JP2003221731A - Staple fiber of polyphenylene sulfide - Google Patents
Staple fiber of polyphenylene sulfideInfo
- Publication number
- JP2003221731A JP2003221731A JP2002018343A JP2002018343A JP2003221731A JP 2003221731 A JP2003221731 A JP 2003221731A JP 2002018343 A JP2002018343 A JP 2002018343A JP 2002018343 A JP2002018343 A JP 2002018343A JP 2003221731 A JP2003221731 A JP 2003221731A
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- JP
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- Prior art keywords
- pps
- fibers
- short fibers
- polyphenylene sulfide
- strength
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、耐熱性、耐薬品性
を有するポリフェニレンサルファイド（以下、ＰＰＳと
略す）短繊維に関する。更に詳しくは良好な機械的強
度、機械的耐久性、及び寸法安定性を有するＰＰＳ短繊
維に関する。TECHNICAL FIELD The present invention relates to a polyphenylene sulfide (hereinafter abbreviated as PPS) short fiber having heat resistance and chemical resistance. More specifically, it relates to PPS short fibers having good mechanical strength, mechanical durability, and dimensional stability.
【０００２】[0002]
【従来の技術】ＰＰＳ重合体よりなる繊維は、ＰＰＳ素
材特有の耐熱性、耐薬品性、難燃性などに優れており、
従来からこの特徴を利用した各種フィルター、電気絶縁
材、抄紙カンバス、電池セパレーターなどの用途への利
用が期待されている。ところがＰＰＳ繊維は機械的強
度、機械的耐久性及び高温下での寸法安定性が未だ不十
分である。Fibers made of PPS polymer have excellent heat resistance, chemical resistance, flame retardancy, etc. peculiar to PPS materials,
It has been expected to be used for various filters, electric insulating materials, papermaking canvases, battery separators, and the like that utilize this feature. However, PPS fibers are still insufficient in mechanical strength, mechanical durability, and dimensional stability at high temperatures.
【０００３】従来、ＰＰＳ繊維の機械的強度、機械的耐
久性及び高温下での寸法安定性を向上させるために、様
々な提案がなされている。例えば、特開平４−２２２２
１７号公報では、耐熱、耐薬品性に優れる素材であるＰ
ＰＳを溶融紡糸した後、ＰＰＳの融点以下で２〜７倍に
延伸し、次いで、ＰＰＳの融点以上の温度で処理するこ
とにより、良好な引張強度、結節強度および引掛強度を
有するとともに、耐屈曲摩擦性および耐屈曲疲労性に優
れたＰＰＳ繊維とその製造方法に関する発明が開示され
ている。Various proposals have hitherto been made to improve the mechanical strength, mechanical durability and dimensional stability of PPS fibers at high temperatures. For example, JP-A-4-2222
According to the publication No. 17, P which is a material excellent in heat resistance and chemical resistance
After melt-spinning PS, it is stretched 2 to 7 times below the melting point of PPS, and then treated at a temperature above the melting point of PPS to have good tensile strength, knot strength and hooking strength, and flex resistance. An invention relating to a PPS fiber excellent in friction resistance and flex fatigue resistance and a method for producing the same is disclosed.
【０００４】また、特開２０００−１７８８２９号公報
では強度特性に優れ、毛羽や繊度斑の欠点が少ないＰＰ
Ｓ繊維及びその製造方法が開示されている。Further, in JP-A-2000-178829, PP is excellent in strength characteristics and has few defects such as fluff and fineness unevenness.
S-fibers and methods of making the same are disclosed.
【０００５】しかしながら、これらの公知技術による方
法では、機械的強度、機械的耐久性及び高温下での寸法
安定性の全てを満足するＰＰＳ繊維を得ることができな
かった。However, these methods according to the known techniques have not been able to obtain PPS fibers satisfying all of mechanical strength, mechanical durability and dimensional stability at high temperature.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、耐熱性、耐
薬品性を有すると供に、良好な機械的強度、機械的耐久
性、及び寸法安定性を有するＰＰＳ短繊維を提供するこ
とにある。DISCLOSURE OF THE INVENTION The present invention provides a PPS staple fiber having heat resistance and chemical resistance as well as good mechanical strength, mechanical durability and dimensional stability. is there.
【０００７】[0007]
【課題を解決するための手段】上述した目的を達成する
ために、本発明は次の構成を有する。In order to achieve the above-mentioned object, the present invention has the following constitution.
【０００８】すなわち、引張強度が３．５ｃＮ／ｄｔｅ
ｘ以上、引張伸度が５０〜８０％、１６０℃乾熱収縮率
が２％以下、熱水収縮率が１％以下であることを特徴と
するポリフェニレンサルファイド短繊維である。That is, the tensile strength is 3.5 cN / dte.
A polyphenylene sulfide short fiber characterized by having an elongation of x or more, a tensile elongation of 50 to 80%, a dry heat shrinkage at 160 ° C. of 2% or less, and a hot water shrinkage of 1% or less.
【０００９】[0009]
【発明の実施の形態】以下、本発明のポリフェニレンサ
ルファイド短繊維について詳細に説明する。BEST MODE FOR CARRYING OUT THE INVENTION The short polyphenylene sulfide fiber of the present invention will be described in detail below.
【００１０】本発明においてＰＰＳとは、繰り返し単位
としてｐ−フェニレンスルフィド単位やｍ−フェニレン
スルフィド単位などのフェニレンスルフィド単位を含有
するポリマーを意味する。ＰＰＳは、ホモポリマーまた
はｐ−フェニレンするフィド単位とｍ−フェニレンスル
フィド単位の両者を有する共重合体であってもよく、ま
た本発明の主旨を逸脱しない限り、他の芳香族スルフィ
ドとの共重合体あるいは混合物であっても構わない。ま
た、ＰＰＳ重合体は重量平均分子量が４００００〜６０
０００であることが望ましい。重量平均分子量が４００
００未満のＰＰＳ重合体を用いて溶融紡糸した場合、紡
糸張力が低く、紡糸時に糸切れが多発し、紡糸工程が著
しく悪くなる。また、得られたＰＰＳ短繊維も力学的特
性の劣ったものになる。一方、重量平均分子量が６００
００を超えるＰＰＳ重合体を用いると溶融紡糸に溶液の
粘度が高くなり、紡糸設備を特殊な高耐圧仕様にしなけ
ればならず、製造設備費用の高騰を招くことになる。In the present invention, PPS means a polymer containing a phenylene sulfide unit such as a p-phenylene sulfide unit or a m-phenylene sulfide unit as a repeating unit. The PPS may be a homopolymer or a copolymer having both a fido unit for p-phenylene and an m-phenylene sulfide unit, and may be a copolymer with another aromatic sulfide without departing from the gist of the present invention. It may be a combination or a mixture. The PPS polymer has a weight average molecular weight of 40,000-60.
It is desirable that it is 000. Weight average molecular weight is 400
When melt spinning is performed using a PPS polymer of less than 00, the spinning tension is low, the yarn breaks frequently during spinning, and the spinning process is significantly deteriorated. Further, the obtained PPS short fibers also have poor mechanical properties. On the other hand, the weight average molecular weight is 600
If a PPS polymer of more than 00 is used, the viscosity of the solution will be high in melt spinning, and the spinning equipment must be made to have a special high withstand pressure specification, resulting in a rise in the cost of manufacturing equipment.
【００１１】本発明にかかるＰＰＳ短繊維の引張強度は
３．５ｃＮ／ｄｔｅｘ以上でなければならない。短繊維
の引張強度特性は、該繊維を用いた布帛の強度／耐久性
に直接寄与しており、引張強度が低いと、該布帛の強度
／耐久性も低下する。引張強度は高い程好ましいが、高
強度を得るためには、ＰＰＳの重合度を高めたり、延伸
工程での延伸倍率を高める必要があり、製造工程を不安
定にさせたり、前記の通り紡糸設備を特殊な高耐圧仕様
にしなければならず、製造設備費用の高騰を招くことに
もなる。よって、ＰＰＳ短繊維の引っ張り強度は３．５
ｃＮ／ｄｔｅｘ〜７．０ｃＮ／ｄｔｅｘ、好ましくは
４．０ｃＮ／ｄｔｅｘ〜６．０ｃＮ／ｄｔｅｘである。The tensile strength of the PPS short fibers according to the present invention must be 3.5 cN / dtex or more. The tensile strength characteristics of the short fibers directly contribute to the strength / durability of the fabric using the fibers, and when the tensile strength is low, the strength / durability of the fabric also decreases. The higher the tensile strength, the more preferable, but in order to obtain high strength, it is necessary to increase the degree of polymerization of PPS or increase the draw ratio in the drawing process, which makes the manufacturing process unstable, and as described above, spinning equipment. Must be made to have a special high withstand voltage specification, which will lead to soaring manufacturing equipment costs. Therefore, the tensile strength of PPS short fibers is 3.5.
cN / dtex to 7.0 cN / dtex, preferably 4.0 cN / dtex to 6.0 cN / dtex.
【００１２】本発明者らは、同一引張強度の短繊維で
は、該短繊維の引張伸度伸度が高い方が、繊維の機械的
耐久性の尺度の一つである往復摩擦特性に優れることを
見出した。本メカニズムは明確ではないが、繊維の引張
伸度が高いと、繊維に負荷が加えられた際、繊維が延び
ることで負荷を吸収するとともに、繊維が延伸されるこ
とで、繊維の引張強度が向上するためと考えられる。よ
って、本発明にかかるＰＰＳ短繊維の引張伸度は、５０
〜８０％の範囲でなければならないものである。The inventors of the present invention have found that, in the case of short fibers having the same tensile strength, the higher the tensile elongation and elongation of the short fibers, the more excellent the reciprocating friction characteristics, which is one of the measures of the mechanical durability of the fibers. Found. Although this mechanism is not clear, when the tensile elongation of the fiber is high, when the load is applied to the fiber, the fiber stretches to absorb the load, and the fiber is stretched, so that the tensile strength of the fiber increases. It is thought to improve. Therefore, the tensile elongation of the PPS short fibers according to the present invention is 50
It must be in the range of -80%.
【００１３】ＰＰＳ短繊維の引張伸度を５０％以上にす
ると、往復摩擦試験における切断するまでの往復摩擦回
数を６０００回以上まで高めることができ、同一引張強
度で引張伸度が５０％未満の繊維に比べて、往復摩擦回
数を１．５倍以上まで向上させることができる。When the tensile elongation of the PPS short fibers is 50% or more, the number of reciprocating frictions before cutting in the reciprocating friction test can be increased to 6000 times or more, and the tensile elongation is less than 50% at the same tensile strength. The number of reciprocating frictions can be improved up to 1.5 times or more as compared with fibers.
【００１４】ＰＰＳ短繊維の引張伸度が８０％より大き
いときは、往復摩擦特性の向上が頭打ちとなり、逆に該
繊維を用いた布帛への加工性が低下することとなり好ま
しくない。When the tensile elongation of the PPS short fibers is more than 80%, the improvement of the reciprocating frictional characteristics reaches a peak, and conversely, the processability of a fabric using the fibers is deteriorated, which is not preferable.
【００１５】ＰＰＳ短繊維の引張強度はより好ましくは
６０〜７５％の範囲である。ＰＰＳ短繊維の引張伸度を
調製する手段の１つを例に挙げると、該繊維の製造工程
において、延伸した繊維を１２０℃以上の弛緩熱処理を
施すことで可能となる。弛緩熱処理温度を高めると、引
張伸度を高めることができる。The tensile strength of the PPS short fibers is more preferably in the range of 60 to 75%. Taking, as an example, one means for adjusting the tensile elongation of PPS short fibers, it becomes possible to subject the drawn fibers to a relaxation heat treatment at 120 ° C. or higher in the manufacturing process of the fibers. The tensile elongation can be increased by increasing the relaxation heat treatment temperature.
【００１６】本発明にかかるＰＰＳ短繊維の１６０℃に
おける乾熱収縮率は２％以下、熱水収縮率は１％でなけ
ればならない。該短繊維を用いた布帛製品は、前記した
通り、高温環境下や熱水中で使用されるため、該環境下
での収縮率が小さいほうが、布帛製品の変形などを抑制
し、寸法安定性が向上する。よって、乾熱収縮率は２％
以下、より好ましくは１％以下である。また熱水収縮率
は１％以下、より好ましくは０．５％以下である。The PPS short fibers according to the present invention should have a dry heat shrinkage at 160 ° C. of not more than 2% and a hot water shrinkage of 1%. Since the fabric product using the short fibers is used in a high temperature environment or hot water as described above, a smaller shrinkage rate under the environment suppresses deformation of the fabric product and dimensional stability. Is improved. Therefore, the dry heat shrinkage is 2%
Or less, more preferably 1% or less. The hot water shrinkage is 1% or less, more preferably 0.5% or less.
【００１７】ＰＰＳ短繊維の乾熱収縮率および熱水収縮
率を調製する手段の１つを例に挙げると、該繊維の製造
工程において、延伸した繊維を１２０℃以上の弛緩熱処
理を施すことにより可能となる。予め弛緩熱処理を施し
て、短繊維を収縮させることにより、該繊維を用いた布
帛の収縮率を低減することが可能となる。ただし、弛緩
熱処理温度を高めたときは、前述の通り、短繊維の引張
伸度が高くなり過ぎるため、極度な高温で弛緩熱処理す
ることは好ましくない。短繊維の乾熱収縮率と引張伸度
のバランスから、該繊維の製造工程における弛緩熱処理
温度は１２０〜１６０℃程度が好ましい。Taking one example of means for adjusting the dry heat shrinkage ratio and the hot water shrinkage ratio of PPS short fibers, the stretched fiber is subjected to a relaxation heat treatment at 120 ° C. or higher in the production process of the fiber. It will be possible. By performing relaxation heat treatment in advance to shrink the short fibers, it becomes possible to reduce the shrinkage rate of the fabric using the fibers. However, when the relaxation heat treatment temperature is increased, as described above, the tensile elongation of the short fibers becomes too high, so it is not preferable to perform the relaxation heat treatment at an extremely high temperature. From the balance of dry heat shrinkage and tensile elongation of the short fibers, the relaxation heat treatment temperature in the production process of the fibers is preferably about 120 to 160 ° C.
【００１８】[0018]
【実施例】以下、実施例を用いて本発明を詳細に説明す
る。EXAMPLES The present invention will be described in detail below with reference to examples.
【００１９】なお、本発明で定義する各特性値は以下の
方法で求めた。
（１）引張強度、引張伸度
ＪＩＳ Ｌ−１０１５−７．７の方法に準じて測定し
た。
（２）乾熱収縮率
ＪＩＳ Ｌ−１０１５−７．１５の方法に準じて処理温
度１６０℃にて測定した。
（３）熱水収縮率
ＪＩＳ Ｌ−１０１５−７．１５の方法に準じて沸騰水
９６℃にて処理し測定した。
（４）往復摩擦回数
ＪＩＳ Ｌ−１０９５−９．１０．２の方法に準じて測
定した。
実施例１〜３
重量平均分子量が５００００のＰＰＳ重合体を紡糸温度
３２０℃で、丸形状の吐出孔を有する紡糸口金（孔数７
０８）から３５０ｇ／分で吐出し、引取速度８００ｍ／
分で紡糸を行った。次に、得られた未延伸糸を集束して
糸条束とし、延伸温度９８℃、延伸速度８０ｍ／ｍｉｎ
で３．２〜３．５倍に延伸し、表１に記載の温度で１５
分間弛緩熱処理を行った。The characteristic values defined in the present invention were obtained by the following methods. (1) Tensile strength and tensile elongation Measured according to the methods of JIS L-1015-7.7. (2) Dry heat shrinkage ratio Measured at a treatment temperature of 160 ° C. according to the method of JIS L-1015-7.15. (3) Hot water shrinkage ratio Measured in accordance with the method of JIS L-1015-7.15 by treating with boiling water at 96 ° C. (4) Number of reciprocating frictions It was measured according to the method of JIS L-1095-9.10.2. Examples 1 to 3 A PPS polymer having a weight average molecular weight of 50,000 was produced at a spinning temperature of 320 ° C. and a spinneret having round discharge holes (7 holes).
08) discharge at 350g / min, take-off speed 800m /
Spinning was done in minutes. Next, the obtained undrawn yarn is bundled into a yarn bundle, and the drawing temperature is 98 ° C. and the drawing speed is 80 m / min.
It is stretched 3.2 times to 3.5 times at a temperature of 15
Relaxation heat treatment was performed for minutes.
【００２０】なお、弛緩熱処理とは、繊維にローラー等
による機械的な緊張を加えないことを意味する。得られ
た弛緩熱処理済みの糸条束を、５１ｍｍに切断して、繊
度２．２ｄｔｅｘのＰＰＳ短繊維を得た。なお、往復摩
擦回数を測定するサンプルのみ、４００ｍｍに切断して
測定用とした。
比較例１〜２
弛緩熱処理温度を表２の温度で処理した以外は実施例１
〜３と同様の方法でＰＰＳ短繊維を得た。
比較例３
重量平均分子量が２５０００のＰＰＳ重合体を用い、弛
緩熱処理温度１３０℃で処理した以外は実施例１〜３と
同様の方法でＰＰＳ短繊維を得た。The relaxation heat treatment means that the fiber is not mechanically tensioned by a roller or the like. The obtained relaxation-heat treated yarn bundle was cut into 51 mm to obtain PPS short fibers having a fineness of 2.2 dtex. Only the sample for measuring the number of reciprocating frictions was cut into 400 mm for measurement. Comparative Examples 1 to 2 Example 1 except that the relaxation heat treatment temperature was the temperature shown in Table 2.
PPS short fibers were obtained in the same manner as described above. Comparative Example 3 PPS staple fibers were obtained in the same manner as in Examples 1 to 3 except that a PPS polymer having a weight average molecular weight of 25000 was used and the relaxation heat treatment temperature was 130 ° C.
【００２１】以上の各実施例、各比較例について評価し
た結果は、表１、表２に示したとおりである。Tables 1 and 2 show the results of evaluation of the above-mentioned examples and comparative examples.
【００２２】[0022]
【表１】 [Table 1]
【００２３】[0023]
【表２】 [Table 2]
【００２４】実施例１〜３と比較例１から確認できるよ
うに、短繊維の引張伸度は往復摩擦性能に関連してい
る。特に、引張伸度５０〜８０％の範囲内で良好な特性
を示している。As can be confirmed from Examples 1 to 3 and Comparative Example 1, the tensile elongation of short fibers is related to the double-sided friction performance. Particularly, good properties are exhibited in the range of tensile elongation of 50 to 80%.
【００２５】比較例２では更に引張伸度を高めたが往復
摩擦回数はそれほど高い値を示さなくなっている。ま
た、重量平均分子量が低い重合体を用いたときは（比較
例３）、短繊維の引張強度が低くなり、該低い引張強度
の繊維の往復摩擦回数は大幅に低いものであることがわ
かる。In Comparative Example 2, the tensile elongation was further increased, but the number of reciprocating frictions did not show such a high value. Moreover, when a polymer having a low weight average molecular weight is used (Comparative Example 3), the tensile strength of the short fibers becomes low, and the number of times of reciprocating friction of the fibers having the low tensile strength is significantly low.
【００２６】[0026]
【発明の効果】本発明によれば、耐熱性、耐薬品性を有
するとともに、良好な機械的強度、機械的耐久性、及び
寸法安定性を有するＰＰＳ短繊維を提供することができ
る。Industrial Applicability According to the present invention, it is possible to provide PPS short fibers having heat resistance and chemical resistance, and having good mechanical strength, mechanical durability and dimensional stability.
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Claims (2)
張伸度が５０〜８０％、１６０℃乾熱収縮率が２％以
下、熱水収縮率が１％以下であることを特徴とするポリ
フェニレンサルファイド短繊維。1. A tensile strength of 3.5 cN / dtex or more, a tensile elongation of 50 to 80%, a dry heat shrinkage of 160 ° C. of 2% or less, and a hot water shrinkage of 1% or less. Polyphenylene sulfide short fiber.
摩擦回数が６０００回以上であることを特徴とする請求
項１記載のポリフェニレンサルファイド短繊維。2. The short polyphenylene sulfide fiber according to claim 1, wherein the number of times of reciprocating friction before cutting in the reciprocating friction test is 6000 times or more.
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| JP2002018343A JP2003221731A (en) | 2002-01-28 | 2002-01-28 | Staple fiber of polyphenylene sulfide |
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