EP0659712B1 - Elastomere-Thermoplaste-Bindemittel enthaltende gaserzeugende pyrotechnische Zusammensetzung zur Herstellung eines reinen, nicht toxischen Gases - Google Patents

Elastomere-Thermoplaste-Bindemittel enthaltende gaserzeugende pyrotechnische Zusammensetzung zur Herstellung eines reinen, nicht toxischen Gases Download PDF

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Publication number
EP0659712B1
EP0659712B1 EP94402714A EP94402714A EP0659712B1 EP 0659712 B1 EP0659712 B1 EP 0659712B1 EP 94402714 A EP94402714 A EP 94402714A EP 94402714 A EP94402714 A EP 94402714A EP 0659712 B1 EP0659712 B1 EP 0659712B1
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Prior art keywords
binder
composition according
pyrotechnic composition
weight
plasticizer
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EP94402714A
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English (en)
French (fr)
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EP0659712A1 (de
Inventor
Bernard Finck
Alain Lefumeux
Christian Perotto
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Societe Nationale des Poudres et Explosifs
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Societe Nationale des Poudres et Explosifs
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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
    • 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
    • C06B45/105—The resin being a polymer bearing energetic groups or containing a soluble organic explosive

Definitions

  • the present invention relates to the field of automotive safety and, more specifically, that of the protection, in the event of a collision, of the occupants of a motor vehicle thanks to cushions inflated by combustion gas of a pyrotechnic composition contained in a gas generator.
  • the invention relates to gas-generating pyrotechnic compositions clean and non-toxic, containing a binder thermoplastic.
  • compositions therefore requires gas generators equipped with powerful filtration means gases.
  • compositions described in this application are mainly consisting of the reaction product of a glycidyl polyazide with a polyisocyanate such as binder and with ammonium nitrate as oxidizing charge. These compositions give all satisfaction to the plan of gas non-toxicity, speed of combustion and the absence of solid residue but however, they are delicate to implement, especially in continuous processes involving a extrusion phase, due to the fact that they use crosslinkable binders which harden very quickly.
  • thermoplastic binder in composite compositions of this type would allow a easier to use, especially for processes continuous; but, if the use of compositions pyrotechnics with thermoplastic binder as propellants for rockets or as explosives is known, for example by USP patents 4,806,613, 4,875,949 and 4,925,503, their job in automotive safety is little used to this day. Indeed the pyrotechnic compositions thermoplastic binder composites known to date do not do not meet all of the requirements in field.
  • US-A 4,806,613 describes, for example, pyrotechnic compositions with binders thermoplastics which may contain (i) a plasticizer energy like nitroglycerin, butanetriol trinitrate (BTTN) or the trimethylolethane trinitrate (TMETN), (ii) an oxidizing charge mineral or organic, (iii) aluminum powder and (iv) additives known to those skilled in the art.
  • BTTN nitroglycerin, butanetriol trinitrate
  • TMETN trimethylolethane trinitrate
  • an oxidizing charge mineral or organic iii
  • aluminum powder aluminum powder and additives known to those skilled in the art.
  • the object of the present invention is precisely to propose such compositions.
  • the invention therefore relates to a composition pyrotechnics whose combustion products are mainly non-toxic clean gases, consisting essentially by a binder which is an elastomer thermoplastic, by an energy plasticizer, by a mineral oxidizing charge and by additives intended for regulate combustion, characterized in that said binder is an oxygenated thermoplastic elastomer, in that that the said plasticizer is a product of polymerization of glycidyl azide and in that the said oxidizing charge is constituted for at least 85% of its weight by ammonium nitrate.
  • the said binder is a block copolymer consisting mainly with polyamide patterns and polyether patterns.
  • the said energy plasticizer is a polyazide of glycidyl with hydroxyl endings whose molecular mass number average is between 1,000 and 7,000.
  • the said additives are chosen from the group consisting of potassium nitrate and perchlorate ammonium.
  • the energy binder / plasticizer set represents between 5 and 15% of the total weight of the composition, the weight of the energy plasticizer representing approximately 30% of the binder weight.
  • compositions according to the invention burn quickly in essentially releasing as combustion gases from nitrogen and carbon dioxide with very little carbon monoxide. Furthermore, they do not produce little or no residue, depending on the additives used solid.
  • pyrotechnic gas generators intended for inflate protective cushions for occupants of a motor vehicle.
  • binder of an elastomer gives granules or blocks of pyrotechnic composition of mechanical properties particularly interesting for products intended to be kept for many years in a motor vehicle.
  • the invention therefore relates to pyrotechnic compositions whose combustion products are mainly clean, non-toxic gases. These compositions are essentially made up of a binder, by an energetic plasticizer, by an oxidizing charge mineral and by additives intended to regulate the combustion of the composition.
  • This type of block copolymer is marketed by ATOCHEM company under the PEBAX® brand.
  • an energy plasticizer is added to the binder which is a product of polymerization of azide glycidyl.
  • a favorite family of plasticizers energy consists of the polyazides of glycidyle with hydroxyl endings whose mass number average molecular is between 1,000 and 7,000 and, preferably between, 1,500 and 2,500.
  • the glycidyl polyazides to hydroxyl endings do not participate in any reaction chemical condensation; they are therefore well used as an energy plasticizer for the thermoplastic elastomer and not as a component of the binder as is usually the case when used in the presence of an isocyanate or other reactive agent with the hydroxyl groups OH.
  • the energy binder / plasticizer set represents preferably between 5% and 15% of the total weight of the composition while the weight of said plasticizer energy preferably represents around 30% of the weight of the binder / plasticizer assembly.
  • the pyrotechnic composition contains a oxidizing charge formed for at least 85% of its weight by ammonium nitrate.
  • an ammonium nitrate will be used stabilized.
  • the stabilizer could for example be consisting of a little nickel oxide NiO.
  • This quality of ammonium nitrate is sold commercially and generally contains 3% by weight of nickel oxide compared to pure ammonium nitrate.
  • the expression "ammonium nitrate” covers the assembly consisting of pure ammonium nitrate and by any stabilizer present.
  • nickel oxide is non-combustible, its presence in small amount is not a problem in the context of present invention.
  • the entire oxidizing charge can be consisting of ammonium nitrate but it is imperative in the context of the present invention that the ammonium nitrate represents, by weight, at least 85% of the oxidizing charge.
  • the oxidizing charge When the oxidizing charge is not formed at 100% with ammonium nitrate, it can be supplemented with triaminoguanidinium nitrate, with nitroguanidine or by a nitramine such as hexogen or octogen.
  • compositions according to the invention also contain additives intended in particular for adjust the rate of combustion of the composition in the pressure range corresponding to the operation of the generator.
  • additives exclude metals or compounds metal likely to constitute residues solids entrainable by combustion gases.
  • These additives could for example be carbon black or m-methyl p-nitroaniline.
  • these additives can also be selected from the group consisting of nitrate of potassium and ammonium perchlorate, additives also playing in the latter case the role of charge oxidizing.
  • compositions as part of the present invention contain as additives a mixture potassium nitrate and ammonium perchlorate, the potassium nitrate representing approximately 7% by weight ammonium nitrate and ammonium perchlorate representing between 4 and 6% of the total weight of the composition.
  • compositions according to the invention can easily be done continuously or batchwise in a mixer-extruder using solvent or solvent-free techniques known from the skilled person.
  • a mixer heated extruder usually at a temperature between 80 ° C and 130 ° C, and preferably at a temperature close to 120 ° C.
  • the binder is introduced and the energy plasticizer then we add the charge oxidizing agent and any additives.
  • the coating load and additives by the binder is complete the paste obtained is extruded to the desired geometry and let cool.
  • the binder using a suitable solvent in a mixer extruder.
  • Binder solvent should not dissolve or chemically attack the oxidative charge and additives.
  • the light alcohols such as ethanol, propanol and preferably butanol, light hydrocarbons such as kerosene or benzene, methyl ethyl ketone, chlorinated or fluorinated hydrocarbons such as chloride methylene, trichlorethylene, perchlorethylene or trichlorofluoromethane.
  • compositions according to the invention burn with speeds compatible with safety requirements automobile by releasing combustion gases essentially consisting of nitrogen and dioxide carbon monoxide content is located within the limits allowed for the automotive safety. Furthermore, these compositions do not produce little or no residue solids, so they can be used in gas generators without a filtration chamber or fitted with very simple filtration devices. Finally the presence of a binder which is an elastomer having elastic properties improves resistance mechanics of the loads arranged inside the gas generators.
  • This block was burned in a gas generator. The combustion was done without solid residues and the carbon monoxide content reduced to a useful volume of 2.7 m 3 which is the standard volume of a passenger compartment of a motor vehicle, was 40 ppm.
  • an 8 g block of double-base powder with nitrocellulose and nitroglycerin gives a similar gas yield but provides a carbon monoxide content of 1000 ppm for a useful volume of 2.7 m 3 .
  • This block was burned in a gas generator. Combustion produced 6% by weight of solid residue based on potassium chloride but the speed of combustion was greater than that of Example 1.
  • the carbon monoxide content reduced to a useful volume of 2.7 m 3 was 40 ppm.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Molecular Biology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Air Bags (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (8)

  1. Pyrotechnische Zusammensetzung zur Erzeugung eines Gases, das zum Aufblasen von Kissen zum Schutz von Kraftfahrzeuginsassen bestimmt ist, bestehend im wesentlichen aus einem Bindemittel, bei dem es sich um ein thermoplastisches Elastomeres handelt, aus einem energetischen Weichmacher, einem oxidierenden Füllstoff und zur Regelung der Verbrennung bestimmten Additiven, dadurch gekennzeichnet, daß es sich beim Bindemittel um ein sauerstoffhaltiges thermoplastisches Elastomeres handelt, daß es sich beim Weichmacher um ein Polymerisationsprodukt von Glycidylazid handelt und daß der oxidierende Füllstoff zu mindestens 85 Gew.-% aus Ammoniumnitrat besteht.
  2. Pyrotechnische Zusammensetzung nach Anspruch 1, dadurch gekennzeichnet, daß es sich beim Bindemittel um ein aliphatisches Blockcopolymeres handelt, das vorwiegend aus Polyamid-Einheiten und Polyether-Einheiten besteht.
  3. Pyrotechnische Zusammensetzung nach Anspruch 2, dadurch gekennzeichnet, daß es sich beim Bindemittel um ein aliphatisches Blockcopolymeres der folgenden Formel handelt: in der:
    Figure 00180001
    C, H und O Kohlenstoff, Wasserstoff bzw. Sauerstoff bedeuten,
    PA ein durch Kondensation von Dodecandisäure mit 1,12-Dodecandiamin erhaltenes Blockpolyamid bedeutet,
    PE einen durch Kondensation von Tetramethylenglykol erhaltenen Blockpolyether bedeutet und
    n eine ganze Zahl von 2 bis 10 bedeutet.
  4. Pyrotechnische Zusammensetzung nach Anspruch 2, dadurch gekennzeichnet, daß es sich beim energetischen Weichmacher um Polyglycidylazid mit Hydroxylendgruppen handelt, dessen durchschnittliche Molekülmasse 1000 bis 7000 beträgt.
  5. Pyrotechnische Zusammensetzung nach Anspruch 4, dadurch gekennzeichnet, daß die durchschnittliche Molekülmasse des Polyglycidylazids mit endständigen Hydroxylgruppen 1500 bis 2500 beträgt.
  6. Pyrotechnische Zusammensetzung nach Anspruch 2, dadurch gekennzeichnet, daß die Additive aus der Gruppe Kaliumnitrat und Ammoniumperchlorat ausgewählt sind.
  7. Pyrotechnische Zusammensetzung nach Anspruch 2, dadurch gekennzeichnet, daß die Gesamtmenge aus Bindemittel/energischem Weichmacher 5 bis 15 Gew.-% des Gesamtgewichts der Zusammensetzung ausmacht.
  8. Pyrotechnische Zusammensetzung nach Anspruch 7, dadurch gekennzeichnet, daß das Gewicht des energetischen Weichmachers etwa 30 Gew.-% der Gesamtmenge aus Bindemittel/Weichmacher ausmacht.
EP94402714A 1993-12-07 1994-11-29 Elastomere-Thermoplaste-Bindemittel enthaltende gaserzeugende pyrotechnische Zusammensetzung zur Herstellung eines reinen, nicht toxischen Gases Expired - Lifetime EP0659712B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9314642A FR2713632B1 (fr) 1993-12-07 1993-12-07 Compositions pyrotechniques génératrices de gaz propres et non toxiques, contenant un liant élastomère thermoplastique.
FR9314642 1993-12-07

Publications (2)

Publication Number Publication Date
EP0659712A1 EP0659712A1 (de) 1995-06-28
EP0659712B1 true EP0659712B1 (de) 1998-07-15

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Country Status (5)

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US (1) US5525171A (de)
EP (1) EP0659712B1 (de)
JP (1) JP2793514B2 (de)
DE (1) DE69411691T2 (de)
FR (1) FR2713632B1 (de)

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GB2310427B (en) * 1996-02-22 2000-06-28 John Douglas Michael Wraige Energetic compositions
FR2750422B1 (fr) * 1996-06-28 1998-08-07 Poudres & Explosifs Ste Nale Compositions pyrotechniques generatrices de gaz propres et application a un generateur de gaz pour la securite automobile
US5847311A (en) * 1996-10-22 1998-12-08 Trw Vehicle Safety Systems Inc. Hybrid inflator with crystalline and amorphous block copolymer
FR2757118B1 (fr) * 1996-12-18 1999-01-08 Livbag Snc Generateur tubulaire integral de gaz par voie pyrotechnique, pour gonfler des coussins de protection
FR2757266B1 (fr) 1996-12-18 1999-01-08 Livbag Snc Generateur pyrotechnique de gaz a chargement composite
JP3641343B2 (ja) * 1997-03-21 2005-04-20 ダイセル化学工業株式会社 低残渣エアバッグ用ガス発生剤組成物
JP3608902B2 (ja) * 1997-03-24 2005-01-12 ダイセル化学工業株式会社 ガス発生剤組成物及びその成型体
DE19742203A1 (de) * 1997-09-24 1999-03-25 Trw Airbag Sys Gmbh Partikelfreies gaserzeugendes Gemisch
FR2772750B1 (fr) * 1997-12-22 2000-01-28 Poudres & Explosifs Ste Nale Composition pyrotechnique generatrice de gaz propres, a faible teneur en oxyde d'azote, et pastilles d'une telle composition
US6143103A (en) * 1998-01-27 2000-11-07 Trw Inc. Gas generating material for vehicle occupant protection device
FR2778576B1 (fr) 1998-05-15 2000-06-23 Poudres & Explosifs Ste Nale Dispositif d'extinction d'incendie comportant un generateur thermochimique de gaz
DE69834107T2 (de) 1998-07-13 2006-09-21 Nof Corp. Gaserzeugende Zusammensetzungen
US6296724B1 (en) * 1998-07-21 2001-10-02 Trw Inc. Gas generating composition for an inflatable vehicle occupant protection device
US6395112B1 (en) 2000-02-04 2002-05-28 The United States Of America As Represented By The Secretary Of The Navy Hydrolyzable polymers for explosive and propellant binders
US6802533B1 (en) * 2000-04-19 2004-10-12 Trw Inc. Gas generating material for vehicle occupant protection device
JP2012106882A (ja) * 2010-11-17 2012-06-07 Nippon Kayaku Co Ltd エンハンサー剤組成物、及びそれを用いたガス発生器
WO2014024322A1 (en) 2012-08-10 2014-02-13 National Institute For Materials Science Glycidyl 4-functionalized-1,2,3-triazole polymer derivatives and method for synthesis of the same

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Also Published As

Publication number Publication date
EP0659712A1 (de) 1995-06-28
JPH07215790A (ja) 1995-08-15
FR2713632B1 (fr) 1996-01-12
US5525171A (en) 1996-06-11
FR2713632A1 (fr) 1995-06-16
DE69411691T2 (de) 1998-12-24
JP2793514B2 (ja) 1998-09-03
DE69411691D1 (de) 1998-08-20

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