EP1890986B1 - Pyrotechnic agent - Google Patents

Pyrotechnic agent Download PDF

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Publication number
EP1890986B1
EP1890986B1 EP06763483A EP06763483A EP1890986B1 EP 1890986 B1 EP1890986 B1 EP 1890986B1 EP 06763483 A EP06763483 A EP 06763483A EP 06763483 A EP06763483 A EP 06763483A EP 1890986 B1 EP1890986 B1 EP 1890986B1
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EP
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Prior art keywords
agent according
pyrotechnic agent
azotetrazolate
nitrate
pyrotechnic
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EP06763483A
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German (de)
French (fr)
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EP1890986A1 (en
Inventor
Ulrich Bley
Rainer Hagel
Julia Havlik
Aleksej Hoschenko
Peter Simon Lechner
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RWS GmbH
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RUAG Ammotec GmbH
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
    • C06C9/00—Chemical contact igniters; Chemical lighters
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
    • C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids

Definitions

  • Pyrotechnic agents in the context of the invention are substances or mixtures of substances which can develop a pyrotechnic effect.
  • the subject of the present invention is a pyrotechnic agent which can be used as a thermal ignition agent.
  • thermal pre-ignition agents are, for example, safety systems, preferably thermal fuses in gas generators or separating elements for batteries.
  • security systems are again preferably used in motor vehicles.
  • Thermal pre-ignition agents are pyrotechnic substances or mixtures which, inter alia, have the task of controlling the usually very thermally stable gas-generating mixtures of the gas generator in the event of a vehicle fire.
  • thermal preignition agents are the use as a pyrotechnic set in separators, preferably for battery terminals. These separators should interrupt the power supply in case of fire, especially a vehicle fire, or in a motor vehicle accident in which the gas generator is triggered.
  • thermal thermal ignition agents are nitrocellulose, propellant powders derived therefrom or those disclosed in the patent application DE 197 30 873 A1 used mixtures based on nitrotriazolone and guanidine nitrate. These mixtures show ignition temperatures of about 160 Ā° C and are insufficiently long-term stability in the case of nitrocellulose.
  • Object of the present invention was to provide a pyrotechnic agent having an ignition temperature of 180 Ā° C and sufficient long-term stability. Another object of the present invention was to provide a pyrotechnic agent that can be used as a thermal ignition agent for gas generators in automotive safety systems. A Another object of the present invention was to provide a pyrotechnic agent that can be used in battery terminal isolators.
  • azotetrazolates are used as component according to the invention.
  • the azotetrazolate component used here is amino guanandine 5,5'-azotetrazolate (C 4 H 14 N 18 ), AGATZ for short, and guanidine 5,5'-azotetrazolate (C 4 , H 12 N 16 ), short GATZ.
  • the US-A-6007,647 offers thermal pre-ignition agents containing GATZ and two oxidants.
  • the azotetrazolate components may be used either alone or in mixtures with each other and / or with other components.
  • the structural formulas of AGATZ and GATZ are as follows:
  • Aminoguanine 5,5'-azotetrazolate (C 4 H 14 N 18 , AGATZ).
  • Guanidine 5,5'-azotetrazolate (C 4 , H 12 N 16 , GATZ).
  • the deflagration point of the pure AGATZ is 209 Ā° C, that of the GATZ is 240 Ā° C.
  • the deflagration temperatures in the range of 165 Ā° C to 195 Ā° C can be controlled and the deflagration temperatures of the mixtures can be lower than that of the individual components.
  • the production and processing takes place according to known and customary methods. These include, for example, kneading, extrusion, extrusion, tabletting or granulation.
  • Table 2 shows the deflagration points, friction and impact sensitivities of the mixtures.
  • the measurement of the friction and impact sensitivities was carried out according to methods of the Federal Institute for Materials Research (BAM), while the measurement of the deflagration points was carried out with the thermogravimetric analysis (Mettler) at a heating rate of 10 Ā° C. per minute.
  • Table 3 summarizes the weight losses and deflagration points after thermal stress (24 h, 125 Ā° C and 400 h, 110 Ā° C) of some of the mixtures selected from the examples.
  • the weight loss was measured analogously to the Holland test.
  • the measurement of the deflagration points was carried out by thermogravimetric analysis (Mettler) at a heating rate of 10 Ā° C per minute.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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Description

Pyrotechnische Mittel im Sinne der Erfindung sind Stoffe oder Stoffgemische, die eine pyrotechnische Wirkung entfalten kƶnnen.Pyrotechnic agents in the context of the invention are substances or mixtures of substances which can develop a pyrotechnic effect.

Insbesondere Gegenstand der vorliegenden Erfindung ist ein pyrotechnisches Mittel, das als thermisches FrĆ¼hzĆ¼ndmittel eingesetzt werden kann.In particular, the subject of the present invention is a pyrotechnic agent which can be used as a thermal ignition agent.

Anwendungsbereiche solcher thermischen FrĆ¼hzĆ¼ndmittel sind beispielsweise Sicherheitssysteme, vorzugsweise thermische Sicherungen in Gasgeneratoren oder Trennelemente fĆ¼r Batterien. Solche Sicherheitssysteme werden wiederum vorzugsweise in Kraftfahrzeugen eingesetzt.Areas of application of such thermal pre-ignition agents are, for example, safety systems, preferably thermal fuses in gas generators or separating elements for batteries. Such security systems are again preferably used in motor vehicles.

Thermische FrĆ¼hzĆ¼ndmittel sind pyrotechnische Substanzen bzw. Mischungen, die unter anderem die Aufgabe haben, die in der Regel thermisch sehr stabilen Gas erzeugenden Mischungen des Gasgenerators im Falle eines Fahrzeugbrandes kontrolliert anzuzĆ¼nden.Thermal pre-ignition agents are pyrotechnic substances or mixtures which, inter alia, have the task of controlling the usually very thermally stable gas-generating mixtures of the gas generator in the event of a vehicle fire.

Ein anderes Anwendungsbeispiel thermischer FrĆ¼hzĆ¼ndmittel ist die Verwendung als pyrotechnischer Satz in Trennelementen, vorzugsweise fĆ¼r Batterieklemmen. Diese Trennelemente sollen im Falle eines Brandes, insbesondere eines Fahrzeugbrandes, oder bei einem Kraftfahrzeugunfall, bei dem der Gasgenerator ausgelƶst wird, die Stromversorgung unterbrechen.Another application of thermal preignition agents is the use as a pyrotechnic set in separators, preferably for battery terminals. These separators should interrupt the power supply in case of fire, especially a vehicle fire, or in a motor vehicle accident in which the gas generator is triggered.

Als thermische FrĆ¼hzĆ¼ndmittel werden beispielsweise Nitrocellulose, daraus abgeleitete Treibladungspulver oder die in der Patentanmeldung DE 197 30 873 A1 beschriebenen Mischungen auf Basis von Nitrotriazolon und Guanidinnitrat eingesetzt. Diese Mischungen zeigen EntzĆ¼ndungstemperaturen von ca. 160Ā°C und sind im Falle der Nitrocellulose nur unzureichend langzeitstabil.Examples of thermal thermal ignition agents are nitrocellulose, propellant powders derived therefrom or those disclosed in the patent application DE 197 30 873 A1 used mixtures based on nitrotriazolone and guanidine nitrate. These mixtures show ignition temperatures of about 160 Ā° C and are insufficiently long-term stability in the case of nitrocellulose.

Aufgabe der vorliegenden Erfindung war die Bereitstellung eines pyrotechnischen Mittels mit einer EntzĆ¼ndungstemperatur um 180Ā°C und ausreichender LangzeitstabilitƤt. Eine weitere Aufgabe der vorliegenden Erfindung war die Bereitstellung eines pyrotechnischen Mittels, das als thermisches FrĆ¼hzĆ¼ndmittel fĆ¼r Gasgeneratoren in Kraftfahrzeugsicherheitssystemen eingesetzt werden kann. Eine weitere Aufgabe der vorliegenden Erfindung war die Bereitstellung eines pyrotechnischen Mittels, das in Trennelementen fĆ¼r Batterieklemmen eingesetzt werden kann.Object of the present invention was to provide a pyrotechnic agent having an ignition temperature of 180 Ā° C and sufficient long-term stability. Another object of the present invention was to provide a pyrotechnic agent that can be used as a thermal ignition agent for gas generators in automotive safety systems. A Another object of the present invention was to provide a pyrotechnic agent that can be used in battery terminal isolators.

ErfindungsgemƤƟ wird diese Aufgabe Ć¼berraschenderweise durch die Merkmale des Hauptanspruchs gelƶst. Vorzugsweise Ausgestaltungen finden sich in den UnteransprĆ¼chen. Dabei werden erfindungsgemƤƟ Azotetrazolate als Komponente eingesetzt. Insbesondere werden dabei als Azotetrazolatkomponente Aminoguandin-5,5'-azotetrazolat (C4H14N18), kurz AGATZ, und Guanidin-5,5'-azotetrazolat (C4,H12N16), kurzGATZ, eingesetzt. Die US-A-6007 647 offerbart thermische FrĆ¼hzĆ¼ndmittel, die GATZ und zwei Oxidationsmittel enthalten.According to the invention, this object is surprisingly achieved by the features of the main claim. Preferred embodiments can be found in the subclaims. In this case, azotetrazolates are used as component according to the invention. In particular, the azotetrazolate component used here is amino guanandine 5,5'-azotetrazolate (C 4 H 14 N 18 ), AGATZ for short, and guanidine 5,5'-azotetrazolate (C 4 , H 12 N 16 ), short GATZ. The US-A-6007,647 offers thermal pre-ignition agents containing GATZ and two oxidants.

Die Azotetrazolatkomponenten kƶnnen entweder alleine oder in Mischungen untereinander und/oder mit weiteren Komponenten verwendet werden. Die Strukturformeln von AGATZ und GATZ sind wie folgt:

Figure imgb0001
Figure imgb0002
 The azotetrazolate components may be used either alone or in mixtures with each other and / or with other components. The structural formulas of AGATZ and GATZ are as follows:
Figure imgb0001
Figure imgb0002

Aminoguandin-5,5'-azotetrazolat (C4H14N18, AGATZ).

Figure imgb0003
Aminoguanine 5,5'-azotetrazolate (C 4 H 14 N 18 , AGATZ).
Figure imgb0003

Guanidin-5,5'-azotetrazolat (C4,H12N16, GATZ).Guanidine 5,5'-azotetrazolate (C 4 , H 12 N 16 , GATZ).

Der Verpuffungspunkt des reinen AGATZ betrƤgt 209Ā°C, der des GATZ betrƤgt 240Ā°C.The deflagration point of the pure AGATZ is 209 Ā° C, that of the GATZ is 240 Ā° C.

Ɯberraschenderweise wurde gefunden, dass sich bei Mischungen von AGATZ und/oder GATZ und/oder ausgewƤhlten Komponenten die Verpuffungstemperaturen im Bereich von 165Ā°C bis 195Ā°C steuern lassen und die Verpuffungstemperaturen der Mischungen tiefer liegen kƶnnen als die der Einzelkomponenten.Surprisingly, it has been found that in blends of AGATZ and / or GATZ and / or selected components, the deflagration temperatures in the range of 165 Ā° C to 195 Ā° C can be controlled and the deflagration temperatures of the mixtures can be lower than that of the individual components.

FĆ¼r FrĆ¼hzĆ¼ndmittel sind Verpuffungstemperaturen unter 200Ā°C besonders interessant. Die erfindungsgemƤƟen pyrotechnischen Mittel erfĆ¼llen diese Forderung bei ausgezeichneter LangzeitstabilitƤt.For FrĆ¼hzĆ¼ndmittel deflagration temperatures below 200 Ā° C are particularly interesting. The pyrotechnic compositions according to the invention meet this requirement with excellent long-term stability.

Als Zusatzstoffe kƶnnen verwendet werden:

  • 1. Oxidationsmittel (einzeln oder in Mischungen) Nitrate der Alkali- oder Erdalkalimetalle oder des Ammoniums wie Natrium-, Kalium- oder Ammoniumnitrat, Perchlorate der Alkali- oder Erdalkalimetalle oder des Ammoniums, Peroxide der Alkali- oder Erdalkalimetalle oder des Zinks.
  • 2. Stickstoffhaltige Verbindungen (einzeln oder in Mischungen) Ammoniumpikrat, Aminoguanidiniumpikrat, Guanidiniumpikrat, Aminoguanidiniumstyphnat, Guanidiniumstyphnat, Nitroguanidin, Nitroaminoguanidin, Aminoguanidinnitrat, Diaminoguanidinnitrat, Triaminoguanidinnitrat, Guanidinnitrat, Dicyandiamidinnitrat.
  • 3. Energiereiche ZuschlƤge (einzeln oder in Mischungen) Hexogen, Oktogen , Nitrocellulose.
  • 4. Reduktionsmittel (einzeln oder in Mischungen) Aluminium, Titan, Titanhydrid, Bor, Borhydrid, Zirkon, Zirkonhydrid, Silicium, Graphit, Aktivkohle, RuƟ.
  • 5. Bindemittel (einzeln oder in Mischungen) Cellulose sowie deren Derivate, Polyvinylbutyrale, Polynitropolyphenylen, Polynitrophenylether, Plexigum, Polyvinylacetat, Copolymere.
  • 6. Abbrandmoderatoren, Stabilisatoren und Verarbeitungshilfen (einzeln oder in Mischungen) Ferrocen und Derivate, Acetonylacetate, Salicylate, Bariumcarbonat, Strontiumcarbonat, Magnesiumcarbonat, Melamin, Zinkoxid, Zinkcarbonat, Silikate, Kieselgele, KieselsƤuren, beispielsweise Aerosil (Fa. Degussa), Bornitrid.
As additives can be used:
  • 1. Oxidizing agents (individually or in mixtures) nitrates of alkali or alkaline earth metals or ammonium such as sodium, potassium or ammonium nitrate, perchlorates of alkali or alkaline earth metals or ammonium, peroxides of alkali or alkaline earth metals or zinc.
  • 2. Nitrogen- containing compounds (individually or in mixtures) ammonium picrate, aminoguanidinium picrate, guanidinium picrate, aminoguanidinium stannate, guanidinium styrenate, nitroguanidine, nitroaminoguanidine, aminoguanidine nitrate, diaminoguanidine nitrate, triaminoguanidine nitrate, guanidine nitrate, dicyandiamide nitrate.
  • 3. High-energy additives (singly or in mixtures) Hexogen, octogen, nitrocellulose.
  • 4. Reducing agents (individually or in mixtures) aluminum, titanium, titanium hydride, boron, borohydride, zirconium, zirconium hydride, silicon, graphite, activated carbon, carbon black.
  • 5. Binders (individually or in mixtures) cellulose and derivatives thereof, polyvinyl butyrals, polynitropolyphenylene, polynitrophenyl ethers, plexigum, polyvinyl acetate, copolymers.
  • 6. Abbrand moderators , stabilizers and processing aids (individually or in mixtures) ferrocene and derivatives, acetonyl acetates, salicylates, barium carbonate, strontium carbonate, magnesium carbonate, melamine, zinc oxide, zinc carbonate, silicates, silica gels, silicas, for example Aerosil (Degussa), boron nitride.

Die Herstellung und Verarbeitung findet nach an sich bekannten und Ć¼blichen Verfahren statt. Hierzu zƤhlen beispielsweise Kneten, Extrudieren, Strangpressen, Tablettieren oder Granulieren.The production and processing takes place according to known and customary methods. These include, for example, kneading, extrusion, extrusion, tabletting or granulation.

Gegenstand der vorliegenden Erfindung ist im Einzelnen:

  • ein pyrotechnisches Mittel, wobei die Azotetrazolatkomponente ausgewƤhlt ist aus Aminoguandin-5,5'-azotetrazolat (AGATZ) und Guanidin-5,5'-azotetrazolat (GATZ) oder Mischungen aus beiden;
  • ein pyrotechnisches Mittel, wobei der Anteil der Azotetrazolatkomponente 20 bis 50 Gew.-% beitrƤgt;
  • ein pyrotechnisches Mittel, das 50 bis 80 Gew.-% eines Zusatzstoffes oder Mischungen mehrerer Zusatzstoffe enthƤlt;
  • ein pyrotechnisches Mittel, wobei die Zusatzstoffe ausgewƤhlt sind aus: Ammoniumpikrat, Aminoguanidiniumpikrat, Guanidiniumpikrat, Aminoguanidiniumstyphnat, Guanidiniumstyphnat, Nitroguanidin, Nitroaminoguanidin, Aminoguanidinnitrat, Diaminoguanidinnitrat, Triaminoguanidinnitrat, Guanidinnitrat, Dicyandiamidinnitrat, Nitrate der Alkali- und/oder Erdalkalimetalle und/oder des Ammoniums, Perchlorate der Alkali- und/oder Erdalkalimetalle und/oder des Ammoniums, Peroxide der Alkali- und/oder der Erdalkalimetalle und/oder des Zinks; Aluminium, Titan, Titanhydrid, Bor, Borhydrid, Zirkon, Zirkonhydrid, Silicium, Graphit, Aktivkohle, RuƟ; Cellulose und/oder deren Derivate, Polyvinylbutyrale, Polynitropolyphenylen, Polynitrophenylether, Plexigum, Polyvinylacetat und Copolymere; Hexogen, Oktogen; Ferrocen und/oder deren Derivate, Acetonylacetate, Salicylate, Bariumcarbonat, Strontiumcarbonat, Magnesiumcarbonat, Melamin, Zinkoxid, Zinkcarbonat, Silikate, Kieselgele, KieselsƤuren, beispielsweise Aerosil (Fa. Degussa), Bornitrid;
  • ein pyrotechnisches Mittel, das 30 bis 60 Ges.-% eines Oxidationsmittels enthƤlt;
  • ein pyrotechnisches Mittel, wobei das Oxidationsmittel ausgewƤhlt ist aus einem oder mehreren der Nitrate der Alkali- und/oder Erdalkalimetalle und/oder des Ammoniums, der Perchlorate der Alkali- und/oder Erdalkalimetalle und/oder des Ammoniums, der Peroxide der Alkali- und/oder Erdalkalimetalle und/oder des Zinks;
  • ein pyrotechnisches Mittel, das 15 bis 40 Gew.-% einer stickstoffhaltigen Verbindung enthƤlt;
  • ein pyrotechnisches Mittel, wobei die stickstoffhaltige Verbindung ausgewƤhlt ist aus einem oder mehreren von Ammoniumpikrat, Aminoguanidiniumpikrat, Guanidiniumpikrat, Aminoguanidiniumstyphnat, Guanidiniumstyphnat, Nitroguanidin, Nitroaminoguanidin, Aminoguanidinnitrat, Diaminoguanidinnitrat, Triaminoguanidinnitrat, Guanidinnitrat, Dicyandiamidinnitrat,
  • ein pyrotechnisches Mittel, das 1 bis 40 Gew.-% energetische ZusƤtze enthƤlt;
  • ein pyrotechnisches Mittel, wobei die energetischen ZusƤtze ausgewƤhlt sind aus einem oder mehreren von Hexogen, Oktogen und/oder Nitrocellulose;
  • ein pyrotechnisches Mittel, das 1 bis 15 Gew.-% eines Reduktionsmittel enthƤlt;
  • ein pyrotechnisches Mittel, wobei das Reduktionsmittel ausgewƤhlt ist aus einem oder mehreren von Aluminium, Titan, Titanhydrid, Bor, Borhydrid, Zirkon, Zirkonhydrid, Silicium, Graphit, Aktivkohle, RuƟ;
  • ein pyrotechnisches Mittel, das 1 bis 20 Gew.-% eines Bindemittels enthƤlt;
  • ein pyrotechnisches Mittel, wobei das Bindemittel ausgewƤhlt ist aus einem oder mehreren von Cellulose und deren Derivaten, Polyvinylbutyrale, Polynitropolyphenylen, Polynitrophenylether, Plexigum, Polyvinylacetat und Copolymeren;
  • ein pyrotechnisches Mittel, das 0,1 bis 15 Gew.-%, bevorzugt 1 bis 10 Gew.-% Abbrandmoderatoren, Stabilisatoren und Verarbeitungshilfen enthƤlt;
  • ein pyrotechnisches Mittel, wobei die Abbrandmoderatoren und Verarbeitungshilfen ausgewƤhlt sind aus einem oder mehreren von Ferrocen und dessen Derivaten, Acetonylacetaten, Salicylate, Bariumcarbonat, Strontiumcarbonat, Magnesiumcarbonat, Melamin, Zinkoxid, Zinkcarbonat, Silikate, Kieselgele, KieselsƤuren, beispielsweise Aerosil (Fa. Degussa), und/oder Bornitrid;
  • Verwendung des erfindungsgemƤƟen pyrotechnischen Mittels als thermisches FrĆ¼hzĆ¼ndmittel;
  • Verwendung des erfindungsgemƤƟen pyrotechnischen Mittels als thermische Sicherung;
  • Verwendung des erfindungsgemƤƟen pyrotechnischen Mittels in Kraftfahrzeugsicherheitssystemen;
  • Verwendung des erfindungsgemƤƟen pyrotechnischen Mittels in Gasgeneratoren;
  • Verwendung des erfindungsgemƤƟen pyrotechnischen Mittels in Trennelementen, vorzugsweise fĆ¼r Batterieklemmen.
The subject of the present invention is in detail:
  • a pyrotechnic agent, wherein the azotetrazolate component is selected from aminoguanidine 5,5'-azotetrazolate (AGATZ) and guanidine 5,5'-azotetrazolate (GATZ) or mixtures of both;
  • a pyrotechnic agent, wherein the proportion of the azotetrazolate component contributes from 20 to 50% by weight;
  • a pyrotechnic agent containing from 50 to 80% by weight of an additive or mixtures of several additives;
  • a pyrotechnic agent, wherein the additives are selected from: ammonium picrate, aminoguanidinium picrate, guanidinium picrate, aminoguanidinium typhnate, guanidinium typhnate, nitroguanidine, nitroaminoguanidine, aminoguanidine nitrate, diaminoguanidine nitrate, triaminoguanidine nitrate, guanidine nitrate, dicyandiamide nitrate, nitrates of alkali and / or alkaline earth metals and / or ammonium, perchlorates the alkali and / or alkaline earth metals and / or ammonium, peroxides of the alkali and / or alkaline earth metals and / or zinc; Aluminum, titanium, titanium hydride, boron, borohydride, zirconium, zirconium hydride, silicon, graphite, activated carbon, carbon black; Cellulose and / or derivatives thereof, polyvinyl butyrals, polynitropolyphenylene, polynitrophenyl ethers, plexigum, polyvinyl acetate and copolymers; Hexogen, octogen; Ferrocene and / or derivatives thereof, acetonylacetates, salicylates, barium carbonate, strontium carbonate, magnesium carbonate, melamine, zinc oxide, zinc carbonate, silicates, silica gels, silicas, for example Aerosil (Degussa), boron nitride;
  • a pyrotechnic agent containing 30 to 60% by weight of an oxidizing agent;
  • a pyrotechnic agent, wherein the oxidizing agent is selected from one or more of the nitrates of the alkali and / or alkaline earth metals and / or ammonium, the perchlorates of the alkali and / or alkaline earth metals and / or ammonium, the peroxides of the alkali and / or or alkaline earth metals and / or zinc;
  • a pyrotechnic agent containing 15 to 40% by weight of a nitrogen-containing compound;
  • a pyrotechnic agent, said nitrogenous compound selected from one or more of ammonium picrate, aminoguanidinium picrate, guanidinium picrate, aminoguanidinium styrenate, guanidinium styrenate, nitroguanidine, nitroaminoguanidine, aminoguanidine nitrate, diaminoguanidine nitrate, triaminoguanidine nitrate, guanidine nitrate, dicyandiamide nitrate,
  • a pyrotechnic agent containing 1 to 40% by weight of energetic additives;
  • a pyrotechnic agent, wherein the energetic additives are selected from one or more of hexogen, octogen and / or nitrocellulose;
  • a pyrotechnic agent containing 1 to 15% by weight of a reducing agent;
  • a pyrotechnic agent, wherein the reducing agent is selected from one or more of aluminum, titanium, titanium hydride, boron, borohydride, zirconium, zirconium hydride, silicon, graphite, activated carbon, carbon black;
  • a pyrotechnic agent containing 1 to 20% by weight of a binder;
  • a pyrotechnic agent, wherein the binder is selected from one or more of cellulose and its derivatives, polyvinyl butyrals, polynitropolyphenylene, polynitrophenyl ether, plexigum, polyvinyl acetate and copolymers;
  • a pyrotechnic agent containing from 0.1% to 15%, preferably from 1% to 10%, by weight of burn moderators, stabilizers and processing aids;
  • a pyrotechnic agent, wherein the Abbrandmoderatoren and processing aids are selected from one or more of ferrocene and its derivatives, acetonyl acetates, salicylates, barium carbonate, strontium carbonate, magnesium carbonate, melamine, zinc oxide, zinc carbonate, silicates, silica gels, silicic acids, for example Aerosil (Degussa) , and / or boron nitride;
  • Use of the pyrotechnic agent according to the invention as thermal pre-ignition agent;
  • Use of the pyrotechnic agent according to the invention as a thermal fuse;
  • Use of the pyrotechnic agent according to the invention in motor vehicle safety systems;
  • Use of the pyrotechnic agent according to the invention in gas generators;
  • Use of the pyrotechnic agent according to the invention in separating elements, preferably for battery terminals.

Die Erfindung wird durch die folgenden Beispiele nƤher erlƤutert, ohne sie darauf einzuschrƤnken:

  • In Tabelle 1 sind die Zusammensetzungen von 27 verschiedenen Mischungen des pyrotechnischen Mittels aufgefĆ¼hrt. Die Komponenten wurden in den angegebenen GewichtsverhƤltnissen (Angaben in Gewichtsprozent (Gew.-%)) in PlastikbehƤlter eingewogen und 30 Minuten im Taumelmischer homogenisiert.
Tabelle 1: Mischungen Mischung AGATZ (GATZ) Hexogen Oktogen Aminoguanidiniumpikrat Andere Natriumnitrat Kaliumnitrat 1 * 30 20 50 2 * 30 20 50 3 30 30 40 4 30 10 20 40 5 30 10 20 40 6 30 10 AGSt 20 40 7 30 10 20 40 8 30 10 AGSt 20 40 9 30 GPik 10 AGSt 20 40 10 30 GPik 30 40 11 30 20 AGSt 10 40 12 30 30 40 13 * 30 30 40 14 * 30 30 40 15 30 AGSt 30 40 16 30 10 GPik 20 40 17 30 10 Nigu 20 40 18 30 AGSt 30 40 19 30 10 GSt 20 40 20 GATZ 30 AGSt 30 40 21 GATZ 30 30 40 22 GATZ 30 10 AGSt 20 40 23 30 AGSt 10 APik 20 40 24 30 20 APik 10 40 25 30 APik 30 40 26 30 10 GPik 20 40 27 30 10 GPik 20 40 AGSt: Aminoguanidiniumstyphnat
GPik: Guanidiniumpikrat
Nigu: Nitroguanidin
APik: Ammoniumpikrat
* Vergleichsbeispiel The invention is explained in more detail by the following examples, without limiting them:
  • Table 1 lists the compositions of 27 different pyrotechnic agent blends. The components were weighed in the stated weight ratios (in percent by weight (% by weight)) in plastic containers and homogenized for 30 minutes in a tumble mixer.
Table 1: Mixtures mixture AGATZ (GATZ) hexogen Oktogen Aminoguanidiniumpikrat Other sodium nitrate potassium nitrate 1 * 30 20 50 2 * 30 20 50 3 30 30 40 4 30 10 20 40 5 30 10 20 40 6 30 10 AGSt 20 40 7 30 10 20 40 8th 30 10 AGSt 20 40 9 30 GPik 10 AGSt 20 40 10 30 GPik 30 40 11 30 20 AGSt 10 40 12 30 30 40 13 * 30 30 40 14 * 30 30 40 15 30 AGSt 30 40 16 30 10 GPik 20 40 17 30 10 Nigu 20 40 18 30 AGSt 30 40 19 30 10 GSt 20 40 20 GATZ 30 AGSt 30 40 21 GATZ 30 30 40 22 GATZ 30 10 AGSt 20 40 23 30 AGSt 10 APik 20 40 24 30 20 APik 10 40 25 30 APik 30 40 26 30 10 GPik 20 40 27 30 10 GPik 20 40 AGSt: aminoguanidinium typhnate
GPik: guanidinium picrate
Nigu: nitroguanidine
APik: ammonium picrate
* Comparative Example

In Tabelle 2 sind die Verpuffungspunkte, Reib- und Schlagempfindlichkeiten der Mischungen dargestellt. Die Messung der Reib- und Schlagempfindlichkeiten erfolgte nach Methoden der Bundesanstalt fĆ¼r Materialforschung (BAM), wƤhrend die Messung der Verpuffungspunkte mit der Thermogravimetrie-Analyse (Fa. Mettler) bei einer Aufheizrate von 10Ā°C pro Minute erfolgte. Tabelle 2: Ɯbersicht der Verpuffungstemperaturen, Reib- und Schlagempfindlichkeiten Mischung Verpuffungstemperatur [Ā°C] Reibempfindlichkeit [N] Schlagempfindlichkeit [J] 1 * 180 240 3 2 * 190 240 3 3 182 >360 4 4 165 240 3 5 172 360 2 6 190 >360 2 7 172 >360 2 8 172 >360 4 9 181 >360 5 10 192 >360 8 11 178 >360 6 12 182 >360 4 13 * 221 360 2 14 * 217 240 3 15 172 >360 6 16 192 >360 5 17 191 >360 6 18 174 >360 6 19 182 >360 10 20 181 >360 8 21 195 >360 10 22 180 >360 4 23 180 >360 5 24 180 >360 4 25 175 >360 3 26 175 >360 2 27 180 >360 3 *Vergleichsbeispiel Table 2 shows the deflagration points, friction and impact sensitivities of the mixtures. The measurement of the friction and impact sensitivities was carried out according to methods of the Federal Institute for Materials Research (BAM), while the measurement of the deflagration points was carried out with the thermogravimetric analysis (Mettler) at a heating rate of 10 Ā° C. per minute. Table 2: Overview of the deflagration temperatures, friction and impact sensitivities mixture Deflagration temperature [Ā° C] Friction sensitivity [N] Blow sensitivity [J] 1 * 180 240 3 2 * 190 240 3 3 182 > 360 4 4 165 240 3 5 172 360 2 6 190 > 360 2 7 172 > 360 2 8th 172 > 360 4 9 181 > 360 5 10 192 > 360 8th 11 178 > 360 6 12 182 > 360 4 13 * 221 360 2 14 * 217 240 3 15 172 > 360 6 16 192 > 360 5 17 191 > 360 6 18 174 > 360 6 19 182 > 360 10 20 181 > 360 8th 21 195 > 360 10 22 180 > 360 4 23 180 > 360 5 24 180 > 360 4 25 175 > 360 3 26 175 > 360 2 27 180 > 360 3 * Comparative Example

In Tabelle 3 sind die Gewichtsverluste und Verpuffungspunkte nach thermischer Belastung (24 h, 125Ā°C und 400 h, 110Ā°C) einiger aus den Beispielen ausgewƤhlter Mischungen zusammengefasst. Die Messung des Gewichtsverlustes erfolgte analog dem Holland Test. Die Messung der Verpuffungspunkte erfolgte mit der Thermogravimetrie-Analyse (Fa. Mettler) bei einer Aufheizrate von 10Ā°C pro Minute.Table 3 summarizes the weight losses and deflagration points after thermal stress (24 h, 125 Ā° C and 400 h, 110 Ā° C) of some of the mixtures selected from the examples. The weight loss was measured analogously to the Holland test. The measurement of the deflagration points was carried out by thermogravimetric analysis (Mettler) at a heating rate of 10 Ā° C per minute.

Man erkennt nach 400 h nur geringe Gewichtsverluste von 0,1 bis 0,7 Ges.-% und keine signifikante Ƅnderung der Verpuffungstemperatur nach thermischer Belastung. Tabelle 3: Ɯbersicht der Gewichtsverluste und Verpuffungstemperaturen Mischung Gew.verlust 24h, 125Ā°C [Gew.-%] Gew.verlust 400h, 110Ā°C [Gew.-%] Verpuffungstemp. nach 24h, 125Ā°C [Ā°C] Verpuffungs.-temp.nach 400h, 110Ā°C [Ā°C] 5 0,34 0,7 172 178 12 0,03 0,1 182 191 26 2,11 0,7 175 175 27 0,36 0,2 180 186 It can be seen after 400 h only small weight losses of 0.1 to 0.7 Ges .-% and no significant change in the deflagration temperature after thermal stress. Table 3: Overview of weight losses and deflagration temperatures mixture Weight loss 24h, 125 Ā° C [wt%] Weight loss 400h, 110 Ā° C [wt%] Verpuffungstemp. after 24h, 125 Ā° C [Ā° C] Deflagration temp. After 400h, 110 Ā° C [Ā° C] 5 0.34 0.7 172 178 12 0.03 0.1 182 191 26 2.11 0.7 175 175 27 0.36 0.2 180 186

Die Ergebnisse zeigen, dass die erfindungsgemƤƟ definierten pyrotechnischen Mittel Verpuffungstemperaturen im Bereich von 172 bis 191Ā°C aufweisen und gemƤƟ den Forderungen der Automobilindustrie als stabil anzusehen sind.The results show that the pyrotechnic means defined according to the invention have deflagration temperatures in the range of 172 to 191 Ā° C and are to be regarded as stable according to the requirements of the automotive industry.

Als besonders vorteilhaft, insbesondere auch fĆ¼r die Verwendung in Trennelementen fĆ¼r Batterieklemmen, haben sich daneben folgende Mischungen herausgestellt:

  • 30 Gew.-% Aminoguanidin-5,5'-azotetrazolat, 27,5 Gew.-% Guanidiniumpikrat, 40 Gew.-% Natriumnitrat, 2 Ges.-% Titan und 0,5 Ges.-% Grafit;
  • 29 Ges.-% Aminoguanidin-5,5'-azotetrazolat, 29 Ges.-% Guanidiniumpikrat, 40 Ges.-% Natriumnitrat, 1,5 Ges.-% Bariumcarbonat und 0,5 Ges.-% Aerosil;
  • 24 Ges.-% Aminoguanidin-5,5'-azotetrazolat, 24 Gew.-% Guanidiniumpikrat, 50 Gew.-% Natriumnitrat, 1,5 Ges.-% Bariumcarbonat und 0,5 Ges.-% Aerosil;
  • 29 Ges.-% Aminoguanidin-5,5'-azotetrazolat, 29 Ges.-% Guanidiniumpikrat, 40 Gew.-% Natriumnitrat, 1,5 Ges.-% Strontiumcarbonat und 0,5 Gew.-% Aerosil.
As particularly advantageous, especially for use in separating elements for battery terminals, next to the following mixtures have been found:
  • 30% by weight of aminoguanidine-5,5'-azotetrazolate, 27.5% by weight of guanidinium picrate, 40% by weight of sodium nitrate, 2% by weight of titanium and 0.5% by weight of graphite;
  • 29% by weight aminoguanidine-5,5'-azotetrazolate, 29% by weight guanidinium picrate, 40% by weight sodium nitrate, 1.5% by weight barium carbonate and 0.5% by weight Aerosil;
  • 24% by weight of aminoguanidine-5,5'-azotetrazolate, 24% by weight of guanidinium picrate, 50% by weight of sodium nitrate, 1.5% by weight of barium carbonate and 0.5% by weight of Aerosil;
  • 29% by weight of aminoguanidine-5,5'-azotetrazolate, 29% by weight of guanidinium picrate, 40% by weight of sodium nitrate, 1.5% by weight of strontium carbonate and 0.5% by weight of Aerosil.

Claims (14)

  1. Pyrotechnic agent having deflagration temperatures in the range from 165Ā°C to 195Ā°C, which contains as a component one or more azotetrazolates,
    characterised in that the azotetrazolate component is selected from aminoguanidine-5,5'-azotetrazolate (AGATZ) and guanidine-5,5'-azotetrazolate (GATZ) or mixtures of the two, wherein the amount of the azotetrazolate component is 20 to 50 wt.%, and also contains 50 to 80 wt.% of a mixture of several additives, wherein there are 15 to 40 wt.% of a nitrogen-containing compound, selected from: ammonium picrate, aminoguanidinium picrate, guanidinium picrate, aminoguanidinium styphnate, guanidinium styphnate, nitroguanidine, nitroaminoguanidine, aminoguanidine nitrate, diaminoguanidine nitrate, triaminoguanidine nitrate, guanidine nitrate, dicyandiamidine nitrate, and 30 to 60 wt.% of an oxidising agent, selected from one or more of the nitrates of the alkali and/or alkaline-earth metals and/or of ammonium, perchlorates of the alkali and/or alkaline-earth metals and/or of ammonium, peroxides of the alkali and/or alkaline-earth metals and/or of zinc.
  2. Pyrotechnic agent according to claim 1, characterised in that it contains 1 to 40 wt.% of high-energy additives, selected from one or more of hexogen, octogen and/or nitrocellulose.
  3. Pyrotechnic agent according to claim 1, characterised in that it contains 1 to 15 wt.% of a reducing agent, selected from one or more of aluminium, titanium, titanium hydride, boron, boron hydride, zirconium, zirconium hydride, silicon, graphite, activated charcoal, carbon black.
  4. Pyrotechnic agent according to claim 1, characterised in that it contains 1 to 20 wt.% of a binder, selected from one or more of cellulose and its derivatives, polyvinylbutyrals, polynitropolyphenylene, polynitrophenyl ether, plexigum, polyvinyl acetate and copolymers.
  5. Pyrotechnic agent according to claim 1, characterised in that it contains 0.1 to 15 wt.% of combustion moderators and processing aids, selected from one or more of ferrocene and its derivatives, acetonylacetates, salicylates, barium carbonate, strontium carbonate, magnesium carbonate, melamine, zinc oxide, zinc carbonate, silicates, silica gels and/or boron nitride.
  6. Pyrotechnic agent according to one or more of claims 1 to 5, characterised in that it contains 30 wt.% of aminoguanidine-5,5'-azotetrazolate, 27.5 wt.% of guanidinium picrate, 40 wt.% of sodium nitrate, 2 wt.% of titanium and 0.5 wt.% of graphite.
  7. Pyrotechnic agent according to one or more of claims 1 to 5, characterised in that it contains 29 wt.% of aminoguanidina-5,5'-azotetrazolate, 29 wt.% of guanidinium picrate, 40 wt.% of sodium nitrate, 1.5 wt.% of barium carbonate and 0.5 wt.% of Aerosil.
  8. Pyrotechnic agent according to one or more of claims 1 to 5, characterised in that it contains 24 wt.% of aminoguanidine-5,5'-azotetrazolate, 24 wt.% of guanidinium picrate, 50 wt.% of sodium nitrate, 1.5 wt.% of barium carbonate and 0.5 wit.% of Aerosil.
  9. Pyrotechnic agent according to one or more of claims 1 to 5, characterised in that it contains 29 wit.% of aminoguanidine-5,5'-azotetrazolate, 29 wt.% of guanidinium picrate, 40 wt.% of sodium nitrate, 1.5 wt.% of strontium carbonate and 0.5 wt.% of Aerosil.
  10. Use of a pyrotechnic agent according to one or more of claims 1 to 9 as a thermal early-ignition agent.
  11. Use of a pyrotechnic agent according to one or more of claims 1 to 9 as a thermal safety fuse.
  12. Use of a pyrotechnic agent according to one or more of claims 1 to 9 in motor vehicle safety systems.
  13. Use of a Pyrotechnic agent according to one or more of claims 1 to 9 in gas generators.
  14. Use of a pyrotechnic agent according to one or more of claims 1 to 9 in separators, preferably for battery terminals.
EP06763483A 2005-06-02 2006-06-02 Pyrotechnic agent Not-in-force EP1890986B1 (en)

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PCT/EP2006/062862 WO2006128910A1 (en) 2005-06-02 2006-06-02 Pyrotechnic agent

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WO2021058222A1 (en) 2019-09-27 2021-04-01 Ruag Ammotec Gmbh Method and system for providing a predetermined pyrotechnic energy output
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DE102017118416A1 (en) 2017-08-11 2019-02-14 Ruag Ammotec Gmbh Pyrotechnic separator, system for electrically charging an electric power cell, mobile device and charger
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WO2021058222A1 (en) 2019-09-27 2021-04-01 Ruag Ammotec Gmbh Method and system for providing a predetermined pyrotechnic energy output
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DE102022103535A1 (en) 2022-02-15 2023-08-17 Ruag Ammotec Gmbh Remote trigger for pyrotechnic energy releases

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EP1890986A1 (en) 2008-02-27
JP5388573B2 (en) 2014-01-15

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