JP3277703B2 - Polyester fiber having good abrasion resistance and method for producing the same - Google Patents
Polyester fiber having good abrasion resistance and method for producing the sameInfo
- Publication number
- JP3277703B2 JP3277703B2 JP16935794A JP16935794A JP3277703B2 JP 3277703 B2 JP3277703 B2 JP 3277703B2 JP 16935794 A JP16935794 A JP 16935794A JP 16935794 A JP16935794 A JP 16935794A JP 3277703 B2 JP3277703 B2 JP 3277703B2
- Authority
- JP
- Japan
- Prior art keywords
- polyester
- particles
- silicon oxide
- polyester fiber
- particle
- 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.)
- Expired - Fee Related
Links
Landscapes
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は、耐摩耗性の良好なポリ
エステル繊維に関する。さらに詳しくは、織物とした時
の風合いが良好で、かつ高次工程での摩耗による白粉な
どの糸削れを抑制できる耐摩耗性の良好なポリエステル
繊維に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polyester fiber having good abrasion resistance. More specifically, the present invention relates to a polyester fiber having a good texture when used as a woven fabric and a good abrasion resistance capable of suppressing yarn scraping of white powder and the like due to abrasion in a high-order process.
【0002】[0002]
【従来の技術】近年、紡糸速度5500m/分以上の高
速紡糸プロセスが、ポリエステルなどの溶融紡糸の生産
プロセスとして広まりつつある。これはプロセスそのも
のが大きなコストダウン効果をもつだけでなく、この繊
維からなる織物が従来の紡糸/延伸の二工程法により得
られる繊維からなる織物と比較して、ソフト風合い、染
色性などで優れた特性を示すからである。この良好なソ
フト風合いは、特殊な繊維構造形成の過程を経るため
に、繊維内の非晶部分子鎖の配向が低くなり基質自体が
柔らかくなることに起因する。しかし一方では、紡糸速
度5500m/分以上の高速紡糸で得られる繊維は、整
経、製織、編立てなどの高次工程において、従来の紡糸
/延伸の二工程法により得られる繊維に比して削れ物が
発生しやすい。これらの問題を解決するためには、紡糸
油剤の付与量を増加する手段が採られているが、削れ物
の量は減少するものの、油剤に起因するスカム汚れが激
しくなり必ずしも有効な手段ではない。この削れ物が発
生する理由としては、紡糸速度5500m/分以上の高
速紡糸繊維は極めて高温の状態で構造が形成されるた
め、分子鎖の緩和と結晶化の促進が同時に起こり、その
構造の特徴として非晶部の配向度が低く、ミクロボイド
を有するため、基質が柔らかく、擦過に対してポリマ基
質自体が削れやすく、フィブリル状の削れ物を生じやす
いものと考えている。2. Description of the Related Art In recent years, a high-speed spinning process at a spinning speed of 5500 m / min or more has become widespread as a production process of melt spinning of polyester or the like. This is because not only the process itself has a large cost reduction effect, but the fabric made of this fiber is superior in soft texture, dyeing properties, etc., compared to the fabric made of the fiber obtained by the conventional two-step spinning / drawing method. This is because they exhibit the characteristics shown in FIG. This good soft hand is caused by the fact that the orientation of the molecular chains in the amorphous part in the fiber becomes low and the substrate itself becomes soft because of the special fiber structure forming process. On the other hand, however, fibers obtained by high-speed spinning at a spinning speed of 5500 m / min or more are used in higher-order processes such as warping, weaving, and knitting as compared with fibers obtained by a conventional spinning / drawing two-step method. Shavings are likely to occur. In order to solve these problems, means for increasing the applied amount of the spinning oil agent has been adopted.However, although the amount of shaved material is reduced, scum stain caused by the oil agent becomes severe and is not necessarily an effective means. . The reason for the generation of the shavings is that the structure of a high-speed spun fiber having a spinning speed of 5500 m / min or more is formed at an extremely high temperature, so that the relaxation of molecular chains and the promotion of crystallization occur simultaneously, and the characteristics of the structure are characteristic. It is considered that the substrate has a low degree of orientation in the amorphous part and has microvoids, so that the substrate is soft, and the polymer substrate itself is easily scraped by abrasion, so that a fibril-shaped scrap is easily generated.
【0003】この削れ物を減少させるため、原料ポリエ
ステル中に酸化チタンや酸化ケイ素などの粒子を添加し
ているが、この場合にも削れ物が発生し、添加された粒
子が削れ物の大部分を占めている。この削れ物が発生す
る理由としては、以下に示すA、Bの二つの要因が考え
られいる。 A.従来の酸化チタン、ジメチルジクロロシランで表面
処理した酸化ケイ素(特公平3−35403号公報)な
どの粒子を含むポリエステルの高速紡糸繊維は、 その
繊維表面を観察したところ、二工程法で得られた繊維に
比較して高い突起 が数多く見られた。これは、高速紡
糸プロセスは構造形成の過程が極めて短く、 半流動状
態から一気に結晶化を起こし、密度が急増するので、こ
の時にポリエ ステル中の粒子が繊維表面に押し出さ
れ、高次工程のガイドなどとの擦過に対 して粒子が脱
落しやすくなるものと考えられる。 B.構造形成時の極めて高い応力の影響で、添加粒子と
ポリマ基質が剥離し、粒子周囲に比較的大きなボイドを
生成するため、粒子が脱落しやすいものと考えられる。 以上のことから、ポリエステルとの親和性が高く、分散
性が良好な粒子を含有すれば、得られた繊維の高次工程
での削れ物は激減すると考えた。[0003] Particles such as titanium oxide and silicon oxide are added to the raw material polyester in order to reduce the shavings, but in this case, shavings are also generated, and the added particles make up most of the shavings. Occupy. The following two factors A and B are considered as the reason for the generation of the shaved object. A. Conventional high-speed spun fibers of polyester containing particles such as silicon oxide (Japanese Patent Publication No. 3-35403) surface-treated with titanium oxide and dimethyldichlorosilane were obtained by a two-step method by observing the fiber surface. Many protrusions were seen that were higher than the fibers. This is because, in the high-speed spinning process, the process of forming the structure is extremely short, and crystallization occurs at once from a semi-fluid state, and the density rapidly increases.At this time, the particles in the polyester are extruded to the fiber surface and guide the high-order process. It is considered that particles easily fall off due to rubbing with the like. B. It is considered that the particles are likely to fall off because the added particles and the polymer substrate are separated under the influence of the extremely high stress during the formation of the structure and relatively large voids are generated around the particles. From the above, it was considered that if particles having high affinity to polyester and good dispersibility were contained, the shavings of the obtained fibers in the high-order process were drastically reduced.
【0004】そこで、我々は特殊なアルミナを使用する
ことを提案した(特開平1−285283号公報)。と
ころが、この粒子を含有したポリエステルは、上記課題
である高次工程における削れ物の減少は解決できたもの
の、ポリエステル中での分散性が不十分であるため、紡
糸パック内のフィルター濾過における濾圧上昇が大き
く、安定して生産できないことがわかった。Therefore, we proposed to use a special alumina (Japanese Patent Laid-Open No. 1-285283). However, although the polyester containing these particles could solve the problem of reduction of shavings in the higher order process, the dispersibility in the polyester was insufficient, so that the filtration pressure in the filter filtration in the spinning pack was insufficient. The increase was so large that it could not be produced stably.
【0005】また、ジメチルジクロロシランで表面処理
した酸化ケイ素を使用することを提案した(特公平3−
35403号公報)。ところが、該公報の糸は白粉が発
生しやすい問題があることがわかった。これは酸化ケイ
素は、特公昭43−23960号公報に記載されている
ようにポリエステル中での粒子分散性は不良であり、こ
の表面処理酸化ケイ素はその分散性を改良したものでは
あるが、それでもポリエステル中での粒子の凝集が避け
られず、粒子分散性が不十分であった。It has also been proposed to use silicon oxide surface-treated with dimethyldichlorosilane (Japanese Patent Publication No.
No. 35403). However, it has been found that the yarn disclosed in the publication has a problem that white powder is easily generated. This is because silicon oxide has poor particle dispersibility in polyester as described in JP-B-43-23960, and this surface-treated silicon oxide has improved dispersibility. Agglomeration of the particles in the polyester was unavoidable, and the particle dispersibility was insufficient.
【0006】ところが、このジメチルジクロロシランで
表面処理した酸化ケイ素を使用しても、紡糸パック内の
フィルター濾過を強化すれば、濾圧上昇の大きい問題が
あるものの、上記課題である高次工程における削れ物の
発生の問題は解決できることがわかった。[0006] However, even if silicon oxide surface-treated with dimethyldichlorosilane is used, there is a problem in that the filtration pressure in the spinning pack is increased. It turned out that the problem of shavings can be solved.
【0007】そこで、5500m/分以上の高速紡糸に
おいて、ポリエステルとの親和性が高く、ポリエステル
への分散性が良好な酸化ケイ素粒子の探索にポイントを
絞り、鋭意に検討した結果、本発明に至ったのである。Accordingly, in high-speed spinning at a speed of 5500 m / min or more, a point was sought to search for silicon oxide particles having a high affinity for the polyester and a good dispersibility in the polyester, and as a result of intensive studies, the present invention was concluded. It was.
【0008】[0008]
【発明が解決しようとする課題】本発明の目的は、前記
欠点のないポリエステル繊維、すなわち高速紡糸特有の
ソフトな風合いの織物となり、かつ高次工程での白粉な
ど糸の削れを起こさない耐摩耗性の良好なポリエステル
繊維とその製造方法を提供することにある。SUMMARY OF THE INVENTION It is an object of the present invention to provide a polyester fiber free from the above-mentioned disadvantages, that is, a woven fabric having a soft texture peculiar to high-speed spinning, and which is free from abrasion of yarn such as white powder in a high-order process. An object of the present invention is to provide a polyester fiber having good properties and a method for producing the same.
【0009】[0009]
【課題を解決するための手段】本発明者らは、本目的を
達成するため鋭意検討を重ねた結果、ある特有の酸化ケ
イ素粒子を使用することにより、上記課題を解決できる
ことを見出し、本発明を完成するに至ったのである。す
なわち、本発明はトリメチルシリル誘導体で表面処理し
て粒子表面のシラノール基の40%以上を封鎖した、平
均一次粒子径が5〜50mμの実質的に乾式法で合成し
た酸化ケイ素粒子を0.02〜2.0重量%含有し、t
anδのピーク温度Tmaxが125℃以下、密度が
1.370g/cm3 以上、複屈折率が0.085以上
である耐摩耗性の良好なポリエステル繊維を提供するこ
とである。 本発明における酸化ケイ素粒子は、トリメ
チルシリル誘導体で表面処理して表面のシラノール基の
40%以上封鎖することが必要である。好ましくは60
%以上である。この封鎖率が40%未満であると、ポリ
エステル中で粒子が凝集し、紡糸パック内のフィルター
濾過における濾圧上昇が大きく、また高次工程において
粒子が脱落しやすいという問題を生じる。ここでいう封
鎖とは、酸化ケイ素粒子表面のシラノール基がトリメチ
ルシリル誘導体との反応によって、シラノール基の水素
がトリメチルシリル基と置換することである。したがっ
て、封鎖率とは酸化ケイ素粒子表面のトリメチルシリル
誘導体による処理前後のシラノール基濃度の比率(%)
で表わされる。Means for Solving the Problems The inventors of the present invention have made intensive studies to achieve the object, and as a result, have found that the above problems can be solved by using certain specific silicon oxide particles. Was completed. That is, the present invention provides a silicon oxide particle having a mean primary particle diameter of 5 to 50 μm, which is surface-treated with a trimethylsilyl derivative to block 40% or more of silanol groups on the particle surface, and which is synthesized by a dry method. 2.0% by weight, t
An object of the present invention is to provide an abrasion-resistant polyester fiber having an an δ peak temperature Tmax of 125 ° C. or less, a density of 1.370 g / cm 3 or more, and a birefringence of 0.085 or more. The silicon oxide particles in the present invention need to be surface-treated with a trimethylsilyl derivative to block 40% or more of the silanol groups on the surface. Preferably 60
% Or more. If the sealing ratio is less than 40%, the particles agglomerate in the polyester, causing a large increase in the filtration pressure in the filter filtration in the spinning pack, and the problem that the particles are likely to fall off in the high-order process. The term “blocking” as used herein means that the silanol group on the surface of the silicon oxide particles reacts with the trimethylsilyl derivative to replace the hydrogen of the silanol group with the trimethylsilyl group. Therefore, the blocking rate is the ratio of the silanol group concentration before and after the treatment of the silicon oxide particles with the trimethylsilyl derivative (%).
Is represented by
【0010】また、酸化ケイ素粒子の表面処理にはトリ
メチルシリル誘導体を用いることが必要である。トリメ
チルシリル誘導体は、酸化ケイ素粒子表面のシラノール
基と反応してトリメチルシリル基を有するものであり、
ヘキサメチルジシラザン、トリメチルクロロシラン、ト
リメチルメトキシシランなどが挙げられ、その中でヘキ
サメチルジシラザンが最も好ましい。ヘキサメチルジシ
ラザンで表面処理すると粒子のPHは中性に近くなり、
粒子合成時に副生する塩化水素が微量残存してPHが酸
性となるトリメチルクロロシラン、トリメチルメトキシ
シランなどで表面処理したものよりも、ポリエステルへ
の粒子分散性は良好である。In addition, it is necessary to use a trimethylsilyl derivative for the surface treatment of the silicon oxide particles. The trimethylsilyl derivative has a trimethylsilyl group by reacting with a silanol group on the surface of the silicon oxide particle,
Hexamethyldisilazane, trimethylchlorosilane, trimethylmethoxysilane and the like can be mentioned, among which hexamethyldisilazane is most preferred. When the surface is treated with hexamethyldisilazane, the pH of the particles becomes close to neutral,
Particle dispersibility in polyester is better than that obtained by surface treatment with trimethylchlorosilane, trimethylmethoxysilane, or the like in which a small amount of hydrogen chloride by-produced during the particle synthesis remains and the pH becomes acidic.
【0011】一方、トリメチルシリル誘導体以外のジメ
チルジクロロシラン(特公平3−35403号公報)、
トリクロロメチルシラン、トリクロロオクチルシラン、
または反応基を複数有するシランカップリング剤(特開
平4−74379号、特開平4−298538号公報な
ど)などの表面処理剤で処理しても、表面処理のない酸
化ケイ素粒子に比較してポリエステルへの粒子分散性は
ある程度向上するが、本発明で目的とする高度なポリエ
ステルへの粒子分散性はなお不十分であり、紡糸パック
内のフィルター濾過における濾圧上昇が大きいばかりで
なく、紡糸速度5500m/分以上で糸切れが激しく、
安定して溶融紡糸できない。これら従来公知の表面処理
剤で表面処理した酸化ケイ素粒子が、本発明におけるト
リメチルシリル誘導体で表面処理した酸化ケイ素粒子よ
りもポリエステルへの粒子分散性に劣る理由は、従来の
表面処理による酸化ケイ素粒子は疎水性が低くポリエス
テルとの親和性が低いこと、また粒子表面に反応基が数
多く残るため粒子同士が反応して粗大粒子が副生するこ
となどが考えられる。On the other hand, dimethyldichlorosilane other than trimethylsilyl derivative (Japanese Patent Publication No. 3-35403),
Trichloromethylsilane, trichlorooctylsilane,
Alternatively, even when treated with a surface treating agent such as a silane coupling agent having a plurality of reactive groups (JP-A-4-74379, JP-A-4-298538, etc.), polyesters are compared with silicon oxide particles without surface treatment. Although the particle dispersibility in the polyester obtained by the present invention is improved to some extent, the particle dispersibility in the high-grade polyester intended in the present invention is still insufficient. Above 5500m / min, severe thread breakage,
Melt spinning cannot be performed stably. The reason that silicon oxide particles surface-treated with these conventionally known surface treatment agents are inferior in particle dispersibility to polyester than silicon oxide particles surface-treated with a trimethylsilyl derivative in the present invention is that silicon oxide particles by conventional surface treatment are It is conceivable that the hydrophobicity is low and the affinity with the polyester is low, and that a large number of reactive groups remain on the particle surface so that the particles react with each other to produce a coarse particle as a by-product.
【0012】なお、本発明におけるトリメチルシリル誘
導体で表面処理される酸化ケイ素粒子は、後述する合成
法で得られた酸化ケイ素粒子をそのまま使用しても、あ
るいは一旦ジメチルジクロロシラン、トリクロロメチル
シラン、トリクロロオクチルシラン、または反応基を複
数有するシランカップリング剤などで表面処理してあっ
ても良い。すなわち、酸化ケイ素の最表面がトリメチル
シリル誘導体で表面処理してあれば、ポリエステルとの
親和性が高く粒子分散性が良好となるのである。The silicon oxide particles to be surface-treated with the trimethylsilyl derivative in the present invention may be used as they are, or may be used as they are, or may be used once as dimethyldichlorosilane, trichloromethylsilane, trichlorooctyl. The surface may be treated with silane, a silane coupling agent having a plurality of reactive groups, or the like. That is, if the outermost surface of silicon oxide is surface-treated with a trimethylsilyl derivative, the affinity for polyester is high and the particle dispersibility is good.
【0013】また、本発明における酸化ケイ素粒子は、
乾式法で合成されているか、又は湿式法で合成し更に焼
成した酸化ケイ素粒子であって、乾式法と同様な表面状
態に変性されていることが必要である。乾式法の場合に
は、四塩化ケイ素と水素混合物を空気中で加熱して加水
分解する燃焼法、珪砂とコークスをアーク炉で加熱還元
し空気中の酸素で酸化する加熱法などがある。この乾式
法で合成された酸化ケイ素粒子は、内部表面を持たない
ため、表面シラノール基濃度が通常3個/nm2 以下と
少ないが、トリメチルシリル誘導体で表面処理すること
により、表面シラノール基濃度はさらに低濃度となり、
粒子同士の親和性が低下するため、ポリエステルへの分
散性が向上すると考えられる。一方、珪酸曹達と酸など
を原料とする湿式法で合成した酸化ケイ素粒子は、ポリ
エステルへの分散性が不十分である。これは、表面シラ
ノール基濃度が6〜30個/nm2 と非常に高濃度であ
り、乾式法で合成したものと異なり内部表面を持つた
め、表面処理しても粒子同志の親和性が高いためと考え
られる。なお、湿式法で合成した酸化ケイ素粒子でも、
それを焼成して内部表面をなくし、表面シラノール基濃
度を低くして乾式法と同様な表面状態に変性すれば、表
面シラノール基濃度が通常3個/nm2 以下となって乾
式法で合成した酸化ケイ素粒子と同様に使用できる。Further, the silicon oxide particles in the present invention include:
It is synthesized by a dry method or synthesized by a wet method and
Silicon oxide particles that are formed and have the same surface state as the dry method
It is necessary that it be denatured . In the case of the dry method, there are a combustion method in which a mixture of silicon tetrachloride and hydrogen is heated and hydrolyzed in air, and a heating method in which silica sand and coke are heated and reduced in an arc furnace and oxidized with oxygen in the air. Since the silicon oxide particles synthesized by this dry method do not have an internal surface, the surface silanol group concentration is usually as low as 3 particles / nm 2 or less, but the surface silanol group concentration can be further increased by surface treatment with a trimethylsilyl derivative. Low concentration,
It is considered that the dispersibility in the polyester is improved because the affinity between the particles is reduced. On the other hand, silicon oxide particles synthesized by a wet method using silicate soda and an acid as raw materials have insufficient dispersibility in polyester. This is because the surface silanol group concentration is as high as 6 to 30 particles / nm 2 , and since it has an internal surface unlike those synthesized by the dry method, the affinity of the particles is high even after the surface treatment. it is conceivable that. In addition, even silicon oxide particles synthesized by a wet method,
Eliminate internal surface by firing it, if modifying the surface silanol group concentration was lowered to a similar surface state and a dry method, dry <br/> surface silanol group concentration becomes usually three / nm 2 or less The same can be used as the silicon oxide particles synthesized by the formula method.
【0014】本発明における表面処理酸化ケイ素粒子
は、その平均一次粒子径は5〜50mμ、好ましくは7
〜40mμであることが必要である。この平均一次粒子
径は5mμより小さいと粒子の比表面積が大きくなるた
め、ポリエステル中で粒子が凝集しやすく、一方、50
mμより大きいと二次粒子中の凝結した粗大粒子が多
く、その粒子はポリエステル中で分散しないため、いず
れも粒子分散性が低下して繊維表面突起が高くなり擦過
時に表面突起が脱落し易くなる。The surface-treated silicon oxide particles of the present invention have an average primary particle diameter of 5 to 50 mμ, preferably 7 to 50 μm.
〜40 mμ is required. When the average primary particle diameter is smaller than 5 μm, the specific surface area of the particles increases, so that the particles easily aggregate in the polyester.
When the particle size is larger than mμ, the coagulated coarse particles in the secondary particles are large, and the particles do not disperse in the polyester, so that the particle dispersibility decreases and the fiber surface protrusions increase, and the surface protrusions easily fall off during abrasion. .
【0015】本発明における表面処理した酸化ケイ素粒
子は、ポリエステル繊維中に0.02〜2.0重量%含
有する必要がある。0.02重量%未満では糸の削れを
防止する効果が不十分であり、2.0重量%を越えると
高次工程における削れ物が多くなる。The surface-treated silicon oxide particles in the present invention must be contained in the polyester fiber in an amount of 0.02 to 2.0% by weight. If it is less than 0.02% by weight, the effect of preventing the scraping of the yarn is insufficient, and if it exceeds 2.0% by weight, the shavings in the high-order process increase.
【0016】本発明におけるポリエステルは、ポリエチ
レンテレフタレート、あるいはそれを主成分とした線状
なものであり、ジカルボン酸またはそのエステル形成性
誘導体と、グリコールまたはそのエステル形成性誘導体
とを主たる出発原料としてエステル化またはエステル交
換などの反応により低重合体を合成した後、さらにその
低重合体を高温・減圧下で重縮合反応させることにより
製造できる。The polyester in the present invention is polyethylene terephthalate or a linear one containing the same as a main component, and is composed of a dicarboxylic acid or an ester-forming derivative thereof and a glycol or an ester-forming derivative thereof as a main starting material. It can be produced by synthesizing a low polymer by a reaction such as conversion or transesterification, and then subjecting the low polymer to a polycondensation reaction under high temperature and reduced pressure.
【0017】本発明におけるポリエステルには、共重合
成分として、イソフタル酸、2,6−ナフタレンジカル
ボン酸、5−ナトリウムスルホイソフタル酸、アジピン
酸、セバシン酸、テトラデカン二酸、エイコサン二酸、
ダイマー酸、1,4−シクロヘキサンジカルボン酸など
のジカルボン酸成分、1、4−ブタンジオール、1、6
−ヘキサンジオール、ビスフェノールAまたはそのエチ
レンオキサイド付加物、ビスフェノールSまたはそのエ
チレンオキサイド付加物、1,4−シクロヘキサンジメ
タノール、ジエチレングリコール、ポリエチレングリコ
ール、ポリプロピレングリコール、ポリブチレングリコ
ールなどのジオール成分、パラオキシ安息香酸、ε−カ
プロラクトンなどのオキシカルボン酸成分などの2官能
性成分を15モル%以下共重合していても良く、トリメ
リット酸、ペンタエリスリトールなどの多官能性成分な
ども得られるポリエステルが実質的に線状である量なら
ば、共重合していても良い。更に、制電剤、紫外線吸収
剤、赤外線吸収剤、難燃剤、蛍光増白剤、抗菌剤などの
添加剤を共重合、混合などの方法により、本発明の目的
を逸脱しない範囲で含有しても良い。The polyester in the present invention contains, as copolymerization components, isophthalic acid, 2,6-naphthalenedicarboxylic acid, 5-sodium sulfoisophthalic acid, adipic acid, sebacic acid, tetradecandioic acid, eicosanediacid,
Dicarboxylic acid components such as dimer acid and 1,4-cyclohexanedicarboxylic acid, 1,4-butanediol, 1,6
-Hexanediol, bisphenol A or an ethylene oxide adduct thereof, bisphenol S or an ethylene oxide adduct thereof, diol components such as 1,4-cyclohexanedimethanol, diethylene glycol, polyethylene glycol, polypropylene glycol, polybutylene glycol, paraoxybenzoic acid, A bifunctional component such as an oxycarboxylic acid component such as ε-caprolactone may be copolymerized in an amount of 15 mol% or less, and a polyester from which a polyfunctional component such as trimellitic acid and pentaerythritol can be obtained is substantially linear. As long as the amount is in the form, copolymerization may be performed. Further, additives such as an antistatic agent, an ultraviolet absorber, an infrared absorber, a flame retardant, a fluorescent brightener, and an antibacterial agent are copolymerized and contained by a method such as mixing within a range not departing from the object of the present invention. Is also good.
【0018】次に、この粒子を含有したポリエステル繊
維の特性について述べる。本発明におけるポリエステル
繊維は、tanδのピーク温度Tmaxが125℃以
下、密度が1.370g/cm3 以上、複屈折率が0.
085以上である必要がある。tanδのピーク温度T
maxは、繊維の非晶部分子鎖の動き易さを示す値であ
り、これは125℃を越えると、非晶部分子鎖は動きに
くく、繊維の基質自体が堅いため織物としたときの風合
いがソフトとならない。また、密度は1.370g/c
m3 未満であると、熱に対する寸法安定性が劣るため、
精錬、中間セット、染色などでの織編物の風合いが硬く
なってソフトな風合とならない。複屈折率は0.085
以上である必要がある。0.085未満であると、分子
鎖の配向が低く機械的性質が低くなるため高次加工の各
工程で糸の削れや糸切れなどのトラブルが発生し、本発
明の酸化ケイ素粒子を含有していたとしても、これらを
防止することは極めて困難である。Next, the characteristics of the polyester fiber containing the particles will be described. The polyester fiber in the present invention has a tan δ peak temperature Tmax of 125 ° C. or less, a density of 1.370 g / cm 3 or more, and a birefringence of 0.1.
085 or more. peak temperature T of tan δ
The max is a value indicating the easiness of movement of the amorphous part molecular chains of the fiber. When the temperature exceeds 125 ° C., the amorphous part molecular chains are hard to move, and the texture of the fabric is made because the fiber substrate itself is hard. Does not become soft. The density is 1.370 g / c
If less than m 3, since the dimensional stability against heat is inferior,
The texture of the woven or knitted fabric in refining, intermediate set, dyeing, etc. becomes hard and does not become soft. Birefringence is 0.085
It is necessary to be above. If it is less than 0.085, the orientation of the molecular chains is low and the mechanical properties are low, so troubles such as thread shaving and thread breakage occur in each step of the higher-order processing, and the silicon oxide particles of the present invention are contained. Even if they do, it is extremely difficult to prevent them.
【0019】次に、本発明の耐摩耗性の良好なポリエス
テル繊維の製造方法を示す。特定の極限粘度のポリエス
テルに特異な表面処理を施した粒子を直接粉末のまま添
加、混合することで、酸化ケイ素粒子のポリエステルへ
の分散性が著しく向上することを見出したのである。Next, a method for producing a polyester fiber having good abrasion resistance according to the present invention will be described. It has been found that the dispersibility of silicon oxide particles in polyester is significantly improved by directly adding and mixing particles obtained by subjecting a polyester having a specific intrinsic viscosity to a specific surface treatment as powder.
【0020】本発明において酸化ケイ素粒子を添加する
ポリエステルの極限粘度は0.50dl/g以上、好ま
しくは0.55dl/g以上とする必要がある。極限粘
度が0.50dl/g未満のポリエステルを用いると、
粒子分散性が劣るばかりか、得られた糸の機械特性が損
なわれ、強度、伸度が劣るものとなってしまう。In the present invention, the intrinsic viscosity of the polyester to which the silicon oxide particles are added must be 0.50 dl / g or more, preferably 0.55 dl / g or more . When a polyester having an intrinsic viscosity of less than 0.50 dl / g is used,
Not only is the particle dispersibility poor, but the mechanical properties of the resulting yarn are impaired, resulting in poor strength and elongation.
【0021】また、本発明における酸化ケイ素粒子粉末
を直接添加、混合することが必要である。酸化ケイ素粒
子は、水に分散しないため水スラリーとしての添加が難
しく、また分散が可能な有機溶媒のスラリーで添加して
も、ポリエステルへの粒子分散性が劣り、紡糸パック内
のフィルター濾過における濾圧上昇が大きいばかりでな
く、紡糸速度5500m/分以上で糸切れが激しく、安
定して溶融紡糸できないのである。Further, it is necessary to directly add and mix the silicon oxide particles in the present invention. Silicon oxide particles are difficult to be added as a water slurry because they do not disperse in water, and even when added as a slurry of a dispersible organic solvent, the particle dispersibility in polyester is inferior. Not only the pressure rise is large, but also the yarn breakage is severe at a spinning speed of 5500 m / min or more, and the melt spinning cannot be performed stably.
【0022】本発明における粒子粉末の直接添加混合
は、一旦チップ化した後再溶融したポリエステルに添
加、混合させることも、連続重合したポリエステルに直
接定量的に供給することもできる。また、ベースポリエ
ステルから枝分岐して粒子を混合して得たマスターのポ
リエステルを再度ベースポリエステルと最適量混合して
紡糸しても良く、マスターのポリエステルのままチップ
状、または溶融計量後にベースポリエステルと混合して
紡糸する方法も採用することもできる。The direct addition and mixing of the particle powder in the present invention can be added to and mixed with the polyester once formed into chips and then re-melted, or can be directly and quantitatively supplied to the continuously polymerized polyester. Alternatively, the master polyester obtained by branching and mixing particles from the base polyester may be mixed again with the base polyester in an optimal amount and spun. A method of mixing and spinning can also be adopted.
【0023】粒子粉末のポリエステルへの混合は剪断力
が大きい混合機にて実施することが好ましい。剪断力が
大きい混合機としては、単軸押出機、二軸押出機、多段
押出機、混練機などが好ましく使用でき、二軸以上の押
出機は同方向回転、異方向回転でも、非かみ合い型、か
み合い型いずれでも構わない。重合槽の攪拌など剪断力
が小さい混合機では本発明の表面処理酸化ケイ素粒子は
十分には分散しないため好ましくない。The mixing of the particle powder with the polyester is preferably carried out in a mixer having a large shearing force. As a mixer having a large shearing force, a single-screw extruder, a twin-screw extruder, a multi-stage extruder, a kneader, and the like can be preferably used. , Any meshing type is acceptable. The use of a mixer having a small shearing force such as stirring in a polymerization tank is not preferable because the surface-treated silicon oxide particles of the present invention are not sufficiently dispersed.
【0024】本発明の耐摩耗性の良好なポリエステル繊
維を得るには、紡糸速度5500m/分以上で溶融紡糸
する際、製糸性を高めるためには、紡糸温度を300℃
以上とし、口金下保温ゾーンの長さを20cm以上と
し、冷却ゾーン直後に油剤を付与して紡糸することが好
ましい。In order to obtain the polyester fiber having good abrasion resistance according to the present invention, when spinning at a spinning speed of 5500 m / min or more, the spinning temperature is set to 300 ° C. in order to enhance the spinning property.
As described above, it is preferable that the length of the heat retaining zone under the base is 20 cm or more, and the spinning is performed by applying an oil agent immediately after the cooling zone.
【0025】本発明の繊維およびその製造方法によれ
ば、酸化ケイ素粒子がポリエステル繊維の特に表層部に
均一に分散するので周囲のポリマを硬くすることがで
き、これに起因する繊維表面の突起を脱落しにくくして
いるものと考える。また本発明における酸化ケイ素粒子
はポリエステルとの親和性が高いことから、他の粒子に
見られるような粒子周辺のボイドの生成が見られず、粒
子の脱落が抑制されるものと考える。According to the fiber of the present invention and the method for producing the same, the silicon oxide particles are uniformly dispersed particularly in the surface layer of the polyester fiber, so that the surrounding polymer can be hardened. We think that it is hard to fall off. In addition, since the silicon oxide particles in the present invention have a high affinity for polyester, it is considered that voids around the particles as seen in other particles are not generated and the particles are prevented from falling off.
【0026】[0026]
【実施例】以下の実施例によって本発明をさらに具体的
に説明する。まず本発明における粒子の特性および分散
性、糸物性などの測定法について述べる。The present invention will be described more specifically with reference to the following examples. First, the method of measuring the characteristics, dispersibility, yarn physical properties and the like of the particles in the present invention will be described.
【0027】A.粒子の平均一次粒子径 粒子を10万倍に拡大した電子顕微鏡写真から、各一次
粒子の最長径を測定し、1000個の平均として求め
た、なお、この平均一次粒径は、糸中に粒子が分散して
も変わらない。A. Average primary particle diameter of particles From the electron micrograph of the particles magnified 100,000 times, the longest diameter of each primary particle was measured and determined as an average of 1,000 particles. Does not change even if dispersed.
【0028】 B.粒子の表面シラノール基封鎖率 粒子を100℃減圧下で3時間乾燥後、ジオキサン中リ
チウムアルミニウムハイドライドで還元し、発生した水
素量をガスクロマトグラフィー法により定量分析して単
位重量あたりのシラノール基濃度(個/g)を求め、別
途BET法で求めた粒子の比表面積(m 2 /g )で割
り返すことにより、単位比表面積あたりのシラノール基
濃度を算出した。封鎖率は粒子の表面封鎖処理前後のシ
ラノール基濃度比から算出した。B. Particle surface silanol group blocking rate The particles were dried under reduced pressure at 100 ° C. for 3 hours, reduced with lithium aluminum hydride in dioxane, and the amount of generated hydrogen was quantitatively analyzed by gas chromatography to determine the concentration of silanol groups per unit weight ( / G), and the resulting value was divided by the specific surface area ( m 2 / g ) of the particles separately determined by the BET method, thereby calculating the silanol group concentration per unit specific surface area. The sealing ratio was calculated from the silanol group concentration ratio before and after the surface sealing treatment of the particles.
【0029】C.ポリエステルの極限粘度 o−クロロフェノールに溶解し、25℃で測定した。C. Intrinsic viscosity of polyester The polyester was dissolved in o-chlorophenol and measured at 25 ° C.
【0030】D.紡糸パック内圧上昇 実施例で示す紡糸時の紡糸パック内圧を1時間あたりの
上昇量に換算して示した。内圧上昇が低いものほど、ポ
リエステルへの粒子分散性が良好であることを示す。D. Increase in spinning pack internal pressure The spinning pack internal pressure during spinning shown in Examples was converted into the amount of increase per hour and shown. The lower the internal pressure rise, the better the particle dispersibility in the polyester.
【0031】E.tanδのピーク温度Tmax 東洋ボールドウィン社製バイブロンDDV−II型を用
い、振動数110Hz、昇温速度3℃/分でtanδ−
温度曲線を求め、tanδのピークに対応する温度を読
み取った。E. tan δ peak temperature Tmax Using a Vibron DDV-II type manufactured by Toyo Baldwin Co., Ltd., using a vibron DDV-II at a frequency of 110 Hz and a heating rate of 3 ° C./min.
A temperature curve was determined, and the temperature corresponding to the peak of tan δ was read.
【0032】F.密度 25℃に設定された恒温水槽中にn−ヘプタンと四塩化
炭素よりなる密度勾配管を作成して、常法により測定し
た。F. A density gradient tube made of n-heptane and carbon tetrachloride was prepared in a thermostatic water bath set at a density of 25 ° C., and measurement was performed by a conventional method.
【0033】G.複屈折率 ベレックコンペンセータを装着した偏光顕微鏡を用い、
常法により求めた。G. Birefringence Using a polarizing microscope equipped with a Berek compensator,
It was determined by an ordinary method.
【0034】H.白粉状態 ウォータージェットルームにタテ糸として供給し、筬に
おける白粉発生の状況を洗浄した筬を用い、製織スター
トして24時間後に観察した。H. White powder state A warp yarn was supplied to the water jet loom as a warp yarn, and the state of white powder generation in the reed was observed using a cleaned reed 24 hours after weaving was started.
【0035】I.織物の風合い 縦糸に30デニール12フィラメントのポリエステル繊
維を用い、サンプルを横糸として、36.5本/cmの
密度で製織し、常法により精練、染色して染色布帛を得
た。得られた布帛を官能評価により、ソフト風合いのも
のを○、硬いものを×、硬目のものを△とした。I. Texture of Woven Fabric A 30-denier 12-filament polyester fiber was used for the warp yarn, the sample was woven at a density of 36.5 yarns / cm as the weft yarn, and the fabric was scoured and dyed by a conventional method to obtain a dyed fabric. According to the sensory evaluation, the obtained cloth was evaluated as ○ for a soft texture, × for a hard texture, and Δ for a hard texture.
【0036】実施例1 四塩化ケイ素と水素混合物を空気中で加熱し加水分解し
て得られた平均一次粒子径12mμの酸化ケイ素を、ヘ
キサメチルジシラザンで反応させて、表面シラノール基
の封鎖率が60%の表面処理酸化ケイ素粒子を得た。2
60℃に設定した東芝機械社製二軸混練機において、常
法により得た極限粘度が0.68dl/gのポリエチレ
ンテレフタレートのチップを溶融した状態で、上記酸化
ケイ素粒子を含有量3重量%となるように添加、混合し
脱気しながら押出して極限粘度が0.66dl/gのチ
ップを得た。Example 1 A silicon oxide having an average primary particle diameter of 12 μm obtained by heating and hydrolyzing a mixture of silicon tetrachloride and hydrogen in the air was reacted with hexamethyldisilazane to block the silanol groups on the surface. Obtained surface-treated silicon oxide particles of 60%. 2
In a twin-screw kneader manufactured by Toshiba Machine Co., set at 60 ° C., the above-mentioned silicon oxide particles were contained in an amount of 3% by weight in a state where polyethylene terephthalate chips having an intrinsic viscosity of 0.68 dl / g obtained by a conventional method were melted. The mixture was extruded while being added, mixed and degassed to obtain chips having an intrinsic viscosity of 0.66 dl / g.
【0037】これを、上記0.68dl/gのポリエチ
レンテレフタレートとブレンドして酸化ケイ素の含有量
が0.25重量%となるように仕込み、孔径0.17m
mの18ホール口金、100メッシュサンドおよび絶対
濾過径が10μmのステンレス製不織布フィルターを使
用して、紡糸温度302℃、35cmの保温ゾーン、5
0cmの冷却ゾーンを通過させ、冷却ゾーン直後に油剤
を付与して、50デニール18フィラメントの糸条を交
絡を付与しつつ、紡糸速度7000m/分で引取り、紙
管に巻取った。なお、パック内圧上昇量は0.08kg
/cm2 /hrと少なく、ポリエステルへの粒子分散性
は良好であった。得られた繊維のtanδのピーク温度
Tmax、密度、複屈折率、および製織時の白粉観察結
果を、表1に示す。This was blended with the above 0.68 dl / g polyethylene terephthalate and charged so that the silicon oxide content was 0.25% by weight, and the pore diameter was 0.17 m.
m 18 hole, 100 mesh sand and a stainless steel non-woven fabric filter having an absolute filtration diameter of 10 μm, a spinning temperature of 302 ° C. and a heat retention zone of 35 cm.
After passing through a 0 cm cooling zone, an oil agent was applied immediately after the cooling zone, and a 50-denier 18-filament yarn was taken up at a spinning speed of 7000 m / min while being entangled, and wound around a paper tube. The pack internal pressure rise is 0.08kg
/ Cm 2 / hr, and the particle dispersibility in polyester was good. Table 1 shows the tan δ peak temperature Tmax, density, birefringence, and observation results of white powder during weaving of the obtained fibers.
【0038】実施例2、3、比較例1、2 それぞれ表1に示すような表面シラノール基の封鎖率の
表面処理酸化ケイ素粒子を用いた以外は実施例1と同様
にして、ポリエステルチップ、糸を得た。結果を表1に
示すが、表面封鎖率が低くなるに従いポリエステルへの
粒子分散性が低下してパック内圧上昇量が大きくなると
ともに安定して紡糸できなくなり、また表面封鎖率が4
0%未満では製織時に白粉が発生した。Examples 2 and 3 and Comparative Examples 1 and 2 Polyester chips and yarns were prepared in the same manner as in Example 1 except that surface-treated silicon oxide particles having a surface silanol group blocking ratio as shown in Table 1 were used. I got The results are shown in Table 1. As the surface sealing ratio decreases, the particle dispersibility in the polyester decreases, the amount of increase in the internal pressure of the pack increases, the spinning cannot be performed stably, and the surface sealing ratio is 4%.
If it is less than 0%, white powder was generated during weaving.
【0039】[0039]
【表1】 実施例4〜6、比較例3〜5 それぞれ表2に示すような表面処理剤を用い、実施例1
と同程度の表面封鎖率となるような粒子を用いた以外
は、実施例1と同様にして、ポリエステルチップ、糸を
得た。なお、実施例6では、比較例5で使用した表面処
理酸化ケイ素粒子をさらにヘキサメチルジシラザンで表
面処理して用いた。トリメチルシリル誘導体以外の表面
処理剤を用いると、ポリエステルへの粒子分散性が悪
く、また紡糸速度7000m/分では糸切れが多発して
巻き取れなかった。[Table 1] Examples 4 to 6 and Comparative Examples 3 to 5 The surface treatment agents shown in Table 2 were used, and Example 1 was used.
Polyester chips and yarns were obtained in the same manner as in Example 1 except that particles having a surface sealing rate similar to that of Example 1 were used. In Example 6, the surface-treated silicon oxide particles used in Comparative Example 5 were further subjected to surface treatment with hexamethyldisilazane. When a surface treating agent other than the trimethylsilyl derivative was used, the particle dispersibility in the polyester was poor, and at a spinning speed of 7000 m / min, thread breakage occurred frequently and could not be wound.
【0040】[0040]
【表2】 比較例6〜8 それぞれ表3に示すような粒子のエチレングリコールス
ラリーを、実施例1で示したベースポリエステルと同様
にして重合時に0.25重量%となるように添加して重
合を完結した以外は、実施例1と同様にして、ポリエス
テルチップ、糸を得た。いずれもパック内圧上昇量がや
や大きくポリエステルへの粒子分散性が劣り、糸切れが
発生して安定して巻き取れなかったり、製織時に白粉が
発生した。[Table 2] Comparative Examples 6 to 8 Except that the polymerization was completed by adding an ethylene glycol slurry of the particles shown in Table 3 in the same manner as in the base polyester shown in Example 1 so as to be 0.25% by weight at the time of polymerization. In the same manner as in Example 1, polyester chips and yarns were obtained. In each case, the amount of increase in the internal pressure of the pack was slightly large, the dispersibility of the particles in the polyester was inferior, the yarn was broken, and the yarn could not be stably wound, or white powder was generated during weaving.
【0041】比較例9 酸化ケイ素粒子を添加しないポリエステルを実施例1と
同様の紡糸条件で糸を得た、結果を表3に示すが、製織
時に白粉が発生した。Comparative Example 9 A polyester without silicon oxide particles was obtained under the same spinning conditions as in Example 1. The results are shown in Table 3. As shown in Table 3, white powder was generated during weaving.
【0042】[0042]
【表3】 実施例7〜9、比較例10、11 それぞれ表4に示すような平均一次粒子径の酸化ケイ素
粒子を用いて表面処理させた以外は実施例1と同様にし
て、ポリエステルチップ、糸を得た。平均一次粒子径が
5〜50mμを外れるとポリエステルへの粒子分散性が
低下してパック内圧上昇量が大きくなるとともに、製織
時に白粉が発生した。[Table 3] Examples 7 to 9, Comparative Examples 10 and 11 Polyester chips and yarns were obtained in the same manner as in Example 1 except that the surface treatment was performed using silicon oxide particles having an average primary particle diameter as shown in Table 4, respectively. . If the average primary particle size is out of the range of 5 to 50 μm, the dispersibility of the particles in the polyester decreases, the amount of increase in the internal pressure of the pack increases, and white powder is generated during weaving.
【0043】[0043]
【表4】 実施例10、11、比較例12、13 それぞれ表5に示すようにチップブレンド比を変えて紡
糸した以外は実施例2と同様にして糸を得た。粒子含有
量が0.02〜2.0重量%を外れると、製織時に白粉
が発生した。[Table 4] Examples 10 and 11 and Comparative Examples 12 and 13 Yarns were obtained in the same manner as in Example 2 except that spinning was performed while changing the chip blend ratio as shown in Table 5. When the particle content was out of the range of 0.02 to 2.0% by weight, white powder was generated during weaving.
【0044】[0044]
【表5】 実施例12、13、比較例14 それぞれ表6に示すような紡糸速度で紡糸した以外は実
施例2と同様にして糸を得た。紡糸速度が5500m/
分未満であると、糸の密度、複屈折率が低く、製織時に
白粉が発生した。[Table 5] Examples 12, 13 and Comparative Example 14 Yarns were obtained in the same manner as in Example 2 except that spinning was performed at spinning speeds as shown in Table 6, respectively. Spinning speed is 5500m /
If it is less than 10 minutes, the yarn density and the birefringence are low, and white powder was generated during weaving.
【0045】比較例15 紡糸速度3000m/分で一旦巻き取った後、延伸倍率
1.7倍で延伸した以外は実施例2と同様にして糸を得
た。結果を表6に示すが、Tmaxが高く、糸の密度が
低く、製織布帛の風合いが硬かった。Comparative Example 15 A yarn was obtained in the same manner as in Example 2 except that the yarn was once wound at a spinning speed of 3000 m / min and then stretched at a draw ratio of 1.7. The results are shown in Table 6, where the Tmax was high, the yarn density was low, and the texture of the woven fabric was hard.
【0046】[0046]
【表6】 比較例16 湿式法、すなわち珪酸曹達と硫酸を反応させて濾過・水
洗・乾燥して得た平均一次粒子径28mμの酸化ケイ素
を使用して表面処理した以外は実施例1と同様にして、
ポリエステルチップ、糸を得た。結果を表7に示すが、
ポリエステルへの粒子分散性が劣り、製織時に白粉が発
生した。[Table 6] Comparative Example 16 The same procedure as in Example 1 was carried out, except that the surface treatment was carried out using a wet method, that is, silicon oxide having an average primary particle diameter of 28 mμ obtained by reacting silicate soda and sulfuric acid, filtering, washing and drying, to obtain
Polyester chips and yarns were obtained. Table 7 shows the results.
Particle dispersibility in polyester was poor, and white powder was generated during weaving.
【0047】実施例14 表面処理前に焼成して乾式法酸化ケイ素に匹敵する表面
物性を付与させた以外は比較例16と同様にして、ポリ
エステルチップ、糸を得た。結果を表7に示すが、本発
明の範囲であり、製織時に白粉のない良好な糸が得られ
た。[0047] Except that was granted surface physical properties by firing before Example 14 Surface treatment comparable to dry-type method silicon oxide in the same manner as in Comparative Example 16, to give polyester chips, the thread. The results are shown in Table 7, which is within the scope of the present invention, and a good yarn without white powder was obtained during weaving.
【0048】[0048]
【表7】 実施例15 連続重合し、最終の重合装置から吐出された溶融ポリエ
チレンテレフタレート(極限粘度0.67dl/g)を
連続的に二軸混練機へ直接フィードした以外は、実施例
8と同様にして混練チップ、糸を得た。結果を表8に示
すが、実施例8と同じく製織時に白粉のない良好な糸が
得られた。[Table 7] Example 15 Kneading was carried out in the same manner as in Example 8, except that continuous polymerization was performed and the molten polyethylene terephthalate (intrinsic viscosity: 0.67 dl / g) discharged from the final polymerization apparatus was continuously directly fed to a twin-screw kneader. Chips and yarns were obtained. The results are shown in Table 8. As in Example 8, good yarn without white powder was obtained during weaving.
【0049】実施例16 二軸混練機へ粒子含有量0.5重量%となるように添
加、混合し脱気しながら押出したチップをそのまま紡糸
した以外は、実施例8と同様にして混練チップ、糸を得
た。結果を表8に示すが、実施例8と同じく製織時に白
粉のない良好な糸が得られた。Example 16 Kneaded chips were prepared in the same manner as in Example 8, except that the chips extruded while being added, mixed, and degassed into a twin-screw kneader so as to have a particle content of 0.5% by weight were directly spun. I got a thread. The results are shown in Table 8. As in Example 8, good yarn without white powder was obtained during weaving.
【0050】比較例17 最終の重合装置の前(溶融ポリエチレンテレフタレート
の極限粘度0.43dl/g)に、表面処理酸化ケイ素
粒子を添加して重合装置から吐出させた以外は、実施例
15と同様にして混練チップを得た。結果を表8に示す
が、ポリエステルへの粒子分散性が悪く、紡糸速度70
00m/分では糸切れが多発して巻き取れなかった。Comparative Example 17 Same as Example 15 except that surface-treated silicon oxide particles were added before the final polymerization apparatus (intrinsic viscosity of molten polyethylene terephthalate: 0.43 dl / g) and discharged from the polymerization apparatus. To obtain a kneaded chip. The results are shown in Table 8, where the particle dispersibility in the polyester was poor and the spinning speed was 70%.
At 00 m / min, thread breakage occurred frequently and could not be wound.
【0051】[0051]
【表8】 [Table 8]
【0052】[0052]
【発明の効果】本発明のポリエステル繊維は、酸化ケイ
素粒子のポリエステルとの親和性が高く、表層部に均一
に分散するので周囲のポリマを硬くするため、高次工程
での白粉やスカム汚れを防止しつつ、良好な風合いの布
帛の得られる繊維を供給することができるようになっ
た。また、高次工程以外にも、例えば製糸工程での糸道
ガイドでの擦過による白粉や、白粉に起因する最終製品
の点状の染色欠点を防止することができる。粒子分散性
が極めて良好であるので、パック内圧上昇が小さく、ま
た糸切れも少ないなど安定して操業することが可能であ
る。The polyester fiber of the present invention has a high affinity with the polyester of the silicon oxide particles and is uniformly dispersed in the surface layer, so that the surrounding polymer is hardened. Thus, it is possible to supply fibers from which a fabric having a good texture can be obtained. In addition to the high-order process, it is possible to prevent, for example, white powder due to abrasion with a yarn path guide in a yarn-making process, and dot-like defective defects of a final product due to the white powder. Since the particle dispersibility is extremely good, it is possible to operate stably such that the rise in the internal pressure of the pack is small and the yarn breakage is small.
フロントページの続き (56)参考文献 特開 昭58−149321(JP,A) 特開 昭58−149323(JP,A) 特開 昭60−151374(JP,A) 特開 平4−65519(JP,A) (58)調査した分野(Int.Cl.7,DB名) D01F 6/62 301 - 6/92 309 D01F 6/62 301 - 308 Continuation of the front page (56) References JP-A-58-149321 (JP, A) JP-A-58-149323 (JP, A) JP-A-60-151374 (JP, A) JP-A-4-65519 (JP) , A) (58) Field surveyed (Int. Cl. 7 , DB name) D01F 6/62 301-6/92 309 D01F 6/62 301-308
Claims (5)
チルシリル誘導体で表面処理して粒子表面のシラノール
基の40%以上を封鎖した、平均一次粒子径が5〜50
mμの酸化ケイ素粒子を0.02〜2.0重量%含有
し、tanδのピーク温度Tmaxが125℃以下、密
度が1.370g/cm3 以上、複屈折率が0.085
以上であることを特徴とする耐摩耗性の良好なポリエス
テル繊維。A silicon oxide particle synthesized by a dry method is surface-treated with a trimethylsilyl derivative to block at least 40% of silanol groups on the particle surface, and has an average primary particle diameter of 5 to 50.
The oxidation silicon particles mμ containing 0.02 to 2.0 wt%, the peak temperature Tmax of tanδ is 125 ° C. or less, density of 1.370g / cm 3 or more, the birefringence index is 0.085
A polyester fiber having good abrasion resistance, characterized in that:
粒子をトリメチルシリル誘導体で表面処理して粒子表面
のシラノール基の40%以上を封鎖した、平均一次粒子
径が5〜50mμの酸化ケイ素粒子を0.02〜2.0
重量%含有し、tanδのピーク温度Tmaxが125
℃以下、密度が1.370g/cm 3 以上、複屈折率が
0.085以上であることを特徴とする耐摩耗性の良好
なポリエステル繊維。 2. A silicon oxide synthesized by a wet method and further calcined.
Surface treatment of particles with trimethylsilyl derivative
Average primary particles that block 40% or more of the silanol groups of
Silicon oxide particles having a diameter of
% By weight and a peak temperature Tmax of tan δ of 125
° C or less, density is 1.370 g / cm 3 or more, and birefringence is
Good wear resistance characterized by being 0.085 or more
Polyester fiber.
ルジシラザンで表面処理して、粒子表面のシラノール基
の60%以上を封鎖した酸化ケイ素粒子を含有すること
を特徴とする請求項1または2記載の耐摩耗性の良好な
ポリエステル繊維。3. A surface treated with hexamethyldisilazane trimethylsilyl derivative, resistance of claim 1 or 2, wherein the containing silicon oxide particles were blocked more than 60% of the silanol groups on the particle surface Polyester fiber with good abrasion.
m/分以上で溶融紡糸する際に乾式法で合成した酸化ケ
イ素粒子をトリメチルシリル誘導体で表面処理して粒子
表面のシラノール基の40%以上を封鎖した、平均一次
粒子径が5〜50mμの酸化ケイ素粉末を、極限粘度が
0.50dl/g以上のポリエステルに直接添加、混合
し、ポリエステル繊維中に0.02〜2.0重量%含有
することを特徴とする耐摩耗性の良好なポリエステル繊
維の製造方法。4. A spinning speed of 5500 for a polyester composition.
Oxidation ketone synthesized by dry method when melt spinning at m / min or more
The Lee particles were blocked more than 40% of the surface silanol groups treated with the particle surfaces with trimethylsilyl derivative, the oxidation of silicon powder having an average primary particle diameter of 5~50Emumyu, intrinsic viscosity greater than 0.50 dl / g polyester Add directly to the mixture
A method for producing a polyester fiber having good abrasion resistance , comprising 0.02 to 2.0% by weight of the polyester fiber.
m/分以上で溶融紡糸する際に湿式法で合成し、更に焼
成した酸化ケイ素粒子をトリメチルシリル誘導体で表面
処理して粒子表面のシラノール基の40%以上を封鎖し
た、平均一次粒子径が5〜50mμの酸化ケイ素粉末
を、極限粘度が0.50dl/g以上のポリエステルに
直接添加、混合し、ポリエステル繊維中に0.02〜
2.0重量%含有することを特徴とする耐摩耗性の良好
なポリエステル繊維の製造方法。 5. A spinning speed of 5500 for a polyester composition.
When melt spinning at m / min or more, it is synthesized by a wet method and
Surface of formed silicon oxide particles with trimethylsilyl derivative
Treatment to block more than 40% of silanol groups on the particle surface
Silicon oxide powder having an average primary particle diameter of 5 to 50 mμ
Into a polyester having an intrinsic viscosity of 0.50 dl / g or more.
Direct addition and mixing, 0.02-
Good wear resistance characterized by containing 2.0% by weight
Method for producing a simple polyester fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16935794A JP3277703B2 (en) | 1994-07-21 | 1994-07-21 | Polyester fiber having good abrasion resistance and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16935794A JP3277703B2 (en) | 1994-07-21 | 1994-07-21 | Polyester fiber having good abrasion resistance and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0835118A JPH0835118A (en) | 1996-02-06 |
| JP3277703B2 true JP3277703B2 (en) | 2002-04-22 |
Family
ID=15885085
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16935794A Expired - Fee Related JP3277703B2 (en) | 1994-07-21 | 1994-07-21 | Polyester fiber having good abrasion resistance and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3277703B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012014309A1 (en) | 2010-07-29 | 2012-02-02 | 旭化成せんい株式会社 | Abrasion-resistant polyester fiber and woven/knitted product |
-
1994
- 1994-07-21 JP JP16935794A patent/JP3277703B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012014309A1 (en) | 2010-07-29 | 2012-02-02 | 旭化成せんい株式会社 | Abrasion-resistant polyester fiber and woven/knitted product |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0835118A (en) | 1996-02-06 |
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