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EP0758413B2 - Composition de liant pour la fabrication de non-tisses - Google Patents
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EP0758413B2 - Composition de liant pour la fabrication de non-tisses - Google Patents

Composition de liant pour la fabrication de non-tisses Download PDF

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Publication number
EP0758413B2
EP0758413B2 EP95919367A EP95919367A EP0758413B2 EP 0758413 B2 EP0758413 B2 EP 0758413B2 EP 95919367 A EP95919367 A EP 95919367A EP 95919367 A EP95919367 A EP 95919367A EP 0758413 B2 EP0758413 B2 EP 0758413B2
Authority
EP
European Patent Office
Prior art keywords
powder
mixture
binder
powder coating
fibers
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
EP95919367A
Other languages
German (de)
English (en)
Other versions
EP0758413A1 (fr
EP0758413B1 (fr
Inventor
Stan Thyssen
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.)
Teodur NV
Original Assignee
Teodur NV
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
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Application filed by Teodur NV filed Critical Teodur NV
Publication of EP0758413A1 publication Critical patent/EP0758413A1/fr
Publication of EP0758413B1 publication Critical patent/EP0758413B1/fr
Application granted granted Critical
Publication of EP0758413B2 publication Critical patent/EP0758413B2/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/587—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
    • 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
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/60—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives the bonding agent being applied in dry state, e.g. thermo-activatable agents in solid or molten state, and heat being applied subsequently

Definitions

  • the invention relates to a special binder mixture for the production of nonwovens, as well Process for their production. Furthermore, the made from the nonwovens and binders Prepregs described.
  • molded parts are based on Nonwoven fabrics worth spreading. It is about Nonwovens made of various types of fiber with binders can be mixed. From these non-woven fabrics intermediate products can then be produced, the so-called Prepregs, which are then matched with the appropriate Processing tools shaped, cured and if necessary, assembled. It is the same possible directly from the fibers. and the binder powders to produce the corresponding Fa continuous non-woven goods.
  • These molded parts or planware are widely used Use. In the automotive industry these products for example as molded parts, e.g. as Insulation for hoods, wheel arches or trunk insulation used. Another area of application is the use as planware, e.g.
  • the methods of making non-woven fabrics or to mix these nonwovens with binder powder are known.
  • the fiber material e.g. B. in a fiber mixing chamber, homogenized, and on a conveyor belt laid as a loose fiber layer.
  • the binder mixture is then applied to the fiber material e.g. with metering rollers or vibrating troughs applied. Then the fiber / binder mixture in a closed system using a Air flow swirled and mixed homogeneously.
  • the homogeneous Mixture of fiber and binder powder filed into an endless fleece.
  • the components of this Mixtures can be done either by gentle heating and then cooling glued together be, whereby the prepregs arise or it is manufactured sheet or roll goods that are already complete is cured.
  • the prepregs are not yet finally cured, but are stable in storage. To processing into the final form, these will be Prepregs under the influence of heat at up to 210 ° C thermally cross-linked, whereby three-dimensional thermosetting Moldings are obtained.
  • Binders are relatively expensive. They are also phenolic resins hazardous to health. The industry is strong interested in reducing costs. Especially with the molded parts described above, such as the insulation materials for bonnets, wheel arches or insulation materials is looking for alternatives to the expensive, technical pure resins wanted.
  • JP-A-55-1 48266 describes a molded part Made of nonwoven fabric using synthetic Fibers, powder curl waste and resin made becomes.
  • the object of the present invention is a Binder mixture for the production of nonwoven molded parts to provide in which a significant Part of the commonly used pure resins can be replaced by other components that nevertheless to stable, reactive binder mixtures which leads to the production of nonwoven prepregs or cured nonwoven fabrics are suitable.
  • a Another task is to reduce the proportion of harmful Lower substances.
  • These binder mixtures must meet the usual requirements the manufacture of nonwoven molded parts and this results in hardened, stable molded parts, which adapted to the different applications can be.
  • Fibers are woven, matted or blended fibers.
  • the fibers consist of the known materials, e.g. natural, organic and inorganic fibers. Examples of this are glass fibers, Rock wool fibers, polyester fibers, acrylic resin fibers, Polyolefin fibers, wolf fibers, cotton fibers, Flax fibers or the like.
  • Textile fibers are preferred, especially cotton fibers, e.g. fiber waste from the textile industry.
  • These fibers or the nonwovens made from them are known in the industry.
  • the processes with which they are produced are also known can be. This can be done, for example, by Weaving or matting happen.
  • the emerging Nonwovens are said to be essentially dry, they can optionally be impregnated with additives.
  • phenolic resins are the usual reactive phenolic resins that have long been in the Industry are known.
  • these are reactive, Non-crosslinked, powdery, containing OH groups Phenolic resins.
  • Such resins are already used for the production of molded parts from nonwovens.
  • phenolic resins based of phenol and formaldehyde, as for example are known as resols or novolaks.
  • crosslinkers these resins can be condensation products of formaldehyde included.
  • the reactivity of the phenolic resins will also determined by the type and amount of the crosslinking agent used.
  • a crosslinking reaction generally occurs between 120 ° C and 222 ° C.
  • the resins are generally in powder form in front. Suitable grain sizes are between, for example 0.1 and 500 ⁇ m, preferably between 2 and 150 ⁇ m, particularly preferably between 10 and 60 ⁇ m.
  • the grain sizes of the powder coating waste used lie between 10 and 60 ⁇ m. Are powder coating waste used, their grain sizes too small for the desired application verbakken, it is possible to have larger grain sizes to get the particles.
  • the powder coating waste which can be used according to the invention are those of the usual known powder coatings based on epoxy resins, polyester resins Polyurethane resins or acrylic resins. This powder coating waste fall out as overspray, for example Paint booths or as batches during manufacturing the powder coatings. It is also possible that filter dust be collected and used, as well Residues from grinding the powder.
  • Powder coating waste is not yet networked. They contain reactive groups such as carboxyl groups, Epoxy groups, hydroxyl groups, amino groups, Amide groups or isocyanate derivatives. This can react with each other when heated.
  • the Crosslinking temperature depends on their basic structure from. They are usually between 120 and 220 ° C. Powder coatings with cross-linking temperatures above 180 ° C are preferably added only in small amounts, in order to cure even at curing temperatures Moldings of about 160 ° C as complete as possible Crosslinking of the binder mixture used to reach. In addition, at high crosslinking temperatures, especially when using nonwoven from plastic fibers there is a risk that the Fibers are broken down, leading to a decrease in stability of the molding leads. It is preferred that the Have paint powder / cross-linking temperatures below 160 ° C.
  • the epoxy powder coating materials which can be used according to the invention contain epoxy resins as the main binder component. These often crosslink via hydroxyl groups especially those containing amide or amine groups Harder.
  • Polyester powder coatings are used in which the main binder component are polyesters containing carboxyl groups.
  • the main binder component are polyesters containing carboxyl groups.
  • crosslinkers are, for example, epoxy groups Crosslinking agents or those containing amino or amide groups Known crosslinker. It is common. that each of the crosslinkers are more functional than that Main binder component.
  • Polyurethane powder coatings are based on those containing hydroxyl groups Polyesters that reversibly blocked Polyisocyanates, e.g. with known capping agents protected like caprolactam or ketoxime are able to cross-link or which are present as urethdione.
  • Powder coatings of the acrylate type are general Mixtures of two or more acrylic resins that functional groups such as epoxy groups, carboxyl groups, Hydroxyl groups or isocyanate groups contain. Here are the reacting with each other Groups divided into different molecules.
  • binder powders are e.g. in S.T. Harris, "The Technology of Powder Coatings", 1976 or in THERE. Bate, "The Science of Powder Coatings,” Vol I, 1990 described.
  • the powder coatings can be used individually. In order to achieve a composition of the binder mixture a) which is as constant as possible, it is preferred that a mixture of epoxy powders and polyester powder is present as a 2 ). Up to 60% by weight of a 2 ), preferably up to 30%, can optionally be replaced by polyurethane powder and / or polyacrylate powder. It is possible to directly produce a mixture a 2 ) within the desired weight ratios and to store it. Another possible way of working is that the various powder coating components are stored separately according to the chemical types described above and are only mixed with the phenolic resins before further processing. Within these chemical types, the resulting materials are mixed homogeneously, ie a sample is mixed with the composition and pigmentation in grain size distribution. The quantities required in each case are then mixed together from the mixtures of the resulting powder coating binders in the preparation of the binder powders a). If necessary, it is possible to introduce further additional crosslinkers into the binder mixture.
  • the powder coating waste which can be used according to the invention are available as ground powders. Possibly it is necessary to use proportions of the binder in coarser form are previously available on a suitable Grind grain size. This can be used for the phenolic resins specified order of magnitude.
  • customary additives or additives can be added together with the powders.
  • These can be, for example, catalysts, accelerators or flame retardants.
  • catalysts tin compounds are preferably used as dibutyltin dilaurate, carboxylic acid salts such as lithium benzoate, quaternary ammonium compounds such as tetrabutylammonium bromide, cetyltrimethylammonium bromide, benzyltrimethylammonium chloride, benzyltriethylammonium chloride or tetramethylammonium chloride or tertiary amines such as triisopropylamine or methylimidazole.
  • Suitable accelerators and crosslinkers are, for example, basic compounds containing epoxy groups, such as triglycidyl isocyanurates, glycolurils, dicyandiamide or beta-hydroxylamides. These additives can be added individually as powdery substances. They can also be introduced as a masterbatch mixed with binder proportions or they are metered in as a mixture with the binder powder a 1 ).
  • Flame retardant substances can also be introduced. These are the usual known substances that are contained in fire protection coatings. Examples of such compounds are borates such as sodium borate; Phosphates such as ammonium phosphate or sodium phosphate; Aluminum hydroxides or oxides; other suitable compounds are, for example, heavy metal-containing compounds such as tin oxide compounds or perbrominated or perchlorinated compounds such as tetrabromophenol. However, heavy metal-free and halogen-free flame retardant substances should preferably be used. These flame retardant substances are available as a powder. They can be introduced via a separate masterbatch or they are metered in via the binder powders a 1 ) or a 2 ) in each case as a homogeneous mixture with the powder component.
  • Pigments can also be introduced into the binder mixture a). In general, however, it is preferred not to introduce any additional pigments, but only to use the fibrous fillers of the nonwoven fabric or the pigments contained in the powder coatings a 2 ).
  • Another object of the present invention are molded parts by molding and partial or fully harden the above Mixture made of fibers and binders can be.
  • the mixtures are made of fibers and binders are only partially hardened, the so-called Get prepregs which are then in another Processing step by heating to its final Formed and fully cured can. If the mixture is to be fully cured, so they are in a known manner in the appropriate shape and in the form for each Binder mixture suitable crosslinking temperatures hardened.
  • the prepreg formed before curing or the finished molding generally contains 55 up to 80% by weight of fibers and 20 to 45% by weight of the binder mixture.
  • the binder mixture of 45 to 70 wt .-% phenolic resins and 30 to 55% by weight of powder coating binder.
  • the Additives and additives described above can in an amount of up to 20% by weight, preferably up to 15 % By weight may be included, the sum of the individual Components gives 100 wt .-%. Only one type of powder coating can be used or a mixture of several used are preferred, however, a mixture of polyester and epoxy resins. It is further preferred that the ratio of polyester powder to epoxy powder 0.2: 1 to 7: 1, preferably 0.8: 1 to 3: 1. It should however, be careful when choosing powder coating waste be that these are a sufficient number of own reactive groups.
  • the binder mixtures are homogenized in molded parts and together with any additives the nonwoven applied. This happens through known ones Method.
  • the mixture of binders becomes even distributed on the nonwoven fabric and after that, if necessary a heating step was carried out become.
  • the result is that the binder particles on soften the surface and become firmly attached to the nonwoven connect.
  • Prepregs the storage-stable, still deformable sheet-like Nonwovens result. It is important to ensure that there is no complete networking yet, but the Binder in the heat can be deformed even further as well as flow and network.
  • the binder mixture a), the prepregs and also the hardened moldings have a reduced proportion of free phenols or formaldehyde. This reduces the risk posed by these harmful substances.
  • the molded parts according to the invention can then be produced from the prepregs obtained in this way. This is done according to known methods such as shaping and / or laminating, making up the prepregs. After the prepregs have been brought into a suitable shape, they are crosslinked by applying pressure and heat. Crosslinking takes place at temperatures from 140 to 200 ° C. The time can be between 10 to 500 seconds, preferably less than 120 seconds. It is chosen depending on the phenolic resin a 1 ) used.
  • the binder powder melts and flows, whereby the fibers are at least partially embedded and the resins are chemically crosslinked. This creates a hardened thermoset material.
  • the moldings may contain parts of voids.
  • the density of the molded parts can be between 50 to 1000 kg / m 3 . It depends on the amount and type of fibers and binders.
  • the resulting molded parts have various advantages, such as good heat insulation, dimensional stability up to 130 ° C, good sound insulation, good flexural strength, are physiologically harmless and have a moisture-regulating effect, can be easily processed.
  • molded parts can still be coated or they serve as carriers for other components.
  • Molded parts have an attractive decorative effect.
  • smooth, soft, grained or even chemical resistant coated Surfaces are obtained.
  • flame retardant additives can also be obtained molded parts that are against fire are resistant.
  • the molded parts obtained in this way can be of various Industrial areas are used.
  • the binder mixtures can be used as resins can be used in linings for clutches.
  • these resins for mold making in the foundry industry be used.
  • the resulting molded parts are characterized by great stability and can shaped in a variety of ways. By the addition of various additives or by the Surface coating it is possible in different Application areas.
  • the mixture can be used without further loss of reactivity be stored for a long time.
  • Example 1 It becomes analogous to 70 g of a phenolic resin
  • the mixture has a long shelf life.
  • the powders of Examples 1 to 3 become with a nonwoven fabric produced in a known manner, that contains over 80% cotton fibers, prepregs manufactured.
  • the non-woven fabrics are through mechanical movement homogeneous with the binder powder mixed and passed through a heat channel (approx. 2 - 3 min., 80 ° C - 100 ° C). This creates storage-stable prepregs, in which resin and fiber are combined have connected.
  • the prepregs can be made differently according to size and resin / fiber content.
  • the bulk density is between 25 and 75 kg / m 3 depending on the application.
  • the prepregs are cut in one Press brought into the intended form and there 100 seconds to 110 seconds at temperatures between 140 ° C and 160 ° C hardened. After curing thermoset thermally stable Products. The density can vary over the amount of prepreg or influenced by the set pressure. The resulting cross-linked molded parts can be flocked in a known manner or they are laminated with foils.
  • the molded parts thus obtained have an optical homogeneous surface, they are dimensionally stable and have only a low content of free phenol or formaldehyde.

Landscapes

  • Textile Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Laminated Bodies (AREA)
  • Reinforced Plastic Materials (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Paints Or Removers (AREA)
  • Nonwoven Fabrics (AREA)
  • Ceramic Products (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Glass Compositions (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Processing Of Solid Wastes (AREA)

Claims (7)

  1. Mélange pour la fabrication de pièces moulées à partir de non-tissés, contenant
    a) 20 à 45 % en poids d'un mélange de liants sous forme de poudre, renfermant
    a1) 30 à 90 % en poids de résine phénolique et
    a2) 70 à 10 % en poids de résidus de vernis en poudre,
    b) 80 à 55 % en poids de fibres organiques et/ou inorganiques, caractérisé en ce que le composant a2) est constitué de résidus de vernis en poudre non encore réticulés à base de résines époxyde, de résines polyesters, de résines de polyuréthane et/ou de résines acrylates comportant des groupes réactifs, les grains des résidus de vernis en poudre ayant des dimensions entre 10 et 60 µm.
  2. Mélange selon la revendication 1, caractérisé en ce qu'il contient d'autres additifs et adjuvants.
  3. Mélange selon l'une des revendications 1 et 2, caractérisé en ce que l'on utilise comme résidus de vernis en poudre une résine époxyde et une résine polyester dans un rapport allant de 1:0,2 à 1:7.
  4. Mélange selon l'une des revendications 1 à 3, caractérisé en ce que l'on ajoute comme additif au moins un agent retardateur de flammes.
  5. Pièce moulée obtenue par démoulage et durcissement partiel ou total d'un mélange selon l'une des revendications 1 à 4.
  6. Utilisation des mélanges selon l'une des revendications 1 à 4 pour la fabrication de pièces moulées à partir de non-tissés.
  7. Utilisation des mélanges selon l'une des revendications 1 à 4 pour lier les nappes de fibres.
EP95919367A 1994-05-03 1995-04-29 Composition de liant pour la fabrication de non-tisses Expired - Lifetime EP0758413B2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4415470 1994-05-03
DE4415470 1994-05-03
PCT/EP1995/001643 WO1995030034A1 (fr) 1994-05-03 1995-04-29 Composition de liant pour la fabrication de non-tisses

Publications (3)

Publication Number Publication Date
EP0758413A1 EP0758413A1 (fr) 1997-02-19
EP0758413B1 EP0758413B1 (fr) 1999-04-14
EP0758413B2 true EP0758413B2 (fr) 2002-03-13

Family

ID=6517107

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95919367A Expired - Lifetime EP0758413B2 (fr) 1994-05-03 1995-04-29 Composition de liant pour la fabrication de non-tisses

Country Status (10)

Country Link
US (1) US5852102A (fr)
EP (1) EP0758413B2 (fr)
JP (1) JPH09512575A (fr)
AT (1) ATE178957T1 (fr)
AU (1) AU2523495A (fr)
CZ (1) CZ290886B6 (fr)
DE (1) DE59505660D1 (fr)
ES (1) ES2133770T5 (fr)
WO (1) WO1995030034A1 (fr)
ZA (1) ZA953558B (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4441765A1 (de) * 1994-11-24 1996-05-30 Teodur Nv Bindemittelzusammensetzung zur Herstellung von Faservliesen und Verfahren zur Herstellung von Faservlies-Formteilen
AU2002300833B2 (en) * 1997-08-04 2007-05-17 Boehringer Ingelheim Pharma Gmbh & Co. Kg Aqueous aerosol preparations containing biologically active macromolecules and method for producing the corresponding aerosols
KR100377270B1 (ko) * 2000-02-25 2003-03-26 노동욱 재생플라스틱 제조방법
DE10112620A1 (de) * 2001-03-14 2002-09-19 Bakelite Ag Bindemittelmischungen und ihre Verwendung
US8012889B2 (en) 2001-11-07 2011-09-06 Flexform Technologies, Llc Fire retardant panel composition and methods of making the same
US7906176B2 (en) * 2004-12-17 2011-03-15 Flexform Technologies, Llc Methods of manufacturing a fire retardant structural board
WO2008020768A1 (fr) * 2006-08-15 2008-02-21 Orica New Zealand Limited Matériau composite fabriqué à partir d'un système liant comprenant de la poudre de revêtement de poudre de déchet
DE102009001806A1 (de) * 2009-03-24 2010-09-30 Evonik Degussa Gmbh Prepregs und daraus bei niedriger Temperatur hergestellte Formkörper
DE102009001793A1 (de) * 2009-03-24 2010-10-07 Evonik Degussa Gmbh Prepregs und daraus hergestellte Formkörper
WO2025184697A1 (fr) * 2024-03-05 2025-09-12 Scott Bradley Allen John Matériau polymère certifié écologique et procédé de fabrication

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55148266A (en) * 1979-05-04 1980-11-18 Nippon Tokushu Toryo Co Ltd Bulky nonwoven fabric and method
DE3833656A1 (de) * 1988-10-04 1990-04-12 Hoechst Ag Modifizierte novolake
EP0363539A1 (fr) * 1988-10-14 1990-04-18 MITSUI TOATSU CHEMICALS, Inc. Composition de résine thermodurcissable pour moulage par injection
US4939188A (en) * 1988-12-22 1990-07-03 Borden, Inc. Lithium-containing resole composition for making a shaped refractory article and other hardened articles
WO1995021213A1 (fr) * 1994-02-02 1995-08-10 Seydel Companies, Inc. Compositions d'adhesifs produites avec des polymeres de phtalate et procede de preparation associe

Also Published As

Publication number Publication date
DE59505660D1 (de) 1999-05-20
ZA953558B (en) 1996-01-11
EP0758413A1 (fr) 1997-02-19
CZ290886B6 (cs) 2002-11-13
CZ319496A3 (en) 1997-03-12
EP0758413B1 (fr) 1999-04-14
ATE178957T1 (de) 1999-04-15
US5852102A (en) 1998-12-22
ES2133770T3 (es) 1999-09-16
AU2523495A (en) 1995-11-29
WO1995030034A1 (fr) 1995-11-09
ES2133770T5 (es) 2002-11-01
JPH09512575A (ja) 1997-12-16

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