EP1030937B1 - Borsten oder interdentalreiniger aus einem monofil - Google Patents

Borsten oder interdentalreiniger aus einem monofil Download PDF

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Publication number
EP1030937B1
EP1030937B1 EP98962315A EP98962315A EP1030937B1 EP 1030937 B1 EP1030937 B1 EP 1030937B1 EP 98962315 A EP98962315 A EP 98962315A EP 98962315 A EP98962315 A EP 98962315A EP 1030937 B1 EP1030937 B1 EP 1030937B1
Authority
EP
European Patent Office
Prior art keywords
bristles
monofilament
interdental cleaner
bristle
matrix
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
Application number
EP98962315A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1030937A1 (de
Inventor
Georg Weihrauch
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.)
Pedex GmbH
Original Assignee
Pedex GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Pedex GmbH filed Critical Pedex GmbH
Publication of EP1030937A1 publication Critical patent/EP1030937A1/de
Application granted granted Critical
Publication of EP1030937B1 publication Critical patent/EP1030937B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • A46D1/02Bristles details
    • A46D1/023Bristles with at least a core and at least a partial sheath
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • A46D1/02Bristles details
    • A46D1/0238Bristles with non-round cross-section
    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • A46D1/02Bristles details
    • A46D1/0261Roughness structure on the bristle surface
    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • A46D1/02Bristles details
    • A46D1/0292Bristles having split ends
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46BBRUSHES
    • A46B2200/00Brushes characterized by their functions, uses or applications
    • A46B2200/10For human or animal care
    • A46B2200/1066Toothbrush for cleaning the teeth or dentures

Definitions

  • the invention relates to bristles or interdental cleaners made of a monofilament with reduced secondary binding forces from at least two in geometrically regular Arrangement of coextruded polymers with interfaces running essentially in the axial direction for the production of bristles or interdental cleaners that by the action of mechanical forces essentially in Axis direction are slit.
  • the invention is also based on a process for the production of bristles or interdental cleaners from such monofilaments and on bristle goods such bristles or aimed at interdental cleaners.
  • Bristles for bristle products of any kind e.g. Brushes for Body and dental care, household brushes, technical brushes, Brushes and the like are mostly used today Polymers made by melting the polymer into continuous monofilaments extruded, the monofilaments stretched and, if necessary be stabilized. From such monofilaments the bristles are then cut to the desired length receive. As a rule, the monofilaments, like the Bristles, circular cylindrical cross section. For special ones Bristles with other, e.g. oval or polygonal cross section known. With a the corresponding profile, the monofilament is then extruded.
  • bristles in one fibrous, especially fine-fibrous structure at the end of use use. This applies, for example, to such bristles were used to apply media Surfaces or the like are determined, e.g. Brush. Also then if a fluffy structure is desired, must the bristle should be fine-grained. More recently insights also gained in dental medicine, after which conventional bristles of toothbrushes in their Cleaning effects are inadequate since they are not in the fine fissures penetrate the tooth surface, but glide over them. The same applies to the cleaning effect in the interdental space.
  • the monofilament from polymer blends to extrude To get highly fibrous structures is already have been proposed, the monofilament from polymer blends to extrude. The following effects are used: during the extrusion and subsequent stretching of the The polymer molecules become monofilament in the longitudinal direction of the Oriented to monofilament. The acting in the longitudinal direction primary binding forces ensure high tensile strength. The longitudinal orientation of the molecules also brings the desired bending elasticity. With monofilament from one the only polymer are the so-called secondary binding forces, namely the forces across the molecular extension big enough to fray or unravel to prevent the monofilament or bristle. at Monofilaments made from two different, mixed polymers however, arise between the molecular chains of the polymers while stretching sliding zones in which the secondary binding forces are reduced.
  • Such one Monofilament or a bristle made from it can be by the action of mechanical forces by means of knife-like Shredding tools.
  • the resulting So-called flags have a very irregular Shape, irregular cross sections and frayed Shell surfaces.
  • the flags show uncontrolled Strength properties. They tear out, break off or lay down.
  • Such are frayed bristles consequently unsatisfactory, even for many applications disabled.
  • the use of toothbrushes is hygienic Reasons questionable.
  • a known embodiment has the same disadvantages a bristle (WO97 / 14830), which has a core and a Coat owns that by coextrusion of two different ones Polymers are made. On the usage side The end of the bristle is mechanically or chemically ablated to form a recessed pocket which should take up dentifrice or color. Further describes the formation of flags ("flags") which by shredding the material of the jacket, insofar as this tower over the core, be preserved. This fraying too takes place in a conventional manner by means of knives and guides therefore to the same irregular structures.
  • flags flags
  • Interdental cleaners are also known (WO 96/39117), those made of co-extruded monofilaments in a geometric arrangement consist. Each monofilament consists of at least two polymer components, those in the interface between neighboring ones Monofilaments lead to reduced secondary binding forces. The secondary forces become due to tensile forces in the axial direction degrades and creates a multi-fiber fluffy Structure similar to that of dental floss.
  • the invention has for its object bristles or interdental cleaner from a monofilament propose at least two common extruded polymers.
  • the slotted bristles or Interdental cleaners have reproducible strength properties and form definable according to number, shape and dimensioning Flags or slots. Furthermore, with the invention a method for producing bristles or interdental cleaners from such monofilaments are proposed become.
  • a bristle solving this task with the characteristics of The preamble of claim 1 is distinguished according to the invention in that the interfaces are boundary layers, in which are subject to the reduced secondary binding forces, and that the monofilament is a matrix from which the physical and chemical properties of the bristle or the interdental cleaner determining polymer, and that second polymer in the form of thinner interfaces Layers are embedded in the matrix.
  • the geometry of the boundary layers can be used to predict in what way the monofilament for an interdental cleaner, or cut to length from the monofilament bristles produced by the action of mechanical forces is slit or split.
  • the slots or flags arise exactly in the geometry of the extrudate predetermined contour. Because the boundary layers are longitudinal of the monofilament, each owns Flag the same shape and same along its entire length Cross-section. All flags therefore have the same name Strength properties, in particular the same bending behavior and equal tensile strength. It is also possible by appropriate design of the geometry flags with different cross sections.
  • the flags can with appropriate Cross-sectional shape on the facing edges form that support the cleaning effect.
  • Such a way split bristle is consequently on its outer surface also more effective than conventional bristles.
  • the bristle does not spread too much on.
  • each bristle takes on a monofilament shape and that Flags only come about through axial or radial pressure full effect. This makes it easy to record media and give it back when applying by pressing.
  • the bristles according to the invention and their flags can be produced have the favorable properties of conventional bristles.
  • the bristles according to the invention and their flags can be produced have the favorable properties of conventional bristles.
  • the bristles according to the invention and their flags can be produced have the favorable properties of conventional bristles.
  • the bristle also did not undergo extensive cleaning processes must become.
  • Flagged bristles are defined or defines slotted monofilaments for interdental cleaners get where a progressive splitting or Slitting can be avoided.
  • the polymer of the matrix, as well as the thin layers can be a copolymer or a polymer blend.
  • the above-mentioned advantages are particularly optimal reached when the thin layers share a portion of the Polymers of the matrix included. In this case it breaks Polymer or the bristle when force is applied to the weakest point, namely in the middle of the thin Layers on, however, the adherence of the remaining layers due to the proportion of polymer corresponding to the matrix sufficient at the emerging neighboring flags large to avoid the formation of fine particles.
  • the thin layers preferably have a thickness of a few ⁇ m. Have practical extrusion attempts shown that such thin layers with the polymer let the matrix co-extrude.
  • the two polymers can too about the same parts.
  • the specific execution of the geometry is determined by the desired Properties of the bristle or interdental cleaner certainly. So the thin layers in the Matrix extend to the extent of the monofilament, so that the Slotted monofilament with relatively little force or can be split.
  • the thin layers in of the matrix end at a distance from the circumference of the monofilament. In in this case you need a little bit more force, but it is advantageous here that the resulting Flags also in the edge area from the matrix material exist, i.e. the same wear properties as the coat of the bristle or the flags has.
  • the matrix of the monofilament can have a third have embedded polymer in the matrix, which in primarily to influence the strength properties the resulting flags.
  • the monofilament can usually be of a circular shape, but also one that deviates from the circular shape Have cross-section.
  • cross-section are polygonal ones in particular To mention cross sections in their cleaning effect are more effective than round cross-sections.
  • the thin layers can go to the corners of the polygonal cross section, so that relative sharp edges with an edge angle of less than 90 ° arise.
  • the thin layers can also be added to the Faces of the polygonal cross-section run out, whereby then edges with an edge angle in the range of 90 ° can be realized.
  • the matrix consists of polyamide and the thin layers of a polyolefin, especially polypropylene or polyethylene.
  • a polyolefin especially polypropylene or polyethylene.
  • both can be used to make bristles interdental cleaners can also be used in such a way that which coextrudes the at least two polymers to the monofilament and that the monofilament after extruding, stretching and optionally stabilization by action mechanical forces transverse to the monofil axis on local limited length slotted along the boundary layers becomes.
  • the method according to the invention can be used form fissure-like slits on the jacket of the monofilament, that can be used to hold media.
  • For toothbrushes or interdental cleaners come in particular for this Dental care products or dental medicine or antibacterial Preparations in question. Otherwise the monofilament is preserved Interdental cleaner on the jacket through the slit increased roughness.
  • the interdental cleaners according to the invention can be made from the aforementioned monofilament produce in any length.
  • the same measure can of course also on the bristle cut to length from the monofilament be made.
  • the location of the slit and the expansion of the slots to the length of the bristle be matched to split the bristle end either to avoid or to specifically promote. For example, only the bristle end can be split.
  • the slits still made in the jacket can after the flags have worn down to further split the Bristle serve.
  • the type and number of stored Layers create a corresponding number of flags at the end of use of the bristle.
  • any length is according to a variant of the Procedures provided that the monofilament during or after the action of mechanical forces in the axial direction is compressed. This will make the slotted Areas or the webs delimiting the slots on Monofilament jacket bulged outwards.
  • the mechanical forces are preferably on the most of the circumference of the monofilament or bristle applied to ensure that all boundary layers of the polymers are applied.
  • the slitting of the monofilament or the splitting of the bristles is preferably done by striking forces. Instead can also use crushing or torsional forces to be brought. These forces can be tailored to the Bristle or at the same time on groups of bristles, e.g. on bundles of bristles, before or after their attachment take effect on the bristle holder of the brush.
  • the bristles are preferably on their usage side Ends rounded. This can be done before and / or after splitting happen. In a further preferred embodiment of the method become the multiple that arise after splitting Ends with a length that visually indicates the usable length Mark it. This signals to the user that after the bristle wears down to the mark, So after the split ends wear out, the Change use properties abruptly, because then the much more rigid cross section of the entire bristle comes into effect. Also the split ends ever shorter and therefore mechanically more aggressive. A such notification is particularly advisable if it are toothbrushes, body care brushes or the like.
  • polyamides come as polymers for the matrix 2 (PA) in question, while the thin layers 3 for example from a polymer mixture PA / PP or PA / PE consist.
  • Fig. 3 with a monofilament 1 polygonal, namely triangular cross section. at this embodiment run the stored thin layers, which can also be seen from the center extend outside, in the corners of the polygon. Instead you can of course also on the areas between end the corners.
  • Matrix 2 of monofilament 1 is yet another of several possible polymers extruded in such a way that it is completely embedded in the matrix.
  • it is thread-like structures 5, which according to the manufacture of the bristle and the splitting or slitting the same the bending behavior or the strength of the influence emerging flags.
  • Fig. 5 shows a flat rectangular monofilament 1, in which the thin layers 3 are laid out like a grid, so that from the monofilament a variety of essentially rectangular ones Flags can be generated.
  • Fig. 8 shows finally a monofilament cross section in which the matrix 2 from four identical outer parts with the cross section of circular sectors and a central core that delimited by correspondingly extending thin layers 3 are.
  • a bristle 6 is shown schematically, which consists of a monofilament, for example according to FIG. 2, by cutting to length manufactured and by the action of mechanical forces its end of use is split up, so that individual Flags 7 arise, the shape of the shape of which Matrix 2 forming areas of the monofilament corresponds. It As many flags are created as the Matrix 2 by thin ones Layers 3 is broken down. The usage length of the Flags can be shown, for example, by the one shown in FIG The dash must be optically marked.
  • a monofilament according to FIG. 7 can also be of any length Interdental cleaners ("floss”) serve the slits Take up dentifrices, antiseptics or antibactericides can. Recommended for an interdental cleaner itself to axially compress the monofilament, as shown in Fig. 9 shows that the webs 10 delimiting the slots bulge outward from the matrix polymer.
  • Interdental cleaners serve the slits Take up dentifrices, antiseptics or antibactericides can.
  • Fig. 9 shows that the webs 10 delimiting the slots bulge outward from the matrix polymer.
  • the matrix 2 or the polymer forming it can in the individual cross-sectional parts delimited by the thin layers be different colors.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Brushes (AREA)
  • Multicomponent Fibers (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
EP98962315A 1997-11-05 1998-11-03 Borsten oder interdentalreiniger aus einem monofil Expired - Lifetime EP1030937B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19748733 1997-11-05
DE19748733A DE19748733A1 (de) 1997-11-05 1997-11-05 Monofil zur Herstellung von Borsten und Verfahren zur Herstellung von Borsten aus solchen Monofilen
PCT/EP1998/006954 WO1999024649A1 (de) 1997-11-05 1998-11-03 Monofil für und zur herstellung von borsten oder interdentalreiniger, sowie borstenware mit solchen borsten und interdentalreiniger

Publications (2)

Publication Number Publication Date
EP1030937A1 EP1030937A1 (de) 2000-08-30
EP1030937B1 true EP1030937B1 (de) 2004-05-19

Family

ID=7847605

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98962315A Expired - Lifetime EP1030937B1 (de) 1997-11-05 1998-11-03 Borsten oder interdentalreiniger aus einem monofil

Country Status (18)

Country Link
EP (1) EP1030937B1 (tr)
JP (1) JP2001522948A (tr)
KR (1) KR100568958B1 (tr)
CN (1) CN1105198C (tr)
AR (1) AR010957A1 (tr)
AU (1) AU749645B2 (tr)
BR (1) BR9813195A (tr)
CA (1) CA2308848A1 (tr)
DE (2) DE19748733A1 (tr)
EG (1) EG21972A (tr)
ES (1) ES2219925T3 (tr)
PL (1) PL194178B1 (tr)
RU (1) RU2197572C2 (tr)
TR (1) TR200001242T2 (tr)
TW (1) TW440615B (tr)
UA (1) UA57814C2 (tr)
WO (1) WO1999024649A1 (tr)
ZA (1) ZA9810077B (tr)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19841974A1 (de) * 1998-09-14 2000-03-23 Braun Gmbh Borste für eine Zahnbürste, insbesondere für eine elektrische Zahnbürste, sowie Verfahren zu deren Herstellung
DE19918959A1 (de) * 1999-04-27 2000-11-02 Pedex & Co Gmbh Verfahren zur Bearbeitung von Borsten und Borstenwaren mit solchen Borsten
DE19932376A1 (de) * 1999-07-13 2001-01-18 Coronet Werke Gmbh Borste für Zahnbürsten und Zahnbürste mit solchen Borsten
DE10010572A1 (de) * 2000-03-03 2001-09-06 Coronet Werke Gmbh Borste mit antimikrobieller Ausrüstung, Borstenware mit solchen Borsten sowie Verpackung für solche Borsten oder Borstenwaren
DE10017306A1 (de) 2000-04-09 2001-10-11 Pedex & Co Gmbh Verfahren zur Herstellung von Borsten zum Applizieren von Medien
DE10033256A1 (de) * 2000-07-10 2002-01-24 Coronet Werke Gmbh Verfahren und Vorrichtung zur Herstellung von Borstenwaren sowie Borstenware
DE10212701B4 (de) * 2002-03-21 2015-05-13 Geka Gmbh Borste, Verfahren und Vorrichtung zu ihrer Herstellung sowie Borstenware
JP2007050497A (ja) * 2005-08-19 2007-03-01 Kowa Co Ltd ブラシ用毛材
JP5236864B2 (ja) * 2006-02-15 2013-07-17 Kbセーレン株式会社 デンタルフロス用糸、デンタルフロスおよびその製造方法
JP2007215703A (ja) * 2006-02-15 2007-08-30 Kb Seiren Ltd デンタルフロス用糸およびデンタルフロス
EP2198744B1 (de) * 2008-12-19 2011-11-09 Braun GmbH Borstenbüschel und Zahnbürste mit Borstenbüschel
KR101331936B1 (ko) * 2012-01-17 2013-11-26 장준호 문 고정 장치
EP2921576B1 (en) * 2012-11-19 2019-06-05 Toray Industries, Inc. Conjugated fiber, and process for manufacturing ultrafine fibers
GB201600846D0 (en) 2016-01-18 2016-03-02 Glaxosmithkline Consumer Healt Novel device
EP3516988A1 (en) * 2018-01-30 2019-07-31 GEKA GmbH An improved bristle for brushes

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3117362A (en) * 1961-06-20 1964-01-14 Du Pont Composite filament
US3173163A (en) * 1963-03-29 1965-03-16 E B & A C Whiting Company Flagged brush bristles
JPS4887119A (tr) * 1972-02-24 1973-11-16
US5032456A (en) * 1987-09-11 1991-07-16 Newell Operating Company Microcellular synthetic paintbrush bristles
US5128208A (en) * 1990-12-14 1992-07-07 E. I. Du Pont De Nemours And Company Flaggable synthetic tapered paintbrush bristles
CA2219276A1 (en) * 1995-06-06 1996-12-12 Gillette Canada Inc. Dental floss
BR9611001A (pt) * 1995-06-07 2002-06-04 Kimberly Clark Co Fibras de denier fino e tecidos feitos a partir destas
DE19533815A1 (de) * 1995-09-13 1997-03-20 Coronet Werke Gmbh Zahnbürste und Verfahren zu ihrer Herstellung
US5770307A (en) * 1995-10-18 1998-06-23 E. I. Du Pont De Nemours And Company Coextruded monofilaments
DE29700611U1 (de) * 1997-01-15 1997-03-13 Klaus Sindel RUSI-Kosmetik-Pinsel-Brushes GmbH, 91572 Bechhofen Fasern für Kosmetikbürsten
AU2680197A (en) * 1997-04-24 1998-11-13 E.I. Du Pont De Nemours And Company Monofilaments with split ends

Also Published As

Publication number Publication date
CN1278309A (zh) 2000-12-27
JP2001522948A (ja) 2001-11-20
RU2197572C2 (ru) 2003-01-27
DE19748733A1 (de) 1999-05-06
PL340384A1 (en) 2001-01-29
TR200001242T2 (tr) 2000-09-21
DE59811434D1 (de) 2004-06-24
EP1030937A1 (de) 2000-08-30
UA57814C2 (uk) 2003-07-15
ZA9810077B (en) 1999-05-07
WO1999024649A1 (de) 1999-05-20
TW440615B (en) 2001-06-16
PL194178B1 (pl) 2007-05-31
AU1753399A (en) 1999-05-31
AU749645B2 (en) 2002-06-27
CN1105198C (zh) 2003-04-09
KR100568958B1 (ko) 2006-04-07
AR010957A1 (es) 2000-07-12
ES2219925T3 (es) 2004-12-01
BR9813195A (pt) 2000-08-29
EG21972A (en) 2002-05-31
CA2308848A1 (en) 1999-05-20
KR20010031691A (ko) 2001-04-16

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