EP1543184B1 - Procede de production de fibres de polypropylene a haute tenacite - Google Patents

Procede de production de fibres de polypropylene a haute tenacite Download PDF

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Publication number
EP1543184B1
EP1543184B1 EP03757872A EP03757872A EP1543184B1 EP 1543184 B1 EP1543184 B1 EP 1543184B1 EP 03757872 A EP03757872 A EP 03757872A EP 03757872 A EP03757872 A EP 03757872A EP 1543184 B1 EP1543184 B1 EP 1543184B1
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EP
European Patent Office
Prior art keywords
draw
fiber strands
stage
heated
rolls
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
Application number
EP03757872A
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German (de)
English (en)
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EP1543184A1 (fr
Inventor
Hendrik Tiemeier
Horst Kropat
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Oerlikon Textile GmbH and Co KG
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Oerlikon Textile GmbH and Co KG
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Publication of EP1543184A1 publication Critical patent/EP1543184A1/fr
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Publication of EP1543184B1 publication Critical patent/EP1543184B1/fr
Anticipated expiration legal-status Critical
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D13/00—Complete machines for producing artificial threads
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • D01F6/06—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins from polypropylene

Definitions

  • the invention relates to a process for producing high strength polypropylene fibers having high strength and low elongation by continuous melt spinning, stripping, drawing and cutting fiber strands into the polypropylene fibers.
  • the fiber strands are passed directly after spinning for the purpose of cooling in a water bath and then stretched in a draw zone with a high draw ratio of up to 10: 1.
  • the relatively rapid cooling of the fiber strands in the water bath leads to a relatively high preorientation in the edge region of the individual fibers, with the consequence of poor stretchability.
  • the known method is also only suitable for relatively coarse fibers with a single titer in the range of greater than 3 dtex. manufacture. However, the higher friction effect on the individual filaments caused by the water bath does not allow the spinning of fibers with finer titer.
  • a device for the production of staple fibers which operates at high production speeds.
  • several Galettenduos are used as drafting systems, around which the fibers are each looped several times.
  • the device is designed for specific parameter ranges and is in particular not suitable for the production of fibers with very large fiber titers.
  • Another object of the invention is to provide an apparatus for carrying out the method.
  • the invention is characterized in that on the one hand the low melt temperature during spinning in conjunction with a slow draw speed favors a partial molecular orientation of the undrawn fibers and therefore sets a higher strength of the fiber. Due to the slow withdrawal speeds, significantly lower internal stresses occur between the polymer chains in the filaments during the
  • the partial extension of the fiber strands in the second drawing stage is carried out higher than in the subsequent third drawing stage.
  • the total drawing in the draw stages takes place with decreasing draw ratio.
  • the fiber strands are withdrawn after melt spinning by a first drafting system with several drafting rollers, the shell surfaces are cooled. Subsequently, the fiber strands are guided through a hot stretching channel within the first plug-in stage and heated to a temperature of above 100 ° C. for stretching.
  • the fiber strands are continuously heated to a temperature of> 100 ° C after passing through the first drawing stage to run into the third drawing stage by guiding over several heated draw rolls.
  • the draw rolls of the draw frames forming the second draw step are designed to be heated.
  • a further heat treatment of the fiber strands can be carried out by means of a further hot stretching channel.
  • the fiber strands can be heated both by a hot air or by a superheated steam. Be particularly advantageous has been found that the fiber strands in the first Stretching zone are heated with a hot air and in the second draw zone with a superheated steam.
  • the fiber strands are preferably cooled by guiding over a plurality of cooled draw rolls at a fourth drafting device at the end of the third draw step.
  • the fiber strands are extruded through an annular or rectangular spinneret with a plurality of approximately 60,000 to 120,000 nozzle bores.
  • the device according to the invention for carrying out the method according to the invention according to claim 12 is characterized by the formation and distribution of the drawing stages, so that polypropylene fibers with high strength of more than 6 cN / dtex. can be produced at a low elongation of below 40%, preferably below 20% with appropriate fineness in the individual titers.
  • the draw rolls of the middle draw frames are preferably designed to be heatable in order to obtain a uniform and continuous temperature control of the fiber strands during drawing.
  • the drafting units at the inlet and at the outlet of the overall drawing zone are preferably formed with cooled draw rolls.
  • a first embodiment of a device according to the invention for the single-stage production of polypropylene fibers is shown schematically.
  • Such devices are generally known in the art as compact spinning machines for the production of staple fibers, preferably of polypropylene.
  • the compact systems are available with spinning speeds in the range of max. 250 m / min. operated. This means that very high production capacities of up to 50 t per day can be achieved.
  • the device according to the invention corresponds to such compact systems and has for this purpose a spinning device 1 with a plurality of juxtaposed spinning stations 2.1, 2.2 and 2.3.
  • the number of spinning stations of in Fig. 1 shown embodiment is exemplary.
  • Each of the spinning stations 2.1 to 2.3 is constructed identically, so that it is explained in more detail with reference to the spinning station 2.1.
  • a preferably annular spinneret 3 is provided which has a plurality of nozzle bores on its underside.
  • nozzle bores on its underside.
  • the spinneret 3 is connected to a melt source (not shown here), which supplies the spinneret 3 with a melt stream under pressure.
  • extruders, pumps or combinations of both are suitable as melt sources in order to supply a melt stream to the spinneret 3.
  • the spinnerets 3 of the spinning stations 2.1, 2.2 and 2.3 are arranged in a heated spinning beam 15.
  • Cooling device 4 is arranged below the spinneret 15 in the spinning station 2.1 substantially centrally to the spinneret 3 .
  • the cooling device 4 is formed as an Anblasung in which a cooling air flow is generated from an annular blowing nozzle, so that the cooling air penetrates the annular veil formed by the fiber strands from the inside out and leads to cooling of the fiber strands.
  • the cooling air of the cooling device 4 is supplied from above through the spinning beam 15. However, it is also possible to place the cooling air supply laterally next to the exiting fiber strands.
  • the spinning device 1 are arranged downstream of several treatment facilities.
  • the spinning device 1 is immediately associated with a trigger device 6.
  • the take-off device 6 contains per spinning station devices for preparing and guiding the fiber strands 5.
  • a spin finish can be applied to the fiber strands by rolling.
  • the withdrawal device 6 is arranged below the spinning device 1.
  • the fiber strands 5 of the spinning units 2.1, 2.2 and 2.3 are deflected out of a vertical guide and brought together.
  • the plurality of fiber strands 5, which are also referred to as tow or tow, are deducted by a first drafting system 7.1.
  • the drafting system 7.1 is arranged directly next to the withdrawal device 6.
  • the drafting system 7.1 is followed by a total of three further drafting systems 7.2, 7.3 and 7.4. Between the drafting systems 7.1, 7.2, 7.3 and 7.4 each drawstring is formed. Thus, a first drafting stage 9.1 between the first drafting system 7.1 and the second drafting system 7.2 is formed. A second drafting stage 9.2 is formed between the drafting units 7.2 and 7.3 and the third drafting stage 9.3 between the drafting units 7.3 and 7.4.
  • Each of the drafting systems 7.1 to 7.4 has in each case a plurality of drafting rollers 8, which guide the fiber strands 5 with simple looping.
  • the drafting rollers 8 of the drafting systems 7.1 to 7.4 are driven, wherein the drafting rollers 8 of the drafting systems 7.1 to 7.4 in Depending on the desired draw ratio can be operated at different peripheral speeds.
  • the drafting rollers 8 of the drafting systems 7.1 to 7.4 can have a cooled roll shell or a heated roll shell, as required.
  • a hot stretching channel 10 is provided for the thermal treatment of the fiber strands between the first drafting system 7.1 and the second drafting system 7.2 in the first drafting stage 9.1.
  • the fiber strands 5 can be tempered to a predetermined temperature by means of hot air or by means of a superheated steam.
  • another hot stretching channel 10 is likewise arranged between the drafting arrangements 7.2 and 7.3.
  • an adjusting device 11 and a cutting device 12 are provided in order to cut the fiber strands continuously into staple fibers having a predetermined fiber length.
  • Fig. 1 For carrying out the method according to the invention is in the in Fig. 1
  • the device initially shown a polymer melt of polypropylene in the spinning device 1 via the spinnerets 3 of the spinning units 2.1 to 2.3 extruded under pressure to a plurality of fiber strands.
  • the fiber strands 5 emerging from the spinnerets 2 are conveyed via the draw-off device 6 through the drafting device 7.1 from the spinnerets 3 at a take-off speed below 100 m / min. preferably at a withdrawal speed below 50 m / min. deducted.
  • the fiber strands 5 are cooled by means of the cooling device 4 by a foggy or gaseous cooling medium stream, preferably from air, then prepared and brought together on leaving the discharge device 6 to a tow contained all fiber strands.
  • the drafting rollers 8 of the first drafting system 7.1 are driven at the take-off speed, wherein at the same time further cooling of the fiber strands takes place at the circumference of the drafting rollers 8 of the first drafting system 7.1.
  • the fiber strands 5 takes place in a total of three draw levels 9.1, 9.2 and 9.3, each with different draw ratios.
  • the total draw ratio is above 4: 1.
  • the stretching of the fiber strands in the steps is carried out with different intensity.
  • the fiber strands are stretched in the first draw stage 9.1 with a partial stretch, which accounts for at least 70% of the total drawing.
  • the fiber strands 5 are preferably heated in the hot drawing channel 10 by hot air to a temperature of> 100 ° C and then passed over the likewise heated to a temperature of about 100 ° C drafting rollers 8 of the second drafting system 7.2.
  • the second Operaverstreckung the fiber strands 5 takes place in the second draw stage 9.2, wherein also a treatment in a hot stretching channel 10 is provided.
  • the fiber strands are further partially drawn by the third drafting system 7.2, wherein the partial drawing in the second drawing stage 9.2 is higher than the last partial drawing in the third drawing stage 9.3.
  • the rollers 8 of the third drafting system 7.3 are also heated to a surface temperature of> 100 ° C to obtain a uniform continuous drawing.
  • the fiber strands 5 are cooled by the cooled drafting rollers 8, the fourth drafting system 7.4 and then cut uniformly into fibers in the predetermined fiber length.
  • the rollers of the first drafting system 7.1 were at a take-off speed in the range of 25 to 40 m / min., The drafting rollers of the second drafting system 7.2 at a speed in the range of 80 to 115 m / min., The drafting rollers of the third drafting system 7.3 at a speed in the range of 100 to 140 m / min. and the drafting rollers of the fourth drafting system 7.4 at a speed of 110 to 160 m / min. driven.
  • the surface temperatures of the drafting rollers 8 were at the first drafting system 7.1 about 30 ° C, at the second drafting 7.2> 100 ° C, at the third drafting system 7.3 also> 100 ° C and at the fourth drafting 7.4 about 30 ° C.
  • the temperature control of the fiber strands was carried out in the first drawing stage through the hot drawing channel 10 with a hot air having a temperature of above 100 ° C.
  • the fiber strands were treated with a superheated steam at a temperature ⁇ 100 ° C.
  • the partial stretches achieved thereby for the production of the designated fibers were in the range of 2.8 to 3.2: 1 in the first draw stage 9.1, in the range of 1.05 to 1.5: 1 in the second draw stage 9.2 and in the area 1, 05 to 1.3: 1 in the third draw step 9.3.
  • This slow and steady crystallization has the consequence that a high strength is achieved at low residual strain. Due to the multi-stage stretching can be a particularly fine fiber with Einzeltitern below 2 dtex. produce.
  • Fig. 2 is a further embodiment of a device according to the invention for carrying out the method according to the invention shown schematically.
  • the Spinning device 1 and the discharge device 6 is not shown. These are identical to the previous embodiment, so that reference is made to the preceding description.
  • the treatment of the fiber strands successively arranged treatment facilities are in the in Fig. 2 illustrated embodiment by the drafting systems 7.1, 7.2, 7.3 and 7.4 and a crimping device 13, a drying device 14, and the pulling device 11 and the cutter 12 is formed.
  • the drafting systems 7.1 to 7.4 are designed substantially identical to the previous embodiment, only the number of drafting rollers 8 used per drafting device is different.
  • a hot stretching channel 10 is provided in each of the stretching stages 9.1, 9.2 and 9.3.
  • the treatment of the fiber section in the hot stretching channels 10 in the first drawing stage 9.1 and in the second drawing stage 9.2 is preferably carried out by a hot air and in the third drawing stage 9.3 with a steam.
  • a crimped polypropylene fiber having a strength of greater than 6 cN / dtex, an elongation of ⁇ 40%, preferably ⁇ 30% and a fineness with a single denier of ⁇ 2dtex. having.
  • the fiber strands 5 are curled after stretching by the crimping device 13.
  • the crimping device 13 is usually designed as Stauchschk Hursel Surprise, in which the fiber strands are pressed by a conveyor into a stuffer box. After crimping, the fiber strands are fed to the drying device 14 and then fed by the tensioning device 11 with a defined tension of the cutting device 12.
  • the crimping device is preceded by a cable connection and a damping channel (both not shown).
  • the structure of the embodiments according to Fig. 1 and 2 for the device according to the invention are exemplary in the number and choice of treatment facilities. In principle, it is possible to introduce additional treatments and treatment stages, for example by cable combination to set a suitable for the crimp fiber occupancy. Likewise, more than three draw steps can be formed one behind the other.
  • Essential for the inventive method and apparatus according to the invention is a spinning with low melt temperatures at low take-off speeds in conjunction with a stretching of the fiber strands in at least three draw levels, taking into account a high Crystalverstreckung in the first draw stage.
  • Essential for the success of the method according to the invention is first a slight pre-oriented molecular structure of the fiber section after spinning and cooling, in order then to obtain a uniform and continuous crystallization. In principle, however, it is also possible to process other polymers such as polyester or polyamide with the device according to the invention.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)

Claims (15)

  1. Procédé destiné à la fabrication de fibres de polypropylène à haute résistance ayant une résistance au dessus de 6 cN/dtex et une extension en dessous de 40 %, et dont les étapes sont les suivantes :
    1.1 Filage à l'état fondu d'une multiplicité d'écheveaux de fibres d'une fonte de polypropylène à une température de fonte ≤ 250°C ;
    1.2 tirage des écheveaux de fibres à une vitesse de retrait < 100 m/min, le refroidissement des écheveaux de fibres étant effectué simultanément avec un agent de refroidissement gazéiforme ;
    1.3 étirage des écheveaux de fibres en au moins trois étapes d'étirage qui sont formées par quatre bancs d'étirage, avec un ratio total d'étirage de plus de 4 : 1, les écheveaux de fibres subissant un étirage partiel d'au moins 70 % de l'étirage total dans la première étape d'étirage, et
    1.4 découpage des écheveaux de fibres en fibres de polypropylène avec une longueur de fibre prédéterminée.
  2. Procédé selon la revendication 1, caractérisé en ce que dans la deuxième étape d'étirage l'étirage partiel des écheveaux de fibres est plus grand que l'étirage partiel des écheveaux de fibres dans la troisième étape d'étirage.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu'après le filage à l'état fondu les écheveaux de fibres sont retirés par un premier banc d'étirage avec une pluralité de cylindres-étireurs, les cylindres-étireurs ayant respectivement une surface d'enveloppe réfrigérée.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce qu'à l'intérieur de la première étape d'étirage les écheveaux de fibres sont guidés à travers un canal d'étirage à chaud et chauffés à une température > 100°C.
  5. Procédé selon l'une des revendications 1 à 3, caractérisé en ce qu'après la première étape d'étirage et jusqu'à l'entrée dans la troisième étape d'étirage les écheveaux de fibres sont tempérés à une température > 100°C par le guidage par-dessus une pluralité de cylindres-étireurs chauffés.
  6. Procédé selon la revendication 4, caractérisé en ce que les cylindres-étireurs des bancs d'étirage formant la deuxième étape d'étirage ont des surfaces chauffées à des températures > 100 °C.
  7. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'à l'intérieur de la deuxième étape d'étirage les écheveaux de fibres sont guidés à travers un canal d'étirage à chaud et chauffés.
  8. Procédé selon la revendication 4 ou 7, caractérisé en ce que durant la traversée à travers le canal d'étirage à chaud les écheveaux de fibres sont chauffés par un air chaud et/ou par une vapeur surchauffée.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce qu'après l'étirage les écheveaux de fibres sont réfrigérés, dans quel cas pour être tempérés les écheveaux de fibres sont guidés à la fin de la troisième étape d'étirage par-dessus une pluralité de cylindres-étireurs réfrigérés d'un quatrième banc d'étirage.
  10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce qu'après l'étirage et avant d'être coupés les écheveaux de fibres sont frisés.
  11. Procédé selon l'une des revendications précédentes, caractérisé en ce que les écheveaux de fibres sont extrudés par une filière annulaire avec une multiplicité de 60.000 à 120.000 trous de buse.
  12. Dispositif pour la mise en oeuvre du procédé selon l'une des revendications 1 à 11 pour la fabrication d'écheveaux de fibres (5) à partir de fibres ayant des titres unitaires d'en dessous de 2 dtex., avec un dispositif de filage (1) pour le filage à l'état fondu des écheveaux de fibres (5), avec une pluralité de dispositifs de traitement (6, 7, 10, 11) pour guider et pour traiter les écheveaux de fibres (5) et avec un dispositif de coupe (12) pour découper les écheveaux de fibres (5), les dispositifs de traitement (6, 7, 10, 11) disposant d'une pluralité de bancs d'étirage (7.1, 7.2, 7.3, 7.4) avec respectivement plusieurs cylindres-étireurs (8) pour étirer les écheveaux de fibres (5), caractérisé en ce que quatre bancs d'étirage (7.1 - 7.4) sont agencés au total en trois étapes d'étirage (9.1, 9.2, 9.3) et en ce que des cylindres-étireurs (8) des bancs d'étirage (7.1, 7.4) sont enlacés une fois et sont entraînables relativement l'un par rapport à l'autre de manière telle qu'une différence de vitesse ajustée entre les bancs d'étirage (7.1, 7.4), lesquels forment la première étape d'étirage (9.1), fournit au moins 70% du ratio total d'étirage de plus de 4 : 1.
  13. Dispositif selon la revendication 12, caractérisé en ce que les cylindres-étireurs (8) des bancs d'étirage (7.2, 7.3), formant la deuxième étape d'étirage (9.2), sont réalisés de manière à pouvoir être chauffés.
  14. Dispositif selon la revendication 12 ou 13, caractérisé en ce que les cylindres-étireurs (8) d'un premier banc d'étirage (7.1) sont réalisés de manière à être réfrigérés en amont de la première étape d'étirage (9.1).
  15. Dispositif selon l'une des revendications 12 à 13, caractérisé en ce que les cylindres-étireurs (8) d'un dernier banc d'étirage (7.4) sont réalisés de manière à être réfrigérés à la fin de la troisième étape d'étirage (9.3).
EP03757872A 2002-09-26 2003-09-19 Procede de production de fibres de polypropylene a haute tenacite Expired - Fee Related EP1543184B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10244830 2002-09-26
DE10244830 2002-09-26
PCT/EP2003/010453 WO2004031459A1 (fr) 2002-09-26 2003-09-19 Procede de production de fibres de polypropylene a haute tenacite

Publications (2)

Publication Number Publication Date
EP1543184A1 EP1543184A1 (fr) 2005-06-22
EP1543184B1 true EP1543184B1 (fr) 2009-11-04

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EP03757872A Expired - Fee Related EP1543184B1 (fr) 2002-09-26 2003-09-19 Procede de production de fibres de polypropylene a haute tenacite

Country Status (8)

Country Link
EP (1) EP1543184B1 (fr)
KR (1) KR20050061480A (fr)
CN (1) CN1328423C (fr)
AU (1) AU2003273907A1 (fr)
BR (1) BR0314746A (fr)
DE (1) DE50312095D1 (fr)
RU (1) RU2318085C2 (fr)
WO (1) WO2004031459A1 (fr)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100347354C (zh) * 2006-04-17 2007-11-07 东华大学 制备聚丙烯纤维的装置
CN102453986B (zh) * 2010-10-21 2013-12-04 盟鑫工业股份有限公司 抽捻设备
AU2011369769B2 (en) * 2011-05-30 2015-09-03 The University Of Tokyo High-strength polypropylene fiber and method for producing same
KR101335659B1 (ko) * 2012-02-08 2013-12-03 건국대학교 산학협력단 콘크리트 보강용 구조용 폴리머 섬유 제조 방법
ITMI20130821A1 (it) * 2013-05-21 2013-08-20 M A E S P A Apparecchiatura per lo stiro di fibre acriliche in atmosfera di vapore in pressione e dispositivo automatico di incorsamento per detta apparecchiatura.
DE102016003796A1 (de) 2015-05-06 2016-11-10 Oerlikon Textile Gmbh & Co. Kg Verfahren und Vorrichtung zum Verstecken einer Vielzahl von schmelzgesponnenen Fasersträngen
EP3540107A4 (fr) * 2016-11-08 2020-08-05 Braskem S.A. Procédé et équipement de production d'un fil de polypropylène
CN108570721A (zh) * 2018-06-25 2018-09-25 张家港市金星纺织有限公司 一种聚丙烯纤维的制备装置
CN109295513A (zh) * 2018-12-17 2019-02-01 广东蒙泰高新纤维股份有限公司 一种熔纺—湿法纺丝工艺制备超高强低收缩丙纶长丝的方法
CN109591330B (zh) * 2019-01-18 2024-02-06 无锡盛烨特邦新材料科技有限公司 一种免胶纤维棒料生产线的免胶纤维棒料热定型机
CN112853624B (zh) * 2020-12-30 2022-12-06 天鼎丰聚丙烯材料技术有限公司 隧道专用聚丙烯长丝针刺排水土工布、制备方法及制备系统
CN113774505B (zh) * 2021-09-14 2023-08-01 徐工集团工程机械股份有限公司 一种聚丙烯纤维及制备方法及扫刷

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5846654A (en) * 1995-06-02 1998-12-08 Hercules Incorporated High tenacity, high elongation polypropylene fibers, their manufacture, and use
TW542859B (en) * 1997-12-25 2003-07-21 Chisso Corp Concrete reinforcing fiber

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Publication number Publication date
RU2005112708A (ru) 2007-05-20
CN1685092A (zh) 2005-10-19
AU2003273907A1 (en) 2004-04-23
KR20050061480A (ko) 2005-06-22
BR0314746A (pt) 2005-07-26
WO2004031459A1 (fr) 2004-04-15
CN1328423C (zh) 2007-07-25
DE50312095D1 (de) 2009-12-17
RU2318085C2 (ru) 2008-02-27
EP1543184A1 (fr) 2005-06-22

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