SI9200220A - Fireproof material, process for their production and their use - Google Patents
Fireproof material, process for their production and their use Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
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Abstract
Description
1. SAVA Kranj,industrija gumijevih,usnjenih in kemičnih izdelkov p.o.1. SAVA Kranj, industry of rubber, leather and chemical products p.o.
2. IZOLIRKA industrija izolacijskih materialov Ljubljana p.o.2. INSULATION insulation materials industry Ljubljana p.o.
OGNJEODPOREN MATERIAL,FIRE-RESISTANT MATERIAL,
POSTOPEK ZA NJEGOVO PROIZVODNJO IN NJEGOVA UPORABAPROCEDURE FOR ITS MANUFACTURING AND ITS USE
Predloženi izum se nanaša na nov, ognjeodporen material, na postopek za njegovo proizvodnjo in na njegovo uporabo, npr. v gradbeništvu, rudarstvu, brodogradnji in industriji vozil, kjer se v skladu z zakonskimi predpisi in standardi morajo vgrajevati ognjeodporne materiale/pregrade, ki v primeru požara le-tega lokalizirajo in preprečijo njegovo širjenje.The present invention relates to a new, refractory material, to a process for its production and to its use, e.g. in the construction, mining, shipbuilding and vehicle industries, where fire-resistant materials / barriers must be installed in accordance with legal regulations and standards, which in the event of a fire localize it and prevent its spread.
Obstajala je potreba po novem ognjeodpomem materialu, s katerim bi se dalo preprosto rokovati, ga nameščati, prilagajati in preoblikovati, ki bi bil pri normalni uporabi in pri požarih nestrupen, antikoroziven in neobčutljiv na vlago oziroma v vodi netopen, s trajnimi odpornostnimi lastnostmi in trajno protipožarno učinkovitostjo.There was a need for a new flame retardant material that could be easily handled, installed, adapted and transformed, which would be non-toxic, anti-corrosive and water-insoluble, water-insoluble, durable and durable in normal use and fire. fire efficiency.
Kljub mnogim obstoječim rešitvam so le-te v mnogih primerih zahtevne in komplicirane, pogosto tudi komaj zadovoljive.Despite many existing solutions, they are in many cases demanding and complicated, often even barely satisfactory.
Tako npr. karakteristike za protipožarne pregrade predpisujejo številni mednarodni in nacionalni standardi.So e.g. firewall characteristics are prescribed by many international and national standards.
Naj navedemo za SFRJ najbolj obvezujoče: DIN 4102, ISO 1182, JUS U.J5.715. Kvaliteta ognjeodpomih protipožarnih pregrad se ocenjuje z njihovo vzdržljivostjo proti plamenu določene temperature, ki presega 1000°C, pri čemer se vzdržljivost protipožarnih pregrad izraža v minutah, in njihovo toplotno izolativnostjo, ki preprečuje prenos toplotne energije plamena na zaščiteno podlago, ki je pogosto tudi nosilna.The following are the most binding for the SFRY: DIN 4102, ISO 1182, JUS U.J5.715. The quality of fire retardant barriers is evaluated by their resistance to flame at a certain temperature in excess of 1000 ° C, with fire barrier durability being expressed in minutes, and their thermal insulation, which prevents the transfer of heat energy from the flame to a protected surface, which is often also load-bearing. .
Na splošno so ognjeodporni sistemi sestavljeni iz naravnega mineralnega vermikulita, ki je kemijsko hidratiziran silikat aluminija, železa in magnezija, ter določenih veziv. Poznani so npr. naslednji:Generally, refractory systems consist of natural mineral vermiculite, which is chemically hydrated silicate of aluminum, iron and magnesium, and certain binders. They are known e.g. the following:
- anorganske termoizolacijske plošče iz mineralne volne in veziv, kot fenoplastov; npr.: TERVOL, proizvajalca TERMIKA (reg. blagovna znamka), Škofja Loka;- mineral wool inorganic thermal insulation boards and binders, such as phenoplasts; eg TERVOL, manufacturer of TERMIK (reg. trade mark), Škofja Loka;
- anorganske vermikulitno - cementno - apnene maltne mešanice, ki se jih z vodo meša do želene viskoznosti in nanaša na različne načine, odvisno od njihove viskoznosti in nanašalnih naprav;- inorganic vermiculite - cement - lime mortar mixtures, miscible with water to the desired viscosity and applied in various ways, depending on their viscosity and application devices;
npr.: Verpas (reg. blagovna znamka), proizvajalec STANDARD OPERATIVA, Ljubljana;eg: Verpas (Reg. Trademark), manufactured by STANDARD OPERATIVA, Ljubljana;
- negorljive toge plošče iz vermikulita in ustreznih veziv; plošče se obdelujejo po tehnologiji lesno obdelovalnih postopkov:- non-combustible rigid vermiculite sheets and suitable binders; plates are processed according to the technology of woodworking processes:
npr.: BREST NEGOR (reg. blagovna znamka), proizvajalec BREST, Cerknica;eg: BREST NEGOR (Reg. Trademark), manufacturer BREST, Cerknica;
- porozne anorganske toge plošče ali bloki na osnovi hidrotermalne obdelave silicijevega in kalcijevega oksida in se obdelujejo kot lahka silikatna opeka;- porous inorganic rigid sheets or blocks based on hydrothermal treatment of silicon and calcium oxide and treated as lightweight silicate brick;
npr.: APLAM (reg. blagovna znamka), proizvajalec SALONIT ANHOVO, Anhovo;eg: APLAM (Reg. Trademark), Manufacturer SALONIT ANHOVO, Anhovo;
- tekoči in pastni materiali na osnovi anorganskih polnil in vodno disperznih veziv, ki se mešajo na različne načine, odvisno od njihove viskoznosti in nanašalnih naprav; npr.: PLAMMAL (reg. blagovna znamka), proizvajalec ADING, Skopje;- Liquid and paste based materials of inorganic fillers and water-dispersible binders, which are mixed in different ways, depending on their viscosity and application devices; eg: PLAMMAL (Reg. Trademark), manufacturer ADING, Skopje;
- tekoči materiali na osnovi anorganskih polnil in organskih veziv, ki se nanašajo kot barve ali premazi;- Liquid materials based on inorganic fillers and organic binders, which are applied as paints or coatings;
npr.: PIROSTOP (reg. blagovna znamka), proizvajalca CHROMOS-KATRANeg: PIROSTOP (Reg. Trademark), by CHROMOS-KATRAN
KUTRILIN, Zagreb.KUTRILIN, Zagreb.
Za večino navedenih materialov je značilno, da ob toplotnem udaru nabreknejo in s tem ustvarijo zaščitno bariero, ki preprečuje plamenu neposreden prenos toplotne energije na podlago. Vendar pa je v kritičnih trenutkih njihova protipožarna obstoj nost in zaščita vprašljiva, saj prihaja zaradi različnih temperaturnih razteznostnih koeficientov materialov do odluščenja zaščitne pregrade od nosilne pregrade in s tem porušitve zaščitne vloge protipožarne pregrade.Most of these materials are characterized by swelling during heat stroke, thus creating a protective barrier that prevents the flame from directly transferring thermal energy to the substrate. However, at critical moments, their fire resistance and protection are questionable, because different temperature expansion coefficients of the materials lead to the decision of the barrier against the load barrier and thus to the destruction of the protective role of the fire barrier.
Kritična ocena obstoječih rešitev ognjeodpomih h materialov nedvoumno kaže, da obstaja potreba po novih, tehnično in funkcionalno boljših in uspešnejših rešitvah.The critical evaluation of existing fire retardant solutions clearly shows that there is a need for new, technically and functionally better and more successful solutions.
Ugotovili smo, da zgoraj navedene tehnične probleme rešimo z novim, ognjeodpornim materialom v smislu predloženega izuma, ki ga sestavlja elastomerna matrika, ki vsebuje anorganska polnila z dvojno vlogo:We have found that the above technical problems are solved with a new, refractory material according to the present invention, consisting of an elastomeric matrix containing dual role inorganic fillers:
- narediti elastomemo matriko negorljivo in- make the elastomy matrix non-combustible and
- v teku termične degradacije elastomeme matrike omogočiti materijalu prehod v visoko-temperatumo obstojno, t.j. keramično strukturo.- allow the material to transition to high-temperature in the course of thermal degradation of the elastomeme matrix, i.e. ceramic structure.
ognjeodporen material v smislu predloženega izuma obstaja iz:The fire retardant material of the present invention consists of:
- 100 mas.delov elastomera v obliki trdne ali tekoče matrike, ki jo tvori en sam ali zmes elastomerov, prednostno pri termičnem razpadu netoksičnih elastomerov, izbranih izmed nasičenih ali nenasičenih ogljikovodikov, prednostno brez benzenskih obročev, kot so naravni (NR), poliizoprenski (IR), polibutadienski (BR), izobutilenski ali butilni (IIR), etilen-propilenski (EPDM ali EPM) elastomeri,- 100 parts by weight of elastomers in the form of a solid or liquid matrix formed by a single or a mixture of elastomers, preferably by thermal decomposition of non-toxic elastomers selected from saturated or unsaturated hydrocarbons, preferably without benzene rings, such as natural (NR), polyisoprene ( IR), polybutadiene (BR), isobutylene or butyl (IIR), ethylene-propylene (EPDM or EPM) elastomers,
- 100 do 1000 mas.delov anorganskih polnil, izbranih izmed 30 do 300 mas.delov kovin I. glavne skupine periodnega sistema, 0 do 100 mas.delov kovin II. glavne skupine periodnega sistema in 50 do 500 mas.delov kovin III. glavne skupine periodnega sistema, v obliki oksidov, hidroksidov, karbonatov, sulfatov, boratov, hidratov ali silikatov, ali njihovih zmesi, _ ter v danem primeru vermikulita zrnavosti 0,01 do 10 mm, v razmerju 100 mas. delov (elastomera + anorganskega polnila) : 5-500 mas.delov vermikulita, ter po potrebi premreževalnih/vulkanizacijskih sredstev, topil in dodatkov za regulacijo viskoznosti in konsistentnosti.- 100 to 1000 parts by weight of inorganic fillers selected from 30 to 300 parts by weight of metals of the first group of the periodic system, 0 to 100 parts by weight of metals II. major groups of the periodic system and 50 to 500 parts by weight of metals III. main groups of the periodic system, in the form of oxides, hydroxides, carbonates, sulphates, borates, hydrates or silicates, or mixtures thereof, _ and in the case of vermiculite granularity 0,01 to 10 mm, in a ratio of 100 wt. parts (elastomer + inorganic filler): 5-500 parts by weight of vermiculite, and if necessary crosslinking / vulcanizing agents, solvents and additives for regulating viscosity and consistency.
Oznake NR, IR, BR, IIR, EPDM in EPM so standardne mednarodne kratice za materiale, ki so točno definirani pred temi kraticami, in ustrezajo standardu ISO 1629 nomenklature za kavčuke.The NR, IR, BR, IIR, EPDM and EPM codes are standard international abbreviations for materials that are precisely defined before these abbreviations and conform to ISO 1629 Rubber Nomenclature.
Nadaljnji predmet predloženega izuma je postopek za pripravo novega, ognjeodpornega, materiala, ki poteka tako, da:It is a further object of the present invention to provide a process for the preparation of new, refractory, material which is produced in such a way that:
v 100 mas.delov elastomera v obliki trdne ali tekoče matrike, ki jo tvori en sam ali zmes zmes elastomerov, prednostno pri termičnem razpadu netoksičnih elastomerov, izbranih izmed nasičenih ali nenasičenih ogljikovodikov, prednostno brez benzenskih obročev, kot so naravni (NR), poliizoprenski (IR), polibutadienski (BR), izobutilenski ali butilni (UR), etilen-propilenski (EPDM ali EPM) elastomeri, vgnetemo z gumarsko tehniko mešanja 100 do 1000 mas.delov anorganskih polnil, izbranih izmed 30 do 300 mas.delov kovin I. glavne skupine periodnega sistema, 0 do 100 mas.delov kovin II. glavne skupine periodnega sistema in 50 do 500 mas.delov kovin III. glavne skupine periodnega sistema, v obliki oksidov, hidroksidov, karbonatov, sulfatov, boratov, hidratov ali silikatov, ali njihovih zmesi, ter v danem primeru vermikulit zrnavosti 0,01 do 10 mm, v razmerju 100 mas. delov (elastomera + anorganskega polnila): 5-500 mas.delov vermikulita, ter po potrebi nato dodamo premreževalna/vulkanizacijaska sredstva, topila in dodatke za regulacijo viskoznosti in konsistentnosti.in 100 parts by weight of elastomers in the form of a solid or liquid matrix formed by a single or a mixture of a mixture of elastomers, preferably by thermal decomposition of non-toxic elastomers selected from saturated or unsaturated hydrocarbons, preferably without benzene rings, such as natural (NR), polyisoprene (IR), polybutadiene (BR), isobutylene or butyl (UR), ethylene-propylene (EPDM or EPM) elastomers, agitated by the rubber technique of mixing 100 to 1000 parts by weight of inorganic fillers selected from 30 to 300 parts by weight of metals I main groups of the periodic system, 0 to 100 parts by weight of metals II. major groups of the periodic system and 50 to 500 parts by weight of metals III. main groups of the periodic system, in the form of oxides, hydroxides, carbonates, sulphates, borates, hydrates or silicates, or mixtures thereof, and, if appropriate, vermiculite granules of 0.01 to 10 mm, in a ratio of 100% by weight. parts (elastomer + inorganic filler): 5-500 parts by weight of vermiculite, and then, if necessary, crosslinking / vulcanizing agents, solvents and viscosity and consistency control additives.
V primeri z že obstoječimi materiali in sistemi ima material v smislu izuma naslednje prednosti:Compared to existing materials and systems, the material of the invention has the following advantages:
lahko ga je oblikovati in prilagojevati, enostavno ga je pritrjevati in nanašati na podlage, je pri normalni uporabi in v primeru požara nestrupen oziroma ne sprošča strupenih produktov, je neobčutljiv na vlago in je nevodotopen, za enako ognjeodpornost, z izjemo PIROSTOP-a, ki pa je učinkovit le do 30 minut, so potrebne bistveno manjše debeline (Tabela 1), kar prihrani prostor.it is easy to design and adjust, it is easy to attach and apply to substrates, it is non-toxic or non-toxic in case of fire, it is insensitive to moisture and it is insoluble, with the same fire resistance, with the exception of PIROSTOP, which however, only effective for up to 30 minutes, significantly smaller thicknesses are needed (Table 1), which saves space.
TABELA 1TABLE 1
Primerjava ognjeodpornosti materiala v smislu izuma z obstoječimi tržnimi proizvodiComparison of the fire resistance of the material of the invention with existing marketable products
Ognjeodpornost Naziv materiala (min)ali sistemaFire resistance The name of the material (min) or system
Potrebna debelina (mm)Required thickness (mm)
PIROSTOP 1PIROSTOP 1
VERPAS 10VERPAS 10
PLAMAL-30 50PLAMAL-30 50
BREST NEGORBREST NEGOR
APLAM 45APLAM 45
TERVOL-PVT 75TERVOL-PVT 75
ELASTOMERNI MATERIAL 6 v smislu izuma (Primer 1)ELASTOMERIC MATERIAL 6 according to the invention (Example 1)
Predloženi izum pojasnjujemo z naslednjimi izvedbenimi primeri.The present invention is explained by the following embodiments.
PRIMERIEXAMPLES
Na 100 masnih delov naravnega kavčuka (NR) smo dodali 300 masnih delov alkalijsko-alumosilikatne mešanice, ki smo jo na dvovaljčniku domešali v elastomemo zmes, ki smo jo nato povlekli v ploščo debeline 6 mm. Ognjeodporno elastomerno ploščo smo z dvokomponentnim elastomernim polikloropenskim lepilom nalepili na očiščeno železno ploščo, tako, da smo obe površini premazali z lepilom in nato posušeni spojili. Stran z ognjeodporno elastomemo ploščo smo izpostavili plamenu plinskega gorilnika. Po polurni toplotni obremenitvi je ostala več kot polovica elastomerne zmesi nespremenjena in temperatura kovinske podloge ni presegla 300° C.To the 100 parts by weight of natural rubber (NR), 300 parts by weight of an alkali-alumosilicate mixture were added, which was mixed into an elastomy mixture on a two-roller, which was then dragged into a 6 mm thick plate. The flame retardant elastomeric board was glued to the cleaned iron plate with a two-component elastomeric polychloropenic adhesive, so that both surfaces were coated with glue and then jointed together. The flame retardant elastomeric side was exposed to the gas burner flame. After a half-hour heat load, more than half of the elastomer mixture remained unchanged and the metal substrate temperature did not exceed 300 ° C.
PRIMER 2EXAMPLE 2
Ognjeodporno elastomemo ploščo v skladu s Primerom 1 smo dublirali s polietilensko folijo debeline 1 mm v kompozit tako, da smo elastomemo ploščo predhodno površinsko segreli z vročim zrakom, nakar smo termoplastično polietilensko folijo zalikali na elastomemo ploščo. Kompozit smo izpostavili plamenu plinskega gorilnika. V dveh minutah je PE folija odgorela, nato pa je elastomerna plošča prevzela ognjeodporno vlogo kot v Primeru 1.The flame retardant elastomy plate according to Example 1 was duplicated with a 1 mm thick polyethylene film in the composite by preheating the elastomy plate with hot air and then gluing the thermoplastic polyethylene film to the elastomy plate. The composite was exposed to the flame of a gas burner. Within two minutes, the PE film was burned off, and then the elastomeric plate assumed a fire-resistant role as in Example 1.
PRIMER 3EXAMPLE 3
Ognjeodporni elastomerni kit smo izdelali tako, da smo na 100 masnih delov tekočega elastomera dodali 200 masnih delov mešanice alkalijsko-alumosilikatnih polnil in zmletega vermikulita, velikosti od 0,1 do 2 mm. S tako izdelanim elastomernim kitom smo izpolnili fugo, ki smo jo nato izpostavili plinskemu plamenu. Kit je tudi po polurni toplotni obremenitvi ohranil plinotesnost.The flame retardant elastomer kit was manufactured by adding 200 parts by weight of a mixture of alkali-alumosilicate fillers and ground vermiculite in a size from 0.1 to 2 mm per 100 parts by weight of liquid elastomer. With the elastomer kit thus made, the joint was filled, which was then exposed to the gas flame. The kit retained gas tightness even after a half-hour heat load.
PRIMER 4EXAMPLE 4
Ognjeodporni elastomerni premaz smo izdelali tako, da smo elastomerno zmes v skladu s Primerom 1 razredčili z bencinom in nastali mešanici dodali zmlet vermikulit velikosti od 0,1 do 1,0 mm, da smo dobili premazno maso primerne konsistence, ki smo jo nato z lopatico nanesli na jekleno palico premera 14 mm in dolžine 400 mm. Po enodnevni osušitvi smo izvedli preizkus na ognjeodpomost tako, da smo palico navorno obremenili s 100 N/mm2 v razdalji 400 mm od vpetišča in s premazom v smislu izuma zaščiteno palico segrevali s plamenom v razdalji 200 mm od vpetišča. Nezaščitena palica se je ukrivila po 2,5 minutah, z elastomemim premazom zaščitena palica pa je tudi po polurni požarni obremenitvi ohranila svoje elastične lastnosti.The refractory elastomer coating was made by diluting the elastomer mixture according to Example 1 with gasoline and adding a ground vermiculite of 0.1 to 1.0 mm in size to the resulting mixture to give a coating of suitable consistency, which was then troweled. applied to a steel bar 14 mm in diameter and 400 mm in length. After drying for one day, the fire resistance test was carried out by loading the rod with 100 N / mm2 at a distance of 400 mm from the joint and, using the coating of the invention, heated the flame with a flame within 200 mm of the joint. The unprotected rod curved after 2.5 minutes, and the elastomem coating protected the elastic properties even after half an hour of fire load.
ZaFor
1. SAVA Kranj, industrija gumijevih, usnjenih in kemičnih izdelkov p.o.1. SAVA Kranj, industry of rubber, leather and chemical products p.o.
2. IZOLIRKA industrija izolacijskih materialov Ljubljana p.o.:2. INSULATION insulation materials industry Ljubljana p.o .:
FATEMTNA PISARHAFATEMTNA PISARHA
LJUBLJANALJUBLJANA
Claims (3)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SI9200220A SI9200220A (en) | 1992-09-23 | 1992-09-23 | Fireproof material, process for their production and their use |
DE59308245T DE59308245D1 (en) | 1992-09-23 | 1993-09-23 | Refractory material, process for its production and its use |
EP93115378A EP0589461B1 (en) | 1992-09-23 | 1993-09-23 | Refractory material, process for its preparation and its utilisation |
AT93115378T ATE163966T1 (en) | 1992-09-23 | 1993-09-23 | FIREPROOF MATERIAL, METHOD FOR THE PRODUCTION THEREOF AND ITS USE |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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SI9200220A SI9200220A (en) | 1992-09-23 | 1992-09-23 | Fireproof material, process for their production and their use |
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SI9200220A true SI9200220A (en) | 1994-03-31 |
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SI9200220A SI9200220A (en) | 1992-09-23 | 1992-09-23 | Fireproof material, process for their production and their use |
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EP (1) | EP0589461B1 (en) |
AT (1) | ATE163966T1 (en) |
DE (1) | DE59308245D1 (en) |
SI (1) | SI9200220A (en) |
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GB9807180D0 (en) | 1998-04-04 | 1998-06-03 | Ecc Int Ltd | Pigment products |
BR0009458A (en) | 1999-04-01 | 2002-01-08 | Imerys Pigments Inc | Pigment product for a paper coating composition, processes for making a pigment product for a paper coating composition, and for producing a pigment product, coating composition for use in the production of gloss coatings on paper and others substrates, and, process for coating a sheet of paper and calendering the paper to form a gloss coating on it |
DE10084441T1 (en) | 1999-04-01 | 2002-03-21 | Imerys Pigments Inc | Koalinton pigments, their production and use |
DE19921472A1 (en) * | 1999-05-08 | 2000-11-16 | Sued Chemie Ag | Flame retardant polymer composition |
US6554892B1 (en) | 1999-07-02 | 2003-04-29 | Imerys Kaolin, Inc. | Compositions and methods for making a coarse platey, high brightness kaolin product |
GB0020180D0 (en) | 2000-08-17 | 2000-10-04 | Imerys Minerals Ltd | Kaolin products and their production |
GB0020179D0 (en) | 2000-08-17 | 2000-10-04 | Imerys Minerals Ltd | Kaolin products and their use |
US20030085012A1 (en) | 2001-09-07 | 2003-05-08 | Jones J Philip E | Hyperplaty clays and their use in paper coating and filling, methods for making same, and paper products having improved brightness |
US6808559B2 (en) | 2002-02-26 | 2004-10-26 | Imerys Pigments, Inc. | Kaolin clay pigments suited to rotogravure printing applications and method for preparing the same |
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US4671896A (en) * | 1984-08-14 | 1987-06-09 | Fujikura Ltd. | Flame-retardant composition and flame-retardant cable using same |
JPH01217050A (en) * | 1988-02-26 | 1989-08-30 | Tonen Sekiyukagaku Kk | Flame retardant thermoplastic elastomer composition |
DE3827906C2 (en) * | 1988-08-17 | 1995-05-04 | Continental Ag | Airborne sound curtain |
DE4033116A1 (en) * | 1990-10-18 | 1992-04-23 | Inst Priloschna Mineralogia Ba | Fire-resistant polymer materials for high-temp. applications - contain high- or low-pressure polyethylene@, polypropylene@ or polystyrene, with dried water-glass and/or dried lignin and/or zeolite |
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1992
- 1992-09-23 SI SI9200220A patent/SI9200220A/en unknown
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1993
- 1993-09-23 DE DE59308245T patent/DE59308245D1/en not_active Expired - Fee Related
- 1993-09-23 EP EP93115378A patent/EP0589461B1/en not_active Expired - Lifetime
- 1993-09-23 AT AT93115378T patent/ATE163966T1/en not_active IP Right Cessation
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Publication number | Publication date |
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ATE163966T1 (en) | 1998-03-15 |
EP0589461A1 (en) | 1994-03-30 |
EP0589461B1 (en) | 1998-03-11 |
DE59308245D1 (en) | 1998-04-16 |
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