when knitting with cotton yarn It is what I found. The present invention relates to a compound represented by the following formula 1 having an average particle diameter of 0.01 to 20 μm, a compound represented by the following formula 2 having an average particle diameter of 0.01 to 20 μm, and an average particle diameter of 0.8. 0.01 to 20 parts by weight of at least one selected from compounds represented by the following formula 3 which is 01 to 20 μm is used, and at least one or more selected from silicone oil, mineral oil and ester oil as a base component is 80 to It is a processing agent for elastic fibers constituted by using 99.99 parts by weight.
R 1 —C (O) —NH—R 3 —NH—C (O) —R 2 (Formula 1)
R 4 —NH—C (O) —R 5 —C (O) —NH—R 6 (Formula 2)
R 7 —NH—C (O) —R 8 (Formula 3)
(Formula 1, Formula 2, in Formula 3, R 1, R 2, R 4, R 6, R 7, R 8 represents an organic group, R 3, R 5 is from 1 to 10 carbon atoms aliphatic hydrocarbon Represents an aromatic hydrocarbon group which may have a group or a substituent .
本発明は、上記式１〜３で表わされる化合物より選ばれる少なくとも一種以上の該化合物の分散効率と処理剤中での分散安定性を高めたり、処理剤の粘度を下げるために、シリコーン油／鉱物油とエステル油の総和＝１００／０〜１０／９０（重量比）からなるベース成分中に、上記式１〜３で表わされる化合物より選ばれる少なくとも一種以上の該化合物を、該ベース成分１００重量部当たり０．０１〜２０重量部攪拌混合し、分散剤としてアミノ変性シリコーン及び／又はアミノアルキルシリコーンレジンを該ベース成分／該分散剤＝９９．５／０．５〜８０／２０（重量比）の割合になるよう攪拌混合して、分散し、上記式１〜３で表わされる化合物より選ばれる少なくとも一種以上の該化合物が平均粒子径０．０１〜２０μｍになるように分散された弾性繊維用処理剤である。 In order to increase the dispersion efficiency and dispersion stability of at least one compound selected from the compounds represented by the above formulas 1 to 3 or to reduce the viscosity of the treatment agent, In the base component consisting of the sum of mineral oil and ester oil = 100/0 to 10/90 (weight ratio), at least one compound selected from the compounds represented by the above formulas 1 to 3 is added to the base component 100. 0.01 to 20 parts by weight per 1 part by weight is mixed with stirring, and the amino-modified silicone and / or aminoalkyl silicone resin is added as a dispersant to the base component / the dispersant = 99.5 / 0.5 to 80/20 (weight ratio). ) was stirred and mixed so that the ratio of the dispersed, at least one or more of the compounds selected from the compounds represented by the above formula 1-3 is an average particle diameter 0.01~20μm Sea urchin is distributed elastic fiber-processing agent.
本発明は、解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止の効果を高めるために、上記処理剤１００重量部に対し、ポリエーテル変性シリコーン、カルボキシ変性シリコーン、アミノ変性シリコーン、シリコーンレジン、高級脂肪酸の金属塩、有機スルホン酸化合物、有機硫酸化合物、有機カルボン酸アミン、有機リン酸エステルアミン塩、アミノ変性シリコーンの有機リン酸エステル中和物の少なくとも一種を更に０．０１〜１５重量部含有させた弾性繊維用処理剤が好ましい。
又、本発明の弾性繊維は、上記処理剤が弾性繊維に対して０．１〜１５重量％付与されていることを特徴とする。
本発明の処理剤の粘度は、好ましくは、３０℃における粘度が３〜３０ｍｍ２／Ｓである。３ｍｍ２／Ｓ未満では、処理剤の揮発が問題となり、３０ｍｍ２／Ｓを超えると平滑性に劣る場合がある。
The present invention is based on 100 parts by weight of the above-mentioned treatment agent, polyether-modified silicone, carboxy-modified silicone, amino-modified, in order to enhance the effect of unwinding property, antistatic property, cheese candy shape, smoothness, and fluff adsorption prevention. At least one of silicone, silicone resin, metal salt of higher fatty acid, organic sulfonic acid compound, organic sulfuric acid compound, organic carboxylic acid amine, organic phosphoric acid ester amine salt, and organic phosphoric acid ester neutralized product of amino-modified silicone is further reduced to 0.00. The processing agent for elastic fibers contained in an amount of 01 to 15 parts by weight is preferable.
The elastic fiber of the present invention is characterized in that the treatment agent is added in an amount of 0.1 to 15% by weight with respect to the elastic fiber.
As for the viscosity of the processing agent of this invention, Preferably, the viscosity in 30 degreeC is 3-30 mm < 2 > / S. If it is less than 3 mm 2 / S, volatilization of the treatment agent becomes a problem, and if it exceeds 30 mm 2 / S, the smoothness may be inferior.
本発明の処理剤を用いることにより、良好な解舒性、安定した制電性、良好なチーズ捲形状、良好な平滑性を弾性繊維に与えることができ、又、弾性繊維と綿糸との交編時の風綿吸着が少ないことによる糸切れ回数の減少で、編織機の稼働率向上及び編織物品位を向上させることができる。
又、処理剤の平均粒子径を一定範囲とすることで、処理剤自身の分散安定性が向上する。
更に、分散剤を用いることで、処理剤を効率よく粉砕調整でき、平均粒子径をより微小化し、処理剤の分散安定性をより向上させることができる。
By using the treatment agent of the present invention, it is possible to give the elastic fiber good unwinding property, stable antistatic property, good cheese bottle shape and good smoothness. A reduction in the number of yarn breakage due to a small amount of fluff adsorption during knitting can improve the operating rate of the knitting machine and improve the quality of the knitted fabric.
Moreover, the dispersion stability of processing agent itself improves by making the average particle diameter of processing agent into a fixed range.
Furthermore, by using a dispersant, the treatment agent can be pulverized and adjusted efficiently, the average particle size can be further reduced, and the dispersion stability of the treatment agent can be further improved.
本発明では、平均粒子径が０．０１〜２０μｍである式１で表される化合物、平均粒子径が０．０１〜２０μｍである式２で表される化合物、平均粒子径が０．０１〜２０μｍである式３で表される化合物より選ばれる少なくとも一種以上を０．０１〜２０重量部用いる。０．０１重量部未満では、解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止の効果が不十分であり、２０重量部を超えるとチーズ膠着防止効果が強くなり過ぎて、チーズ捲き形状が崩れ、形状不良となる。
式１で表される化合物、式２で表される化合物、及び式３で表される化合物の平均粒子径は、０．０１〜２０μｍ、好ましくは０．１〜５μｍである。０．０１μｍより小さいと、処理剤の粘度が高くなり、取り扱い性が悪くなったり、膠着防止性が低下することがある。２０μｍより大きいと、処理剤中における分散性が悪くなり、弾性繊維の加工工程等において、編針やガイドとの摩擦が大きくなることがある。上記の式１、式２及び式３で表されるＲ１、Ｒ２、Ｒ４、Ｒ６、Ｒ７、Ｒ８は、有機基であり、好ましくは、置換基を有してもよい炭素数１０〜３０のアルキル基及び、置換基を有してもよい炭素数１０〜３０のアルケニル基であり、更に好ましくは、置換基として水酸基を有してもよい炭素数１２〜２２のアルキル基及び、置換基として水酸基を有してもよい炭素数１２〜２２のアルケニル基である。上記の式１及び式２で表されるＲ３、Ｒ５は炭素数１〜１０の脂肪族炭化水素基、置換基を有してもよい芳香族炭化水素基であり、好ましくは、炭素数１〜８のアルキレン基及び、炭素数１〜８の置換基を有してもよい芳香族炭化水素基である。
本発明に好適な上記式１で表される化合物の具体例としては、Ｎ，Ｎ′−カプリン酸エチレンビスアミド、Ｎ，Ｎ′−ラウリン酸エチレンビスアミド、Ｎ−ラウリン酸−Ｎ′−ステアリン酸メチレンビスアミド、Ｎ−ミリスチン酸−Ｎ′−パルミチン酸エチレンビスアミド、Ｎ，Ｎ′−パルミチン酸ヘキサメチレンビスアミド、Ｎ，Ｎ′−ステアリン酸エチレンビスアミド、Ｎ，Ｎ′−オレイン酸エチレンビスアミド、Ｎ，Ｎ′−ステアリン酸メチレンビスアミド、Ｎ，Ｎ′−オレイン酸メチレンビスアミド、Ｎ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミド、Ｎ，Ｎ′−ステアリン酸ブチレンビスアミド、Ｎ，Ｎ′−イソステアリン酸エチレンビスアミド、Ｎ，Ｎ−ベヘン酸ヘキサメチレンビスアミド、Ｎ，Ｎ′−ヒドロキシステアリン酸ヘキサメチレンビスアミド、Ｎ，Ｎ′−ステアリン酸ヘキサメチレンビスアミド、Ｎ，Ｎ′−オレイン酸ヘキサメチレンビスアミド、Ｎ，Ｎ−リシノレイン酸ヘキサメチレンビスアミド、Ｎ−ステアリン酸−Ｎ′−オレイン酸エチレンビスアミド、Ｎ−オレイン酸−Ｎ′−ベヘン酸エチレンビスアミド、Ｎ，Ｎ′−ベヘン酸エチレンビスアミド、Ｎ，Ｎ′−ステアリン酸キシリレンビスアミド、Ｎ，Ｎ′−エルカ酸エチレンビスアミド、Ｎ，Ｎ′−リシノレイン酸エチレンビスアミド等のＮ，Ｎ′−置換脂肪酸ビスアミドが例示できる。特に好ましくは、Ｎ，Ｎ′−ステアリン酸エチレンビスアミド、Ｎ，Ｎ′−オレイン酸エチレンビスアミド、Ｎ，Ｎ′−ステアリン酸メチレンビスアミド、Ｎ，Ｎ′−オレイン酸メチレンビスアミド、Ｎ，Ｎ′−ステアリン酸ヘキサメチレンビスアミド、Ｎ，Ｎ′−オレイン酸ヘキサメチレンビスアミド、Ｎ，Ｎ′−ベヘン酸エチレンビスアミド、Ｎ，Ｎ′−ステアリン酸キシリレンビスアミド、Ｎ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドである。
式２で表される化合物の具体例としては、Ｎ，Ｎ′−ジオレイルアジピン酸アミド、Ｎ，Ｎ′−ジステアリルアジピン酸アミド、Ｎ，Ｎ′−ジオレイルセバシン酸アミド、Ｎ，Ｎ′−ジステアリルセバシン酸アミド、Ｎ，Ｎ′−ジステアリルテレフタル酸アミド、Ｎ，Ｎ′−ジステアリルイソフタル酸アミド、Ｎ−ラウリル−Ｎ′−ステアリルアジピン酸アミド、Ｎ−ステアリル−Ｎ′−オレイルセバシン酸アミド、Ｎ−ステアリル−Ｎ′−オレイルテレフタル酸アミド、Ｎ−ミリスチル−Ｎ′−パルミチルイソフタル酸アミド等のＮ，Ｎ′−置換脂肪族ジアミドが例示できる。特に好ましくは、Ｎ，Ｎ′−ジオレイルアジピン酸アミド、Ｎ，Ｎ′−ジステアリルアジピン酸アミド、Ｎ，Ｎ′−ジオレイルセバシン酸アミド、Ｎ，Ｎ′−ジステアリルセバシン酸アミド、Ｎ，Ｎ′−ジステアリルテレフタル酸アミド、Ｎ，Ｎ′−ジステアリルイソフタル酸アミド、Ｎ−ステアリル−Ｎ′−オレイルセバシン酸アミド、Ｎ−ステアリル−Ｎ′−オレイルテレフタル酸アミドである。
式３で表される化合物の具体例としては、Ｎ−ラウリルステアリン酸アミド、Ｎ−エイコサニルミリスチン酸アミド、Ｎ−パルミチルステアリン酸アミド、Ｎ−ステアリルステアリン酸アミド、Ｎ−オレイルパルミチン酸アミド、Ｎ−オレイルステアリン酸アミド、Ｎ−ステアリルベヘン酸アミド、Ｎ−ステアリルオレイン酸アミド、Ｎ−ステアリルエルカ酸アミド等のＮ−置換脂肪酸アミドが例示できる。特に好ましくは、Ｎ−パルミチルステアリン酸アミド、Ｎ−ステアリルステアリン酸アミド、Ｎ−オレイルステアリン酸アミド、Ｎ−ステアリルベヘン酸アミド、Ｎ−ステアリルエルカ酸アミドである。
In the present invention, the compound represented by Formula 1 having an average particle size of 0.01 to 20 μm, the compound represented by Formula 2 having an average particle size of 0.01 to 20 μm, and an average particle size of 0.01 to 0.01 to 20 parts by weight of at least one selected from the compound represented by Formula 3 which is 20 μm is used. If it is less than 0.01 parts by weight, the effects of unwinding, antistatic, cheese bottle shape, smoothness, and fluff adsorption prevention are insufficient, and if it exceeds 20 parts by weight, the cheese anti-sticking effect is too strong. , The cheese whispering shape collapses and the shape becomes defective.
The average particle diameter of the compound represented by Formula 1, the compound represented by Formula 2, and the compound represented by Formula 3 is 0.01 to 20 μm, preferably 0.1 to 5 μm. If it is smaller than 0.01 μm, the viscosity of the treatment agent becomes high, the handleability may be deteriorated, and the anti-sticking property may be lowered. When it is larger than 20 μm, the dispersibility in the treatment agent is deteriorated, and the friction with the knitting needle or the guide may be increased in the processing step of the elastic fiber. Formula 1 above, R 1, R 2, R 4 of formula 2 and formula 3, R 6, R 7, R 8 is an organic group, preferably an optionally substituted carbon An alkyl group having 10 to 30 carbon atoms and an alkenyl group having 10 to 30 carbon atoms which may have a substituent, and more preferably an alkyl group having 12 to 22 carbon atoms which may have a hydroxyl group as a substituent; And it is a C12-C22 alkenyl group which may have a hydroxyl group as a substituent. R 3 and R 5 represented by the above formulas 1 and 2 are an aliphatic hydrocarbon group having 1 to 10 carbon atoms and an aromatic hydrocarbon group which may have a substituent, preferably a carbon number. It is an aromatic hydrocarbon group which may have a 1-8 alkylene group and a C1-C8 substituent.
Specific examples of the compound represented by the above formula 1 suitable for the present invention include N, N'-capric acid ethylene bisamide, N, N'-lauric acid ethylene bisamide, N-lauric acid-N'-methylene stearate. Bisamide, N-myristic acid-N′-palmitic acid ethylene bisamide, N, N′-palmitic acid hexamethylene bisamide, N, N′-stearic acid ethylene bisamide, N, N′-oleic acid ethylene bisamide, N, N ′ -Stearic acid methylene bisamide, N, N'-oleic acid methylene bisamide, N, N'-12-hydroxystearic acid ethylene bisamide, N, N'-stearic acid butylene bisamide, N, N'-isostearic acid ethylene bisamide, N , N-Behenic acid hexamethylenebisamide, N, N'-hydroxy Tearic acid hexamethylene bisamide, N, N'-stearic acid hexamethylene bisamide, N, N'-oleic acid hexamethylene bisamide, N, N-ricinoleic acid hexamethylene bisamide, N-stearic acid-N'-oleic acid ethylene bisamide N-oleic acid-N'-behenic acid ethylene bisamide, N, N'-behenic acid ethylene bisamide, N, N'-stearic acid xylylene bisamide, N, N'-erucic acid ethylene bisamide, N, N'- Examples thereof include N, N′-substituted fatty acid bisamides such as ricinoleic acid ethylene bisamide. Particularly preferred are N, N'-stearic acid ethylene bisamide, N, N'-oleic acid ethylene bisamide, N, N'-stearic acid methylene bisamide, N, N'-oleic acid methylene bisamide, N, N'-stearin. Acid hexamethylene bisamide, N, N'-oleic acid hexamethylene bisamide, N, N'-behenic acid ethylene bisamide, N, N'-stearic acid xylylene bisamide, N, N'-12-hydroxystearic acid ethylene bisamide is there.
Specific examples of the compound represented by the formula 2 include N, N′-dioleyl adipic acid amide, N, N′-distearyl adipic acid amide, N, N′-dioleyl sebacic acid amide, N, N ′. -Distearyl sebacic acid amide, N, N'-distearyl terephthalic acid amide, N, N'-distearyl isophthalic acid amide, N-lauryl-N'-stearyl adipic acid amide, N-stearyl-N'-oleyl sebacin Examples thereof include N, N′-substituted aliphatic diamides such as acid amide, N-stearyl-N′-oleyl terephthalic acid amide, N-myristyl-N′-palmitylisophthalic acid amide. Particularly preferably, N, N′-dioleyl adipate amide, N, N′-distearyl adipate amide, N, N′-dioleyl sebacinate amide, N, N′-distearyl sebacinate amide, N, N'-distearyl terephthalic acid amide, N, N'-distearyl isophthalic acid amide, N-stearyl-N'-oleyl sebacic acid amide, N-stearyl-N'-oleyl terephthalic acid amide.
Specific examples of the compound represented by Formula 3 include N-lauryl stearamide, N-eicosanyl myristate amide, N-palmityl stearamide, N-stearyl stearamide, N-oleyl palmitate And N-substituted fatty acid amides such as N-oleyl stearic acid amide, N-stearyl behenic acid amide, N-stearyl oleic acid amide, N-stearyl erucic acid amide. Particularly preferred are N-palmityl stearamide, N-stearyl stearamide, N-oleyl stearamide, N-stearyl behenamide, N-stearyl erucamide.
式１で表される化合物、式２で表される化合物、そして式３で表される化合物は、例えばホモミキサー、コロイドミル、サンドミル、ビスコミル、ダイノーミル、コボールミル等のような高剪断性の混合または粉砕装置中で、平均粒子径については、特に限定はしないが、通常、市販されている平均粒子径が３０〜２００μｍ程度の式１で表される化合物及び式２で表される化合物及び式３で表される化合物を、処理剤のベース成分でもあるシリコーン油、鉱物油及びエステル油より選ばれる少なくとも一種以上と共に入れ、攪拌混合することにより調整できると共に、この処理により、式１で表される化合物及び式２で表される化合物及び式３で表される化合物の平均粒子径を本発明にとって必要な０．０１〜２０μｍに粉砕調整することができる。平均粒子径の調整は混合または粉砕装置の回転速度、攪拌羽根の形状及び処理時間を選定することにより行うことができる。経済性の面からより好ましい装置はビスコミル、ダイノーミル、またはコボールミルである。 The compound represented by the formula 1, the compound represented by the formula 2, and the compound represented by the formula 3 are mixed with a high shearing force such as a homomixer, a colloid mill, a sand mill, a visco mill, a dyno mill, a coball mill or the like. In the pulverizer, the average particle size is not particularly limited, but usually, the commercially available compound represented by Formula 1 having an average particle size of about 30 to 200 μm, the compound represented by Formula 2, and Formula 3 The compound represented by the formula (1) can be prepared by adding together with at least one selected from silicone oil, mineral oil and ester oil, which is also the base component of the treating agent, and stirring and mixing. Adjusting the average particle size of the compound, the compound represented by Formula 2 and the compound represented by Formula 3 to 0.01 to 20 μm necessary for the present invention. it can. The average particle diameter can be adjusted by selecting the rotational speed of the mixing or pulverizing apparatus, the shape of the stirring blade, and the treatment time. A more preferable apparatus from the economical aspect is a visco mill, a dyno mill, or a coball mill.
本発明では、下記式１で表される化合物、下記式２で表される化合物、下記式３で表される化合物より選ばれる少なくとも一種以上を、シリコーン油／鉱物油とエステル油の総和＝１００／０〜１０／９０（重量比）からなるベース成分１００重量部当たり０．０１〜２０重量部使用し、該ベース成分／分散剤＝９９．５／０．５〜８０／２０（重量比）の割合でアミノ変性シリコーン及び／又はアミノアルキルシリコーンレジンからなる該分散剤を使用し、該ベース成分及び該分散剤と混合または粉砕装置で攪拌混合することにより、調整できると共に、この処理により、下記の式１で表される化合物及び式２で表される化合物及び式３で表される化合物の平均粒子径を本発明にとって必要な０．０１〜２０μｍに効率よく、粉砕調整することができる。０．０１重量部未満では、解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止の効果が不十分であり、少量であるため、分散処理の経済性が悪く、２０重量部を超えるとチーズ膠着防止効果が強くなり過ぎて、チーズ捲き形状が崩れ、形状不良となる。
該ベース成分のシリコーン油／鉱物油とエステル油の総和の重量比について、シリコーン油の重量比が１０未満では、アミノ変性シリコーン及び／又はアミノアルキルシリコーンレジンからなる該分散剤が該ベース成分に相溶し難い場合があり、充分な分散効果が得られない。
該ベース成分／該分散剤の重量比について、該分散剤の重量比が０．５未満では、平均粒子径の微小化や微小化に伴う増粘の抑制などの分散効果が不十分であり、２０を超えると本来の目的である分散効果に対し、過剰量となり、不経済である。本発明で分散剤として用いられるアミノ変性シリコーンは、下記式４で表わされるアミノアルキル基含有オルガノポリシロキサンが好ましい。
Ｒ９（Ｒ１０）２ＳｉＯ−［（Ｒ１０）２ＳｉＯ］ｋ−［（Ｒ１０Ｒ１１）ＳｉＯ］ｌ−ＳｉＲ９（Ｒ１０）２ （式４）
（式中、Ｒ９はＨ２Ｎ（ＣＨ２）３−、１価炭化水素基、アルコキシ基から選択される基、Ｒ１０は１価炭化水素基又はアルコキシ基、Ｒ１１は１価炭化水素基、Ｈ２Ｎ（ＣＨ２）３−、Ｈ２Ｎ（ＣＨ２）２ＮＨ（ＣＨ２）３−から選択される基、ｋは５〜１０，０００の正数、ｌは０．１〜４００の正数）
上記式４中、Ｒ９、Ｒ１０、Ｒ１１はそのうちの少なくとも一つ以上はＨ２Ｎ（ＣＨ２）３−及び／又はＨ２Ｎ（ＣＨ２）２ＮＨ（ＣＨ２）３−であり、これらのアルキルアミノ基を含有することにより、処理剤中での式１〜３の化合物の分散安定性向上と平均粒子径を微小化する効果が得られる。
Ｒ９はＨ２Ｎ（ＣＨ２）３−、１価炭化水素基、アルコキシ基から選択される基を表し、好ましくは、Ｈ２Ｎ（ＣＨ２）３−、メチル基、メトキシ基である。Ｒ１０は１価炭化水素基又はアルコキシ基を表し、好ましくは、メチル基、メトキシ基である。Ｒ１１は１価炭化水素基、Ｈ２Ｎ（ＣＨ２）３−、Ｈ２Ｎ（ＣＨ２）２ＮＨ（ＣＨ２）３−から選択される基を表し、好ましくは、メチル基、Ｈ２Ｎ（ＣＨ２）３−、Ｈ２Ｎ（ＣＨ２）２ＮＨ（ＣＨ２）３−である。
ｋとｌの総和が５．１未満では、揮発性が問題となることがあり、ｋが１０，０００を超え、且つｌが４００を超える場合は、処理剤の粘度が高くなり、平滑性に悪影響を及ぼす。
本発明で分散剤として用いられるアミノアルキルシリコーンレジンは、下記式５で表わされるものが好ましい。
〔（Ｈ２ＮＲ１２ＮＨＲ１３ＳｉＯ１．５）ｎ（Ｒ１４ＳｉＯ１．５）ｍ〕ｔ （式５）
（式中、Ｒ１２は炭素数１〜３の側鎖を有していてもよい炭化水素基、Ｒ１３は炭素数１〜５の側鎖を有していてもよい炭化水素基、Ｒ１４は炭素数４〜１０の側鎖を有していてもよい飽和または不飽和の炭化水素基、ｎは０．１〜０．５の正数、ｍは０．５〜０．９の正数であり、ｎ＋ｍ＝１。ｔは５〜５０の正数を表わす）
上記式５中、Ｒ１２はメチレン、エチレン、トリメチレン、プロピレン、ビニレン等の炭素数１〜３の炭化水素基を表す。好ましくはエチレンである。
Ｒ１３はメチレン、エチレン、トリメチレン、テトラメチレン、ペンタメチレン、プロピレン、シクロペンチレン、ビニレン等の炭素数１〜５の炭化水素基、好ましくはプロピレンである。Ｒ１４はｎ−ブチル、ｔｅｒｔ−ブチル、ｓｅｃ−ブチル、ペンチル、ヘキシル、オクチル、２−エチルヘキシル、デシル、シクロペンチル、シクロヘキシル、ベンジル、フェニル等の側鎖や不飽和基を有していてもよいアルキル、アリール、アラルキル、シクロアルキル等から選ばれた炭素数４〜１０の炭化水素基、好ましくは側鎖を有していてもよいアルキル基である。ｎは０．１〜０．５、好ましくは０．１〜０．２であり、ｍは０．５〜０．９、好ましくは０．８〜０．９である。ｎ＋ｍ＝１である。ｔは５〜５０、より好ましくは３０〜４０である。この範囲において、処理剤中での上記式１〜３の化合物の分散安定性向上と平均粒子径を微小化する効果が得られる。
In the present invention, at least one or more selected from the compound represented by the following formula 1, the compound represented by the following formula 2, and the compound represented by the following formula 3 is the sum of silicone oil / mineral oil and ester oil = 100. 0.01 to 20 parts by weight per 100 parts by weight of the base component consisting of / 0 to 10/90 (weight ratio), and the base component / dispersant = 99.5 / 0.5 to 80/20 (weight ratio) By using the dispersant comprising the amino-modified silicone and / or aminoalkylsilicone resin at a ratio of, and mixing with the base component and the dispersant or stirring and mixing in a pulverizer, The average particle diameter of the compound represented by Formula 1 and the compound represented by Formula 2 and the compound represented by Formula 3 is efficiently adjusted to 0.01 to 20 μm necessary for the present invention. Door can be. If the amount is less than 0.01 parts by weight, the effects of unwinding property, antistatic property, cheese cake shape, smoothness, and fluff adsorption prevention are insufficient, and since the amount is small, the economics of dispersion treatment is poor, and 20 weights. If it exceeds the part, the cheese anti-sticking effect becomes too strong, the cheese whispering shape collapses, and the shape becomes defective.
When the weight ratio of the silicone oil / mineral oil and ester oil of the base component is less than 10, the dispersant comprising the amino-modified silicone and / or aminoalkyl silicone resin is compatible with the base component. It may be difficult to dissolve, and a sufficient dispersion effect cannot be obtained.
With respect to the weight ratio of the base component / the dispersant, if the weight ratio of the dispersant is less than 0.5, the dispersion effect such as the suppression of the increase in viscosity due to the miniaturization of the average particle diameter and the miniaturization is insufficient. If it exceeds 20, the amount is excessive with respect to the original dispersion effect, which is uneconomical. The amino-modified silicone used as a dispersant in the present invention is preferably an aminoalkyl group-containing organopolysiloxane represented by the following formula 4.
R 9 (R 10) 2 SiO - [(R 10) 2 SiO] k - [(R 10 R 11) SiO] l-SiR 9 (R 10) 2 ( Equation 4)
(Wherein R 9 is a group selected from H 2 N (CH 2 ) 3 —, a monovalent hydrocarbon group and an alkoxy group, R 10 is a monovalent hydrocarbon group or an alkoxy group, and R 11 is a monovalent hydrocarbon. A group selected from the group H 2 N (CH 2 ) 3 —, H 2 N (CH 2 ) 2 NH (CH 2 ) 3 —, k is a positive number of 5 to 10,000, and l is 0.1 to 0.1 400 positive number)
In the above formula 4, at least one of R 9 , R 10 and R 11 is H 2 N (CH 2 ) 3 — and / or H 2 N (CH 2 ) 2 NH (CH 2 ) 3 —. By containing these alkylamino groups, the effects of improving the dispersion stability of the compounds of formulas 1 to 3 in the treating agent and reducing the average particle size can be obtained.
R 9 represents a group selected from H 2 N (CH 2 ) 3 —, a monovalent hydrocarbon group, and an alkoxy group, and preferably H 2 N (CH 2 ) 3 —, a methyl group, and a methoxy group. R 10 represents a monovalent hydrocarbon group or an alkoxy group, preferably a methyl group or a methoxy group. R 11 represents a group selected from a monovalent hydrocarbon group, H 2 N (CH 2 ) 3 —, H 2 N (CH 2 ) 2 NH (CH 2 ) 3 —, preferably a methyl group, H 2 N (CH 2 ) 3 —, H 2 N (CH 2 ) 2 NH (CH 2 ) 3 —.
When the sum of k and l is less than 5.1, volatility may be a problem. When k exceeds 10,000 and l exceeds 400, the viscosity of the treatment agent increases and smoothness is improved. Adversely affect.
The aminoalkyl silicone resin used as a dispersant in the present invention is preferably represented by the following formula 5.
[(H 2 NR 12 NHR 13 SiO 1.5 ) n (R 14 SiO 1.5 ) m ] t (Formula 5)
(In the formula, R 12 is a hydrocarbon group which may have a side chain having 1 to 3 carbon atoms, R 13 is a hydrocarbon group which may have a side chain having 1 to 5 carbon atoms, R 14. Is a saturated or unsaturated hydrocarbon group which may have a side chain having 4 to 10 carbon atoms, n is a positive number of 0.1 to 0.5, and m is a positive number of 0.5 to 0.9. N + m = 1, t represents a positive number of 5 to 50)
Among the above formula 5, R 12 represents a methylene, ethylene, trimethylene, propylene, a hydrocarbon group having 1 to 3 carbon atoms such as vinylene. Ethylene is preferable.
R 13 is a hydrocarbon group having 1 to 5 carbon atoms such as methylene, ethylene, trimethylene, tetramethylene, pentamethylene, propylene, cyclopentylene, vinylene, preferably propylene. R 14 is n-butyl, tert-butyl, sec-butyl, pentyl, hexyl, octyl, 2-ethylhexyl, decyl, cyclopentyl, cyclohexyl, benzyl, phenyl or any other alkyl which may have an unsaturated group. , A hydrocarbon group having 4 to 10 carbon atoms selected from aryl, aralkyl, cycloalkyl and the like, preferably an alkyl group optionally having a side chain. n is 0.1 to 0.5, preferably 0.1 to 0.2, and m is 0.5 to 0.9, preferably 0.8 to 0.9. n + m = 1. t is 5 to 50, more preferably 30 to 40. Within this range, an effect of improving the dispersion stability of the compounds of the above formulas 1 to 3 in the treating agent and miniaturizing the average particle diameter can be obtained.
本発明において、平均粒子径は、処理剤をベース成分で希釈し、バッチセルを用いて粒度分布測定装置「ＬＡ−９１０」（堀場製作所製）により測定するか、デジタルマイクロスコープ「ＶＨ−７０００」（キーエンス社製）で測定する。 In the present invention, the average particle size is measured by diluting the treatment agent with the base component and measuring it with a particle size distribution measuring apparatus “LA-910” (manufactured by Horiba, Ltd.) using a batch cell, or digital microscope “VH-7000” ( Measured by Keyence Corporation).
本発明の処理剤には、解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止の効果を高めるために、高級脂肪酸の金属塩、有機スルホン酸化合物、有機硫酸化合物、有機リン酸エステルアミン塩、アミノ変性シリコーンの有機リン酸エステル中和物が０．０１〜１５重量部添加されていても良い。高級脂肪酸の金属塩としては、従来より、弾性繊維に用いられている公知のものを用いることができ、ステアリン酸Ａｌ、ステアリン酸Ｃａ、ステアリン酸Ｍｇ、ステアリン酸Ｂａ、ステアリン酸亜鉛等が好ましい。 In the treatment agent of the present invention, a metal salt of a higher fatty acid, an organic sulfonic acid compound, an organic sulfuric acid compound, organic, 0.01-15 parts by weight of phosphoric acid ester amine salt and neutralized organic phosphoric acid ester of amino-modified silicone may be added. As the metal salt of higher fatty acid, known ones conventionally used for elastic fibers can be used, and Al stearate, Ca stearate, Mg stearate, Ba stearate, zinc stearate and the like are preferable.
本発明の処理剤には、解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止の効果を高めるために、従来の公知の変性シリコーン（アルキル変性シリコーン、エステル変性シリコーン、ポリエーテル変性シリコーン、カルビノール変性シリコーン、カルボキシ変性シリコーン、メルカプト変性シリコーン、リン酸変性シリコーン、エポキシ変性シリコーン、式：Ｒ１５Ｒ１６Ｒ１７ＳｉＯ１／２（式中、Ｒ１５、Ｒ１６、Ｒ１７は一価炭化水素基である。）で示されるシロキサン単位と式：ＳｉＯ２で示されるシロキサン単位とからなるオルガノポリシロキサン樹脂、式：Ｒ１５Ｒ１６Ｒ１７ＳｉＯ１／２（式中、Ｒ１５、Ｒ１６、Ｒ１７は一価炭化水素基である。）で示されるシロキサン単位と式：ＳｉＯ２で示されるシロキサン単位及び式：Ｒ１８ＳｉＯ３／２（式中、Ｒ１８は一価炭化水素基である。）で示されるシロキサン単位からなるオルガノポリシロキサン樹脂、式：Ｒ１８ＳｉＯ３／２（式中、Ｒ１８は一価炭化水素基である。）で示されるシロキサン単位からなるオルガノポリシロキサン樹脂等）や制電剤、つなぎ剤、酸化防止剤、紫外線吸収剤等、通常弾性繊維の処理剤に用いられる成分を配合することができる。 In the treatment agent of the present invention, conventionally known modified silicones (alkyl-modified silicones, ester-modified silicones, polyesters) are used in order to enhance the effects of unwinding properties, antistatic properties, cheese candy shape, smoothness, and fluff adsorption prevention. ether-modified silicone, carbinol Roh Lumpur modified silicone, carboxy-modified silicones, mercapto-modified silicone, phosphate-modified silicone, epoxy-modified silicone, wherein: R 15 R 16 R 17 SiO 1/2 ( wherein, R 15, R 16, R 17 is a monovalent hydrocarbon group) and an organopolysiloxane resin comprising a siloxane unit represented by the formula: SiO 2 and a formula: R 15 R 16 R 17 SiO 1/2 (wherein , R 15 , R 16 , and R 17 are monovalent hydrocarbon groups) and the formula: SiO 2 Siloxane units and formula that: R 18 SiO 3/2 (. Wherein, R 18 is a monovalent hydrocarbon group) consisting of siloxane units represented by the organopolysiloxane resin, the formula: R 18 SiO 3/2 (wherein R 18 is a monovalent hydrocarbon group.) Organopolysiloxane resin comprising siloxane units represented by the following formula)), antistatic agents, binders, antioxidants, ultraviolet absorbers, etc. Ingredients used in can be blended.
本発明の弾性繊維は、上記処理剤が弾性繊維に対して０．１〜１５重量％付与されていることを特徴とする。 The elastic fiber of the present invention is characterized in that 0.1 to 15% by weight of the treatment agent is applied to the elastic fiber.
以下実施例により本発明を具体的に説明する。
なお具体例における、各特性の評価は次の方法に従って行った。
（油剤の作用効果の評価法）
粘度：キャノンフェンスケ粘度計を用い、一定温度（例えば、２５℃、３０℃）における試料液の動粘度を求めた。
The present invention will be specifically described below with reference to examples.
In addition, evaluation of each characteristic in a specific example was performed according to the following method.
(Method for evaluating the effect of oil)
Viscosity: Using a Canon Fenceke viscometer, the kinematic viscosity of the sample solution at a constant temperature (for example, 25 ° C., 30 ° C.) was determined.
アミン価：イソプロピルアルコール、キシレン／イソプロピルアルコール（１／１）混合等の溶剤に溶解した試料を、０．１Ｎ−ＨＣｌエチレングリコール／イソプロピルアルコール溶液で自動電位差滴定装置（平沼社製ＣＯＭ−９００）を使用して電位差滴定して、終点の滴定量（ｍｌ）を測定し、下式６よりアミン価を算出した。尚、アミン価とは試料１ｇを中和するのに要するＨＣｌと当量となるＫＯＨのｍｇ数で表されるものである。
アミン価（ＫＯＨｍｇ／ｇ）＝（Ａ×Ｆ×５．６１）／Ｗ （式６）
（式６において、Ａ＝滴定量（ｍｌ）、Ｆ＝０．１Ｎ−ＨＣｌの力価、Ｗ＝試料重量（ｇ））
Amine value: A sample dissolved in a solvent such as isopropyl alcohol, xylene / isopropyl alcohol (1/1) mixture, etc. is subjected to an automatic potentiometric titrator (COM-900 manufactured by Hiranuma Co., Ltd.) with a 0.1N HCl ethylene glycol / isopropyl alcohol solution. Using the potentiometric titration, the titration amount (ml) at the end point was measured, and the amine value was calculated from the following formula 6. The amine value is expressed in mg of KOH equivalent to HCl required to neutralize 1 g of the sample.
Amine value (KOHmg / g) = (A × F × 5.61) / W (Formula 6)
(In Formula 6, A = titer (ml), F = 0.1 N-HCl titer, W = sample weight (g))
ローラー静電気：図１において、解舒速度比測定機の解舒側に処理剤を付与した繊維のチーズ（１）をセットし、５０ｍ／分の周速で回転させ、チーズ上２ｃｍのところにおいて、春日式電位差測定装置（２）で、回転を始めて１時間後の発生静電気を測定する。 Roller static electricity: In FIG. 1, set the fiber cheese (1) to which the treatment agent is applied on the unwinding side of the unwinding speed ratio measuring machine, rotate it at a peripheral speed of 50 m / min, and at 2 cm above the cheese, With the Kasuga-type potentiometer (2), the generated static electricity 1 hour after the start of rotation is measured.
編成張力：図２において、チーズ（３）から縦取りした弾性糸（４）をコンペンセーター（５）を経てローラー（６）、編み針（７）を介して、Ｕゲージ（８）に付したローラー（９）を経て速度計（１０）、巻き取りローラー（１１）に連結する。速度計（１０）での走行速度が定速（例えば、１０ｍ／分、１００ｍ／分）になるように巻き取りローラーの回転速度を調整して、巻き取りローラーに巻き取り、そのときの編成張力をＵゲージ（８）で測定し、繊維／編み針間の摩擦（ｇ）を計測する。走行糸条より１ｃｍのところで春日式電位差測定装置（１２）で発生静電気を測定する。 Knitting tension: In FIG. 2, a roller in which an elastic yarn (4) vertically taken from cheese (3) is attached to a U gauge (8) via a compensator (5) and a roller (6) and a knitting needle (7). It connects with a speedometer (10) and a winding roller (11) through (9). The rotational speed of the take-up roller is adjusted so that the traveling speed of the speedometer (10) becomes a constant speed (for example, 10 m / min, 100 m / min), and the knitting tension at that time is taken up by the take-up roller. Is measured with a U gauge (8), and the friction (g) between the fibers / knitting needles is measured. The generated static electricity is measured with a Kasuga-type potentiometer (12) at a distance of 1 cm from the running yarn.
繊維間摩擦係数（Ｆ／ＦμＳ）：図３において、処理剤が付与された弾性繊維のモノフィラメントを５０〜６０ｃｍ程取り、一方の端に荷重Ｔ１（１３）を吊り、ローラー（１４）を介して、Ｕゲージ（１５）にもう一方の端を掛けて定速（例えば、３ｃｍ／分）で引っ張り、そのときの２次張力Ｔ２をＵゲージ（１５）で測定し、式７により、繊維間摩擦係数を求める。
摩擦係数（Ｆ／ＦμＳ）＝１／θ・ｌｎ（Ｔ２／Ｔ１） （式７）
（式７において、θ＝２π、ｌｎ＝自然対数、Ｔ１は２２ｄｔｅｘ当り１ｇ）
Friction coefficient between fibers (F / FμS): In FIG. 3, take about 50 to 60 cm of an elastic fiber monofilament provided with a treatment agent, suspend a load T1 (13) at one end, and pass through a roller (14). The other end is put on the U gauge (15) and pulled at a constant speed (for example, 3 cm / min), and the secondary tension T2 at that time is measured with the U gauge (15). Find the coefficient.
Friction coefficient (F / FμS) = 1 / θ · ln (T2 / T1) (Expression 7)
(In Equation 7, θ = 2π, ln = natural logarithm, T1 is 1 g per 22 dtex)
チーズ捲形状（捲き崩れ有無）：評価に供する処理剤が付与されたモノフィラメントチーズ（巻き量４００ｇ）の捲形状にバルジや綾等の捲き崩れが有るか無いかを目視で確認した。 Cheese cocoon shape (whether crushed or not): It was visually confirmed whether or not the cocoon shape of monofilament cheese (rolling amount 400 g) provided with a treatment agent used for evaluation had crushed pieces such as bulges and twills.
風綿吸着試験法：図４においてチーズ（１６）から２０ｍ／分の速度で弾性糸を出し、コンペンセーター（１７）を経てローラー（１８）から風綿の吸糸口（１９）を経て巻取ローラー（２０）で８０ｍ／分で巻取る。綿糸（２１）は、ガイド（２２）からローラー（２３）と編針（２４）を経て巻取ローラー（２５）で８０ｍ／分の速度で巻取られる。風綿はローラー（２３）と編針（２４）の間で綿糸を１回撚りでこすり合わせて発生させる。６０分間弾性繊維を走行させたときの吸糸口に集積する風綿の重量を測定する。弾性繊維及び綿糸は２０℃、４５％ＲＨの雰囲気下で３日間調湿したものを用いた。測定雰囲気は２０℃、４５％ＲＨで行った。吸糸口は、直径０．２ｍｍ、長さ１０ｍｍ、その材質はアルミナである。 Fluff adsorption test method: In FIG. 4, the elastic yarn is drawn out from the cheese (16) at a speed of 20 m / min, passed through the compensator (17), from the roller (18) through the fluff sucking port (19) and the winding roller. Wind at 80 m / min in (20). The cotton yarn (21) is wound from the guide (22) through the roller (23) and the knitting needle (24) by the winding roller (25) at a speed of 80 m / min. Cotton is generated by rubbing the cotton yarn once by twisting between the roller (23) and the knitting needle (24). The weight of the fluff accumulated at the yarn suction port when the elastic fiber is run for 60 minutes is measured. Elastic fibers and cotton yarns were conditioned for 3 days in an atmosphere of 20 ° C. and 45% RH. The measurement atmosphere was 20 ° C. and 45% RH. The yarn suction port has a diameter of 0.2 mm, a length of 10 mm, and the material thereof is alumina.
解舒速度比：図５において、解舒速度比測定機の解舒側に処理剤を付与した繊維のチーズ（２６）をセットし、巻き取り側に紙管（２７）をセットする。巻き取り速度を一定速度にセットした後、ローラー（２８）及び（２９）を同時に起動させる。この状態では糸（３０）に張力はほとんどかからないため、糸はチーズ上で膠着して離れないので、解舒点（３１）は図５に示す状態にある。解舒速度を変えることによって、チーズからの糸（３０）の解舒点（３１）が変わるので、この点がチーズとローラーとの接点（３２）と一致するように解舒速度を設定する。解舒速度比は式８によって求める。この値が小さいほど、解舒性が良いことを示す。
解舒速度比（％）＝（巻取速度−解舒速度）÷解舒速度Ｘ１００（式８）
Unwinding speed ratio: In FIG. 5, the fiber cheese (26) to which the treatment agent is applied is set on the unwinding side of the unwinding speed ratio measuring machine, and the paper tube (27) is set on the winding side. After setting the winding speed to a constant speed, the rollers (28) and (29) are activated simultaneously. In this state, since the tension is hardly applied to the yarn (30), the yarn is stuck on the cheese and does not leave, so the unwinding point (31) is in the state shown in FIG. By changing the unwinding speed, the unwinding point (31) of the yarn (30) from the cheese changes, and the unwinding speed is set so that this point coincides with the contact point (32) between the cheese and the roller. The unraveling speed ratio is obtained by Equation 8. The smaller this value is, the better the unpacking property is.
Unwinding speed ratio (%) = (winding speed−unwinding speed) ÷ unwinding speed X100 (Equation 8)
分散安定性：処理剤を１００ｍｌのすり栓付き試験管に入れ、２５℃にて１ヶ月又は６ヶ月静置した後、処理剤の外観を観察し、下記の基準で評価した。○：透明な層や沈澱が無い。 △：透明な層がある。 ×：沈澱がある。 Dispersion stability: The treatment agent was placed in a 100 ml test tube with a stopper and allowed to stand at 25 ° C. for 1 month or 6 months, and then the appearance of the treatment agent was observed and evaluated according to the following criteria. ○: There is no transparent layer or precipitation. Δ: There is a transparent layer. X: There is precipitation.
処理剤−１の調製：Ｎ，Ｎ′−ステアリン酸エチレンビスアミド（平均粒子径５０μｍ）２重量部を、２５℃における粘度が５ｍｍ２／ｓのシリコーン油９８重量部に分散し、この液をビスコミルＣＶＭ−２（五十嵐機械社製）に通してＮ，Ｎ′−ステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸エチレンビスアミドの平均粒子径は０．７μｍであった。 Preparation of Treatment Agent-1: 2 parts by weight of N, N′-stearic acid ethylene bisamide (average particle size 50 μm) is dispersed in 98 parts by weight of silicone oil having a viscosity of 5 mm 2 / s at 25 ° C. N, N′-stearic acid ethylene bisamide was pulverized through CVM-2 (manufactured by Igarashi Machine Co., Ltd.). The average particle diameter of the obtained N, N′-stearic acid ethylenebisamide was 0.7 μm.
処理剤−２の調製：Ｎ，Ｎ′−ジステアリルテレフタル酸アミド（平均粒子径５０μｍ）１重量部を、３０秒の流動パラフィン９９重量部に分散し、この液をビスコミルＣＶＭ−２（五十嵐機械社製）に通してＮ，Ｎ′−ジステアリルテレフタル酸アミドを粉砕した。得られたＮ，Ｎ′−ジステアリルテレフタル酸アミドの平均粒子径は０．７μｍであった。 Preparation of Treatment Agent-2: 1 part by weight of N, N′-distearyl terephthalic acid amide (average particle size 50 μm) was dispersed in 99 parts by weight of liquid paraffin for 30 seconds, and this liquid was added to Viscomil CVM-2 (Igarashi Machinery Co., Ltd.). N, N'-distearyl terephthalic amide was pulverized. The average particle size of the obtained N, N′-distearyl terephthalic acid amide was 0.7 μm.
処理剤−３の調製：Ｎ，Ｎ′−ステアリン酸エチレンビスアミド（平均粒子径５０μｍ）１重量部とＮ−ステアリルベヘン酸アミド（平均粒子径５０μｍ）１重量部を、イソオクチルラウレート９８重量部に分散し、この液をビスコミルＣＶＭ−２（五十嵐機械社製）に通してＮ，Ｎ′−ステアリン酸エチレンビスアミドとＮ−ステアリルベヘン酸アミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸エチレンビスアミドとＮ−ステアリルベヘン酸アミドの平均粒子径は共に０．７μｍであった。 Preparation of Treatment Agent-3: 1 part by weight of N, N′-stearic acid ethylenebisamide (average particle size 50 μm) and 1 part by weight of N-stearyl behenamide (average particle size 50 μm), 98 parts by weight of isooctyl laurate Then, this liquid was passed through Viscomil CVM-2 (manufactured by Igarashi Machinery Co., Ltd.) to grind N, N′-stearic acid ethylene bisamide and N-stearyl behenic acid amide. The obtained N, N′-stearic acid ethylene bisamide and N-stearyl behenic acid amide both had an average particle size of 0.7 μm.
処理剤−４の調製：Ｎ，Ｎ′−ステアリン酸エチレンビスアミド（平均粒子径５０μｍ）５重量部とＮ，Ｎ′−ジステアリルアジピン酸アミド（平均粒子径５０μｍ）５重量部を、４０秒の流動パラフィン６０重量部、イソオクチルラウレート３０重量部に分散し、この液をビスコミルＣＶＭ−２（五十嵐機械社製）に通してＮ，Ｎ′−ステアリン酸エチレンビスアミドとＮ，Ｎ′−ジステアリルアジピン酸アミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸エチレンビスアミドとＮ，Ｎ′−ジステアリルアジピン酸アミドの平均粒子径は共に０．９μｍであった。 Preparation of Treatment Agent-4: 5 parts by weight of N, N′-stearic acid ethylenebisamide (average particle size 50 μm) and 5 parts by weight of N, N′-distearyl adipic acid amide (average particle size 50 μm) were added for 40 seconds. Disperse in 60 parts by weight of liquid paraffin and 30 parts by weight of isooctyl laurate, and pass this solution through Viscomil CVM-2 (manufactured by Igarashi Kikai Co., Ltd.). N, N'-stearic acid ethylene bisamide and N, N'-distearyl Adipic amide was ground. The obtained N, N′-stearic acid ethylene bisamide and N, N′-distearyl adipic acid amide both had an average particle size of 0.9 μm.
処理剤−５の調製：Ｎ，Ｎ′−ステアリン酸エチレンビスアミド（平均粒子径５０μｍ）２重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油９７重量部、アミノ変性シリコーン〔側鎖ジアミン変性型のアミノ変性シリコーン、アミン価５ＫＯＨｍｇ／ｇ、粘度１２００ｍｍ２／ｓ（２５℃）〕１重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸エチレンビスアミドの平均粒子径は０．３μｍであった。 Preparation of Treatment Agent-5: 2 parts by weight of N, N′-stearic acid ethylenebisamide (average particle diameter 50 μm), 97 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., amino-modified silicone [side chain diamine Modified amino-modified silicone, amine value 5 KOH mg / g, viscosity 1200 mm 2 / s (25 ° C.)] was dispersed in 1 part by weight, and this liquid was passed through a dyno mill to grind N, N′-stearic acid ethylenebisamide. The average particle size of the obtained N, N′-stearic acid ethylenebisamide was 0.3 μm.
処理剤−６の調製：Ｎ，Ｎ′−ステアリン酸エチレンビスアミド（平均粒子径５０μｍ）２重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油９７重量部、アミノアルキルシリコーンレジン〔アミン価１１ＫＯＨｍｇ／ｇ、粘度３００ｍｍ２／ｓ（２５℃）〕１重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸エチレンビスアミドの平均粒子径は０．３μｍであった。 Preparation of Treatment Agent-6: 2 parts by weight of N, N′-stearic acid ethylenebisamide (average particle size 50 μm), 97 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., aminoalkyl silicone resin [amine value 11 KOH mg / g, viscosity 300 mm 2 / s (25 ° C.)] was dispersed in 1 part by weight, and this liquid was passed through a dyno mill to grind N, N′-stearic acid ethylenebisamide. The average particle size of the obtained N, N′-stearic acid ethylenebisamide was 0.3 μm.
処理剤−７の調製：Ｎ，Ｎ′−ステアリン酸メチレンビスアミド（平均粒子径５０μｍ）１重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油８８．５重量部、４０秒の流動パラフィン１０重量部、アミノ変性シリコーン〔側鎖ジアミン変性型のアミノ変性シリコーン、アミン価１ＫＯＨｍｇ／ｇ、粘度１４５００ｍｍ２／ｓ（２５℃）〕０．５重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ステアリン酸メチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸メチレンビスアミドの平均粒子径は０．３μｍであった。 Preparation of Treatment Agent-7: 1 part by weight of N, N′-stearic acid methylenebisamide (average particle size 50 μm), 88.5 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., liquid paraffin of 40 seconds 10 parts by weight, amino-modified silicone (side-chain diamine-modified type amino-modified silicone, amine value 1 KOH mg / g, viscosity 14500 mm 2 / s (25 ° C.)) is dispersed in 0.5 part by weight, and this solution is passed through a dyno mill. N, N'-stearic acid methylene bisamide was ground. The average particle diameter of the obtained N, N′-stearic acid methylenebisamide was 0.3 μm.
処理剤−８の調製：Ｎ，Ｎ′−ステアリン酸メチレンビスアミド（平均粒子径５０μｍ）１重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油８８．５重量部、４０秒の流動パラフィン１０重量部、アミノアルキルシリコーンレジン〔アミン価１１ＫＯＨｍｇ／ｇ、粘度３００ｍｍ２／ｓ（２５℃）〕０．５重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ステアリン酸メチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸メチレンビスアミドの平均粒子径は０．３μｍであった。 Preparation of Treatment Agent-8: 1 part by weight of N, N′-stearic acid methylene bisamide (average particle size 50 μm), 88.5 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., liquid paraffin of 40 seconds 10 parts by weight, aminoalkyl silicone resin (amine value 11 KOH mg / g, viscosity 300 mm 2 / s (25 ° C.)) 0.5 part by weight, this solution was passed through a dynomill and N, N′-stearic acid methylene bisamide Was crushed. The average particle diameter of the obtained N, N′-stearic acid methylenebisamide was 0.3 μm.
処理剤−９の調製：Ｎ，Ｎ′−ステアリン酸ヘキサメチレンビスアミド（平均粒子径５０μｍ）３重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油７５重量部、イソオクチルラウレート２０重量部、アミノ変性シリコーン〔両末端モノアミン変性型のアミノ変性シリコーン、アミン価２５ＫＯＨｍｇ／ｇ、粘度７０ｍｍ２／ｓ（２５℃）〕２重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ステアリン酸ヘキサメチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸ヘキサメチレンビスアミドの平均粒子径は０．４μｍであった。 Preparation of treatment agent-9: 3 parts by weight of N, N′-stearic acid hexamethylenebisamide (average particle size 50 μm), 75 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., 20 parts by weight of isooctyl laurate Parts, amino-modified silicone [mono-terminal-modified amino-modified silicone, amine value 25 KOH mg / g, viscosity 70 mm 2 / s (25 ° C.)] 2 parts by weight, this solution was passed through a dyno mill to obtain N, N ′ -Hexamethylenebisamide stearate was ground. The average particle size of the obtained N, N′-stearic acid hexamethylenebisamide was 0.4 μm.
処理剤−１０の調製：Ｎ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミド（平均粒子径５０μｍ）５重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油７３重量部、４０秒の流動パラフィン１０重量部、イソオクチルラウレート１０重量部、アミノ変性シリコーン〔側鎖モノアミン変性型のアミノ変性シリコーン、アミン価２８ＫＯＨｍｇ／ｇ、粘度９００ｍｍ２／ｓ（２５℃）〕２重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドの平均粒子径は０．３μｍであった。 Preparation of Treatment Agent-10: 5 parts by weight of N, N′-12-hydroxystearic acid ethylenebisamide (average particle size 50 μm), 73 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., flow for 40 seconds Dispersed in 10 parts by weight of paraffin, 10 parts by weight of isooctyl laurate, 2 parts by weight of amino-modified silicone (side-chain monoamine-modified amino-modified silicone, amine value 28 KOH mg / g, viscosity 900 mm 2 / s (25 ° C.)), This liquid was passed through a dyno mill to grind N, N′-12-hydroxystearic acid ethylene bisamide. The average particle size of the obtained N, N′-12-hydroxystearic acid ethylene bisamide was 0.3 μm.
処理剤−１１の調製：Ｎ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミド（平均粒子径５０μｍ）５重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油７３重量部、４０秒の流動パラフィン１０重量部、イソオクチルラウレート１０重量部、アミノアルキルシリコーンレジン〔アミン価１１ＫＯＨｍｇ／ｇ、粘度３００ｍｍ２／ｓ（２５℃）〕２重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドの平均粒子径は０．３μｍであった。 Preparation of treatment agent -11: N, N'-12- hydroxystearic acid ethylene bisamide (average particle size 50 [mu] m) 5 parts by weight, the silicone oil 73 parts by weight of a viscosity at 25 ° C. is 10 mm 2 / s, flow of 40 seconds Disperse in 10 parts by weight of paraffin, 10 parts by weight of isooctyl laurate, 2 parts by weight of an aminoalkyl silicone resin [amine value 11 KOH mg / g, viscosity 300 mm 2 / s (25 ° C.)]. N'-12-hydroxystearic acid ethylene bisamide was ground. The average particle size of the obtained N, N′-12-hydroxystearic acid ethylene bisamide was 0.3 μm.
処理剤−１２の調製：Ｎ，Ｎ′−ジステアリルアジピン酸アミド（平均粒子径５０μｍ）４重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油９４重量部、アミノアルキルシリコーンレジン〔アミン価１１ＫＯＨｍｇ／ｇ、粘度３００ｍｍ２／ｓ（２５℃）〕２重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ジステアリルアジピン酸アミドを粉砕した。得られたＮ，Ｎ′−ジステアリルアジピン酸アミドの平均粒子径は０．４μｍであった。 Preparation of Treatment Agent-12: 4 parts by weight of N, N′-distearyladipic acid amide (average particle diameter 50 μm), 94 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., aminoalkyl silicone resin [amine 1 KOH mg / g, viscosity 300 mm 2 / s (25 ° C.)] was dispersed in 2 parts by weight, and this liquid was passed through a dyno mill to grind N, N′-distearyl adipate amide. The average particle size of the obtained N, N′-distearyladipic acid amide was 0.4 μm.
処理剤−１３の調製：Ｎ−ステアリルステアリン酸アミド（平均粒子径５０μｍ）２重量部とＮ，Ｎ′−ステアリン酸メチレンビスアミド（平均粒子径５０μｍ）２重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油９４重量部、アミノアルキルシリコーンレジン〔アミン価１１ＫＯＨｍｇ／ｇ、粘度３００ｍｍ２／ｓ（２５℃）〕２重量部に分散し、この液をダイノーミルに通してＮ−ステアリルステアリン酸アミドとＮ，Ｎ′−ステアリン酸メチレンビスアミドを粉砕した。得られたＮ−ステアリルステアリン酸アミドとＮ，Ｎ′−ステアリン酸メチレンビスアミドの平均粒子径は共に０．４μｍであった。 Preparation of Treatment Agent-13: 2 parts by weight of N-stearyl stearic acid amide (average particle size 50 μm) and 2 parts by weight of N, N′-stearic acid methylenebisamide (average particle size 50 μm) had a viscosity of 10 mm 2 at 25 ° C. / S silicone oil 94 parts by weight, aminoalkyl silicone resin [amine value 11 KOH mg / g, viscosity 300 mm 2 / s (25 ° C.)] 2 parts by weight, this solution is passed through a dyno mill and N-stearyl stearamide And N, N'-stearic acid methylenebisamide were ground. The obtained N-stearyl stearamide and N, N′-stearic acid methylenebisamide both had an average particle size of 0.4 μm.
平均粒子径の測定，デジタルマイクロスコープ「ＶＨ−７０００」（キーエンス社製）により、２０箇所の粒子径を測定し、その平均を算出した。 Measurement of average particle diameter, a digital microscope “VH-7000” (manufactured by Keyence Corporation) was used to measure 20 particle diameters and calculate the average.
実施例１〜１４及び比較例１〜５
紡糸原液の調整：数平均分子量２０００のポリテトラメチレンエーテルグリコールと４，４’−ジフェニルメタンジイソシアネートをモル比率１：２で反応させ、次いで１，２−ジアミノプロパンのジメチルホルムアミド溶液を用いて鎖延長し、ポリマー濃度２７％のジメチルホルムアミド溶液を得た。３０℃での濃度は１５００ｍＰａＳであった。
Examples 1-14 and Comparative Examples 1-5
Preparation of the spinning dope: polytetramethylene ether glycol having a number average molecular weight of 2000 and 4,4′-diphenylmethane diisocyanate were reacted at a molar ratio of 1: 2, and then chain extension was performed using a 1,2-diaminopropane solution in dimethylformamide. A dimethylformamide solution having a polymer concentration of 27% was obtained. The concentration at 30 ° C. was 1500 mPaS.
実施例１
ポリウレタン紡糸原液を１９０℃のＮ２気流中に吐出して乾式紡糸した。紡糸中走行糸に上記で調製した処理剤−１をオイリングローラーにより繊維に対して６重量％付与した後、毎分５００ｍの速度でポビンに巻き取り４４ｄｔｅｘモノフィラメントチーズ（巻き量４００ｇ）を得た。得られたチーズを３５℃、５０％ＲＨの雰囲気中に４８時間放置して評価に供した。油剤性能の評価結果を表１及び表２に示した。
Example 1
The polyurethane spinning dope was discharged into a 190 ° C. N 2 stream and dry-spun. The treatment agent-1 prepared above was applied to the fiber during spinning by 6% by weight with respect to the fiber by an oiling roller, and then wound on a pobbin at a speed of 500 m / min to obtain 44 dtex monofilament cheese (amount of winding 400 g). The obtained cheese was left for 48 hours in an atmosphere of 35 ° C. and 50% RH for evaluation. Tables 1 and 2 show the evaluation results of the oil agent performance.
実施例２
上記で調製した処理剤−２を付与した以外は、実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 2
A polyurethane elastic yarn was spun and wound up on cheese in the same manner as in Example 1 except that the treatment agent-2 prepared above was applied.
実施例３
上記で調製した処理剤−３を付与した以外は、実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 3
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 1 except that Treatment Agent-3 prepared above was applied.
実施例４
上記で調製した処理剤−４を付与した以外は、実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 4
A polyurethane elastic yarn was spun and wound up on cheese in the same manner as in Example 1 except that Treatment Agent-4 prepared above was applied.
実施例５
実施例２の処理剤に、更にアルカンスルホネートＮａ塩を３重量部添加した
以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 5
A polyurethane elastic yarn was spun and wound on cheese in the same manner as in Example 1 except that 3 parts by weight of alkanesulfonate Na salt was further added to the treatment agent of Example 2.
実施例６
実施例２の処理剤に、更にラウリルサルフェートトリエタノールアミン塩を３重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 6
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 1 except that 3 parts by weight of lauryl sulfate triethanolamine salt was further added to the treating agent of Example 2.
実施例７
実施例４の処理剤に、更に２−エチルヘキシル酸ジエタノールアミン塩を３重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 7
Polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 1 except that 3 parts by weight of 2-ethanolhexyl diethanolamine salt was further added to the treating agent of Example 4.
実施例８
実施例４の処理剤に、更に２−エチルヘキシルホスフェートジエタノールアミン塩を３重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 8
A polyurethane elastic yarn was spun and wound on cheese in the same manner as in Example 1 except that 3 parts by weight of 2-ethylhexyl phosphate diethanolamine salt was further added to the treating agent of Example 4.
実施例９
実施例１の処理剤に、更にポリエーテル変性シリコーン〔信越化学工業社製、「ＫＦ−３５１」；粘度１００ｍｍ２／ｓ（２５℃）〕を０．３重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 9
Example 1 except that 0.3 parts by weight of a polyether-modified silicone [manufactured by Shin-Etsu Chemical Co., Ltd., “KF-351”; viscosity 100 mm 2 / s (25 ° C.)] was further added to the treating agent of Example 1. Similarly, polyurethane elastic yarn was spun and wound around cheese.
実施例１０
実施例１の処理剤に、更に両末端カルボキシ変性タイプのカルボキシ変性シリコーン（粘度１４０ｍｍ２／ｓ）を０．５重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 10
A polyurethane elastic yarn was spun in the same manner as in Example 1 except that 0.5 parts by weight of carboxy-modified silicone (viscosity 140 mm 2 / s) at both ends was further added to the treatment agent of Example 1. Rolled up on cheese.
実施例１１
実施例１の処理剤に、更にアミノ変性シリコーン〔側鎖アミノ変性型のアミノ変性シリコーン、アミン価６ＫＯＨｍｇ／ｇ、粘度９０ｍｍ２／ｓ（２５℃）〕を５重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 11
Example 1 except that 5 parts by weight of amino-modified silicone [side-chain amino-modified amino-modified silicone, amine value of 6 KOH mg / g, viscosity of 90 mm 2 / s (25 ° C.)] was further added to the treating agent of Example 1. In the same manner as above, polyurethane elastic yarn was spun and wound on cheese.
実施例１２
実施例３の処理剤に、更にＭＱ比が１．０のシリコーンレジンを２０重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 12
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 1 except that 20 parts by weight of a silicone resin having an MQ ratio of 1.0 was further added to the treatment agent of Example 3.
実施例１３
実施例４の処理剤に、更にステアリン酸Ａｌを２重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 13
A polyurethane elastic yarn was spun and wound on cheese in the same manner as in Example 1 except that 2 parts by weight of Al stearate was further added to the treatment agent of Example 4.
実施例１４
実施例１の処理剤に、更にアミノ変性シリコーン〔側鎖アミノ変性型のアミノ変性シリコーン、アミン価３７ＫＯＨｍｇ／ｇ、粘度８００ｍｍ２／ｓ（２５℃）〕と２−エチルヘキシルホスフェートの中和塩を５重量部添加した以外は実施例１と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 14
To the treating agent of Example 1, amino-modified silicone [side-chain amino-modified amino-modified silicone, amine value 37 KOH mg / g, viscosity 800 mm 2 / s (25 ° C.)] and 2-ethylhexyl phosphate neutralized salt were further added. A polyurethane elastic yarn was spun in the same manner as in Example 1 except for adding parts by weight, and wound on cheese.
比較例１
実施例１において、平均粒子径が５０μｍのＮ，Ｎ′−ステアリン酸エチレンビスアミド２重量部と、２５℃における粘度が５ｍｍ２／ｓのシリコーン油９８重量部とからなる処理剤を付与した以外は、実施例１と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 1
In Example 1, except that a treating agent consisting of 2 parts by weight of N, N′-stearic acid ethylenebisamide having an average particle size of 50 μm and 98 parts by weight of silicone oil having a viscosity at 25 ° C. of 5 mm 2 / s was applied. In the same manner as in Example 1, an elastic yarn was spun and wound up.
比較例２
実施例１において、平均粒子径が５０μｍの Ｎ，Ｎ′−ジステアリルテレフタル酸アミド１重量部と、３０秒の流動パラフィン９９重量部とからなる処理剤を付与した以外は、実施例１と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 2
Example 1 was the same as Example 1 except that a treatment agent consisting of 1 part by weight of N, N′-distearyl terephthalic acid amide having an average particle size of 50 μm and 99 parts by weight of liquid paraffin for 30 seconds was applied. Then, an elastic yarn was spun and wound up.
比較例３
実施例１において、平均粒子径が５０μｍのＮ，Ｎ′−ステアリン酸エチレンビスアミド５重量部、平均粒子径が５０μｍのＮ，Ｎ′−ジステアリルアジピン酸アミド５重量部、４０秒の流動パラフィン６０重量部、イソオクチルラウレート３０重量部とからなる処理剤を付与した以外は、実施例１と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 3
In Example 1, 5 parts by weight of N, N′-stearic acid ethylene bisamide having an average particle size of 50 μm, 5 parts by weight of N, N′-distearyladipic acid amide having an average particle size of 50 μm, and 40 seconds of liquid paraffin 60 An elastic yarn was spun and wound in the same manner as in Example 1 except that a treating agent consisting of parts by weight and 30 parts by weight of isooctyl laurate was added.
比較例４
実施例１において、平均粒子径が０．７μｍのステアリン酸マグネシウム１重量部、３０秒の流動パラフィン９９重量部とからなる処理剤を付与した以外は、実施例１と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 4
In Example 1, an elastic yarn was spun in the same manner as in Example 1 except that a treating agent consisting of 1 part by weight of magnesium stearate having an average particle size of 0.7 μm and 99 parts by weight of liquid paraffin for 30 seconds was applied. And wound up.
比較例５
実施例１において、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油２０重量部、６０秒の流動パラフィン８０重量部とからなる処理剤を付与した以外は、実施例１と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 5
In Example 1, an elastic yarn was prepared in the same manner as in Example 1 except that a treatment agent consisting of 20 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C. and 80 parts by weight of liquid paraffin for 60 seconds was applied. Spinned and wound up.
表１及び表２の評価結果からわかるように、本発明の処理剤−１〜４を用いた実施例１〜１４のチーズからの解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止性は良好で、処理剤自身も沈澱や分離が無く、分散安定性に優れていた。一方、比較例１〜５は解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止性が良くなく、処理剤自身の分散安定性が劣る。 As can be seen from the evaluation results in Tables 1 and 2, the unwinding property, antistatic property, cheese cake shape, smoothness and wind from the cheeses of Examples 1 to 14 using the treating agents -1 to 4 of the present invention. The cotton adsorption-preventing property was good, the treatment agent itself did not precipitate or separate, and was excellent in dispersion stability. On the other hand, Comparative Examples 1 to 5 are poor in unwinding property, antistatic property, cheese candy shape, smoothness, and fluff adsorption prevention property, and the dispersion stability of the treatment agent itself is inferior.
実施例１５〜２６及び比較例６〜１２
紡糸原液の調整：
数平均分子量２０００のポリテトラメチレングリコール１００重量部と４，４’−ジフェニルメタンジイソシアネート２５重量部を７０℃で反応させ、Ｎ，Ｎ’−ジメチルアセトアミド２５０重量部を加え冷却しながら反応混合物を溶解させた。１，２−ジアミノプロパン５重量部をＮ，Ｎ’−ジメチルアセトアミド１８４重量部に溶解させたものを添加した。この様にしてポリウレタン紡糸原液を得た。
Examples 15 to 26 and Comparative Examples 6 to 12
Preparation of spinning dope:
100 parts by weight of polytetramethylene glycol having a number average molecular weight of 2000 and 25 parts by weight of 4,4′-diphenylmethane diisocyanate are reacted at 70 ° C., and 250 parts by weight of N, N′-dimethylacetamide is added and the reaction mixture is dissolved while cooling. It was. A solution prepared by dissolving 5 parts by weight of 1,2-diaminopropane in 184 parts by weight of N, N′-dimethylacetamide was added. In this way, a polyurethane spinning dope was obtained.
実施例１５
ポリウレタン紡糸原液を２つの細孔を有する紡糸口金より１９０℃のＮ２気流中に吐出して乾式紡糸した。紡糸中走行糸に上記で調整した処理剤−５をオイリングローラーにより繊維に対して６重量％付与した後、毎分４００ｍの速度でボビンに巻き取り、２２ｄｔｅｘマルチフィラメントのチーズ（巻き量４００ｇ）を得た。得られたチーズを３５℃、５０％ＲＨの雰囲気中に４８時間放置して評価に供した。油剤性能の評価結果を表３及び表４に示した。
Example 15
The polyurethane spinning dope was discharged from a spinneret having two pores into a 190 ° C. N 2 stream and dry-spun. After applying 6 wt% of the treatment agent-5 prepared above to the running yarn during spinning with respect to the fiber by an oiling roller, it was wound around a bobbin at a speed of 400 m / min, and 22 dtex multifilament cheese (wound amount 400 g) was obtained. Obtained. The obtained cheese was left for 48 hours in an atmosphere of 35 ° C. and 50% RH for evaluation. The evaluation results of the oil agent performance are shown in Tables 3 and 4.
実施例１６
上記で調整した処理剤−６を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 16
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 15 except that the treatment agent-6 prepared above was applied.
実施例１７
上記で調整した処理剤−７を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 17
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 15 except that Treatment Agent-7 prepared above was applied.
実施例１８
上記で調整した処理剤−８を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
実施例１９
Example 18
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 15 except that the treatment agent-8 prepared above was applied.
Example 19
上記で調整した処理剤−９を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。 A polyurethane elastic yarn was spun and wound up on cheese in the same manner as in Example 15 except that Treatment Agent-9 prepared above was applied.
実施例２０
上記で調整した処理剤−１０を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 20
A polyurethane elastic yarn was spun and wound on cheese in the same manner as in Example 15 except that the treatment agent-10 prepared above was applied.
実施例２１
上記で調整した処理剤−１１を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 21
A polyurethane elastic yarn was spun and wound around cheese in the same manner as in Example 15 except that the treatment agent 11 prepared above was applied.
実施例２２
上記で調整した処理剤−１２を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 22
A polyurethane elastic yarn was spun and wound on cheese in the same manner as in Example 15 except that the treatment agent-12 prepared above was applied.
実施例２３
上記で調整した処理剤−１３を付与した以外は、実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 23
A polyurethane elastic yarn was spun and wound up on cheese in the same manner as in Example 15 except that Treatment Agent-13 prepared above was applied.
実施例２４
実施例１５の処理剤に、更にアミノ変性シリコーン〔側鎖アミノ変性型のアミノ変性シリコーン、アミン価３７ＫＯＨｍｇ／ｇ、粘度８００ｍｍ２／ｓ（２５℃）〕と２−エチルヘキシルホスフェートの中和塩を５重量部添加した以外は実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 24
To the treating agent of Example 15, amino-modified silicone [side-chain amino-modified amino-modified silicone, amine value 37 KOH mg / g, viscosity 800 mm 2 / s (25 ° C.)] and 2-ethylhexyl phosphate neutralized salt were further added. A polyurethane elastic yarn was spun and wound up on cheese in the same manner as in Example 15 except that parts by weight were added.
実施例２５
実施例１６の処理剤に、更にＭＱ比が１．０のシリコーンレジンを２０重量部添加した以外は実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 25
A polyurethane elastic yarn was spun and wound on cheese in the same manner as in Example 15 except that 20 parts by weight of a silicone resin having an MQ ratio of 1.0 was further added to the treatment agent of Example 16.
実施例２６
実施例２２の処理剤に、更にポリエーテル変性シリコーン〔信越化学工業社製、「ＫＦ−３５１」；粘度１００ｍｍ２／ｓ（２５℃）〕を０．３重量部添加した以外は実施例１５と同様にして、ポリウレタン弾性糸を紡糸し、チーズに巻き取った。
Example 26
Example 15 is the same as Example 15 except that 0.3 parts by weight of a polyether-modified silicone [manufactured by Shin-Etsu Chemical Co., Ltd., “KF-351”; viscosity 100 mm 2 / s (25 ° C.)] is further added to the treating agent of Example 22. Similarly, polyurethane elastic yarn was spun and wound around cheese.
比較例６
実施例１５において、平均粒子径が５０μｍのＮ，Ｎ′−ステアリン酸エチレンビスアミド２重量部と、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油９７重量部、アミノ変性シリコーン〔側鎖ジアミン変性型のアミノ変性シリコーン、アミン価５ＫＯＨｍｇ／ｇ、粘度１２００ｍｍ２／ｓ（２５℃）〕１重量部とからなる処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 6
In Example 15, 2 parts by weight of N, N′-stearic acid ethylenebisamide having an average particle diameter of 50 μm, 97 parts by weight of silicone oil having a viscosity at 25 ° C. of 10 mm 2 / s, amino-modified silicone [side chain diamine-modified type Amino-modified silicone, an amine value of 5 KOH mg / g, a viscosity of 1200 mm 2 / s (25 ° C.)] except that a treating agent comprising 1 part by weight was applied, and an elastic yarn was spun and wound in the same manner as in Example 15. It was.
比較例７
実施例１５において、平均粒子径が５０μｍのＮ，Ｎ′−ステアリン酸メチレンビスアミド１重量部と、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油８８．５重量部、４０秒の流動パラフィン１０重量部、アミノ変性シリコーン〔側鎖ジアミン変性型のアミノ変性シリコーン、アミン価１ＫＯＨｍｇ／ｇ、粘度１４５００ｍｍ２／ｓ（２５℃）〕０．５重量部とからなる処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 7
In Example 15, 1 part by weight of N, N′-stearic acid methylenebisamide having an average particle diameter of 50 μm, 88.5 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., 10 parts by weight of liquid paraffin for 40 seconds Example, except that a treatment agent comprising 0.5 parts by weight, amino-modified silicone [side-chain diamine-modified type amino-modified silicone, amine value of 1 KOH mg / g, viscosity of 14500 mm 2 / s (25 ° C.)] was added. The elastic yarn was spun and wound up in the same manner as in No.15.
比較例８
実施例１５において、平均粒子径が５０μｍのＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミド５重量部と、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油７３重量部、４０秒の流動パラフィン１０重量部、イソオクチルラウレート１０重量部、アミノ変性シリコーン〔側鎖モノアミン変性型のアミノ変性シリコーン、アミン価２８ＫＯＨｍｇ／ｇ、粘度９００ｍｍ２／ｓ（２５℃）〕２重量部とからなる処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡し、巻き取った。
Comparative Example 8
In Example 15, 5 parts by weight of N, N′-12-hydroxystearic acid ethylenebisamide having an average particle diameter of 50 μm, 73 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., and liquid paraffin 10 of 40 seconds A treating agent comprising, by weight, 10 parts by weight of isooctyl laurate, 2 parts by weight of amino-modified silicone (side-chain monoamine-modified amino-modified silicone, amine value 28 KOH mg / g, viscosity 900 mm 2 / s (25 ° C.)). An elastic yarn was spun and wound up in the same manner as in Example 15 except that it was applied.
比較例９
Ｎ，Ｎ′−ステアリン酸エチレンビスアミド（平均粒子径５０μｍ）２重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油９８重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−ステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−ステアリン酸エチレンビスアミドの平均粒子径は０．７μｍであった。このようにして調整した処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 9
2 parts by weight of N, N′-stearic acid ethylenebisamide (average particle size 50 μm) is dispersed in 98 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., and this liquid is passed through a dyno mill to give N, N ′. -Grinding stearic acid ethylenebisamide. The average particle diameter of the obtained N, N′-stearic acid ethylenebisamide was 0.7 μm. An elastic yarn was spun and wound up in the same manner as in Example 15 except that the treatment agent thus adjusted was applied.
比較例１０
Ｎ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミド（平均粒子径５０μｍ）５重量部を、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油７５重量部、４０秒の流動パラフィン１０重量部、イソオクチルラウレート１０重量部に分散し、この液をダイノーミルに通してＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドを粉砕した。得られたＮ，Ｎ′−１２−ヒドロキシステアリン酸エチレンビスアミドの平均粒子径は０．９μｍであった。このようにして調整した処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 10
5 parts by weight of N, N′-12-hydroxystearic acid ethylene bisamide (average particle size 50 μm), 75 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C., 10 parts by weight of liquid paraffin for 40 seconds, isooctyl The dispersion was dispersed in 10 parts by weight of laurate, and this liquid was passed through a dyno mill to grind N, N′-12-hydroxystearic acid ethylene bisamide. The average particle size of the obtained N, N′-12-hydroxystearic acid ethylene bisamide was 0.9 μm. An elastic yarn was spun and wound up in the same manner as in Example 15 except that the treatment agent thus adjusted was applied.
比較例１１
実施例１５において、平均粒子径が０．７μｍのステアリン酸マグネシウム１重量部、４０秒の流動パラフィン９９重量部とからなる処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 11
In Example 15, an elastic yarn was spun in the same manner as in Example 15 except that a treatment agent consisting of 1 part by weight of magnesium stearate having an average particle size of 0.7 μm and 99 parts by weight of liquid paraffin for 40 seconds was applied. And wound up.
比較例１２
実施例１５において、２５℃における粘度が１０ｍｍ２／ｓのシリコーン油５０重量部、４０秒の流動パラフィン５０重量部とからなる処理剤を付与した以外は、実施例１５と同様にして弾性糸を紡糸し、巻き取った。
Comparative Example 12
In Example 15, an elastic yarn was prepared in the same manner as in Example 15 except that a treatment agent consisting of 50 parts by weight of silicone oil having a viscosity of 10 mm 2 / s at 25 ° C. and 50 parts by weight of liquid paraffin for 40 seconds was applied. Spinned and wound up.
表３及び表４の評価結果からわかるように、本発明の処理剤−５〜１３を用いた実施例１５〜２６のチーズからの解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止性は良好で、処理剤自身も沈澱や分離が無く、分散安定性に優れていた。一方、比較例６〜８及び比較例１１〜１２は解舒性、制電性、チーズ捲形状、平滑性、風綿吸着防止性が良くなく、処理剤自身の分散安定性が劣る。実施例１５〜２６では分散剤を用いて分散処理しているため、分散剤を用いずに分散処理した比較例９〜１０に比べ、平均粒子径がより小さく、長期における分散安定性に優れる。 As can be seen from the evaluation results in Table 3 and Table 4, the unwinding property, antistatic property, cheese candy shape, smoothness, wind from the cheeses of Examples 15 to 26 using the treating agents -5 to 13 of the present invention. The cotton adsorption-preventing property was good, the treatment agent itself did not precipitate or separate, and was excellent in dispersion stability. On the other hand, Comparative Examples 6 to 8 and Comparative Examples 11 to 12 are poor in defatting property, antistatic property, cheese candy shape, smoothness, and fluff adsorption prevention property, and the dispersion stability of the treatment agent itself is inferior. In Examples 15 to 26, since the dispersion treatment was performed using the dispersant, the average particle size is smaller and the dispersion stability in the long term is excellent as compared with Comparative Examples 9 to 10 in which the dispersion treatment was performed without using the dispersant.
１ 弾性繊維のチーズ、
２ 春日式電位差測定装置、
３ 弾性繊維のチーズ、
４ 糸、
５ コンペンセーター、
６ ローラー、
７ 編み針、
８ Ｕゲージ、
９ ローラー、
１０ 速度計、
１１ 巻き取りローラー、
１２ 春日式電位差測定装置、
１３ 荷重、
１４ ローラー、
１５ Ｕゲージ、
１６ 弾性繊維のチーズ、
１７ コンペンセーター、
１８ ローラー、
１９ 風綿の吸糸口、
２０ 弾性繊維の巻取ローラー、
２１ 綿糸、
２２ ガイド、
２３ ローラー、
２４ 編針、
２５ 綿糸の巻取ローラー、
２６ チーズ、
２７ 巻き取り用紙管、
２８ ローラー、
２９ ローラー、
３０ 走行糸条、
３１ 解舒点、
３２ チーズとローラーの接点
1 Elastic fiber cheese,
2 Kasuga potentiometer,
3 Elastic fiber cheese,
4 Yarn,
5 Compensation sweater
6 rollers,
7 Knitting needles
8 U gauge,
9 rollers,
10 Speedometer,
11 Take-up roller,
12 Kasuga-type potentiometer,
13 load,
14 rollers,
15 U gauge,
16 Elastic fiber cheese,
17 Compensation sweater
18 rollers,
19 Cotton spout
20 Elastic fiber take-up roller,
21 Cotton yarn,
22 guides,
23 rollers,
24 Knitting needles,
25 Cotton thread take-up roller,
26 Cheese,
27 Winding paper tube,
28 rollers,
29 rollers,
30 running yarn,
31 Unraveling point,
32 Point of contact between cheese and roller
Claims (7)
Ｒ１−Ｃ（Ｏ）−ＮＨ−Ｒ３−ＮＨ−Ｃ（Ｏ）−Ｒ２ （式１）
Ｒ４−ＮＨ−Ｃ（Ｏ）−Ｒ５−Ｃ（Ｏ）−ＮＨ−Ｒ６ （式２）
Ｒ７−ＮＨ−Ｃ（Ｏ）−Ｒ８ （式３）
（式１、式２、式３において、Ｒ１、Ｒ２、Ｒ４、Ｒ６、Ｒ７、Ｒ８は有機基を表し、Ｒ３、Ｒ５は炭素数１〜１０の脂肪族炭化水素基、置換基を有してもよい芳香族炭化水素基を表す。） A compound represented by the following formula 1 having an average particle diameter of 0.01 to 20 μm, a compound represented by the following formula 2 having an average particle diameter of 0.01 to 20 μm, and an average particle diameter of 0.01 to 20 μm 0.01 to 20 parts by weight of at least one selected from the compound represented by the following formula 3 is used, and at least one or more selected from silicone oil, mineral oil and ester oil is used as the base component in an amount of 80 to 99.99% by weight. A processing agent for elastic fibers composed of parts.
R 1 —C (O) —NH—R 3 —NH—C (O) —R 2 (Formula 1)
R 4 —NH—C (O) —R 5 —C (O) —NH—R 6 (Formula 2)
R 7 —NH—C (O) —R 8 (Formula 3)
(Formula 1, Formula 2, in Formula 3, R 1, R 2, R 4, R 6, R 7, R 8 represents an organic group, R 3, R 5 is from 1 to 10 carbon atoms aliphatic hydrocarbon Represents an aromatic hydrocarbon group which may have a group or a substituent .
Ｒ １ −Ｃ（Ｏ）−ＮＨ−Ｒ ３ −ＮＨ−Ｃ（Ｏ）−Ｒ ２ （式１）
Ｒ ４ −ＮＨ−Ｃ（Ｏ）−Ｒ ５ −Ｃ（Ｏ）−ＮＨ−Ｒ ６ （式２）
Ｒ ７ −ＮＨ−Ｃ（Ｏ）−Ｒ ８ （式３）
（式１、式２、式３において、Ｒ １ 、Ｒ ２ 、Ｒ ４ 、Ｒ ６ 、Ｒ ７ 、Ｒ ８ は有機基を表し、Ｒ ３ 、Ｒ ５ は炭素数１〜１０の脂肪族炭化水素基、置換基を有してもよい芳香族炭化水素基を表す。） Table under following formula 1-3 silicone oil / mineral oil and ester oil of total = 100 / 0-10 / 90 consisting of (weight ratio) base component and said base component per 100 parts by weight of 0.01 to 20 parts by weight At least one selected from the above compounds, and further, amino-modified silicone and / or aminoalkylsilicone resin as a dispersant, the base component / the dispersant = 99.5 / 0.5 to 80/20 (weight ratio) ) was used in a ratio of elastic fiber-processing agent having an average particle size of at least one or more is dispersed in 0.01~20μm selected from the compounds represented by the following following formula 1-3.
R 1 —C (O) —NH—R 3 —NH—C (O) —R 2 (Formula 1)
R 4 —NH—C (O) —R 5 —C (O) —NH—R 6 (Formula 2)
R 7 —NH—C (O) —R 8 (Formula 3)
(Formula 1, Formula 2, in Formula 3, R 1, R 2, R 4, R 6, R 7, R 8 represents an organic group, R 3, R 5 is from 1 to 10 carbon atoms aliphatic hydrocarbon Represents an aromatic hydrocarbon group which may have a group or a substituent.)
Ｒ９(Ｒ１０)２ＳｉＯ-[(Ｒ１０)２ＳｉＯ] ｋ -[(Ｒ１０Ｒ１１)ＳｉＯ] ｌ -ＳｉＲ９(Ｒ１０)２ （式４）
（式中、Ｒ９はＨ２Ｎ（ＣＨ２）３−、１価炭化水素基、アルコキシ基から選択される基、Ｒ１０は１価炭化水素基又はアルコキシ基、Ｒ１１は１価炭化水素基、Ｈ２Ｎ（ＣＨ２）３−、Ｈ２Ｎ（ＣＨ２）２ＮＨ（ＣＨ２）３−から選択される基、ｋは５〜１０，０００の正数、ｌは０．１〜４００の正数を表す。） The treatment agent for elastic fibers according to claim 2, wherein in the amino-modified silicone used as a dispersant, the amino-modified silicone is an aminoalkyl group-containing organopolysiloxane represented by the following formula 4.
R 9 (R 10) 2 SiO - [(R 10) 2 SiO] k - [(R 10 R 11) SiO] l -SiR 9 (R 10) 2 ( Equation 4)
(Wherein R 9 is a group selected from H 2 N (CH 2 ) 3 —, a monovalent hydrocarbon group and an alkoxy group, R 10 is a monovalent hydrocarbon group or an alkoxy group, and R 11 is a monovalent hydrocarbon. A group selected from the group H 2 N (CH 2 ) 3 —, H 2 N (CH 2 ) 2 NH (CH 2 ) 3 —, k is a positive number of 5 to 10,000, and l is 0.1 to 0.1 Represents a positive number of 400.)
〔（Ｈ２ＮＲ１２ＮＨＲ１３ＳｉＯ１．５) ｎ (Ｒ１４ＳｉＯ１．５)ｍ〕ｔ （式５）
（式中、Ｒ１２は炭素数１〜３の側鎖を有していてもよい炭化水素基、Ｒ１３は炭素数１〜５の側鎖を有していてもよい炭化水素基、Ｒ１４は炭素数４〜１０の側鎖を有していてもよい飽和または不飽和の炭化水素基、ｎは０．１〜０．５の正数、ｍは０．５〜０．９の正数であり、ｎ＋ｍ＝１。ｔは５〜５０の正数を表す。） In aminoalkyl silicone resin used as the dispersing agent, the elastic fiber-processing agent according to claim 2 in which the amino alkyl silicone resin represented by the following formula 5.
[(H 2 NR 12 NHR 13 SiO 1.5 ) n (R 14 SiO 1.5 ) m ] t (Formula 5)
(In the formula, R 12 is a hydrocarbon group which may have a side chain having 1 to 3 carbon atoms, R 13 is a hydrocarbon group which may have a side chain having 1 to 5 carbon atoms, R 14. Is a saturated or unsaturated hydrocarbon group which may have a side chain having 4 to 10 carbon atoms, n is a positive number of 0.1 to 0.5, and m is a positive number of 0.5 to 0.9. N + m = 1, t represents a positive number of 5-50 .
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