EP0976423B1 - Verfahren und Vorrichtung zum Löschen von Bränden - Google Patents

Verfahren und Vorrichtung zum Löschen von Bränden Download PDF

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Publication number
EP0976423B1
EP0976423B1 EP99113153A EP99113153A EP0976423B1 EP 0976423 B1 EP0976423 B1 EP 0976423B1 EP 99113153 A EP99113153 A EP 99113153A EP 99113153 A EP99113153 A EP 99113153A EP 0976423 B1 EP0976423 B1 EP 0976423B1
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EP
European Patent Office
Prior art keywords
gas
composition
aerosol
der
complete oxidation
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Expired - Lifetime
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EP99113153A
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German (de)
English (en)
French (fr)
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EP0976423A1 (de
Inventor
Nikolaj Vasil'evic d.7 kv.13 Drakin
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R Amtech International Inc
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R Amtech International Inc
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Priority claimed from RU98113952/12A external-priority patent/RU2147903C1/ru
Priority claimed from RU98122276/12A external-priority patent/RU2142306C1/ru
Application filed by R Amtech International Inc filed Critical R Amtech International Inc
Publication of EP0976423A1 publication Critical patent/EP0976423A1/de
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    • AHUMAN NECESSITIES
    • A62LIFE-SAVING; FIRE-FIGHTING
    • A62CFIRE-FIGHTING
    • A62C99/00Subject matter not provided for in other groups of this subclass
    • A62C99/0009Methods of extinguishing or preventing the spread of fire by cooling down or suffocating the flames
    • A62C99/0018Methods of extinguishing or preventing the spread of fire by cooling down or suffocating the flames using gases or vapours that do not support combustion, e.g. steam, carbon dioxide
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61DVETERINARY INSTRUMENTS, IMPLEMENTS, TOOLS, OR METHODS
    • A61D1/00Surgical instruments for veterinary use
    • A61D1/06Castrating appliances
    • AHUMAN NECESSITIES
    • A62LIFE-SAVING; FIRE-FIGHTING
    • A62CFIRE-FIGHTING
    • A62C5/00Making of fire-extinguishing materials immediately before use
    • A62C5/006Extinguishants produced by combustion

Definitions

  • the invention relates to the field of fire extinguishing technology, in particular Process for extinguishing fires using gas-aerosol mixtures, those when burning pyrotechnic compositions arise.
  • the method according to the invention and the device for deleting of fires ensure effective extinguishing of fires in extreme fire situations, as well as the survival of people and other living things that are in the fire zone.
  • Russian Patent 2,072,135 describes a method for Extinguishing fires known when burning a pyrotechnic charge creates a gas-aerosol mixture that interacts with combustion products in the fire zone and extinguishes the fire.
  • the gas-aerosol mixture Before the introduction to the protective space, the gas-aerosol mixture is cooled, whereby the mixture interacts with substances that are high heat absorbing and have gas-releasing properties, e.g. Carbonates, hydrates, hydrooxides, oxalates, and which are in the form of Have granules or tablets.
  • the device for realizing this method exists from a housing with a pyrotechnic composition, a heat protection layer and an outlet opening.
  • the pyrotechnic Composition is ignited with a standard igniter.
  • the cooling of the gas-aerosol mixture that occurs during combustion the pyrotechnic composition arises in a cooling block that acts as a container filled with coolants shaped and in the housing between the pyrotechnic Composition and the outlet opening is arranged.
  • a pyrotechnic gas aerosol-forming composition which as an oxidizing agent contains 67 to 72 percent by weight potassium nitrate with a particle surface area of at least 1500 cm 2 / g, and as a fuel binder 8 to 12 percent by weight phenol formaldehyde resin with a particle size of not more than 100 ⁇ m, and the balance gas aerosol forming agent, namely dicyandiamide having a particle size of not more than 15 ⁇ m.
  • the composition can additionally contain potassium carbonate, potassium benzoate or potassium hexacyanoferrate in an amount of 4 to 12% by mass.
  • oxidation catalysts become the combustion products used, selected from: metals: nickel, Cobalt, iron, manganese, chrome, aluminum, magnium, copper, platinum, Silver, their oxides and / or peroxides, salts, and their Alloys and mixtures.
  • the aerosol generating composition, the heat absorbing filling and the oxidation filling can be coated with the catalysts mentioned be or contain them in their compositions.
  • oxidant are selected from the following substances: ammonium nitrate, Potassium nitrate, sodium nitrate, calcium nitrate, barium nitrate, Strontium nitrate, ammonium perchlorate, potassium perchlorate, Sodium perchlorate and their mixtures.
  • gas aerosol images dicyandiamide is used, as a combustible binder, a polycondensate of formaldehyde with phenol, and as an oxidizing agent, potassium nitrate.
  • the gas aerosol images, the fuel binder and the oxidizing agent each consist of two fractions: 40 to 80 ⁇ m and 7 to 15 ⁇ m with a mass ratio of 80:20, 70 to 120 ⁇ m and 10 to 25 ⁇ m with a mass ratio of 70 : 30 or 15 to 25 ⁇ m and 1 to 7 ⁇ m with a mass ratio of 25:75, with the following composition of the components in% of the mass: Gas-aerosol Images 9 to 20 flammable binder 6 to 14 oxidant Rest.
  • the proportion of small size particles should be increased. This is achieved in that as gas-aerosol images dicyandiamide with a particle size of 40 to 80 microns and 7 to 15 microns with a mass ratio of 10:90, as an oxidizing agent potassium nitrate with a particle size of 15 to 25 microns and 1 to 7 ⁇ m at a mass ratio of 5:95, and a polycondensate of formaldehyde with phenol is used as the binder, the composition of the components in percent by mass being as follows: Gas-aerosol Images 9 to 20 Flammable binder 6 to 14 oxidant Rest.
  • Particles of the phenol-formaldehyde resin are previously in Ethyl alcohol dissolved.
  • the 60% solution obtained is for used to obtain the pyrotechnic composition. While the preservation of the composition becomes the ethyl alcohol away. This solution ensures a firing temperature profile from 460 ° C in the condensed phase to 1050 ° C in the hottest Point of flame.
  • the following types of artificial zeolites are currently known: KA, NaA, NaX, which correspond to types 3A, 4A, 13X in the US classification.
  • the structure of type A zeolites consists of smaller and larger adsorption cavities.
  • the chemical formula of the NaA zeolite is: Na 2 O • Al 2 O 3 • 2SiO 2 • 4SH 2 O.
  • An elementary cell consists of a larger and a smaller cavity.
  • the larger cavity has a practically spherical shape with a diameter of 1.14 nm. It is over eight-membered oxygen rings with a diameter of 0.42 nm with six adjacent larger cavities and over six-membered oxygen rings with a diameter of 0.22 nm with eight smaller ones Cavities connected.
  • Figure 1 shows the structure of synthetic zeolites of types A (a) and X (b).
  • the type X zeolite has a similar structure. The difference is that each larger cavity has four entry openings, which are formed by twelve-membered oxygen rings with a diameter of 0.8 to 0.9 nm. Therefore, the structure of zeolites of this type is more open and accessible to gas molecules (NV Kel'cev. "Osnovy adsorbcionnoj techniki.” M.:Chimija. 1984).
  • the hot ( ⁇ ⁇ 750 ° C) gas aerosol that is released during the firing of the pyrotechnic composition leads to the heating of the zeolite surface.
  • the increase in temperature leads to an increase in the thermal pulsation of the zeolite lattice, which enables the gas molecules to penetrate more easily into the adsorption cavity formed by the oxygen rings.
  • Conditions arise within the cavity under which reactions of catalytic neutralization take place on the active surface of the zeolite cavities: 2NO t ⁇ N 2 + O 2 ; 2CO t ⁇ 2C + O 2
  • the neutralization reactions (1) and the subsequent reactions of complete oxidation (2) proceed effectively at temperatures above 700 ° C.
  • the area of complete oxidation in the form of a zeolite layer, which is enclosed between two metallic grids, is arranged in this connection in the area of the highest firing temperature (750 ° C.) of the specified pyrotechnic composition.
  • the rate of reactions (1) and (2) is slow.
  • temperatures above 800 ° C there are larger thermal pulsations of the zeolite lattice which lead to the collapse of the cavities and the reactions do not take place.
  • the effectiveness of the catalytic reactions can be increased by mounting the zeolite on a grid made of copper or a copper alloy.
  • a grid made of copper or a copper alloy When the zeolite structure is thermally pulsed, Cu 2+ cations can be introduced into these instead of Na + cations.
  • the modified zeolite resulting from the action of the hot gas-aerosol mixture increases its catalytic activity and, as a result, the concentration of toxic gases within the gas-aerosol mixture decreases.
  • Highly porous activated aluminum oxide can also be used as a catalytically active substance with a highly developed surface (300 to 345 m 2 / g).
  • the gas phase enters one Space containing the block of complete oxidation and the cooling block separates where they deal with the solid phase of the combustion products mixed the pyrotechnic composition.
  • the gas-aerosol mixture cleaned of the toxic products of incomplete combustion cools down through direct contact with the solid coolant.
  • Solid coolants such as: silica gel, zeolite and their mixtures and aluminum oxide. These substances have highly developed surfaces and porous structures that can adsorb various chemical compounds, including water.
  • the gas-aerosol mixture is cooled with the solid coolant mentioned by heat exchange.
  • the heat of the hot mixture is used to heat the solid coolant, to desorb the water and to convert the water to the vapor-like state.
  • Carbon which is excreted when the pyrotechnic composition is burned undergoes endothermic reactions with the desorbed water vapors as a result of reaction (1): C + 2H 2 O ⁇ CO 2 + 2H 2 - 178.15 kJ
  • the proposed method of extinguishing fires can be done with the known devices for extinguishing fires not in can be fully realized.
  • a device for extinguishing fires consisting of a housing with a pyrotechnic Charge, a heat protection layer, an outlet opening, an ignition device and a cooling block.
  • the cooling block is designed in the form of a room with granules or tablets of a coolant, and which is between the pyrotechnic charge and the outlet opening is.
  • the coolants are selected from: carbonates, hydrates, Hydrooxides and oxalates that have high heat absorption Features and high gas-excreting properties.
  • the main disadvantage of this device is that they receive a non-toxic gas-aerosol mixture cannot guarantee.
  • the reason for this is that the cooling block is arranged in front of the outlet opening, and the cooling process even from the excretion of toxic carbon oxides is accompanied without complete oxidation and filtration together with the gas-aerosol mixture in the to be protected Get space.
  • the heat absorbing load can additionally 10 to 60% of the Contain mass of an oxidizing agent, which from ammonium, Potassium, sodium, calcium, barium, stronzium nitrates is selected or from ammonium, potassium, sodium perchlorates or from their mixtures.
  • an oxidizing agent which from ammonium, Potassium, sodium, calcium, barium, stronzium nitrates is selected or from ammonium, potassium, sodium perchlorates or from their mixtures.
  • the device mentioned has a major disadvantage, namely the high toxicity of the fire-extinguishing gas-aerosol mixture.
  • This disadvantage can be explained by the choice of substances that are used as oxidizing agents. During their decomposition, these substances not only excrete oxygen, which is used for the complete oxidation of CO, NO, NH 3 , HCN, but also toxic products. Thus, when the nitrates are broken down, NO, NO 2 is eliminated, and when the perchlorates are broken down - HCl, NH 3 , Cl 2 .
  • the oxidizing agent of this type is located, namely as part of the heat-absorbing charge or as a separate oxidizing charge, the gas-aerosol mixture emerging from this device thus contains toxic products.
  • the proposed device overcomes these disadvantages.
  • the technical tasks set are suggested by the Fire extinguishing device solved, consisting from a housing with an outlet opening, one of the housing walls heat-insulated combustion chamber with arranged in it pyrotechnic composition, an ignition device, a block of catalytic complete oxidation, which is designed in the form of two metallic grids, taking the space between the grids with catalytically active Aluminosilicate (e.g. zeolite granulate) is filled.
  • a complete cooling block is arranged block of the complete oxidation.
  • a space between the blocks is used to mix the fully oxidized gas phase with the solid phase of the combustion products.
  • the cooling block is in the form of at least two Grid formed, the space between them with granules of fabrics filled, selected from the group of aluminosilicates, Silica gels or their mixtures with natural or artificial Humidity.
  • the number and size of openings in the grilles that are required for the block of complete oxidation and the cooling block depends on the required outflow speed of the gas-aerosol mixture and is tested taking into account the gasodynamic resistance of these blocks found.
  • Granules in various geometric shapes (cylinders, cones) as well as in various functions of the granulate distribution in terms of size. It plays an essential role the distance between the grids, the one to be filled with granules Defines space. With a locking ring with specified In height, each pair of grids can be arranged relative to one another.
  • the device for extinguishing fires is also included a compensation unit provided in the form of an elastic Spring trained and in different areas of the Housing can be arranged.
  • This unit compensates for the linear shift of the temperature profile when burning the pyrotechnic composition and ensures a constant Distance between the maximum temperature range of the temperature profile when burning and blocking the catalytic complete oxidation.
  • the device shown in Fig. 3 has a cylindrical Housing 1 with an inside diameter of approx. 50 mm, in one, in Fig. 3 lower end a pressed pyrotechnic Composition 4 is arranged on the central one Ignition device 5 is attached. On the upper face of the Composition 4 is a spacer ring 11a with a height of 10 mm placed, the outer diameter of which essentially Corresponds to the inner diameter of the housing 1.
  • a Artificial zeolite 7 of type A (NaY) with natural Moisture are placed, the granules are spherical is (diameter of the balls 2.6 to 4.5 mm).
  • spacer ring 11a Within the spacer ring 11a is between the pyrotechnic Composition and the cooling block 6 a combustion chamber 3rd educated.
  • the combustion chamber 3 and block 7 is the housing wall with thermal insulation 12 provided.
  • a compensation unit is in shape on the upper grid 8b a steel spring 10 arranged by a spacer ring 11b surrounded by a height of 12mm, on which there is a cooling block 9 supports the two in the longitudinal direction of the housing 1 in Spaced brass grids 8c, 8d in the form of nets with a cell size of 2.0 x 2.0 mm, between which 30 g of a spherical zeolite 13 of type A (NaY) 7 with natural moisture are arranged.
  • the second embodiment shown in FIGS Device differs from the first embodiment in that two cooling blocks 9a, 9b are provided, which by a spacer ring 11d are kept at a distance.
  • in the block 6 for full oxidation are four lengthways of the housing 1 extending through channels 15 are provided.
  • in the adjacent cooling block 9a are also four in the longitudinal direction through-channels 17 of housing 1 are formed, which are offset from the channels 15.
  • the spring 10 is provided below the composition 4 in the housing 1 because the pyrotechnic composition 4 not with the walls of the Thermal protection 12 is adhesively connected.
  • the ignition device 5 is housed in a central channel of composition 4.
  • FIGS. 8 and 9 also two cooling blocks 9a, 9b are provided, between their facing grids 8d, 8e the spring 10 is arranged. channels are not formed in blocks 6 and 9a, 9b.
  • the coat 16 of the housing 1 is stiffened by ribs for thermal insulation. In the cavity between the ribs is a heat absorbent Fabric is filled, e.g. Zeolite particles.
  • the Ignition device 5 is decentrally attached to the composition.
  • the ignition device 5 ignites the pyrotechnic composition 4, which is arranged in the combustion chamber 3.
  • a hot gas-aerosol mixture is formed, consisting of a solid phase of aerosol particles (K 2 CO 3 , KHCO 3 , NH 4 HCO 3 , KNO 2 , C and others) and a gas phase (CO, CO 2 , NO, NO 2 , HCN, NH 3 , CH 4 , H 2 O).
  • the gas-aerosol mixture obtained passes through the openings of the grid 8a into the block 6 for complete catalytic oxidation, where it interacts with the granules of the aluminosilicate (zeolite) 7.
  • Solid phase particles of the gas-aerosol mixture are considerably larger than the windows in the interior cavity of the Zeolite (Fig. 1) do not flow into the cavities, but on along the zeolite surface through channels in the granules arose when pouring in.
  • Gases the molecules of which do not exceed the size of 0.4 nm (CO, CO 2 , NH 3 , NO, NO 2 ), enter the interior cavities through the windows in the zeolite structure, which are formed by oxygen atoms, where their catalytic complete oxidation also takes place at a temperature of approx. 750 ° C.
  • the gas phase and the solid phase and the stability of the Ensuring temperature conditions becomes a pyrotechnic Composition with a given function in relation on the particle size of their components and their given Mass fraction used.
  • the device To temperature fluctuations during the complete oxidation due to shifts in the maximum temperature range of the Avoid temperature profile when firing the composition, the device is provided with the steel spring 10, which by the spring force block 6 of the catalytic complete Oxidation presses on the spacer ring 11a.
  • the height the spacer ring 11a ensures a constant distance between the maximum temperature range of the temperature profile when burning the composition and the block 6 of the catalytic complete oxidation.
  • Block 6 follows during the combustion of the composition of catalytic complete oxidation slowly shifting temperature profile. Block 6 thus remains catalytic complete oxidation constantly in the maximum temperature range until the end of the firing process of the composition.
  • the cooling block 9 is fixed in the housing 1 via the Spacer rings 11a, b, c.
  • the security film 14 e.g. out Aluminum foil can exist
  • a pyrotechnic composition with progressive Firing form e.g. cylinders with one or more Channels of different geometry; two or more cylinders one Diameter; two or more cylinders of different diameters; in the manner of "tube in tube” and the like
  • the block 6 can complete oxidation and the cooling block 9 with additional Channels 15 are provided (Fig. 6, 7), the pressure reduction and serve a safe operation of the device.
  • the fire extinguishing device of Fig. 3 becomes Prepared to extinguish a test fire.
  • 100 g of a pyrotechnic composition taken to the Preparation 18.33 g of a 60% mixture of phenol-formaldehyde resin in ethyl alcohol in a paddle mixer are given.
  • the proportion of phenol-formaldehyde resin is so 11.0 g.
  • the solution is put up in a reactor with a water jacket heated to + 50 ° C and processed in a mixer that at a speed of 85 revolutions per minute rotates.
  • the duration of the dissolution in ethylene alcohol is one Hour.
  • the finished solution does not contain any clot from either dissolved resin.
  • the mixture obtained is placed in a granulator, which with calibration chambers with a diameter of 1.5 mm is provided. After the mixture has passed through the calibration chambers you get a granulate of the mixture with a Length of 3 mm and the following mass ratio of the components: Potassium nitrate 70 ⁇ 0.5% of the mass, diziandiamide - 19 ⁇ 0.5% of the Mass, phenol-formaldehyde resin - 11 ⁇ 0.5% of the mass.
  • the granules obtained are placed in troughs which are in a Drying cabinet can be arranged at a temperature of + 45 ° C. During drying, which lasts 4 hours the content of the remaining volatile constituents is not 0.8% the crowd.
  • the composition is formed from the granules obtained by compression molding at a specific pressure of 1000 kp / cm 2 (100 MPa).
  • the pressing is carried out by pressing in once at a speed of 0.003 m / s, followed by holding under pressure for 5 seconds in a cylindrical heat protection made of paper with a wall thickness of 1.5 mm.
  • the pyrotechnic composition 4 a cylindrical channelless shape with a diameter of 50 mm and a recess in its central part in which a standard ignition device 5 is placed with a mass of 1 g.
  • the device is further assembled according to Figure 3.
  • the composite fire extinguishing device was used to extinguish gasoline to simulate a fire in manufacturing rooms.
  • the volume of the space to be protected was 2.5 m 3 per 100 g of the pyrotechnic composition.
  • Burning rate of the pyrotechnic composition mass fraction the solid phase of the aerosol, mass fraction of the Particles of size 1 to 2 ⁇ m in aerosol, fire extinguishing Concentration, firing temperature of the composition, as well as the Temperature of the housing, both at the outlet opening also at a distance of 200 mm from the outlet opening (The measurement was carried out using a thermoelectric contact method with Chromel-Alumel thermocouples with a soldering diameter of 100 ⁇ m).
  • the content analysis of the toxic products in the gas-aerosol mixture was carried out by taking samples via air lines, which were arranged in the middle part of the test chamber.
  • nitrogen oxides and cyanides became the gas phase over a collecting container filled with water with glass filter for 10 minutes with a pressure mixer mixed, at a rate of 2 l / min.
  • the ammonia was determined by a colorimetric method, via the product of the interaction with a Nessler reagent.
  • the lowest measurement limit in relation to the sample amount (2 ml) was 2 ⁇ g, which corresponds to a concentration of 0.5 mg / m 3 .
  • the nitrogen oxide was determined by a colorimetric method, via the product of the interaction with a Griess-Ilosvay reagent.
  • the lowest measurement limit in relation to the sample amount (2 ml) was 0.3 ⁇ g, which corresponds to a concentration of 0.075 mg / m 3 .
  • Cyanides were determined by a colorimetric method, via the reaction of the formation of iron rhodanide.
  • the lowest measurement limit in relation to the sample amount (5 ml) was 2 ⁇ g, which corresponds to a concentration of 0.1 mg / m 3 .
  • composition, burning rate and fire extinguishing characteristics of the invention and the closest prior art Name of the components in the composition Component quantity in% of the mass in the invention with a predetermined distribution function of the component particles by size Component quantity according to the patent RU 2 101 054 Potassium nitrate 70 70 dicyandiamide 19 19 Phenol-formaldehyde resin 11 11 Burning speed in mm / s 3.2 2.1 Fire extinguishing characteristics of the devices (modifications) of the invention Fig.2 Figure 3 Figure 4 Patent RU-2 101 054 Solid phase outlet of the gas-aerosol mixture,% 70 69 71 57 Mass fraction of the particles 1-2 ⁇ m in solid phase,% 68 70 69 64 Fire extinguishing effectiveness, g / m 3 36 38 34 40 Temperature, ° C Casing, 62 69 60 - Outlet opening, 320 370 325 - at a distance of 200 mm 115
  • a wide raw material base of the component used, the simplicity and reliability of the proposed method and the device are criteria for a wide industrial Speak applicability.
  • the advantages of the proposed method and the device for its implementation are: low temperature and Toxicity of the fire extinguishing gas aerosol mixture, which in given the space to be protected, the lack of flames and sparks while maintaining high fire-extinguishing effectiveness.

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  • Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Emergency Management (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Business, Economics & Management (AREA)
  • Veterinary Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Surgery (AREA)
  • Air Bags (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Fire-Extinguishing Compositions (AREA)
  • Fire-Extinguishing By Fire Departments, And Fire-Extinguishing Equipment And Control Thereof (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
EP99113153A 1998-07-30 1999-07-07 Verfahren und Vorrichtung zum Löschen von Bränden Expired - Lifetime EP0976423B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
RU98113952/12A RU2147903C1 (ru) 1998-07-30 1998-07-30 Состав для получения пиротехнического аэрозолеобразующего состава для тушения пожаров и способ получения пиротехнического аэрозолеобразующего состава для тушения пожаров
RU98113952 1998-07-30
RU98122276/12A RU2142306C1 (ru) 1998-12-15 1998-12-15 Способ пожаротушения и устройство для его осуществления
RU98122276 1998-12-15

Publications (2)

Publication Number Publication Date
EP0976423A1 EP0976423A1 (de) 2000-02-02
EP0976423B1 true EP0976423B1 (de) 2004-10-06

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EP99113153A Expired - Lifetime EP0976423B1 (de) 1998-07-30 1999-07-07 Verfahren und Vorrichtung zum Löschen von Bränden

Country Status (8)

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US (1) US6089326A (no)
EP (1) EP0976423B1 (no)
AU (1) AU750077B2 (no)
BR (1) BR9903251A (no)
CA (1) CA2276382C (no)
DE (2) DE19909083C2 (no)
NO (1) NO318285B1 (no)
SA (1) SA99200480B1 (no)

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AU750077B2 (en) 2002-07-11
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BR9903251A (pt) 2000-04-18
AU4105299A (en) 2000-02-24
SA99200480B1 (ar) 2006-10-11
NO318285B1 (no) 2005-02-28
NO992765L (no) 2000-01-31
US6089326A (en) 2000-07-18
EP0976423A1 (de) 2000-02-02
DE59910706D1 (de) 2004-11-11
CA2276382A1 (en) 2000-01-30
DE19909083C2 (de) 2002-03-14
CA2276382C (en) 2007-12-11

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