EP0607446B1 - Gaserzeugungsmittel für airbags - Google Patents

Gaserzeugungsmittel für airbags Download PDF

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Publication number
EP0607446B1
EP0607446B1 EP93910338A EP93910338A EP0607446B1 EP 0607446 B1 EP0607446 B1 EP 0607446B1 EP 93910338 A EP93910338 A EP 93910338A EP 93910338 A EP93910338 A EP 93910338A EP 0607446 B1 EP0607446 B1 EP 0607446B1
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EP
European Patent Office
Prior art keywords
gas generating
composition
generating composition
combustion
parts
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
Application number
EP93910338A
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English (en)
French (fr)
Other versions
EP0607446A4 (de
EP0607446A1 (de
Inventor
Tadao Yoshida
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Otsuka Chemical Co Ltd
Daicel Corp
Nippon Koki Co Ltd
Original Assignee
Otsuka Chemical Co Ltd
Nippon Koki Co Ltd
Daicel Chemical Industries Ltd
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
Priority claimed from JP4185253A external-priority patent/JPH0632690A/ja
Priority claimed from JP4185251A external-priority patent/JPH0632689A/ja
Application filed by Otsuka Chemical Co Ltd, Nippon Koki Co Ltd, Daicel Chemical Industries Ltd filed Critical Otsuka Chemical Co Ltd
Publication of EP0607446A1 publication Critical patent/EP0607446A1/de
Publication of EP0607446A4 publication Critical patent/EP0607446A4/de
Application granted granted Critical
Publication of EP0607446B1 publication Critical patent/EP0607446B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
    • C06B29/02—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate of an alkali metal
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
    • C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate

Definitions

  • This invention relates to an air bag gas generating composition.
  • a gas generating composition is ignited, either electrically or mechanically, in an instant on sensing a car crash to thereby inflate the bag with the gas so generated.
  • the gas generating composition is generally supplied as molded into a pellet or disk form. It is essential that such a gas generating composition insures an appropriate burning velocity. If the burning velocity is too low, the bag cannot be inflated in an instant so that the system fails to achieve its object.
  • the gas generating composition is a powdery composition having the property to get ignited by a shock. Shock ignitability is the sensitivity of a powder to shock ignition and an excessively high shock sensitivity is undesirable from the standpoint of safety because it represents a high risk of explosion in the course of production, e.g. in the mixing stage or in the molding stage. Therefore, shock sensitivity is preferably as low as possible.
  • the combustion temperature of the gas generating composition be not too high. This is because, to absorb the shock of a car crash to the driver or passenger and help him to escape, generally the inflated air bag then releases the internal gas to shrink but if the combustion temperature is too high, the released gas is also hot enough to cause the passenger to sustain a burn, perforate the bag to detract from its function, or burn the bag to induce a car fire.
  • Known air bag gas generating compositions comprise sodium azide as the gas generating base and certain additives such as an oxidizing agent [e.g. metal oxides such as TiO 2 , MnO 2 , Fe 2 O 3 , CuO, etc., nitrates such as NaNO 3 , KNO 3 , Cu(NO 3 ) 2 , etc., perchlorates such as KClO 4 , NaClO 4 , etc.
  • an oxidizing agent e.g. metal oxides such as TiO 2 , MnO 2 , Fe 2 O 3 , CuO, etc.
  • nitrates such as NaNO 3 , KNO 3 , Cu(NO 3 ) 2 , etc.
  • perchlorates such as KClO 4 , NaClO 4 , etc.
  • chlorates such as KClO 3 , NaClO 3 , etc.], a reducing metal [Zr, Mg, Al, Ti, etc.], a cooling agent [Na 2 CO 3 , K 2 CO 3 , CaCO 3 , FeSO 4 , etc.], a pH control agent [iron sulfate etc.], a mechanical performance agent [MoS 2 , KBr, graphite, etc.] and so on.
  • sodium azide-based gas generating compositions are in common use today partly because the generated gas is nitrogen gas for the most part and partly because they have adequate burning velocities and relatively low combustion temperatures.
  • sodium azide has the following disadvantages.
  • JP-A-118979/75 discloses an air bag gas generating composition
  • a nitrogen-containing compound such as azodicarbonamide, trihydrazinotriazine or the like and an oxidizing agent such as potassium permanganate, manganese dioxide, barium dichromate, barium peroxide or the like.
  • an oxidizing agent such as potassium permanganate, manganese dioxide, barium dichromate, barium peroxide or the like.
  • US-A-5 125 684 discloses a stable extrudable non-azide crash bag propellant composition for generating high quality nitrogen gas and a low temperature process for producing the same from an extrudable mass containing an effective amount of a cellulose-based binder.
  • the disclosed composition contains, as one component, an energetic component selected from nitroguanidine, triaminoguanidine nitrate, ethylene dinitramine, cyclotriethylenetrinitramine, cyclotetramethylenetetranitramine, trinitrotoluene and pentaerythritol tetranitrate.
  • DE-A-23 51 401 discloses an air bag gas generating composition
  • an air bag gas generating composition comprising (i) an alkali or alkaline earth metal azide (e.g. sodium azide), (ii) an alkali metal salt of perchloric acid (or, alternatively, an alkali metal bi-chromate) and (iii) aminotetrazole, hydrated aminotetrazole, azodicarbonamide (ADCA) or azotetrazole.
  • the main component of the gas generating base is a metal azide as the component (i).
  • aminotetrazole is used as component (iii).
  • US-A-4 386 979 discloses an air bag gas generating composition
  • an air bag gas generating composition comprising dicyanodiamide or a similar cyanamide compound and an oxidizer such as an oxo halogen acid salt, a salt of nitric acid or the like.
  • the disclosed gas generating composition involves a high burning temperature in the range of from 1200°C to 1600°C.
  • Another object of this invention is to provide an air bag gas generating composition which is either equivalent to or even higher than the sodium azide-based gas generating composition in burning velocity and gas output.
  • a still further object of this invention is to provide an air bag gas generating composition which is free from the above-mentioned disadvantages (1) through (6) of the azide compound.
  • the inventor of this invention made an extensive exploration to accomplish the above objects with his attention focused on a nitrogen-containing compound which by itself has very low risks of fire or intoxication hazards due to decomposition or combustion and found that by causing azodicarbonamide to react directly with a defined oxidizing agent, that is a halogen oxo acid salt, taking advantage of the reducing property of the former instead of combusting the nitrogen-containing compound with the heat of a redox reaction, there can be realized not only a shock sensitivity either equivalent to or lower than that of the sodium azide-based gas generating composition but also a burning velocity and a gas output, both of which are either equivalent to or higher than those of said sodium azide-based composition, as well as a practically useful, low combustion temperature.
  • a defined oxidizing agent that is a halogen oxo acid salt
  • This invention is, therefore, directed to an air bag gas generating composition consisting of azodicarbonamide and a halogen oxo acid salt in certain relative amounts as given below, as well as certain optional compounds specified hereinbelow.
  • azocarbonamide is used as the gas generation base.
  • the form or grain size of the azodicarbonamide and a suitable one can be selectively employed.
  • the oxidizing agent to be used in this invention is a halogen oxo acid salt.
  • the halogen oxo acid salt any of the known species can be employed. Preferred are halogenates and perhalogenates and particularly preferred are the corresponding alkali metal salts.
  • the alkali metal halogenates include chlorates and bromates such as potassium chlorate, sodium chlorate, potassium bromate and sodium bromate, among others.
  • the alkali metal perhalogenates include perchlorates and perbromates such as potassium perchlorate, sodium perchlorate, potassium perbromate and sodium perbromate, among others. These halogen oxo acid salts may be used alone or in combination.
  • the amount of the halogen oxo acid salt is generally stoichiometric, that is to say the amount necessary for complete oxidation and combustion of azodicarbonamide based on its oxygen content, but since the burning velocity, combustion temperature and combustion product composition can be freely controlled by varying the ratio of halogen oxo acid salt to azodicarbonamide, its amount can be selected from a relatively broad range, i.e., 20 to 233.3 parts by weight, preferably 20 - 200 parts by weight, more preferably 30 - 200 parts by weight, of the halogen oxo acid salt can be used per 100 parts by weight of azodicarbonamide.
  • the form and grain size of the halogen oxo acid are not particularly critical and can be selected in each case.
  • composition of this invention may contain, within the range not affecting its performance characteristics, at least one additive selected from burning control catalysts, antidetonation agents and oxygen donor compounds in addition to said two essential components.
  • the combustion control catalyst is a catalyst for adjusting the burning velocity, which is one of the basic performance parameters, according to conditions of the intended application, with safety parameters such as low shock ignition and non-detonation properties and other basic performance parameters such as the gas output being fully retained.
  • combustion control catalysts include, among others, the oxides, chlorides, carbonates and sulfates of Group IV or Group VI elements of the periodic table of the elements, cellulosic compounds and organic polymers.
  • the oxides, chlorides, carbonates and sulfates of Group IV or VI elements include ZnO, ZnCO 3 , MnO 2 , FeCl 3 , CuO, Pb 3 O 4 , PbO 2 , PbO, Pb 2 O 3 , S, TiO 2 , V 2 O 5 , CeO 2 , Ho 2 O 3 , CaO 2 , Yb 2 O 3 , Al 2 (SO 4 ) 3 , ZnSO 4 , MnSO 4 , FeSO 4 , etc.
  • cellulosic compounds may be mentioned carboxymethylcellulose and its ether, hydroxymethylcellulose and so on.
  • the organic polymers mentioned above include, among others, soluble starch, polyvinyl alcohol and its partial saponification product, and so on.
  • These combustion control catalysts can be used alone or in combination.
  • the amount of the combustion control catalyst is not critical and can be liberally selected from a broad range. Generally, however, this catalyst is used in a proportion of about 0.1 - 50 parts by weight, preferably about 0.2 - 10 parts by weight, based on 100 parts by weight of azodicarbonamide and said halogen oxo acid salt combined.
  • the grain size of the combustion control catalyst is not critical and can be appropriately selected.
  • the antidetonation agent is added for preventing the detonation which may occur when the gas generating composition is involved in a fire in the course of production, handling or transportation or subjected to an extraordinary impact.
  • antidetonation agent eliminates the risk of detonation, the safety of the gas-generating composition in various stages of production, handling and transportation can be further enhanced.
  • the antidetonation agent a variety of known substances can be utilized. Thus, for example, oxides such as bentonite, alumina, diatomaceous earth, etc. and carbonates and bicarbonates of metals such as Na, K, Ca, Mg, Zn, Cu, Al, etc. can be mentioned.
  • the amount of such antidetonation agent is not critical and can be liberally selected from a broad range. Generally, it can be used in a proportion of about 5 - 30 parts by weight relative to 100 parts by weight of azodicarbonamide and said halogen oxo acid salt combined.
  • the oxygen donor compound is effective in augmenting the O 2 concentration of the combustion product gas liberated from the composition of this invention.
  • the oxygen donor compound is not critical in kind and a variety of known substances can be employed. For example, CuO 2 , K 2 O 4 , etc. can be mentioned.
  • the amount of the oxygen donor compound is not so critical and can be liberally selected. Generally, however, this donor can be used in a proportion of about 10 - 100 parts by weight based on 100 parts by weight of azodicarbonamide and said halogen oxo acid salt combined.
  • the composition of this invention may further contain, within the range not affecting its performance characteristics, a combustion temperature control agent and/or a burning velocity control agent.
  • the combustion temperature control agent includes the carbonates and bicarbonates of metals such as Na, K, Ca, Mg, etc., among others.
  • the burning velocity control agent includes the sulfates of Al, Zn, Mn, Fe, etc., among others.
  • the proportion of such combustion temperature control agent and/or burning velocity control agent may generally be about 10 parts by weight, preferably about 5 parts by weight or less, based on 100 parts by weight of azodicarbonamide and said halogen oxo acid salt combined.
  • the composition of this invention can be manufactured by blending the above-mentioned components. While the resulting mixture as such can be used as the gas generating composition, it may be provided in the form of a molded composition.
  • a molded composition can be manufactured by the conventional procedure.
  • the composition of this invention may be mixed with a binder in a suitable ratio and the mixture be molded.
  • the binder may be any binder that is routinely employed.
  • the form of such molded composition is not critical. Thus, it may be a pellet, disk, ball, bar, hollow cylinder, confetti or tetrapod, for instance. It may be solid or porous (e.g. honeycomb-shaped). It is also possible to process each component into a discrete preparation and mix them in use.
  • composition of this invention has the following advantages.
  • ADCA means azodicarbonamide
  • ADCA and halogen oxo acid salt, with or without a combustion control catalyst, were blended according to the formulas shown below in Table 1 to provide compositions (No. 1 - No. 7) of this invention.
  • each of the above compositions of this invention was compressed at 60 kg/cm 2 to prepare pellets (5 mm in diameter and 5.0 mm high) and each pellet sample was subjected to the 7.5-liter bomb test. The results are shown in Table 2.
  • CP max represents the maximum pressure (kg/cm 2 ) in the reaction chamber
  • W 1/2 represents the time (ms) in which the internal pressure of the chamber travels 1/2 of the maximum pressure
  • BP max represents the maximum pressure (kg/cm 2 ) within the bomb
  • T 90 represents the time (ms) in which the internal pressure of the bomb reaches 90% of the maximum pressure
  • BT max represents the maximum temperature (°C) within the bomb.
  • T 90 is a value simulating the inflation time of the air bag.
  • CP max is an index, the values of which indicate that the compositions of this invention retain a satisfactory performance as gas generating compositions.
  • W 1/2 is a parameter simulating the burning velocity of the gas generating composition within the chamber.
  • BP max is a parameter indicating the gas generating capacity per unit mass of the gas generating composition.
  • BT max is a parameter simulating the temperature of the gas in the fully inflated air bag.
  • ADCA and halogen oxo acid salt, with or without the combustion control catalyst, were blended according to the formulas (wt. %) shown below in Table 3 to provide compositions of this invention.
  • compositions of this invention were subjected to the following shock ignitability (sensitivity) test.
  • prior art gas generating compositions NaN 3 -KClO 4 -Fe 3 O 4 and NaN 3 -CuO were also subjected to the shock ignitiability test.
  • Table 3 shows the ignition limit gap length (ignitable up to that gap length) and the non-ignition limit gap length (not ignitable beyond that gap length).
  • a greater critical gap length value represents a higher shock ignition sensitivity.
  • the greater the critical ignition gap length the higher is the shock ignition sensitivity and, hence, the risk of hazards.
  • ADCA Azodicarbonamide
  • a halogen oxo acid salt with or without a combustion control catalyst, were blended according to the formulas (wt. %) shown in Table 4 to provide compositions of this invention.
  • An air bag inflator reactor was loaded with 20 g of pellets (12.3 mm dia. x 3 mm thick) of the composition of this invention comprising 45 parts by weight of azodicarbonamide, 55 parts by weight of sodium chlorate and 2.75 parts by weight of MnO 2 and the loaded inflator was connected to a 28.6-liter tank equipped with a pressure sensor. Using 1 g of B-KNO 3 , the pellets were ignited for combustion. The maximum pressure within the tank was 4.3 kgf/cm 2 gauge and the tank internal pressure rise time associated with combustion of this composition was 50 ms.
  • ADCA azodicarbonamide
  • a control gas generating composition was prepared according to the suggestion made in JP-B 21171/74. Thus, 200 parts by weight of azodicarbonamide was blended with 90 parts by weight of sodium chlorate and 10 parts by weight of Zr powder to provide a control composition.
  • composition of this invention was subjected to the strand burner test (cf. "Combustion characteristics of sodium aside gas generating systems", the Proceedings of the 1992 Annual Meeting of the Industrial Explosives Association, Pages 98-99).
  • the measured burning velocities were 28.3 mm/sec. at 10 kgf/cm 2 , 37.9 mm/s at 20 kgf/cm 2 , and 46.0 mm/s at 40 kgf/cm 2 .
  • the burning velocity (mm/sec.) was measured as in Example 8. No ignition occurred at 10 kgf/cm 2 . At 40 kgf/cm 2 , the burning velocity was 48.3 mm/s.
  • An air bag inflator reactor was loaded with 40 g of pellets (12.3 mm in diameter x 3 mm thick) of the composition of this invention as obtained by blending 45 parts by weight of azodicarbonamide with 55 parts by weight of potassium perchlorate and 10 parts by weight of copper oxide and this inflator was connected to a 28.6-liter tank equipped with a pressure sensor.
  • the pellets were ignited with 1 g of B-KNO 3 for combustion of the composition of this invention.
  • Fig. 1 is a longitudinal section view showing the gas trapping bomb used in the bomb test.
  • Figs. 2 and 3 are diagrammatic illustrations showing the chamber mounted in the gas trapping bomb on exaggerated scale.
  • Figs. 4-7 are diagrammatic representations of the procedure of the shock sensitivity test.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Air Bags (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)

Claims (8)

  1. Gaserzeugende Zusammensetzung für Airbags, bestehend aus Azodicarbonamid, einem Halogenoxosäuresalz und gegebenenfalls mindestens einer Substanz ausgewählt aus Verbrennungregelungskatalysatoren, Antidetonationsmitteln, Sauerstoffdonor-Verbindungen, Verbrennungstemperatur-Reguliermifteln und Verbrennungsgeschwindigkeits-Reguliermitteln, wobei das Halogenoxosäuresalz in einer Menge von 20 bis 233.3 Gewichtsteilen pro 100 Gewichtsteile Azodicarbonamid vorliegt und die Zusammensetzung frei von reduzierendem Metall ist.
  2. Gaserzeugende Zusammensetzung nach Anspruch 1, worin das Halogenoxosäuresalz ein Halogenat und/oder ein Perhalogenat ist.
  3. Gaserzeugende Zusammensetzung nach Anspruch 2, worin das Halogenat ein Alkalimetallhalogenat ist.
  4. Gaserzeugende Zusammensetzung nach Anspruch 2, worin das Perhalogenat ein Alkalimetallperhalogenat ist.
  5. Gaserzeugende Zusammensetzung nach Anspruch 1, worin der Verbrennungsregelungskatalysator mindestens eine aus den Oxiden, Chloriden und Carbonaten der Elemente der Gruppe IV und der Gruppe VI des Periodensystems der Elemente ausgewählte Substanz ist.
  6. Gaserzeugende Zusammensetzung nach Anspruch 1, worin der Verbrennungsregelungskatalysator mindestens eine aus Cellulose-Verbindungen und organischen Polymeren ausgewählte Substanz ist.
  7. Geformte Masse, bestehend aus einer gaserzeugenden Zusammensetzung für Airbags nach irgendeinem der Ansprüche 1 bis 6 und einem Bindemittel.
  8. Geformte Masse nach Anspruch 7 als Pellet, Scheibe, Kugel, Stab, Hohlzylinder, Dragee oder Tetrapod.
EP93910338A 1992-07-13 1993-05-13 Gaserzeugungsmittel für airbags Expired - Lifetime EP0607446B1 (de)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
JP185253/92 1992-07-13
JP4185253A JPH0632690A (ja) 1992-07-13 1992-07-13 エアバッグ用ガス発生剤
JP4185251A JPH0632689A (ja) 1992-07-13 1992-07-13 エアバッグ用ガス発生剤
JP185251/92 1992-07-13
PCT/JP1993/000634 WO1994001381A1 (en) 1992-07-13 1993-05-13 Gas generating agent for air bags

Publications (3)

Publication Number Publication Date
EP0607446A1 EP0607446A1 (de) 1994-07-27
EP0607446A4 EP0607446A4 (de) 1995-03-29
EP0607446B1 true EP0607446B1 (de) 1999-02-03

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Application Number Title Priority Date Filing Date
EP93910338A Expired - Lifetime EP0607446B1 (de) 1992-07-13 1993-05-13 Gaserzeugungsmittel für airbags

Country Status (5)

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EP (1) EP0607446B1 (de)
KR (1) KR100242401B1 (de)
CA (1) CA2115557C (de)
DE (1) DE69323410T2 (de)
WO (1) WO1994001381A1 (de)

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JPH11292678A (ja) 1998-04-15 1999-10-26 Daicel Chem Ind Ltd エアバッグ用ガス発生剤組成物
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Also Published As

Publication number Publication date
EP0607446A4 (de) 1995-03-29
DE69323410T2 (de) 1999-09-02
KR100242401B1 (ko) 2000-02-01
EP0607446A1 (de) 1994-07-27
WO1994001381A1 (en) 1994-01-20
DE69323410D1 (de) 1999-03-18
CA2115557C (en) 2000-07-25

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