WO2005094366A2 - Systeme generateur de gaz - Google Patents

Systeme generateur de gaz Download PDF

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Publication number
WO2005094366A2
WO2005094366A2 PCT/US2005/010684 US2005010684W WO2005094366A2 WO 2005094366 A2 WO2005094366 A2 WO 2005094366A2 US 2005010684 W US2005010684 W US 2005010684W WO 2005094366 A2 WO2005094366 A2 WO 2005094366A2
Authority
WO
WIPO (PCT)
Prior art keywords
gas generating
gas
salts
compositions
binder
Prior art date
Application number
PCT/US2005/010684
Other languages
English (en)
Other versions
WO2005094366A3 (fr
Inventor
Jeffrey W. Halpin
Sean P. Burns
Graylon K. Williams
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.
Priority to DE112005000805T priority Critical patent/DE112005000805T5/de
Priority to JP2007506510A priority patent/JP2007534587A/ja
Publication of WO2005094366A2 publication Critical patent/WO2005094366A2/fr
Publication of WO2005094366A3 publication Critical patent/WO2005094366A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
    • C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
    • C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
    • C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
    • 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 generally to gas generating systems, and to gas generant compositions employed in gas generator devices for automotive restraint systems, for example.
  • the present invention relates to nontoxic gas generating compositions that upon combustion rapidly generate gases that are useful for inflating occupant safety restraints in motor vehicles and specifically, the invention relates to thermally stable nonazide gas generants having not only acceptable burn rates, but that also, upon combustion, exhibit a relatively high gas volume to solid paniculate ratio at acceptable flame temperatures.
  • the evolution from azide-based gas generants to nonazide gas generants is well-documented in the prior art.
  • the advantages of nonazide gas generant compositions in comparison with azide gas generants have been extensively described in the patent literature, for example, U.S. Pat. Nos.
  • 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.
  • nonazide gas generant compositions are used to control the ignitability and combustion properties of the gas generant.
  • One of the disadvantages of known nonazide gas generant compositions is the amount and physical nature of the solid residues formed during combustion. When employed in a vehicle occupant protection system, 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.
  • phase stabilized ammonium nitrate as an oxidizer, for example, is desirable because it generates abundant nontoxic gases and minimal solids upon combustion.
  • gas generants for automotive applications must be thermally stable when aged for 400 hours or more at 107. degree. C.
  • the compositions must also retain structural integrity when cycled between -40. degree. C. and 107. degree. C.
  • gas generant compositions incorporating phase stabilized or pure ammonium nitrate sometimes exhibit poor thermal stability, and produce unacceptably high levels of toxic gases, CO and NO x for example, depending on the composition of the associated additives such as plasticizers and binders.
  • binders are often necessary to retain the shape of the propellant or gas generant tablets, and inhibit fragmentation of the same over time.
  • Certain water soluble binders such as carboxyl cellulosic binders, exhibit hygroscopic properties given their water solubility. Accordingly, these types of binders result in compositions that often have poor thermal stability, and in particular with compositions containing preferred oxidizers such as phase stabilized ammonium nitrate.
  • Known water insoluble binders such as cellulosic esters or alkyl celluloses such as cellulose acetate, cellulose acetate propionate, and cellulose acetate butyrate contain a cellulose backbone substituted with only alkyl substitutions (acetyl, propionyl, butyryl) and hydroxyl groups.
  • alkyl celluloses are nonhygroscopic and also exhibit excellent thermal stability. Nevertheless, these compositions typically have poor oxygen balance thereby inhibiting the addition of energetic fuels.
  • compositions of the present invention contain a primary binder containing both carboxyl substitutions and alkyl substitutions.
  • Known fuels, oxidizers, and other additives may be incorporated into these compositions as known in the art and as determined by design criteria.
  • gas generating systems such as airbag inflators and vehicle occupant protection systems incorporate these gas generating compositions.
  • the present invention includes gas generant compositions that optimize the production of gas combustion products and minimize solid combustion products while retaining other design requirements such as reduced hygroscopicity, thermal stability, production safety, and reduced environmental impact.
  • FIG. 1 is an exemplary airbag inflator containing a gas generant composition formed in accordance with the present invention.
  • FIG. 2 is a schematic representation of an exemplary vehicle occupant restraint system incorporating the inflator of FIG. 1 and a gas generant in accordance with the present invention.
  • the present invention includes gas generant compositions that contain a fuel, an oxidizer, and a primary binder.
  • the primary binder is selected from the group of cellulosic polymers wherein each polymeric binder contains carboxyl functionality, alkyl functionality, and hydroxyl functionality. Stated another way, A preferred binder selected from this group is carboxymethylcellulose acetate butyrate (CMCAB).
  • CMCAB carboxymethylcellulose acetate butyrate
  • Other carboxy alkyl celluloses binders are contemplated, and are exemplified by those compounds containing a cellulose backbone substituted with both carboxyl substitutions and alkyl substitutions, and salts of these compounds including nonmetal, metal, and alkali and alkaline earth metal salts including potassium, sodium, strontium, and ammonium salts thereof.
  • carboxy alkyl celluloses may be formed simply be reacting the carboxy alkyl celluloses with a base such as potassium hydroxide or ammonium hydroxide.
  • Carboxyl substitutions include carboxymethyl, succinyl, and maleyl groups.
  • Alkyl substitutions include acetyl, propionyl, butyryl groups with hydroxyl groups.
  • the primary binder is generally provided at about 0.1 -20%, and more preferably at 1 -10% by weight of the composition. It has been found that cellulosic polymers containing hydroxyl (-OH) groups on an anhydroglucose backbone can be reacted with various cyclic anhydrides to produce other carboxyl alkyl cellulose binders.
  • cyclic anhydrides suitable for reaction with the base polymer include succinic anhydride and maleic anhydride.
  • Other known anhydrides are available that will provide carboxyl functionality by the same process.
  • Gas generant compositions of the present invention may also contain the following constituents in the weight percents indicated.
  • a primary fuel is selected from the group containing azoles such as 5-aminotetrazole; nonmetal salts of azoles such as potassium 5-aminotetrazole; nonmetal salts of azoles such as mono- or diammonium salt of 5,5'-bis-1 H-tetrazole; nitrate salts of azoles such as 5-aminotetrazole nitrate; nitramine derivatives of azoles such as 5-nitraminotetrazole; metal salts of nitramine derivatives of azoles such as dipotassium 5-nitraminotetrazole; metal salts of nitramine derivatives of azoles such as dipotassium 5-nitraminotetrazole; nonmetal salts of nitramine derivatives such as mono- or diammonium 5- nitraminotetrazole and; guanidines such as dicyandiamide, nitroguanidine, and guanidine nitrate; salts of guanidine
  • the primary fuel is typically employed at 0- 80% by weight and more preferably at about 10-70% by weight. It will be appreciated that in certain compositions, the amount of binder employed will also provide fuel effective amounts of the binder whereby the binder functions as a binder/fuel. Accordingly, in that instance, the primary fuel may not be included in the composition.
  • An optional secondary fuel selected from the same group of fuels is typically provided at about 0-50%, and more preferably at about 0-30% by weight.
  • a nonmetal or metal primary oxidizer may be selected from nitrate salts such as ammonium nitrate, phase stabilized ammonium nitrate stabilized in a known manner and more preferably with about 10% by weight of potassium nitrate, potassium nitrate, and strontium nitrate; nitrite salts such as potassium nitrite; chlorate salts such as potassium chlorate; perchlorate salts such as ammonium perchlorate and potassium perchlorate; oxides such as iron oxide and copper oxide; basic nitrate salts such as basic copper nitrate and basic iron nitrate; and mixtures thereof.
  • the primary oxidizer may be provided at about 0.1 -80% by weight, and more preferably at about 10-70% by weight.
  • Secondary oxidizers may also be employed and are selected from the oxidizers described above.
  • the secondary oxidizers are typically provided at about 0-50%, and more preferably 0-30%, by weight of the gas generant composition.
  • An optional secondary binder may be selected from cellulose derivatives such as cellulose acetate, cellulose acetate butyrate, carboxymethylcellulose, salts of carboxymethylcellulose; silicone; polyalkene carbonates such as polypropylene carbonate and polyethylene carbonate; and mixtures thereof.
  • secondary binders may be provided at about 0-10%, and more preferably, 0-5% by weight.
  • An optional slag former may be selected from silicon compounds such as elemental silicon and silicon dioxide; silicones such as polydimethylsiloxane; silicates such as potassium silicates; natural minerals such as clays, talcs, and micas; fumed metal oxides such as fumed silica and fumed alumina.
  • slag formers may be provided at about 0- 10%, and more preferably, 0-5% by weight.
  • Other exemplary fuels, oxidizers, and other gas generant constituents are described in U.S Patent Nos. 5,035,757, 5,756,929, 5,872,329, 6,074,502, 6,287,400, 6,210,505, and 6,306,232, each herein incorporated by reference in its entirety.
  • Carboxymethylcellulose acetate butyrate is available from Eastman Chemical Company in Kingsport, Tennessee. It is known as a water-dispersable polymer, which means that it can be solvated by combining a lesser amount of an organic solvent with water.
  • Other gas generant constituents may be provided by known suppliers such as Aldrich Chemical Company. In an aqueous/organic solvent mixture the following constituents may be added, and homogeneously mixed as they are added, in the weight percents given.
  • a primary binder, CMCAB, at 0.1 -20% and more preferably 1 -10% is added to the mixture.
  • Secondary binders may also be added at 0- 10%, and more preferably .1 -5%, and are selected from the group including cellulose derivatives such as cellulose acetate, cellulose acetate butyrate, and carboxymethylcellulose; salts of carboxymethylcellulose; silicone; polyalkene carbonates such as polypropylene carbonate and polyethylene carbonate.
  • Gas generant compositions of the present invention may be formed as known in the art.
  • Examples of typical manufacturing processes include: ( 1 ) blending and/or grinding oxidizer, fuel, binders, and other components without solvent and compacting the powdered material on a press; (2) solvating the cellulosic binder in an aqueous/organic solution, adding the desired constituents such as fuel, oxidizer, and other additives, and molding into a propellant grain. The solvent is then dried off; (3) Solvating the cellulosic binder, adding oxidizers, fuels, and other components and extruding the propellant under pressure through a die to form various shapes. The shapes may then be cut to length and the solvent evaporated or heated off. The drying process may be accelerated by applying heat to the final homogeneous mixture.
  • An exemplary gas generating system includes an airbag device or vehicle occupant protection system shown in FIG. 2 to include airbag modules, airbag inflators or gas generators, and more generally, vehicle occupant restraint systems, all built or designed as well known in the art.
  • PSAN Phase-stabilized Ammonium Nitrate
  • BzA bis tetrazole diammonium salt
  • Eastman products were prepared in the weight percents shown in Table 1 .
  • the materials chosen for comparison were Eastman Cellulose acetate butyrate CAB381 -20BP and Eastman Carboxymethyl cellulose acetate butyrate CMCAB641 -0.2.
  • the compositions and burn rates are shown in Table 1 .
  • the two Eastman cellulosic binders provide very similar performance when mixed in the same ratios.
  • One benefit of using Carboxymethylcellulose Acetate Butyrate(CMCAB) in these formulations is reflected in the amount of organic solvent required for processing.
  • Cellulose Acetate Butyrate (CAB) can only be solvated by purely organic solvents/mixtures.
  • CMCAB can be solvated by water- organic mixtures and used in the same process, thereby decreasing the amount of environmentally harmful waste generated.
  • Dispersion method II as described in Eastman online publication gn431 allows for the use of approximately 50 / 50 water- organic mixtures used as solvent.
  • carboxy celluloses like CMC with preferred oxidizers such as ammonium nitrate or phase stabilized ammonium nitrate is significantly reduced due to interactions with the relatively greater number of hydroxyl substitutions on the polymer backbone (as compared to CMCAB).
  • CMC and its salts exhibit a color change from off-white to black, and mass loss of 0.7% to 10% in 400 hours, while mixtures with alkyl celluloses, such as CAB with a relatively lower hydroxyl substitution, exhibit mass loss of less than 0.2%, even after 1000 hours at 107C. This fact reflects favorably on the alkyl substitutions or groups in CMCAB.
  • exemplary advantages of celluloses like CMCAB over celluloses such as Cellulose Acetate (CA), Cellulose Acetate Propionate (CAP), and Cellulose Acetate Butyrate (CAB) at least one or more of the following advantages: improved oxygen balance (as illustrated in Table 2), and the capacity to be solvated with a mixture of organic solvent and water to reduce the amount of harmful waste in processing, and to provide a safer process with regard to flammability and volatility.
  • CA Cellulose Acetate
  • CAP Cellulose Acetate Propionate
  • CAB Cellulose Acetate Butyrate
  • an exemplary inflator incorporates a dual chamber design to tailor the force of deployment an associated airbag.
  • an inflator containing a gas generant 1 2 formed as described herein may be manufactured as known in the art.
  • U.S. Patent Nos. 6,422,601 , 6,805,377, 6,659,500, 6,749,219, and 6,752,421 exemplify typical airbag inflator designs and are each incorporated herein by reference in their entirety.
  • the exemplary inflator 10 described above may also be incorporated into an airbag system 200.
  • Airbag system 200 includes at least one airbag 202 and an inflator 10 containing a gas generant composition 1 2 in accordance with the present invention, coupled to airbag 202 so as to enable fluid communication with an interior of the airbag.
  • Airbag system 200 may also include (or be in communication with) a crash event sensor 210.
  • Crash event sensor 210 includes a known crash sensor algorithm that signals actuation of airbag system 200 via, for example, activation of airbag inflator 10 in the event of a collision.
  • airbag system 200 may also be incorporated into a broader, more comprehensive vehicle occupant restraint system 1 80 including additional elements such as a safety belt assembly 1 50.
  • FIG. 2 shows a schematic diagram of one exemplary embodiment of such a restraint system.
  • Safety belt assembly 1 50 includes a safety belt housing 1 52 and a safety belt 100 extending from housing 1 52.
  • a safety belt retractor mechanism 1 54 (for example, a spring-loaded mechanism) may be coupled to an end portion of the belt.
  • a safety belt pretensioner 1 56 containing propellant 1 2 may be coupled to belt retractor mechanism 1 54 to actuate the retractor mechanism in the event of a collision.
  • Typical seat belt retractor mechanisms which may be used in conjunction with the safety belt embodiments of the present invention are described in U.S. Pat. Nos. 5,743,480, 5,553,803, 5,667, 1 61 , 5,451 ,008, 4,558,832 and 4,597,546, incorporated herein by reference.
  • Safety belt assembly 1 50 may also include (or be in communication with) a crash event sensor 1 58 (for example, an inertia sensor or an accelerometer) including a known crash sensor algorithm that signals actuation of belt pretensioner 1 56 via, for example, activation of a pyrotechnic igniter (not shown) incorporated into the pretensioner.
  • a crash event sensor 1 58 for example, an inertia sensor or an accelerometer
  • a crash sensor algorithm that signals actuation of belt pretensioner 1 56 via, for example, activation of a pyrotechnic igniter (not shown) incorporated into the pretensioner.

Abstract

L'invention concerne de manière générale des compositions génératrices de gaz destinées par exemple à des dispositifs de gonflage de systèmes de retenue d'occupant. La composition (12) génératrice de gaz formée selon l'invention comprend un liant cellulosique à base de carboxyle alkyle. Un système (180) de protection d'occupant de véhicule et d'autres systèmes générateurs de gaz comprennent les compositions de l'invention.
PCT/US2005/010684 2004-03-30 2005-03-30 Systeme generateur de gaz WO2005094366A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE112005000805T DE112005000805T5 (de) 2004-03-30 2005-03-30 Gaserzeugungssystem
JP2007506510A JP2007534587A (ja) 2004-03-30 2005-03-30 ガス生成システム

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US55747304P 2004-03-30 2004-03-30
US60/557,473 2004-03-30

Publications (2)

Publication Number Publication Date
WO2005094366A2 true WO2005094366A2 (fr) 2005-10-13
WO2005094366A3 WO2005094366A3 (fr) 2007-08-30

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PCT/US2005/010684 WO2005094366A2 (fr) 2004-03-30 2005-03-30 Systeme generateur de gaz

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US (1) US20050263223A1 (fr)
JP (1) JP2007534587A (fr)
DE (1) DE112005000805T5 (fr)
WO (1) WO2005094366A2 (fr)

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Also Published As

Publication number Publication date
DE112005000805T5 (de) 2008-11-20
WO2005094366A3 (fr) 2007-08-30
JP2007534587A (ja) 2007-11-29
US20050263223A1 (en) 2005-12-01

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