JPH0441713A - Production of superfine fiber composed of melt-anisotropic aromatic polyester - Google Patents

Production of superfine fiber composed of melt-anisotropic aromatic polyester

Info

Publication number
JPH0441713A
JPH0441713A JP14668290A JP14668290A JPH0441713A JP H0441713 A JPH0441713 A JP H0441713A JP 14668290 A JP14668290 A JP 14668290A JP 14668290 A JP14668290 A JP 14668290A JP H0441713 A JPH0441713 A JP H0441713A
Authority
JP
Japan
Prior art keywords
melt
aromatic polyester
polyester
anisotropic aromatic
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.)
Pending
Application number
JP14668290A
Other languages
Japanese (ja)
Inventor
Junyo Nakagawa
潤洋 中川
Toru Saneto
徹 実藤
Yukio Sugita
杉田 幸男
Yoshio Kishino
岸野 喜雄
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.)
Kuraray Co Ltd
Original Assignee
Kuraray 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 Kuraray Co Ltd filed Critical Kuraray Co Ltd
Priority to JP14668290A priority Critical patent/JPH0441713A/en
Publication of JPH0441713A publication Critical patent/JPH0441713A/en
Pending legal-status Critical Current

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  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Artificial Filaments (AREA)
  • Multicomponent Fibers (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

PURPOSE:To obtain the subject fiber excellent in strength by treating conjugate fiber in which a melt-anisotropic aromatic polyester is divided into plural segments with a readily alkali-decomposable polyester with an alkaline solution and then heat-treating the treated fiber. CONSTITUTION:Conjugate fiber in which a melt-anisotropic aromatic polyester is divided into >=2 segments with a readily alkali-decomposable polyester is spun and then treated with an alkaline solution to remove the readily alkali- decomposable polyester. The conjugate fiber is divided into respective segments, which are subsequently heat-treated at a temperature of >=(the melting point of the melt-anisotropic aromatic polyester constituting the aforementioned segments -80 deg.C) and <= the melting point thereof. Thereby, the strength is increased by >=30% to afford the objective fiber.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、溶融異方性芳香族ポリエステルからなる極細
繊維の製造方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing ultrafine fibers made of melt-anisotropic aromatic polyester.

〔従来の技術〕[Conventional technology]

溶融異方性を示す芳香族ポリエステルを紡糸して、優れ
た高強度・高弾性率の繊維が得られることは、特開昭5
4−77691号公報、籍開平1−92408号公報等
で公知であり、溶融異方性芳香族ポリエステルと他のポ
リマーを複合紡糸することFi特開平1−26719号
公報、%開平1−31835号公報、特開平2−806
40号公報等で公知である。
The fact that fibers with excellent high strength and high modulus of elasticity can be obtained by spinning aromatic polyester exhibiting melt anisotropy was disclosed in JP-A No. 5
4-77691, Japanese Patent Publication No. 1-92408, etc., and it is known that composite spinning of melt anisotropic aromatic polyester and other polymers is carried out in Japanese Patent Application Publication No. 1-26719, Japanese Patent Application Publication No. 1-31835. Publication, JP-A-2-806
It is publicly known from Publication No. 40 and the like.

また、ポリエチレンテレフタレートとアルカリ易分解性
ポリエステルとを複合紡糸して分割型複合繊維を得、該
繊維をアルカリ処理して極細繊維に分割することは%開
昭54−138620号公報等で公知である。
Furthermore, it is known in Japanese Patent Publication No. 138620/1983 to obtain splittable composite fibers by composite spinning polyethylene terephthalate and alkali-ready polyester, and to divide the fibers into ultrafine fibers by treating them with alkali. .

c本発明が解決しようとする課題〕 今日まで、溶融異方性ポリマーは紡糸ノズルを通過する
時の剪断力により著しく配向するため、いわゆる紡糸ド
ラフトをあまり大きくすることが出きす、加えて延伸を
することが実質的に不可能である。このため単繊維デニ
ールの小さいもの(%に、3デニール以下)を操業的に
安定に製造することは出来なかった。
c) Problems to be Solved by the Present Invention Until now, molten anisotropic polymers have been significantly oriented by the shear force when passing through a spinning nozzle, making it possible to make the so-called spinning draft too large, and in addition, it has been difficult to draw It is virtually impossible to do so. For this reason, single fibers with a small denier (3 denier or less) could not be stably produced operationally.

本発明は、細デニール、特に3デニール以下の高強度芳
香族ポリエステル*維を提供するにある。
The present invention provides a high-strength aromatic polyester* fiber having a fine denier, particularly 3 denier or less.

〔課題を解決するための手段〕[Means to solve the problem]

不発明に溶融異方性芳香族ポリエステルが、アルカリ易
分解性ボ1ノエステルによって、少なくとも2個のセグ
メントに分割された複合繊維を紡糸し、該複合繊維をア
ルカリ性溶液で処理し、アルカリ易分解性ポリエステル
を除去し、各セグメントに分割した後、各セグメントを
該セグメントを構成する溶融異方性芳香族ポリエステル
の(融点−80℃)以上融点以下の温度で熱処理し、強
度を30%以上増加させることを特徴とする溶融異方性
芳香族ポリエステル繊維からなる極細繊維の裏道方法で
ある。
Inventively, a conjugate fiber in which a melting anisotropic aromatic polyester is divided into at least two segments by an alkali easily decomposable bonoester is spun, and the conjugate fiber is treated with an alkaline solution to form an alkali easily decomposable polyester. After removing the polyester and dividing into each segment, each segment is heat treated at a temperature above (melting point -80°C) and below the melting point of the melting anisotropic aromatic polyester constituting the segment to increase the strength by 30% or more. This is a method for producing ultrafine fibers made of melt anisotropic aromatic polyester fibers.

不発明に言う溶融異方性芳香族ポリエステルの好ましい
例は、下記■〜■に示す反復成分の組合せからなるもの
である。
Preferred examples of the melt anisotropic aromatic polyester referred to in the invention are those consisting of a combination of repeating components shown in (1) to (4) below.

〔ここでXおよびYqHld、Br又1jCH3Tあり
、 Zは舎、−@−0−@−1Ωこ これらに、20重量%以下の他の共重合成分あるいは、
通常便用される添加剤(#i料、カーボン。
[Here, X and YqHld, Br or 1jCH3T are present, Z is sha, -@-0-@-1Ω, and other copolymer components of up to 20% by weight or,
Additives commonly used (#i additives, carbon.

熱安定剤、紫外線吸収剤、滑剤、螢光増白剤)等が含着
れていてもよい。
A heat stabilizer, an ultraviolet absorber, a lubricant, a fluorescent whitening agent, etc. may be included.

本発明の効果が最も顕著に発揮されるのに1本質的に下
記[:lL  [fflの反復111e、単位から成る
部分が801i%以上であるポリマー tP#に[(I
tの成分が3〜45係である芳香族ポリエステルであ本
発明に言う溶融異方性とは、溶融相において光学的異方
性を示すものである。このような特性/′i、公知の方
法、例えば、ホットステージにのせ九試料を窒素雰囲気
下で昇温加熱し、その透過光を観察することにより容易
に認足することが出来る0 溶融異方性を示す芳香族ポリエステルは、ノズルを通過
するときの剪断速度が103〜105secl  とな
ると著しい分子配向が生じ、延伸しなくとも優れ走置強
度・高弾性率の繊維となる。
In order for the effects of the present invention to be most conspicuous, 1 essentially the following [:lL[ffl repetition 111e, polymer tP# in which the portion consisting of units is 801i% or more [(I
The melt anisotropy referred to in the present invention in the aromatic polyester in which the component t is 3 to 45 indicates optical anisotropy in the melt phase. Such characteristics can be easily recognized by known methods such as heating a sample on a hot stage in a nitrogen atmosphere and observing the transmitted light.0 Melting anisotropy When the shearing rate of the aromatic polyester when passing through a nozzle is 10 3 to 10 5 sec, remarkable molecular orientation occurs in the aromatic polyester, which exhibits excellent running strength and high elastic modulus even without stretching.

本発明に言う剪断速度ンとは、円型ノズルの場合は次式
により求められる。
In the case of a circular nozzle, the shear rate referred to in the present invention is determined by the following equation.

但し、r:ノズル孔の半径(副) Q:単孔当りのポリマー吐出量(m/5ec)本発明に
言うアルカリ易分解性ポリエステルとは、ポリアルキレ
ングリコール共重合ポリエチレンテレフタレート、イン
フタレート共重合ポリエチレンテレフタレート、5−ソ
ジウムスルホイソフタレート共重合ポリエチレンテレフ
タレート等であり、これらは混合して用いても良い。最
も好ましい例に、5−ソジュウムスルホイソ7タレート
を1〜5モルチ共重合したポリエチレンテレフタレート
である。
However, r: Radius of nozzle hole (minor) Q: Polymer discharge amount per single hole (m/5ec) The alkali easily degradable polyester referred to in the present invention refers to polyalkylene glycol copolymerized polyethylene terephthalate, inphthalate copolymerized polyethylene terephthalate, 5-sodium sulfoisophthalate copolymerized polyethylene terephthalate, etc., and these may be used in combination. The most preferred example is polyethylene terephthalate obtained by copolymerizing 1 to 5 moles of 5-sodium sulfoiiso7thaleate.

特に前記[1]、(113を主成分とする溶融異方性ポ
リエステルと、5−ソジュウムスルホイソフタレートを
1〜5モル憂共重合したポリエチレンテレフタレートで
複合紡糸した場合に最も有効に行なわれる。即ち、複合
紡糸がスムーズに行なわれ、2成分のアルカリ分解層が
10倍以上異なるため、アルカリ性溶液による処理が、
工業的に短時間で行う事が出来る。かつ易分解成分をほ
ぼ完全に線除去できるので、次の熱処理工程で融着等の
トラブルの発生が生じない。
In particular, it is most effective when composite spinning is performed using a melt anisotropic polyester containing the above-mentioned [1] (113) as a main component and polyethylene terephthalate copolymerized with 1 to 5 moles of 5-sodium sulfoisophthalate. In other words, composite spinning is carried out smoothly, and the alkaline decomposition layers of the two components differ by more than 10 times, so treatment with an alkaline solution
It can be done industrially in a short time. In addition, since easily decomposable components can be almost completely removed, troubles such as fusion will not occur in the next heat treatment step.

本発明の主目的は、高強度の極細繊維(%に3デニール
以下の繊維)を得ることであり、そのためKは、溶融異
方性ポリエステルをアルカリ易分解性ポリエステルによ
って少なくとも2個のセグメン)K分割された形態で複
合紡糸する必要がある。先にも述べたように溶融異方性
ポリエステルは、ノズル通過時に著しい分子配向が生じ
るため、その後の延伸(いわゆる紡糸ドラフト)をめま
り大きくとることが出来ない。良好紡糸調子を得るには
、ドラフトは10〜40倍である。このため紡糸原糸の
段階では、5〜10デニールより小さいものは得られ難
い。そのため、本発明の目的としている3デニール以下
の極細糸を得るKは、2ヶ以上のセグメントに分割して
おく必要がある○好ましくは、4〜10個である。易分
解性成分の占める割合いは、少ない方が好ましいが、セ
グメントに分割を完全にする必要上、全繊維に対して1
0〜50重量%とすることが適当である。
The main objective of the present invention is to obtain high-strength ultrafine fibers (fibers with a denier of less than 3 denier in %), for which K is a melt-anisotropic polyester with at least two segments (K It is necessary to perform composite spinning in a divided form. As mentioned above, melt anisotropic polyester undergoes significant molecular orientation when passing through a nozzle, so it is impossible to draw it afterward (so-called spinning draft) to a large extent. To obtain good spinning condition, the draft is 10 to 40 times. For this reason, it is difficult to obtain yarns smaller than 5 to 10 deniers at the spinning stage. Therefore, K to obtain the ultrafine yarn of 3 deniers or less, which is the object of the present invention, requires dividing into two or more segments. Preferably, the number is 4 to 10. It is preferable that the proportion of easily degradable components be small, but because it is necessary to completely divide the fibers into segments, it is necessary to
A suitable range is 0 to 50% by weight.

本発明の複合形態の横断面例の概略図を第1図に示す。A schematic diagram of a cross-sectional example of a composite form of the present invention is shown in FIG.

本発明に言うアルカリ溶液での処理とに、水酸化ナトリ
ウム、水酸化カリウム等を主成分とする処理液であり、
緩衝剤や分解促進剤等を含んでいてもよい。また処理法
としては、浸漬法、デイツプニップ法、ローラーバット
法いずれも可能であるO 繊維の形態としては、フィラメント、ステープル、ある
いは織物、編物、不織布等で行うこともできる。
In the treatment with an alkaline solution referred to in the present invention, a treatment liquid containing sodium hydroxide, potassium hydroxide, etc. as a main component,
It may also contain a buffer, a decomposition accelerator, and the like. Further, as a treatment method, any of a dipping method, a dip nip method, and a roller butt method are possible.As for the form of the fiber, filament, staple, woven fabric, knitted fabric, nonwoven fabric, etc. can also be used.

分割処理後、中和、水洗、乾燥処理が行なわれるのが普
通である。
After the division process, neutralization, washing with water, and drying processes are usually performed.

熱処理は、該溶融異方性ポリエステルの融点をTm(℃
)とするとき、−以下(Trri−80℃)以上の温度
で行なわれる。Tmは、一般Vこ熱処理につれて上昇す
るので、処理温Ifは順次上昇していく温度パターンが
好ましい。
The heat treatment lowers the melting point of the melt anisotropic polyester to Tm (℃
), it is carried out at a temperature of - or lower (Trri-80°C) or higher. Since Tm generally increases with heat treatment, a temperature pattern in which the treatment temperature If increases sequentially is preferable.

該熱処理としては、窒素等の不活性ガスや、真空中ある
いは空気の如き酸素含有の活性ガス雰囲気で行うことが
出来る。この熱処理にエリ分割された各セグメントの強
度を30%以上増大させることが出来る。本発明で得ら
れる極細繊維は衣料用、産業資材用途において広く使用
される。衣料用途としては、各種作業服、スポーツ衣料
、防護衣料、また産業資材用としては、高温用あるいに
耐薬品用のワイピングクロス、各種テン7ヨンメンバー
 コート類、フィルター マット、テント類等に使用て
れる。
The heat treatment can be performed in an inert gas such as nitrogen, in a vacuum, or in an oxygen-containing active gas atmosphere such as air. This heat treatment can increase the strength of each segment by 30% or more. The ultrafine fibers obtained by the present invention are widely used in clothing and industrial material applications. Clothing applications include various work clothes, sports clothing, and protective clothing.As for industrial materials, it is used for high temperature and chemical resistant wiping cloths, various ten-member coats, filter mats, tents, etc. I can see it.

以下、実施例により本発明をエフ具体的に説明するが、
本発明は、これらの実施例により@定されるものではな
い。
Hereinafter, the present invention will be specifically explained with reference to Examples.
The present invention is not limited to these Examples.

実施例1 構成単位〔I〕と〔■〕が7.3:2.7である溶融異
方性芳香族ポリエステルポリマーを作成した。このポリ
マーの性質は η1nh−5,7dz/f Tm=280℃ テアツタ。ηinhの測定は試料をペンタフルオロフェ
ノールに0.1重1%溶解しく60〜80℃)。
Example 1 A melt anisotropic aromatic polyester polymer in which the structural units [I] and [■] were in a ratio of 7.3:2.7 was prepared. The properties of this polymer are η1nh-5,7dz/f Tm=280°C. To measure ηinh, dissolve the sample in pentafluorophenol at 0.1% by weight (60-80°C).

60℃の恒温槽中で、ウソベローデ型粘度計で測定する
Measurement is performed using an Usoberohde viscometer in a constant temperature bath at 60°C.

−の測定は、示差走査熱量計(メトラー社gDSC)で
行い観察される主吸熱のピーク温度を而と足めた。
- was measured using a differential scanning calorimeter (Mettler gDSC) and the observed peak temperature of the main endotherm was added.

易分解性ポリエステルとして5−ソジュウムスルホイソ
フタレートを3モル%某重合したポリエチレンテレフタ
レートを用いた。
As the easily decomposable polyester, polyethylene terephthalate obtained by polymerizing 3 mol% of 5-sodium sulfoisophthalate was used.

この嶌のの固有粘度〔η〕は0.48 d4/fであっ
た。
The intrinsic viscosity [η] of this product was 0.48 d4/f.

〔η〕の測定は、フェノールとテトラクロルエタンの等
量混合溶媒を用い30℃の恒温槽中で測定した0 各ポリマーを2台の押出機より溶融し、ギヤポンプから
7:3の重量割合(溶融異方性ポリマーニア、易分解性
ポリマー:3)で紡糸ヘッドに導き、第1図(C)の断
面形状を有する150d/15fのマルチフィラメント
を紡糸した0 この本のを穴のめいたステンレス製ボビンに巻き、  
5 % NaOH水溶液に浸し、90℃で40分間処理
した。
[η] was measured using a mixed solvent of equal amounts of phenol and tetrachloroethane in a constant temperature bath at 30°C. Each polymer was melted using two extruders, and a weight ratio of 7:3 was measured using a gear pump. A 150d/15f multifilament with a cross-sectional shape shown in Figure 1 (C) was spun by guiding it to the spinning head using a melting anisotropic polymer (3), an easily degradable polymer. Wind it on a made bobbin,
It was immersed in a 5% NaOH aqueous solution and treated at 90°C for 40 minutes.

この処理による重量減少は31チであり、易分解性ポリ
マーは、はぼ完全に除却され、各フィラメントFi、6
個に分割されていた0このものをリン酸液で中和し、熱
湯で十分洗浄した後乾燥した。
The weight loss due to this treatment was 31 inches, the easily degradable polymer was almost completely removed, and each filament Fi, 6
This material, which had been divided into pieces, was neutralized with a phosphoric acid solution, thoroughly washed with boiling water, and then dried.

このもののヤーン強度fl、 9.1 r/d″′Cあ
つ九。
The yarn strength of this material is fl, 9.1 r/d'''C.

また単糸の繊度は0.3〜1.8デニールであり平均は
0.86デニールであった。
Further, the fineness of the single yarn was 0.3 to 1.8 denier, and the average was 0.86 denier.

このボビンを熱風炉(ボビンの内側よジ糸層を通り外部
に抜ける)に入れ、260℃で1時間、270℃で2時
間、270℃から285℃に上昇しながら5時間処理し
た。処理気体は露点が一70℃の除湿空気を用いた。
This bobbin was placed in a hot air oven (passing through the inner weft layer of the bobbin to the outside) and treated at 260°C for 1 hour, at 270°C for 2 hours, and for 5 hours while increasing from 270°C to 285°C. Dehumidified air with a dew point of 170° C. was used as the processing gas.

このものは、膠着等のトラブルは全くなく、通常の紙管
に巻返すことが出きた0ヤ一/強度は24 f/d T
 アff、強fllF1163 * %増大した。
This product had no problems such as sticking and could be rewound into a normal paper tube.The strength was 24 f/d T.
Aff, strongly increased by F1163*%.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明の分割前の複合繊維の断面の例である。 特徴出願人 株式会社 り ラ し FIG. 1 is an example of a cross section of the composite fiber of the present invention before division. Characteristics Applicant: RiRashi Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] 溶融異方性芳香族ポリエステルが、アルカリ易分解性ポ
リエステルによつて、少なくとも2個のセグメントに分
割された複合繊維を紡糸し、該複合繊維をアルカリ性溶
液で処理し、アルカリ易分解性ポリエステルを除去し各
セグメントに分割した後、各セグメントを該セグメント
を構成する溶融異方性芳香族ポリエステルの(融点−8
0℃)以上融点以下の温度で熱処理し、強度を30%以
上増加させることを特徴とする溶融異方性芳香族ポリエ
ステル繊維からなる極細繊維の製造方法。
Spinning a conjugate fiber in which the melt anisotropic aromatic polyester is divided into at least two segments by the alkali easily decomposable polyester, and the conjugate fiber is treated with an alkaline solution to remove the alkali easily decomposable polyester. After dividing into each segment, each segment is divided into (melting point -8
1. A method for producing ultrafine fibers made of melt-anisotropic aromatic polyester fibers, characterized in that the fibers are heat-treated at temperatures above 0° C.) and below their melting point to increase their strength by 30% or more.
JP14668290A 1990-06-04 1990-06-04 Production of superfine fiber composed of melt-anisotropic aromatic polyester Pending JPH0441713A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP14668290A JPH0441713A (en) 1990-06-04 1990-06-04 Production of superfine fiber composed of melt-anisotropic aromatic polyester

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP14668290A JPH0441713A (en) 1990-06-04 1990-06-04 Production of superfine fiber composed of melt-anisotropic aromatic polyester

Publications (1)

Publication Number Publication Date
JPH0441713A true JPH0441713A (en) 1992-02-12

Family

ID=15413206

Family Applications (1)

Application Number Title Priority Date Filing Date
JP14668290A Pending JPH0441713A (en) 1990-06-04 1990-06-04 Production of superfine fiber composed of melt-anisotropic aromatic polyester

Country Status (1)

Country Link
JP (1) JPH0441713A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07316926A (en) * 1994-05-19 1995-12-05 Kuraray Co Ltd Sheath-core type conjugate yarn, coated yarn and its production
JP2008214842A (en) * 2007-02-07 2008-09-18 Toray Ind Inc Method for producing liquid crystal polyester fiber

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07316926A (en) * 1994-05-19 1995-12-05 Kuraray Co Ltd Sheath-core type conjugate yarn, coated yarn and its production
JP2008214842A (en) * 2007-02-07 2008-09-18 Toray Ind Inc Method for producing liquid crystal polyester fiber

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