EP0960251B1 - Fire-resistant opening seal - Google Patents

Fire-resistant opening seal Download PDF

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Publication number
EP0960251B1
EP0960251B1 EP98908030A EP98908030A EP0960251B1 EP 0960251 B1 EP0960251 B1 EP 0960251B1 EP 98908030 A EP98908030 A EP 98908030A EP 98908030 A EP98908030 A EP 98908030A EP 0960251 B1 EP0960251 B1 EP 0960251B1
Authority
EP
European Patent Office
Prior art keywords
closure
heat
fire
composite block
expanding
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
EP98908030A
Other languages
German (de)
French (fr)
Other versions
EP0960251A1 (en
Inventor
Robert Graf
Maria-Elisabeth Kaiser
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.)
Cognis IP Management GmbH
Original Assignee
Cognis Deutschland GmbH and Co KG
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Publication date
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Publication of EP0960251A1 publication Critical patent/EP0960251A1/en
Application granted granted Critical
Publication of EP0960251B1 publication Critical patent/EP0960251B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62C—FIRE-FIGHTING
    • A62C3/00—Fire prevention, containment or extinguishing specially adapted for particular objects or places
    • A62C3/16—Fire prevention, containment or extinguishing specially adapted for particular objects or places in electrical installations, e.g. cableways
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/913—Material designed to be responsive to temperature, light, moisture
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/92—Fire or heat protection feature
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/92—Fire or heat protection feature
    • Y10S428/921—Fire or flameproofing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/696—Including strand or fiber material which is stated to have specific attributes [e.g., heat or fire resistance, chemical or solvent resistance, high absorption for aqueous compositions, water solubility, heat shrinkability, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/699—Including particulate material other than strand or fiber material

Definitions

  • the invention relates to a fire-resistant, elastic opening closure in the form of a preformed composite body.
  • DE 35 42 326 C1 describes a flame-retardant composite foam made of polyurethane foam flakes described. This is made by placing the foam flakes in the In the event of fire, inflatable intumescent materials are mixed as a binder and / or additive and then be pressed. Intumescent materials in the form of expanded graphite and as binders can be used as additives can be intumescent materials in the form of an epoxy resin with a melamine hydrohalide Binders can be used. The composite foam obtained in this way is suitable as a composite foam panel for laying on surfaces to be protected.
  • EP-A-0706979 describes a fire-resistant, elastic opening closure in Form of a preformed composite body made of elastically compressible particles, one at A blowing agent that becomes effective when exposed to heat Binder and an adhesive through which the individual components to a composite body are connected.
  • the opening closure according to the invention can be produced in a simple manner and largely or entirely using recycled materials.
  • the opening closure according to the invention has excellent mechanical properties, especially what a strength, abrasion resistance and Elasticity concerns.
  • the opening closure according to the invention has excellent fire engineering Characteristics. It can easily be formulated so that its fire resistance is above F90 according to DIN 4102. His fire resistance is therefore the same as the fire resistance of Concrete components, which is particularly advantageous.
  • the blowing agent which becomes effective when the heat develops, leads to a fire Volume increase and ensures a particularly tight seal of the opening. Furthermore, additional cavities are created, which provide thermal insulation enlarge.
  • the at least one heat-binding binder becomes sticky under the influence of heat and ensures that the individual Keep components of the composite body together in the event of fire and not crumble. At least two at different temperatures are advantageous rising heat-binding agents provided.
  • As a heat-effective Binders are particularly suitable for organic thermoplastics, which are used in lower Melting temperatures, inorganic hot melt adhesives such as borates, Ammonium polyphosphate, which softens over a wide temperature range and at the same time has flame retardant properties, as well as glass, its Adhesive properties developed at higher temperatures.
  • the glass is lying in particular to avoid segregation of the raw materials, preferably in finely divided form, in particular in the form of fibers, hollow microspheres or glass powder, in front.
  • At least two are used as blowing agents different blowing agents are provided. This too can control the blowing properties over a wide temperature range become. Expandable graphite and, if one, are particularly suitable as blowing agents Bloating is desirable even at high temperatures, even uninflated Vermiculite and / or pearlite.
  • the individual components can be in finely divided Pre-mixed form, after which the mixture is provided with the adhesive, preferably by spraying it onto the moving mixture.
  • the one with the Glue wetted mixture is then preferably under the action of heat pressed into a block, the heat in particular using a Burst of steam can be introduced evenly into the mixture.
  • this is at least one Blowing agent and the at least one heat-binding binder in the form of both Granules containing ingredients. This will make it a very even one
  • the composite bodies composed of 10 - 50% by weight, in particular approx. 40% by weight of elastic compressible particles, 20 - 70 wt%, in particular 40 - 60 wt% from the Combination of thermally active blowing agents and thermally active binders and 0.5-20% by weight, in particular approximately 10% by weight of adhesive.
  • the combination of thermally active blowing agents and thermally active binders split in the Usually in 40 - 80% by weight, in particular 30 - 50% blowing agent, in particular blowing agent mixture, and 60 - 20% by weight, in particular Binder mixture.
  • the adhesive holding the components of the composite body together is one preferred embodiment, a diisocyanate, in particular Diphenylmethane diisocyanate, which is preferably set with water.
  • a diisocyanate in particular Diphenylmethane diisocyanate
  • water preferably set with water.
  • a thermoplastic especially an in aqueous medium, for example as a dispersion, applicable thermoplastic. This can also serve as a heat-binding agent.
  • Thermoplastics are polyvinyl acetate / ethylene copolymers and Polyvinyl acetate / ethylene / vinyl chloride terpolymers.
  • the opening closure according to the invention is preferably porous and has especially a rough surface. This makes it particularly good on the one hand compressible. On the other hand, the rough surface gives good adhesion in the openings to be closed.
  • the elastically compressible particles can be essentially solid, such as Pieces of rubber or cork. However, they are preferably porous. This is the case with one preferred embodiment of the composite body, a composite foam body, and the elastically compressible particles are foam particles. As compressible Particles are also suitable for fiber balls. Also fibers and others can compressible particles are present in combination with one another.
  • compressible particles are open-pored, such as this is the case with fiber balls and open-cell foam particles.
  • open-pore particles can smaller components of the mixture in the Partially penetrate pores, which further promotes homogeneity.
  • the Particle size of the individual components can vary within wide limits.
  • the compressible particles it is usually between 1 and 20 mm, especially 1 and 5 mm.
  • the remaining ingredients can be in the form of powders or particles with a particle size of 0.001-10 mm, preferably 0.1-5 mm, in particular 0.3 - 5 mm, are present.
  • the opening closures according to the invention are preferably made from larger blocks. From these can plates be cut to a suitable thickness. This is easily possible because the Material of the composite body is easily cut, for example with knives, scissors or hot wires. Punching is also possible. As a result, without special shapes must be kept in stock, any sizes and Designs are made on opening closures. The resulting waste can be easily recycled by starting from scratch Composite body is used as an elastically compressible particle. This one Particles can then already contain the heat-effective binders and blowing agents the amount of which will be withdrawn accordingly. It is an advantage too possible openings and recesses for the opening closures Prepare to pass through lines, for example by partially Punching.
  • the opening closures contain 800-400, in particular 750-600
  • the modulus of elasticity of the opening closures is generally 1 ⁇ 10 3 to 1 ⁇ 10 5 N / m 2 , preferably 4 to 10 ⁇ 10 3 N / m 2 , in particular approx. 7 ⁇ 10 3 N / m 2 .
  • the opening closures advantageously have a compression hardness (at 40% compression) of 1 ⁇ 10 2 to 7 ⁇ 10 3 N / mm 2 , preferably 1.3 to 5 ⁇ 10 2 N / mm 2 , in particular approx. 1.7 ⁇ 10 2 N / mm 2 .
  • the Shore A hardness of the opening closures is preferably in the range of 10-40, preferably 12 to 20, in particular approximately 15. These mechanical properties can be varied in a suitable manner by controlling the production conditions.
  • a dry mixture is made from the following ingredients: 45 parts by weight Schnitzel made of flexible polyurethane foam with different particle sizes in the range of 1 - 7 mm 10 parts by weight Zinc borate as an inorganic hot melt adhesive 12.5 parts by weight Hollow glass microspheres 9.5 parts by weight Ammonium polyphosphate and 13 parts by weight Expandable graphite.
  • the composite body obtained had a Shore A hardness of 15, a modulus of elasticity of 6 ⁇ 10 3 N / m 2 and a compression hardness (40%) of 2 ⁇ 10 2 N / mm 2 .
  • the cut surfaces were porous and not sticky. They had an even one black-gray color, whereby individual expandable graphite particles were recognizable.
  • the composite body was cut plates, from which in turn the desired forms of opening closures (cylinders, cuboids and the like) were punched out. For the formation of cable bushings were different large holes are pre-punched so that the respective hole cores at the construction site without Tool could be pushed out by hand.
  • the opening closures could be bent without risk of breakage and be squeezed together. They are so firm that they hammer into openings hammered in and out of the openings without risk of breakage or tearing could be pulled out.
  • Cylindrical parts with a thickness of 6 cm can be cut from the composite bodies become. These cylinders are suitable for sealing off holes in components, through which electrical cables are led. Will two of these cylinders become one Hole in a 120 mm thick concrete wall, through which electrical cables of up to 20 mm in diameter can be performed with this Fire resistance of more than 120 minutes according to DIN 3102, part 9.
  • Example 1 was repeated, first of all producing a granulate containing blowing agent and heat-effective binder.
  • the cake obtained is granulated into granules with a particle size of 1-3 mm.
  • a dry mixture is produced from 45% by weight of a swelling agent granulate according to DE 39 30 722 A1, which already contains heat-binding agent, and 50% by weight of a rubber foam ground to a size of 1-3 mm.
  • This mixture is sprayed with 5% by weight of diphenylmethane diisocyanate, which is diluted 1: 1 with water.
  • This intermediate product is heated in a heated press mold with several bursts of steam to approx. 170 ° C., whereby it solidifies into a composite body with a density of 380 kg / m 3 .
  • the composite body has a modulus of elasticity of 2 ⁇ 10 4 N / m 2 and a compression hardness (40%) of 2.5 ⁇ 10 2 N / mm 2.
  • the cross-section of trapezoidal bodies is cut from the composite body. which can be used to seal the trapezoidal sheet metal beads above walls inside buildings.
  • the composite bodies with a thickness of 120 mm have a fire resistance duration of more than 2 hours.

Landscapes

  • Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Business, Economics & Management (AREA)
  • Emergency Management (AREA)
  • Sealing Material Composition (AREA)
  • Building Environments (AREA)
  • Control Of Combustion (AREA)
  • Fire-Detection Mechanisms (AREA)
  • Insulated Conductors (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Laminated Bodies (AREA)

Abstract

A fire-resistant composite substrate for use in making structural openings fire-resistant, the substrate containing: (a) elastically compressible particles; (b) at least one heat-activated expanding agent; (c) at least one heat-activated binder; and (d) a diisocyanate adhesive.

Description

Die Erfindung betrifft einen feuerwiderstandsfähigen, elastischen Öffnungsverschluß in Form eines vorgeformten Verbundkörpers.The invention relates to a fire-resistant, elastic opening closure in the form of a preformed composite body.

In brandschutztechnisch klassifizierten Bauteilen (Wände, Decken) sind Öffnungen nicht zulässig, da sich im Falle eines Brandes Feuer und Rauch durch die Öffnungen hindurch in die angrenzenden Räume ausbreiten kann. Insbesondere dann, wenn durch diese Öffnungen Leitungen (Kabel, Rohre) hindurchgeführt werden, sind an den Werkstoff, der zum Verschluß der Restöffnung verwendet werden soll, besondere Anforderungen zu richten. Für die Abschottung solcher Öffnungen sind bisher bekannt:

  • Mineralfaserplatten oder lose Mineralfaser in Kombination mit Brandschutzbeschichtungen und Kitten,
  • Mörtelprodukte,
  • Brandschutzkissen sowie
  • Polyurethan-Schaumkörper.
    • Openings are not permitted in components classified as fire protection (walls, ceilings), since in the event of a fire, fire and smoke can spread through the openings into the adjacent rooms. In particular, if lines (cables, pipes) are passed through these openings, special requirements must be made of the material to be used to close the remaining opening. For the sealing off of such openings are known so far:
  • Mineral fiber boards or loose mineral fibers in combination with fire protection coatings and putty,
  • Mortar products,
  • Fire protection pillow as well
  • Polyurethane foam body.

    • Diese Produkte haben zum Teil sehr gute Eigenschaften. Angestrebt wird jedoch die Kombination einer einfachen Herstellung und Verarbeitung, verbunden mit geringen Materialkosten, mit einem hohen Feuerwiderstand und der Möglichkeit eines raschen Ein- und Ausbauens.Some of these products have very good properties. However, the aim is Combination of simple manufacture and processing combined with low Material costs, with a high fire resistance and the possibility of a quick Installation and expansion.

    Aus dem deutschen Gebrauchsmuster G 87 16 908.6 ist ein feuer- und rauchdichter Verschluß für Wanddurchbrüche bekannt. Dieser Verschluß wird in Form eines konischen Stopfens hergestellt, indem ein feinporiger Zweikomponenten-Schaumstoff in einer geeigneten Rohform aufgeschäumt wird. In der Praxis hat sich gezeigt, daß derartige konische Stopfen in der Handhabung schwierig sind, was durch die klebrige Außenhaut verstärkt wird. Außerdem müssen zahlreiche Hohlformen vorgehalten werden, um verschieden große Stopfen zu erhalten.From the German utility model G 87 16 908.6 is a fire and smoke proof Closure known for wall openings. This closure is in the form of a conical stopper made by a fine-pored two-component foam is foamed in a suitable raw form. In practice it has shown that such conical plugs are difficult to handle, which is reinforced by the sticky outer skin. In addition, numerous hollow molds must be kept to get different sized plugs.

    In der DE 35 42 326 C1 ist ein schwer entflammbarer Verbundschaum aus Polyurethan-Schaumstoffflocken beschrieben. Dieser wird dadurch hergestellt, dass die Schaumstoffflocken mit im Brandfall aufblähbaren Intumeszenzmassen als Binder und/oder Zuschlagstoff vermischt und dann verpresst werden. Als Zuschlagstoff können Intumeszenzmassen in Form von Blähgraphit und als Binder können Intumeszenzmassen in Form eines Epoxidharzes mit einem Melamin-Hydrohalogenid als Bindemittel verwendet werden. Der so gewonnene Verbundschaum eignet sich als Verbundschaumplatte zum Auflegen auf zu schützende Flächen.DE 35 42 326 C1 describes a flame-retardant composite foam made of polyurethane foam flakes described. This is made by placing the foam flakes in the In the event of fire, inflatable intumescent materials are mixed as a binder and / or additive and then be pressed. Intumescent materials in the form of expanded graphite and as binders can be used as additives can be intumescent materials in the form of an epoxy resin with a melamine hydrohalide Binders can be used. The composite foam obtained in this way is suitable as a composite foam panel for laying on surfaces to be protected.

    EP-A-0706979 beschreibt beschreibt einen feuerwiderstandsfähigen, elastischen Öffnungsverschluss in Form eines vorgeformten Verbundkörpers aus elastisch komprimierbaren Partikeln, einem bei Hitzeeinwirkung wirksam werdenden Blähmittel, einem bei Hitzeeinwirkung wirksam werdenden Bindemittel und einem Klebstoff, durch den die einzelnen Bestandteile zu einem Verbundkörper verbunden sind. EP-A-0706979 describes a fire-resistant, elastic opening closure in Form of a preformed composite body made of elastically compressible particles, one at A blowing agent that becomes effective when exposed to heat Binder and an adhesive through which the individual components to a composite body are connected.

    Gegenstand der Erfindung ist ein feuerwiderstandsfähiger, elastischer Öffnungsverschluss in Form eines vorgeformten Verbundkörpers aus

  • a) mindestens einer Art von elastisch komprimierbaren Parikeln,
  • b) mindestens einem bei Hitzeentwicklung wirksam werdenden Blähmittel,
  • c) mindestens einem bei Hitzeentwicklung wärmewirksamen Bindemittel und
  • d) mindestens einem Klebstoff, durch den die elastisch komprimierbaren Partikel und die anderen Bestandteile zu dem Verbundkörper verbunden sind, wobei die Klebstoffe d) ausgewählt werden aus der Gruppe der Diisocyanate.
    • The invention relates to a fire-resistant, elastic opening closure in the form of a preformed composite body
  • a) at least one type of elastically compressible particle,
  • b) at least one blowing agent which becomes effective when heat is generated,
  • c) at least one binder which is thermally effective in the event of heat and
  • d) at least one adhesive through which the elastically compressible particles and the other constituents are connected to form the composite body, the adhesives d) being selected from the group of the diisocyanates.

    • Der erfindungsgemäße Öffnungsverschluß läßt sich in einfacher Weise herstellen und zwar weitgehend oder vollständig unter Verwendung von Recyclingmaterial. Der erfindungsgemäße Öffnungsverschluß hat hervorragende mechanische Eigenschaften, insbesondere was eine Festigkeit, Abriebbeständigkeit und Elastizität betrifft. Der erfindungsgemäße Öffnungsverschluss hat hervorragende brandtechnische Eigenschaften. Er kann ohne Schwierigkeiten so formuliert werden, dass sein Feuerwiderstand über F90 nach DIN 4102 liegt. Damit liegt sein Feuerwiderstand in der Größe des Feuerwiderstandes von Betonbauteilen, was besonders vorteilhaft ist. The opening closure according to the invention can be produced in a simple manner and largely or entirely using recycled materials. The opening closure according to the invention has excellent mechanical properties, especially what a strength, abrasion resistance and Elasticity concerns. The opening closure according to the invention has excellent fire engineering Characteristics. It can easily be formulated so that its fire resistance is above F90 according to DIN 4102. His fire resistance is therefore the same as the fire resistance of Concrete components, which is particularly advantageous.

    Das bei Hitzeentwicklung wirksam werdende Blähmittel führt im Brandfalle zu einer Volumenvergrößerung und sorgt für einen besonders dichten Abschluß der Öffnung. Ferner werden zusätzliche Hohlräume geschaffen, die die Wärmeisolation vergrößern. Das mindestens ein bei Hitzeentwicklung wärmewirksames Bindemittel wird unter Einwirkung von Hitze klebrig und sorgt dafür, daß die einzelnen Bestandteile des Verbundkörpers im Brandfalle zusammenhalten und nicht zerbröseln. Von Vorteil sind mindestens zwei bei verschiedenen Temperaturen anspringende wärmewirksame Bindemittel vorgesehen. Als wärmewirksame Bindemittel eigenen sich insbesondere organische Thermoplaste, die bei niederen Temperaturen schmelzen, anorganische Schmelzkleber, wie Borate, Ammoniumpolyphosphat, das über einen weiten Temperaturbereich erweicht und gleichzeitig flammhemmende Eigenschaften besitzt, sowie Glas, das seine Klebeeigenschaften bei höheren Temperaturen entwickelt. Das Glas liegt insbesondere zur Vermeidung einer Entmischung der Rohstoffe vorzugsweise in feinteiliger Form, insbesondere in Form von Fasern, Mikrohohlkugeln oder Glasmehl, vor.The blowing agent, which becomes effective when the heat develops, leads to a fire Volume increase and ensures a particularly tight seal of the opening. Furthermore, additional cavities are created, which provide thermal insulation enlarge. The at least one heat-binding binder becomes sticky under the influence of heat and ensures that the individual Keep components of the composite body together in the event of fire and not crumble. At least two at different temperatures are advantageous rising heat-binding agents provided. As a heat-effective Binders are particularly suitable for organic thermoplastics, which are used in lower Melting temperatures, inorganic hot melt adhesives such as borates, Ammonium polyphosphate, which softens over a wide temperature range and at the same time has flame retardant properties, as well as glass, its Adhesive properties developed at higher temperatures. The glass is lying in particular to avoid segregation of the raw materials, preferably in finely divided form, in particular in the form of fibers, hollow microspheres or glass powder, in front.

    Bei einer bevorzugten Ausführungsform sind als Blähmittel mindestens zwei bei verschiedenen Temperaturen aufblähende Blähmittel vorgesehen. Auch hierdurch können die Bläheigenschaften über einen weiten Temperaturbereich gesteuert werden. Als Blähmittel eignet sich insbesondere Blähgraphit und, wenn eine Aufblähung auch bei hohen Temperaturen erwünscht ist, auch ungeblähter Vermiculit und/oder Perlit.In a preferred embodiment, at least two are used as blowing agents different blowing agents are provided. This too can control the blowing properties over a wide temperature range become. Expandable graphite and, if one, are particularly suitable as blowing agents Bloating is desirable even at high temperatures, even uninflated Vermiculite and / or pearlite.

    Zur Herstellung des Verbundkörpers können die einzelnen Bestandteile in feinteiliger Form vorgemischt werden, wonach die Mischung mit dem Kleber versehen wird, vorzugsweise indem dieser auf die bewegte Mischung aufgesprüht wird. Die mit dem Kleber benetzte Mischung wird daraufhin vorzugsweise unter Einwirkung von Wärme zu einem Block verpreßt, wobei die Wärme insbesondere mit Hilfe eines Dampfstoßes gleichmäßig in die Mischung eingebracht werden kann.To produce the composite body, the individual components can be in finely divided Pre-mixed form, after which the mixture is provided with the adhesive, preferably by spraying it onto the moving mixture. The one with the Glue wetted mixture is then preferably under the action of heat pressed into a block, the heat in particular using a Burst of steam can be introduced evenly into the mixture.

    Bei einer bevorzugten Ausführungsform der Erfindung liegt das mindestens eine Blähmittel und das mindestens eine wärmewirksame Bindemittel in Form eines beide Bestandteile enthaltenden Granulats vor. Dadurch wird eine sehr gleichmäßige In a preferred embodiment of the invention, this is at least one Blowing agent and the at least one heat-binding binder in the form of both Granules containing ingredients. This will make it a very even one

    Verteilung der Bestandteile im Öffnungsverschluß erhalten, wodurch sich sehr gleichmäßige mechanische und brandtechnische Eigenschaften ergeben. Besonders geeignete Granulate dieser Art sind in der DE 39 30 722 A1 als Quellmittelzusammensetzung beschrieben. Auf den Inhalt dieser Druckschrift wird hier ausdrücklich Bezug genommen. In der Regel sind die Verbundkörper zusammengesetzt aus 10 - 50 Gew%, insbesondere ca. 40 Gew% an elastisch komprimierbaren Partikeln, 20 - 70 Gew%, insbesondere 40 - 60 Gew% aus der Kombination von wärmewirksamen Blähmitteln und wärmewirksamen Bindemittel sowie 0,5 - 20 Gew%, insbesondere ca. 10 Gew% Kleber. Die Kombination aus wärmewirksamen Blähmittel und wärmewirksamen Bindemittel spaltet sich in der Regel auf in 40 - 80 Gew%, insbesondere 30 - 50 % Blähmittel, insbesondere Blähmittelmischung, und 60 - 20 Gew%, insbesondere Bindemittelmischung.Distribution of the components in the opening lock obtained, which is very result in uniform mechanical and fire properties. Especially Suitable granules of this type are described in DE 39 30 722 A1 Described swelling agent composition. On the content of this publication expressly referred to here. As a rule, the composite bodies composed of 10 - 50% by weight, in particular approx. 40% by weight of elastic compressible particles, 20 - 70 wt%, in particular 40 - 60 wt% from the Combination of thermally active blowing agents and thermally active binders and 0.5-20% by weight, in particular approximately 10% by weight of adhesive. The combination of thermally active blowing agents and thermally active binders split in the Usually in 40 - 80% by weight, in particular 30 - 50% blowing agent, in particular blowing agent mixture, and 60 - 20% by weight, in particular Binder mixture.

    Der die Bestandteile des Verbundkörpers zusammenhaltende Klebstoff ist bei einer bevorzugten Ausführungsform ein Diisocynat, insbesondere Diphenylmethandiisocynat, das vorzugsweise mit Wasser abgebunden ist. Zum Abbinden kann das Wasser des Dampfstoßes oder das wässrige Medium, mit dem der Kleber zudosiert wird, verwendet werden. Bei einer anderen, ebenfalls bevorzugten Ausführungsform der Erfindung ist der die Bestandteile des Verbundkörpers zusammenhaltende Klebstoff ein Thermoplast, insbesondere ein in wässrigem Medium, zum Beispiel als Dispersion, aufbringbarer Thermoplast. Dieser kann gleichzeitig als wärmewirksames Bindemittel dienen. Beispiele für solche Thermoplaste sind Polyvinylacetat/Ethylen-Copolymere und Polyvinylacetet/Ethylen/Vinylchlorid-Terpolymere.The adhesive holding the components of the composite body together is one preferred embodiment, a diisocyanate, in particular Diphenylmethane diisocyanate, which is preferably set with water. To the The water from the steam jet or the aqueous medium with which the adhesive is added, can be used. Another, too preferred embodiment of the invention is the components of the Composite body-holding adhesive a thermoplastic, especially an in aqueous medium, for example as a dispersion, applicable thermoplastic. This can also serve as a heat-binding agent. Examples of such Thermoplastics are polyvinyl acetate / ethylene copolymers and Polyvinyl acetate / ethylene / vinyl chloride terpolymers.

    Der erfindungsgemäße Öffnungsverschluß ist vorzugsweise porös und weist insbesondere eine rauhe Oberfläche auf. Dadurch ist er einerseits besonders gut komprimierbar. Auf der anderen Seite bringt die rauhe Oberfläche eine gute Haftung in den zu verschließenden Öffnungen.The opening closure according to the invention is preferably porous and has especially a rough surface. This makes it particularly good on the one hand compressible. On the other hand, the rough surface gives good adhesion in the openings to be closed.

    Interessanterweise hat sich herausgestellt, daß der erfindungsgemäße Öffnungsverschluß trotz seiner heterogenen Zusammensetzung die Eigenschaften eines homogenen Körpers besitzt. Dies ist zum Teil dadurch bedingt, daß die Teilchengröße der einzelnen Bestandteile, insbesondere der elastisch verformbaren Partikel, verschieden ist, wodurch eine gleichmäßige und dichte Packung ermöglicht ist. Die elastisch komprimierbaren Partikel können im wesentlichen massiv sein, wie Gummistücke oder Korkstücke. Sie sind jedoch vorzugsweise porös. So ist bei einer bevorzugten Ausführungsform der Verbundkörper ein Verbundschaumkörper, und die elastisch komprimierbaren Partikel sind Schaumstoffpartikel. Als komprimierbare Partikel eigenen sich auch Faserknäuel. Auch können Fasern und andere komprimierbare Partikel in Kombination miteinander vorliegen. Die elastisch komprimierbaren Partikel sind bei bevorzugten Ausführungsformen offenporig, wie dies bei Faserknäueln und offenporigen Schaumstoffpartikeln der Fall ist. Bei solchen offenporigen Partikeln können kleinere Bestandteile der Mischung in die Poren teilweise eindringen, wodurch die Homogenität weiter gefördert wird. Die Teilchengröße der einzelnen Bestandteile kann innerhalb weiter Grenzen variieren. Bei den komprimierbaren Partikeln liegt sie in der Regel zwischen 1 und 20 mm, insbesondere 1 und 5 mm. Die übrigen Bestandteile können in Form von Pulvern oder Partikeln mit einer Teilchengröße von 0,001 - 10 mm, vorzugsweise 0,1 - 5 mm, insbesondere 0,3 - 5 mm, vorliegen.Interestingly, it has been found that the invention Opening closure despite its heterogeneous composition the properties of a homogeneous body. This is partly due to the fact that Particle size of the individual components, especially the elastically deformable Particle, is different, which enables an even and dense packing is. The elastically compressible particles can be essentially solid, such as Pieces of rubber or cork. However, they are preferably porous. This is the case with one preferred embodiment of the composite body, a composite foam body, and the elastically compressible particles are foam particles. As compressible Particles are also suitable for fiber balls. Also fibers and others can compressible particles are present in combination with one another. The elastic In preferred embodiments, compressible particles are open-pored, such as this is the case with fiber balls and open-cell foam particles. at Such open-pore particles can smaller components of the mixture in the Partially penetrate pores, which further promotes homogeneity. The Particle size of the individual components can vary within wide limits. For the compressible particles, it is usually between 1 and 20 mm, especially 1 and 5 mm. The remaining ingredients can be in the form of powders or particles with a particle size of 0.001-10 mm, preferably 0.1-5 mm, in particular 0.3 - 5 mm, are present.

    Die erfindungsgemäßen Öffnungsverschlüsse sind, wie oben bereits erwähnt, vorzugsweise aus größeren Blöcken hergestellt. Aus diesen können Platten geeigneter Dicke geschnitten werden. Dies ist in einfacher Weise möglich, da das Material der Verbundkörper leicht schneidbar ist, zum Beispiel mit Messern, Scheren oder Heißdrähten. Auch ein Ausstanzen ist möglich. Dadurch können, ohne daß besondere Formen vorrätig gehalten werden müssen, beliebige Größen und Gestalten an Öffnungsverschlüssen hergestellt werden. Dabei anfallender Verschnitt kann in einfacher Weise recycelt werden, indem er bei der Produktion von neuem Verbundkörper als elastisch komprimierbare Partikel verwendet wird. Da diese Partikel dann schon die wärmewirksamen Bindemittel und Blähmittel enthalten, kann deren Menge entsprechend zurückgenommen werden. Es ist mit Vorteil auch möglich, in den Öffnungsverschlüssen Durchbrechungen und Ausnehmungen für die Hindurchführung von Leitungen vorzubereiten, zum Beispiel durch teilweises Stanzen. As already mentioned above, the opening closures according to the invention are preferably made from larger blocks. From these can plates be cut to a suitable thickness. This is easily possible because the Material of the composite body is easily cut, for example with knives, scissors or hot wires. Punching is also possible. As a result, without special shapes must be kept in stock, any sizes and Designs are made on opening closures. The resulting waste can be easily recycled by starting from scratch Composite body is used as an elastically compressible particle. This one Particles can then already contain the heat-effective binders and blowing agents the amount of which will be withdrawn accordingly. It is an advantage too possible openings and recesses for the opening closures Prepare to pass through lines, for example by partially Punching.

    Da die Dichte der Ausgangsmaterialien in der Regel bei ca. 1 liegt, enthalten die Öffnungsverschlüsse entsprechend 800 - 400, insbesondere 750 - 600 | Gas/m3. Der Elastizitätsmodul der Öffnungsverschlüsse liegt in der Regel bei 1 · 103 bis 1 · 105 N/m2, vorzugsweise bei 4 bis 10 · 103 N/m2, insbesondere bei ca. 7 · 103 N/m2. Die Öffnungsverschlüsse besitzen vorteilhafterweise eine Stauchhärte (bei 40 % Stauchung) von 1 · 102 bis 7 · 103 N/mm2, vorzugsweise 1,3 bis 5 · 102 N/mm2, insbesondere ca. 1,7 · 102 N/mm2. Die Shore-A-Härte der Öffnungsverschlüsse liegt bevorzugt im Bereich von 10 - 40, vorzugsweise 12 bis 20, insbesondere ca. 15. Diese mechanischen Eigenschaften lassen sich durch Steuerung der Herstellungsbedingungen in geeigneter Weise variieren.Since the density of the starting materials is usually around 1, the opening closures contain 800-400, in particular 750-600 | Gas / m 3 . The modulus of elasticity of the opening closures is generally 1 · 10 3 to 1 · 10 5 N / m 2 , preferably 4 to 10 · 10 3 N / m 2 , in particular approx. 7 · 10 3 N / m 2 . The opening closures advantageously have a compression hardness (at 40% compression) of 1 · 10 2 to 7 · 10 3 N / mm 2 , preferably 1.3 to 5 · 10 2 N / mm 2 , in particular approx. 1.7 · 10 2 N / mm 2 . The Shore A hardness of the opening closures is preferably in the range of 10-40, preferably 12 to 20, in particular approximately 15. These mechanical properties can be varied in a suitable manner by controlling the production conditions.

    Weitere Merkmale und Vorteile der Erfindung ergeben sich aus der nachfolgenden Beschreibung von Beispielen in Verbindung mit den Unteransprüchen. Hierbei können die einzelnen Merkmale jeweils für sich und zu mehreren Kombinationen miteinander bei einer Ausführungsform der Erfindung verwirklicht sein.Further features and advantages of the invention result from the following Description of examples in connection with the subclaims. in this connection the individual characteristics can be used individually and in several combinations be realized with one another in one embodiment of the invention.

    Beispiel 1example 1

    Es wird eine trockene Mischung hergestellt aus folgenden Bestandteilen: 45 Gewichtsteilen Schnitzel aus Polyurethan-Weichschaum mit unterschiedlicher Teilchengröße im Bereich von 1 - 7 mm 10 Gewichtsteilen Zinkborat als anorganischer Schmelzkleber 12,5 Gewichtsteilen Glasmikrohohlkugeln 9,5 Gewichtsteilen Ammoniumpolyphosphat und 13 Gewichtsteilen Blähgraphit. A dry mixture is made from the following ingredients: 45 parts by weight Schnitzel made of flexible polyurethane foam with different particle sizes in the range of 1 - 7 mm 10 parts by weight Zinc borate as an inorganic hot melt adhesive 12.5 parts by weight Hollow glass microspheres 9.5 parts by weight Ammonium polyphosphate and 13 parts by weight Expandable graphite.

    Während die Mischung weiter vermischt wird, werden ihr 10 Gewichtsteile Diphenylmethandiisocyanat, das in Wasser dispergiert ist, zugedüst. Danach wird die Mischung in einer beheizten Preßform durch mehrere Dampfstöße auf ca. 150 °C erwärmt, wodurch sie zu einem porösen Schaumstoffverbundkörper mit einer Dichte von 300 kg/m3 verpreßt und verfestigt wurde. While the mixture is being mixed further, 10 parts by weight of diphenylmethane diisocyanate dispersed in water are sprayed into it. The mixture is then heated to about 150 ° C. in a heated press mold by means of several bursts of steam, as a result of which it is pressed and solidified to form a porous foam composite body with a density of 300 kg / m 3 .

    Der dabei erhaltene Verbundkörper hatte eine Shore-A-Härte von 15, einen Elastizitätsmodul von 6 · 103 N/m2 und eine Stauchhärte (40 %) von 2 · 102 N/mm2.The composite body obtained had a Shore A hardness of 15, a modulus of elasticity of 6 · 10 3 N / m 2 and a compression hardness (40%) of 2 · 10 2 N / mm 2 .

    Die Schnittflächen waren porös und nicht klebrig. Sie hatten eine gleichmäßig schwarz-graue Farbe, wobei einzelne Blähgraphitteilchen zu erkennen waren. Aus dem Verbundkörper wurden Platten geschnitten, aus denen wiederum die gewünschten Formen der Öffnungsverschlüsse (Zylinder, Quader und dergleichen) ausgestanzt wurden. Für die Bildung von Kabeldurchführungen wurden verschieden große Löcher so vorgestanzt, daß die jeweiligen Lochkerne an der Baustelle ohne Werkzeug von Hand herausgedrückt werden konnten.The cut surfaces were porous and not sticky. They had an even one black-gray color, whereby individual expandable graphite particles were recognizable. Out The composite body was cut plates, from which in turn the desired forms of opening closures (cylinders, cuboids and the like) were punched out. For the formation of cable bushings were different large holes are pre-punched so that the respective hole cores at the construction site without Tool could be pushed out by hand.

    Die Öffnungsverschlüsse konnten ohne Bruchgefahr gebogen und zusammengedrückt werden. Sie sind so fest, daß sie mit dem Hammer in Öffnungen eingeschlagen und ohne Bruch- oder Zerreißgefahr aus den Öffnungen wieder herausgezogen werden konnten.The opening closures could be bent without risk of breakage and be squeezed together. They are so firm that they hammer into openings hammered in and out of the openings without risk of breakage or tearing could be pulled out.

    Aus den Verbundkörpern können zylinderförmige Teile mit Dicke 6 cm geschnitten werden. Diese Zylinder eigenen sich zur Abschottung von Bohrungen in Bauteilen, durch welche Elektrokabel geführt werden. Werden zwei dieser Zylinder in eine Bohrung in einer 120 mm dicken Betonwand eingebaut, durch welche Elektrokabel von bis zu 20 mm Durchmesser geführt werden, so läßt sich hiermit ein Feuerwiderstand von mehr als 120 Minuten nach DIN 3102, Teil 9, erreichen.Cylindrical parts with a thickness of 6 cm can be cut from the composite bodies become. These cylinders are suitable for sealing off holes in components, through which electrical cables are led. Will two of these cylinders become one Hole in a 120 mm thick concrete wall, through which electrical cables of up to 20 mm in diameter can be performed with this Fire resistance of more than 120 minutes according to DIN 3102, part 9.

    Beispiel 2Example 2

    Beispiel 1 wurde wiederholt, wobei zunächst ein Blähmittel und wärmewirksames Bindemittel enthaltendes Granulat hergestellt wurde. Hierzu wurden 25 Gew% Polyvinylacetat in Form eines feinen Granulats, 35 Gew% Blähgraphit, 30 Gew% Glasmikrohohlkugeln mit einem Schmelzbeginn von ca. 700 °C sowie 9,5 Gew% Borax und 0,5 Gew% hydrophobe Kieselsäure unter Erwärmen miteinander vermischt, wobei das thermoplastische Polyvinylacetat erweicht und eine Bindung der Mischung herbeiführte. Nach dem Erkalten wird der erhaltene Kuchen zu einem Granulat mit einer Teilchengröße von 1 - 3 mm granuliert. 50 Gewichtsteile dieses Granulats wurden mit 40 Gewichtsteilen Polyurethan-Weichschaumschnitzeln sorgfältig vermischt, wonach 10 Gewichtsteile Polyvinylacetat/Ethylencopolymer-Pulver zugegeben wurden. Diese Mischung wird in eine Form eingefüllt, auf 120 °C aufgeheizt, 15 Minuten bei dieser Temperatur belassen und dann auf Raumtemperatur abgekühlt. Aus dem erhaltenen Verbundkörper bzw. den daraus geschnittenen Platten wurden wiederum Öffnungsverschlüsse ausgeschnitten bzw. ausgestanzt. Diese hatten ähnliche physikalische Eigenschaften wie in Beipiel 1. Bei Zugabe von Wasser quollen die Verschlüsse an der Oberfläche auf. was zu einem Verschließen und damit Abdichten der Porosität der Öffnungsverschlüsse an ihren Oberflächen führte.Example 1 was repeated, first of all producing a granulate containing blowing agent and heat-effective binder. For this purpose 25% by weight Polyvinyl acetate in the form of fine granules, 35% by weight expandable graphite, 30% by weight Glass micro hollow spheres with a melting start of approx. 700 ° C as well 9.5% by weight Borax and 0.5% by weight hydrophobic silica mixed together with heating, the thermoplastic polyvinyl acetate softening and causing the mixture to bind. After cooling, the cake obtained is granulated into granules with a particle size of 1-3 mm. 50 parts by weight of these granules were carefully mixed with 40 parts by weight of flexible polyurethane foam chips, after which 10 parts by weight of polyvinyl acetate / ethylene copolymer powder were added. This mixture is poured into a mold, heated to 120 ° C., left at this temperature for 15 minutes and then cooled to room temperature. Opening closures were again cut or punched out of the composite body obtained or the plates cut therefrom. These had similar physical properties as in Example 1. When water was added, the closures swelled on the surface. which led to a sealing and thus sealing of the porosity of the opening closures on their surfaces.

    Beispiel 3Example 3

    Es wird eine trockene Mischung hergestellt aus 45 Gew% eines Quellmittelgranulats nach DE 39 30 722 A1, welches bereits wärmewirksames Bindemittel enthält, und 50 Gew% eines auf eine Größe von 1 - 3 mm gemahlenen Kautschukschaumes. Diese Mischung wird-mit 5 Gew% Diphenylmethandiisocynat, welches 1:1 mit Wasser verdünnt ist, besprüht. Dieses Vorprodukt wird in einer beheizten Preßform mit mehreren Dampfstößen auf ca. 170 °C erwärmt, wodurch es sich zu einem Verbundkörper mit Dichte 380 kg/m3 verfestigt. Der Verbundkörper besitzt einen Elastizitätsmodul von 2 · 104 N/m2 und eine Stauchhärte (40 %) von 2,5 · 102 N/mm2 Aus dem Verbundkörper werden im Querschnitt trapezförmige Körper zugeschnitten. die zur Abdichtung der Trapezblechsicken oberhalb von Wänden innerhalb von Gebäuden verwandt werden können Bei einem Brandversuch nach DIN 4102, Teil 2, besitzen die Verbundkörper bei einer Dicke von 120 mm eine Feuerwiderstandsdauer von mehr als 2 Stunden.A dry mixture is produced from 45% by weight of a swelling agent granulate according to DE 39 30 722 A1, which already contains heat-binding agent, and 50% by weight of a rubber foam ground to a size of 1-3 mm. This mixture is sprayed with 5% by weight of diphenylmethane diisocyanate, which is diluted 1: 1 with water. This intermediate product is heated in a heated press mold with several bursts of steam to approx. 170 ° C., whereby it solidifies into a composite body with a density of 380 kg / m 3 . The composite body has a modulus of elasticity of 2 · 10 4 N / m 2 and a compression hardness (40%) of 2.5 · 10 2 N / mm 2. The cross-section of trapezoidal bodies is cut from the composite body. which can be used to seal the trapezoidal sheet metal beads above walls inside buildings. In a fire test according to DIN 4102, part 2, the composite bodies with a thickness of 120 mm have a fire resistance duration of more than 2 hours.

    Claims (15)

    1. A fire-resistant elastic closure for openings in the form of a preformed composite block of
      a) at least one type of elastically compressible particles,
      b) at least one heat-activated expanding agent,
      c) at least one heat-activated binder and
      d) at least one adhesive by which the elastically compressible particles
         and the other constituents are joined to form the composite block,
      characterized in that the adhesives d) are selected from the group of diisocyanates.
    2. A closure as claimed in claim 1, characterized in that at least two binders which kick in at different temperatures are provided.
    3. A closure as claimed in claim 1 or 2, characterized in that organic thermoplastics and/or inorganic hotmelt adhesives, such as in particular ammonium polyphosphate, zinc borate and/or glass are provided as the at least one heat-activated binder.
    4. A closure as claimed in any of the preceding claims, characterized in that at least two expanding agents expanding at different temperatures are provided as the expanding agents.
    5. A closure as claimed in any of the preceding claims, characterized in that expanded graphite and optionally unexpanded vermiculite and/or perlite are provided as the expanding agents.
    6. A closure as claimed in any of the preceding claims, characterized in that the at least one expanding agent and the at least one heat-activated binder are present in the form of granules containing both constituents.
    7. A closure as claimed in any of the preceding claims, characterized in that the adhesive which holds the constituents of the composite block together is diphenyl methane diisocyanate (MDI) which is set in particular with water.
    8. A closure as claimed in any of the preceding claims, characterized in that the composite block is porous and has a rough surface.
    9. A closure as claimed in any of the preceding claims, characterized in that the composite block is a composite foam block and the elastically compressible particles are foam particles.
    10. A closure as claimed in any of the preceding claims, characterized in that it is formed by cutting or the like from a relatively large composite block.
    11. A closure as claimed in any of the preceding claims, characterized in that it has an elasticity modulus of 1·103 to 1·105 N/m2 and more particularly of the order of 7·103 N/m2.
    12. A closure as claimed in any of the preceding claims, characterized in that it has a compression hardness (40%) of 1·102 to 1·103 N/mm2 and more particularly of the order of 1.7·102 N/mm2.
    13. A closure as claimed in any of the preceding claims, characterized in that it has a Shore A hardness of 10 to 40 and more particularly of the order of 15.
    14. A closure as claimed in any of the preceding claims, characterized in that it has a density in the range from 200 to 600 kg/m2 and more particularly in the range from 250 to 400 kg/m2.
    15. A closure as claimed in any of the preceding claims, characterized in that it has a fire resistance of 30 to 120 minutes (according to DIN 4102).
    EP98908030A 1997-02-08 1998-01-31 Fire-resistant opening seal Expired - Lifetime EP0960251B1 (en)

    Applications Claiming Priority (3)

    Application Number Priority Date Filing Date Title
    DE19704833A DE19704833A1 (en) 1997-02-08 1997-02-08 Fire-resistant opening lock
    DE19704833 1997-02-08
    PCT/EP1998/000517 WO1998035122A1 (en) 1997-02-08 1998-01-31 Fire-resistant opening seal

    Publications (2)

    Publication Number Publication Date
    EP0960251A1 EP0960251A1 (en) 1999-12-01
    EP0960251B1 true EP0960251B1 (en) 2003-04-02

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    EP (1) EP0960251B1 (en)
    AT (1) ATE236337T1 (en)
    AU (1) AU721890B2 (en)
    DE (2) DE19704833A1 (en)
    DK (1) DK0960251T3 (en)
    WO (1) WO1998035122A1 (en)

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    DE59807738D1 (en) 2003-05-08
    AU721890B2 (en) 2000-07-13
    DK0960251T3 (en) 2003-07-28
    EP0960251A1 (en) 1999-12-01
    DE19704833A1 (en) 1998-08-13
    WO1998035122A1 (en) 1998-08-13
    US6544445B1 (en) 2003-04-08
    ATE236337T1 (en) 2003-04-15
    AU6618298A (en) 1998-08-26

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