JPH01239109A - Polyphenylene sulfide fiber, its production and false-twisted yarn of said fiber - Google Patents
Polyphenylene sulfide fiber, its production and false-twisted yarn of said fiberInfo
- Publication number
- JPH01239109A JPH01239109A JP5952988A JP5952988A JPH01239109A JP H01239109 A JPH01239109 A JP H01239109A JP 5952988 A JP5952988 A JP 5952988A JP 5952988 A JP5952988 A JP 5952988A JP H01239109 A JPH01239109 A JP H01239109A
- Authority
- JP
- Japan
- Prior art keywords
- fiber
- polyphenylene sulfide
- melt viscosity
- poise
- temperature
- 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
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 77
- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 50
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 238000009987 spinning Methods 0.000 claims abstract description 53
- 239000000155 melt Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 abstract description 39
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 20
- 230000000704 physical effect Effects 0.000 description 17
- 238000006116 polymerization reaction Methods 0.000 description 13
- 238000009776 industrial production Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- -1 polyethylene terephthalate Polymers 0.000 description 4
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229940117389 dichlorobenzene Drugs 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- AYOOGWWGECJQPI-NSHDSACASA-N n-[(1s)-1-(5-fluoropyrimidin-2-yl)ethyl]-3-(3-propan-2-yloxy-1h-pyrazol-5-yl)imidazo[4,5-b]pyridin-5-amine Chemical compound N1C(OC(C)C)=CC(N2C3=NC(N[C@@H](C)C=4N=CC(F)=CN=4)=CC=C3N=C2)=N1 AYOOGWWGECJQPI-NSHDSACASA-N 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000011090 industrial biotechnology method and process Methods 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- IAQLJCYTGRMXMA-UHFFFAOYSA-M lithium;acetate;dihydrate Chemical compound [Li+].O.O.CC([O-])=O IAQLJCYTGRMXMA-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
- D01F6/765—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products from polyarylene sulfides
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、耐熱性・耐薬品性が要求される、各種フィル
ターに好適なポリフェニレンサルファイド繊維、その製
造方法更には該繊維の仮撚加工糸に関するもので、更に
詳しくは、高強度・低収縮率といった優れた特性を有す
るポリフェニレンサルファイド繊維、及び紡糸・延伸時
の糸切れ、毛羽発生が極めて少ないレベルで該繊維を工
業的製造を可能にした製造方法に関する。Detailed Description of the Invention [Industrial Application Field] The present invention relates to a polyphenylene sulfide fiber suitable for various filters that requires heat resistance and chemical resistance, a method for producing the same, and a false twisted yarn of the fiber. More specifically, it is a polyphenylene sulfide fiber that has excellent properties such as high strength and low shrinkage, and that enables industrial production of this fiber with extremely low occurrence of yarn breakage and fuzz during spinning and drawing. Regarding the manufacturing method.
［従来技術］
ポリフェニレンサルファイドは耐熱性・耐薬品性に優れ
たポリマーであり、近年、電気、゛電子分野、自動車分
野、ｖ１械分野等に使用され、生産量ら急激に増加し始
めている。一方、その繊維化についても、多くの提案が
なされている（例えば、特開昭５２−３０６０９号公報
、特開昭５８−２０４０４７号公報。[Prior Art] Polyphenylene sulfide is a polymer with excellent heat resistance and chemical resistance.In recent years, it has been used in the fields of electricity, electronics, automobiles, V1 machinery, etc., and its production volume has begun to increase rapidly. On the other hand, many proposals have been made regarding its fiberization (for example, JP-A-52-30609 and JP-A-58-204047).
特開昭５７−１４３５１８号公報、特開昭６１−７５８
１２号公報）、しかしながら、従来の提案では、（ａ）
モノフィラメント如き、極めて線径が太いものを得るに
過ぎないｆｂ） ＯＩ性面でも不十分なものしか得られ
ていない、更に（Ｃ）マルチフィラメントを高生産性と
高物性を以て得るような試みは、はとんどない。JP-A-57-143518, JP-A-61-758
However, in the conventional proposal, (a)
(c) Attempts to obtain multifilaments with high productivity and high physical properties have resulted in only insufficient results in terms of OI properties. There's no way.
すなわち、その生産技術という観点から見てみると、従
来のポリマー例えば、ポリエチレンテレフタレート、ナ
イロンの足元にも及ばない、従って、本発明の如く強度
が充分に高く、寸法安定性ら優れた特性を有し、しかも
単糸デニールが１〜４ｄＯといった細いフィラメントか
ら構成されるマルチフィラメントにさえも適用可能な工
業的技術に関してはその技術確立が強く要望されてはい
る。That is, from the viewpoint of production technology, it is not even as good as conventional polymers such as polyethylene terephthalate and nylon.Therefore, the present invention has sufficiently high strength and excellent properties such as dimensional stability. However, there is a strong desire to establish an industrial technology that can be applied even to multifilaments composed of thin filaments with a single filament denier of 1 to 4 dO.
［発明の目的］
本発明の第１の目的は、機械的性質更には寸法安定性に
潰れたポリフェニレンサルファイド繊維、その製造方法
、更には該繊維の仮撚加工糸を提供する事にある０本発
明の第２の目的は、紡糸・延伸過程での断糸及び単糸切
れが少ない、該繊維の製造方法を提供する事にある。[Object of the Invention] The first object of the present invention is to provide a polyphenylene sulfide fiber with improved mechanical properties and dimensional stability, a method for producing the same, and a false twisted yarn of the fiber. A second object of the invention is to provide a method for producing the fiber in which yarn breakage and single filament breakage during spinning and drawing processes are reduced.
本発明の第３の目的は、紡糸時のバックの圧力上昇が小
さくて、連続紡糸可能なポリフェニレンサルファイド繊
維及びその製造法を提供する事にある。A third object of the present invention is to provide a polyphenylene sulfide fiber that can be continuously spun with a small increase in bag pressure during spinning, and a method for producing the same.
本発明の第４の目的は、毛羽発生が少なく、製織性良好
なポリフェニレンサルファイド繊維、更にはその仮撚加
工系を提供する事にある。A fourth object of the present invention is to provide a polyphenylene sulfide fiber with less fluff and good weavability, and a false twisting system thereof.
（構成）
本発明者等は、前記目的を達成すべく検討を重ねたとこ
ろ、繊維物性と製糸性とを両立させるには、ポリフェニ
レンサルファイドの溶融粘度特性に極めて臨界性が存在
していることを見い出した。(Structure) After repeated studies to achieve the above object, the present inventors found that the melt viscosity characteristics of polyphenylene sulfide are extremely critical in achieving both fiber properties and spinnability. I found it.
つまり、成る特定の重合度及び分子鎖について特定の直
線性とを有するポリフェニレンサルファイドを用いると
き、前述の目的が達成されることを見い出したのである
。In other words, it has been found that the aforementioned object is achieved when using polyphenylene sulfide having a specific degree of polymerization and a specific linearity of the molecular chains.
かくして、本発明は、以下の構成からなる。Thus, the present invention consists of the following configuration.
（１）下記［１］〜［３］の条件を同時に満足する事を
特徴とするポリフェニレンサルファイド！！。(1) Polyphenylene sulfide characterized by simultaneously satisfying the following conditions [1] to [3]! ! .
■ 該繊維は、温度３２０℃、剪断速度（？）１０００
５ｆ３Ｃ’での溶融粘度（ＭＶ ）が７００〜１２
００ポイズであり、温度３２０℃、剪断速度（テ） ３
０００ｓｅｃ−１での溶融粘度（ＭＶ ）が６００
ポイズ以上であり、かつ、該Ｆｇ融粘度差＜ Ｍ Ｖ
ｙ Ｖ ３０００ ）が２００ポイズ以下である
ような線状ポリフェニレンサルファイドからなること。■ The fiber has a temperature of 320°C and a shear rate (?) of 1000
Melt viscosity (MV) at 5f3C' is 700-12
00 poise, temperature 320℃, shear rate (te) 3
Melt viscosity (MV) at 000 sec-1 is 600
poise or more, and the Fg melt viscosity difference < MV
y V 3000 ) is 200 poise or less.
■ 繊維強度（Ｓｔ）が４．０ ｇ／ｄａ以上、シルク
ファクター（ＳＦ）が２０以上であること。■ Fiber strength (St) is 4.0 g/da or more and silk factor (SF) is 20 or more.
■ 温度１８０℃での乾熱収縮率（ＨＳ ）が１５％以
下であること。■ Dry heat shrinkage (HS) at a temperature of 180°C is 15% or less.
（２）上記■のポリマーを口金温度が３１０〜３３０°
Ｃ１紡糸速度１０００ｍ／分以下で紡糸し、延伸熱処理
する事を特徴とする上記ポリフェニレンサルファイド繊
維の製造法。(2) Use the polymer described in ■ above at a base temperature of 310 to 330°.
C1 A method for producing the polyphenylene sulfide fiber described above, characterized in that the fiber is spun at a spinning speed of 1000 m/min or less and subjected to drawing heat treatment.
以下、本発明について、詳細に説明する。The present invention will be explained in detail below.
一般に、結晶性の熱可塑性ポリマーを紡糸する場合、紡
糸温度は（融点＋３０〜７０）”Ｃの温度傾城を採用す
る事が多い、勿論、同一ポリマーでも、重合度・紡糸機
内でのポリマーの滞溜時間等により、微調整が必要であ
る事は言うまでもない、−般ボリフェニレンサルファイ
ドの融点は、ＤＴＡの測定値では、２８４℃近傍の値と
なり、紡糸温度は３２０℃〜３５０°Ｃ，ポリマー溶融
温度としては、３１０〜３３０°Ｃ程度が好ましい、そ
の際、ポリマーの粘度特性が繊維の物性及び紡糸延伸性
に極めて多きな影響を与え、両者を両立させる意味で特
に、ポリフェニレンサルファイドの場合は、適性範囲が
極めて狭い事が判明した。Generally, when spinning crystalline thermoplastic polymers, a temperature gradient of (melting point +30 to 70) C is often adopted for the spinning temperature. Needless to say, fine adjustment is required depending on the distillation time, etc. - The melting point of general polyphenylene sulfide is around 284°C as measured by DTA, the spinning temperature is 320°C to 350°C, and the polymer melting temperature is 320°C to 350°C. The temperature is preferably about 310 to 330°C. In this case, the viscosity characteristics of the polymer have a very large influence on the physical properties and spinning drawability of the fiber, and in order to achieve both, especially in the case of polyphenylene sulfide, It turns out that the range of suitability is extremely narrow.
すなわち、生産性及び繊維特性が大きく改善され、かつ
両者を同時に満足するためにはミ温度り２０℃、剪断速
度（−ｉ−） １０００ｓｅｃ４での溶融粘度（ＭＶｌ
ｏｏ。）が７００〜１２００ポイズであり、温度３２０
℃、剪断速度（−ｒ） ３０００ｓｅｃ−’での溶融粘
度（ＭＶ３ｏｏ。）が６００ポイズ以上であり、カッ、
該溶融粘度差（ＭＶ Ｍ Ｖ ３０００ ）が２
００ポイズ以下の線状ポリフェニレンサルファイドを用
いる事が必須である。すなわち、この２つの異なる剪断
速度１？）での溶融粘度（ＭＶ 、及びＭＶ３００
０ ）の値は、高生産性と高物性とを兼ねそなえたポリ
フェニレンサルファイド繊維を得るための１つの指標と
なる。すなわち温度３２０℃、剪断速度１０００ ｓｅ
ｃ″Ｎでの溶融粘度（ＭＶ１０００）が７００ポイズ未
満の時は、重合度が低過ぎるため、（１）物性、特に強
度の面で充分なものを得る事が出来ない、■延伸時の単
糸切れが多発する、（１）未延伸糸の経過変化が進みや
すいため、未延伸糸の保管に間頚か出やすい、更には、
（へ）延伸時の高温セットの際に、単糸切れ・毛羽が出
やすくなるため、好ましくない、一方、温度３２０°Ｃ
１剪断速度１０００ｓｅｃ−１での溶融粘度が１２００
ポイズを超える場合、重合度かあまりにも高過ぎるため
、（１）紡糸速度を高める事が出来ない（紡糸速度を高
くしていくと、未延伸糸の段階で毛羽・ループが多発し
、断糸しやすくなる）■）延伸倍率を高くする事が出来
ないので、高物性の繊維を得る事が出来ず、かつ、延伸
時の単糸切れも多く好ましくない。In other words, productivity and fiber properties are greatly improved, and in order to satisfy both simultaneously, the melt viscosity (MVl) at a temperature of 20°C and a shear rate (-i-) of 1000 sec4 is required.
oo. ) is 700 to 1200 poise, and the temperature is 320
℃, the melt viscosity (MV3oo.) at a shear rate (-r) of 3000 sec-' is 600 poise or more,
The melt viscosity difference (MV MV 3000) is 2
It is essential to use linear polyphenylene sulfide of 00 poise or less. That is, these two different shear rates 1? ) at melt viscosity (MV, and MV300
0) is one indicator for obtaining polyphenylene sulfide fibers that have both high productivity and high physical properties. That is, the temperature is 320°C and the shear rate is 1000 se.
When the melt viscosity (MV1000) at c″N is less than 700 poise, the degree of polymerization is too low, resulting in (1) insufficient physical properties, especially strength; Frequent thread breakage occurs; (1) undrawn threads tend to change over time; therefore, undrawn threads are prone to cracking during storage;
(f) Unfavorable because single yarn breakage and fuzz are likely to occur during high-temperature setting during stretching; on the other hand, the temperature is 320°C.
1 The melt viscosity at a shear rate of 1000 sec-1 is 1200
If it exceeds poise, the degree of polymerization is too high, so (1) the spinning speed cannot be increased (if the spinning speed is increased, fuzz and loops will occur frequently in the undrawn yarn stage, and yarn breakage will occur). (1) Since the drawing ratio cannot be increased, fibers with high physical properties cannot be obtained, and single fiber breakage occurs frequently during drawing, which is undesirable.
次に、剪断速度３０００ ｓｅｃ’の溶融粘度（ＭＶ３
０００ ）との関係が重要である。一般に、高分子の溶
融粘度は、剪断速度に依存し、剪断速度を大きくすると
、溶融粘度は減少する。その際の剪断速度依存性は、高
分子鎖の形態にも依存する６例えば、架橋高分子・枝分
れ高分子等の非鎖状性（直線性の悪い）高分子鎖の場合
は、剪断速度が小さいと高い溶融粘度を示すが、剪断速
度を大きくし−ていくと、溶融粘度は急激に低下する挙
動を示すという、剪断速度依存性が大きい特徴を有する
。Next, the melt viscosity (MV3
000) is important. Generally, the melt viscosity of a polymer depends on the shear rate, and as the shear rate increases, the melt viscosity decreases. The shear rate dependence at this time also depends on the morphology of the polymer chain6.For example, in the case of non-chain polymer chains (poor linearity) such as cross-linked polymers and branched polymers, shear rate dependence It exhibits a high melt viscosity when the shear rate is low, but as the shear rate increases, the melt viscosity shows a behavior that rapidly decreases, and is characterized by a large dependence on shear rate.
一方、直線性の良い高分子鎖は、剪断速度が小さい場合
、溶融粘度は非直線性高分子鎖の場合程、高くはないが
、剪断速度を大きくしても、溶融粘度の低下の程度はそ
れ程大きくならないという、剪断速度依存性が小さいと
いう特徴を有する。所で、ポリフェニレンサルファイド
ポリマーは、必ずしも直線性の良いポリマーだけではな
いため、そのｍ帷化の際は、上記特性が極めて重要にな
ってくる。この点、本発明者等は、ポリフェニレンサル
ファイドの場合、前記２つの粘度差（ＭＶ１０００−Ｍ
Ｖ３０００ ）の値が、２００ポイズ以下であるポリマ
ーが直線性の面で好ましい事を見い出した。On the other hand, for polymer chains with good linearity, when the shear rate is small, the melt viscosity is not as high as for non-linear polymer chains, but even if the shear rate is increased, the degree of decrease in melt viscosity is It is characterized by a small shear rate dependence that does not increase that much. By the way, since polyphenylene sulfide polymers are not necessarily polymers with good linearity, the above characteristics become extremely important when making them into m-threads. In this regard, the present inventors found that in the case of polyphenylene sulfide, the above two viscosity differences (MV1000-M
It has been found that a polymer having a V3000 value of 200 poise or less is preferable in terms of linearity.
すなわち、この溶融粘度差（ＭＶ１０００ ＭＶ３０
００ ’の値が、２００ポイズを越える場合は、目標と
する高生産・高物性を有するポリフェニレンサルファイ
ド繊維を得る事は出来ない、何故なら、この場合、高分
子鎖の直線性が良くないため、（１）紡糸時のパック圧
の上昇が大きく、長期的な連続運転が出来ない、０）紡
糸速度を高める事が出来ない、（１）物性面で充分なも
のを得る事が出来ない、（へ）延伸性が不良であり、単
糸切れ・断糸が多発する等の不利益が生じる。That is, this melt viscosity difference (MV1000 MV30
If the value of 00' exceeds 200 poise, it is not possible to obtain polyphenylene sulfide fibers with the target high production and high physical properties, because in this case, the linearity of the polymer chain is not good. (1) The increase in pack pressure during spinning is large and long-term continuous operation is not possible; 0) It is not possible to increase the spinning speed; (1) It is not possible to obtain sufficient physical properties; f) Stretchability is poor, resulting in disadvantages such as frequent single yarn breakage and yarn breakage.
尚、ＭＶ３ｏｏｏの値は、重合度・直線性の関係で、６
００ポイズ以上は必要である。すなわちＭ■３ｏ０゜が
６００ポイズ未満の時は、重合度が著しく低いかあるい
は直線性が極めて悪いなめ、目標とする、高生産性及び
高特性を兼備したポリフェニレンサルファイド繊維を得
る事ができない。In addition, the value of MV3ooo is 6 due to the relationship between the degree of polymerization and linearity.
00 poise or more is required. That is, when M3o0° is less than 600 poise, the degree of polymerization is extremely low or the linearity is extremely poor, making it impossible to obtain polyphenylene sulfide fibers that have both high productivity and high properties as desired.
本発明で用いるポリフェニレンサルファイドは、公知の
合成法、例えば極性有機溶剤中で無水硫化ナトリウムと
多ハロ置換の環状化合物とを反応させることによって得
ることができるが、その際本発明の粘度要件を満足させ
るためには、後記の実施例に示すように重合温度と重合
時間とを適宜調整することが肝要である。尚、本発明で
いうポリフェニレンサルファイドとは、ポリマーの繰り
返し単位の９０％以上が＋バ層Ｘｓ＋で構成されたポリ
マーである。勿論、他に１０％未満のメタフェニ性と製
糸性とを確保するためには、紡糸の際、紡糸口金面温度
を３１０〜３３０℃に設定する事が肝要である０口金温
度が３１０℃未満の時は、口金面温度が低過ぎるなめ、
目的とする高生産性・高物性のポリフェニレンサルファ
イドを得る事は出来ない、一方、口金面温度が３３０’
Ｃを越える場合は、温度が高過ぎ、繊維の着色化が進み
、紡糸性の低下、更には、延伸性も低下し好ましくない
。The polyphenylene sulfide used in the present invention can be obtained by a known synthesis method, for example, by reacting anhydrous sodium sulfide with a polyhalo-substituted cyclic compound in a polar organic solvent, and in this case, it satisfies the viscosity requirements of the present invention. In order to achieve this, it is important to appropriately adjust the polymerization temperature and polymerization time as shown in Examples below. In addition, polyphenylene sulfide as used in the present invention is a polymer in which 90% or more of the repeating units of the polymer are constituted by a layer Xs+. Of course, in order to ensure less than 10% metaphenylicity and spinning properties, it is important to set the spinneret surface temperature to 310 to 330°C during spinning. When the mouthpiece surface temperature is too low,
It is not possible to obtain the desired polyphenylene sulfide with high productivity and high physical properties.On the other hand, when the die surface temperature is 330'
If it exceeds C, the temperature is too high, the coloring of the fibers progresses, the spinnability decreases, and the drawability also decreases, which is not preferable.
一方、紡糸速度としてはｊｏｏｏｍ ／分未満、好まし
くは、３００〜８００ｍ／分が採用される。紡糸速度が
１０００ｍ ／分を越える場合は、（１）得られる延伸
糸の強度が充分でない、Ｃ）延伸工程での単糸切れが多
発する、（ｎ）毛羽も出やすい、といった欠点がある。On the other hand, the spinning speed is less than jooom/min, preferably 300 to 800 m/min. When the spinning speed exceeds 1000 m/min, there are disadvantages such as (1) insufficient strength of the drawn yarn obtained, C) frequent breakage of single filaments during the drawing process, and (n) fuzzing.
尚、紡糸速度が３００ｍ／分未満の場合は、生産性が低
くなる。Note that if the spinning speed is less than 300 m/min, productivity will be low.
ここで、紡糸設備としては、紡糸温度３４０〜３５０”
Ｃ程度の高温紡糸可能な設備であれば、ポリエステルに
採用している既存の設備をそのまま使用できる。罐、本
発明においては、紡糸口金温度の適性化が、高生産性・
高特性を満足する上で重要であるので、紡糸口金面に温
度検出端を挿入し、紡糸温度・［ｉ全面周りの温度調整
により、口金面温度をコントロールする事が必要である
６次に、延伸・熱処理操作であるが、本発明においては
、延伸熱処理を一度で行なうのではなく、−度、１５０
°Ｃ未満の温度での延伸で配向結晶化させてから、１５
０℃以上の温度で熱処理する方法が好ましい、又延伸速
度も必ずしも制限されるものではなく、通常の延伸速度
、例えば、１００〜８００ｍ／分程度を採用すればよい
。Here, the spinning equipment has a spinning temperature of 340 to 350"
Existing equipment used for polyester can be used as is, as long as it is capable of spinning at a high temperature of about C. In the present invention, optimization of the spinneret temperature leads to high productivity and
Since it is important to satisfy high properties, it is necessary to control the spinneret surface temperature by inserting a temperature detection end into the spinning nozzle surface and adjusting the temperature around the entire surface of the spinning nozzle.6 Next, Although the stretching and heat treatment operations are performed, in the present invention, the stretching heat treatment is not performed at once, but at 150 degrees
Oriented crystallization by stretching at temperatures below 15 °C
A method of heat treatment at a temperature of 0° C. or higher is preferable, and the stretching speed is not necessarily limited, and a normal stretching speed, for example, about 100 to 800 m/min may be adopted.
このようにして得られる本発明のポリフェニレンサルフ
ァイド繊維は強度が４．Ｏｆ／ｄｅ以上でシルクファク
ター（強度×ＦＷ雇）が２０以上と、力学的性質が従来
のポリフェニレンサルファイド繊維では見られなかった
卓越したらのとなる。力学的性質、例えば強度は、ｍ編
物の引き裂き強力に影響を及ぼず重要な因子である。す
なわち、高強度な繊維程、織編物の軽量化という面で有
利な事は言うまでもない、一方、シルクファクターが小
さい繊維の場合は、高強度繊維を得るためには、伸度を
かなり小さくしなければならず、毛羽等の品位面で問題
が発生し、しかも、延伸工程では、断糸、単糸切れが多
発し、工業的生産は困難である。この点、本発明で得ら
れるポリフェニレンサルファイド繊維は、シルクファク
ターが２０以上と極めて大きいため、伸度を例えば、２
０〜３０％と比較的残すような伸度倍率でも強度が４−
０ｇ／ｄｅ以上の繊維を得る事がｕ１来るなめ、工業的
生産が可能となるわけである。The polyphenylene sulfide fiber of the present invention thus obtained has a strength of 4. With a Silk Factor (Strength x FW) of 20 or more at Of/de or higher, the mechanical properties are outstanding, which has not been seen in conventional polyphenylene sulfide fibers. Mechanical properties, such as strength, are important factors that do not affect the tearing strength of m-knitted fabrics. In other words, it goes without saying that the higher the strength of the fiber, the more advantageous it is in terms of reducing the weight of woven or knitted products.On the other hand, in the case of fibers with a small silk factor, in order to obtain high strength fibers, the elongation must be considerably reduced. Not only that, problems arise in terms of quality such as fluff, and moreover, yarn breakage and single yarn breakage occur frequently in the drawing process, making industrial production difficult. In this regard, since the polyphenylene sulfide fiber obtained by the present invention has an extremely large silk factor of 20 or more, the elongation can be reduced to 2, for example.
Even at a relatively low elongation ratio of 0 to 30%, the strength is 4-4.
Since it is possible to obtain fibers of 0 g/de or more, industrial production becomes possible.
更に、本発明の繊維の優れた特性としては、１８０℃で
の乾熱収縮率（無荷重下）が１５％以下で、寸法安定性
に極めて優れている事である。ポリフェニレンサルファ
イド１ｉｌｌＩｌ維は、その耐熱性・耐薬品性を生かし
、工業用フィルター等に使用される。Further, the excellent properties of the fiber of the present invention include that the dry heat shrinkage rate (under no load) at 180° C. is 15% or less, and it has extremely excellent dimensional stability. Polyphenylene sulfide fibers are used in industrial filters and the like because of their heat resistance and chemical resistance.
その際、織物の仕上げ過稈で、高温処理するなめ、繊維
自体の収縮率を小さくしないと、布帛にシボあるいはス
ジが入り性能・品位共に低下する。−方、ポリフェニレ
ンサルファイド繊維の延伸工程での熱処理は、充分に配
向した繊維でないと単糸切れ・毛羽が多発し、工業的生
産には供し得ない。At this time, if the woven fabric is overfinished, treated at high temperature, and the shrinkage rate of the fiber itself is not reduced, the fabric will develop grains or streaks, reducing both performance and quality. - On the other hand, heat treatment during the drawing process of polyphenylene sulfide fibers causes frequent breakage and fuzzing of single filaments unless the fibers are sufficiently oriented, making it unsuitable for industrial production.
この点、本発明の繊維においては、延伸工程での配向が
同等トラブルなく行われたるめ、引き続いて行なわれる
熱処理操作がスムーズに行なわれるわけである６以上の
ように、本発明のポリフェニレンサルファイド繊維は、
優れた生産性を有するだけでなく、物性面でも従来のポ
リフェニレンサルファイド繊維にない優れたものとなる
。In this regard, in the fibers of the present invention, the orientation during the drawing process is performed without any trouble, so the subsequent heat treatment operation is carried out smoothly.6 As mentioned above, the polyphenylene sulfide fibers of the present invention teeth,
Not only does it have excellent productivity, but it also has superior physical properties that are not found in conventional polyphenylene sulfide fibers.
更に、本発明の他の態様によれば、上述のポリフェニレ
ンサルファイド繊維を仮撚加工することにより、下記■
〜■の条件を同時に満足するポリフェニレンサルファイ
ド仮撚加工系。Furthermore, according to another aspect of the present invention, by false-twisting the polyphenylene sulfide fibers described above, the following
A polyphenylene sulfide false-twisting system that simultaneously satisfies the conditions of ~■.
■ 該仮撚加工糸は、温度３２０℃、剪断速度（■）
１０００ｓｅｃ−’での溶融粘度（Ｍ■１ｏｏｏ）が７
００〜１２００ポイズであり、温度３２０°Ｃ１剪断速
度３０００ｓｅｃ−１での′／８融粘度（ＭＶ３０００
）が６００ポイズ以上であり、かつ、該溶融粘度差（Ｍ
Ｖ Ｍ Ｖ ３ｏｏ□ ）が２００ポイズ以下
であるような線状ポリフェニレンサルファイドからなる
こと。■ The false twisted yarn has a temperature of 320°C and a shear rate (■).
Melt viscosity (M 1ooo) at 1000sec-' is 7
00 to 1200 poise, and the melt viscosity (MV3000
) is 600 poise or more, and the melt viscosity difference (M
It is made of linear polyphenylene sulfide having a V M V 3oo□ of 200 poise or less.
■ 捲縮率（’ｒＣ）力着０％以上、収縮率（Ｆｓ）が
１０％以下９強度（Ｓｔ）が２．０ ｇ／ｄｅ以上。■ Crimp ratio ('rC): 0% or more, shrinkage ratio (Fs): 10% or less; 9 Strength (St): 2.0 g/de or more.
シルクファクター（ＳＦ）が１０以上であること。Silk factor (SF) must be 10 or more.
この点について述べると、従来、ポリフェニレンサルフ
ァイド繊維について強伸度と製糸性を両立させるような
提案がなかつたことは、前述の通りであり、ましてやこ
の繊維の仮撚加工糸について皆無である。Regarding this point, as mentioned above, there has been no proposal to achieve both strength and elongation and spinnability for polyphenylene sulfide fibers, and even less for false twisted yarns of this fiber.
ポリフェニレンサルファイドのｍｕ化に関しては、ポリ
マー面及び製糸技術面の両面において、まだまだ未熟で
あり、従って、工業的に生産可能な仮撚加工技術となる
と、従来の技術では、実質的不可能なためである。つま
り、従来の技術の組み合せても（１）仮撚加工にはなり
得るが、毛羽・断糸が多く生産技術として採用できない
、（１１）物性面（例えば、捲縮性能・力学的性能）で
も不充分であり、実用上必要な高物性と高生産性の両立
が不可能であったためである。そのなめ、ポリフェニレ
ンサルファイド繊維の嵩高糸の工業的製品の形態として
は、ステープルファイバーがあるのみであった。しかし
、ステープルファイバーの場合は、そのままでは、使用
する事が出来ず、事後に必ず紡績が必要であり、工程的
にも長くなる欠点があった。又、嵩高性の面でもより高
いものが必要であった。それゆえ、通常の汎用ポリマー
（例えば、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、ナイロン−６等）の長繊維の形で採用
されているのが現状である。従って、長繊維をそのまま
仮撚加工して嵩高糸を得る、工業的技術の確立が強く要
望されていたわけである。With regard to making polyphenylene sulfide into mu, it is still in its infancy in terms of both the polymer and the spinning technology.Therefore, it is virtually impossible to create a false twisting technology that can be produced industrially using conventional technology. be. In other words, even if the conventional techniques are combined, (1) false twisting can be achieved, but there are too many fluffs and yarn breaks that make it impossible to use as a production technique, and (11) physical properties (for example, crimp performance and mechanical performance) are also poor. This is because it was insufficient and it was impossible to achieve both the high physical properties and high productivity required for practical use. For this reason, staple fibers have been the only industrial product form of bulky yarns made of polyphenylene sulfide fibers. However, in the case of staple fibers, they cannot be used as they are, and must be spun afterward, which has the drawback of lengthening the process. In addition, there was a need for something with higher bulkiness. Therefore, it is currently employed in the form of long fibers of ordinary general-purpose polymers (eg, polyethylene terephthalate, polybutylene terephthalate, nylon-6, etc.). Therefore, there has been a strong demand for the establishment of an industrial technique for obtaining bulky yarns by false twisting long fibers as they are.
本発明で得られるポリフェニレンサルファイド仮撚加工
糸は捲縮率（’ｒ’ｃ）が１０％以上、収縮率（Ｆｓ）
が１０％以下という１憂れた特性を有する。The polyphenylene sulfide false twisted yarn obtained by the present invention has a crimp rate ('r'c) of 10% or more and a shrinkage rate (Fs)
It has one worrying characteristic of being less than 10%.
捲縮率（’Ｉ” ｃ ）は、嵩高性の目安であり、本発
明の仮撚加工糸は、１０％以上、好ましくは１５〜３５
％の高い値を安定して保有するものである。The crimp ratio ('I"c) is a measure of bulkiness, and the false twisted yarn of the present invention has a crimp ratio of 10% or more, preferably 15 to 35%.
It is a stable holding of a high value of %.
捲縮率（Ｔｃ）が１０％未満の場合は、嵩高性が低く、
好ましくない、又、本発明の仮撚加工糸は収縮率（Ｆｓ
）が１０％以下、好ましくは７％以下と、寸法安定性が
極めて優れている。When the crimp ratio (Tc) is less than 10%, the bulkiness is low;
The shrinkage rate (Fs
) is 10% or less, preferably 7% or less, and the dimensional stability is extremely excellent.
一方、本発明の仮撚加工糸の機械的特性は、強度２．０
ｇ／ｄｅ以上シルクファクターが１０以上である。On the other hand, the mechanical properties of the false twisted yarn of the present invention have a strength of 2.0
g/de or more and the silk factor is 10 or more.
力学的性質、例えば強度は、織編物の引き裂き強力に影
響を及ぼす重要な因子である。すなわち、高強度な繊維
程、織編物の軽量化という面で有利な事は言うまでもな
い、一方、シルクファクターが小さい繊維の場合は、高
強度繊維を得るためには、伸度をかなり小さくしなけれ
ばならず、毛羽等が発生し品位の面で問題が発生し、し
かも、生産工程では、断糸が多発し、工業的生産は困難
である。これに対して、本発明で得られるポリフェニレ
ンサルファイド仮撚加工糸はシルクファクターが１０以
上と大きいため、伸度を例えば、２０〜３０％と比較的
残す設定でも強度が２．０ｇ／ｄｅ以上の加工糸を得る
事が出来るため、工業的生産が可能となるわけである。Mechanical properties, such as strength, are important factors that affect the tear strength of woven or knitted materials. In other words, it goes without saying that the higher the strength of the fiber, the more advantageous it is in terms of reducing the weight of woven or knitted products.On the other hand, in the case of fibers with a small silk factor, in order to obtain high strength fibers, the elongation must be considerably reduced. Not only that, fluff and the like occur, causing problems in terms of quality, and moreover, yarn breakage occurs frequently during the production process, making industrial production difficult. On the other hand, the polyphenylene sulfide false twisted yarn obtained in the present invention has a large silk factor of 10 or more, so even if the elongation is set to remain relatively high at, for example, 20 to 30%, the strength is 2.0 g/de or more. Since processed yarn can be obtained, industrial production becomes possible.
このような仮撚加工糸の用途としては、その「ｎ熱・耐
薬品性を生かした産業用資材（例えば、１（熱・耐薬品
性フィルター等）分野がある。その際織物の仕上げ過程
で、高温処理するため、繊維自体の収縮率を小さくしな
いと、布帛にシボあるいはスジが入り、性能・品位共に
低下する。一方、収縮率を下げる目的で仮撚加工での加
工温度を高温にすると、ポリマーの溶融粘度特性が本発
明の領域以外の場合は、毛羽・断糸が多発して工業的生
産にはなり得ないのである。Applications of such false twisted yarn include industrial materials that take advantage of its heat and chemical resistance (for example, 1 (heat and chemical resistant filters, etc.). , because of the high temperature treatment, if the shrinkage rate of the fiber itself is not reduced, wrinkles or streaks will appear in the fabric, reducing both performance and quality.On the other hand, if the processing temperature during false twisting is increased to lower the shrinkage rate, If the melt viscosity characteristics of the polymer are outside the range of the present invention, fluffing and yarn breakage will occur frequently and industrial production will not be possible.
すなわち、溶融粘度差（Ｍ■１ｏｏｏ−Ｍ■３ｏｏ０）
の値が、２００ポイズを越える場合は、目標とする高生
産・高物性を有するポリフェニレンサルファイド仮撚加
工糸を得る事は出来ない、つまりこの場合、高分子銀の
直線性が良くないため、（１）物性面で充分なものを得
る事が出来ない（［ｌ）仮撚加工性が不良であり、毛羽
及び断糸が多発する等の欠点があり、好ましくない、尚
、Ｍ■３ｏｏｏの値は、重合度、直線性の関係で、６０
０ポイズ以上は必要である。すなわち、Ｍ■３ｏｏｏが
６００ポイズ未満の時は、重合度か著しく低いか：ある
いは直線性が極めて悪いため、目標とする高生産性及び
高特性を兼備したポリフェニレンサルファイド仮撚加工
糸を得る事ができない。That is, the melt viscosity difference (M■1ooo-M■3oo0)
If the value of exceeds 200 poise, it is not possible to obtain polyphenylene sulfide false-twisted yarn with the target high productivity and high physical properties.In other words, in this case, the linearity of polymeric silver is not good, 1) It is not possible to obtain sufficient physical properties ([l) There are disadvantages such as poor false twisting processability and frequent fluffing and yarn breakage, etc., which is undesirable, and the value of M■3ooo is 60 due to the degree of polymerization and linearity.
0 poise or more is required. In other words, when M■3ooo is less than 600 poise, the degree of polymerization is extremely low, or the linearity is extremely poor, making it difficult to obtain a polyphenylene sulfide false twisted yarn that has the targeted high productivity and high properties. Can not.
上記の優れた特性を発揮させるためには、紡糸の際紡糸
口金温度を３１０〜３３０℃に設定する事が、大切であ
る１口金面温度かが３１０°Ｃ未満の時は、口金面温度
が低過ぎるため、毛羽が多くなり目的とする高生産性・
高物性の仮撚加工糸を得る事は出来ない、一方、口金面
温度が３３０℃を越える場合は、温度が高過ぎ、繊維の
着色化が進み、紡糸性の低下、更には延伸性及び仮撚加
工性も低下し、好ましくない。In order to exhibit the above excellent properties, it is important to set the spinneret temperature at 310 to 330°C during spinning.If the spinneret surface temperature is less than 310°C, If the temperature is too low, there will be a lot of fuzz and the desired high productivity/
It is not possible to obtain a false twisted yarn with high physical properties. On the other hand, if the spindle surface temperature exceeds 330°C, the temperature is too high and the coloring of the fibers progresses, resulting in a decrease in spinnability and even lower drawability and false twisting. Twisting workability also deteriorates, which is not preferable.
又、紡糸速度は１０００ｍ／分未満、好ましくは、３０
０〜８００ ｍ／分が良い、紡糸速度が１０００ｒｎ／
分を越える場合は、（１）得られる仮撚加工糸の強度が
充分でない、（Ｉｆ）仮撚工程での糸切れが多発する、
■又は、毛羽も出やすい、という不利益がある。Also, the spinning speed is less than 1000 m/min, preferably 30 m/min.
0 to 800 m/min is good, spinning speed is 1000rn/
If the time exceeds 10 minutes, (1) the resulting false-twisted yarn will not have sufficient strength, (If) the yarn will break frequently during the false-twisting process.
■Also, there is a disadvantage that fuzz is likely to appear.
尚、紡糸速度が３００ｍ／分未満の場合は、生産性が低
くなる。Note that if the spinning speed is less than 300 m/min, productivity will be low.
延伸・熱処理操作であるが、本発明においては、延伸熱
処理を一度で行なうのではなく、−度、１５０℃未満の
温度での延伸で配向結晶化させてから、１５０°Ｃ以上
の温度で熱処理する方法が好ましい、又延伸速度も必ず
しも制限されるものではなく、通常の延伸温度、例えば
、１００〜８００ｍ／分程度を採用すればよい。Regarding the stretching and heat treatment operations, in the present invention, the stretching heat treatment is not carried out all at once, but after stretching at a temperature of -150°C or less to crystallize the orientation, the heat treatment is performed at a temperature of 150°C or higher. The method of stretching is preferred, and the stretching speed is not necessarily limited, and a normal stretching temperature, for example, about 100 to 800 m/min may be adopted.
次に、仮撚加工方法であるが、前述の如く、本発明で、
使用する未延伸糸は、紡糸速度が１０００ｍ／分未満で
捲き取られるため、その破断伸度が極めて大きいので、
Ｉｎ−Ｄｒａｗ方式（延伸と仮撚とを同時に行なう）は
困難であり、Ｏｕｔ Ｄｒａｗ方式（延伸後板撚加工）
を採用する事が大切である。Next, regarding the false twisting method, as mentioned above, in the present invention,
Since the undrawn yarn used is wound at a spinning speed of less than 1000 m/min, its elongation at break is extremely high.
The In-Draw method (drawing and false twisting are performed at the same time) is difficult, and the Out-Draw method (sheet twisting after stretching) is difficult.
It is important to employ
仮撚加工の装置・条件については、汎用素材であるポリ
エチレンテレフタレートのそれを採用する事が出来、例
えば、加工速度１００ｍ／分、加工温度１８０〜２４０
℃程度で、有用な仮撚加工糸を得る事が出来る。Regarding the equipment and conditions for false twisting, those for polyethylene terephthalate, which is a general-purpose material, can be adopted, for example, processing speed 100 m/min, processing temperature 180-240 m/min.
Useful false twisted yarn can be obtained at temperatures around ℃.
（作用効果）
ポリフェニレンサルファイドは、耐熱性・耐薬品性に優
れたポリマーであり、その１ＩｊＪ維化についても数多
くの報告がなされていることは前述の通りである。(Effects) Polyphenylene sulfide is a polymer with excellent heat resistance and chemical resistance, and as described above, there have been many reports regarding its 1IjJ fibrillation.
しかしながら、高物性を有し、しかも、工業的に高生産
性を有する製造技術については、未だ実現されていなか
ったか、本発明により、実用繊維という観点からは、（
１）強度４．０ｇ／ｄｅ以上、シルクファクター２０以
上という優れた力学的性質、■１８０℃での乾熱収縮率
が１５％以下という優れた寸法安定性が、実現され、更
に生産技術という観点からは、（１）紡糸時のバック内
の圧力上昇（濾過抵抗圧力上昇）が小さくて、連続運転
可能である、ａ）紡糸・延伸時の断糸・単糸切れがなく
なる、（１）紡糸速度及び延伸速度が充分に高く、生産
効率が良い、といったことが、又、品質という観点から
は、（１）品質変動が少ない、（！ｉ）毛羽がないとい
った工業的に生産する上での厳しい要求が全て満足され
る。However, a manufacturing technology with high physical properties and high industrial productivity has not yet been realized, or the present invention has made it possible to achieve (
1) Excellent mechanical properties such as a strength of 4.0 g/de or more and a silk factor of 20 or more; ■ Excellent dimensional stability with a dry heat shrinkage rate of 15% or less at 180°C, and from the perspective of production technology. (1) The pressure increase in the bag during spinning (filtration resistance pressure increase) is small and continuous operation is possible; a) There is no yarn breakage or single yarn breakage during spinning or drawing; (1) Spinning In addition, from the perspective of quality, the speed and drawing speed are sufficiently high and the production efficiency is good. All strict requirements are met.
しかも、本発明においては、単繊維の繊度（デニール）
が１〜２ｄｅと極めて細いものまでも適用できるところ
に大きな特徴がある。勿論、単糸繊度が２ｄｅ以上の太
い繊維について適用できるのは、言うまでもない。又、
フィラメント数についても、ハイマルチ化が可能であり
、例えば１００〜１５０ｆ ｉ ｌのマルチフィラメン
トにも適用できる。フィラメントの断面形状は丸断面、
中実糸の場合が多いが、必ずしもこれに制限されるわけ
ではなく、必要に応じて、異形断面糸、更には中空糸に
も適用しても、何ら問題はない。勿論本発明は、長繊維
、その仮撚加工糸だけでなく、短繊維の製造に際しても
適用できる。尚、上記の生糸、仮撚糸は長・短繊維を問
わずば耐熱性を要求されるミシン糸の全成分または一成
分としても有用である。Moreover, in the present invention, the fineness (denier) of the single fiber
A major feature is that it can be applied even to extremely thin objects of 1 to 2 de. Of course, it goes without saying that this method can be applied to thick fibers having a single filament fineness of 2 de or more. or,
As for the number of filaments, high multifilament is possible, for example, it is applicable to multifilaments of 100 to 150 filaments. The cross-sectional shape of the filament is round,
Although it is often a solid yarn, it is not necessarily limited to this, and if necessary, it may be applied to irregular cross-section yarns or even hollow fibers without any problem. Of course, the present invention can be applied not only to long fibers and their false twisted yarns, but also to the production of short fibers. Incidentally, the above-mentioned raw silk and false twisted yarn, regardless of whether they are long or short fibers, are useful as all or one component of sewing thread which requires heat resistance.
［実施例］
以下、本発明を実施例により更に説明する１本実施例に
おいて、用いる物性は、下記の方法で測定したものであ
る。[Example] Hereinafter, the present invention will be further explained with reference to examples.In this example, the physical properties used were measured by the following methods.
（１）ポリマーの粘度特性（Ｍ Ｖ 、 Ｍ Ｖ
３０００ ）島原＠製降下式フロテスターを用いた。試
料量５ ｇ、ノズル寸法０．５φＸ ４ ｍｎ 、 ド
ラム回転数１ ｒｐｍ 、荷重２０〜１００ ｋｇ＋温
度３２０°Ｃの条件で測定し、ＦｇＭｔ粘度（ＭＶ）を
算出した。次いで、両対数グラフを用いて、粘度（ＭＶ
）と剪断速度（γ）との関係をグラフ化し、剪断速度（
−ｒ） １０００ｓｅｃ−１及び剪断速度（？ ） ３
０００５ｅＣ−１で？８＠粘度を読み取った。(1) Polymer viscosity characteristics (M V , M V
3000) A descending type float tester manufactured by Shimabara@ was used. The FgMt viscosity (MV) was calculated by measuring under the conditions of a sample amount of 5 g, a nozzle size of 0.5φ×4 mn, a drum rotation speed of 1 rpm, a load of 20 to 100 kg, and a temperature of 320°C. Then, using a log-log graph, the viscosity (MV
) and shear rate (γ).
-r) 1000sec-1 and shear rate (?) 3
With 0005eC-1? 8 @ Viscosity was read.
（２）強度（Ｓｔ）、伸度ＣＥＩ ）
通常の引っ張り型試験機にて、室温２５℃、温度６０％
で試料長１０■、引っ張り速度２００ｍｍ／分の条件で
応力−伸度曲線を求め、応力が最大となる点の伸度（Ｅ
りを読み取った。又、最大応力を試料の繊度で割った値
を強度（Ｓｔ）とした。(2) Strength (St), elongation CEI) At room temperature 25℃, temperature 60% using a normal tensile tester.
Obtain the stress-elongation curve under the conditions of sample length 10 cm and pulling speed 200 mm/min, and calculate the elongation (E) at the point where the stress is maximum.
I read it. Moreover, the value obtained by dividing the maximum stress by the fineness of the sample was defined as the strength (St).
（３乾熱収縮率
マルチフィラメントの「カセ」を作り、１８０°Ｃに設
定した乾燥機内で、３０分間、無荷重下で処理した時の
収縮率を以下の式より求めた。(3. Dry heat shrinkage rate) The shrinkage rate when a multifilament "skein" was made and processed under no load for 30 minutes in a dryer set at 180°C was determined from the following formula.
ｌａ ｉ工
収縮率（％） ＝ −ｘ １００
！０
（４） シルクファクター（ＳＦ）
（２）で求めた強度（Ｓｔ）と伸度（Ｅりの値を用いて
、以下の式より求めた。la i engineering shrinkage rate (%) = -x 100! 0 (4) Silk factor (SF) It was determined from the following formula using the values of strength (St) and elongation (E) determined in (2).
５Ｆ＝Ｓｔ （ｇ／ｄｅ）ｘＦ■Ｔ（％）（５） 断
糸・単糸切れ状況
紡糸・延伸時の断糸・単糸切れを状況を肉眼で観察し、
定性的に評価した。5F=St (g/de) x F T (%) (5) Situation of yarn breakage and single yarn breakage Visually observe the situation of yarn breakage and single yarn breakage during spinning and drawing.
Evaluated qualitatively.
（ａ 毛羽１発生状況
ボビンに捲かれた、未延伸糸・および延伸糸の表面を肉
眼で観察し、定性的に評価した。(a) Status of fuzz 1 occurrence The surfaces of the undrawn yarn and drawn yarn wound around the bobbin were observed with the naked eye and qualitatively evaluated.
（７）捲縮率（’Ｔ’ｃ）
捲縮フィラメン１〜の「カセ」をつくり、この「カセ」
に軽荷重（２■／デニール）及び重荷重（２００＋ｕｒ
／デニール）をかけた時の長さを１ｏ、次いで軽荷重下
で沸騰水中で３０分処理し、荷重を除去して、自然乾燥
ｆ＆（２４ｈｒ後）軽荷重及び重荷重をかけた時の長さ
を１１１次いで、軽荷重下のみの長さを１２として、以
下の式より求めた。(7) Crimp rate ('T'c) Make a "skein" of crimped filament 1~, and make this "skein"
Light load (2■/denier) and heavy load (200+ur)
/ denier) is 1o, then treated in boiling water for 30 minutes under a light load, the load is removed, and air dried f & (after 24 hours) the length when a light load and a heavy load are applied. The length was set to 111, and the length only under light load was set to 12, and the length was determined from the following formula.
ｌｘ １２
捲縮率（’Ｔ’ Ｃ） ＝ −Ｘ １００！ ０
（８）収縮率（％）
マルチフィラメントの「カセＪをつくり、この「カセ」
に軽荷重（２Ｎ／デニール）１重荷重（０，２■／デニ
ール）をかけた時の長さをＲｏ、次いで軽荷重下で沸騰
水中で３０分処理し、荷重を取って自然乾燥後（２４ｈ
ｒ後）、再び軽荷重及び重荷重をかけた時の長さを２１
とし、以下の式より求めた。lx 12 Crimp rate ('T' C) = -X 100! 0 (8) Shrinkage rate (%) Make a multifilament ``skein J'' and
The length when a light load (2N/denier) and one heavy load (0,2■/denier) is applied to Ro is then treated in boiling water for 30 minutes under a light load, after removing the load and air drying ( 24 hours
r), the length when applying a light load and a heavy load again is 21
It was calculated using the following formula.
ｌａ ｌｌ
収縮率（Ｆ Ｓ ） ＝ −ｘ １００（９）仮撚加工
時の断糸状況
仮撚加工での糸切れ状況を肉眼で観察し、定性的に評価
した。la ll Shrinkage rate (FS) = -x 100 (9) Yarn breakage during false twisting The yarn breakage during false twisting was visually observed and qualitatively evaluated.
（財）仮撚加工時の毛羽発生状況
ボビンに捲かれた、仮撚加工糸の表面を肉眼で観察し、
定性的に評価した。(Foundation) Condition of fuzz generation during false twisting The surface of the false twisted yarn wound around the bobbin was observed with the naked eye.
Evaluated qualitatively.
旧） 仮撚加工 仮撚加工は、スピンドル型の仮撚加工機を使用した。Old) False twisting A spindle type false twisting machine was used for the false twisting process.
（ａ）撚係数（α）
以下の式で表わされる撚数（Ｔ ／ ｍ ）の時、撚係
数α−１と定義した。(a) Twisting coefficient (α) When the number of twists (T/m) is expressed by the following formula, the twisting coefficient is defined as α-1.
撚数（Ｔ／ｍ）＝−
Ｓ璽
撚係数α−０，８５とは、上記撚数に０．８５を重しな
撚数を言う。Number of twists (T/m)=-S twist coefficient α-0.85 refers to the number of twists that is the above twist number plus 0.85.
（Ｂ） ０ｖｅｒ Ｆｅｅｄ （％）ヒーターを介し
て存在する、２つのローラーの周速比の大小で、例えば
： ｏｖｅｒ Ｆｅｅｄ ２％とは、第１０−ラーの周
速が第２０−ラーの周速より２％大きいことを示す。(B) 0ver Feed (%) The size of the circumferential speed ratio of two rollers that exist via the heater, for example: over Feed 2% means that the circumferential speed of the 10th roller is the same as the circumferential speed of the 20th roller. 2% larger than
［実施例１〜５．比較例１〜６］
Ａ、ポリマーの合成
（１）後記の表−１中、比較例−２、比較例−３〜４お
よび実施例−１〜５で用いる、ＭＶ１０００−８７０Ｐ
ｏｉｓａ、 ＭＶ ＝６８０Ｐｏｉｓｅ、 ＭＶ、
ｏｏｏ−ＭＶ３ｏｏｏ＝１９０ポイズノ；ｔ？’Ｊ７−
合成：硫化ナトリウム９５．４ｇ、酢酸リチウム２水和
物７６．５ｇ 、 ＮＭＰ （Ｎ−メチルピロリドン）
１８５ｇ、水１４ｇをガラスフラスコに仕込み、２１０
°Ｃで２時間処理し、留出物を４４ＣＣ生じさせた。[Examples 1-5. Comparative Examples 1 to 6] A. Synthesis of Polymer (1) MV1000-870P used in Comparative Example 2, Comparative Examples 3 to 4, and Examples 1 to 5 in Table 1 below
oisa, MV =680Poise, MV,
ooo-MV3ooo=190 poison;t? 'J7-
Synthesis: Sodium sulfide 95.4g, lithium acetate dihydrate 76.5g, NMP (N-methylpyrrolidone)
Put 185g and 14g of water into a glass flask, and make 210g.
C. for 2 hours yielding 44 cc of distillate.
次に、ＮＭＰ８０ｇ、ＤＣＢ （ジクロルベンゼン）２
２５ｇの溶液を添加し、窒素シール中で、２６０℃で４
時間加熱した（圧力は５ ｋｇ／ ｃｓｊ ）。Next, 80 g of NMP, 2 DCB (dichlorobenzene)
Add 25g of solution and heat at 260°C under nitrogen blanket for 4 hours.
(pressure is 5 kg/csj).
次いで生成物を熱水で１０回洗浄し、乾燥し、チップ化
した。The product was then washed 10 times with hot water, dried and chipped.
（２）後記の表−１中、比較例−１で用いる、ＭＶ
＝５８０ポイズ、 Ｍ Ｖ ３ｏｏｏ＝ ４５０ポイ
ズ１ＭＶ−Ｍｖ３ｏｏｏ−１３０ポイズのポリマー合成
：
上記（１）の合成法において、重合時間を３時間とした
以外は、同様の処法により試料を得た。(2) MV used in Comparative Example-1 in Table-1 below
=580 poise, MV3ooo=450 poise Polymer synthesis of 1MV-Mv3ooo-130 poise: A sample was obtained by the same method as in the synthesis method (1) above except that the polymerization time was changed to 3 hours.
（ａ 後記の表−１中、比較例−５で用いるＭ Ｖ
＝ １３００ポイズ、ＭＶ３ｏｏＯ＝１１５０ポイズ
。(a In Table 1 below, MV used in Comparative Example 5
= 1300 poise, MV3ooO=1150 poise.
Ｍｖ −Ｍ■３ｏｏｏ＝１５０ポイズポリマーの合成
：
上記（１）の合成法において、硫化ナトリウムの量を９
８「とじ且つ、重合時間を５時間とした以外は、同様の
処法により試料を得た。Mv −M■3ooo=150 Synthesis of poise polymer: In the synthesis method of (1) above, the amount of sodium sulfide was changed to 9
Samples were obtained using the same procedure except for binding and polymerization time of 5 hours.
（４）後記の表−１中、比較例−６で用いる、ＭＶ
＝７５０ポイズ、ＭＶ３ｏｏｏ−５１０ポイズ。(4) MV used in Comparative Example-6 in Table-1 below
=750 poise, MV3ooo-510 poise.
ＭＶ１ｏｏｏ−ＭＶ３０ｏｏ−２３０ポイズのポリマー
合成：
１．５１のＮＭＰ及び１０８４ｇのＮａ２ Ｓ −９Ｈ
２０をガラスフラスコに入れ、水和水が蒸溜されるまで
、撹拌しながら、加熱し、７７７ｇの蒸留物を除いた後
、Ｐ−ジクロルベンゼン６６２ｇを投入し、２３０°Ｃ
で１４時間加熱し、得られた固型物を熱水で洗浄し、乾
燥した。次いで、２の試料を２７０°Ｃで１゜５時間処
理した後、チップ化して紡糸用の試料とした。Polymer synthesis of MV1ooo-MV30oo-230 poise: 1.51 NMP and 1084 g Na2S-9H
20 was placed in a glass flask and heated while stirring until the water of hydration was distilled. After removing 777 g of distillate, 662 g of P-dichlorobenzene was added and the temperature was heated at 230°C.
The solid substance obtained was washed with hot water and dried. Next, the sample No. 2 was treated at 270°C for 1°5 hours, and then chipped to give a sample for spinning.
Ｂ、紡糸、延伸
Ａで得た各チップを１８０°Ｃの熱風乾燥機中で４時間
乾燥したポリフェニレンサルファイドのチップを３４０
℃で溶融し、孔径０．３５φ１ランド長０．７０市の丸
孔が１００個設置させた紡糸口金より押し出した。その
際、表−１に示すように、７８融粘度特性の異なるポリ
マーを用い、更に、口金面温度。B. Spinning and stretching polyphenylene sulfide chips obtained by drying each chip obtained in A for 4 hours in a hot air dryer at 180°C.
It was melted at ℃ and extruded from a spinneret equipped with 100 round holes with a hole diameter of 0.35φ and a land length of 0.70 mm. At that time, as shown in Table 1, 78 polymers with different melt viscosity characteristics were used, and the mouth surface temperature was also adjusted.
紡糸速度、及び延伸後２００ｄｅ ／１００ｆｉｌにな
るように、吐出量を変更して行った。引き続き押し出さ
れたポリマー流を冷却固化させ、油剤を付与させた後、
捲きとった。The spinning speed and the discharge amount were changed so that the spinning speed was 200 de/100 fil after stretching. After cooling and solidifying the extruded polymer stream and applying an oil agent,
I turned it over.
次に、得られた未延伸糸を、表面温度か１００″Ｃ及び
１２０℃のローラー間で延伸を行ない、次いで表面ロー
ラー温度が２１０°Ｃのローラーで熱処理を行なった後
、冷却ローラーを通して、３５０ｍ／分の速度で捲き取
った。尚、各実験における全延伸倍率は表−１に示す、
又、得られた繊維の物性。Next, the obtained undrawn yarn was drawn between rollers with a surface temperature of 100"C and 120°C, then heat treated with a roller with a surface roller temperature of 210"C, and then passed through cooling rollers for 350 m It was rolled up at a speed of /min.The total stretching ratio in each experiment is shown in Table-1.
Also, the physical properties of the obtained fibers.
断糸・単糸・糸切れ状況及び毛羽の発生状況を表−２に
示す。Table 2 shows the yarn breakage, single yarn, yarn breakage, and occurrence of fuzz.
比較例−１では、用いたポリマーの重合度が低いなめ、
強度及びシルクファクターが低いものであった。又、延
伸時の断糸及び単糸切れが多く毛羽の発生ら多かった。In Comparative Example-1, the degree of polymerization of the polymer used was low;
The strength and silk factor were low. Furthermore, there were many yarn breaks and single yarn breakages during drawing, and there was a lot of fuzz.
比較例−２では、ポリマーの溶融粘度特性は好ましいが
、紡糸時の口金面温度が低いため、力学的性質も弱糸的
傾向を示し、又、紡糸、延伸性の面で改善の余地があり
、毛羽も多少存在した。実施例−１〜５は、本発明の好
ましい例であり、繊維物性は優れたものであり、又、紡
糸・延伸時の断糸・単糸切れが極皆無で、毛羽の発生も
ほとんど見られなかった。In Comparative Example 2, the melt viscosity characteristics of the polymer are favorable, but the mechanical properties tend to be weak due to the low spinneret surface temperature during spinning, and there is room for improvement in terms of spinning and drawing properties. , some fluff was also present. Examples 1 to 5 are preferred examples of the present invention, and the fiber properties are excellent, and there is extremely no yarn breakage or single yarn breakage during spinning and drawing, and almost no fuzz is observed. There wasn't.
比較例−３では、ポリマーの溶融粘度特性は好ましいが
、紡糸時の［１金面温度が高過ぎるため、吐出されたａ
維の着色の程度が大きく、紡糸・延伸中での単糸切れが
目立った。In Comparative Example 3, although the melt viscosity characteristics of the polymer were favorable, the [1 metal surface temperature during spinning was too high, so the ejected a
The degree of coloration of the fibers was large, and single fiber breakage during spinning and drawing was noticeable.
比較例−４では、ポリマーの溶融粘度特性は好ましいか
、紡糸速度が高過ぎるため、断糸・単糸切れが多発し、
又、毛羽も多かった。In Comparative Example-4, whether the melt viscosity characteristics of the polymer were favorable or because the spinning speed was too high, yarn breakage and single yarn breakage occurred frequently.
Also, there was a lot of fluff.
比較例−５では、繊維物性は良好であるが、ポリマーの
溶融粘度が高過ぎ、延伸時の単糸切れ、毛羽の発生が多
かった。In Comparative Example 5, the fiber properties were good, but the melt viscosity of the polymer was too high, and single filament breakage and fluffing occurred frequently during drawing.
比較例−６では、（ＭＶ −ＭＶ ）の値が大
きく、直線性が不良であるポリマーのため、強度及び伸
度更にシルクファクターの変動が極めて大きかった。又
、延伸時の単糸切れ及び断糸が極めて多く、毛羽も多か
った。In Comparative Example 6, since the polymer had a large value of (MV - MV ) and poor linearity, fluctuations in strength, elongation, and silk factor were extremely large. Furthermore, there were extremely many single yarn breakages and yarn breakages during drawing, and there was also a lot of fuzz.
尚、本発明で述べている断糸・単糸切れ・毛羽の発生状
況は以下の定義による。Incidentally, the occurrence of yarn breakage, single yarn breakage, and fluff described in the present invention is based on the following definitions.
［ｌ！ｙｉ糸発生］
Ａ、紡糸での断糸
Ｂ、延伸での断糸
［、× ： ツノ
１） ３ 回置上［単糸切
れ］
Ａ、紡糸での単糸切れ
Ｂ、延伸での単糸切れ
［毛羽状況］
未延伸糸・延伸糸共
［実施例６及び比較例７］
表−２に示す各延伸糸を以下の条件で仮撚加工した。[l! yi yarn occurrence] A, Yarn breakage during spinning B, Yarn breakage during drawing [, ×: Horn
1) 3 turns [Single yarn breakage] A, Single yarn breakage during spinning B, Single yarn breakage during drawing [Fuzz condition] Both undrawn yarn and drawn yarn [Example 6 and Comparative Example 7] Table-2 Each drawn yarn shown in was subjected to false twisting under the following conditions.
（仮撚条件）
表−３
本 比較の１−６の延伸糸は、力学・性質（強（ｌｌｔ
文）が変量Ｎ゛る。(False twisting conditions) Table 3 The comparative drawn yarns 1-6 have mechanical properties (strong
sentence) has N variables.
比較例−１の延伸糸の場合は、捲縮特性は良好であった
が、用いたポリマーの重合度が低いため強度及びシルク
ファクターが低いものであった。In the case of the drawn yarn of Comparative Example 1, the crimp properties were good, but the strength and silk factor were low because the degree of polymerization of the polymer used was low.
又、仮撚加工時の断糸が多く、得られる加工糸の毛羽は
多かった。Furthermore, there were many yarn breaks during false twisting, and the resulting processed yarn had a lot of fuzz.
比較例−２の延伸糸の場合は、用いたポリマーの溶融粘
度特性は好ましいが、紡糸時の口金面温度が低いため、
紡糸・延伸時の毛羽か多く、引き続き行った仮撚加工で
は、断糸・毛羽の点で改良の余地があった。In the case of the drawn yarn of Comparative Example-2, although the melt viscosity characteristics of the polymer used were favorable, the spinneret surface temperature during spinning was low;
There was a lot of fuzz during spinning and drawing, and there was room for improvement in terms of yarn breakage and fuzz in the subsequent false twisting process.
実施例１〜５の延伸糸の場合は、本発明の好ましい例で
あり、捲縮性能は勿論、力学的性質も満足できる状態で
あった。又、仮撚加工時の断糸は皆無で毛羽の発生も見
られなかった。The drawn yarns of Examples 1 to 5 are preferred examples of the present invention, and were satisfactory not only in crimp performance but also in mechanical properties. Furthermore, there was no yarn breakage during false twisting, and no fuzz was observed.
比較例−３の延伸糸の場合は、ポリマーの粘度特性は好
ましいが、紡糸時の口金温度が高過ぎるため、吐出され
た繊維が劣化気味で着色の程度が大きく、紡糸・延伸時
の毛羽が目立ち、引き続いて行った仮撚加工では、断糸
・毛羽が多少多かった。In the case of the drawn yarn of Comparative Example 3, the viscosity characteristics of the polymer are favorable, but because the spinneret temperature during spinning is too high, the discharged fibers are slightly deteriorated and have a large degree of coloring, and the fluff during spinning and drawing is poor. This was noticeable, and during the subsequent false twisting process, there were some yarn breaks and fuzz.
比較例−４の延伸糸の場合は、紡糸速度が高過ぎるなめ
、原糸（未延伸糸）の段階で毛羽が目立ち、仮撚加工で
は、断糸・毛羽が多発した。In the case of the drawn yarn of Comparative Example 4, the spinning speed was too high, fuzz was noticeable at the stage of raw yarn (undrawn yarn), and yarn breakage and fuzz occurred frequently during false twisting.
比較例−５の延伸糸の場合は、ポリマーの溶融粘度が高
過ぎて、繊維物性は良好であるが、延伸時の単糸切れが
多少多く、引き続き行った仮撚加工では、断糸・毛羽の
点で改良の余地があった。In the case of the drawn yarn of Comparative Example 5, the melt viscosity of the polymer is too high, and the fiber properties are good, but there are a few single fiber breakages during drawing, and the subsequent false twisting process causes yarn breakage and fluffing. There was room for improvement in this respect.
比較例−６の延伸糸の場合は（ＭＶｔｏｏｏ ＭＶ３
０００ ）の差が大きく、直線性が不良であるため、延
伸性が極めて悪く、引き続いて行った仮撚加工では、断
糸が多発し、毛羽も極めて多かった。In the case of the drawn yarn of Comparative Example-6 (MVtoo MV3
000), and the linearity was poor, resulting in extremely poor stretchability, and during the subsequent false twisting process, yarn breakage occurred frequently and there was an extremely large amount of fuzz.
尚、本発明で述べている、断糸・毛羽の発生状況は、以
下の定義による。Incidentally, the occurrence of yarn breakage and fluff described in the present invention is based on the following definition.
［断糸発生］ ［毛羽発生状況］ しＸ・繊維が解舒できない程大きい。[Thread breakage] [Fuzz generation status] ・The fiber is so large that it cannot be unwound.
Claims (3)
特徴とするポリフェニレンサルファイド繊維。 ［１］該繊維は、温度３２０℃、剪断速度（■）１００
０ｓｅｃ＾−＾１での溶融粘度（ＭＶ＿１＿０＿０＿０
）が７００〜１２００ポイズであり、温度３２０℃、剪
断速度（■）３０００ｓｅｃ＾−＾１での溶融粘度（Ｍ
Ｖ＿３＿０＿０＿０）が６００ポイズ以上であり、かつ
、該溶融粘度差（ＭＶ＿１＿０＿０＿０−ＭＶ＿３＿０
＿０＿０）が２００ポイズ以下であるような線状ポリフ
ェニレンサルファイドからなること。 ［２］繊維強度（Ｓｔ）が４．０ｇ／ｄｅ以上、シルク
ファクター（ＳＦ）が２０以上であること。 〔シルクファクター（ＳＦ）は、繊維強度（Ｓｔ）、繊
維伸度（Ｅｌ）より、以下の式で求めたものを表わす。 ＳＦ＝Ｓｔ（ｇ／ｄｅ）×√Ｅｌ（％）〕 ［３］温度１８０℃での乾熱収縮率（ＨＳ）が１５％以
下であること。(1) A polyphenylene sulfide fiber characterized by simultaneously satisfying the following conditions [1] to [3]. [1] The fiber has a temperature of 320°C and a shear rate (■) of 100
Melt viscosity at 0 sec^-^1 (MV_1_0_0_0
) is 700 to 1200 poise, and the melt viscosity (M
V_3_0_0_0) is 600 poise or more, and the melt viscosity difference (MV_1_0_0_0-MV_3_0
_0_0) is made of linear polyphenylene sulfide of 200 poise or less. [2] Fiber strength (St) is 4.0 g/de or more and silk factor (SF) is 20 or more. [Silk factor (SF) is calculated from fiber strength (St) and fiber elongation (El) using the following formula. SF=St (g/de)×√El (%)] [3] The dry heat shrinkage rate (HS) at a temperature of 180° C. is 15% or less.
サルファイドを口金温度３１０〜３３０℃、紡糸速度１
０００ｍ／分以下で紡糸し、延伸熱処理する事を特徴と
する請求項（１）記載のポリフェニレンサルファイド繊
維の製造法。 ［１］温度３２０℃、剪断速度（■）１０００ｓｅｃ＾
−＾１での溶融粘度（ＭＶ＿１＿０＿０＿０）が７００
〜１２００ポイズであり、温度３２０℃、剪断速度（■
）３０００ｓｅｃ＾−＾１での溶融粘度（ＭＶ＿３＿０
＿０＿０）が６００ポイズ以上であり、かつ、該溶融粘
度差（ＭＶ ＿１＿０＿０＿０−ＭＶ＿３＿０＿０＿０）が２００ポ
イズ以下であるような線状ポリフェニレンサルファイド
からなること。(2) Linear polyphenylene sulfide that satisfies the conditions of [1] below is spun at a spinneret temperature of 310 to 330°C and a spinning speed of 1.
2. The method for producing polyphenylene sulfide fiber according to claim 1, wherein the fiber is spun at a speed of 000 m/min or less and subjected to drawing heat treatment. [1] Temperature 320℃, shear rate (■) 1000sec^
- Melt viscosity at 1 (MV_1_0_0_0) is 700
~1200 poise, temperature 320℃, shear rate (■
) Melt viscosity at 3000sec^-^1 (MV_3_0
_0_0) is 600 poise or more, and the melt viscosity difference (MV_1_0_0_0-MV_3_0_0_0) is 200 poise or less.
特徴とするポリフェニレンサルファイド仮撚加工糸。 ［１］該仮撚加工糸は温度３２０℃剪断速度（■）１０
００ｓｅｃ＾−＾１での溶融粘度（ＭＶ＿１＿０＿０＿
０）が７００〜１２００ポイズであり、温度３２０℃、
剪断速度３０００ｓｅｃ＾−＾１での溶融粘度（ＭＶ＿
３＿０＿０＿０）が６００ポイズ以上であり、かつ、該
溶融粘度差（ＭＶ＿１＿０＿０＿０−ＭＶ＿３＿０＿０
＿０）が２００ポイズ以下であるような線状ポリフェニ
レンサルファイドからなること。 ［２］捲縮率（ＴＣ）が１０％以上、収縮率（Ｆｓ）が
１０％以下、強度（Ｓｔ）が２．０ｇ／ｄｅ以上、シル
クファクター（ＳＦ）が１０以上であること。(3) A polyphenylene sulfide false twisted yarn characterized by simultaneously satisfying the following conditions [1] to [2]. [1] The false twisted yarn has a temperature of 320°C and a shear rate (■) of 10
Melt viscosity at 00sec^-^1 (MV_1_0_0_
0) is 700 to 1200 poise, temperature is 320℃,
Melt viscosity (MV_
3_0_0_0) is 600 poise or more, and the melt viscosity difference (MV_1_0_0_0-MV_3_0_0
_0) is made of linear polyphenylene sulfide of 200 poise or less. [2] The crimp rate (TC) is 10% or more, the shrinkage rate (Fs) is 10% or less, the strength (St) is 2.0 g/de or more, and the silk factor (SF) is 10 or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5952988A JPH01239109A (en) | 1988-03-15 | 1988-03-15 | Polyphenylene sulfide fiber, its production and false-twisted yarn of said fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5952988A JPH01239109A (en) | 1988-03-15 | 1988-03-15 | Polyphenylene sulfide fiber, its production and false-twisted yarn of said fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01239109A true JPH01239109A (en) | 1989-09-25 |
Family
ID=13115893
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5952988A Pending JPH01239109A (en) | 1988-03-15 | 1988-03-15 | Polyphenylene sulfide fiber, its production and false-twisted yarn of said fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01239109A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01239132A (en) * | 1988-03-16 | 1989-09-25 | Toyobo Co Ltd | Sewing thread |
| US5178813A (en) * | 1990-03-23 | 1993-01-12 | Kureha Kagaku Kogyo K.K. | Method of producing poly(phenylene sulfide) fibers |
| US5372760A (en) * | 1992-06-18 | 1994-12-13 | Hoechst Aktiengesellschaft | Process for producing polyarylene sulfide fiber and thereby obtainable polyarylene sulfide multifilament yarn |
| JP2008540850A (en) * | 2005-03-18 | 2008-11-20 | ディオレン インドゥストリアル ファイバース ベスローテン フェノートシャップ | Method for producing polyphenylene sulfide filament yarn |
| CN102677198A (en) * | 2011-03-18 | 2012-09-19 | 四川得阳工程塑料开发有限公司 | Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology |
| WO2016104236A1 (en) * | 2014-12-22 | 2016-06-30 | 東レ株式会社 | Polyphenylene sulfide monofilament and manufacturing method therefor, and package |
| JP2019173212A (en) * | 2018-03-28 | 2019-10-10 | 帝人フロンティア株式会社 | Sea-island type conjugate fiber bundle |
| JP2020033680A (en) * | 2018-08-31 | 2020-03-05 | 帝人フロンティア株式会社 | Sea-island type composite fiber bundles, medical supplies containing its ultrafine fibers, and filters for food manufacturing processes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6175812A (en) * | 1984-08-07 | 1986-04-18 | バイエル・アクチエンゲゼルシヤフト | Polyarylsulfide fiber or filament |
| JPS61152828A (en) * | 1984-12-26 | 1986-07-11 | Kureha Chem Ind Co Ltd | Production of drawn multifilament of polyarylene sulfide |
-
1988
- 1988-03-15 JP JP5952988A patent/JPH01239109A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6175812A (en) * | 1984-08-07 | 1986-04-18 | バイエル・アクチエンゲゼルシヤフト | Polyarylsulfide fiber or filament |
| JPS61152828A (en) * | 1984-12-26 | 1986-07-11 | Kureha Chem Ind Co Ltd | Production of drawn multifilament of polyarylene sulfide |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01239132A (en) * | 1988-03-16 | 1989-09-25 | Toyobo Co Ltd | Sewing thread |
| US5178813A (en) * | 1990-03-23 | 1993-01-12 | Kureha Kagaku Kogyo K.K. | Method of producing poly(phenylene sulfide) fibers |
| US5405695A (en) * | 1990-03-23 | 1995-04-11 | Kureha Kagaku Kogyo K.K. | Poly(phenylene Sulfide) fibers and production process thereof |
| US5372760A (en) * | 1992-06-18 | 1994-12-13 | Hoechst Aktiengesellschaft | Process for producing polyarylene sulfide fiber and thereby obtainable polyarylene sulfide multifilament yarn |
| JP2008540850A (en) * | 2005-03-18 | 2008-11-20 | ディオレン インドゥストリアル ファイバース ベスローテン フェノートシャップ | Method for producing polyphenylene sulfide filament yarn |
| CN102677198A (en) * | 2011-03-18 | 2012-09-19 | 四川得阳工程塑料开发有限公司 | Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology |
| WO2016104236A1 (en) * | 2014-12-22 | 2016-06-30 | 東レ株式会社 | Polyphenylene sulfide monofilament and manufacturing method therefor, and package |
| US10106917B2 (en) | 2014-12-22 | 2018-10-23 | Toray Industries, Inc. | Polyphenylene sulfide monofilament and manufacturing method therefor, and package |
| JP2019173212A (en) * | 2018-03-28 | 2019-10-10 | 帝人フロンティア株式会社 | Sea-island type conjugate fiber bundle |
| JP2020033680A (en) * | 2018-08-31 | 2020-03-05 | 帝人フロンティア株式会社 | Sea-island type composite fiber bundles, medical supplies containing its ultrafine fibers, and filters for food manufacturing processes |
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