JPH02242960A - Production of unidirectionally oriented nonwoven fabric and apparatus therefor - Google Patents
Production of unidirectionally oriented nonwoven fabric and apparatus thereforInfo
- Publication number
- JPH02242960A JPH02242960A JP1058384A JP5838489A JPH02242960A JP H02242960 A JPH02242960 A JP H02242960A JP 1058384 A JP1058384 A JP 1058384A JP 5838489 A JP5838489 A JP 5838489A JP H02242960 A JPH02242960 A JP H02242960A
- Authority
- JP
- Japan
- Prior art keywords
- nonwoven fabric
- filaments
- filament
- spun
- vibrating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004745 nonwoven fabric Substances 0.000 title claims description 101
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 239000012530 fluid Substances 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 39
- 238000009987 spinning Methods 0.000 claims abstract description 31
- 230000015271 coagulation Effects 0.000 claims description 10
- 238000005345 coagulation Methods 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000000839 emulsion Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 4
- 238000010030 laminating Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 claims description 2
- 239000002657 fibrous material Substances 0.000 claims 1
- 230000001788 irregular Effects 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 description 11
- 239000000853 adhesive Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000005304 joining Methods 0.000 description 3
- 239000002998 adhesive polymer Substances 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229920003174 cellulose-based polymer Polymers 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000000578 dry spinning Methods 0.000 description 1
- 238000004049 embossing Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
- D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
- D04H3/05—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments in another pattern, e.g. zig-zag, sinusoidal
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Woven Fabrics (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高分子物質を溶融または溶解して紡糸してな
る不織布の製法および装置において、不織布を構成する
フィラメントを一方向に配列させた不織布のＭ法および
装置に間するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention provides a method and apparatus for producing a nonwoven fabric made by melting or spinning a polymeric substance, in which filaments constituting the nonwoven fabric are arranged in one direction. The present invention relates to M method and equipment for nonwoven fabrics.
〔従来技術及び本発明が解決しようとする問題点〕従来
のスパンボンド不織布は、カサ高性や風合いは良いが、
フィラメントがほぼランダムに配列しているため、タテ
ヨコ方向に寸法安定性が悪く、強度も小さかった。これ
らを解決する手段として、本発明人等は、先に特願昭６
２−１７３９２７号（以下光発明と略称する）に、不織
布をタテまたはヨコに延伸する方法および装置、および
タテ延伸した不織布とヨコ延伸した不織布を経緯積層す
る手段および紡糸したフィラメントを一方向に配列させ
る手段等について提案した。本発明はこのフィラメント
を一方向に配列した不織布を製造する別の新たな発明に
間し、先発明の追加的特許でもある。[Prior art and problems to be solved by the present invention] Conventional spunbond nonwoven fabrics have good bulk and texture, but
Since the filaments were arranged almost randomly, the dimensional stability in the vertical and horizontal directions was poor, and the strength was also low. As a means to solve these problems, the present inventors previously filed a patent application in 1983.
No. 2-173927 (hereinafter referred to as Hikari Invention) discloses a method and apparatus for vertically or horizontally stretching a nonwoven fabric, a means for warp-warp laminating a vertically stretched nonwoven fabric and a horizontally stretched nonwoven fabric, and a method for arranging spun filaments in one direction. We proposed ways to do so. The present invention is another new invention for manufacturing a nonwoven fabric in which filaments are arranged in one direction, and is an additional patent to the previous invention.
先発明でも述べたように、従来のランダム不織布を、単
にタテまたはヨコに延伸しても、フィラメント間をつな
いでいる絡みや接着が外れるだけのことが多く、フィラ
メントの延伸には到らず、不織布の強度アップにならな
いことが多い、そこで、一方向にフィラメントが配列し
た不織布をフィラメントの配列方向に延伸することによ
り、フィラメントの延伸も起こり、不織布の強度のアッ
プすることが判明した。不織布を構成するフィラメント
の種類により、延伸しなくて、単にフィラメントが配列
しているだけで、その配列方向に充分強度や寸法安定性
が出せるものもある。先発明では、熱風を使用して飛散
させたため、溶剤や分散媒体を使用した湿式や乾式また
はエマルジョン紡糸による不織布製造には適応が困難で
あった。As mentioned in the previous invention, even if conventional random nonwoven fabrics are simply stretched vertically or horizontally, the entanglements and adhesives that connect the filaments often come off, and the filaments cannot be stretched. In many cases, the strength of nonwoven fabrics cannot be increased. Therefore, it has been found that by stretching a nonwoven fabric in which filaments are arranged in one direction in the direction in which the filaments are arranged, the filaments are also stretched, and the strength of the nonwoven fabric is increased. Depending on the type of filaments constituting the nonwoven fabric, some nonwoven fabrics can provide sufficient strength and dimensional stability in the direction of arrangement simply by arranging the filaments without stretching. In the previous invention, hot air was used for scattering, so it was difficult to apply to nonwoven fabric production by wet, dry, or emulsion spinning using a solvent or dispersion medium.
また、先発明では、紡出されたフィラメントをまず巾方
向に旋回または振動させる手段として、やはり熱風で行
ったため、高分子物質の種類によってはフィラメントが
安定に旋回や振動してくれないために、その後の熱風を
交差させても安定して一方向に配列して°くれない場合
があった。In addition, in the previous invention, hot air was used as a means to first swirl or vibrate the spun filament in the width direction, so depending on the type of polymer material, the filament may not rotate or vibrate stably. Even if the hot air was then crossed, there were cases where the arrangement was not stable in one direction.
これらの問題を、鋭意研究した結果、湿式紡糸や乾式紡
糸、エマルジョン紡糸にも適応出来、どの様な紡出フィ
ラメントでも、安定に旋回や振動して、フィラメントを
一方向に配列性良く飛散させる製法や装置を発明するに
到った。As a result of intensive research into these problems, we have developed a manufacturing method that can be applied to wet spinning, dry spinning, and emulsion spinning, and allows any type of spun filament to stably swirl and vibrate to scatter the filaments in one direction with good alignment. He came to invent a device.
高分子物質を溶融させた溶融紡糸による不織布の製法に
おいて、紡出フィラメントを先発明のように風で飛散さ
せようとすると、その高分子物質の融点以上に加熱した
熱風を用いないと飛散が不十分て、塊やツブが生じたり
、飛散中が小さかったり、また配列が不十分などの問題
点があった。In the method of manufacturing nonwoven fabric by melt-spinning a polymeric material, if you try to scatter the spun filaments with wind as in the previous invention, the scattering will not occur unless you use hot air heated above the melting point of the polymeric material. However, there were problems such as lumps and bulges, small particles being scattered, and insufficient alignment.
多量のエアーを加熱するには熱エネルギイ的にも損失で
あり、熱風を勢い良く噴出すると周りの冷風を巻き込ん
で熱風湿度が低下してしまう問題点もあった。また、良
く飛散するためには、紡出したフィラメントが粘度が小
さく、曳糸性も大きくなければ飛散が不十分であるが、
紡糸する溶融ポリマーの温度は、ポリマーの熱安定性や
紡糸ＭＩｌｌの耐熱性の範囲より、おのずと限界があっ
た０以上の問題点を解決する手段として、ポリマーを溶
剤に溶解するか、液体中にエマルジョン状に分散させて
（以下簡略のため、溶液型紡糸液と称する）紡糸するこ
とにより、フィラメントを飛散させる流体も加熱する必
要がない、紡糸液の粘度も曳糸性の良い高分子量のポリ
マーを使用しても、紡糸液の濃度を下げることにより自
由に選択出来る。There is also a loss of thermal energy when heating a large amount of air, and there is also the problem that when hot air is jetted out vigorously, surrounding cold air is drawn in, reducing the humidity of the hot air. In addition, in order to scatter well, the spun filament must have a low viscosity and high spinnability, otherwise scattering will be insufficient.
The temperature of the molten polymer to be spun has a natural limit due to the thermal stability of the polymer and the heat resistance range of the spun MIll.As a means of solving the above-mentioned problems, the polymer can be dissolved in a solvent or immersed in a liquid. A high-molecular-weight polymer that is dispersed in an emulsion (hereinafter referred to as a solution-type spinning solution for simplicity) and then spun, so there is no need to heat the fluid that scatters the filaments, and the spinning solution has a high viscosity and good spinnability. Even if used, it can be freely selected by lowering the concentration of the spinning solution.
フィラメントを飛散させる前段階として、フィラメント
を敢闘から数＋１望ましくは５鴎より５０５ｍ＋の範囲
の据輻で、数１０回／分ないし数百回７秒、望ましくは
３００回／分以上の周期で旋回または往復運動している
必要がある（以下簡略のため振動と称することにする）
、先発明のもう一つの問題点は、この振動を紡口近傍の
微弱な熱風に頼っていたが、ポリマーの種類や粘度によ
っては不安定で、安定な振動が出来ない場合があった。As a preliminary step to scattering the filament, the filament is rotated several tens of times per minute to several hundred times for 7 seconds, preferably 300 times per minute or more, at a fixed distance of 505 m+ from Kakuto to several +1, preferably from 5 to 5. Or it must be in reciprocating motion (hereinafter referred to as vibration for simplicity)
Another problem with the previous invention was that this vibration relied on weak hot air near the spinneret, but depending on the type and viscosity of the polymer, it was unstable and could not produce stable vibration.
本発明では、紡口そのものを振動させることにより、全
てのポリマーの融解や、溶液型紡糸液でも、粘度にかか
わらず安定に振動させることが出来ることを見い出した
ことにある。実験の結果、振動の振幅の範囲が１ｍＩＩ
より以下であると、振動している効果は見いだせず、５
−以上あることが望ましい。また、振幅の範囲が３００
−を越える広い巾で振幅すると飛散の均一性を保つこと
が出来ず、望ましくは５Ｃ１ｗ以下であることが望まし
いことが判った。振動の周期もあまり遅い６０回／分以
下では、不織布の生産性も悪く、飛散したフィラメント
の集積も不十分である。不織布を形成させるためには、
望ましくは３００回／分以上で振動する必要がある。さ
らに望ましくは３０回／秒（１８００回／分）以上の周
期で旋回または往復運動している状態では、その後の飛
散が安定していた。The present invention is based on the discovery that by vibrating the spinneret itself, it is possible to stably vibrate all types of polymers and even solution-type spinning solutions regardless of their viscosity. As a result of the experiment, the range of vibration amplitude is 1 mII.
If it is less than 5, no oscillating effect can be found.
- It is desirable that there be at least one. Also, the amplitude range is 300
It has been found that if the amplitude is wider than -, the uniformity of scattering cannot be maintained, and it is desirable that the amplitude be 5C1w or less. If the frequency of vibration is too slow, less than 60 times/min, the productivity of the nonwoven fabric will be poor and the accumulation of scattered filaments will be insufficient. In order to form a nonwoven fabric,
Desirably, it is necessary to vibrate at 300 times/min or more. More preferably, in a state of rotating or reciprocating at a cycle of 30 times/second (1800 times/minute) or more, subsequent scattering was stable.
上記の溶液型紡糸液や紡口そのものを振動させる発明に
よって、フィラメントを振動させたり飛散させる流体と
して、加熱気体ばかりでなく、加熱されていない気体、
液体または蒸気、または液体を含む気体でも使用できる
ことが判明した。さらに、これらの流体に勢いをつける
ために重さのある固体や接着性のある固体の微粉末を混
入しても良い、これらの流体は振動や飛散ばかりでなく
、フィラメントの凝固や接着性を助ける流体である場合
もある。With the above-mentioned invention that vibrates the solution-type spinning solution and the spinneret itself, not only heated gas but also unheated gas can be used as the fluid that vibrates and scatters the filaments.
It turns out that liquids or vapors, or even gases containing liquids, can be used. Furthermore, in order to give momentum to these fluids, fine powders of heavy solids or adhesive solids may be mixed.These fluids not only vibrate and scatter, but also cause coagulation and adhesiveness of the filament. It may also be a helping fluid.
紡出されたフィラメントを振動させる方法として、紡口
近傍のエアーによる方法と紡口の振動の２つの方法につ
いて述べた。他の方法として、電場や磁場を用い、その
電場や磁場の極性を変化させて振動を与えても良い０例
えば、紡出フィラメントに高電圧を掛け、帯電されたフ
ィラメントにプラス、マイナスの電場を交互に与え、紡
出されたフィラメントを振動させることも出来る。この
方法は紡口より多数本のフィラメントを紡出する場合に
、紡出フィラメント同士がまとまらないで良く離散する
ので、特に適している０以上のエアーや紡口の振動や電
荷なとの種々の方法を併用し・でも良い。Two methods of vibrating the spun filament have been described: one using air near the spinneret and the other using vibration of the spinneret. Another method is to use an electric field or a magnetic field and change the polarity of the electric field or magnetic field to give vibration. For example, a high voltage is applied to the spun filament, and a positive or negative electric field is applied to the charged filament. It is also possible to vibrate the spun filament by applying it alternately. This method is particularly suitable when spinning a large number of filaments from the spinneret, since the spun filaments do not come together and are often dispersed. It is okay to use both methods.
本発明のもう一つの特徴として、フィラメントの断面が
流体の作用を受けやすいように真円よりずれた楕円形断
面や異形断面であるように、紡口を長方形、楕円、異形
断面など真円よりずれた形状にすることが有効であるこ
とを見いだした点にある。このような真円よりずれた断
面のフィラメントにすることにより、少量で低圧の流体
でも、フィラメントの飛散も配列の程度も良い。Another feature of the present invention is that the cross section of the filament is an elliptical cross-section or a modified cross-section that deviates from a perfect circle so as to be easily affected by the fluid. The point is that it was discovered that it is effective to make the shapes shifted. By making the filament have a cross section that is deviated from a perfect circle, the filament can be scattered and arranged well even in a small amount of low-pressure fluid.
紡糸されるフィラメントはモノフィラメント状に単独の
フィラメントでも良いが、マルチフィラメント状に多数
本同時に紡糸し、同時に振動し、同時に飛散させると、
生産効率も良い、また不織布のメルトブロー法のように
、紡口より気体と一緒に噴出さ、噴出したフィラメント
を振動させ、飛散させても良い。The spun filament may be a single filament in the form of a monofilament, but if a large number of filaments are spun simultaneously in the form of a multifilament, vibrated at the same time, and scattered at the same time,
Production efficiency is also good, and like in the melt-blowing method for nonwoven fabrics, filaments may be ejected from a spinneret together with gas, and the ejected filaments may be vibrated and scattered.
振動して次の飛散に向かうフィラメントは、まだ完全に
は凝固しておらず、２倍以上のドラフト性が残っている
必要があり、この段階で凝固が完了してドラフト性を失
っている場合は、次の飛散プロセスに移っても、飛散が
不十分で配列も良くないことを実験より確かめた。望ま
しくは、１０倍以上、更に望ましくは１００倍以上のド
ラフト性があると飛散したフィラメントの巾も広く、配
列度も配列の均一性も良い、溶液型紡糸液による場合で
、紡糸直後に凝固浴を通し、凝固浴出口で振動させるこ
とによりフィラメントを振動させても良い、この場合、
凝固が完全には終了しているとドラフト性が漸くなるの
で、少なくとも２倍以上のドラフト性のある状態で飛散
工程に進む必要がある。The filament that vibrates and heads to the next scattering has not yet been completely solidified and must have more than twice the draft ability, and if the filament has completed solidification at this stage and has lost its draft ability. confirmed through experiments that even after moving on to the next scattering process, the scattering was insufficient and the arrangement was not good. Preferably, if the draft property is 10 times or more, and more preferably 100 times or more, the width of the scattered filaments will be wide, and the degree of alignment and uniformity of alignment will be good.When using a solution-type spinning solution, it is preferable to use a coagulation bath immediately after spinning. The filament may be vibrated by passing it through the coagulation bath and vibrating it at the coagulation bath outlet; in this case,
If the coagulation is completely completed, the draft property will gradually decrease, so it is necessary to proceed to the scattering step in a state where the draft property is at least twice as high.
次ぎに、振動しているフィラメントを飛散させる流体の
当て方について説明する。これには２つの方法があり、
その一つは、振動しているフィラメントを中心にして側
方よりほぼ左右対称の一対以上の流体をフィラメント上
で正面衝突させて、フィラメントを流体の噴出方向と直
角方向に飛散させる方法である。もう一つの方法は、振
動しているフィラメントを中心にして側方よりほぼ左右
対称の一対以上の流体を、フィラメントの振動範囲で交
差させて、フィラメントを流体の噴出方向とほぼ平行方
向に飛散させる方法である。この場合、左右の流体を交
互に間欠的に噴出して、流体の噴出方向にそれぞれフィ
ラメントを飛散させることも出来、これも本発明に含ま
れる。この左右の流体を間欠的に出す場合は、左右の流
体を同時に出した場合、正面衝突するような焦点に噴出
さしても良い、これら２つの方法で飛散させる流体の発
生源は一対とは限らず、一つの紡口に対して２対、３対
設置した方が効率が良いが、以下の説明では煩雑さを避
けるために、一対について述べる。これらの２°っの方
法については、図面の簡単な説明の項で詳述する。Next, a method of applying fluid to scatter the vibrating filament will be explained. There are two ways to do this:
One method is to cause a pair or more of fluids to collide head-on on the filament with a pair of fluids that are approximately bilaterally symmetrical from the sides of a vibrating filament, thereby scattering the filament in a direction perpendicular to the jetting direction of the fluid. Another method is to intersect a pair or more of fluids that are approximately symmetrical from the sides around a vibrating filament within the filament's vibration range, and scatter the filaments in a direction that is approximately parallel to the jetting direction of the fluid. It's a method. In this case, the left and right fluids may be alternately and intermittently ejected to scatter filaments in the respective fluid ejection directions, which is also included in the present invention. When the left and right fluids are ejected intermittently, when the left and right fluids are ejected at the same time, they may be ejected at a focal point where they collide head-on.The sources of the fluids that are scattered in these two methods are not necessarily a pair. Although it is more efficient to install two or three pairs of spindles for one spindle, in the following explanation, one pair will be described to avoid complexity. These 2° methods are described in detail in the brief description of the drawings.
本発明の一方向配列不織布は、先発明の方法により、フ
ィラメントの配列方向へ延伸や圧延することが望ましい
場合が多い、延伸や圧延の方法は先発明で詳述した０本
発明の方法による一方向配列不織布は、厚みの均一性が
良く、フィラメントの配列度もよく、ツブや塊も出難い
ことより、延伸に特に適した不織布となる０本発明の方
法において、一方向配列不織布を製造し、さらにこれに
積層する形で先の不織布とは直角方向に配列した不織布
を製造し、積層した不織布のそれぞれのフィラメントの
配列方向に２軸的に延伸することによる直交不織布を製
造することもできる。この場合の２軸延伸は逐次２軸で
も同時２軸でも良い。It is often desirable to stretch or roll the unidirectionally aligned nonwoven fabric of the present invention in the direction in which the filaments are arranged by the method of the earlier invention. The unidirectionally aligned nonwoven fabric has good thickness uniformity, good filament alignment, and does not easily generate lumps or lumps, making it a nonwoven fabric particularly suitable for stretching. Furthermore, it is also possible to produce a perpendicular nonwoven fabric by laminating a nonwoven fabric arranged in a direction perpendicular to the previous nonwoven fabric, and biaxially stretching the laminated nonwoven fabric in the direction in which each filament is arranged. . In this case, the biaxial stretching may be carried out sequentially or simultaneously.
また、ｌ軸延伸でも２軸延伸でも、延伸前に不織布を軽
く接着または接合しておくことが延伸による強度アップ
に適している場合が多い、延伸後は接着や機械的接合に
よりフィラメント間を接合しておくことが強い不織布と
しては望まれる。In addition, in both l-axis stretching and biaxial stretching, lightly adhering or joining the nonwoven fabric before stretching is often suitable for increasing the strength by stretching.After stretching, the filaments are joined by adhesive or mechanical bonding. It is desirable for a strong non-woven fabric to be kept as long as possible.
本発明の一方向配列不織布は、それ単独として使用する
ことも出来るが、−船釣には、それと直角方向に配列し
た不織布または繊維材ウェブ（例えば、糸または延伸テ
ープを一定間隔で配列したもの、トウを拡幅したもの、
紡績のカード上がりウェブなと）を組合わせて、直交不
織布の形態で使用することも多い。組み合わせる工程は
、不織布製造ラインで行っても良いし、別ラインで行っ
ても良い。組み合わせる素材は、同様の製法で、ただ流
体の噴出方向の違いで、タテ方向とヨコ方向に配列した
不織布を組み合わせても良い。また、斜め方向に配列し
た不織布を互いの配列方向が直交するように組み合わせ
ても良い。ここで直交と云うのは、厳密に角度９０度で
交わる場合のみでなく、３０〜１５０度で交わってもよ
い、斜交しているものに、タテ方向またはヨコ方向配列
の素材を朝み合わせて、３軸や４軸の不織布にすること
も出来る。また、組み合わせる素材は、同様な製法で、
配列方向のみ異なる素材ばかりでなく、全く別の素材、
また素材としては類似していても、製法の全く異なるも
のと絹み合わせることもできる。物性のバランス上、朝
み合わせる素材が、本発明の不織布のフィラメントの配
列方向と直交するように配列していることが望ましいこ
とが多い。The unidirectionally aligned nonwoven fabric of the present invention can be used alone; however, for boat fishing, nonwoven fabrics or fibrous webs (e.g. threads or stretched tapes arranged at regular intervals) aligned at right angles to the unidirectionally aligned nonwoven fabric of the present invention can be used alone. , widened toe,
It is often used in the form of an orthogonal non-woven fabric by combining it with a spun carded web. The combining process may be performed on a nonwoven fabric production line, or may be performed on a separate line. The materials to be combined may be a combination of nonwoven fabrics arranged in the vertical and horizontal directions using the same manufacturing method, but with a difference in the direction of fluid ejection. Alternatively, nonwoven fabrics arranged diagonally may be combined so that their arrangement directions are orthogonal to each other. Here, orthogonal means not only when they intersect at a strictly 90 degree angle, but also when they intersect at an angle of 30 to 150 degrees. It is also possible to make a 3- or 4-axis nonwoven fabric. In addition, the materials to be combined are made using the same manufacturing method.
Not only materials that differ only in the arrangement direction, but also completely different materials,
Also, even though the materials are similar, silk can be combined with completely different manufacturing methods. In view of the balance of physical properties, it is often desirable that the materials to be mixed be arranged perpendicularly to the direction in which the filaments of the nonwoven fabric of the present invention are arranged.
組み合わせて接合する方法は、粉末やエマルジョンなど
の接着剤を利用しても良いし、ニードルバンチなどの機
械的接合を行っても良い。また、本発明の不織布は非常
にファインデニールになるので・不織布の製造ラインで
組み合わせれば、なんら接着剤が不要で、ファインフィ
ラメント同士の絡み合いによる接合も可能である。また
、本発明の不織布の製造の際、多数の紡口の中に接着性
を持ったフィラメントを紡出するようにして、不織布自
身に接着剤を含むようにして、後で単に加熱のみで他の
素材と接合するようにすることも出来る。また、溶液型
紡糸液の場合、一方向配列フィラメントとして飛散し集
積した後でも、凝固が完了しておらず、そのためにまだ
自己接着性を持つものは、その接着性を利用してフィラ
メント同士の接着を行う。As for the method of combining and joining, adhesives such as powder or emulsion may be used, or mechanical joining such as needle bunching may be used. In addition, since the nonwoven fabric of the present invention has a very fine denier, if it is combined on a nonwoven fabric production line, no adhesive is required, and fine filaments can be joined by intertwining with each other. In addition, when manufacturing the nonwoven fabric of the present invention, filaments with adhesive properties are spun into a large number of spindles so that the nonwoven fabric itself contains an adhesive, and later it can be used with other materials simply by heating. It is also possible to connect it with In addition, in the case of a solution-type spinning solution, even after scattering and accumulating as unidirectionally aligned filaments, coagulation is not completed, and therefore those that still have self-adhesive properties can use their adhesive properties to bind filaments to each other. Perform gluing.
本発明を利用する有効な方法の一つとして、特願昭６３
−８１１８７号の追加的発明になるが、本発明の方法で
フィラメントをヨコ方向に配列させ、そのヨコに配列し
たフィラメントでタテ方向に走行する糸群の配列を固定
することが出来る。As one of the effective methods of utilizing the present invention, patent application No. 63
This is an additional invention of No.-81187, but by the method of the present invention, the filaments are arranged in the horizontal direction, and the arrangement of the thread groups running in the vertical direction can be fixed by the filaments arranged in the horizontal direction.
この場合のフィラメントとしては、接着性ポリマーであ
ることが望ましい、このように走行する糸群の配列固定
されたウェブは、特公昭５３−３８７８３号などのよう
な経緯積層機の緯ウェブとしても、利用することが出来
る。In this case, it is preferable that the filament be an adhesive polymer.A web in which the running thread group is arranged in a fixed manner can also be used as a weft web of a weft and weft laminating machine as disclosed in Japanese Patent Publication No. 53-38783. You can.
本発明に利用される不織布の原料としては、ＨＤＰＥや
ＰＰなとのポリオレフィンおよびポリエステル、ポリア
ミド、塩ビ系、アクリルニトリル系、ポリビニルアルコ
ール系、ポリウレタンなど熱可塑性ポリマーやガラス、
ピッチ、接着性ポリマー またこれらを溶剤に溶解した
もの、界面活性剤と共に分散液に分散してエマルジョン
にしたものも使用することが出来る。また、溶融紡糸が
困難なセルローズ系ポリマーの溶剤に溶解したものなど
も特に有効である。これらのポリマーで重要なことは、
振動し、飛散される際、そのフィラメントがまだ曳糸性
があり、数十〜数千倍にドラフトが可能なことが必要な
条件である。Raw materials for the nonwoven fabric used in the present invention include polyolefins and polyesters such as HDPE and PP, thermoplastic polymers such as polyamide, PVC, acrylonitrile, polyvinyl alcohol, and polyurethane, glass,
Pitch, adhesive polymer It is also possible to use those dissolved in a solvent or dispersed in a dispersion liquid together with a surfactant to form an emulsion. Furthermore, cellulose-based polymers that are difficult to melt-spun dissolved in a solvent are also particularly effective. The important thing about these polymers is that
The necessary condition is that the filament still has stringiness when vibrating and being scattered, and that it can be drafted tens to thousands of times.
本発明により、従来安定性の範囲が掻めて狭かった一方
向配向不織布の製法を、どの様なポリマーでも安定に一
方向配列性良く製造することが出来るようになった。そ
のため、溶液型紡糸液でもタテ、またはヨコに配列した
フィラメントを容易に製造できるようになり、そのまま
直角方向に配列する不織布と組み合わせてタテヨコに寸
法安定性の良い不織布にすることが出来た。また粘度の
高い溶融ポリマーでも、一方向に良く配列したフィラメ
ントになり、これは、フィラメントの配列方向に延伸し
て強い不織布を製造するのに特に適していた。The present invention has made it possible to stably produce unidirectionally oriented nonwoven fabrics using any polymer with good unidirectional alignment, although the conventional method of producing unidirectionally oriented nonwoven fabrics had a very narrow range of stability. Therefore, it has become possible to easily produce filaments arranged vertically or horizontally using a solution-type spinning solution, and by combining this with a nonwoven fabric arranged in the right angle direction, it has become possible to create a nonwoven fabric with good vertical and horizontal dimensional stability. Also, molten polymers with high viscosity resulted in filaments that were well aligned in one direction, which was particularly suitable for producing strong nonwoven fabrics by drawing in the direction of filament alignment.
以下、実施の様体を図面で具体的に説明する。 Hereinafter, the mode of implementation will be specifically explained with reference to the drawings.
第１図は、本発明による不織布の製造の例を示したもの
で、溶融したポリマーがフレキシブルな導管１を通じて
紡糸口群２−Ｌ２−２．２−３に導かれる。これらの紡
糸口群は駆動装置ｔ（図示していない）によって、図面
のｘＹＺ軸のＹ軸平行方向に振動している。紡糸された
フィラメント３−１は巾方向に紡糸口と同一周期で振動
している。この巾方向に振動しているフィラメント３−
１を中心にしてほぼ左右対称の位置よりＸ軸方向に一対
の流体４−１ａと４−１ｂをフィラメント上で正面衝突
させ、その正面衝突した流体がＹ清水平方向に飛散する
勢いでフィラメントもＹ軸方向へ配列して５−１のよへ
に飛散して、Ｘ軸方向を手前へ走行するコンベアベルト
上に集積される。コンベアベルトには予め別の製法で作
られたタテ方向に配列したフィラメント群７が集積され
ており、コンベア上でヨコに配列したフィラメントと層
状に積層され不織布とする。FIG. 1 shows an example of the production of a nonwoven fabric according to the invention, in which molten polymer is led through a flexible conduit 1 to a spinneret group 2-L2-2.2-3. These spinneret groups are vibrated in a direction parallel to the Y axis of the xYZ axes in the drawing by a drive device t (not shown). The spun filament 3-1 vibrates in the width direction at the same frequency as the spinneret. Filament 3- vibrating in the width direction
A pair of fluids 4-1a and 4-1b are caused to collide head-on on the filament in the X-axis direction from approximately symmetrical positions with respect to 1 as the center. They are arranged in the Y-axis direction, scattered as shown in 5-1, and accumulated on a conveyor belt running forward in the X-axis direction. A group of filaments 7 arranged in the vertical direction made in advance using a different manufacturing method are accumulated on the conveyor belt, and are laminated in layers with the filaments arranged horizontally on the conveyor to form a nonwoven fabric.
第２図は、紡出フィラメントを流体により振動させる流
体の噴出孔の配置の例で、図ＡとＢにおいて紡糸口の部
分を下から見た図で、８は紡糸装置の下板で、９は紡糸
口である０図Ａは紡糸口９の回りに一直線に流体の噴出
孔１０−１．１０−２、φ・・、１Ｏ−６が配列してい
る例で、図Ｂは、紡糸口９の周囲に円周状に流体の噴出
孔１１−１１１−２、・・・、１１−６が配置されてい
る例である。Figure 2 is an example of the arrangement of fluid jet holes that vibrate spun filaments with fluid, and is a view of the spinning nozzle seen from below in Figures A and B, where 8 is the lower plate of the spinning device and 9 is the bottom plate of the spinning device. Figure A shows an example in which fluid ejection holes 10-1, 10-2, φ..., 1O-6 are arranged in a straight line around the spinneret 9, and Figure B shows the spinneret. This is an example in which fluid ejection holes 11-111-2, . . . , 11-6 are arranged circumferentially around 9.
ともに流体は紡糸口９より紡糸液と同時に噴出する成分
があっても良い、また流体の噴出孔はフィラメントの紡
出方向に対して、多少角度をもって孔が間けられている
ことが望ましい。Both fluids may have components that are ejected from the spinning nozzle 9 at the same time as the spinning solution, and it is desirable that the fluid ejection holes be spaced at some angle with respect to the direction in which the filaments are spun.
第３図は飛散させる流体の当て方の例を示したもので、
Ａ図はＹ軸に平行に振動してくるフィラメント１２に振
動方向に垂直（Ｘ軸方向）に、フィラメントを中心にし
て側方より対称の一対の流体の噴出流１３ａと１３ｂを
図のＰの位置で正面衝突させ、その衝突した流体がＹ軸
方向へ飛散する時、その流体と同時にフィラメントもＹ
軸方向へ左右に飛散し、Ｙ軸に平行に配列したフィラメ
ントの集合体１４となる。図Ｂは、やはりＹ軸に平行方
向に振動しているフィラメント１５に対してＸ軸方向よ
り一対の流体の噴出流１Ｇ＆と１６ｂとを噴出させるが
、への場合と異なり、１６ａと１６ｂは正面衝突せず、
振動するフィラメント上の別の焦点ＱとＲで交差し、フ
ィラメントに当たった流体は対称位置より来る流体にあ
まり邪魔されずに突き進むことができ、その流体によっ
て飛散されるフィラメントは、はぼＸ軸方向に配列して
飛散するフィラメントの集合体１７どなる。Figure 3 shows an example of how to apply the splashing fluid.
Figure A shows a pair of fluid jets 13a and 13b that are symmetrical from the sides with the filament centered, perpendicular to the vibration direction (X-axis direction) of the filament 12 vibrating parallel to the Y-axis. When a head-on collision occurs at a position and the collided fluid scatters in the Y-axis direction, the filament also moves in the Y-axis direction at the same time as the fluid.
The filaments scatter left and right in the axial direction, forming an aggregate 14 of filaments arranged parallel to the Y axis. In Figure B, a pair of fluid jets 1G& and 16b are ejected from the X-axis direction to the filament 15, which is also vibrating in a direction parallel to the Y-axis. No collision,
Another focal point Q and R on the vibrating filament intersect, and the fluid that hits the filament can advance without much interference from the fluid coming from the symmetrical position, and the filament scattered by the fluid is approximately on the X axis. A collection of filaments 17 that are arranged and scattered in the same direction roar.
ＡまたはＢにおいて、フィラメントの配列方向は、下で
集積するコンベアや、不織布の走行方向と、この飛散流
体の当て方の相対的関係でとの様な方向にも配列させる
ことが出来る０図ＡもＢも、フィラメント１２．１５が
ヨコに振動している例で示したが、円状に旋回していて
も良い。In A or B, the filaments can be arranged in the following directions depending on the relative relationship between the conveyor that collects them below, the running direction of the nonwoven fabric, and the way in which this scattering fluid is applied. In both cases, the filaments 12 and 15 are shown as vibrating horizontally, but they may also be rotating in a circle.
第４図に、本発明によるフィラメントの配列の例で、矢
印の方向がタテ方向で、構造が判りやすいように、層の
上の部分の１部を剥して示しである。（イ）はタテに配
列したフィラメントの層と、ヨコに配列したフィラメン
トの層を積層した例で、両方向のフィラメントも本発明
の方法を使用した例である。（ロ）は本発明の方法によ
るヨコ配列フィラメントとタテ方向は在来のヤーンを一
定ピッチで配列したものを積層した場合で、図示してな
いがヤーン層をこの上に重ねても良い、（ハ）は、本発
明のフィラメントの配列方向が斜めの層と、それと斜交
して別の斜め方向に配列している層とが積層している例
である。（ハ）の斜交している場合は、他にタテ方向や
ヨコ方向にフィラメントの配列している別の不織布や繊
維ウェブを積層して３軸または４軸の不織布とすること
もできる。FIG. 4 shows an example of the arrangement of filaments according to the present invention, with the direction of the arrow pointing in the vertical direction, and a portion of the upper part of the layer removed to make the structure easier to understand. (A) is an example in which a layer of filaments arranged vertically and a layer of filaments arranged horizontally are laminated, and the method of the present invention is also used for filaments in both directions. (B) is a case in which filaments arranged horizontally according to the method of the present invention and conventional yarns arranged at a constant pitch in the vertical direction are laminated.Although not shown in the figure, a yarn layer may be superimposed on this. C) is an example in which a layer in which the filaments of the present invention are arranged diagonally and a layer in which the filaments are arranged in another diagonal direction are laminated. In the case of (c), in which the filaments are diagonally crossed, another nonwoven fabric or fiber web having filaments arranged in the vertical or horizontal direction may be laminated to form a triaxial or quadriaxial nonwoven fabric.
実施例１．ポリエチレンテレフタレートの極限粘度ηが
０．７２のペレットを押出機で２６０’Ｃに溶融押出し
、第１図の方法でフレキシブル導管を通じて３個の紡糸
口に導かれる。紡糸口は紙面に平行方向にヨコに３５Ｍ
巾に２４０ｏ回／分で振動している。紡糸されたフィラ
メントは巾方向に２５−巾に紡糸口と同一周期で振動し
ている。この巾方向に振動しているフィラメントを中心
にしてほぼ左右対称の位置より紙面より垂直方向に一対
の３００℃に加熱されたエアーを正面衝突させた。その
正面衝突したエアーがヨコ方向に飛散する勢いでフィラ
メントも紙面のヨコ方向へ配列して一つの紡糸口当たり
約３５０−の巾でヨコに配列して飛散して、下に４０
ｒｎ ／分で走行するコンベアベルト上に集積される。Example 1. Pellets of polyethylene terephthalate having an intrinsic viscosity η of 0.72 are melt-extruded in an extruder at 260'C and guided through flexible conduits to three spinnerets in the manner shown in FIG. The spinneret is 35M horizontally parallel to the paper surface.
It vibrates at 240 degrees per minute across its width. The spun filaments vibrate in a 25-width direction at the same frequency as the spinneret. A pair of air heated to 300° C. was caused to collide head-on in a direction perpendicular to the plane of the paper from approximately symmetrical positions around the filament vibrating in the width direction. Due to the force of the head-on air scattering in the horizontal direction, the filaments are also arranged in the horizontal direction of the page and scattered horizontally with a width of about 350 mm per spinneret, and the filaments are scattered downward.
It is collected on a conveyor belt running at rn/min.
コンベアベルト上では３個の紡糸口によるヨコ配列フィ
ラメントが境を若干型なった状態で全体中はぼ１１００
（１のヨコ配列不織布となった。コンヘアベルトには通
常の不織布製造装置で製造されたタテ方向に配列した不
織布が前工程で製造されており、コンベア上でヨコに配
列したフィラメントと層状に積層された。積層されたフ
ィラメント群は、ざらに表面をタテ方向に配列した不織
布と積層され、一対のエンボスローラによりこれらの眉
間を接着して、不織布とし、この不織布をタテ方向に３
．２倍、ヨコ方向へ２．８倍それぞれ延伸して、延伸後
エマルジョン接着剤に含浸後乾燥して直交不織布を得た
。On the conveyor belt, the horizontally arranged filaments from the three spinnerets are slightly shaped at the border, and the overall diameter is approximately 1100.
(This resulted in the horizontally arranged nonwoven fabric of No. 1.) Conhair belts are made with vertically arranged nonwoven fabrics manufactured using normal nonwoven fabric manufacturing equipment in the previous process, and are layered with the horizontally arranged filaments on the conveyor. The laminated filament group was laminated with a nonwoven fabric whose surface was arranged vertically, and a pair of embossing rollers adhered the glabella to form a nonwoven fabric.
．． It was stretched 2 times and 2.8 times in the horizontal direction, and after stretching, it was impregnated with an emulsion adhesive and dried to obtain an orthogonal nonwoven fabric.
製造された不織布は３５ ｇ ／ ＴＩＩ″で、タテ強
度２７．２ｋｇ１５ｃｍ巾で伸度２２％、ヨコ強度は２
２゜５ ｋ ｇ ／ ５ ａｍで伸度２８％のタテヨコ
に強い不織布であり、従来のポリエステルランダム不織
布に比較して３〜４倍の強度をもつ不織布であった。The manufactured nonwoven fabric has a weight of 35 g/TII'', a vertical strength of 27.2 kg, a width of 15 cm, an elongation of 22%, and a horizontal strength of 2.
It was a nonwoven fabric that was strong in both vertical and horizontal directions with an elongation of 2.5 kg/5 am and an elongation of 28%, and was 3 to 4 times stronger than conventional polyester random nonwoven fabric.
実施例２．高密度ポリエチレンの１５％デカリン溶）α
を、第２図のＢのノズルより紡出し、第３図Ｂの方式で
タテに配列したフィラメントを得た。Example 2. 15% decalin solution of high density polyethylene) α
was spun from the nozzle shown in FIG. 2B, and filaments arranged vertically in the manner shown in FIG. 3B were obtained.
この場合第２図Ｂの振動するためのエアーおよび第３図
Ｂの飛散させるエアーともに特に加熱していない室温の
エアーを用いた。得られた不織布は非常に細い（はとん
どが１デニールより迩かに小さい）フィラメントからな
り、特に接着することをせずとも、非常にフィラメント
間の接着性の良い不織布となった。この不織布をタテ方
向に５倍近接ローラ延伸することにより坪ｔ１５ｇ／ｖ
ｒ１″、タテ強度１７．４ｋｇ１５ｃ＋＋＋タテ伸度２
７％のタテに強い不織布となった。これは経緯積層不織
布の原料ウェブとして最適の性質を持った不織布である
。In this case, both the vibrating air in FIG. 2B and the scattering air in FIG. 3B were room temperature air that had not been particularly heated. The obtained nonwoven fabric was made of very thin filaments (most of which were much smaller than 1 denier), and the filaments had very good adhesion even without any particular adhesion. By stretching this nonwoven fabric 5 times in the vertical direction with close rollers, the tsubo t15g/v
r1'', vertical strength 17.4kg15c+++ vertical elongation 2
7% vertically resistant nonwoven fabric. This is a nonwoven fabric with optimal properties as a raw material web for laminated nonwoven fabrics.
実施例３．リンターパルプの鋼アンモニア溶液（ｉｓ度
８％）を、紡口より紡糸し濾斗へ水と同時に流すことに
より、若干凝固と延伸をかけ、まだドラフト性が２０倍
以上ある状態で濾斗の出口先端を約１０ｍｍの巾で６０
０回／分の周間で水平方向へ振動させ、出てきたフィラ
メントが水の勢いで３０間巾に振動している所へ、今度
は垂直方向より一対の水を噴射して（第３図Ａの方法）
、水を衝突させ、ヨコに飛散する水の勢いでヨコに配列
したフィラメントを走行するコンベアベルト上に集積し
た。集積されたフィラメントはまだ凝固が完了していな
いが、前工程で製造されコンヘアに堆積されて運ばれて
来ている通常の方法の銅アンモニア法によるセルローズ
不織布くタテに配列している）と層状に積層され、両方
−緒に酸で処理されタテヨコに寸法安定性のある不織布
となった。この場合はタテヨコ積層された時点では、ま
だ凝固が完了しておらないため、フィラメント同士の接
着性があり特に接着処理は必要でなかった。Example 3. A steel ammonia solution (IS degree 8%) of linter pulp is spun from the spinneret, and by flowing it into the funnel simultaneously with water, it is slightly solidified and stretched, and when the draft property is still 20 times or more, it is passed through the exit of the funnel. 60 with a width of about 10mm at the tip
The filament was vibrated horizontally at a frequency of 0 times per minute, and a pair of water was sprayed vertically onto the area where the emerging filament was vibrating over a width of 30 minutes due to the force of the water (Figure 3). Method A)
, water was collided with the filaments, and the force of the horizontally scattered water caused the filaments arranged horizontally to accumulate on a running conveyor belt. Although the accumulated filaments have not yet finished coagulating, they are arranged vertically in a cellulose nonwoven fabric produced in the previous process, deposited on a conhair, and transported by the usual copper ammonia method. They were laminated together and both were treated with acid to form a non-woven fabric with vertical and horizontal dimension stability. In this case, when the filaments were laminated vertically and horizontally, coagulation had not yet been completed, and the filaments were adhesive to each other, so no particular adhesive treatment was necessary.
第１図は、本発明の不織布の製造の例を示したもので、
第２図は紡糸したフィラメントを流体で振動させる場合
の流体噴出孔の配置の例で、Ａは紡糸口の周りに流体噴
出孔が一列に並べた例で、Ｂは円周状に配置した例であ
る。第３図は飛散させるための流体の噴出流の当て方の
例で、Ａは噴出流が正面衝突する場合で、Ｂは交差する
場合である。第４図は本発明による不織布のフィラメン
トの配列方向の例を示したもので、（イ）はタテヨコ方
向とも本発明による配列不織布による例で、（ロ）はヨ
コ方向は本発明でヨコに配列した不織布で、タテ方向は
在来のヤーンを配置した例で、（ハ）は本発明の方法に
よる斜交不織布の例である。
主な記号の説明
１は紡糸液を送るフレキシブル導管
２−１．２−２．２−３は振動されている紡糸口３−１
は振動している紡出フィラメント４−１ａ、４−１ｂは
正面衝突する流体５−１は、ヨコに配列して飛散してい
るフィラメント群
６はコンベアベルト
７はタテ配列不織布
８は紡糸装置の下板、
９は紡糸口
１０−１． １０−２、争や・１０−６．１１−１゜１
１−２、φ・−１１−６は、フィラメントを振動させる
ための流体噴出孔
１２．１５は振動しているフィラメントｔａａ、ｔａｂ
、１６ａ、１６ｂは、振動しているフィラメントを飛散
させる流体の噴射流１４．１７は、配列して飛散してい
るフィラメント群
Ｐ、Ｑ、Ｒは流体がフィラメントに当たる場所出願人
株式会社 高分子加工研究所
季
圀
茅
圀
竿
づ
暮
第
圀
（イフ
（ロ）FIG. 1 shows an example of manufacturing the nonwoven fabric of the present invention.
Figure 2 shows examples of the arrangement of fluid jet holes when spinning filaments are vibrated with fluid; A is an example in which the fluid jet holes are arranged in a row around the spinneret, and B is an example in which they are arranged in a circumferential manner. It is. FIG. 3 shows an example of how to apply jets of fluid for scattering, where A is a case where the jets collide head-on, and B is a case where they intersect. FIG. 4 shows an example of the arrangement direction of the filaments of the nonwoven fabric according to the present invention. (a) is an example in which the filaments are arranged in the vertical and horizontal directions according to the present invention, and (b) is an example in which the filaments are arranged in the horizontal direction according to the present invention. (C) is an example of a diagonal nonwoven fabric produced by the method of the present invention. Explanation of main symbols 1 is a flexible conduit that sends the spinning solution 2-1.2-2.2-3 is a vibrating spinning nozzle 3-1
The spun filaments 4-1a and 4-1b are vibrating and collide head-on.The fluid 5-1 is arranged horizontally and the filaments 6 are scattered.The conveyor belt 7 is arranged vertically.The non-woven fabric 8 is the spinning device. Lower plate 9 indicates spinning nozzle 10-1. 10-2, Conflict・10-6.11-1゜1
1-2, φ・-11-6 are fluid jet holes 12 for vibrating the filament.15 are vibrating filaments taa, tab
, 16a, 16b are jet streams of fluid that scatter the vibrating filaments. 14. 17 are filament groups P, Q, and R that are arrayed and scattered. Applicants are locations where the fluid hits the filaments.
Polymer Processing Laboratory Co., Ltd.
Claims (1)
高分子物質を紡口より紡出してなる不織布の製法におい
て、 （１）紡出フィラメントが旋回または巾方向に振動する
ように紡糸され、 （２）その旋回または振動しているフィラメントがまだ
２倍以上のドラフト性がある状態で、（３）その旋回ま
たは振動しているフィラメントを中心にして、側方より
ほぼ左右対称の一対以上の流体を作用させて、フィラメ
ントを一方向に配列するように飛散させることによる一
方向配列不織布の製法。 （２） 高分子物質の溶融された高分子物質が紡口より
紡出されたフィラメントからなる不織布の製法において
、 （１）フィラメントが旋回または巾方向に振動するよう
に紡口を円運動または振動しながら紡糸し、（２）その
旋回または振動しているフィラメントがまだ２倍以上の
ドラフト性がある状態で、（３）その旋回または振動し
ているフィラメントを中心にして、側方よりほぼ左右対
称の一対以上の流体を作用させて、フィラメントを一方
向に配列するように飛散させることによる一方向配列不
織布の製法。 （３） 請求項（１）において、紡出フィラメントに旋
回または振動を与える方法として、紡出直後に紡口近傍
より微弱な流体を作用させることによる一方向配列不織
布の製法。 （４） 請求項（１）において、紡出フィラメントに旋
回または振動を与える方法として、紡口そのものを円運
動または振動、往復運動させることによる一方向配列不
織布の製法。 （５） 請求項（１）（２）において、紡出フィラメン
トに旋回または振動を与える方法として、紡出フィラメ
ントに電荷を与え、そのフィラメントに極性が交互に変
化する電場または磁場により紡出フィラメントを旋回ま
たは振動、往復運動させることによる一方向配列不織布
の製法。 （６） 請求項（１）において、紡出フィラメントが完
全に凝固しない程度の凝固ゾーンを経た後、請求項（３
）（４）（５）の方法および凝固浴出口を円運動、振動
させたり、凝固浴出口で流体を作用させて、フィラメン
トに旋回または振動運動を与えることによる一方向配列
不織布の製法。 （７） 請求項（１）（２）において、紡出フィラメン
トが１ｍｍから３００ｍｍ、望ましくは５ｍｍより５０
ｍｍの範囲の振幅で、６０回／分以上、さらに望ましく
は３００回／分以上の周期で旋回または往復運動してい
る状態で流体により飛散されることによる一方向配列不
織布の製法。 （８） 請求項（１）（２）において、紡口より紡出さ
れるフィラメントの断面が流体の作用を受けやすいよう
に楕円形や異形の真円よりずれた断面であることによる
一方向配列不織布の製法。 （９） 請求項（１）（２）において、紡出フィラメン
トが旋回または振動している状態に流体を作用させて飛
散させる方法として、フィラメントを中心にして側方よ
りほぼ左右対称の一対以上の流体をフィラメント上で衝
突させて、フィラメントを流体の噴出方向と直角方向に
飛散させることによる一方向配列不織布の製法。 （１０） 請求項（１）（２）において、紡出フィラメ
ントが旋回または振動している状態に流体を作用させて
飛散させる方法として、フィラメントを中心にして側方
よりほぼ左右対称の一対以上の流体をフィラメントの旋
回または振動範囲で交差させて、フィラメントを流体の
噴出方向と平行方向に飛散させることによる一方向配列
不織布の製法。 （１１） 請求項（１）（２）において、飛散して一方
向に配列した不織布を、さらにその配向方向に延伸する
ことによる一方向配列不織布の製法。 （１２） 請求項（１）（２）（１１）における一方向
配列不織布と、それと直角方向に配列した不織布または
繊維材ウェブを組み合わせる事による直交不織布の製法
。 （１３） 請求項（１）（２）の方法でフィラメントを
ヨコ方向に配列させ、そのヨコに配列したフィラメント
でタテ方向に走行する糸群の配列を固定する方法。 （１４） 請求項（１）（２）の方法において、一方向
配列不織布を製造し、さらにこれに積層する形で先の不
織布とは直角方向に配列した不織布を製造し、積層した
不織布のそれぞれのフィラメントの配列方向に２軸的に
延伸することによる直交不織布の製法。 （１５） フィラメントを紡糸してなる不織布の製造装
置において、溶融、溶剤に溶解、または液体に分散され
た高分子物質が紡口より紡出されて、フィラメントが旋
回または巾方向に振動するように紡口を円運動または振
動させる装置と、それによって旋回または振動するフィ
ラメントを中心にして側方よりほぼ左右対称の一対以上
の流体を作用させる流体噴出装置により一方向に配列し
て飛散したフィラメントにする装置からなる一方向配列
不織布製造装置。 （１６） フィラメントを紡糸してなる不織布の製造装
置において、紡口より紡出されるフィラメントが帯電す
るように紡糸液に荷電させる装置と、紡出されたフィラ
メントに極性が交互に変換する電場または磁場を作用さ
せる装置を具備することにより、フィラメントを旋回ま
たは巾方向に振動させ、その旋回または振動しているフ
ィラメントを中心にして側方よりほぼ左右対称の一対以
上の流体を作用させる流体噴出装置によりフィラメント
を一方向に飛散させる装置からなる一方向配列不織布製
造装置。 （１７） 請求項（１５）（１６）において、紡口より
紡出されるフィラメントの断面が真円よりずれた楕円形
断面や異形断面になるように、紡口を真円よりずれた形
状にした一方向配列不織布の製造装置。[Scope of Claims] (1) A method for producing a nonwoven fabric by spinning a polymeric substance dissolved in a solvent or dispersed in an emulsion form from a spinneret, comprising: (2) the swirling or vibrating filament still has twice the draftiness, and (3) the swirling or vibrating filament is approximately symmetrical from the side. A method for producing a unidirectionally aligned nonwoven fabric by applying one or more pairs of fluids to scatter filaments so that they are aligned in one direction. (2) In a method for manufacturing a nonwoven fabric consisting of filaments spun from a molten polymer material through a spinneret, (1) the spinneret is moved in a circular motion or vibrated so that the filaments swirl or vibrate in the width direction; (2) While the swirling or vibrating filament still has a draft property of twice or more, (3) With the swirling or vibrating filament in the center, it is almost left and right from the side. A method for producing a unidirectionally aligned nonwoven fabric by applying one or more pairs of symmetrical fluids to scatter filaments so that they are aligned in one direction. (3) A method for producing a unidirectionally aligned nonwoven fabric according to claim (1), in which a weak fluid is applied from near the spinneret immediately after spinning as a method of imparting swirl or vibration to the spun filaments. (4) A method for producing a unidirectionally aligned nonwoven fabric according to claim (1), in which the spinneret itself is subjected to circular motion, vibration, or reciprocating motion as a method of imparting swirl or vibration to the spun filaments. (5) In claims (1) and (2), the method of giving swirl or vibration to the spun filament is to apply an electric charge to the spun filament and to cause the spun filament to move using an electric field or a magnetic field whose polarity alternately changes. A method for producing unidirectionally aligned nonwoven fabric by rotating, vibrating, or reciprocating motion. (6) In claim (1), after passing through a coagulation zone where the spun filament is not completely coagulated, the spun filament in claim (3)
) (4) and (5), and a method for producing a unidirectionally aligned nonwoven fabric by circularly moving or vibrating the coagulation bath outlet, or by applying a fluid at the coagulation bath outlet to give swirling or vibrating motion to the filaments. (7) In claims (1) and (2), the spun filament has a diameter of 1 mm to 300 mm, preferably 5 mm to 50 mm.
A method for producing a unidirectionally aligned nonwoven fabric by scattering it with a fluid while rotating or reciprocating at a period of 60 times/minute or more, more preferably 300 times/minute or more, with an amplitude in the range of mm. (8) A unidirectionally aligned nonwoven fabric according to claims (1) and (2), in which the cross section of the filaments spun from the spinneret is oval or irregularly deviated from a perfect circle so as to be easily affected by fluid. manufacturing method. (9) In claims (1) and (2), as a method of applying a fluid to the spinning or vibrating spun filament to scatter it, a pair or more of approximately symmetrical particles from the sides with the filament as the center are used. A method for manufacturing a unidirectionally aligned nonwoven fabric by colliding fluid on filaments and scattering the filaments in a direction perpendicular to the jetting direction of the fluid. (10) In claims (1) and (2), as a method of applying a fluid to the spinning or vibrating spun filament and scattering the spun filament, a pair or more of approximately bilaterally symmetrical spun filaments from the sides are used. A method for producing a unidirectionally aligned nonwoven fabric by causing the fluid to intersect in the swirling or vibrating range of the filaments and scattering the filaments in a direction parallel to the jetting direction of the fluid. (11) A method for producing a unidirectionally aligned nonwoven fabric according to claims (1) and (2), by further stretching the scattered nonwoven fabric in the unidirectionally aligned direction. (12) A method for producing an orthogonal nonwoven fabric by combining the unidirectionally aligned nonwoven fabric according to claims (1), (2), and (11) with a nonwoven fabric or fibrous material web aligned in a direction perpendicular to the unidirectionally aligned nonwoven fabric. (13) A method of arranging the filaments in the horizontal direction using the method of claims (1) and (2), and fixing the arrangement of the thread group running in the vertical direction using the filaments arranged in the horizontal direction. (14) In the method of claims (1) and (2), a unidirectionally arranged nonwoven fabric is produced, and further, nonwoven fabrics arranged in a direction perpendicular to the previous nonwoven fabric are produced by laminating this, and each of the laminated nonwoven fabrics is A method for producing an orthogonal nonwoven fabric by biaxially stretching the filaments in the direction in which they are arranged. (15) In an apparatus for manufacturing a nonwoven fabric formed by spinning filaments, a polymer substance melted, dissolved in a solvent, or dispersed in a liquid is spun out from a spinneret, and the filaments are rotated or vibrated in the width direction. A device that causes the spinneret to move in a circular motion or vibrates, and a fluid ejecting device that applies a pair or more of fluids that are approximately bilaterally symmetrical from the sides around the rotating or vibrating filament. A unidirectional nonwoven fabric manufacturing device consisting of a device that (16) In an apparatus for manufacturing a nonwoven fabric formed by spinning filaments, there is a device that charges the spinning solution so that the filaments spun from the spinneret are charged, and an electric or magnetic field that alternately changes the polarity of the spun filaments. The filament is rotated or vibrated in the width direction by being equipped with a device that acts on the filament, and a fluid ejecting device that applies a pair or more of fluids that are approximately symmetrical from the sides around the swirling or vibrating filament. A unidirectional array nonwoven fabric manufacturing device consisting of a device that scatters filaments in one direction. (17) In claims (15) and (16), the spinneret is formed in a shape that deviates from a perfect circle so that the cross section of the filament spun from the spindle has an elliptical cross section or an irregular cross section that deviates from a perfect circle. Equipment for producing unidirectional nonwoven fabric.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1058384A JPH076126B2 (en) | 1989-03-10 | 1989-03-10 | Manufacturing method and device for unidirectionally arranged nonwoven fabric |
| EP90904418A EP0414917B2 (en) | 1989-03-10 | 1990-03-12 | Nonwoven fabric, production thereof, and apparatus therefor |
| PCT/JP1990/000318 WO1990010743A1 (en) | 1989-03-10 | 1990-03-12 | Nonwoven fabric, production thereof, and apparatus therefor |
| US07/613,542 US5312500A (en) | 1989-01-27 | 1990-03-12 | Non-woven fabric and method and apparatus for making the same |
| CA002028853A CA2028853C (en) | 1989-03-10 | 1990-03-12 | Non-woven fabric and method and apparatus for making the same |
| DE69025517T DE69025517T3 (en) | 1989-03-10 | 1990-03-12 | NON-WOVEN FABRIC, THE PRODUCTION AND DEVICE THEREOF |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1058384A JPH076126B2 (en) | 1989-03-10 | 1989-03-10 | Manufacturing method and device for unidirectionally arranged nonwoven fabric |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02242960A true JPH02242960A (en) | 1990-09-27 |
| JPH076126B2 JPH076126B2 (en) | 1995-01-30 |
Family
ID=13082840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1058384A Expired - Lifetime JPH076126B2 (en) | 1989-01-27 | 1989-03-10 | Manufacturing method and device for unidirectionally arranged nonwoven fabric |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0414917B2 (en) |
| JP (1) | JPH076126B2 (en) |
| CA (1) | CA2028853C (en) |
| DE (1) | DE69025517T3 (en) |
| WO (1) | WO1990010743A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5789328A (en) * | 1996-06-18 | 1998-08-04 | Nippon Petrochemicals Company, Limited | Bulky nonwoven fabric and method for producing the same |
| US6132661A (en) * | 1996-11-19 | 2000-10-17 | Nippon Petrochemical Company, Limited | Longitudinally stretched nonwoven fabric and method for producing the same |
| US6984350B2 (en) | 2001-02-27 | 2006-01-10 | Nippon Petrochemicals Co., Ltd. | Method of and apparatus for manufacturing a web having filaments aligned in a transverse direction |
| WO2009119696A1 (en) * | 2008-03-24 | 2009-10-01 | Kureha Engineering Co., Ltd. | Process for producing shaped contact-filtration member, shaped contact-filtration member, filtration apparatus, and method of processing soiled water |
| JP2016160558A (en) * | 2015-03-03 | 2016-09-05 | 日本ノズル株式会社 | Nonwoven fabric production apparatus, nonwoven fabric produced by the same, and nonwoven fabric production method |
| JP2017031515A (en) * | 2015-07-30 | 2017-02-09 | パナソニックＩｐマネジメント株式会社 | Laminate nonwoven fabric and air cleaning machine |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ZA92308B (en) | 1991-09-11 | 1992-10-28 | Kimberly Clark Co | Thin absorbent article having rapid uptake of liquid |
| US6344050B1 (en) | 1998-12-21 | 2002-02-05 | Light Sciences Corporation | Use of pegylated photosensitizer conjugated with an antibody for treating abnormal tissue |
| JP4233181B2 (en) | 1999-09-30 | 2009-03-04 | 新日本石油株式会社 | Method and apparatus for producing a horizontally arranged web |
| US7329621B2 (en) | 2002-12-26 | 2008-02-12 | Kimberly-Clark Worldwide, Inc. | Stretchable film laminates and methods and apparatus for making stretchable film laminates |
| DE102006016584B4 (en) | 2005-09-27 | 2016-02-25 | Illinois Tool Works Inc. | Method and apparatus for applying adhesive threads and dots to a substrate |
| JPWO2022009321A1 (en) * | 2020-07-08 | 2022-01-13 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4971263A (en) * | 1972-11-17 | 1974-07-10 | ||
| JPS4985369A (en) * | 1972-12-19 | 1974-08-15 | ||
| JPS6218661A (en) * | 1985-07-17 | 1987-01-27 | Canon Inc | Recording or reproducing device |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2200782A1 (en) † | 1972-01-08 | 1973-08-02 | Metallgesellschaft Ag | Endless fibrous fleece mfr - with uniformly distributed threads, by rotating them during deposition onto a moving support |
| DE2408080A1 (en) † | 1974-02-20 | 1975-08-28 | Benecke Gmbh J | Continuous filament depositing system - uses a rotating air jet to swirl filaments in a spiral on to carrier conveyor |
| DE2460755A1 (en) † | 1974-12-21 | 1976-07-01 | Hoechst Ag | METHOD AND DEVICE FOR MANUFACTURING A FLEECE FROM FILAMENTS |
| DE3907215C2 (en) † | 1988-05-27 | 1993-11-25 | Corovin Gmbh | Device for producing a nonwoven from continuous filaments and multilayered nonwoven produced therewith |
| JPH06215372A (en) * | 1993-01-19 | 1994-08-05 | Fuji Photo Film Co Ltd | Production and apparatus for production of magnetic recording medium |
-
1989
- 1989-03-10 JP JP1058384A patent/JPH076126B2/en not_active Expired - Lifetime
-
1990
- 1990-03-12 CA CA002028853A patent/CA2028853C/en not_active Expired - Fee Related
- 1990-03-12 DE DE69025517T patent/DE69025517T3/en not_active Expired - Fee Related
- 1990-03-12 EP EP90904418A patent/EP0414917B2/en not_active Expired - Lifetime
- 1990-03-12 WO PCT/JP1990/000318 patent/WO1990010743A1/en active IP Right Grant
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4971263A (en) * | 1972-11-17 | 1974-07-10 | ||
| JPS4985369A (en) * | 1972-12-19 | 1974-08-15 | ||
| JPS6218661A (en) * | 1985-07-17 | 1987-01-27 | Canon Inc | Recording or reproducing device |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5789328A (en) * | 1996-06-18 | 1998-08-04 | Nippon Petrochemicals Company, Limited | Bulky nonwoven fabric and method for producing the same |
| US6132661A (en) * | 1996-11-19 | 2000-10-17 | Nippon Petrochemical Company, Limited | Longitudinally stretched nonwoven fabric and method for producing the same |
| US6984350B2 (en) | 2001-02-27 | 2006-01-10 | Nippon Petrochemicals Co., Ltd. | Method of and apparatus for manufacturing a web having filaments aligned in a transverse direction |
| WO2009119696A1 (en) * | 2008-03-24 | 2009-10-01 | Kureha Engineering Co., Ltd. | Process for producing shaped contact-filtration member, shaped contact-filtration member, filtration apparatus, and method of processing soiled water |
| JP2016160558A (en) * | 2015-03-03 | 2016-09-05 | 日本ノズル株式会社 | Nonwoven fabric production apparatus, nonwoven fabric produced by the same, and nonwoven fabric production method |
| JP2017031515A (en) * | 2015-07-30 | 2017-02-09 | パナソニックＩｐマネジメント株式会社 | Laminate nonwoven fabric and air cleaning machine |
Also Published As
| Publication number | Publication date |
|---|---|
| WO1990010743A1 (en) | 1990-09-20 |
| EP0414917A4 (en) | 1991-09-11 |
| EP0414917A1 (en) | 1991-03-06 |
| DE69025517T2 (en) | 1996-08-01 |
| CA2028853C (en) | 1999-06-01 |
| JPH076126B2 (en) | 1995-01-30 |
| DE69025517T3 (en) | 2001-08-09 |
| EP0414917B1 (en) | 1996-02-28 |
| CA2028853A1 (en) | 1990-09-11 |
| DE69025517D1 (en) | 1996-04-04 |
| EP0414917B2 (en) | 2001-01-03 |
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