EP0905108B1 - Mélange générateur de gaz sans particules - Google Patents
Mélange générateur de gaz sans particules Download PDFInfo
- Publication number
- EP0905108B1 EP0905108B1 EP98118023A EP98118023A EP0905108B1 EP 0905108 B1 EP0905108 B1 EP 0905108B1 EP 98118023 A EP98118023 A EP 98118023A EP 98118023 A EP98118023 A EP 98118023A EP 0905108 B1 EP0905108 B1 EP 0905108B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- mixture
- mixture according
- nitrate
- ammonium nitrate
- ammonium
- 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
Links
Classifications
-
- 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
- the invention relates to a particle-free, gas-generating mixture for use in gas generators for safety devices, in particular in gas generators for vehicle occupant restraint systems.
- Gas generators for safety devices usually contain a solid fuel based on sodium azide as a gas supplier Main component.
- sodium azide is toxic and can become easily with heavy metals forming extremely dangerous and violent implement reacting connections. Therefore, both in manufacturing the gas-generating mixtures as well as in the disposal Defective or unused gas generators require special measures.
- blowing agents containing sodium azide also a range of solids through suitable filter devices removed from the gas flow in the gas generator or in the gas generator have to be held back. There have therefore been attempts to Production of blowing agents which burn off essentially without residues made.
- US-A-5 545 272 describes a gas generating composition; which consists essentially of 35 to 55 wt .-% nitroguanidine and about 45 to 65 wt .-% phase-stabilized ammonium nitrate.
- phase stabilizing agents e.g. Potassium nitrate and potassium perchlorate, but also potassium dichromate, Potassium oxalate and mixtures thereof in an amount from 5 to about 25 % By weight, preferably 10 to 15%.
- the gas generating composition of US-A-5 545 272 can due to the relatively high proportion of phase stabilizing additives not residue-free for the ammonium nitrate, i.e. without solid combustion residues, burn down.
- this fuel burns up thus smoke formation caused by filter devices in the gas generator can only be suppressed incompletely.
- the known mixture is difficult to ignite and has a relative low burning rate.
- the high proportion of ammonium nitrate also leads to high hygroscopicity, which Storage and use in the gas generator an increased Effort requires an undesirable change in the fuel mixture to prevent.
- DE 195 05 568 A1 discloses a propellant for gas generators, the fuel as at least one compound from the group Tetrazoles, triazoles, triazines, cyanic acid, urea, their derivatives, Descendants or their salts, at least three as oxidizing agents Compounds from the group of peroxides, nitrates, chlorates or Perchlorate, as well as combustion moderators and the proportion of toxic Contains gas reducing supplements. Can be used as urea derivatives Biuret, guanidine, nitroguanidine, guanidine nitrate, aminoguanidine, Aminoguanidine nitrate, thiourea and triaminoguanidine nitrate be used.
- EP 0 659 712 A1 describes a gas-generating pyrotechnic composition, which essentially consists of an oxygen-containing thermoplastic Elastomer as a binder, based on a high-energy plasticizer of polyglyzidyl azide, an inorganic oxidizer and control additives burn rate, with the oxidizer at least 85 % By weight is ammonium nitrate. Binder and plasticizer form about 5 to 15 % By weight of the composition.
- additives to control the burning rate is a mixture of ammonium perchlorate and potassium nitrate used, the potassium nitrate about 7% by weight and the ammonium perchlorate forms between 4 and 6% by weight of the composition.
- the invention accordingly provides an acid-free, particle-free burning, gas generating mixture for use in a gas generator ready for a safety device, which consists of a high-energy Fuel with an oxygen value of not less than -35%, with an oxidizer mixture of ammonium nitrate and ammonium perchlorate an ammonium nitrate content of 35 to 50 wt .-% and an ammonium perchlorate content of between 3 and 10% by weight, based in each case on the Total weight of the mixture, possibly a phase stabilizing one Additive for the ammonium nitrate in a proportion of at most 5% by weight, based on the weight of the ammonium nitrate, Burning moderators in a proportion of 0 to 3 wt .-%, based on the Total weight of the mixture and processing aids in one Proportion of 0 to 5% by weight, based on the total weight of the mixture, consists.
- the total water content of the gas-generating mixture is at most 0.3%.
- the ammonium nitrate content is preferably between 40 and 50%, particularly preferably between 40 and 45%.
- the ammonium perchlorate content is preferably in the range between 3 and 7% by weight.
- the high-energy fuel is preferably from guanidine nitrate, Nitroguanidine, triaminoguanidine nitrate, urea nitrate, Nitro urea, nitropenta, nitrotriazalon, hexogen, octogen or their mixtures selected existing group. Particularly preferred is the fuel guanidine nitrate and / or nitroguanidine. The latter is the most preferred fuel.
- the ammonium nitrate used in the invention can be small amounts contain phase stabilizing additives to increase storage stability, those made of copper oxide, zinc oxide, complex zinc compounds or mixtures of existing groups are selected. It it has been found that, in contrast to those in US-A-5 545 272 required amounts of 10 to 15% of potassium compounds for phase stabilization in the application according to the invention at most 5% of the mentioned additives are needed. Surprisingly, it was found that while controlling the water content of the overall mixture the proportion of phase-stabilizing additives reduced to zero can be. While phase stabilizing at water contents of 0.1 to 0.3% Additions of 3 to 5% to ensure storage stability can be used if the water content is below 0.1% phase-stabilizing additives are completely dispensed with. All in all this results in a reduction in solid emissions compared to US Pat. No. 5,545,272 by the mixture according to the invention from 50 to 100%.
- the compounds known in the art can be used as the combustion moderator. These include transition metal compounds and carbon black.
- the transition metal compounds can be selected from the group of transition metal oxides, hydroxides, nitrates, carbonates and organometallic compounds of the transition metals. Exemplary examples of this are iron oxides, copper oxides, chromium oxides, zinc oxide, copper chromite, basic copper nitrate, zinc carbonate, copper resorcylate and ferrocene.
- carbon black as a combustion moderator, optionally in a mixture with transition metal compounds, is preferred, however, because carbon black is inexpensive on the one hand and burns off without residue with the formation of CO 2 .
- processing aids are added, which from the from the Pressing aids, trickling aids or lubricants existing group selected are.
- processing aids are Polyethylene glycol, cellulose, methyl cellulose, graphite, wax, magnesium stearate, Zinc stearate, boron nitride, talc, bentonite, silicon dioxide or molybdenum sulfide.
- Ammonium nitrate content ensures that the inherently unfavorable properties, such as. the low structural stability, hygroscopicity, the poor willingness to ignite and the slow burning rate of mixtures containing ammonium nitrate through the addition of ammonium perchlorate can be compensated.
- an ammonium perchlorate content of less than 3% there is no significant improvement with regard to the willingness to ignite and the burning rate of the Fuel.
- An ammonium perchlorate content of above 10% by weight leads to the formation of free hydrogen chloride, which is due to the strict toxicity requirements for propellant gases for occupant protection systems is undesirable.
- ammonium perchlorate leads also in the small proportion of 3 to 10% by weight Increase in the willingness to ignite and burning rate of the invention Propellant. Due to the higher oxygen content of Ammonium perchlorate can also the ammonium nitrate in the Mixture can be reduced more.
- the invention thus creates a gas yield of up to 100 percent burning gas-generating mixture from which an essentially particle-free gas mixture is released and that physiologically is harmless.
- the use of an oxidizer mixture Ammonium nitrate and ammonium perchlorate also ensure good Willingness to ignite and a high burning rate. At the same time points the mixture according to the invention has high thermal and chemical stability on.
- a temperature storage test at 110 ° C. was also carried out with the mixture carried out over 400 h.
- the measured weight loss was below 0.8%; the mixture is therefore sufficiently stable.
- a thermal shock test was also carried out on tablets with different moisture contents.
- the tablets were first dried in vacuo ( ⁇ 1 mbar) at 100 ° C for 18 hours, then part of it was in a desiccator over 8 hours at 45% rel. Moisture again moistened in a defined way.
- the H 2 O content of the dried tablets was 0.08%, the H 2 O content of the moistened tablets was 0.30%.
- the tablets were hermetically sealed in an aluminum container and subjected to a temperature change between - 35 ° C and + 85 ° C (56 cycles). While the tablets with the increased moisture content swelled strongly after the test, were partially broken and thus had become unusable for the intended use, the dry tablets showed no change in their mechanical properties.
- the tablets with a moisture content of 0.20% were the in Example 1 subjected to thermal cycling. To The tablets showed no change when the stress was complete their mechanical properties.
- Example 1 Tablets processed and ignited in a gas generator 51.5 g dried nitroguanidine, 40.0 g dried ammonium nitrate, 8.0 g of dried ammonium perchlorate, 2 g of copper chromite and 0.5 g of carbon black was added in the manner described in Example 1 Tablets processed and ignited in a gas generator.
- the average burning rate at 200 bar was 23 mm / s.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Organic Chemistry (AREA)
- Air Bags (AREA)
Claims (13)
- Mélange exempt d'azide engendrant du gaz et brûlant sans particules, destiné à être utilisé dans un générateur de gaz pour un dispositif de sécurité, en particulier pour un système de retenue de passager, avec une teneur totale en eau du mélange engendrant du gaz de 0,3 % au maximum, constitué para) un combustible riche en énergie avec un taux d'oxygène qui n'est pas inférieur à -35 %;b) un mélange oxydant de nitrate d'ammoniaque et de perchlorate d'ammonium, le nitrate d'ammoniaque étant contenu dans une proportion de 35 à 50 % en poids et le perchlorate d'ammonium dans une proportion de 3 à 10 % en poids, respectivement par rapport au poids totale du mélange ;c) le cas échéant un additif stabilisateur de phase pour le nitrate d'ammoniaque, dans une proportion de 5 % en poids au maximum, par rapport au poids du nitrate d'ammoniaque ;d) 0 à 3 % en poids de modérateurs de brûlage, par rapport au poids total du mélange ; ete) 0 à 5 % en poids de produits auxiliaires, par rapport au poids total du mélange.
- Mélange selon la revendication 1, caractérisé en ce que le combustible est choisi parmi le groupe de nitrate de guanidine, de nitroguanidine, de triaminoguanidine, de nitrate d'urée, de nitro-urée, de nitropenta, de nitrotriazolon, d'hexogène, d'octogène ou de leurs mélanges.
- Mélange selon la revendication 2, caractérisé en ce que le combustible est du nitrate de guanidine et/ou de la nitroguanidine.
- Mélange selon la revendication 3, caractérisé en ce que le combustible est de la nitroguanidine.
- Mélange selon l'une des revendications 1 à 4, caractérisé en ce que l'additif stabilisateur de phase est choisi parmi le groupe constitué d'oxyde de cuivre, d'oxyde de zinc, d'un composé de zinc complexe ou de leurs mélanges.
- Mélange selon l'une des revendications 1 à 5, caractérisé en ce que le modérateur de brûlage est de la suie.
- Mélange selon l'une des revendications 1 à 5, caractérisé en ce que le modérateur de brûlage est un composé de métal transitoire, de préférence un mélange avec de la suite.
- Mélange selon la revendication 7, caractérisé en ce que le composé de métal transitoire est choisi parmi le groupe des oxydes de métal transitoire, les hydroxydes de métal transitoire, les nitrates de métal transitoire, les carbonates de métal transitoire et les compositions organométalliques des métaux transitoires.
- Mélange selon l'une des revendications 1 à 8, caractérisé en ce que les produits auxiliaires sont choisis parmi le groupe constitué des auxiliaires de pressage, des auxiliaires de ruissellement ou des lubrifiants.
- Mélange selon la revendication 9, caractérisé en ce que les produits auxiliaires sont choisis parmi le groupe de polyéthylèneglycol, de cellulose, de cellulose méthylique, de graphite, de cire, de stéarate de magnésium, de stéarate de zinc, de nitrure de bore, de talc, de bentonite et de sulfure de molybdène ainsi que de leurs mélanges.
- Mélange selon l'une des revendications 1 à 10, caractérisé en ce que la teneur totale en eau du mélange est de 0,1 à 0,3 % en poids et la proportion d'additifs stabilisateurs de phase pour le nitrate d'ammoniaque est de 3 à 5 %.
- Mélange selon l'une des revendications 1 à 10, caractérisé en ce que la teneur totale en eau du mélange est inférieure à 0,1 % en poids et en ce que le nitrate d'ammoniaque est exempts d'additifs stabilisateurs de phase.
- Mélange selon la revendication 1, caractérisé en ce que le mélange est composé par :51,5 % en poids de nitroguanidine ;43,0 % en poids de nitrate d'ammoniaque ;5,0 % en poids de perchlorate d'ammonium ;0,5 % en poids de suie.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19742203A DE19742203A1 (de) | 1997-09-24 | 1997-09-24 | Partikelfreies gaserzeugendes Gemisch |
DE19742203 | 1997-09-24 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0905108A1 EP0905108A1 (fr) | 1999-03-31 |
EP0905108B1 true EP0905108B1 (fr) | 2002-11-27 |
Family
ID=7843508
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98118023A Expired - Lifetime EP0905108B1 (fr) | 1997-09-24 | 1998-09-23 | Mélange générateur de gaz sans particules |
Country Status (3)
Country | Link |
---|---|
US (1) | US5989367A (fr) |
EP (1) | EP0905108B1 (fr) |
DE (2) | DE19742203A1 (fr) |
Families Citing this family (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6296724B1 (en) * | 1998-07-21 | 2001-10-02 | Trw Inc. | Gas generating composition for an inflatable vehicle occupant protection device |
US6132538A (en) * | 1998-07-30 | 2000-10-17 | Autoliv Development Ab | High gas yield generant compositions |
JP2000086375A (ja) * | 1998-09-09 | 2000-03-28 | Daicel Chem Ind Ltd | ガス発生剤組成物 |
JP2000086376A (ja) * | 1998-09-14 | 2000-03-28 | Daicel Chem Ind Ltd | ガス発生剤組成物 |
DE29821544U1 (de) | 1998-12-02 | 1999-02-18 | TRW Airbag Systems GmbH & Co. KG, 84544 Aschau | Azidfreie, gaserzeugende Zusammensetzung |
DE29821541U1 (de) | 1998-12-02 | 1999-02-18 | TRW Airbag Systems GmbH & Co. KG, 84544 Aschau | Azidfreie, gaserzeugende Zusammensetzung |
US6017404A (en) * | 1998-12-23 | 2000-01-25 | Atlantic Research Corporation | Nonazide ammonium nitrate based gas generant compositions that burn at ambient pressure |
US6143102A (en) * | 1999-05-06 | 2000-11-07 | Autoliv Asp, Inc. | Burn rate-enhanced basic copper nitrate-containing gas generant compositions and methods |
US6176950B1 (en) * | 1999-05-17 | 2001-01-23 | James C. Wood | Ammonium nitrate and paraffinic material based gas generating propellants |
US6149746A (en) * | 1999-08-06 | 2000-11-21 | Trw Inc. | Ammonium nitrate gas generating composition |
US6361630B2 (en) * | 1999-08-17 | 2002-03-26 | Trw Inc. | Cool burning gas generating composition |
US20030066584A1 (en) * | 2000-03-01 | 2003-04-10 | Burns Sean P. | Gas generant composition |
US6550808B1 (en) * | 2000-11-17 | 2003-04-22 | Autoliv Asp. Inc. | Guanylurea nitrate in gas generation |
US6547900B2 (en) * | 2001-01-24 | 2003-04-15 | Breed Automotive Technology, Inc. | Method of stabilizing the density of gas generant pellets containing nitroguanidine |
US6589375B2 (en) | 2001-03-02 | 2003-07-08 | Talley Defense Systems, Inc. | Low solids gas generant having a low flame temperature |
US6875295B2 (en) | 2001-12-27 | 2005-04-05 | Trw Inc. | Cool burning gas generating material for a vehicle occupant protection apparatus |
DE10230402B4 (de) * | 2002-07-05 | 2007-01-11 | Trw Airbag Systems Gmbh & Co. Kg | Verfahren zur Herstellung einer gaserzeugenden Zusammensetzung |
US7758709B2 (en) | 2006-06-21 | 2010-07-20 | Autoliv Asp, Inc. | Monolithic gas generant grains |
US9193639B2 (en) * | 2007-03-27 | 2015-11-24 | Autoliv Asp, Inc. | Methods of manufacturing monolithic generant grains |
US8057611B2 (en) * | 2007-08-13 | 2011-11-15 | Autoliv Asp, Inc. | Multi-composition pyrotechnic grain |
US8815029B2 (en) | 2008-04-10 | 2014-08-26 | Autoliv Asp, Inc. | High performance gas generating compositions |
WO2009126182A1 (fr) * | 2008-04-10 | 2009-10-15 | Autoliv Asp, Inc. | Agents générateurs de gaz monolithiques contenant des oxydants à base de perchlorate et leurs procédés de fabrication |
US8808476B2 (en) | 2008-11-12 | 2014-08-19 | Autoliv Asp, Inc. | Gas generating compositions having glass fibers |
US9051223B2 (en) | 2013-03-15 | 2015-06-09 | Autoliv Asp, Inc. | Generant grain assembly formed of multiple symmetric pieces |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3708357A (en) * | 1971-04-21 | 1973-01-02 | Us Army | Oxidizers with improved thermal stability and method of making same |
US4111728A (en) * | 1977-02-11 | 1978-09-05 | Jawaharlal Ramnarace | Gas generator propellants |
CA1147593A (fr) * | 1979-08-24 | 1983-06-07 | Michael S. Ady | Systeme de propulsion pour fusee modele, y compris un grain de combustible propulsif solide et un orifice de combustion cylindrique adjacent au diffuseur de la buse |
US4552597A (en) * | 1984-08-17 | 1985-11-12 | Megabar Explosives Corporation | Soft composite explosives and process for making same |
US4604151A (en) * | 1985-01-30 | 1986-08-05 | Talley Defense Systems, Inc. | Method and compositions for generating nitrogen gas |
KR100411997B1 (ko) * | 1993-08-04 | 2004-04-03 | 오토모티브 시스템즈 라보라토리, 인코포레이티드 | 저잔류 아지드-유리 가스 발생체 조성물 |
FR2713632B1 (fr) * | 1993-12-07 | 1996-01-12 | Poudres & Explosifs Ste Nale | Compositions pyrotechniques génératrices de gaz propres et non toxiques, contenant un liant élastomère thermoplastique. |
DE4435523C1 (de) * | 1994-10-05 | 1996-06-05 | Fraunhofer Ges Forschung | Festtreibstoff auf der Basis von phasenstabilisiertem Ammoniumnitrat |
DE4435524C2 (de) * | 1994-10-05 | 1996-08-22 | Fraunhofer Ges Forschung | Festtreibstoff auf der Basis von reinem oder phasenstabilisiertem Ammoniumnitrat |
DE19505568A1 (de) * | 1995-02-18 | 1996-08-22 | Dynamit Nobel Ag | Gaserzeugende Mischungen |
US5545272A (en) * | 1995-03-03 | 1996-08-13 | Olin Corporation | Thermally stable gas generating composition |
US5780768A (en) * | 1995-03-10 | 1998-07-14 | Talley Defense Systems, Inc. | Gas generating compositions |
DE19531130A1 (de) * | 1995-08-24 | 1997-02-27 | Bayern Chemie Gmbh Flugchemie | Gaserzeugende Masse mit einem Verschlackungsmittel |
EP0801045A4 (fr) * | 1995-09-29 | 2000-11-02 | Otsuka Kagaku Kk | Generateur de gaz pour airbag |
EP0801044A4 (fr) * | 1995-09-29 | 1999-07-21 | Otsuka Kagaku Kk | Agent generateur de gaz pour airbags |
JPH09328387A (ja) * | 1996-06-03 | 1997-12-22 | Daicel Chem Ind Ltd | ガス発生剤組成物 |
-
1997
- 1997-09-24 DE DE19742203A patent/DE19742203A1/de not_active Withdrawn
-
1998
- 1998-09-23 DE DE59806422T patent/DE59806422D1/de not_active Expired - Lifetime
- 1998-09-23 EP EP98118023A patent/EP0905108B1/fr not_active Expired - Lifetime
- 1998-09-24 US US09/159,917 patent/US5989367A/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
DE59806422D1 (de) | 2003-01-09 |
EP0905108A1 (fr) | 1999-03-31 |
US5989367A (en) | 1999-11-23 |
DE19742203A1 (de) | 1999-03-25 |
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