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WO1998039275A1 - Generateur de gaz comprenant des complexes carbonate de metal amines - Google Patents

Generateur de gaz comprenant des complexes carbonate de metal amines Download PDF

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Publication number
WO1998039275A1
WO1998039275A1 PCT/US1998/003885 US9803885W WO9839275A1 WO 1998039275 A1 WO1998039275 A1 WO 1998039275A1 US 9803885 W US9803885 W US 9803885W WO 9839275 A1 WO9839275 A1 WO 9839275A1
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WO
WIPO (PCT)
Prior art keywords
gas generant
nitrate
metal
generant composition
group
Prior art date
Application number
PCT/US1998/003885
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English (en)
Inventor
Norman H. Lundstrom
Original Assignee
Automotive Systems Laboratory, Inc.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Automotive Systems Laboratory, Inc. filed Critical Automotive Systems Laboratory, Inc.
Publication of WO1998039275A1 publication Critical patent/WO1998039275A1/fr

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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 present invention relates to nontoxic gas generating compositions which upon combustion, rapidly generate gases that are useful for inflating occupant safety restraints in motor vehicles and specifically, the invention relates to gas generants that produce combustion products having not only acceptable toxicity levels, but that also exhibit a relatively high gas volume to solid particulate ratio at acceptable flame temperatures.
  • pyrotechnic nonazide gas generants contain ingredients such as oxidizers to provide the required oxygen for rapid combustion and reduce the quantity of toxic gases generated, a catalyst to promote the conversion of toxic oxides of carbon and nitrogen to innocuous gases, and a slag forming constituent to cause the solid and liquid products formed during and immediately after combustion to agglomerate into filterable clinker-like particulates .
  • Other optional additives such as burning rate enhancers or ballistic modifiers and ignition aids, are used to control the ignitability and combustion properties of the gas generant.
  • nonazide gas generant compositions One of the disadvantages of known nonazide gas generant compositions is the amount and physical nature of the solid residues formed during combustion. The solids produced as a result of combustion must be filtered and otherwise kept away from contact with the occupants of the vehicle. It is therefore highly desirable to develop compositions that produce a minimum of solid particulates while still providing adequate quantities of a nontoxic gas to inflate the safety device at a high rate.
  • complexes comprise a cationic metal template, an oxidizing anion to balance the charge of the complex, and a neutral ligand containing hydrogen and nitrogen.
  • the complexes are desirable because they rapidly combust or decompose producing water and gases comprised only of hydrogen, oxygen, and/or nitrogen, and furthermore, occupy a relatively smaller volume when compared to known gas generant compositions.
  • the neat metallic complexes are friction and impact sensitive, and therefore complicate safe handling, processing, and transportation requirements .
  • U.S. Patent No. 2,220,891 describes the use of metal ammine complexes in combination with ammonium nitrate.
  • the noncarbonated metal ammine complexes increase the sensitiveness of the composition thereby providing high density compositions desirable in quarry blasting where it is important to secure the maximum blasting effect.
  • a gas generant for a vehicle passenger restraint system employing at least one carbonato metal ammine complex and at least one oxidizer compound.
  • the carbonated metal complex comprises at least one neutral ammonia ligand and at least one carbon-containing ligand coordinated to a transitional metal cation, and, at least one nitrate, nitrite, or perchlorate oxidizing anion to balance the complex charge.
  • Incorporating the carbon ligand within the metal ammine complex decreases the impact and friction sensitivity of the complex, and also increases the gas generating properties of the composition.
  • Combining the carbonated metallic complex with an oxidizer results in a high density gas generant, and relatively speaking, produces abundant amounts of water vapor and gas such as carbon dioxide, nitrogen, and oxygen when compared to known gas generants. Carbon monoxide formation is inhibited by adding the oxygen rich compound. If desired, one or more azide or nonazide fuels may be added to the composition to enhance the gas generating properties.
  • the gas generants of this invention are prepared by wet, aqueous or nonaqueous, and/or wet/dry blending and compaction of the comminuted ingredients.
  • the preferred gas generant compositions comprise, in particular, at least one carbonated metal ammine coordination complex (hereinafter also referred to as a complex, carbonato complex, coordination complex, ammine complex, etc.) having at least one neutral ammonia ligand and at least one carbon containing ligand, each coordinated to a transition metal cationic template, and a nitrate, nitrite, or perchlorate based anion to balance the charge of the complex.
  • at least one carbonated metal ammine coordination complex hereinafter also referred to as a complex, carbonato complex, coordination complex, ammine complex, etc.
  • the complex is combined with at least one organic and/or inorganic oxidizer, and if desired, one or more additional fuels.
  • additional fuels When choosing a balancing anion, nitrate based anions are preferred, however, other oxygenated ions may also be used as described above.
  • the carbonated metal complex generally functions as a fuel and comprises 20-80%, but more preferably 35-65% by weight of the total gas generant composition.
  • exemplary examples of carbonated metal ammine complexes include, but are not limited to, carbonatopentamminecobalt (III) nitrate, Co(NH 3 ) 5 C0 3 N0 3 , and carbonatotetramminecobalt (III) nitrate, Co(NH 3 ) 4 C0 3 N0 3 .
  • Other examples include cobalt (III), rhodium (III) , and iridium (III) carbonatopentammine complexes comprising perchlorate or halide based anions.
  • the carbonated ligands contribute to low impact and friction sensitivity, in contrast to the elevated sensitivity of neat metal ammine complexes not containing carbon.
  • An oxidizer compound is selected from a group comprising alkali and alkaline earth metal nitrates, nitrites, and perchlorates; organic and inorganic nonmetal nitrates and nitrites; transitional metal oxides, nitrates, nitrites, complex polynitrites, and complex polynitrates; and combinations thereof. These include, for example, phase stabilized ammonium nitrate, ammonium nitrate, ammonium perchlorate, sodium nitrate, potassium nitrate, strontium nitrate, and copper oxide.
  • transitional metal complex polynitrites and polynitrates are commercially available from Aldrich Chemical, Alfa Aesar, Strem Chemical, and ACROS . Others may be prepared as taught in copending PCT Application No. US95/00029, the entire teachings of which are herein incorporated by reference.
  • the oxidizer generally comprises 20-80%, but more preferably 35-65% by weight of the total gas generant composition.
  • a fuel rich system combined with an oxidizer in the above percentages, ensures that the carbonated complexes produce minimal solids and advantageous gases such as carbon dioxide, nitrogen, water, and oxygen.
  • gases such as carbon dioxide, nitrogen, water, and oxygen.
  • the oxidizer functions as a diluent and therefore also contributes to decreased sensitivity of the complex.
  • addition of a diluent increases the density of the complex thereby accommodating a low volume gas generator.
  • nonazide fuels are preferably incorporated, however, high nitrogen azide or metal azido complex fuels, such as sodium azide, potassium azide, lithium azide, and azido pentammine cobalt (III) nitrate, may also be utilized.
  • Nonazide fuels are selected from a group comprising azoles, tetrazoles, triazoles, and triazines; nonmetal and metal derivatives of tetrazoles, triazoles, and triazines; cyclic nitramines, linear nitramines, and caged nitramines; derivatives of guanidine, hydrazine, hydroxylamine, and ammonia; and mixtures thereof.
  • guanidine derivative fuels include, but are not limited to, guanidine nitrate, aminoguanidine nitrate, diaminoguanidine nitrate, triaminoguanidine nitrate (wetted or unwetted) , guanidine perchlorate (wetted or unwetted) , triaminoguanidine perchlorate
  • guanidine compounds include 2, 4, 6-trihydrazino-s-triazine (cyanuric hydrazide) ; 2 , 4 , 6-triamino-s-triazine (melamine) ; other guanidine compounds such as the metal and nonmetal salts of nitroaminoguanidine, metal and nonmetal salts of nitroguanidine, metal and nonmetal derivatives or salts of cyanoguanidine ; nitroguanidine nitrate, and nitroguanidine perchlorate; azoles and tetrazoles such as urazole, aminourazole, lH-tetrazole, 5-aminotetrazole, 5-nitrotetrazole, 5-nitroaminotetrazole, 5, 5' -bitetrazole, diguanidinium-5, 5' - azotetra
  • An auxiliary azide or nonazide fuel as described not only enhances the gas producing capabilities, but also functions as a diluent and in certain cases, increases the density of the gas generant compositions, as described below.
  • compositions of the present invention may also include some of the additives heretofore used with gas generant compositions such as slag formers, compounding aids, ignition aids, ballistic modifiers, coolants, and NOX and CO scavenging agents.
  • additives heretofore used with gas generant compositions such as slag formers, compounding aids, ignition aids, ballistic modifiers, coolants, and NOX and CO scavenging agents.
  • Ballistic modifiers influence the temperature and pressure sensitivity, and the rate at which the gas generant or propellant burns.
  • the ballistic modifier (s) is selected from a group comprising alkali metal, alkaline earth metal, transitional metal, organometallic, and/or ammonium, guanidine, and triaminoguanidine salts of cyanoguanidine; alkali, alkaline earth, and transition metal oxides, sulfides, halides, chelates, metallocenes, ferrocenes, chromates, dichromates, trichromates, and chromites; and/or alkali metal, alkaline earth metal, guanidine, and triaminoguanidine borohydride derivatives; elemental sulfur; antimony trisulfide; and/or transition metal salts of acetylacetone; either separately or in combinations thereof.
  • Ballistic modifiers are employed in concentrations from about 0 to 25% by weight of the total gas generant composition, and utilize
  • a catalyst aids in reducing the formation of toxic carbon monoxide, nitrogen oxides, and other toxic species.
  • a catalyst may be selected from a group comprising triazolates and/or tetrazolates; alkali, alkaline earth, and transition metal salts of tetrazoles, bitetrazoles, and triazoles; transition metal oxides; guanidine nitrate; nitroguanidine; amines; and mixtures thereof.
  • a catalyst is employed in concentrations of 0 to 20% by weight of the total gas generant composition.
  • Suitable slag formers and coolants include lime, borosilicates, vycor glasses, bentonite clay, silica, alumina, silicates, aluminates, transition metal oxides, and mixtures thereof.
  • a slag former is employed in concentrations of 0 to 10% by weight of the total gas generant composition.
  • An ignition aid controls the temperature of ignition, and is selected from the group comprising finely divided elemental sulfur, boron, carbon black, and/or magnesium, aluminum, titanium, zirconium, or hafnium metal powders, and/or transition metal hydrides, and/or transition metal sulfides, and the hydrazine salt of 3-nitro-l, 2 , 4-triazole-5-one, in combination or separately.
  • An ignition aid is employed in concentrations of 0 to 20% by weight of the total gas generant composition.
  • Processing aids are utilized to facilitate the compounding of homogeneous mixtures.
  • Suitable processing aids include alkali, alkaline earth, and transition metal stearates; aqueous and/or nonaqueous solvents; molybdenum disulfide; graphite; boron nitride; polyethylene glycols; polypropylene carbonates; polyacetals; polyvinyl acetate; fluoropolymer waxes commercially available under the trade name "Teflon” or "Viton", and silicone waxes.
  • the processing aid is employed in concentrations of 0 to 15% by weight of the total gas generant composition.
  • references involving nonazide gas generant compositions describing various additives useful in the present invention include U.S. Patents No. 5,035,757; 5,084,118; 5,139,588; 4,948,439; 4,909,549; and 4,370,181, the teachings of which are herein incorporated by reference .
  • an oxidizer containing an alkaline earth metal, such as strontium may also function as a slag former, a ballistic modifier ignition aid, and a processing aid. Preparation of the carbonated coordination complexes of the present invention are described in the continuing series,
  • the manner and order in which the components of the fuel composition of the present invention are combined and compounded is not critical so long as a uniform mixture is obtained and the compounding is carried out under conditions which do not create unduly hazardous conditions or cause decomposition of the components employed.
  • the materials may be wet blended, or dry blended and attrited in a ball mill or Red Devil type paint shaker and then pelletized by compression molding.
  • the materials may also be ground separately or together in a fluid energy mill, sweco vibroenergy mill or bantam micropulverizer and then blended or further blended in a v-blender prior to compaction. Multimodal particle size distribution will provide an optimum fit to ensure that any interstitial voids are filled, thereby resulting in a high density gas generant composition.
  • compositions of the present invention are less sensitive than compositions employing neat noncarbon-containing metal ammine complexes, carbonated complexes having a perchlorate anion may still be somewhat sensitive. As such, handling and compositional studies of perchlorate salts should be tailored to reflect the increased sensitivity.
  • compositions having components more sensitive to friction, impact, and electrostatic discharge should be wet ground separately followed by drying.
  • the resulting fine powder of each of the components may then be wet blended by tumbling with ceramic cylinders in a ball mill jar, for example, and then dried. Less sensitive components may be dry ground and dry blended at the same time.
  • the ratio of oxidizer to fuel, wherein the metal complex comprises the fuel is adjusted such that the oxygen balance is between -10.0% and +10.0% 0 2 by weight of composition as described above. More preferably, the ratio of oxidizer to fuel is adjusted such that the composition oxygen balance is between -4.0% and 1.0% 0 2 by weight of composition. Most preferably, the ratio of oxidizer to fuel is adjusted such that the composition oxygen balance is between - 2.0% and 0.0% 0 2 by weight of composition.
  • the oxygen balance is the weight percent of 0 2 in the composition which is needed or liberated to form the stoichiometrically balanced products. Therefore, a negative oxygen balance represents an oxygen deficient composition whereas a positive oxygen balance represents an oxygen rich composition. It can be appreciated that the relative amounts of oxidizer and fuel will depend on the nature of the selected complex.
  • the gas generant compositions of the present invention may incorporate fuels and oxidizers that further desensitize the carbonated metal ammine complexes due to a variety of physical and/or chemical parameters, such as chemical structure, hydration or water of crystallization, stoichiometry, particle size, packing, and coating.
  • the use of a substantially insensitive fuel with a low sensitive carbonated metal ammine complex results in a high density, volumetrically efficient composition.
  • the monomodal particle size of the carbonato complex contributes to the formation of interstitial voids that may be left vacant in a neat carbonated metal ammine complex.
  • the vacancies contribute to sensitivity.
  • the voids are filled with a negligible increase in volume. Filling the voids increases the density of the complex and results in more gas per gram of gas generant. As such, the gas generating properties are significantly enhanced without a substantial increase in gas generant volume, or in solids formation upon combustion.
  • the less sensitive nature of the fuels decreases the sensitivity of the carbonato complexes once the interstitial voids are occupied.
  • Optional coolants desensitize the carbonated complexes in the same manner.
  • known metal ammine complex formulations as taught in WO 95/19944, utilize conventional inorganic metal fuels such as boron, magnesium, aluminum, silicon, titanium, and zirconium, and preclude the formation of gaseous carbon species upon combustion. Not only do certain of these fuels significantly increase the gas generant volume, they also result in more solids and less gas produced upon combustion. Practically speaking, greater volumetric efficiency facilitates increased design flexibility depending on the quantities of gas desired. Due to greater gas and minimal solids production, reduced filtration needs result in correspondingly smaller filters and inflators.
  • conventional inorganic metal fuels such as boron, magnesium, aluminum, silicon, titanium, and zirconium
  • compositions of the present invention are generally envisioned for use in conventional pyrotechnic gas inflators, for example, those referred to in U.S. Patent No, 4,369,079, incorporated herein by reference.
  • the methods of the prior art involve the use of a hermetically sealed metallic cartridge containing fuel, oxidizer, slag former, initiator and other selected additives.
  • the gas generants may also be tailored for use in hybrid inflators utilizing pressurized gases.
  • Hybrid inflator technology is based on heating a stored inert gas such as argon or helium to a desired temperature by burning a small amount of propellant.
  • Hybrid inflators that inherently operate at a lower temperature do not require cooling filters that must be used with pyrotechnic inflators to cool combustion gases.
  • the present invention is illustrated by the following theoretical examples wherein the components are quantified in weight percent of the total composition. Values of the products are obtained based on the given compositions and reactions .
  • Example 1 Carbonatopentamminecobalt (III) Nitrate and Ammonium Nitrate * Co(NH 3 ) 5 C0 3 N0 3 + 5 NH 4 N0 3 ⁇ CoO + 35/2 H 2 0 + C0 2 + 8 N 2 +
  • a mixture of 39.94% Co (NH 3 ) 5 C0 3 N0 3 and 60.06% NH 4 N0 3 is prepared as follows.
  • the components are separately ground to a fine powder by tumbling with ceramic cylinders in a ball mill jar.
  • the powder is then separated from the grinding cylinders and granulated to improve the flow characteristics of the material.
  • the ground components are blended in a v- blender prior to compaction. If desired, the homogeneously blended granules may then be cautiously compression molded into pellets by methods known to those skilled in the art.
  • the end products include 11.26% CoO (s) , 47.30% H 2 0 (v) , 6.61% C0 2 (g) , 33.63% N 2 (g) , and 1.20% 0 2 ; the moles/100 gms of gas generant for each of these end products, respectively, is 0.150M, 2.628M, 0.150M, 1.201M, and 0.038M.
  • the total weight percent of gaseous and vapor products is 88.74%.
  • the total gaseous and vapor moles/lOOg of gas generant is 4.017M.
  • nitrate or nitrite examples of which are phase stabilized ammonium nitrate, alkali metal nitrates, alkaline earth metal nitrates, transition metal nitrates, transitional metal complex polynitrites and polynitrates, inorganic nonmetallic nitrates, inorganic nonmetallic nitrites, organic nitrates, and combinations thereof, are applicable.
  • nitrate or nitrite examples of which are phase stabilized ammonium nitrate, alkali metal nitrates, alkaline earth metal nitrates, transition metal nitrates, transitional metal complex polynitrites and polynitrates, inorganic nonmetallic nitrates, inorganic nonmetallic nitrites, organic nitrates, and combinations thereof, are applicable.
  • Example 3 Carbonatopentamminecobalt (III) Nitrate, Ammonium Nitrate * , and Strontium Nitrate *
  • a mixture of 50.00% Co (NH 3 ) 5 C0 3 N0 3 , 30.08% NH 4 N0 3 , and 19.92% Sr(N0 3 ) 2 is prepared as in Example 1.
  • the end products include 14.10% CoO (s) , 9.77% SrO (s) , 38.91% H 2 0 (v) , 8.27% C0 2 (g) , and 28.95% N 2 (g) ; the moles/lOO gms of gas generant for each of these end products, respectively, is 0.188M, 0.094M, 2.162M, 0.188M, and 1.034M.
  • the total weight percent of gaseous and vapor products is 85.90%.
  • the total gaseous and vapor moles/lOOg of gas generant is 3.384M.
  • nitrate or nitrite examples of which are phase stabilized ammonium nitrate, alkali metal nitrates, alkaline earth metal nitrates, transition metal nitrates, transitional metal complex polynitrites and polynitrates, inorganic nonmetallic nitrates, inorganic nonmetallic nitrites, organic nitrates, and combinations thereof, are applicable.
  • a mixture of 54.01% Co (NH 3 ) 4 C0 3 N0 3 and 45.99% Sr(N0 3 ) 2 is prepared as in Example 1.
  • the end products include 16.27% CoO (s) , 22.56% SrO (s) , 23.43% H 2 0 (v) , 9.54% C0 2 (g) , 21.26% N 2 (g) , and 6.94% 0 2 ;
  • the moles/lOO gms of gas generant for each of these end products, respectively, is 0.217M, 0.217M, 1.302M, 0.217M, 0.759M, and 0.217M.
  • the total weight percent of gaseous and vapor products is 61.17%.
  • the total gaseous and vapor moles/lOOg of gas generant is 2.495M.
  • nitrate or nitrite examples of which are phase stabilized ammonium nitrate, alkali metal nitrates, alkaline earth metal nitrates, transition metal nitrates, transitional metal complex polynitrites and polynitrates, inorganic nonmetallic nitrates, inorganic nonmetallic nitrites, organic nitrates, and combinations thereof, are applicable.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Chemistry (AREA)
  • Air Bags (AREA)

Abstract

La présente invention concerne des compositions de génération de gaz à haute teneur en azote convenant particulièrement au gonflage des airbags. Ces compositions comprennent au moins un complexe de coordination métallique carbonaté en combinaison avec au moins un oxydant riche en oxygène. Cette combinaison permet d'obtenir des générateurs de gaz qui sont relativement plus stables et moins sensibles que les générateurs de gaz connus, tout en dégageant relativement plus de gaz et moins de solides. L'utilisation d'un composé riche en oxygène, conjointement avec un complexe carbonaté garantit une génération abondante de gaz, tout en inhibant la production de monoxyde de carbone.
PCT/US1998/003885 1997-03-05 1998-02-27 Generateur de gaz comprenant des complexes carbonate de metal amines WO1998039275A1 (fr)

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US81169897A 1997-03-05 1997-03-05
US08/811,698 1997-03-05

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WO1998039275A1 true WO1998039275A1 (fr) 1998-09-11

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000006524A1 (fr) * 1998-07-30 2000-02-10 Autoliv Development Ab Compositions generant un grand volume de gaz
EP1068165A4 (fr) * 1998-12-28 2001-04-25 Autoliv Dev Generateurs de gaz non azide presentant une productivite elevee de gaz et un taux de combustion ameliore
CN109219539A (zh) * 2016-05-23 2019-01-15 均胜安全系统收购有限责任公司 产气组合物及其制备和使用方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5429691A (en) * 1993-08-10 1995-07-04 Thiokol Corporation Thermite compositions for use as gas generants comprising basic metal carbonates and/or basic metal nitrates
US5542999A (en) * 1994-01-18 1996-08-06 Fraunhofer Gesellschaft Zur Forderung Der Angewandten Forschung E.V. Gas-generating mixture
US5592812A (en) * 1994-01-19 1997-01-14 Thiokol Corporation Metal complexes for use as gas generants
US5608183A (en) * 1996-03-15 1997-03-04 Morton International, Inc. Gas generant compositions containing amine nitrates plus basic copper (II) nitrate and/or cobalt(III) triammine trinitrate
US5725699A (en) * 1994-01-19 1998-03-10 Thiokol Corporation Metal complexes for use as gas generants

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5429691A (en) * 1993-08-10 1995-07-04 Thiokol Corporation Thermite compositions for use as gas generants comprising basic metal carbonates and/or basic metal nitrates
US5542999A (en) * 1994-01-18 1996-08-06 Fraunhofer Gesellschaft Zur Forderung Der Angewandten Forschung E.V. Gas-generating mixture
US5592812A (en) * 1994-01-19 1997-01-14 Thiokol Corporation Metal complexes for use as gas generants
US5725699A (en) * 1994-01-19 1998-03-10 Thiokol Corporation Metal complexes for use as gas generants
US5608183A (en) * 1996-03-15 1997-03-04 Morton International, Inc. Gas generant compositions containing amine nitrates plus basic copper (II) nitrate and/or cobalt(III) triammine trinitrate

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000006524A1 (fr) * 1998-07-30 2000-02-10 Autoliv Development Ab Compositions generant un grand volume de gaz
EP1068165A4 (fr) * 1998-12-28 2001-04-25 Autoliv Dev Generateurs de gaz non azide presentant une productivite elevee de gaz et un taux de combustion ameliore
US6383318B1 (en) 1998-12-28 2002-05-07 Autoliv Asp, Inc. Burn rate-enhanced high gas yield non-azide gas generants
CN109219539A (zh) * 2016-05-23 2019-01-15 均胜安全系统收购有限责任公司 产气组合物及其制备和使用方法

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