EP0467731B1 - Pyrotechnische, einen anorganischen Binder enthaltende und ein nichttoxisches Gas erzeugende Zusammensetzung und Verfahren zu ihrer Herstellung - Google Patents

Pyrotechnische, einen anorganischen Binder enthaltende und ein nichttoxisches Gas erzeugende Zusammensetzung und Verfahren zu ihrer Herstellung Download PDF

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Publication number
EP0467731B1
EP0467731B1 EP91401701A EP91401701A EP0467731B1 EP 0467731 B1 EP0467731 B1 EP 0467731B1 EP 91401701 A EP91401701 A EP 91401701A EP 91401701 A EP91401701 A EP 91401701A EP 0467731 B1 EP0467731 B1 EP 0467731B1
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EP
European Patent Office
Prior art keywords
composition
binder
weight
alkali
constituents
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
EP91401701A
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English (en)
French (fr)
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EP0467731A1 (de
Inventor
Christian Perotto
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Livbag SAS
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Livbag SAS
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Anticipated expiration legal-status Critical
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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
    • C06B35/00—Compositions containing a metal azide

Definitions

  • the present invention relates to the field of automobile safety. More precisely, the invention relates to a new pyrotechnic composition generating non-toxic cold gases and its manufacturing process.
  • the composition according to the invention can in particular be used in pyrotechnic generators intended to inflate, in the event of an accident, protective cushions for occupants of a motor vehicle.
  • a group of pyrotechnic compositions satisfying these requirements is made up of compositions comprising an alkali or alkaline earth azide such as sodium azide and a mineral oxidant such as an alkali or alkaline earth nitrate, an alkali or alkaline earth perchlorate, a metal oxide, a metal sulfide or even sulfur.
  • Such compositions are for example described in American patents 4,369,079, 4,092,190, 4,243,443 or 4,203,787.
  • compositions have the drawback of requiring, in the generator, an effective filtration chamber since they give off during combustion many hot solid particles which are entrained with the combustion gases but which must absolutely not enter the bag. inflatable so as not to introduce hot spots. Furthermore, some of these particles, consisting of sodium oxide, are extremely corrosive.
  • the basic constituents, azide, oxidant and possibly silica are used in powder form.
  • the mixture is agglomerated by simple compression, generally in the form of pellets which are stored in the combustion chamber. These pellets do not have good mechanical cohesion and tend to deteriorate over time under the effect of vibrations transmitted by the motor vehicle. This mechanical alteration leads to an alteration of the combustion law of the composition.
  • sodium azide is a body sensitive to humidity and the generator containing this type of composition must be well protected against humidity.
  • the object of the present invention is to provide pyrotechnic compositions generating non-toxic cold gases based on azide which have good mechanical strength, good protection of the azide against humidity and a reduction in the solid particles emitted during combustion.
  • the invention therefore relates to a solid pyrotechnic composition generating non-toxic gases comprising at least one alkali or alkaline earth azide, a mineral oxidant chosen from the group consisting of alkali or alkaline earth nitrates, alkaline or alkaline earth perchlorates, metal oxides, metal sulfides and sulfur, characterized in that it contains an inorganic binder which is the product of an inorganic polycondensation reaction of mixtures based on alkali silico-aluminates and whose content by weight relative to the total weight of said composition is between 5% and 40%, said polycondensation reaction being carried out after mixing all the constituents of the composition.
  • the said mineral binder is the product of polymerization of a silico-aluminate of formula (Si2O5, Al2O2) and silica SiO2 in the presence of aqueous soda and / and aqueous potassium hydroxide.
  • the invention also relates to a process for manufacturing the compositions according to the invention characterized in that, after mixing and shaping of the various constituents of the composition, the said binder is first polymerized by heating said constituents in a sealed sealed enclosure and in that, in a second step, the composition is dried.
  • compositions according to the invention find a preferred application in pyrotechnic generators of non-toxic cold gases intended to inflate in the event of an accident, airbags for occupants of a motor vehicle.
  • the invention relates to a solid pyrotechnic composition generating non-toxic cold gases comprising at least one alkali or alkaline earth azide and a mineral oxidant.
  • azide sodium azide will advantageously be used.
  • mineral oxidant it is possible to use most of the mineral oxidants traditionally used in gas-generating compositions containing an azide and in particular alkali or alkaline earth nitrates, alkali or alkaline earth perchlorates, metal oxides, metal sulfides, sulfur.
  • mineral oxidant which can be used in the context of the present invention, potassium nitrate, calcium nitrate, potassium perchlorate, iron oxides, manganese dioxide, nickel oxide, molybdenum alone or in admixture with sulfur.
  • the mineral oxidants preferred in the context of the present invention are alkali or alkaline earth nitrates and in particular potassium nitrate.
  • a composition according to the invention contains a mineral binder.
  • the mineral binders which can be used in the context of the present invention are the product of an inorganic polycondensation reaction of mixtures based on alkaline silico-aluminates. These mineral polymers are obtained by polymerization of a mixture of silicon and aluminum oxides in the presence of aqueous soda and / or aqueous potassium hydroxide. They are, for example, described, with their methods of obtaining, in French patents 2,464,227, 2,489,290 and 2,489,291 or their American correspondents 4,349,386 and 4,472,199.
  • the preferred polymers in the context of the present invention are obtained by polymerization of a silico-aluminate of formula (Si2O5, Al2O2) and colloidal silica SiO2 in the presence of aqueous sodium hydroxide and / or aqueous potassium hydroxide.
  • a silico-aluminate of formula (Si2O5, Al2O2) and colloidal silica SiO2 in the presence of aqueous sodium hydroxide and / or aqueous potassium hydroxide.
  • poly (sialate-siloxo) of sodium and / or potassium and correspond to the formula following global: in which : M represents a sodium or potassium atom, If represents a silicon atom, Al represents an aluminum atom, O represents an oxygen atom, n represents an integer.
  • silico-aluminate oxide Si2O5, Al2O2 which is different from ordinary silico-aluminate (2SiO2, Al2O3) is for example described in French patent 2,621,260 or in its American correspondent 4,859,367.
  • compositions according to the invention may contain between 5% and 40% by weight of mineral binder relative to the total weight of the composition, and preferably between 10% and 30% by weight. Thanks to the presence of the mineral binder which, after polymerization, is a real cement, the compositions according to the invention exhibit remarkable mechanical resistance, in particular when they are in the form of pellets. It has also been observed by the applicant that, despite the presence of the mineral binder, the compositions according to the invention have a combustion rate which is entirely compatible with the standards imposed in terms of motor vehicle safety and which is even sometimes higher. at the burning speed of traditional equivalent compositions without binder.
  • the binder being entirely mineral, it does not generate any toxic gas during the combustion of the composition according to the invention and, after combustion, the compositions according to the invention have a mass of pulverulent residues much lower than the equivalent traditional compositions without binder because the polymerized binder does not disintegrate and functions, during combustion, as a first internal filter.
  • the compositions according to the invention therefore require in a pyrotechnic gas generator for airbag fewer filters and reduce the weight of the generator.
  • the presence of the polymerized mineral binder provides partial protection of the azide against humidity.
  • compositions according to the invention are therefore very suitable for constituting the loading of a pyrotechnic generator of non-toxic cold gases intended to inflate a safety bag for occupants of a motor vehicle.
  • the compositions according to the invention make it possible in particular to constitute in this case fillings in the form of pellets which have an excellent capacity of preservation over time.
  • the invention also relates to a process for manufacturing the compositions according to the invention.
  • This process consists, after having mixed the various constituents of the composition and having put them in the form of use of the composition, pellets, blocks or other forms, to first ensure the polymerization of said binder and secondly separate the drying of the composition.
  • the constituents of the solid compositions according to the invention are of two kinds: on the one hand the traditional constituents such as azide and mineral oxidants which are pulverulent solids and on the other hand the mineral binder which, before polymerization, is in the form liquid and most often is marketed in the form of two separate solutions.
  • the preferred binders of the invention are generally marketed in the form of an aqueous solution of silico-aluminate and of an aqueous solution of colloidal silica in soda and / or potash, the pH of which is generally close to 14.
  • the pulverulent constituents will be mixed in a solid mixer while the mineral binder is prepared not polymerized by mixing its constituent solutions.
  • the unpolymerized binder thus prepared does not react at room temperature and can be stored in the liquid state.
  • the unpolymerized mineral binder and the mixture of pulverulent solids are then introduced into a kneader and all the constituents of the composition are mixed by rotating the kneader.
  • the kneader will generally be cooled to avoid any heating of the constituents of the composition and any start of polymerization of the mineral binder.
  • the mixture of the constituents of the composition is put into the form desired for the final composition: generally pellets, blocks or granules. At this stage it is necessary to distinguish different types of mixtures according to the content of the mixture in non-polymerized liquid binder.
  • the mixtures in which the weight of unpolymerized binder is less than or equal to 15% of the total weight of the constituents of the composition have the consistency of a very slightly wet flour. These mixtures can be shaped by pelletizing, even if they have a slight tendency to form lumps. They can also be shaped by compression in a mold to form a block.
  • Mixtures in which the weight of non-polymerized binder is greater than 25% of the total weight of the constituents of the composition have the consistency of a flowable paste. They lend themselves well to the extrusion-injection technique to form granules.
  • the preferred surfactants of the applicant are phosphorus-containing organo titanates.
  • the mineral binder is first polymerized by heating the constituents.
  • the rate of polymerization increases with the heating temperature, but, taking into account the particular nature of the other constituents of the composition, the latter cannot be raised too much.
  • the Applicant has found that heating for 24 hours at 60 ° C. ensures complete polymerization without risk.
  • the polymerization reaction involves the participation of water molecules, it is important not to lose water by evaporation during polymerization. The applicant therefore recommends carrying out the polymerization in a sealed closed enclosure. It has been experimentally observed that water does not degrade the azide during this polymerization phase due to the strongly basic pH of the medium, and this despite the heating operation which accompanies the polymerization.
  • the composition is subsequently dried by removing excess water.
  • This drying is advantageously carried out by heating in a ventilated enclosure, at ordinary pressure or at reduced pressure.
  • a simple solution consists in maintaining the composition in the polymerization enclosure, the doors of which are opened, and in maintaining the heating at 60 ° C. for a new period of 24 hours.
  • compositions according to the invention are then available ready for use.
  • This example is given for comparison. It relates to a traditional composition, without binder, based on sodium azide, potassium nitrate and silica in the following proportions: NaN3 56 parts by weight KNO3 17 parts by weight If 27 parts by weight
  • composition cylinders were placed in a closed desiccator with 100% relative humidity in a ventilated oven at 60 ° C for 4 hours. We then measured their tensile strength which is almost zero.
  • a composition according to the invention was made from the following constituents: NaN3 69 parts by weight KNO3 21 parts by weight binder 10 parts by weight surfactant 0.1 part by weight
  • the surfactant used was a phosphorus organo-titanate marketed by the company KENRICH Pperichemicals under the name "LICA 12".
  • the powdered azide / nitrate mixture was prepared in a "Turbula" type solid mixer.
  • the preparation time was one hour.
  • the unpolymerized liquid binder was introduced and, after starting, the pulverulent mixture was added in successive fractions.
  • the total duration of the mixing was one hour.
  • the mixture of constituents thus obtained was put into the form of cylinders by compression.
  • the actual polymerization was carried out in a closed enclosure heated to 60 ° C. for 24 hours.
  • the drying was carried out in a ventilated oven, heated to 60 ° C, for 24 hours.
  • the breaking strength of these cylinders was more than 147N and their elasticity of 4.1%.
  • Example 2 The procedure was as in Example 2 starting from the following constituents: - NaN3 53.5 parts by weight - K NO3 16.3 parts by weight - binder 30 parts by weight - surfactant 0.2 parts by weight
  • the binder was obtained by mixing 13.4 parts by weight of solution B with 16.6 parts by weight of solution A.
  • the surfactant was the same as that used in set 2.
  • Example 3 The procedure was as in Example 3 starting from the following constituents: - NaN3 53.5 parts by weight - K NO3 16.3 parts by weight - binder 30 parts by weight
  • the binder was obtained by mixing 10.4 parts by weight of solution B with 19.6 parts by weight of solution A.
  • Example 3 The procedure was as in Example 3 starting from the following constituents: - NaN3 53.5 parts by weight - K NO3 16.2 parts by weight - binder 30 parts by weight - surfactant 0.3 parts by weight
  • the binder was obtained by mixing 10.4 parts by weight of solution B with 19.6 parts by weight of solution A.
  • the surfactant was the same as that used in Example 2.

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

Claims (10)

  1. Feste pyrotechnische, kalte ungiftige Gase erzeugende Zusammensetzung, die wenigstens ein Alkali- oder Erdalkalimetallnitrid und ein mineralisches Oxidationsmittel aufweist, das aus der aus den Alkali- oder Erdalkalimetallnitraten, den Alkali- oder Erdalkalimetallperchloraten, den Metalloxiden, den Metallsulfiden und dem Schwefel bestehenden Gruppe gewählt ist,
    dadurch gekennzeichnet,
    daß sie bezüglich des Gesamtgewichts der Zusammensetzung zwischen 5 und 40 Gew.% eines mineralischen Bindemittels enthält, das das Produkt einer mineralischen Polykondensationsreaktion eines Gemisches auf Basis von Silico-Alkalimetallaluminaten ist, wobei die Polykondensationsreaktion nach Vermischen der Gesamtheit der Bestandteile der Zusammensetzung erfolgt.
  2. Zusammensetzung nach dem Anspruch 1,
    dadurch gekennzeichnet,
    daß das Bindemittel das Polymerisationsprodukt eines Alumino-Silikats der Formel (Si₂O₅·Al₂O₂) und von Siliziumdioxid SiO₂ in Gegenwart von wässerigern NaOH und/oder KOH ist.
  3. Zusammensetzung nach dem Anspruch 1,
    dadurch gekennzeichnet,
    daß der Gewichtsgehalt an Bindemittel bezüglich des Gesamtgewichts der Zusammensetzung im Bereich von 10 % bis 30 % ist.
  4. Zusammensetzung nach dem Anspruch 1,
    dadurch gekennzeichnet,
    daß das mineralische Oxidationsmittel ein Alkali- oder Erdalkalimetallnitrat ist.
  5. Zusammensetzung nach dem Anspruch 4,
    dadurch gekennzeichnet,
    daß das mineralische Oxidationsmittel Kaliumnitrat ist.
  6. Zusammensetzung nach dem Anspruch 5,
    dadurch gekennzeichnet,
    daß das Nitrid Natriumnitrid ist.
  7. Verfahren zur Herstellung einer Zusammensetzung nach irgendeinem der Ansprüche 1 bis 6,
    dadurch gekennzeichnet,
    daß man nach Vermischung und Formgebung der verschiedenen Bestandteile der Zusammensetzung in einer ersten Zeit die Polymerisation des Bindemittels durch Erhitzung der Bestandteile in einem geschlossenen dichten Behälter sichert und daß man in einer zweiten Zeit die Trocknung der Zusammensetzung sichert.
  8. Verfahren nach dem Anspruch 7,
    dadurch gekennzeichnet,
    daß die Polymerisation bei einer Temperatur nahe 60 °C durchgeführt wird.
  9. Verfahren nach dem Anspruch 7,
    dadurch gekennzeichnet,
    daß die Trocknung durch Erhitzen der Zusammensetzung in einem belüfteten Behälter durchgeführt wird.
  10. Verfahren nach dem Anspruch 9,
    dadurch gekennzeichnet,
    daß die Temperatur während der Trocknung nahe 60 °C ist.
EP91401701A 1990-06-27 1991-06-25 Pyrotechnische, einen anorganischen Binder enthaltende und ein nichttoxisches Gas erzeugende Zusammensetzung und Verfahren zu ihrer Herstellung Expired - Lifetime EP0467731B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9008096A FR2663924B1 (fr) 1990-06-27 1990-06-27 Composition pyrotechnique generatrice de gaz non toxiques comportant un liant mineral et son procede de fabrication.
FR9008096 1990-06-27

Publications (2)

Publication Number Publication Date
EP0467731A1 EP0467731A1 (de) 1992-01-22
EP0467731B1 true EP0467731B1 (de) 1994-12-14

Family

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EP91401701A Expired - Lifetime EP0467731B1 (de) 1990-06-27 1991-06-25 Pyrotechnische, einen anorganischen Binder enthaltende und ein nichttoxisches Gas erzeugende Zusammensetzung und Verfahren zu ihrer Herstellung

Country Status (5)

Country Link
US (1) US5236526A (de)
EP (1) EP0467731B1 (de)
JP (1) JPH0725634B2 (de)
DE (1) DE69105846D1 (de)
FR (1) FR2663924B1 (de)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
US8574358B2 (en) 2005-12-06 2013-11-05 James Hardie Technology Limited Geopolymeric particles, fibers, shaped articles and methods of manufacture

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US5470406A (en) * 1992-04-10 1995-11-28 Nof Corporation Gas generator composition and process for manufacturing the same
DE59309691D1 (de) * 1992-09-21 1999-08-12 Honda Motor Co Ltd Gasgenerator für einen Airbag
US5566543A (en) * 1993-11-17 1996-10-22 Morton International, Inc. PVC-based gas generant for hybrid gas generators
US5536340A (en) * 1994-01-26 1996-07-16 Breed Automotive Technology, Inc. Gas generating composition for automobile airbags
US5650590A (en) * 1995-09-25 1997-07-22 Morton International, Inc. Consolidated thermite compositions
US6858566B1 (en) * 2002-05-31 2005-02-22 Halliburton Energy Services, Inc. Methods of generating gas in and foaming well cement compositions
FR2997695B1 (fr) * 2012-11-07 2014-12-12 Eurenco France Explosif solide a liant mineral geopolymerique
DE102015014821A1 (de) * 2015-11-18 2017-05-18 Rheinmetall Waffe Munition Gmbh REACh konformer pyrotechnischer Verzögerungs- und Anzündsatz mit variabel einstellbaren Leistungsparametern

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Publication number Priority date Publication date Assignee Title
US8574358B2 (en) 2005-12-06 2013-11-05 James Hardie Technology Limited Geopolymeric particles, fibers, shaped articles and methods of manufacture

Also Published As

Publication number Publication date
FR2663924A1 (fr) 1992-01-03
JPH0725634B2 (ja) 1995-03-22
US5236526A (en) 1993-08-17
EP0467731A1 (de) 1992-01-22
DE69105846D1 (de) 1995-01-26
JPH04240179A (ja) 1992-08-27
FR2663924B1 (fr) 1994-05-06

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