EP0541552B1 - Procede et dispositif de filage pour la production de microfilaments - Google Patents
Procede et dispositif de filage pour la production de microfilaments Download PDFInfo
- Publication number
- EP0541552B1 EP0541552B1 EP90917481A EP90917481A EP0541552B1 EP 0541552 B1 EP0541552 B1 EP 0541552B1 EP 90917481 A EP90917481 A EP 90917481A EP 90917481 A EP90917481 A EP 90917481A EP 0541552 B1 EP0541552 B1 EP 0541552B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- spinning
- microfilaments
- nozzle
- melt
- hot air
- 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 - Lifetime
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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
- D04H3/02—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
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- 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
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
- D01D4/025—Melt-blowing or solution-blowing dies
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
- D01D5/0985—Melt spinning methods with simultaneous stretching by means of a flowing gas (e.g. melt-blowing)
-
- 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
Definitions
- the invention relates to a method for producing microfilaments according to the preamble of claim 1, and the invention also relates to a spinning device for producing microfilaments.
- microfilaments Synthetic filaments with a single titer of less than 1 dtex are referred to as microfilaments (the specification 1 dtex means that 10 km of the thread or filament weighs 1 gram).
- the microfilaments therefore have a very small diameter and are twisted in a known manner to form microfilament yarns.
- These microfilament yarns can be woven or knitted to make a textile. Due to the single titer of less than 1 dtex, the textiles are characterized by a very soft feel and a noble case, so that they have a silk-like character and can follow the fashion trend of silk fabrics.
- microfilaments takes place in that the microfilament is drawn off and stretched at a high take-off speed from the spinning hole of a spinneret fed with a melt and is taken up on a roll after passing through an area blown transversely with cooling air. This is followed by twisting with a large number of microfilaments to form a microfilament yarn from which the desired textile can be produced by weaving.
- spunbonded nonwovens from the microfilaments by pulling the filaments emerging from spinnerets under the action of an injector after passing through an area blown transversely with cooling air and depositing them on a continuously moving deposit belt.
- Such spunbonded nonwovens made from microfilaments are also covered by the invention.
- the filament diameter is below 12 »m for polypropylene and below 11» m for polyamide or below 10 »m for polyester.
- the microfilament yarns obtained from it which are mostly offered as polyamide and polyester yarns, generally have a single titer that is only slightly less than 1 dtex.
- the microfilament yarns and textile products resemble the fashionably preferred natural silk due to their soft feel.
- the textile yarns made from microfilaments have yet another advantage that is due to the tightness of the fabric.
- Fabrics made from microfilament yarns can be woven so densely that their diffusion properties are similar to semi-permeable diaphragms. These fabrics breathe, that is, they let gases and vapors such as water vapor through easily, even though they are poorly wettable at the same time. The poor wettability is due to the small filament diameter and the resulting unfavorable angles between two filament surfaces.
- the polymer melt is extruded through the spinneret, cooled by an air stream below the spinneret and drawn off at high speed - usually around 6,000 m / min.
- the aim in practice is to reduce the diameter of the microfilaments during their manufacture to a single titer of significantly less than 1 dtex.
- the number of microfilaments in the yarn or the number of nozzle holes per microfilament yarn must be used increase proportionally to the reduction in the individual titer in d-tex, because several microfilaments are then required to produce a microfilament yarn with the same diameter.
- the filament surface is inversely proportional to the third power of the filament diameter for the same volume. If, for example, the individual titer is halved, the thinner filament has an eightfold surface.
- the larger surface area can be seen in connection with the cooling of the microfilament. Basically, the stretching of the microfilament requires a certain temperature, and if it cools down too much, there is a risk that the microfilament will become brittle and tear off, especially at the usual high take-off speeds of 6,000 m / min.
- hypothermic skin will form on the surface of the microfilament. This skin is responsible for the filament breaks.
- the skin is already rigid, while the inner mass, which is surrounded by the skin, is still in a stretchable state.
- a cut-off is only possible here if the take-off speed is considerably reduced, and at the same time the mass flow of the melt through the spinneret must be reduced accordingly. In the other case, if the mass flow remains constant, the reduction in the draw-off speed would result in the filaments not being able to be produced with the desired small diameter.
- a cylindrical screen is arranged concentrically within the pressure chamber, and warm air under pressure is supplied to the pressure chamber from outside and pressed through the cylindrical screen, in which the filaments freshly extruded from the spinneret are drawn.
- the warm air is supplied in a direction which is predominantly transverse to the direction in which the filaments are drawn off, as a result of which the filaments are subjected to a load within the pressure chamber or within the cylindrical screen.
- turbulence inevitably occurs in the cylindrical sieve, which places an additional load on the freshly drawn filaments.
- the filaments can only be enveloped by the warm air in a jacket-like manner after they have left the outlet pipe adjoining the pressure chamber below.
- the known method is not suitable for the production of microfilaments, i.e. filaments with a single titer of less than 1 dtex, because the stresses mentioned are within the pressure chamber or within the cylindrical sieve, i.e. in an area that is directly adjacent to the outlet opening of the Spinning hole connects, are too large. Otherwise, the filaments in a cooling area are not blown with cooling air parallel to the direction of the filaments.
- EP-A-0 245 011 also discloses a similar process for the production of filaments, the filaments being drawn off and stretched from a spinneret fed with a melt through a spinning hole after passing through a cooling area at a high take-off speed.
- a chamber with a cylindrical sieve immediately adjoins the spinning hole, through which warm air is fed under pressure transversely to the direction of the filaments. Only after leaving the chamber mentioned does the warm air supplied run in one direction parallel to the filaments.
- the disadvantages mentioned above apply to the area directly at the outlet opening of the spinning hole when it comes to the production of microfilaments with a very small diameter.
- the invention has for its object to provide a method which allows the production of microfilaments with very small diameters without deterioration of economy and quality, and also to be created by the invention, a spinning device which allows economical production of microfilaments with small diameters .
- this object is achieved in the method presupposed in the preamble of patent claim 1 by the features of the characterizing part, and with regard to the spinning device, the object in a spinning apparatus according to the preamble of patent claim 10 is achieved by the method characteristic features solved.
- the invention provides that the microfilaments are accompanied by a downward flow of hot air immediately after they exit the spinning hole.
- the extruded filament is thus embedded in a warm air stream after exiting the spinning hole, which preferably surrounds the filament in the form of a jacket.
- the hot air coating compensates for the negative influence of the large surface area of the microfilaments, which leads to rapid cooling. This prevents the filament from cooling too quickly - due to the much higher specific surface area.
- a major advantage of the invention is therefore that the filament can be drawn off easily even at the usual high speeds of 4,000-6,000 n / min.
- microfilament yarns produced by the method according to the invention thus guarantee a significantly better quality, the disadvantages described at the outset being eliminated.
- the protective jacket made of hot air protects the just extruded and formed filament from cooling too quickly immediately after it emerges from the spinning hole of the spinneret. Thus, no rapidly cooled outer skin of the filament can arise, which would be damaged by the shear stress caused by the rapid filament draw-off without cracks and would lead to a filament breakage.
- the filament cools gradually, so that - viewed radially - a uniform structure is formed. This allows the very fine microfilament with a small diameter to be stretched optimally. Furthermore, differences between the individual filaments of a multifilament spinneret are largely suppressed, which leads to a significant improvement in quality.
- the cooling of the microfilament is under control, so that the risk of microfilaments with different diameters being avoided is avoided.
- deviations in the diameters in the prior art are only slight, they are nevertheless noticeable, e.g. in that when the microfilaments or the textile are colored, the color of the different microfilaments with different diameters is also taken up differently. As a result, the uniform color impression of the product used as a high-quality textile suffers.
- the method for producing microfilaments also includes known very small diameter Polymers used that are spinnable from a melt.
- polyolefins, especially polypropylene, furthermore polyester and polyamide 6 and 6,6 can be spun by the process according to the invention.
- Known bicomponent nozzles can advantageously be used, whereby it must be ensured that the outer part of the combined spinneret is modified in such a way that a uniform distribution of the hot air over all bores is ensured. Furthermore, the outer holes of the combined nozzle must be adapted to the air flow.
- Such bicomponent nozzles have a jacket-core arrangement, in which case only the core nozzle is used for spinning the polymer melt and the hot air flow is generated at the jacket nozzle.
- the spinning conditions with regard to the polymer melt can essentially be maintained in the invention as they are set when spinning a conventional spinning device.
- the air temperatures in the outer part of the spinneret (bicomponent nozzle) depend on the melting temperature Embodiment of the invention is provided that the temperature difference between the two components should not be exceeded ⁇ 10 ° C. In the optimal case, the temperatures of the two components, melt and air, are equal.
- the amount of air in the hot air can be adjusted in a simple manner, a minimum setting being necessary in order to ensure that a clean free jet is formed at each spinning hole at least just below the spinneret.
- the microfilaments After running a distance of approximately 100 to 500 mm below the spinneret, the microfilaments can be cooled more intensely by cross-blowing, whereby the usual blowing chutes can be used here.
- aerodynamic take-off devices in the form of an injector can also be used expediently within the scope of the invention, so that the microfilaments formed according to the invention can be used in a known manner and Wise also a spunbond can be formed.
- the spinning device designated as a whole with the reference number 10 in FIG. 1 is known per se. It has a spinneret 12 with a spinning hole 14, through which melt 16 exits and is stretched into a microfilament 18.
- the representation according to FIG. 1 shows only the case of a single microfilament. In practice, if a large number of microfilaments are produced, the spinneret 12 has a corresponding number of spinning holes 14.
- the melt 16 When leaving the spinning hole 14, the melt 16 has a temperature of approximately 280 ° C. A transverse blowing with cooling air is indicated by the arrow 22, and the microfilament 18 cools down to such an extent that it still has a temperature of about 60 ° C. at the bottom of the roll.
- the microfilament 18 is thus stretched by the roll, the rotational speed of which is decisive for the take-off speed.
- a usual value of the take-off speed in FIG. 1 is 4000 to 6000 m / min.
- FIG. 1 shows a spinning device for production clarified by microfilament yarns from which a textile can be woven or knitted
- FIG. 2 shows a spinning device for the production of spunbonded webs known per se.
- the take-off device is designed aerodynamically and is formed by an injector 24.
- the microfilaments are deposited on a laterally moving catch belt 36.
- a practical embodiment of the method according to the invention results from the exemplary embodiment of the spinning device according to FIG. 3.
- the extruded microfilament 18 is embedded in a warm air flow indicated by the arrows A.
- This warm air flow A accompanies the microfilament essentially within the stretching area 38, which is the main stretching area with a length of approximately 30 to 50 cm.
- the total distance 1 between the bicomponent nozzle 26 and the roller 20 is approximately 1 m.
- the microfilament 18 is blown transversely with cooling air 22 as in FIGS. 1 and 2.
- the temperature of which is the melt temperature of 280 ° C at the exit through the spinning hole 14 should not exceed or differ by ⁇ 10 ° C., too rapid cooling of the microfilament 18 is prevented. Rather, the cooling of the microfilament 18 is delayed and carried out continuously in the invention.
- the invention ensures that, despite a reduction in the diameter of the microfilament 18, it is possible to work with the usual take-off speed of 4000-6000 m / min, so that the economy of a spinning system is not lost if smaller diameters of the microfilaments are desired.
- a bicomponent nozzle 26 which is shown in more detail in FIG. 4 and which has a core nozzle 28 and a jacket nozzle 30 and also has an annular gap 32, can be used to generate the hot air flow A which is decisive in the invention.
- the annular gap 32 surrounds an annular shape the spinning hole 34 from which the melt emerges.
- melt is extruded both through the spinning hole 34 of the core nozzle 28 and through the annular gap 32 of the jacket nozzle 30, it is provided according to FIG. 4 that the melt exits exclusively via the inner core nozzle 28.
- the hot air flow is supplied or generated through the annular gap 36 under pressure p and temperature T, which then surrounds the microfilament 18 in the form of a jacket.
- the invention can also be used for the production of spunbonded fabric in a spinning device according to FIG. 2.
- microfilament yarns with a super fine single titer of 0.33 dtex can be produced without sacrificing the economy of a spinning system, so that it is possible to produce textiles that are practically equivalent to natural silk.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Artificial Filaments (AREA)
Claims (13)
- Procédé de fabrication de microfilaments de petit diamètre pour fils synthétiques ou pour matières textiles, les microfilaments sortant des filières alimentés par une masse fondue à travers un trou de filière (alésage) après passage d'une zone qui est refroidie transversalement par un courant d'air froid, étant tirés et étirés à grande vitesse d'extraction, caractérisé en ce que les microfilaments sortent directement du trou de filière et sont exposés à un courant d'air chaud de façon que le courant d'air chaud enveloppe comme un manteau le microfilament aussitôt après qu'il soit sorti du trou de filière.
- Procédé suivant la revendication 1, caractérisé en ce que le courant d'air chaud est envoyé sous pression et à une température correspondant à peu près à la température de la masse fondue.
- Procédé suivant l'une des revendications précédentes 1 et 2, caractérisé en ce que la différence de la température de la masse fondue et la température de l'air chauffé va jusqu'à environ + ou - 10° C.
- Procédé suivant l'une des revendications précédentes 1 à 3, caractérisé en ce que les microfilaments sont refroidis par un courant d'air froid transversal à une certaine distance au-dessous de la filière.
- Procédé suivant la revendication 4, caractérisé en ce que la distance est d'au moins environ 100 mm, de préférence 500 mm.
- Procédé suivant l'une des revendications précédentes 1 à 5, caractérisé en ce que les filaments tirés et étirés sont retordus ou enroulés en un fil de microfilaments.
- Procédé suivant l'une des revendications 1 à 5, carac térisé en ce que les microfilaments tirés et étirés sont tiragés en une matières textiles.
- Procédé suivant la revendication 7, caractérisé en ce que les microfilaments sont tirés par un dispositif de tirage aérodynamique.
- Dispositif de filage pour la fabrication de microfilaments de petit diamètre pour fils synthétiques ou pour matières textiles, sortant des filières alimentées par une masse fondue par un trou de filière (alésage) après passage d'une zone qui est refroidie transversalement par de l'air froid, les microfilaments étant tirés et étirés à grande vitesse d'extraction, caractérisé en ce que le dispositif de filage (10) comporte une filière multiple (26) avec plusieurs trous de filière (34), par lesquels sort la masse fondue et en ce que la filière multiple est prévue concentrique à chaque trou de filière (34) avec une sortie (32) par laquelle sort un courant d'air chaud (A).
- Dispositif de filage suivant la revendication 9, caractérisé en ce que la filière multiple 526) est formée selon la technique d'une filière bicomposante avec une filière centrale (28) et une filière enveloppante (30).
- Dispositif de filage suivant la revendication 10,caractérisé en ce que la filière enveloppante (30) se compose d'une fente annulaire (32) entourant concentriquement la filière centrale (28) prévue pour la sortie de la masse fondue (16), fente par laquelle sort sous pression (p) de l'air chauffé (A).
- Dispositif de filage suivant l'une des revendications précédentes 9 à 11, caractérisé en ce que le dispositif de filage comporte une poulie (20) servant de dispositif de tirage mécanique pour les microfilaments (18).
- Dispositif de filage suivant l'une des revendications précédentes 9 à 11, caractérisé en ce que le dispositif de filage contient un injecteur (24) servant de dispositif de tirage aérodynamique pour les microfilaments (18) ainsi qu'une bande de réception pour la formation d'une matière textile.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3941824A DE3941824A1 (de) | 1989-12-19 | 1989-12-19 | Verfahren und spinnvorrichtung zur herstellung von mikrofilamenten |
DE3941824 | 1989-12-19 | ||
PCT/DE1990/000941 WO1991009162A1 (fr) | 1989-12-19 | 1990-12-03 | Procede et dispositif de filage pour la production de microfilaments |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0541552A1 EP0541552A1 (fr) | 1993-05-19 |
EP0541552B1 true EP0541552B1 (fr) | 1994-06-29 |
Family
ID=6395741
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP90917481A Expired - Lifetime EP0541552B1 (fr) | 1989-12-19 | 1990-12-03 | Procede et dispositif de filage pour la production de microfilaments |
Country Status (7)
Country | Link |
---|---|
US (1) | US5310514A (fr) |
EP (1) | EP0541552B1 (fr) |
JP (1) | JP2918332B2 (fr) |
KR (1) | KR920703889A (fr) |
AT (1) | ATE107971T1 (fr) |
DE (2) | DE3941824A1 (fr) |
WO (1) | WO1991009162A1 (fr) |
Families Citing this family (14)
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SG67284A1 (en) * | 1991-09-06 | 1999-09-21 | Akzo Nobel Nv | Apparatus for high speed spinning multifilament yarns and use thereof |
US5382400A (en) | 1992-08-21 | 1995-01-17 | Kimberly-Clark Corporation | Nonwoven multicomponent polymeric fabric and method for making same |
US5405682A (en) | 1992-08-26 | 1995-04-11 | Kimberly Clark Corporation | Nonwoven fabric made with multicomponent polymeric strands including a blend of polyolefin and elastomeric thermoplastic material |
CA2092604A1 (fr) | 1992-11-12 | 1994-05-13 | Richard Swee-Chye Yeo | Fils polymeres hydrophiles composites; non-tisses obtenus avec ces fils |
US5482772A (en) | 1992-12-28 | 1996-01-09 | Kimberly-Clark Corporation | Polymeric strands including a propylene polymer composition and nonwoven fabric and articles made therewith |
BR9400682A (pt) * | 1993-03-05 | 1994-10-18 | Akzo Nv | Aparelho para a fiação em fusão de fios multifilamentares e sua aplicação |
US5759926A (en) * | 1995-06-07 | 1998-06-02 | Kimberly-Clark Worldwide, Inc. | Fine denier fibers and fabrics made therefrom |
KR100445769B1 (ko) | 1995-11-30 | 2004-10-15 | 킴벌리-클라크 월드와이드, 인크. | 극세섬유 부직웹 |
JP3662455B2 (ja) * | 1999-11-22 | 2005-06-22 | ユニ・チャーム株式会社 | ポリプロピレン製不織布およびその製造方法 |
DE10026281B4 (de) * | 2000-05-26 | 2005-06-02 | Sächsisches Textilforschungsinstitut e.V. | Verfahren zur Herstellung von Spinnvliesen |
BR0107280A (pt) | 2001-09-17 | 2004-03-23 | Rhodia Poliamida Ltda | Microfibras para reforço de matrizes inorgânicas, como cimento, argamassa. gesso e concreto, microfibras à base de poliamida para reforço de matrizes inorgânicas, processo para obtenção de microfibras à base de poliamida para reforço de matrizes inorgânicas e produtos à base de fibrocimento |
BRPI0906807B1 (pt) * | 2008-01-21 | 2019-02-19 | Imerys Pigments, Inc. | Fibra monofilamentar |
CN106555257B (zh) * | 2016-12-02 | 2019-05-10 | 武汉纺织大学 | 一种利用熔喷超细纤维进行喷气纺纱的装置和方法 |
CN106835417B (zh) * | 2016-12-02 | 2019-05-10 | 武汉纺织大学 | 一种利用熔喷超细纤维制备包芯纱的装置及方法 |
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1989
- 1989-12-19 DE DE3941824A patent/DE3941824A1/de active Granted
-
1990
- 1990-12-03 JP JP3500064A patent/JP2918332B2/ja not_active Expired - Fee Related
- 1990-12-03 AT AT90917481T patent/ATE107971T1/de not_active IP Right Cessation
- 1990-12-03 WO PCT/DE1990/000941 patent/WO1991009162A1/fr active IP Right Grant
- 1990-12-03 DE DE59006327T patent/DE59006327D1/de not_active Expired - Fee Related
- 1990-12-03 KR KR1019920701460A patent/KR920703889A/ko not_active Application Discontinuation
- 1990-12-03 US US07/862,570 patent/US5310514A/en not_active Expired - Fee Related
- 1990-12-03 EP EP90917481A patent/EP0541552B1/fr not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
JP2918332B2 (ja) | 1999-07-12 |
DE3941824C2 (fr) | 1992-01-16 |
DE59006327D1 (de) | 1994-08-04 |
JPH05502483A (ja) | 1993-04-28 |
KR920703889A (ko) | 1992-12-18 |
DE3941824A1 (de) | 1991-06-27 |
ATE107971T1 (de) | 1994-07-15 |
US5310514A (en) | 1994-05-10 |
EP0541552A1 (fr) | 1993-05-19 |
WO1991009162A1 (fr) | 1991-06-27 |
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