JPH11189923A - Polyester conjugate fiber - Google Patents

Polyester conjugate fiber

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Publication number
JPH11189923A
JPH11189923A JP35364897A JP35364897A JPH11189923A JP H11189923 A JPH11189923 A JP H11189923A JP 35364897 A JP35364897 A JP 35364897A JP 35364897 A JP35364897 A JP 35364897A JP H11189923 A JPH11189923 A JP H11189923A
Authority
JP
Japan
Prior art keywords
component
polyester
polymer
viscosity
fiber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP35364897A
Other languages
Japanese (ja)
Other versions
JP3473890B2 (en
Inventor
Junichi Kojima
潤一 小島
Jinichiro Kato
仁一郎 加藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Asahi Chemical Industry Co Ltd
Original Assignee
Asahi Chemical Industry Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Asahi Chemical Industry Co Ltd filed Critical Asahi Chemical Industry Co Ltd
Priority to JP35364897A priority Critical patent/JP3473890B2/en
Publication of JPH11189923A publication Critical patent/JPH11189923A/en
Application granted granted Critical
Publication of JP3473890B2 publication Critical patent/JP3473890B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Multicomponent Fibers (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain a polyester conjugate fiber capable of giving a cloth which can express adequate degree of crimp shrinkage by a heat treatment, and has soft and bulky feeling while keeping smooth surface property, and useful for the usage of an outer wear an inner, a sportswear or the like free from stretching feeling on elbows and knees when they are bent and having good wearability. SOLUTION: In side-by-side polyester conjugate fiber consisting of a first component and a second component, the first component is a polytrimethylene terephthalate polymer having the intrinsic viscosity [η] of 0.4-1.0, and the second component is a polyester polymer whose melt viscosity is higher than that of the first component by 200-500 poise. The both components are closely adhered to each other over the whole length of the fiber, and are arranged in a parallel or eccentric state.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、ポリエステル系複
合繊維に関する。さらに詳しくは、熱処理により適度な
捲縮と収縮を発現する染色性の良好なサイドバイサイド
型のポリエステル系複合繊維に関する。
[0001] The present invention relates to a polyester-based conjugate fiber. More specifically, the present invention relates to a side-by-side polyester-based composite fiber having good dyeability, which exhibits appropriate crimp and shrinkage by heat treatment.

【0002】[0002]

【従来の技術】従来、2種類の収縮特性または溶融粘度
の異なった重合体を繊維軸長さ方向にわたって互いに密
着させ、偏心または並列的に複合紡糸したのち、延伸
し、弛緩状態で熱処理することによって捲縮糸を得る技
術は公知である。特に、ポリエステル系複合繊維は、力
学的な性質、熱安定性、ウォッシュアンドウエアー性等
に優れているうえに、その繊維自身が捲縮性を有してい
るため、仮撚加工など捲縮を与えるための後加工が必要
ないなどの利点がある。
2. Description of the Related Art Conventionally, two kinds of polymers having different shrinkage characteristics or different melt viscosities are closely adhered to each other over the length of a fiber axis, eccentrically or in parallel composite spinning, and then stretched and heat-treated in a relaxed state. The technique of obtaining a crimped yarn by the above method is known. In particular, polyester-based composite fibers are excellent in mechanical properties, thermal stability, wash and wear properties, etc., and since the fibers themselves have crimping properties, crimping such as false twisting is not possible. There are advantages such as no need for post-processing to give.

【0003】上記のようなポリエステル系複合繊維とし
ては、ポリエチレンテレフタレート重合体の重合度に差
があるものからなる複合繊維、あるいはホモのポリエチ
レンテレフタレートと共重合ポリエステルとの複合繊維
などが提案されてきた。これらの複合紡糸による捲縮繊
維は、糸の状態、または織物として捲縮発現熱処理を行
い、嵩高糸または平滑な表面の嵩高織物として利用する
ためには、適切な捲縮数と共に適度な捲縮発現力、捲縮
保持率を備えなければならない。即ち、延伸糸に捲縮発
現処理を施して嵩高糸とし、編織物とする場合には製
編、製織工程で張力を受けながらも十分に保ち得る良好
な捲縮安定性を持つ必要があり、延伸糸を織物とした
後、捲縮発現処理して嵩高織物とする場合は、組織内で
糸が受ける張力に対して十分に捲縮発現し得る良好な捲
縮発現力が必要である。
[0003] As the above-mentioned polyester-based composite fiber, a composite fiber comprising a polyethylene terephthalate polymer having a different degree of polymerization or a composite fiber of homopolyethylene terephthalate and a copolymerized polyester has been proposed. . These composite spun crimped fibers are subjected to crimp development heat treatment as a yarn state or a woven fabric, and to be used as a bulky yarn or a bulky woven fabric having a smooth surface, an appropriate number of crimps together with an appropriate number of crimps are used. It must have a developing ability and a crimp retention rate. That is, it is necessary to have a good crimp stability that can be sufficiently maintained while receiving tension in the knitting and weaving process when a drawn yarn is subjected to a crimp development treatment to give a bulky yarn and a knitted fabric. In the case where the drawn yarn is formed into a woven fabric and then subjected to a crimp development treatment to form a bulky woven fabric, it is necessary to have a good crimp developing force capable of sufficiently developing the crimp with respect to the tension applied to the yarn in the tissue.

【0004】しかしながら、このような従来の複合繊維
を使った布帛では、大きな欠点が見られた。その一つ
は、嵩高性のものは得られるがストレッチ性は小さく、
弾性回復性も劣る場合、また、今一つは、逆にストレッ
チ性は大きいがシボ状の斑が発生し平滑性が失われる場
合である。さらに、剛性が高すぎるため風合いが硬くな
る事等である。
[0004] However, such a fabric using the conventional conjugate fiber has a serious drawback. One of them is that bulky ones are obtained but stretchability is small,
Another is the case where elastic recovery is poor, and the other is the case where the stretchability is large but grain-like spots are generated and the smoothness is lost. Further, the texture becomes hard because the rigidity is too high.

【0005】これらの欠点を補う複合繊維として、たと
えば、特公昭43−19108号公報に開示されている
ポリトリメチレンテレフタレートとポリエチレンテレフ
タレートの組み合わせによるサイドバイサイド型複合繊
維がある。この複合繊維は、高収縮性成分として高分子
量のポリトリメチレンテレフタレートを使用しているた
め繊維の剛性が高く、堅い風合いになってしまう。ま
た、固有粘度の高いポリトリメチレンテレフタレートを
得るためにを固相重合により分子量を増大させる方法を
示しているが、これは、原料コストが非常に高くなって
しまう点で経済的に問題である。
As a conjugate fiber for compensating for these drawbacks, there is, for example, a side-by-side conjugate fiber comprising a combination of polytrimethylene terephthalate and polyethylene terephthalate disclosed in JP-B-43-19108. Since this composite fiber uses polytrimethylene terephthalate having a high molecular weight as a high shrinkage component, the fiber has a high rigidity and a hard texture. Also, a method of increasing the molecular weight by solid-phase polymerization to obtain polytrimethylene terephthalate having a high intrinsic viscosity is shown, but this is economically problematic in that the raw material cost becomes extremely high. .

【0006】特開昭52−128420号公報に述べら
れている非弾性ポリエステルであるポリブチレンテレフ
タレートと弾性ブロックポリエーテルエステルの組み合
わせによるサイドバイサイド型の複合繊維がある。しか
しながら、この組み合わせにより得られる布帛は、分散
染料で染色した時のドライクリーニング堅牢度が著しく
悪いため、アウター、裏地のような用途には使用できな
い。
[0006] There is a side-by-side type composite fiber made of a combination of an elastic block polyetherester and polybutylene terephthalate, which is an inelastic polyester described in JP-A-52-128420. However, the fabric obtained by this combination has extremely poor dry cleaning fastness when dyed with a disperse dye, and cannot be used for applications such as outerwear and lining.

【0007】[0007]

【発明が解決しようとする課題】本発明の課題は、服地
にしたときに平滑な表面性を保ちながらソフトでふくら
み感のある風合いを示し、かつその布帛が10%程度の
ストレッチを発現することにより非常に着心地が良くな
り、さらに、分散染料に効率よく染着し、ドライクリー
ニング堅牢度も実用の範囲内である、衣料に最適なポリ
エステル系複合繊維を提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to provide a soft and swelling texture while maintaining a smooth surface when garmented, and that the fabric exhibits a stretch of about 10%. Accordingly, it is an object of the present invention to provide a polyester-based composite fiber most suitable for apparel, which is extremely comfortable to wear, efficiently dyes a disperse dye, and has a dry cleaning fastness within a practical range.

【0008】[0008]

【課題を解決するための手段】本発明者らは、上記の従
来の問題点を解決するため種々検討した結果、熱処理に
より適切な捲縮・収縮を発現する複合繊維を得るために
は、複合ポリマーの1つの成分として弾性特性を有する
ポリマーを使用する事および適切な粘度のポリマーの組
み合わせを選ぶことが最も重要であることを突き止め、
本発明を完成させるに至った。
Means for Solving the Problems The present inventors have conducted various studies to solve the above-mentioned conventional problems. As a result, in order to obtain a conjugate fiber exhibiting appropriate crimping and shrinkage by heat treatment, the conjugate fiber has to be obtained. Ascertaining that it is most important to use a polymer with elastic properties as one component of the polymer and to select a combination of polymers of appropriate viscosity,
The present invention has been completed.

【0009】すなわち、本発明は、第一成分と第二成分
とのサイドバイサイド型の複合繊維において、上記第一
成分が極限粘度[η]0.4〜1であるポリトリメチレ
ンテレフタレートポリマーであり、上記第二成分が第一
成分の溶融粘度に対し200〜500ポイズ高い粘度の
ポリエステルポリマーであり、かつ第一成分と第二成分
とが繊維全長にわたって互いに密着し、配置されている
ことを特徴とするポリエステル系複合繊維、である。
That is, the present invention is a polytrimethylene terephthalate polymer wherein the first component has an intrinsic viscosity [η] of 0.4 to 1, in a side-by-side type composite fiber of a first component and a second component. The second component is a polyester polymer having a viscosity of 200 to 500 poise higher than the melt viscosity of the first component, and the first component and the second component are in close contact with each other over the entire length of the fiber, and are arranged. Polyester composite fiber.

【0010】本発明に用いられるポリトリメチレンテレ
フタレートポリマーは、弾性率Q(g/d)と弾性回復
率R(%)が、式(1)に示される範囲の特性を有し、
ソフト性と弾性特性とを併せ持つポリエステル系繊維が
得られること、また、染色性や染色堅牢性が良好である
ことが知られている。 0.2≦Q/R≦0.45 …(1) このような弾性的特性を有するポリトリメチレンテレフ
タレートポリマーを複合ポリマーの一成分として使用す
ることにより、従来の二つの成分間の大きな収縮率差を
利用して捲縮・収縮を得るサイドバイサイド糸に比較し
て、捲縮数・収縮率は劣るものの、織物などの拘束下で
も布帛に10%程度のストレッチ性を付与することがで
きることを見出した。
The polytrimethylene terephthalate polymer used in the present invention has an elastic modulus Q (g / d) and an elastic recovery rate R (%) in the range shown by the formula (1).
It is known that a polyester fiber having both softness and elasticity can be obtained, and that the dyeability and the color fastness are good. 0.2 ≦ Q / R ≦ 0.45 (1) By using the polytrimethylene terephthalate polymer having such elastic properties as one component of the composite polymer, the conventional large shrinkage ratio between the two components is obtained. Compared to a side-by-side yarn that obtains crimp / shrinkage by utilizing the difference, it has been found that although the number of crimps and shrinkage are inferior, it is possible to impart a stretch property of about 10% to a cloth even under the constraint of a woven fabric or the like. Was.

【0011】本発明で用いられるポリトリメチレンテレ
フタレートは、実質的にテレフタル酸と1、3−プロパ
ンジオールを重縮合せしめて得られるポリトリメチレン
テレフタレートである。本発明において実質的にとは、
ポリトリメチレンテレフタレートホモポリマーであって
も以下に示すポリトリメチレンテレフタレートコポリマ
ーであってもよいことを示す。すなわち、本発明の効果
を損なわない範囲で、イソフタル酸、コハク酸、アジピ
ン酸、2,6−ナフタレンジカルボン酸、5−スルホイ
ソフタル酸テトラブチルポスホニウム塩等の酸成分や、
1,4−ブタンジオール、1,6−ヘキサンジオール、
シクロヘキサンジメタノール等のグリコール成分、ε−
カプロラクトン、4−ヒドロキシ安息香酸、ポリオキシ
エチレングリコール、ポリテトラメチレングリコール等
が10重量%未満共重合されていてもよい。
The polytrimethylene terephthalate used in the present invention is a polytrimethylene terephthalate obtained by substantially polycondensing terephthalic acid with 1,3-propanediol. In the present invention, substantially means
It indicates that the polymer may be a polytrimethylene terephthalate homopolymer or a polytrimethylene terephthalate copolymer shown below. That is, as long as the effects of the present invention are not impaired, acid components such as isophthalic acid, succinic acid, adipic acid, 2,6-naphthalenedicarboxylic acid, and 5-sulfoisophthalic acid tetrabutyl phosphonium salt;
1,4-butanediol, 1,6-hexanediol,
Glycol components such as cyclohexanedimethanol, ε-
Less than 10% by weight of caprolactone, 4-hydroxybenzoic acid, polyoxyethylene glycol, polytetramethylene glycol and the like may be copolymerized.

【0012】また、必要に応じて、各種の添加剤、例え
ば、艶消し剤、熱安定剤、消泡剤、整色剤、難燃剤、酸
化防止剤、紫外線吸収剤、赤外線吸収剤、結晶核剤、蛍
光増白剤などを共重合、または混合してもよい。本発明
に用いるポリトリメチレンテレフタレートポリマーは、
極限粘度[η]0.4〜1.0であり、好ましくは0.
5〜0.8である。さらに好ましくは0.6〜0.7で
ある。この範囲では、ポリマーの溶融粘度が100〜3
00ポイズとなり、低粘度のポリトリメチレンテレフタ
レートが、高粘度の第二成分を包み込む形態となり、適
度な捲縮と収縮を与えることができる。極限粘度が0.
4未満の場合は、ポリマーの分子量が低すぎるため強度
発現が困難となり、逆に、極限粘度が1.0を越える場
合は、流動性が低いため低粘度のポリトリメチレンテレ
フタレートに変形が起こらず捲縮、収縮発現力が弱く、
好ましくない。
If necessary, various additives such as a matting agent, a heat stabilizer, an antifoaming agent, a tinting agent, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, and a crystal nucleus. Agents, optical brighteners and the like may be copolymerized or mixed. Polytrimethylene terephthalate polymer used in the present invention,
Intrinsic viscosity [η] is 0.4 to 1.0, preferably 0.1.
5 to 0.8. More preferably, it is 0.6 to 0.7. In this range, the melt viscosity of the polymer is 100 to 3
Thus, the low viscosity polytrimethylene terephthalate wraps around the high viscosity second component, and can provide appropriate crimp and shrinkage. The intrinsic viscosity is 0.
If it is less than 4, the molecular weight of the polymer is too low, and it becomes difficult to develop strength. Conversely, if the intrinsic viscosity is more than 1.0, the low viscosity polytrimethylene terephthalate does not deform due to low fluidity. The crimp and shrinkage expression power is weak,
Not preferred.

【0013】表面の平滑性を保ちながらソフトでふくら
み感のある布帛を得るためには、粘度差により発現する
適度な捲縮・収縮が必要である。第一成分と第二成分と
の粘度差は、200〜500ポイズである。好ましくは
250〜450ポイズ、さらに好ましくは300〜40
0ポイズであり、適度な大きさの捲縮と収縮が得られ
る。粘度差200ポイズ以下では捲縮の発現が見られ
ず、500ポイズ以上では、吐出孔直下において、溶融
粘度の異なる二つの成分を複合紡糸する場合、吐出孔直
下において糸条が溶融粘度の大きい方へ偏曲するニーイ
ング現象により操業性に問題が生じるので好ましくな
い。
In order to obtain a soft and swelling fabric while maintaining the smoothness of the surface, it is necessary to have an appropriate crimping / shrinking developed due to a difference in viscosity. The viscosity difference between the first component and the second component is 200 to 500 poise. Preferably 250-450 poise, more preferably 300-40
It has 0 poise, and crimps and shrinks of an appropriate size can be obtained. At a viscosity difference of 200 poises or less, no crimping is observed. At a viscosity difference of 500 poises or more, when two components having different melt viscosities are compositely spun immediately below the discharge hole, the yarn having a higher melt viscosity just below the discharge hole is used. It is not preferable because the operability is problematic due to the kneeing phenomenon that is deflected.

【0014】本発明での第二成分として用いられるポリ
エステルポリマーとしては、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、ポリトリメチレンテ
レフタレート、ポリテトラメチレンテレフタレートなど
のポリエステル系重合体及びこれらの共重合体からなる
もの、また、これらの重合体及びこれらの共重合体から
なるものが挙げられる。これらの重合体または共重合体
に制電剤、難燃剤、耐熱剤、耐候剤、酸化チタン等の添
加剤を加えることは何ら差し支えない。
Examples of the polyester polymer used as the second component in the present invention include polyester polymers such as polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, polytetramethylene terephthalate, and copolymers thereof. Moreover, what consists of these polymers and these copolymers is mentioned. Addition of additives such as an antistatic agent, a flame retardant, a heat resistant agent, a weathering agent, and titanium oxide to these polymers or copolymers can be carried out without any problem.

【0015】本発明のポリエステル系複合繊維は、第一
成分と第二成分のポリマーが繊維全長にわたって互いに
密着し、配置されていることが必要である。二つの成分
の配置のされ方は特に限定されないが、低粘度のポリト
リメチレンテレフタレートポリマーが、高粘度の第二成
分ポリエステルポリマーを包み込む形態をとるのが好ま
しい。この場合、繊維の断面を見ると、低粘度のポリト
リメチレンテレフタレートポリマーが三日月状に、高粘
度の第二成分ポリエステルポリマーを包み込んだ形態を
とっている。このように二つの成分が配置されているこ
とにより、繊維に適度な捲縮と収縮を与えることができ
る。
In the polyester composite fiber of the present invention, it is necessary that the polymer of the first component and the polymer of the second component are closely adhered to each other over the entire length of the fiber. The arrangement of the two components is not particularly limited, but it is preferable that the low-viscosity polytrimethylene terephthalate polymer takes a form enclosing the high-viscosity second component polyester polymer. In this case, when the cross section of the fiber is viewed, the low-viscosity polytrimethylene terephthalate polymer is in a crescent shape and wraps around the high-viscosity second component polyester polymer. By arranging the two components in this manner, the fiber can be given an appropriate crimp and shrinkage.

【0016】本発明のポリエステル系複合繊維は、二種
類の極限粘度の違うポリエステル系成分が繊維の全長に
わたって互いに密着し、配置される様に共通の紡糸孔よ
り押し出し得るような、従来公知の複合紡糸方法により
紡糸し製造することができる。また二種類のポリエステ
ルを等容量比で押し出してもよく、各成分の比を適当に
変えることもできる。複合紡糸する両成分の比率は、3
0〜70/70〜30の範囲が好適である。更に好まし
くは40〜60/60〜40である。ポリトリメチレン
テレフタレート成分が70%以上の場合は、捲縮性は向
上するが、複合繊維としての強度が低下する。一方、3
0%未満の場合は、捲縮性が不足する。
The polyester conjugate fiber of the present invention has a conventionally known conjugated property, in which two kinds of polyester components having different intrinsic viscosities can be extruded from a common spinning hole so that they are in close contact with each other over the entire length of the fiber and are arranged. It can be manufactured by spinning by a spinning method. Further, two types of polyesters may be extruded at an equal volume ratio, and the ratio of each component may be appropriately changed. The ratio of both components for composite spinning is 3
The range of 0 to 70/70 to 30 is preferred. More preferably, it is 40-60 / 60-40. When the polytrimethylene terephthalate component is 70% or more, the crimpability is improved, but the strength as a conjugate fiber is reduced. Meanwhile, 3
If it is less than 0%, the crimpability is insufficient.

【0017】溶融粘度の異なる二つの成分を複合紡糸す
る場合、吐出孔直下において糸条が溶融粘度の大きい方
へ偏曲するニーイング現象が生じ、これが糸質を劣化さ
せるのみならず、紡糸性を妨げ、ときには紡糸口金板に
粘着して生産を不可能にすることがある。ニーイングを
防止する方法として紡糸口金孔の細工による方法がある
が、例えば英国特許第965729号明細書に示されて
いるように、ニーイングする方向と逆の方向に、予め、
口金孔を曲げておいて口金面からポリマーを垂直に吐出
する方法が、本発明のポリエステル系複合繊維の製造に
おいても有効である。
In the case of composite spinning of two components having different melt viscosities, a kneading phenomenon occurs in which the yarn is deflected to a portion having a higher melt viscosity immediately below the discharge hole, which not only deteriorates the yarn quality but also reduces the spinnability. In some cases, it can interfere with the production and make it impossible to adhere to the spinneret. As a method of preventing kneeling, there is a method of working a spinneret. However, as shown in, for example, British Patent No. 965729, in a direction opposite to the kneeing direction,
A method in which the polymer is vertically discharged from the surface of the die by bending the die hole is also effective in the production of the polyester-based composite fiber of the present invention.

【0018】本発明のポリエステル系複合繊維は、加重
下での熱処理でも適度な捲縮と収縮を発現するものとな
り、通常の織編物で平滑な表面性を保ちながらソフトで
ふくらみ感のある風合いを示す布帛が得られ、かつその
布帛が10%程度のストレッチを発現する。また、通常
のポリエステル分散染料を用いて染色することができ
る。本発明のポリエステル系複合繊維を用いた布帛は、
肘、膝を曲げた時や腕を伸ばした時の突っ張り感がなく
なり、非常に着心地のよい衣料となる。従って、アウタ
ー、裏地、スポーツ等の用途に極めて有用である。
The polyester-based conjugate fiber of the present invention develops a suitable crimp and shrinkage even when heat-treated under a load, and has a soft and swelling texture while maintaining a smooth surface with a normal woven or knitted fabric. As a result, the obtained fabric exhibits a stretch of about 10%. In addition, dyeing can be performed using a general polyester disperse dye. Fabric using the polyester-based composite fiber of the present invention,
The feeling of tension when the elbows and knees are bent or the arms are extended is eliminated, making the clothing very comfortable. Therefore, it is extremely useful for uses such as outerwear, lining, and sports.

【0019】[0019]

【発明の実施の形態】以下、実施例を挙げて本発明をよ
り詳細に説明する。なお、実施例中の主な測定値は以下
の方法で測定した。 (1)極限粘度 この極限粘度[η]は次の定義式に基づいて求められる
値である。
DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in more detail by way of examples. In addition, the main measurement value in an Example was measured by the following method. (1) Intrinsic Viscosity This intrinsic viscosity [η] is a value determined based on the following definition formula.

【0020】[0020]

【数1】 (Equation 1)

【0021】定義式のηrは純度98%以上のo−クロ
ロフェノールで溶解したポリエステルポリマーの希釈溶
液の35℃での粘度を、同一温度で測定した上記溶剤自
体の粘度で割った値であり、相対粘度と定義されている
ものである。またCは、上記溶液100ml中のグラム
単位による溶質重量値である。 (2)溶融粘度 キャピログラフ〔東洋精機(株)製、キャピログラフ1
B〕の装置を使用し290℃、剪断速度7780cm−
1で測定したときの値である。 (3)破断伸度、弾性率 島津製作所製オートグラフ引張試験機を用い、糸長20
0mm、引張速度200mm/分、N=5で、破断伸
度、初期弾性率を測定した。 (4)捲縮数 130℃でフリーの乾熱処理した長さ約20cmの糸を
2mg/dの張力下におき、糸の1インチあたりの捲縮
数を数える。 (5)乾熱収縮率 1m長の10回巻き綛を作成し、一定重量の錘を下げて
初期長L0を測定する。錘の水準は、5mg/d、50
mg/dとする。加重状態で130℃×30分乾熱処理
を実施する。その後、標準状態で一昼夜放置した後、加
重状態で長さLを測定し、収縮率を算出した。
Ηr in the definition formula is a value obtained by dividing the viscosity at 35 ° C. of a diluted solution of a polyester polymer dissolved in o-chlorophenol having a purity of 98% or more by the viscosity of the solvent itself measured at the same temperature. It is defined as relative viscosity. C is the solute weight value in grams in 100 ml of the solution. (2) Melt viscosity Capillograph [Capillograph 1 manufactured by Toyo Seiki Co., Ltd.
290 ° C., shear rate 7780 cm −
This is the value measured at 1. (3) Elongation at break, modulus of elasticity Using an autograph tensile tester manufactured by Shimadzu Corporation, yarn length 20
The elongation at break and the initial elastic modulus were measured at 0 mm, a tensile speed of 200 mm / min, and N = 5. (4) Number of crimps A yarn having a length of about 20 cm, which has been subjected to free dry heat treatment at 130 ° C., is placed under a tension of 2 mg / d, and the number of crimps per inch of the yarn is counted. (5) Dry Heat Shrinkage A 10-fold skein with a length of 1 m is prepared, and the initial length L0 is measured by lowering the weight of a fixed weight. The weight level is 5 mg / d, 50
mg / d. A dry heat treatment is performed at 130 ° C. for 30 minutes in a weighted state. Then, after leaving all day and night in the standard state, the length L was measured in the weighted state, and the contraction rate was calculated.

【0022】 乾熱収縮率=(L0−L)/L0 ×100(%) (6)染料の吸尽率 試料はポリエステル複合繊維の一口編地を用い、スコア
ロール400を2g/リットルで含む温水を用いて70
℃、20分間精錬処理し、タンブラー乾燥機で乾燥さ
せ、次いでピンテンターを用いて、180℃、30秒の
熱セットを行ったものを使用した。吸尽率は、40℃か
ら95℃に昇温後、さらにそのまま1時間保持した後の
吸尽率で評価した。染料は、カヤロンポリエステルブル
ー3RSF(日本化薬(株)製)を使用し、6%ow
f、浴比1:50で染色した。分散剤はニッカサンソル
ト7000(日華化学(株)製)を0.5g/リットル
使用し、酢酸0.25ミリリットル/リットルと酢酸ナ
トリウム1g/リットルを加え、pHを5に調製した。
Dry heat shrinkage = (L0−L) / L0 × 100 (%) (6) Exhaust rate of dye The sample is a single piece knitted fabric of polyester composite fiber, and hot water containing score roll 400 at 2 g / liter. 70 using
After refining at 20 ° C. for 20 minutes and drying with a tumbler dryer, a heat set at 180 ° C. for 30 seconds using a pin tenter was used. The exhaustion rate was evaluated based on the exhaustion rate after the temperature was raised from 40 ° C. to 95 ° C. and further kept for 1 hour. The dye used was Kayaron Polyester Blue 3RSF (produced by Nippon Kayaku Co., Ltd.), and was 6% ow.
f, dyeing at a bath ratio of 1:50. As a dispersant, Nikka Sun Salt 7000 (manufactured by Nikka Chemical Co., Ltd.) was used in an amount of 0.5 g / liter, and the pH was adjusted to 5 by adding 0.25 ml / liter of acetic acid and 1 g / liter of sodium acetate.

【0023】吸尽率は、染料原液の吸光度x、染色後の
染液の吸光度yを分光光度計から求め、以下の式に代入
して求めた。吸光度は当該染料の最大吸収波長である5
80nmでの値を採用した。 吸尽率=(x−y)/x×100 (%) (7)DC染色堅牢度 上記(6)の方法で染色した一口編地500mgを用い
てDC染色堅牢度の評価を行った。ドライクリーニング
堅牢性はJIS−L−0860に準じて行った。
The exhaustion rate was determined by determining the absorbance x of the stock dye solution and the absorbance y of the dye solution after dyeing using a spectrophotometer and substituting them into the following equation. The absorbance is 5 which is the maximum absorption wavelength of the dye.
The value at 80 nm was adopted. Exhaustion rate = (xy) / x × 100 (%) (7) DC dyeing fastness DC dyeing fastness was evaluated using 500 mg of one-piece knitted fabric dyed by the above method (6). Dry cleaning fastness was measured in accordance with JIS-L-0860.

【0024】(8)布帛緯伸び カトーテック(株)製のKES−FB1を用いて、20
cm×20cmの織物を引張速度が0.2mm/秒で緯
方向に伸長し、500g/cmの応力下での緯伸びS
(%)を次式によって求めた。 S=(M−N/20)×100 M:500g/cmの応力下で伸びた長さ(cm) N:織物の元の長さ=20cm
(8) Fabric Weft Elongation Using KES-FB1 manufactured by Kato Tech Co., Ltd.
cm × 20 cm woven fabric is stretched in the weft direction at a tensile speed of 0.2 mm / sec, and the weft elongation S under a stress of 500 g / cm.
(%) Was determined by the following equation. S = (M−N / 20) × 100 M: Length (cm) extended under stress of 500 g / cm N: Original length of woven fabric = 20 cm

【0025】[0025]

【実施例1】テレフタル酸ジメチルと1,3−プロパン
ジオールを1:2のモル比で仕込み、テレフタル酸ジメ
チルの0.1重量%に相当するチタンテトラブトキシド
を加え、徐々に昇温し240℃でエステル交換反応を完
結させた。得られたエステル交換物にチタンテトラブト
キシドを更に理論ポリマー量の0.1重量%添加し、2
70℃で3時間反応させた。得られたポリマーの極限粘
度は0.7であった。このポリマーを水冷後、チップ状
にカットしポリトリメチレンテレフタレートのポリマー
(A)を得た。このポリマーの290℃における溶融粘
度は280ポイズであった。
Example 1 Dimethyl terephthalate and 1,3-propanediol were charged at a molar ratio of 1: 2, and titanium tetrabutoxide corresponding to 0.1% by weight of dimethyl terephthalate was added. To complete the transesterification reaction. Titanium tetrabutoxide was further added to the obtained transesterified product at 0.1% by weight of the theoretical polymer amount,
The reaction was performed at 70 ° C. for 3 hours. The intrinsic viscosity of the obtained polymer was 0.7. After cooling with water, the polymer was cut into chips to obtain polytrimethylene terephthalate polymer (A). The melt viscosity of the polymer at 290 ° C. was 280 poise.

【0026】これとは別に、公知の方法でポリエチレン
テレフタレートのポリマー(B)を得た。このポリマー
の極限粘度は0.5で、290℃における溶融粘度は、
630ポイズであった。ポリマー(A)とポリマー
(B)をそれぞれ複合紡糸機に供給し、同一の口金より
量比1:1、温度290℃で紡糸して、並列関係に密着
している256d/24fの未延伸糸を得た。この未延
伸糸を80℃に延伸しポリエステル系複合繊維の糸条
(原糸)を得た。得られたポリエステル系複合繊維の糸
条の物性および乾熱処理糸の捲縮・収縮特性を表1に示
す。また、染色特性を表1に示す。
Separately, a polyethylene terephthalate polymer (B) was obtained by a known method. The intrinsic viscosity of this polymer is 0.5, and the melt viscosity at 290 ° C. is
It was 630 poise. The polymer (A) and the polymer (B) are supplied to the composite spinning machine, respectively, and spun from the same die at a ratio of 1: 1, at a temperature of 290 ° C., and a 256d / 24f undrawn yarn closely adhered in a parallel relationship. I got This undrawn yarn was drawn at 80 ° C. to obtain a yarn (original yarn) of a polyester-based composite fiber. Table 1 shows the physical properties of the yarn of the obtained polyester-based composite fiber and the crimping / shrinking characteristics of the dry heat-treated yarn. Table 1 shows the dyeing characteristics.

【0027】得られたポリエステル系複合繊維の糸条を
用いてタテ密度100本/インチ、ヨコ密度81本/イ
ンチ、目付50g/m2、生機幅131.5cmの織物
を製織した。得られた織物をピンテンターにより、19
0℃×30秒の条件で生機幅に対し15%の幅入れを行
った。次に2g/リットルの炭酸ソーダと2g/リット
ルのスコアロール(花王(株)製)を投入した液で、液
流染色機によって130℃×10分の精錬を行った。こ
の布帛の物性測定結果を、表2示す。
A woven fabric having a warp density of 100 yarns / inch, a weft density of 81 yarns / inch, a basis weight of 50 g / m2 and a greige width of 131.5 cm was woven using the obtained polyester composite fiber yarn. The obtained woven fabric is 19
Under the condition of 0 ° C. × 30 seconds, a width of 15% with respect to the width of the greige was performed. Next, refining was performed at 130 ° C. for 10 minutes by a liquid jet dyeing machine using a liquid charged with 2 g / liter of sodium carbonate and 2 g / liter of score roll (manufactured by Kao Corporation). Table 2 shows the measurement results of the physical properties of the cloth.

【0028】[0028]

【比較例1】実施例1と同様に、通常の方法で重合した
溶融粘度735ポイズのポリエチレンテレフタレート
(C)と溶融粘度220ポイズのポリエチレンテレフタ
レート(D)を複合紡糸し未延伸糸を得た。これを80
℃のホットプレート上で3.2倍に延伸し80d/24
fの延伸糸(原糸)を得た。物性を表1に示す。延伸糸
では、26山/inchの捲縮が見られたが、荷重下で
の乾熱処理により捲縮が無くなってしまった。さらに、
荷重下での収縮率は小さかった。実施例1と同様に布帛
を製織し、熱セット、精錬処理を行った結果を表2に示
す。緯伸びは小さくストレッチ性は見られなかった。
Comparative Example 1 In the same manner as in Example 1, an undrawn yarn was obtained by composite spinning of polyethylene terephthalate (C) having a melt viscosity of 735 poise and polyethylene terephthalate (D) having a melt viscosity of 220 poise, which were polymerized by a usual method. This is 80
Stretched 3.2 times on a hot plate at 80 ° C and 80d / 24
Thus, a drawn yarn (original yarn) of f was obtained. Table 1 shows the physical properties. In the drawn yarn, a crimp of 26 peaks / inch was observed, but the crimp disappeared by the dry heat treatment under the load. further,
Shrinkage under load was small. Table 2 shows the results of weaving the fabric in the same manner as in Example 1, and performing heat setting and refining. Weft elongation was small and stretchability was not seen.

【0029】[0029]

【比較例2】従来の方法で固相重合し極限粘度を1.3
まで増大させた、ポリトリメチレンテレフタレート
(E)をつくった。このポリマーの溶融粘度は600ポ
イズであった。また、比較例1と同様に従来の方法で重
合した溶融粘度630ポイズのポリエチレンテレフタレ
ート(F)を作った。この2つのポリマーを実施例1と
同様に複合紡糸し、ホットプレート80℃、延伸倍率
3.5倍で延伸し、80d/24fの延伸糸(原糸)を
得た。物性を表1に示す。延伸糸では全く捲縮がなかっ
たが、130℃乾熱処理により捲縮が発現した。しか
し、実施例1に比べて弾性率が高い。実施例1と同様に
布帛を製織し評価した結果を表2に示す。良好な緯伸び
性が見られるが、しぼ状の斑が表面に見られ、また風合
いも堅い。
Comparative Example 2 Solid-state polymerization was performed by a conventional method, and the limiting viscosity was 1.3.
A polytrimethylene terephthalate (E) was produced, which was increased to The melt viscosity of this polymer was 600 poise. Further, polyethylene terephthalate (F) having a melt viscosity of 630 poise polymerized by a conventional method in the same manner as in Comparative Example 1 was produced. The two polymers were subjected to composite spinning in the same manner as in Example 1, and stretched at a hot plate temperature of 80 ° C. and a draw ratio of 3.5 to obtain a 80d / 24f drawn yarn (original yarn). Table 1 shows the physical properties. The drawn yarn did not crimp at all, but crimped by dry heat treatment at 130 ° C. However, the elastic modulus is higher than that of Example 1. Table 2 shows the results of weaving and evaluating the fabric in the same manner as in Example 1. Good weft elongation is observed, but grain-like spots are observed on the surface and the texture is firm.

【0030】[0030]

【表1】 [Table 1]

【0031】[0031]

【表2】 [Table 2]

【0032】[0032]

【発明の効果】本発明のポリエステル系複合繊維は、熱
処理により適度な捲縮と収縮を発現する結果、平滑な表
面性を保ちながらソフトでふくらみ感のある風合いを示
す布帛が得られ、かつその布帛が10%程度のストレッ
チを発現するため、肘、膝を曲げた時や腕を伸ばした時
の突っ張り感がなくなり、非常に着心地のよい衣料が得
られる。さらに、分散染料に効率よく染着し、ドライク
リーニング堅牢度も実用の範囲内である。
The polyester-based conjugate fiber of the present invention exhibits moderate crimping and shrinkage by heat treatment, and as a result, a fabric having a soft and swelling feel while maintaining a smooth surface property can be obtained. Since the fabric exhibits a stretch of about 10%, the feeling of tension when the elbows and knees are bent or the arms are extended is eliminated, and a very comfortable garment can be obtained. Furthermore, the dye is efficiently dyed on the disperse dye, and the fastness to dry cleaning is within the practical range.

【0033】従って、アウター、裏地、スポーツ等の用
途に極めて有用である。
Therefore, it is extremely useful for uses such as outerwear, lining, and sports.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 第一成分と第二成分とのサイドバイサイ
ド型の複合繊維において、上記第一成分が極限粘度
[η]0.4〜1であるポリトリメチレンテレフタレー
トポリマーであり、上記第二成分が第一成分の溶融粘度
に対し200〜500ポイズ高い粘度のポリエステルポ
リマーであり、かつ第一成分と第二成分とが繊維全長に
わたって互いに密着し、配置されていることを特徴とす
るポリエステル系複合繊維。
1. A side-by-side conjugate fiber comprising a first component and a second component, wherein the first component is a polytrimethylene terephthalate polymer having an intrinsic viscosity [η] of 0.4 to 1, and Is a polyester polymer having a viscosity of 200 to 500 poise higher than the melt viscosity of the first component, and wherein the first component and the second component are in close contact with each other over the entire length of the fiber and are arranged. fiber.
JP35364897A 1997-12-22 1997-12-22 Polyester composite fiber Expired - Fee Related JP3473890B2 (en)

Priority Applications (1)

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Applications Claiming Priority (1)

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Publication Number Publication Date
JPH11189923A true JPH11189923A (en) 1999-07-13
JP3473890B2 JP3473890B2 (en) 2003-12-08

Family

ID=18432276

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JP2002266180A (en) * 2001-03-01 2002-09-18 Toray Ind Inc Long and short composite yarn and polyester-based stretchable woven fabric
US6689461B2 (en) 2001-04-17 2004-02-10 Asahi Kasei Kabushiki Kaisha False twisted yarn of polyester composite fiber and method for production thereof
US6673443B2 (en) 2001-09-18 2004-01-06 Asahi Kasei Kabushiki Kaisha Polyester conjugate fiber pirn and method for producing same
KR100462501B1 (en) * 2001-11-05 2004-12-17 주식회사 효성 Manufacture of elastic fabric
US6982118B2 (en) 2001-11-06 2006-01-03 Asahi Kasei Fibers Corporation Polyester type conjugate fiber package
US6824869B2 (en) 2001-11-06 2004-11-30 Asahi Kasei Fibers Corporation Polyester type conjugate fiber package
US6846560B2 (en) 2002-05-27 2005-01-25 Asahi Kasei Kabushiki Kaisha Conjugate fiber and method of producing same
WO2003100145A1 (en) * 2002-05-27 2003-12-04 Asahi Kasei Fibers Corporation Composite fiber and process for producing the same
CN1307331C (en) * 2002-05-27 2007-03-28 旭化成纤维株式会社 Composite fiber and process for producing the same
WO2004094706A1 (en) * 2003-04-24 2004-11-04 Huvis Corporation. Polyester conjugated yarn having high-self-crimping properties and method of manufacturing the same
CN100344809C (en) * 2003-04-24 2007-10-24 株式会社Huvis Polyester conjugated yarn having high-self-crimping properties and method of manufacturing the same
KR100804044B1 (en) 2005-09-26 2008-02-18 주식회사 코오롱 Polyester conjugated yarn with excellent shrinkage and process of preaparing for the same
JP2010196212A (en) * 2009-02-26 2010-09-09 Fujix Ltd Machine sewing thread

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