JP2010196179A - Antistatic polyester blended yarn having excellent wrinkle recovery - Google Patents
Antistatic polyester blended yarn having excellent wrinkle recovery Download PDFInfo
- Publication number
- JP2010196179A JP2010196179A JP2009039189A JP2009039189A JP2010196179A JP 2010196179 A JP2010196179 A JP 2010196179A JP 2009039189 A JP2009039189 A JP 2009039189A JP 2009039189 A JP2009039189 A JP 2009039189A JP 2010196179 A JP2010196179 A JP 2010196179A
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- JP
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- Prior art keywords
- polyester
- less
- antistatic
- elongation
- yarn
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000011084 recovery Methods 0.000 title claims abstract description 20
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- 239000002216 antistatic agent Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- -1 hydroxy hydrocarbon Chemical class 0.000 claims description 36
- 125000004432 carbon atom Chemical group C* 0.000 claims description 20
- 230000008646 thermal stress Effects 0.000 claims description 17
- 125000003118 aryl group Chemical group 0.000 claims description 16
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- 125000002252 acyl group Chemical group 0.000 claims description 3
- 125000002947 alkylene group Chemical group 0.000 claims description 3
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- 150000004714 phosphonium salts Chemical group 0.000 description 2
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- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
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- ZRPKEUVFESZUKX-UHFFFAOYSA-N 2-(2-hydroxyethoxy)benzoic acid Chemical compound OCCOC1=CC=CC=C1C(O)=O ZRPKEUVFESZUKX-UHFFFAOYSA-N 0.000 description 1
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- RSROEZYGRKHVMN-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;oxirane Chemical class C1CO1.CCC(CO)(CO)CO RSROEZYGRKHVMN-UHFFFAOYSA-N 0.000 description 1
- QWGRWMMWNDWRQN-UHFFFAOYSA-N 2-methylpropane-1,3-diol Chemical compound OCC(C)CO QWGRWMMWNDWRQN-UHFFFAOYSA-N 0.000 description 1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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- XQKKWWCELHKGKB-UHFFFAOYSA-L calcium acetate monohydrate Chemical compound O.[Ca+2].CC([O-])=O.CC([O-])=O XQKKWWCELHKGKB-UHFFFAOYSA-L 0.000 description 1
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- Multicomponent Fibers (AREA)
Abstract
Description
本発明は、制電性を有し、しかも皺回復性に優れた新規なポリエステル混繊糸に関するものである。 The present invention relates to a novel polyester mixed yarn having antistatic properties and excellent wrinkle recovery.
極細ポリエステル糸は、布帛にした時、柔らかな風合が得られ、保温性、吸水、吸湿性などの性能も向上するため、衣料用途をはじめ、幅広く使われている。
しかしながら、本来、ポリエステルは疎水性であるため、制電性が要求される分野では、従来から、ポリエステルに親水性を付与して制電性を発現させようとする試みが行われており、これまでに数多くの提案がなされている。
Ultra fine polyester yarns are widely used for clothing and other purposes because they provide a soft texture when made into a fabric and improve performance such as heat retention, water absorption, and moisture absorption.
However, since polyester is inherently hydrophobic, in the field where antistatic properties are required, attempts have been made to impart antistatic properties by imparting hydrophilicity to polyesters. Many proposals have been made.
例えばポリエステルにポリオキシアルキレン系ポリエーテル化合物を配合せしめる方法（特公昭３９−５２１４号公報）、並びにポリエステルに実質的に非相溶性のポリオキシアルキレン系ポリエーテル化合物と有機・無機のイオン性化合物とを配合せしめる方法（特公昭４４−３１８２８号公報、特公昭６０−１１９４４号公報、特開昭５３−８０４９７号公報、特開昭５３−１４９２４７号公報、特開昭６０−３９４１３号公報、特開平３−１３９５５６号公報等）が知られている。
しかしながら通常の延伸（ＦＯＹ）においては、制電性を有するものの、仮撚加工糸においては、捲縮糸で撚り変形により、毛羽が発生する為、制電性を有するものはないのが実情であった。
For example, a method of blending a polyester with a polyoxyalkylene polyether compound (Japanese Patent Publication No. 39-5214), a polyoxyalkylene polyether compound substantially incompatible with the polyester, and an organic / inorganic ionic compound (Japanese Patent Publication No. 44-31828, Japanese Patent Publication No. 60-11944, Japanese Patent Publication No. 53-80497, Japanese Patent Publication No. 53-149247, Japanese Patent Publication No. 60-39413, Japanese Patent Laid-Open No. Hei. 3-139556 gazette etc.) is known.
However, in normal drawing (FOY), although it has antistatic properties, in the false twisted yarn, fluff is generated by twisting deformation of the crimped yarn, so there is actually no antistatic property. there were.
又上記の問題を解決するために特開平４−１４６２１５号公報にはポリエステルに実質的に非相溶性のポリオキシアルキレン系ポリエーテル化合物と有機・無機のイオン性化合物からなる制電剤を芯部ポリエステルに含む芯鞘型ポリエステル複合繊維が提案されている。確かに芯鞘型複合繊維とすることによりある程度仮撚工程での毛羽発生は抑えられるものの、そのためには紡糸延伸仮撚り工程で厳密な制御を必要とし、制電性と断糸、毛羽の発生等の生産の安定性を両立させる点で十分とは言えなかった。 In order to solve the above problem, Japanese Patent Laid-Open No. 4-146215 discloses a core containing an antistatic agent comprising a polyoxyalkylene polyether compound substantially incompatible with polyester and an organic / inorganic ionic compound. A core-sheath type polyester composite fiber included in polyester has been proposed. Although the generation of fluff in the false twisting process can be suppressed to some extent by using a core-sheath type composite fiber, strict control is required in the spinning draw false twisting process, and antistaticity, yarn breakage, and generation of fluff are required. It was not sufficient in terms of achieving both production stability and the like.
更に単糸繊度が１．５ｄｔｅｘより小さい極細糸においては芯／鞘形成のバラツキ、単糸繊度のバラツキにより、実用的に制電性繊維と呼べるものはないのが実情であった。
そして近年、織編物の風合い、肌触り、外観等に関する要求がますます高まってきており、特に、婦人衣料、ブラウス、シャツなどの用途において、着用時や保管時などに衣服に皺が入ると該皺が取れ難くなる場合があり、極細繊度で制電性を有するとともに皺回復性の良いポリエステル糸の要望が強まってきた。
Furthermore, in the case of extra fine yarns having a single yarn fineness of less than 1.5 dtex, there is no practically no antistatic fiber due to variations in core / sheath formation and single yarn fineness.
In recent years, there has been an increasing demand for the texture, feel, appearance, etc. of woven and knitted fabrics. There are cases where it is difficult to remove the polyester yarn, and there is an increasing demand for a polyester yarn having an ultrafine fineness, antistatic property and good wrinkle recovery.
本発明の目的は、従来の極細ポリエステル延伸糸が持つ、柔らかな風合、保温性、吸水、吸湿性などの性能も維持し、制電性能及び皺回復性にも優れた布帛を得るのに好適なポリエステル混繊糸及びそれを安定して製造する方法を提供することにある。 The object of the present invention is to obtain a fabric having excellent softness, heat retention, water absorption, hygroscopicity, etc., and excellent in antistatic performance and wrinkle recovery properties, which is possessed by conventional ultra fine polyester drawn yarns. An object of the present invention is to provide a suitable polyester blended yarn and a method for stably producing the same.
本発明者らの研究によれば、上記本発明の目的は、
単糸繊度が１．５ｄｔｅｘ以下で、伸度（ＥＬＡ）が８０％以上、１０％伸長時の弾性回復率（ＥＲＡ）が５０％以下、伸長剛性率（ＥＭＡ）が５．８９ＧＰａ以下、結晶化度（ＸｐＡ）が２５％以上、沸水収縮率（ＢＷＳＡ）が３％以下、１６０℃における熱応力（ＴＳＡ）が０．４４ｍＮ／ｄｔｅｘ以下の芯鞘型複合繊維であって、芯部が制電性ポリエステルＣで形成され、他方、鞘部が艶消し剤を０〜１０ｗｔ％含むポリエステルＤで形成されるポリエステルマルチ繊維（Ａ）を弛緩熱処理した後 伸度（ＥＬＢ）が４０％以下、伸長剛性率（ＥＭＢ）が７．８５ＧＰａ以上、沸水収縮率（ＢＷＳＢ）が５％以上、１６０℃における熱応力（ＴＳＢ）が０．８８ｍＮ／ｄｔｅｘ以上のポリエステマルチ繊維（Ｂ）と合糸し，その後交絡処理し、且つ下記要件を満足することを特徴とするポリエステル混繊糸の製造方法。
（１）ポリエステルマルチ繊維Ａの芯部の面積と鞘部の面積との比が５：９５〜８０：２０であること。
（２）混繊糸の摩擦帯電圧が２０００Ｖ以下であること。
（３）ポリエステルマルチ繊維Ａ／ポリエステルマルチ繊維Ｂの重量比が４５／５５〜７０／３０であること。
（４）制電性ポリエステルＣが芳香族ポリエステル１００重量部に対して、制電剤として、下記一般式（１）で表されるポリオキシアルキレン系ポリエーテルを０．２〜３０重量部及び該ポリエステルと実質的に非反応性の有機イオン性化合物０．０５〜１０重量部を含有してなる制電性ポリエステルであること。
Ｚ−［（ＣＨ２ＣＨ２Ｏ）ｎ（Ｒ１Ｏ）ｍ−Ｒ２］ｋ 式（１）
［式中、Ｚは１〜６個の活性水素原子を有する有機化合物残基、Ｒ１は炭素原子数６以上のアルキレン基又は置換アルキレン基、Ｒ２は水素原子、炭素原子数１〜４０の一価の炭化水素基、炭素原子数２〜４０の一価のヒドロキシ炭化水素又は炭素原子数２〜４０の一価のアシル基、ｋは１〜６の整数、ｎはｎ≧７０／ｋを満足する整数、ｍは１以上の整数］により達成できることが見出された。
According to the study by the present inventors, the object of the present invention is as follows.
Single yarn fineness is 1.5 dtex or less, elongation (ELA) is 80% or more, elastic recovery (ERA) at 10% elongation is 50% or less, elongation rigidity (EMA) is 5.89 GPa or less, crystallization The core-sheath type composite fiber having a degree (XpA) of 25% or more, a boiling water shrinkage (BWSA) of 3% or less, and a thermal stress (TSA) at 160 ° C. of 0.44 mN / dtex or less. The polyester multifiber (A), which is made of polyester D with a sheath part of 0 to 10% by weight of matting agent, is subjected to relaxation heat treatment, and the elongation (ELB) is 40% or less. Combined with polyester multifiber (B) having a rate (EMB) of 7.85 GPa or more, boiling water shrinkage (BWSB) of 5% or more, and thermal stress (TSB) at 160 ° C. of 0.88 mN / dtex or more, and then entangled place A method for producing a polyester blended yarn, characterized by satisfying the following requirements:
(1) The ratio of the area of the core part of polyester multi fiber A and the area of a sheath part is 5: 95-80: 20.
(2) The friction band voltage of the blended yarn is 2000 V or less.
(3) The weight ratio of polyester multifiber A / polyester multifiber B is 45/55 to 70/30.
(4) The antistatic polyester C is 0.2 to 30 parts by weight of polyoxyalkylene polyether represented by the following general formula (1) as an antistatic agent with respect to 100 parts by weight of the aromatic polyester. It is an antistatic polyester comprising 0.05 to 10 parts by weight of an organic ionic compound that is substantially non-reactive with polyester.
Z - [(CH 2 CH 2 O) n (R 1 O) m-R 2] k equation (1)
[Wherein, Z is an organic compound residue having 1 to 6 active hydrogen atoms, R 1 is an alkylene group or substituted alkylene group having 6 or more carbon atoms, R 2 is a hydrogen atom, having 1 to 40 carbon atoms. A monovalent hydrocarbon group, a monovalent hydroxy hydrocarbon having 2 to 40 carbon atoms or a monovalent acyl group having 2 to 40 carbon atoms, k is an integer of 1 to 6, and n is n ≧ 70 / k. It has been found that a satisfactory integer, m is an integer greater than or equal to 1, can be achieved.
本発明は、特に、後工程における、高圧染色を経て顕著に現れ耐熱性に強く実用的である。本発明に使用するポリエステルマルチ繊維Ｂは熱収縮するため、ポリエステルマルチ繊維Ａが混繊糸の外側に配置し、ポリエステルマルチ繊維Ｂが内側に配置する構造となり、本発明のポリエステル混繊糸を用いると、皺回復性が良好で、且つふくらみ感に富みソフトな風合い触感のある布帛が得られる。 In particular, the present invention is noticeable after high-pressure dyeing in the post-process and is practical and strong in heat resistance. Since the polyester multi-fiber B used in the present invention is thermally shrunk, the polyester multi-fiber A is arranged outside the mixed yarn and the polyester multi-fiber B is arranged inside, and the polyester multi-fiber of the present invention is used. Thus, it is possible to obtain a fabric that has good wrinkle recovery and is rich in swelling and has a soft hand feeling.
以下本発明の実施形態について詳細に説明する。
本発明で使用するポリエステルは、芳香環を重合体の連鎖単位に有する芳香族ポリエステルであって、二官能性芳香族カルボン酸またはそのエステル形成性誘導体とジオールまたはそのエステル形成性誘導体との反応により得られる重合体を対象とする。
Hereinafter, embodiments of the present invention will be described in detail.
The polyester used in the present invention is an aromatic polyester having an aromatic ring in a polymer chain unit, which is obtained by reacting a bifunctional aromatic carboxylic acid or an ester-forming derivative thereof with a diol or an ester-forming derivative thereof. The obtained polymer is an object.
ここでいう二官能性芳香族カルボン酸としてはテレフタル酸、イソフタル酸、オルトフタル酸、１，５―ナフタレンジカルボン酸、２，５―ナフタレンジカルボン酸、２，６―ナフタレンジカルボン酸、４，４′―ビフェニルジカルボン酸、３，３′―ビフェニルジカルボン酸、４，４′―ビフェニルエーテルジカルボン酸、４，４′―ビフェニルメタンジカルボン酸、４，４′―ビフェニルスルホンジカルボン酸、４，４′―ビフェニルイソプロピリデンジカルボン酸、１，２―ビス（フェノキシ）エタン―４，４′―ジカルボン酸、２，５―アントラセンジカルボン酸、２，６―アントラセンジカルボン酸、４，４′―ｐ―フェニレンジカルボン酸、２，５―ピリジンジカルボン酸、β―ヒドロキシエトキシ安息香酸、ｐ―オキシ安息香酸等をあげることができ、特にテレフタル酸が好ましい。 Examples of the bifunctional aromatic carboxylic acid herein include terephthalic acid, isophthalic acid, orthophthalic acid, 1,5-naphthalenedicarboxylic acid, 2,5-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid, 4,4′- Biphenyl dicarboxylic acid, 3,3'-biphenyl dicarboxylic acid, 4,4'-biphenyl ether dicarboxylic acid, 4,4'-biphenylmethane dicarboxylic acid, 4,4'-biphenyl sulfone dicarboxylic acid, 4,4'-biphenyl isopropyl Redene dicarboxylic acid, 1,2-bis (phenoxy) ethane-4,4'-dicarboxylic acid, 2,5-anthracene dicarboxylic acid, 2,6-anthracene dicarboxylic acid, 4,4'-p-phenylenedicarboxylic acid, 2 , 5-Pyridinedicarboxylic acid, β-hydroxyethoxybenzoic acid, p-oxybenzoic acid Etc. can be mentioned, in particular, terephthalic acid is preferred.
これらの二官能性芳香族カルボン酸は２種以上併用してもよい。なお、少量であればこれらの二官能性芳香族カルボン酸とともにアジピン酸、アゼライン酸、セバシン酸、ドデカンジオン酸の如き二官能性脂肪族カルボン酸、シクロヘキサンジカルボン酸の如き二官能性脂環族カルボン酸、５―ナトリウムスルホイソフタル酸等を１種または２種以上併用することができる。 Two or more of these difunctional aromatic carboxylic acids may be used in combination. In addition, in a small amount, these bifunctional aromatic carboxylic acids and bifunctional aliphatic carboxylic acids such as adipic acid, azelaic acid, sebacic acid and dodecanedioic acid, and bifunctional alicyclic carboxylic acids such as cyclohexanedicarboxylic acid are used. An acid, 5-sodium sulfoisophthalic acid, etc. can be used alone or in combination of two or more.
また、ジオール化合物としてはエチレングリコール、プロピレングリコール、ブチレングリコール、ヘキシレングリコール、ネオペンチルグリコール、２―メチル―１，３―プロパンジオール、ジエチレングリコール、トリメチレングリコールの如き脂肪族ジオール、１，４―シクロヘキサンジメタノールの如き脂環族ジオール等およびそれらの混合物等を好ましくあげることができる。また、少量であればこれらのジオール化合物と共に両末端または片末端が未封鎖のポリオキシアルキレングリコールを共重合することができる。 Examples of diol compounds include ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, neopentyl glycol, aliphatic diols such as 2-methyl-1,3-propanediol, diethylene glycol and trimethylene glycol, and 1,4-cyclohexane. Preferable examples include alicyclic diols such as dimethanol and mixtures thereof. If the amount is small, polyoxyalkylene glycol having both ends or one end unblocked can be copolymerized with these diol compounds.
更に、ポリエステルが実質的に線状である範囲でトリメリット酸、ピロメリット酸の如きポリカルボン酸、グリセリン、トリメチロールプロパン、ペンタエリスリトールの如きポリオールを使用することができる。 Furthermore, polycarboxylic acids such as trimellitic acid and pyromellitic acid, and polyols such as glycerin, trimethylolpropane, and pentaerythritol can be used as long as the polyester is substantially linear.
具体的な好ましい芳香族ポリエステルとしてはポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリヘキシレンテレフタレート、ポリエチレンナフタレート、ポリブチレンナフタレート、ポリエチレン―１，２―ビス（フェノキシ）エタン―４，４′―ジカルボキシレート等のほか、ポリエチレンイソフタレート・テレフタレート、ポリブチレンテレフタレート・イソフタレート、ポリブチレンテレフタレート・デカンジカルボキシレート等のような共重合ポリエステルをあげることができる。なかでも機械的性質、成形性等のバランスのとれたポリエチレンテレフタレートおよびポリブチレンテレフタレートが特に好ましい。 Specific preferred aromatic polyesters include polyethylene terephthalate, polybutylene terephthalate, polyhexylene terephthalate, polyethylene naphthalate, polybutylene naphthalate, polyethylene-1,2-bis (phenoxy) ethane-4,4'-dicarboxylate. In addition, there may be mentioned copolyesters such as polyethylene isophthalate / terephthalate, polybutylene terephthalate / isophthalate, polybutylene terephthalate / decane dicarboxylate, and the like. Of these, polyethylene terephthalate and polybutylene terephthalate having a good balance of mechanical properties and moldability are particularly preferable.
かかる芳香族ポリエステルは任意の方法によって合成される。例えばポリエチレンテレフタレートついて説明すれば、テレフタル酸とエチレングリコールとを直接エステル化反応させるか、テレフタル酸ジメチルの如きテレフタル酸の低級アルキルエステルとエチレングリコールとをエステル交換反応させるかまたはテレフタル酸とエチレンオキサイドとを反応させるかして、テレフタル酸のグリコールエステルおよび／またはその低重合体を生成させる第１段反応、次いでその生成物を減圧下加熱して所望の重合度になるまで重縮合反応させる第２段の反応とによって容易に製造される。 Such aromatic polyester is synthesized by any method. For example, for polyethylene terephthalate, terephthalic acid and ethylene glycol are directly esterified, or a lower alkyl ester of terephthalic acid such as dimethyl terephthalate is transesterified with ethylene glycol, or terephthalic acid and ethylene oxide are reacted. In the first stage reaction to produce a glycol ester of terephthalic acid and / or a low polymer thereof, and then the product is heated under reduced pressure to undergo a polycondensation reaction until the desired degree of polymerization is reached. It is easily produced by a stage reaction.
本発明に使用するポリエステルＣの制電剤の一方成分として使用するポリオキシアルキレン系ポリエーテルは、ポリエステルに実質的に不溶性のものであれば、単一のオキシアルキレン単位からなるポリオキシアルキレングリコールであっても、二種以上のオキシアルキレン単位からなる共重合ポリオキシアルキレングリコールであってもよく、また、下記一般式（１）、
Ｚ−［（ＣＨ２ＣＨ２Ｏ）ｎ（Ｒ１Ｏ）ｍ−Ｒ２］ｋ 式（１）
［式中、Ｚは１〜６個の活性水素原子を有する有機化合物残基、Ｒ１は炭素原子数６以上のアルキレン基又は置換アルキレン基、Ｒ２は水素原子、炭素原子数１〜４０の一価の炭化水素基、炭素原子数２〜４０の一価のヒドロキシ炭化水素又は炭素原子数２〜４０の一価のアシル基、ｋは１〜６の整数、ｎはｎ≧７０／ｋを満足する整数、ｍは１以上の整数］で表わされるポオキシエチレン系ポリエーテルが好ましい。
The polyoxyalkylene polyether used as one component of the antistatic agent for polyester C used in the present invention is a polyoxyalkylene glycol composed of a single oxyalkylene unit as long as it is substantially insoluble in the polyester. Or a copolymerized polyoxyalkylene glycol composed of two or more oxyalkylene units, and the following general formula (1),
Z - [(CH 2 CH 2 O) n (R 1 O) m-R 2] k equation (1)
[Wherein, Z is an organic compound residue having 1 to 6 active hydrogen atoms, R 1 is an alkylene group or substituted alkylene group having 6 or more carbon atoms, R 2 is a hydrogen atom, having 1 to 40 carbon atoms. A monovalent hydrocarbon group, a monovalent hydroxy hydrocarbon having 2 to 40 carbon atoms or a monovalent acyl group having 2 to 40 carbon atoms, k is an integer of 1 to 6, and n is n ≧ 70 / k. A satisfactory integer, m is an integer of 1 or more] is preferred.
かかるポリオキシアルキレン系ポリエーテルの具体例としては、分子量が４０００以上のポリオキシエチレングリコール、分子量が１０００以上のポリオキシプロピレングリコール、ポリオキシテトラメチレングリコール、分子量が２０００以上のエチレンオキサイド、プロピレンオキサイド共重合体、分子量４０００以上のトリメチロールプロパンエチレンオキサイド付加物、分子量３０００以上のノニルフェノールエチレンオキサイド付加物、並びにこれらの末端ＯＨ基に炭素数が６以上の置換エチレンオキサイドが付加した化合物があげられ、なかでも分子量が１００００〜１０００００のポリオキシエチレングコール、及び分子量が５０００〜１６０００の、ポリオキシエチレングリコールの両末端に炭素数が８〜４０のアルキル基置換エチレンオキサイドが付加した化合物が好ましい。
かかるポリオキシアルキレン系ポリエーテルの配合量は、前記芳香族ポリエステル１００重量部に対して０．２〜３０重量部の範囲である。０．２重量部より少ないときは親水性が不足して充分な制電性を呈することができない。一方３０重量部より多くしても最早制電性の向上効果は認められず、かえって得られる組成物の機械的性質を損うようになる上、該ポリエーテルがブリードアウトし易くなるため溶融成形時チップのルーダーへのかみこみ性が低下して、成形安定性も悪化するようになる。
Specific examples of such polyoxyalkylene polyethers include polyoxyethylene glycol having a molecular weight of 4000 or more, polyoxypropylene glycol having a molecular weight of 1000 or more, polyoxytetramethylene glycol, ethylene oxide having a molecular weight of 2000 or more, and propylene oxide. Polymers, trimethylolpropane ethylene oxide adducts having a molecular weight of 4000 or more, nonylphenol ethylene oxide adducts having a molecular weight of 3000 or more, and compounds in which a substituted ethylene oxide having 6 or more carbon atoms is added to the terminal OH group. However, polyoxyethylene glycol having a molecular weight of 10,000 to 100,000 and an alkyl group having 8 to 40 carbon atoms at both ends of the polyoxyethylene glycol having a molecular weight of 5000 to 16000. Compound conversion of ethylene oxide are added are preferred.
The blending amount of the polyoxyalkylene polyether is in the range of 0.2 to 30 parts by weight with respect to 100 parts by weight of the aromatic polyester. When the amount is less than 0.2 parts by weight, the hydrophilicity is insufficient and sufficient antistatic property cannot be exhibited. On the other hand, even if the amount exceeds 30 parts by weight, the antistatic effect is no longer recognized, but the mechanical properties of the resulting composition are deteriorated, and the polyether is easily bleed out, so that it is melt molded. In some cases, the insertability of the chip into the ruder is reduced, and the molding stability is also deteriorated.
本発明に使用する制電剤のもう一方の成分である有機イオン性化合物としては、例えば下記一般式（２）、（３）で示されるスルホン酸金属塩及びスルホン酸第４級ホスホニウム塩を好ましいものとしてあげることができる。
ＲＳＯ３Ｍ 式（２）
式中、Ｒは炭素原子数３〜３０のアルキル基又は炭素原子数７〜４０のアリール基、Ｍはアルカリ金属又はアルカリ土類金属を示す。上記式（２）においてＲがアルキル基のときはアルキル基は直鎖状であっても又は分岐した側鎖を有していてもよい。ＭはＮＣ，Ｋ，Ｌｉ等のアルカリ金属又はＭｇ，ＣＣ等のアルカリ土類金属であり、なかでもＬｉ，ＮＣ，Ｋが好ましい。かかるスルホン酸金属塩は１種のみを単独で用いても２種以上を混合して使用してもよい。好ましい具体例としてはステアリルスルホン酸ナトリウム、オクチルスルホン酸ナトリウム、ドデシルスルホン酸ナトリウム、炭素原子数の平均が１４であるアルキルスルホン酸ナトリウム混合物、ドデシルベンゼンスルホン酸ナトリウム混合物、ドデシルベンゼンスルホン酸ナトリウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸リチウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸マグネシウム（ハード型、ソフト型）等をあげることができる。
ＲＳＯ３ＰＲ１Ｒ２Ｒ３Ｒ４ 式（３）
式中、Ｒは上記式（２）におけるＲの定義と同じであり、Ｒ１、Ｒ２、Ｒ３及びＲ４はアルキル基又はアリール基でなかでも低級アルキル基、フェニル基又はベンジル基が好ましい。かかるスルホン酸第４級ホスホニウム塩は１種のみを単独で用いても２種以上を混合して使用してもよい。好ましい具体例としては炭素原子数の平均が１４であるアルキルスルホン酸テトラブチルホスホニウム、炭素原子数の平均が１４であるアルキルスルホン酸テトラフェニルホスホニウム、炭素原子数の平均が１４であるアルキルスルホン酸ブチルトリフェニルホスホニウム、ドデシルベンゼンスルホン酸テトラブチルホスホニウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸テトラフェニルホスホニウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸ベンジルトリフェニルホスホニウム（ハード型、ソフト型）等をあげることができる。
As the organic ionic compound which is the other component of the antistatic agent used in the present invention, for example, sulfonic acid metal salts and sulfonic acid quaternary phosphonium salts represented by the following general formulas (2) and (3) are preferable. It can be given as a thing.
RSO 3 M Formula (2)
In the formula, R represents an alkyl group having 3 to 30 carbon atoms or an aryl group having 7 to 40 carbon atoms, and M represents an alkali metal or an alkaline earth metal. In the above formula (2), when R is an alkyl group, the alkyl group may be linear or have a branched side chain. M is an alkali metal such as NC, K, Li or the like, or an alkaline earth metal such as Mg, CC, among which Li, NC, K is preferable. Such sulfonic acid metal salts may be used alone or in combination of two or more. Preferred examples include sodium stearyl sulfonate, sodium octyl sulfonate, sodium dodecyl sulfonate, a mixture of sodium alkyl sulfonate having an average of 14 carbon atoms, a mixture of sodium dodecyl benzene sulfonate, sodium dodecyl benzene sulfonate (hard type) Soft type), lithium dodecylbenzenesulfonate (hard type, soft type), magnesium dodecylbenzenesulfonate (hard type, soft type) and the like.
RSO 3 PR 1 R 2 R 3 R 4 Formula (3)
In the formula, R is the same as the definition of R in the above formula (2), and R 1 , R 2 , R 3 and R 4 are preferably an alkyl group or an aryl group, particularly a lower alkyl group, a phenyl group or a benzyl group. . Such sulfonic acid quaternary phosphonium salts may be used alone or in combination of two or more. Preferred examples include tetrabutylphosphonium alkyl sulfonate having an average of 14 carbon atoms, tetraphenyl phosphonium alkyl sulfonate having an average of 14 carbon atoms, and butyl alkyl sulfonate having an average of 14 carbon atoms. Triphenylphosphonium, tetrabutylphosphonium dodecylbenzenesulfonate (hard type, soft type), tetraphenylphosphonium dodecylbenzenesulfonate (hard type, soft type), benzyltriphenylphosphonium dodecylbenzenesulfonate (hard type, soft type), etc. Can give.
かかる有機のイオン性化合物は１種でも、２種以上併用してもよく、その配合量は、芳香族ポリエステル１００重量部に対して０．０５〜１０重量部の範囲が好ましい。０．０５重量部未満では制電性向上の効果が小さく、１０重量部を越えると組成物の機械的性質を損なうようになる上、該イオン性化合物もブリードアウトし易くなるため、溶融成形時のチップのルーダーかみこみ性が低下して、成形安定性も悪化するようになる。 Such organic ionic compounds may be used alone or in combination of two or more thereof, and the blending amount thereof is preferably in the range of 0.05 to 10 parts by weight with respect to 100 parts by weight of the aromatic polyester. If the amount is less than 0.05 parts by weight, the effect of improving antistatic properties is small. If the amount exceeds 10 parts by weight, the mechanical properties of the composition are impaired, and the ionic compound also tends to bleed out. As a result, the insertability of the chip of the chip decreases, and the molding stability also deteriorates.
本発明で使用するポリエステルＤは、本発明の目的を阻害しない範囲で、公知の艶消し剤を配合する。艶消し剤が１０ｗｔ％を超えると本発明の親糸となる未延伸糸の紡糸性が悪化するので、その範囲は０〜１０ｗｔ％とするのが好ましい。 Polyester D used in the present invention is blended with a known matting agent as long as the object of the present invention is not impaired. If the matting agent exceeds 10 wt%, the spinnability of the undrawn yarn that becomes the parent yarn of the present invention is deteriorated, so the range is preferably 0 to 10 wt%.
制電性ポリエステルＣに、制電剤である水不溶性ポリオキシエチレン系ポリエーテルと有機イオン性化合物、および必要に応じて酸化防止剤を配合することができるが、任意の方法により、上記成分を同時にまたは任意の順序で芳香族ポリエステルに配合することができる。即ち、ポリエステル繊維の紡糸が終了するまでの任意の段階、例えば芳香族ポリエステルの重縮合反応開始前、重縮合反応途中、重縮合反応終了時であってまだ溶融状態にある時点、粉粒状態、または紡糸段階等において、芳香族ポリエステルと添加成分のそれぞれを予め溶融混合して１回の操作で添加してもよく、または２回以上に分割添加してもよく、各添加成分を予め別々に芳香族ポリエステルに配合した後、これらを紡糸前等において混合してもよい。さらに、重縮合反応中期以前に添加成分を添加するときは、グリコール等の溶媒に溶解または分散させて添加してもよい。 The antistatic polyester C can contain a water-insoluble polyoxyethylene-based polyether as an antistatic agent, an organic ionic compound, and, if necessary, an antioxidant. They can be blended with the aromatic polyester simultaneously or in any order. That is, at any stage until the spinning of the polyester fiber, for example, before the start of the polycondensation reaction of the aromatic polyester, during the polycondensation reaction, at the end of the polycondensation reaction and still in a molten state, Alternatively, in the spinning stage, each of the aromatic polyester and the additive component may be melt-mixed in advance and added in one operation, or may be added in two or more divided portions, and each additive component is separately separated in advance. After blending with the aromatic polyester, these may be mixed before spinning. Furthermore, when an additional component is added before the middle stage of the polycondensation reaction, it may be added after being dissolved or dispersed in a solvent such as glycol.
本発明を構成するポリエステルマルチ繊維Ａ（単に繊維Ａと呼ぶ場合がある）は芯鞘型複合繊維であり、使用する芯成分ポリエステルＣと鞘成分ポリエステルＤの面積比は５：９５〜８０：２０の範囲にする必要がある。面積比が５：９５より小さい場合にはポリエステルＣによる制電性能の発現が不十分になり、８０：２０よりも大きくなる場合は、１０％以上のアルカリ減量を施した場合に、芯部の制電性ポリエステルＣが溶出し、制電性能が低下するとともに糸の強度が低下し、３．０ｃＮ／ｄｔｅｘ以下となり、布帛にした場合の強度が不足する為、スポーツ衣料等、強度を必要とする用途には適さず、用途が限られたものとなるので好ましくない。 The polyester multi-fiber A (simply referred to as fiber A) constituting the present invention is a core-sheath type composite fiber, and the area ratio of the core component polyester C to the sheath component polyester D used is 5:95 to 80:20. It is necessary to be in the range. When the area ratio is less than 5:95, the expression of the antistatic performance by the polyester C becomes insufficient. When the area ratio is larger than 80:20, when the alkali weight loss of 10% or more is applied, The antistatic polyester C is eluted, the antistatic performance is lowered and the strength of the yarn is reduced to be 3.0 cN / dtex or less, and the strength when used as a fabric is insufficient. This is not suitable for the purpose of use and is not preferable because the use is limited.
また、本発明の制電性ポリエステルマルチ繊維Ａの芯部および鞘部の芳香族ポリエステルには、酸化防止剤、熱安定剤、紫外線吸収剤等を配合してもよく、またそうすることは好ましいことである。その他、必要に応じて、難燃剤、蛍光増白剤、艶消削１着色剤、不活性微粒子その他の任意の添加剤を配合してもよい。 Further, the aromatic polyester of the core and sheath of the antistatic polyester multifiber A of the present invention may be blended with an antioxidant, a heat stabilizer, an ultraviolet absorber, etc., and it is preferable to do so. That is. In addition, you may mix | blend a flame retardant, a fluorescent whitening agent, the matting 1 coloring agent, an inert fine particle, and other arbitrary additives as needed.
酸化防止剤は、繊維の溶融紡糸工程等における高温度、低吐出速度、および長時間滞留などに起因する前記制電剤であるポリオキシエチレン系ポリエーテルの熱分解を抑制し、その水溶性化およびアルカリ耐久性の低下などの発生を防止することができる。本発明において用いられる酸化防止剤としては、それが酸化防止能を有する限り、その種類に制限はない。 Antioxidant suppresses thermal decomposition of polyoxyethylene-based polyether, which is the antistatic agent, due to high temperature, low discharge speed, and long-term residence in the fiber spinning process, etc. Further, it is possible to prevent the occurrence of a decrease in alkali durability. The antioxidant used in the present invention is not limited as long as it has antioxidant ability.
酸化防止剤としては、ヒンダードフェノール系化合物、チオプロピオネート系化合物、ホスファイト系化合物などが挙げられ、１種のみを単独で用いても２種以上を混合して使用してもよい。また酸化防止剤の配合量は、芳香族ポリエステルに対して０．０２〜３重量％の範囲にあることが好ましい。この配合量が０．０２重量％より少ないときは、ポリオキシエチレン系ポリエーテル重合体に対する熱分解抑制効果が不充分であり、また、それを３重量％より多くしても、その熱分解抑制効果は飽和してそれ以上の向上は認められず、かえって得られる繊維の機械的性質や色相等が損なわれるようになる。 Examples of the antioxidant include hindered phenol compounds, thiopropionate compounds, phosphite compounds and the like, and only one kind may be used alone or two or more kinds may be mixed and used. Moreover, it is preferable that the compounding quantity of antioxidant exists in the range of 0.02 to 3 weight% with respect to aromatic polyester. When the blending amount is less than 0.02% by weight, the thermal decomposition inhibiting effect on the polyoxyethylene-based polyether polymer is insufficient, and even if it is more than 3% by weight, the thermal decomposition is inhibited. The effect is saturated and no further improvement is recognized, but the mechanical properties, hue, etc. of the resulting fiber are impaired.
また、本発明のポリエステルマルチ繊維Ａの外周の断面形状、ならびに芯部分が形成する図形の形状は、織編物の電性、張り、腰、風合、光沢なとの目的に応じて任意の形状をとることができ、例えば、円形断面の他、三角、偏平、四角、三角、星形、六角、ブーメラン形等を例示できる。また芯成分と鞘成分とは同心形状である必要はなく、芯の中心が偏った形状のものでもよく、また、外周の断面形状と芯部分が形成する図形の形状も、同じ形状であってもよいし異なった形状でもよい。 Moreover, the cross-sectional shape of the outer periphery of the polyester multi-fiber A of the present invention and the shape of the figure formed by the core portion can be any shape depending on the purpose of the woven or knitted fabric such as electrical properties, tension, waist, texture, and gloss. For example, in addition to a circular cross section, a triangle, a flat shape, a square, a triangle, a star, a hexagon, a boomerang, and the like can be exemplified. In addition, the core component and the sheath component do not have to be concentric, may have a shape in which the center of the core is deviated, and the cross-sectional shape of the outer periphery and the shape of the figure formed by the core portion are the same shape. Or different shapes.
本発明のポリエステルマルチ繊維Ａは、例えば従来公知の複合紡糸装置を用い、鞘側に前述したポリエステルＤを、芯部に制電剤である水不溶性ポリオキシエチレン系ポリエーテルと有機イオン性化合物、および必要に応じて上記ホスファイト系等の酸化防止剤の少なくとも１種を配合した制電性ポリエステルＣを使用して、２０００〜３０００ｍ／分の速度で溶融紡糸して得ることができる。 The polyester multi-fiber A of the present invention uses, for example, a conventionally known composite spinning apparatus, the polyester D described above on the sheath side, a water-insoluble polyoxyethylene-based polyether as an antistatic agent and an organic ionic compound in the core part, And if necessary, it can be obtained by melt spinning at a speed of 2000 to 3000 m / min using antistatic polyester C blended with at least one of the above-mentioned antioxidants such as phosphite.
本発明の制電性ポリエステルマルチ繊維Ａは、伸度（ＥＬＡ）は８０％以上、好ましくは１００〜２００％である必要があり、１０％伸長時の弾性回復率（ＥＲＡ）は５０％以下、好ましくは４０％以下である必要があり、伸長剛性率（ＥＭＡ）は５．８９ＧＰａ（６００ｋｇ／ｍｍ２）以下、好ましくは１．９６〜４．９１ＧＰａ（２００〜５００ｋｇ／ｍｍ２）である必要があり、結晶化度（ＸｐＡ）は２５％以上、好ましくは３６〜６０％である必要があり、１６０℃における熱応力（ＴＳＡ）が０．４４ｍＮ／ｄｔｅｘ（５０ｍｇ／ｄｅ）以下である必要があり、さらには沸水収縮率（ＢＷＳＡ）は３％以下である必要がある。このような特性を示す時、制電性ポリエステルマルチ繊維Ａは混繊糸を加熱処理したとき浮いた状態となり且つ伸長方向に荷重が掛かっても応力負担をせずに嵩性向上のみに寄与し、結果として皺の発生を抑制する。 The antistatic polyester multifiber A of the present invention needs to have an elongation (ELA) of 80% or more, preferably 100 to 200%, and an elastic recovery rate (ERA) at 10% elongation of 50% or less, preferably should be 40% or less, elongation modulus (EMA) is 5.89GPa (600kg / mm 2) or less, preferably have a 1.96~4.91GPa (200~500kg / mm 2) Yes, the crystallinity (XpA) needs to be 25% or more, preferably 36 to 60%, and the thermal stress (TSA) at 160 ° C. needs to be 0.44 mN / dtex (50 mg / de) or less. Further, the boiling water shrinkage (BWSA) needs to be 3% or less. When exhibiting such characteristics, the antistatic polyester multi-fiber A is in a floating state when the mixed yarn is heat-treated, and contributes only to improvement in bulk without applying a stress even when a load is applied in the elongation direction. As a result, the generation of wrinkles is suppressed.
このような特性を有するポリエステルマルチ繊維Ａは、例えば、前述のポリエステルを温度２８０〜３００℃で溶融し、紡糸口金から溶融吐出し、冷却固化した紡出糸条に油剤を付与し、空気噴射孔が３孔以上のインターレース付与装置を用いて圧力０．１〜０．３ＭＰａの空気を噴射してインターレースを付与した後、ポリエステルのガラス転移温度以下に設定した予熱ローラーおよび延伸ローラーを介して（予熱ローラー引取速度：１５００〜２５００ｍ／分、延伸倍率：１．１〜１．５）を一旦ワインダーに捲き取る。次いで、得られた延伸糸を、速度５００〜１４００ｍ／分で、７０〜１１０℃に加熱した予熱ローラーおよび１７０〜２４０℃に設定した非接触式ヒータを経て、０．８〜１．１倍の延伸倍率で熱セット（延伸倍率１以下では弛緩熱セットとなる）を施すことにより得ることができる。 The polyester multi-fiber A having such characteristics is obtained by, for example, melting the above-described polyester at a temperature of 280 to 300 ° C., melting and discharging from the spinneret, and applying an oil agent to the cooled and solidified spinning yarn. After applying interlace by spraying air with a pressure of 0.1 to 0.3 MPa using an interlace applying device having 3 or more holes, it is passed through a preheating roller and a drawing roller set below the glass transition temperature of polyester (preheating). Roller take-up speed: 1500-2500 m / min, draw ratio: 1.1-1.5) are once wound up in a winder. Subsequently, the obtained drawn yarn was passed through a preheating roller heated to 70 to 110 ° C. at a speed of 500 to 1400 m / min and a non-contact heater set to 170 to 240 ° C. It can be obtained by applying a heat set at a draw ratio (a relaxed heat set at a draw ratio of 1 or less).
次に、本発明の混繊糸を構成する他方成分であるポリエステルマルチ繊維Ｂ（単に繊維Ｂと呼ぶ場合がある）は、伸長方向の荷重を主として負担して形態安定性や後加工工程での安定性を保持するため、伸度（ＥＬＢ）は４０％以下、好ましくは３０％以下である必要があり、伸長剛性率（ＥＭＢ）は７．８５ＧＰａ（８００ｋｇ／ｍｍ２）以上、好ましくは８．８３〜１４．７ＧＰａ（９００〜１５００ｋｇ／ｍｍ２）である必要がある。また、熱処理により良好な嵩性を発現させるために沸水収縮率（ＢＷＳＢ）は５％以上、好ましくは７〜２０％である必要があり、さらには、布帛とした後にピンテンター等で熱セットする際に前記ポリエステルマルチ繊維Ａに応力が掛からないようにして風合の低下を抑制するため、１６０℃における熱応力（ＴＳＢ）は０．８８ｍＮ／ｄｔｅｘ（１００ｍｇ／ｄｔｅｘ）以上、好ましくは１．７６ｍＮ／ｄｔｅｘ（２００ｍｇ／ｄｔｅｘ）以上とする必要がある。 Next, the polyester multi-fiber B (which may be simply referred to as fiber B), which is the other component constituting the blended yarn of the present invention, mainly bears a load in the elongation direction and is used in form stability and post-processing steps. In order to maintain stability, the elongation (ELB) needs to be 40% or less, preferably 30% or less, and the elongation rigidity (EMB) is 7.85 GPa (800 kg / mm 2 ) or more, preferably 8. It is necessary to be 83 to 14.7 GPa (900 to 1500 kg / mm 2 ). Also, in order to develop good bulkiness by heat treatment, the boiling water shrinkage (BWSB) needs to be 5% or more, preferably 7 to 20%. In order to prevent the polyester multi-fiber A from being stressed and to suppress a decrease in feel, the thermal stress (TSB) at 160 ° C. is 0.88 mN / dtex (100 mg / dtex) or more, preferably 1.76 mN / It is necessary to set it to dtex (200 mg / dtex) or more.
このような特性を有するポリエステルマルチ繊維Ｂは、例えば、前述のポリエステテルからなる未延伸繊維を延伸する際、その延伸温度や延伸倍率などを適宜調整すればよい。例えば、伸度や剛性率は延伸倍率によって調整し、沸水収縮率は延伸時の熱セット条件によって調整すればよい。特に高収縮を望む場合には、ノープレート延伸などが適当である。熱応力は、延伸倍率や延伸時の加熱温度、さらには、未延伸繊維の紡糸速度によって調整することができる。しかし、あまりに紡糸引取速度が高すぎると、延伸後の熱応力を高くできなくなる場合があるので、２５００ｍ／分以下、好ましくは１７００ｍ／分以下の低紡速の未延伸繊維を延伸するのが好ましい。なお、これらの特性を調整する別の方法として、ポリエステルに第３成分を共重合する方法があり、例えばイソフタル酸成分を共重合すると高収縮特性を有するものが容易に得られる。 For example, when the unstretched fiber made of the above-mentioned polyester is stretched, the polyester multifiber B having such characteristics may be appropriately adjusted in its stretching temperature, stretch ratio, and the like. For example, the elongation and rigidity can be adjusted by the draw ratio, and the boiling water shrinkage can be adjusted by the heat setting conditions during drawing. In particular, when high shrinkage is desired, no-plate stretching or the like is appropriate. The thermal stress can be adjusted by the draw ratio, the heating temperature during drawing, and the spinning speed of the undrawn fiber. However, if the spinning take-up speed is too high, the thermal stress after drawing may not be increased. Therefore, it is preferable to draw undrawn fibers with a low spinning speed of 2500 m / min or less, preferably 1700 m / min or less. . In addition, as another method for adjusting these characteristics, there is a method of copolymerizing a third component with polyester. For example, when an isophthalic acid component is copolymerized, a polyester having high shrinkage characteristics can be easily obtained.
本発明の混繊糸は、上記制電性ポリエステルマルチ繊維Ａを弛緩熱処理後ポリエステルマルチ繊維Ｂとを交絡混繊する必要がある。糸条に熱的変形を与える、例えば仮撚捲縮加工を施すことは好ましくなく、かかる方法であっては皺回復効果は得られなくなる。その理由は、第一は仮撚捲縮加工における加熱処理、伸長、捩じりなどによってポリエステルマルチ繊維Ａの物性が変わり、伸度が減ったり熱応力が高くなったり弾性回復率が向上したりしてズルズル伸びる性質が失われたり、ポリエステルマルチ繊維Ａに捲縮が付与されると、隣の糸と絡んだり抵抗が増えたりして、織物等の布帛になした時に織組織の中でずれた糸の位置が元に戻り難くなって皺が発生しやすくなるものと推察される。 The blended yarn of the present invention needs to be entangled with the polyester multifiber B after relaxation heat treatment of the antistatic polyester multifiber A. It is not preferable to give the yarn a thermal deformation, for example, a false twist crimping process. With such a method, the wrinkle recovery effect cannot be obtained. The reason is that the physical properties of the polyester multi-fiber A change due to heat treatment, stretching, twisting, etc. in the false twist crimping process, the elongation decreases, the thermal stress increases, and the elastic recovery rate improves. As a result, when the polyester multi-fiber A is crimped, the entangled property of the polyester multi-fiber A is entangled with the adjacent yarn or the resistance increases. It is presumed that the position of the warp thread is difficult to return to the original position and wrinkles are likely to occur.
なお、空気噴射による交絡の場合、空気の噴射方向は糸と直角方向に当てても糸の進行方向に沿って当ててもよいが、前者によれば比較的光沢に優れた製品が得られ、一方後者によれば比較的ソフトな風合の製品が得られる。 In the case of entanglement by air injection, the air injection direction may be applied in the direction perpendicular to the yarn or along the traveling direction of the yarn, but according to the former, a product with relatively high gloss is obtained, On the other hand, according to the latter, a relatively soft product can be obtained.
さらに、ポリエステルマルチ繊維Ａ、ポリエステルマルチ繊維Ｂの間にオーバーフィード差を設けて空気複合加工してもよいが、あまりに差を付けすぎるとループが多数発生しやすくなるので、通常はほぼ同一のオーバーフィード率が採用される。 Furthermore, it is possible to provide an overfeed difference between the polyester multi-fiber A and the polyester multi-fiber B and perform air composite processing. However, if too much difference is made, many loops are likely to occur, so usually the same over Feed rate is adopted.
ポリエステルマルチ繊維Ａとポリエステルマルチ繊維Ｂとの複合割合（混繊比）は、ポリエステルマルチ繊維Ａ／ポリエステルマルチ繊維Ｂの重量比で４５／５５〜７０／３０である必要がある。特にポリエステルマルチ繊維Ａの方が多い方が本発明の効果が発生しやすいので、ポリエステルマルチ繊維Ａ／ポリエステルマルチ繊維Ｂの重量割合で５５／４５〜７０／３０が特に好ましい。なお、今まではポリエステルマルチ繊維Ａ、ポリエステルマルチ繊維Ｂは夫々１本の糸条を例として説明したが、これらは勿論２本以上の糸条を用いてもよく、要するに本発明が要件としている物性を満足する繊維であれば何本の糸条を用いてもよい。さらには、本発明にかかる上記物性を満足しない第３の糸条を添えて複合しても構わない。例えば、金属メッキ繊維やカーボン粒子混入繊維を複合して導電性を付与してもよいが、このような繊維の割合が多くなりすぎると、本発明の目的である皺回復性の改善が不十分となるので、併用率は高々３０％とするのが望ましい。 The composite ratio (mixing ratio) of the polyester multifiber A and the polyester multifiber B needs to be 45/55 to 70/30 in terms of the weight ratio of the polyester multifiber A / polyester multifiber B. Since the effect of this invention is easy to generate | occur | produce especially the one where there are many polyester multi fiber A, 55 / 45-70 / 30 is especially preferable at the weight ratio of polyester multi fiber A / polyester multi fiber B. Heretofore, the polyester multi-fiber A and the polyester multi-fiber B have been described using one yarn as an example, but of course, two or more yarns may be used, and in short, the present invention is a requirement. Any number of yarns may be used as long as they satisfy the physical properties. Furthermore, it may be combined with a third yarn that does not satisfy the above physical properties according to the present invention. For example, metal plated fibers or carbon particle-containing fibers may be combined to impart conductivity. However, if the proportion of such fibers increases too much, the improvement of wrinkle recovery that is the object of the present invention is insufficient. Therefore, the combined use rate is desirably 30% at most.
以下、実施例をあげて本発明をさらに具体的に説明する。なお、実施例中の各測定項目は下記の方法で測定した。 Hereinafter, the present invention will be described more specifically with reference to examples. In addition, each measurement item in an Example was measured with the following method.
（１）風合い
（ソフト感）
レベル１：ソフトでしなやかな感触がある
レベル２：ややソフト感が乏しいが反撥性は感じられる
レベル３：カサカサした触感あるいは硬い触感である。
(1) Texture (soft feeling)
Level 1: Soft and supple feel Level 2: Slightly soft feeling but repellent feel Level 3: Crispy or hard feel
（２）帯電性試験方法
Ｃ法（半減期測定法）
本発明の複合延伸糸を、筒編みし、染色し、調湿後、試験片をコロナ放電場で
帯電させた後、試験片を回転させながら摩擦布で摩擦し、発生した帯電圧を測定する。
Ｌ１０９４帯電性試験方法Ｄ法（摩擦帯電圧測定法）に順ずる。
制電効果については、摩擦帯電圧が、約２０００Ｖ以下（好ましくは１５００Ｖ以下）
であれば、制電効果が奏される。
(2) Chargeability test method C method (half-life measurement method)
The composite drawn yarn of the present invention is knitted, dyed, conditioned, and charged with a test piece in a corona discharge field, then rubbed with a friction cloth while rotating the test piece, and the generated charged voltage is measured. .
Conforms to L1094 chargeability test method D (friction charging voltage measurement method).
Regarding the antistatic effect, the frictional voltage is about 2000 V or less (preferably 1500 V or less).
Then, the antistatic effect is produced.
（３）伸度（ＥＬ）
ＪＩＳ Ｌ １０１３に準拠して測定した。
(3) Elongation (EL)
It measured based on JISL1013.
（４）１０％伸長時弾性回復率（ＥＲ）
ＪＩＳ Ｌ １０１３に準拠し、試料の試長を２５ｃｍとして初荷重をデニール当り１／３０ｇ掛けた状態で両端をエアチャックで把持固定する。測定条件は引張速度を２０％／分として１０％伸長させたのち、返り速度を２０％／分で除重しながら、初荷重点まで返す。測定回数は３回行いその平均値を求めた。
１０％伸長時弾性回復率＝（１０％伸長時の伸び−残留伸び）／１０％伸長時の伸び×１００
(4) Elastic recovery (ER) at 10% elongation
In accordance with JIS L 1013, the sample length is 25 cm and both ends are gripped and fixed with an air chuck with an initial load of 1/30 g per denier. The measurement condition is that the tensile speed is 20% / min, the elongation is 10%, and the weight is returned to the initial load point while the return speed is 20% / min. The measurement was performed three times, and the average value was obtained.
Elastic recovery at 10% elongation = (Elongation at 10% elongation−Residual elongation) / 10% elongation at elongation × 100
（５）伸長剛性率（ＥＭ）
定速伸長引張試験機とこれに連動した記録装置を用いて測定する。試料の試長を２５ｃｍとして初荷重をデニール当り１／３０ｇ掛けた状態で両端をエアチャックで把持固定する。測定条件は引張速度２０％／分で初期荷伸曲線図により最傾斜曲線部分に接線を引き、１００％伸長時の応力を読み取る。測定は５回行い、その平均値を求めた。
伸長剛性率（ＥＭ）＝９×１００×１％伸長時の応力（ｇ）×試料比重／繊度（デニール）
(5) Elongation rigidity (EM)
Measurement is performed using a constant-speed extension tensile tester and a recording device linked to this. The sample length is 25 cm and the both ends are gripped and fixed with an air chuck in a state where the initial load is 1/30 g per denier. The measurement condition is a tensile rate of 20% / min. A tangent line is drawn on the slope of the slope of the initial load-drawing curve, and the stress at 100% elongation is read. The measurement was performed 5 times, and the average value was obtained.
Elongation rigidity (EM) = 9 × 100 × 1% Elongation stress (g) × Sample specific gravity / fineness (denier)
（６）沸水収縮率（ＢＷＳ）
試料を検尺機（１周１．１２５ｍ）にて１０回転し綛を作製する。次に、デニール当り１／３０ｇの軽荷重を掛けて綛の長さを測定する。次に軽荷重を外し、収縮が防げられない様にガーゼに包みさらに金網カゴに入れて沸水中に３０分間浸漬させた後、取り出して布で水分を切り自然乾燥し再び軽荷重を綛に掛けて長さを計る。沸水収縮率は次式より算出し、測定はｎ＝５で行ってその平均値を求めた。
沸水収縮率（ＢＷＳ）＝（浸漬前の長さ−自然乾燥後の長さ）／浸漬前の長さ×１００
(6) Boiling water shrinkage (BWS)
The sample is rotated 10 times with a measuring machine (1 round 1.125 m) to produce a ridge. Next, the length of the ridge is measured by applying a light load of 1/30 g per denier. Next, remove the light load, wrap it in gauze so that shrinkage cannot be prevented, put it in a wire mesh basket, soak it in boiling water for 30 minutes, take it out, drain the moisture with a cloth, let it dry naturally, and apply the light load again to the bag. And measure the length. The boiling water shrinkage was calculated from the following equation, and the measurement was performed at n = 5 to obtain the average value.
Boiling water shrinkage (BWS) = (length before immersion−length after natural drying) / length before immersion × 100
（７）熱応力（ＴＳ）（１６０℃における）
熱応力測定器と、これに連動した記録装置を用いて測定する。資料をサンプリング治具を用いて５ｃｍの輪を作る。次に熱応力測定器と記録装置を２０℃〜３００℃、応力０〜２０ｇの範囲が測定可能な状態に準備し、先にサンプリングした試料５ｃｍの輪を熱応力測定器の上部、下部のフックに掛けてデニール当り１／３０ｇの初荷重を掛けた後、熱応力の測定に入る。昇温速度は３００℃／１２０秒で行う。３００℃に昇温した時点で測定を完了する。測定は３回行う。熱応力（１６０℃）は、１６０℃点の応力ｇを読取り、１ｄｔｅｘ当たりの応力に換算した。
(7) Thermal stress (TS) (at 160 ° C)
The measurement is performed using a thermal stress measuring instrument and a recording device linked to this. Make a 5cm ring using the sampling jig. Next, the thermal stress measuring instrument and the recording device are prepared in a state in which the range of 20 ° C. to 300 ° C. and the stress of 0 to 20 g can be measured. After applying an initial load of 1/30 g per denier, measurement of thermal stress is started. The heating rate is 300 ° C./120 seconds. The measurement is completed when the temperature is raised to 300 ° C. The measurement is performed three times. For the thermal stress (160 ° C.), the stress g at the 160 ° C. point was read and converted to a stress per 1 dtex.
［実施例１］
テレフタル酸ジメチル１００部、エチレングリコール６０部、酢酸カルシウム１水塩０．０６部（テレフタル酸ジメチルに対して０．０６６モル％）および整色剤として酢酸コバルト４水塩０．０１３部（テレフタル酸ジメチルに対して０．０１モル％）をエステル交換反応缶に仕込み、この反応物を窒素ガス雰囲気下で４時間かけて１４０℃から２２０℃まで昇温し、反応缶中に生成するメタノールを系外に留去しながらエステル交換反応させた。エステル交換反応終了後、反応混合物に安定剤としてリン酸トリメチル０．０５８部（テレフタル酸ジメチルに対して０．０８０モル％）、および消泡剤としてジメチルポリシロキサンを０．０２４部加えた。次に、１０分後に、反応混合物に三酸化アンチモン０．０４１部（テレフタル酸ジメチルに対して０．０２７モル％）を添加し、同時に過剰のエチレングリコールを留去しながら２４０℃まで昇温し、その後、反応混合物を重合反応缶に移した。次いで１時間４０分かけて７６０ｍｍＨｇから１ｍｍＨｇまで減圧するとともに２４０℃から２８０℃まで昇温して重縮合反応せしめた後、
（ポリエステルＣの作成）
制電剤としてポリオキシアルキレン系ポリエーテルとして下記式（４）
100 parts of dimethyl terephthalate, 60 parts of ethylene glycol, 0.06 part of calcium acetate monohydrate (0.066 mol% with respect to dimethyl terephthalate) and 0.013 part of cobalt acetate tetrahydrate as a color adjuster (terephthalic acid) 0.01 mol% with respect to dimethyl) was charged into a transesterification reactor, and the reaction product was heated from 140 ° C. to 220 ° C. over 4 hours under a nitrogen gas atmosphere. The ester exchange reaction was carried out while distilling out. After completion of the transesterification reaction, 0.058 parts of trimethyl phosphate (0.080 mol% with respect to dimethyl terephthalate) as a stabilizer and 0.024 parts of dimethylpolysiloxane as an antifoaming agent were added to the reaction mixture. Next, after 10 minutes, 0.041 part of antimony trioxide (0.027 mol% with respect to dimethyl terephthalate) was added to the reaction mixture, and the temperature was raised to 240 ° C. while distilling off excess ethylene glycol. Thereafter, the reaction mixture was transferred to a polymerization reactor. Next, after reducing the pressure from 760 mmHg to 1 mmHg over 1 hour and 40 minutes and raising the temperature from 240 ° C. to 280 ° C. to cause the polycondensation reaction,
(Creation of polyester C)
The following formula (4) as a polyoxyalkylene polyether as an antistatic agent
（ポリエステルＤの作成）
制電剤を添加しないものをポリエステルＤとし、常法によりチップ化した。
(Creation of polyester D)
A polyester to which no antistatic agent was added was polyester D, which was chipped by a conventional method.
（ポリエステルマルチ繊維Ａの製造）
製糸化は以下の通り行った。乾燥ポリマーを紡糸設備にて各々常法で溶融し、ギヤポンプを経て２成分複合紡糸ヘッドに供給した。芯と鞘ポリマーの比率が表１記載の値となるように設定した。同時に供給された芯部と鞘部の溶融ポリマーは、ノズル孔径０．２５ｍｍの円形複合紡糸孔を７２個穿設した紡糸口金から、通常のクロスフロー型紡糸筒からの冷却風で冷却・固化し、紡糸油剤を付与しつつ一つの糸条として集束し、３０００ｍ／ｍｉｎの速度で引き取り、複屈折率０．０３５の９０ｄｔｅｘ／７２フィラメント（単糸繊度１．２５ｄｔｅｘ）の芯鞘型ポリエステル未延伸糸を得た。伸度（ＥＬＡ）は１２０％、１０％伸長時の弾性回復率（ＥＲＡ）は３０％、伸長剛性率（ＥＭＡ）は３．９２ＧＰａ（４００ｋｇ／ｍｍ２）、結晶化度（ＸｐＡ）は４０％、沸水収縮率（ＢＷＳＡ）は１％、１６０℃における熱応力（ＴＳＡ）は０．２６ｍＮ／ｄｔｅｘ（３０ｍｇ／ｄｔｅｘ）であった。
(Manufacture of polyester multi-fiber A)
The yarn production was performed as follows. The dried polymer was melted in a usual manner in a spinning facility, and supplied to a two-component composite spinning head via a gear pump. It set so that the ratio of a core and a sheath polymer might become the value of Table 1. The molten polymer in the core and the sheath supplied simultaneously is cooled and solidified by cooling air from a normal cross-flow type spinning cylinder from a spinneret having 72 circular composite spinning holes having a nozzle hole diameter of 0.25 mm. The core sheath type polyester unstretched yarn of 90 dtex / 72 filaments (single yarn fineness of 1.25 dtex) having a birefringence of 0.035 and being bundled as a single yarn while being applied with a spinning oil, taken up at a speed of 3000 m / min. Got. The elongation (ELA) is 120%, the elastic recovery rate (ERA) at 10% elongation is 30%, the elongation rigidity (EMA) is 3.92 GPa (400 kg / mm 2 ), and the crystallinity (XpA) is 40%. The boiling water shrinkage (BWSA) was 1%, and the thermal stress (TSA) at 160 ° C. was 0.26 mN / dtex (30 mg / dtex).
（ポリエステルマルチ繊維Ｂの製造）
一方、イソフタル酸を１０モル％共重合した固有粘度（３５℃のオルソクロロフェノール溶液で測定）が０．６４のポリエチレンテレフタレートを紡糸口金から溶融吐出し、該吐出糸条を冷却固化させた後に油剤を付与し、紡速１２００ｍ／分で一旦捲取った後、予熱ローラー温度８５℃、熱セットヒーター（接触式）温度１７０℃、延伸倍率３．１倍、延伸速度１２００ｍ／分で行い５５ｄｔｅｘ／１２フィラメントのポリエステルマルチ繊維Ｂ（単糸繊度４．６ｄｔｅｘ）を得た。ポリエステルマルチ繊維Ｂの伸度（ＥＬＢ）は３０％、伸長剛性率（ＥＭＢ）は１１．７７ＧＰａ（１２００ｋｇ／ｍｍ２）、沸水収縮率（ＢＷＳＢ）は１７％、１６０℃における熱応力（ＴＳＢ）は４．４ｍＮ／ｄｔｅｘであった。
(Manufacture of polyester multifiber B)
On the other hand, polyethylene terephthalate having an intrinsic viscosity (measured with an orthochlorophenol solution at 35 ° C.) of 0.64 copolymerized with 10 mol% of isophthalic acid is melted and discharged from a spinneret, and the discharged yarn is cooled and solidified, and then the oil agent And after having been picked once at a spinning speed of 1200 m / min, a preheating roller temperature of 85 ° C., a heat set heater (contact type) temperature of 170 ° C., a draw ratio of 3.1 times, and a draw speed of 1200 m / min are carried out to 55 dtex / 12. A filament polyester multi-fiber B (single yarn fineness 4.6 dtex) was obtained. The elongation (ELB) of the polyester multi-fiber B is 30%, the elongation rigidity (EMB) is 11.77 GPa (1200 kg / mm 2 ), the boiling water shrinkage (BWSB) is 17%, and the thermal stress (TSB) at 160 ° C. is It was 4.4 mN / dtex.
（混繊糸の作成）
前記制電性ポリエステルマルチ繊維Ａを、予熱ローラー温度１１０℃、熱セットヒーター（非接触式）温度２３０℃、弛緩率２％、速度６００ｍ／分で弛緩熱処理した後、前記ポリエステル繊維Ｂと合糸して空気交絡ノズルで混繊交絡して複合糸となし、ワインダーに捲取って１５０ｄｔｅｘ／８４フィラメントの混繊糸を得た。制電性ポリエステルマルチ繊維Ａの単糸繊度は１．２ｄｔｅｘであった。
得られた混繊糸を経糸及び緯糸に用い、羽二重に製織し、常法にしたがって精練、熱セット、染色を施して無地の染め織物を得た。評価結果を表３に示す。
なお、風合についての各評価項目は、熟練した５人のパネラーによる官能評価で、全員が極めて良好と判定したものを（良）、３人以上が良好と判断したものを（可）、３人以上が不良と判定したものを（不可）と、三段階にランク付けした。
また皺回復性の評価としては、図２のような器具に織物を筒状に挿入し、これに重しを置いて３時間放置後、重しを取って３０分放置した時の皺の程度を表１の基準で採点したものである。
(Making mixed yarn)
The antistatic polyester multi-fiber A is subjected to a relaxation heat treatment at a preheating roller temperature of 110 ° C., a heat set heater (non-contact type) temperature of 230 ° C., a relaxation rate of 2%, and a speed of 600 m / min, and then combined with the polyester fiber B. Then, mixed fibers were entangled with an air entangled nozzle to form a composite yarn, which was wound by a winder to obtain a mixed yarn of 150 dtex / 84 filament. The single yarn fineness of the antistatic polyester multifiber A was 1.2 dtex.
The obtained blended yarn was used for warp and weft, woven double-folded, and subjected to scouring, heat setting and dyeing according to a conventional method to obtain a plain dyed fabric. The evaluation results are shown in Table 3.
In addition, each evaluation item about the texture is a sensory evaluation by five skilled panelists, all judged to be very good (good), three or more judged good (possible), 3 Those that were judged as bad by people or more were ranked as (impossible) in three stages.
The evaluation of wrinkle recovery is the degree of wrinkle when a woven fabric is inserted into a tool as shown in Fig. 2 and placed on it for 3 hours and then left for 30 minutes. Are scored according to the criteria in Table 1.
［実施例２、比較例１〜４］
表２に示す条件で行った以外は実施例１と同様な方法で行った。
[Example 2, Comparative Examples 1 to 4]
The procedure was the same as in Example 1 except that the procedure was performed under the conditions shown in Table 2.
細繊度で風合いに優れ、皺回復性も向上しているので、用途として、学生服、ユニフォームに有用である。 Because it has fineness, excellent texture, and improved wrinkle recovery, it is useful for school uniforms and uniforms.
（イ）：皺回復評価器具に織物を挿入した状態
（ロ）：織物に重しを置いた状態
(I): A state in which the fabric is inserted into the wrinkle recovery evaluation instrument (B): A state in which a weight is placed on the fabric
Claims (2)
（１）ポリエステルマルチ繊維Ａの芯部の面積と鞘部の面積との比が５：９５〜８０：２０であること。
（２）混繊糸の摩擦帯電圧が２０００Ｖ以下であること。
（３）ポリエステルマルチ繊維Ａ／ポリエステルマルチ繊維Ｂの重量比が４５／５５〜７０／３０であること。
（４）制電性ポリエステルＣが芳香族ポリエステル１００重量部に対して、制電剤として、下記一般式（１）で表されるポリオキシアルキレン系ポリエーテルを０．２〜３０重量部及び該ポリエステルと実質的に非反応性の有機イオン性化合物０．０５〜１０重量部を含有してなる制電性ポリエステルであること。
Ｚ−［（ＣＨ２ＣＨ２Ｏ）ｎ（Ｒ１Ｏ）ｍ−Ｒ２］ｋ 式（１）
［式中、Ｚは１〜６個の活性水素原子を有する有機化合物残基、Ｒ１は炭素原子数６以上のアルキレン基又は置換アルキレン基、Ｒ２は水素原子、炭素原子数１〜４０の一価の炭化水素基、炭素原子数２〜４０の一価のヒドロキシ炭化水素又は炭素原子数２〜４０の一価のアシル基、ｋは１〜６の整数、ｎはｎ≧７０／ｋを満足する整数、ｍは１以上の整数］ Single yarn fineness is 1.5 dtex or less, elongation (ELA) is 80% or more, elastic recovery (ERA) at 10% elongation is 50% or less, elongation rigidity (EMA) is 5.89 GPa or less, crystallization A core-sheath type composite fiber having a degree (XpA) of 25% or more, a boiling water shrinkage (BWSA) of 3% or less, and a thermal stress (TSA) at 160 ° C. of 0.44 mN / dtex or less, wherein the core part is antistatic. The polyester multifiber (A), which is formed of polyester D with a sheath part of 0 to 10% by weight of matting agent, is relaxed and heat-treated, and the elongation (ELB) is 40% or less. Polyester multifiber (B) with a rate (EMB) of 7.85 GPa or more, boiling water shrinkage (BWSB) of 5% or more, and thermal stress (TSB) at 160 ° C. of 0.88 mN / dtex or more, and then entangled And a method for producing a polyester mixed yarn characterized by satisfying the following requirements.
(1) The ratio of the area of the core part of polyester multi fiber A and the area of a sheath part is 5: 95-80: 20.
(2) The friction band voltage of the blended yarn is 2000 V or less.
(3) The weight ratio of polyester multifiber A / polyester multifiber B is 45/55 to 70/30.
(4) Antistatic polyester C is 0.2 to 30 parts by weight of polyoxyalkylene polyether represented by the following general formula (1) as an antistatic agent with respect to 100 parts by weight of aromatic polyester and It is an antistatic polyester comprising 0.05 to 10 parts by weight of an organic ionic compound that is substantially non-reactive with polyester.
Z - [(CH 2 CH 2 O) n (R 1 O) m-R 2] k equation (1)
[Wherein, Z is an organic compound residue having 1 to 6 active hydrogen atoms, R 1 is an alkylene group or substituted alkylene group having 6 or more carbon atoms, R 2 is a hydrogen atom, having 1 to 40 carbon atoms. A monovalent hydrocarbon group, a monovalent hydroxy hydrocarbon having 2 to 40 carbon atoms or a monovalent acyl group having 2 to 40 carbon atoms, k is an integer of 1 to 6, and n is n ≧ 70 / k. Satisfied integer, m is an integer of 1 or more]
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042521A (en) * | 2019-05-15 | 2019-07-23 | 江南大学 | The production method of multicomponent fibre Intelligent Hybrid mixed yarn |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042521A (en) * | 2019-05-15 | 2019-07-23 | 江南大学 | The production method of multicomponent fibre Intelligent Hybrid mixed yarn |
| CN110042521B (en) * | 2019-05-15 | 2021-07-06 | 江南大学 | Production method of multi-component fiber intelligent mixed blended yarn |
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