EP1216977B1 - Compositions pyrotechniques génératrices de gaz à liant hydrocarboné et procédé de fabrication en continu - Google Patents

Compositions pyrotechniques génératrices de gaz à liant hydrocarboné et procédé de fabrication en continu Download PDF

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Publication number
EP1216977B1
EP1216977B1 EP01403255A EP01403255A EP1216977B1 EP 1216977 B1 EP1216977 B1 EP 1216977B1 EP 01403255 A EP01403255 A EP 01403255A EP 01403255 A EP01403255 A EP 01403255A EP 1216977 B1 EP1216977 B1 EP 1216977B1
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EP
European Patent Office
Prior art keywords
nitrate
composition
gum
binder
compartment
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
EP01403255A
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German (de)
English (en)
French (fr)
Other versions
EP1216977A2 (fr
EP1216977A3 (fr
Inventor
Dimitri Charrette
Georges Chounet
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.)
Safran Ceramics SA
Original Assignee
SNPE Materiaux Energetiques SA
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Publication date
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Publication of EP1216977A2 publication Critical patent/EP1216977A2/fr
Publication of EP1216977A3 publication Critical patent/EP1216977A3/fr
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B25/00—Compositions containing a nitrated organic compound
    • 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
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033—Shaping the mixture
    • C06B21/0075—Shaping the mixture by extrusion
    • 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
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
    • 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

Definitions

  • the present invention relates to the field technical pyrotechnic generation of gas usable especially in protection systems occupants of a motor vehicle by means of cushions that are inflated by the flue gases of a pyrotechnic loading. More specifically, the invention pyrotechnic compositions generating to acceptable temperatures for automotive safety clean and non-toxic gases. The invention relates to also a continuous manufacturing process of such compositions.
  • pyrotechnic gas generators For different pyrotechnic needs including to ensure proper inflation of the cushions protection, pyrotechnic gas generators must provide in extremely short times, the order of thirty milliseconds, clean gases that is to say free from solid particles likely to constitute hot spots that can damage the wall cushion, and non-toxic that is to say low levels of nitrogen oxides, carbon oxides and chlorinated products.
  • a first family concerns compositions to base of alkaline or alkaline earth azide in the presence a mineral oxidant such as potassium nitrate or of a metal oxide.
  • These compositions that can binder, where appropriate, have major disadvantages. On the one hand, they produce of their combustion a lot of dust that must be filtered by filtration systems relatively large, which increases both the weight and price of the generator.
  • azides are very toxic products that exhibit in addition, the possibility of forming azides of lead or other heavy metals that are explosives primary. These compositions are therefore difficult to keep in good condition for several years in a motor vehicle.
  • compositions to nitrocellulose and nitroglycerin base are very interesting because they burn very quickly and without producing dust. But they have the disadvantage of not to be totally stable over time, and at high temperature.
  • a third family concerns compositions so-called "composites” constituted basically by a organic binder and an oxidizing mineral filler as especially mineral perchlorate. These compositions are a priori very interesting because they present good burning speed and excellent aging stability.
  • compositions have also been proposed constituted by a silicone binder crosslinkable to ambient temperature, still known as RTV (Room Temperature Vulcanizable), and potassium perchlorate, the potassium atom playing the role of internal chlorine sensor.
  • RTV Room Temperature Vulcanizable
  • Such compositions are, for example, described in FR-A-2 190 776 and FR-B-2 213 254 or in their corresponding US-A-3,986,908 and US-A-3,964,256. These compositions, however, the disadvantage of generating very rich oxygen gases that are not sought after by the builders of automobile industry.
  • compositions consisting of a silicone binder and a mixture of ammonium perchlorate and sodium nitrate. Of such compositions do not contain a solvent. They are for example described in the French patent FR-A-2 728 562 or in its American correspondent US-A-5,610,444. These compositions generate many gases clean, high in nitrogen and non-toxic but present the disadvantage of burning at very high temperatures and to produce a high solid residue rate.
  • compositions exist involve the presence of a solvent for adjust the viscosity.
  • a solvent for adjust the viscosity.
  • the use of a solvent has many disadvantages and especially at the level of industrial.
  • the solvent must be removed from the composition and this operation may create porosity in the pyrotechnic charge.
  • the object of the present invention is precisely to propose such compositions and a process allowing them to be implemented.
  • the invention therefore relates to a composition pyrotechnic gas generator comprising a binder, a nitrogenous organic compound, additives and a charge oxidizing agent comprising ammonium perchlorate and a chlorine sensor, said binder being a binder at least two components hydrocarbon, one of the components being constituted by an eraser, characterized in that when the gum is a polyester gum, it is associated with a polyester resin and in that, when the gum is an acrylic gum, it is associated with one of its plasticizers.
  • a gum is called a polymer whose mass molecular weight is greater than 200 000.
  • Acrylic gums used are also called rubbers acrylics or polyacrylates. These erasers may have reactive terminations of the chlorine / carboxyl type, chlorine, hydroxyl or epoxy.
  • polyester gums used are rubbers with ester motives and which may have reactive terminations of the hydroxyl type.
  • the binder is constituted by the combination of an eraser acrylic and one of its plasticizers.
  • the plasticizer of the acrylic gum is chosen from the group consisting of by dioctyl adipate and dioctyl azelate.
  • a crosslinking agent will generally be associated with the binder.
  • the binder is constituted by the combination of an eraser polyester and a polyester resin.
  • the composition further comprises an isocyanate type crosslinking agent.
  • the weight content of the charges is greater than or equal to 85% of the total weight of the composition.
  • the oxidizing charge comprises perchlorate ammonium and a chlorine sensor.
  • the chlorine sensor is selected from the group consisting of nitrate sodium, calcium carbonate, carbonate of lithium, potassium nitrate, nitrate strontium, barium nitrate, chlorate potassium, potassium perchlorate and copper.
  • a preferred chlorine sensor is nitrate sodium.
  • the composition also comprises a compound organic nitrogen.
  • the nitrogenous organic compound is chosen in the group consisting of nitroguanidine, the guanidine nitrate, aminoguanidine nitrate, oxamide, dicyandiamide, guanylurea nitramide and metallic cyanamides.
  • the content weight of this nitrogen compound is between 3 and 15% of the total weight of the composition.
  • the composition further comprises a ballistic catalyst selected from the group consisting of titanium oxide, copper oxide, basic copper nitrate, copper chromite and iron oxide.
  • a ballistic catalyst selected from the group consisting of titanium oxide, copper oxide, basic copper nitrate, copper chromite and iron oxide.
  • the catalyst Ballistic preferred is iron oxide.
  • Content weight of the ballistic catalyst is preferably between 0% and 4% of the weight total of the composition.
  • the The composition further comprises a wetting agent.
  • This wetting agent is selected from the group consisting of organosilanes, titanates and aziridines.
  • the Preferred organosilanes are the trialkoylsilanes the functional group is a vinyl, epoxy, amine group or metacrylic.
  • the weight content of the wetting agent is preferably between 0.5% and 2% by weight total of the composition.
  • This component reduces porosity residual product.
  • the ballistic catalyst and the wetting agent constitute the preferred additives of the compositions according to the invention.
  • the nitrogenous organic compound and gum are premixed and introduced into the mixing and mixing by the feed opening of the solids.
  • the pressure of the compression compartment is less than 50 ⁇ 10 3 Pa, ie 500 mbar.
  • the temperature of the mixing compartment and mixing is between 15 ° C and 75 ° C.
  • the pressure in the extrusion head is between 6.10 6 Pa and 15.10 6 Pa, ie between 60 bars and 150 bars.
  • the hydrocarbon binder comprises a an eraser and a liquid component which is either a resin or a plasticizer.
  • a pasty binder When we incorporate in this binder the oxidizing charge, the nitrogenous organic compound and various additives, this binder has sufficient resistance to be extruded in the form of rushes. So there is no need neither thickening agent nor solvent.
  • the rushes are then cut into loads and the binder structure is definitely frozen by crosslinking in an oven at a temperature between 100 ° C and 150 ° C.
  • Figure 1 represents, in the form of partly cut-off diagram, an installation allowing the implementation of the method according to the invention.
  • the bis-screw extruder-mixer 1 comprises a part upstream 2 in which the operations of mixing and kneading of the composition, a part downstream 3 in which takes place the degassing operation of the composition and an extrusion head 4.
  • a plug is formed of material that separates the downstream part 2 of the part upstream 3.
  • the gum and the nitrogenous organic compound are premixed.
  • the gum will be an eraser acrylic and the nitrogen compound will be nitrate guanidine.
  • the inert constituents namely the plasticizer and the various additives.
  • the various constituents are introduced continuously into the mixing and mixing chamber.
  • Solids A are introduced without solvent by means of a hopper.
  • the B liquids are introduced without solvent by means of a dosing pump 6.
  • the liquids B consist of the plasticizer and the wetting agent.
  • Solids A are the acrylic gum / guanidine nitrate mixture, the charge oxidizing agent comprising ammonium perchlorate and additives other than wetting agent.
  • Ammonium perchlorate particles are used two different grain sizes.
  • the particle size is between 10 ⁇ m and 50 ⁇ m.
  • Ammonium perchlorate producing by combustion chlorinated derivatives it is attached a sensor of chlorine.
  • the preferred chlorine sensor in the context of the invention is sodium nitrate which fixes the chlorine in the form of sodium chloride submicron, so without risk of deterioration of airbag walls.
  • Sodium nitrate will also be introduced by the feed opening of solids A.
  • the ratio between ammonium perchlorate and sodium nitrate is between 1 and 2.
  • the rate of oxidizing charges is preferentially about 80% of the total weight of the composition, for have a fairly balanced composition in balance in oxygen.
  • the weight content of the charges i.e. oxidizing charge, nitrogenous organic compound and additives
  • the weight content of the charges is greater than or equal to 85% of the total weight of composition. These are therefore binder compositions heavily loaded.
  • the content of the composition by binding and crosslinker will advantageously be close to 15%.
  • the preferred additives are the wetting agent and the ballistic catalyst.
  • the preferred ballistic catalyst is iron oxide.
  • the constituents are transported and kneaded in the mixing and mixing compartment 2.
  • the constituents are mixed using the elements of kneading 7 so as to form a homogeneous paste.
  • the temperature within this compartment is included between 15 ° C and 75 ° C.
  • the dough formed in the mixing and mixing compartment 2 is then degassed in the compression compartment 3, at a pressure of less than 30 ⁇ 10 3 Pa, ie 300 mbar.
  • This paste is then extruded, by means of a extrusion head 4, in the form of rods 8.
  • the pressure in the extrusion head is preferably close to 100 bars.
  • These rods are then cut into loads 9 to using a cutting device 10.
  • These loads 9 are recovered by a conveyor belt 11 and conveyed to an oven 12.
  • This oven 12 is heated to a temperature between 100 and 150 ° C. Preferably, this oven is heated to 120 ° C.
  • the loads remain in this oven for about 3 hours in order to complete the crosslinking of the constituents of the binder and to thus freeze the load structure 9.
  • the loads 9 have the shape of hollow cylindrical blocks presenting the more often axial channels.
  • the loads thus formed find their preferential application as loading pyrotechnics in gas generators intended for inflate a protective cushion for occupants of a motor vehicle. Indeed, the speed of combustion of these shipments, as well as the rate of solid residues products and the rate of carbon monoxide and oxides nitrogen products are particularly suitable for automotive safety requirements.
  • the weight content of the charges is 88%.
  • the combustion temperature of this composition is of the order of 2400 ° C.
  • the burning rate is 33mm / s under 20 MPa.
  • the weight content of the charges is 87.9%
  • the combustion temperature of this composition is of the order of 2400 ° C.
  • the burning rate is 43mm / s under 20 MPa.
  • the weight content of the charges is 85%.
  • the combustion temperature of this composition is of the order of 2400 ° C.
  • the burning rate is 20mm / s under 20Mpa.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Air Bags (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
EP01403255A 2000-12-22 2001-12-14 Compositions pyrotechniques génératrices de gaz à liant hydrocarboné et procédé de fabrication en continu Expired - Lifetime EP1216977B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0016879A FR2818636B1 (fr) 2000-12-22 2000-12-22 Compositions pyrotechniques generatrices de gaz a liant hydrocarbone et procede de fabrication en continu
FR0016879 2000-12-22

Publications (3)

Publication Number Publication Date
EP1216977A2 EP1216977A2 (fr) 2002-06-26
EP1216977A3 EP1216977A3 (fr) 2002-09-11
EP1216977B1 true EP1216977B1 (fr) 2005-07-27

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EP01403255A Expired - Lifetime EP1216977B1 (fr) 2000-12-22 2001-12-14 Compositions pyrotechniques génératrices de gaz à liant hydrocarboné et procédé de fabrication en continu

Country Status (10)

Country Link
US (1) US6824626B2 (es)
EP (1) EP1216977B1 (es)
JP (1) JP3825316B2 (es)
KR (1) KR100446267B1 (es)
AT (1) ATE300508T1 (es)
BR (1) BR0106250B1 (es)
CA (1) CA2364135C (es)
DE (1) DE60112231T2 (es)
FR (1) FR2818636B1 (es)
MX (1) MXPA01012981A (es)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3687962B1 (fr) * 2017-09-29 2024-06-12 ArianeGroup SAS Composition generatrice de gaz

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FR3073775B1 (fr) * 2017-11-23 2020-12-25 Arianegroup Sas Installation d'extrusion munie d'un systeme de controle apte a detecter une anomalie
FR3099155B1 (fr) * 2019-07-25 2021-07-30 Arianegroup Sas Propergol solide composite
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3687962B1 (fr) * 2017-09-29 2024-06-12 ArianeGroup SAS Composition generatrice de gaz

Also Published As

Publication number Publication date
FR2818636A1 (fr) 2002-06-28
CA2364135A1 (fr) 2002-06-22
JP2002255679A (ja) 2002-09-11
US20020079031A1 (en) 2002-06-27
US6824626B2 (en) 2004-11-30
DE60112231T2 (de) 2006-05-24
EP1216977A2 (fr) 2002-06-26
KR20020051850A (ko) 2002-06-29
CA2364135C (fr) 2009-02-03
BR0106250A (pt) 2002-08-13
EP1216977A3 (fr) 2002-09-11
JP3825316B2 (ja) 2006-09-27
MXPA01012981A (es) 2002-10-21
FR2818636B1 (fr) 2003-02-28
KR100446267B1 (ko) 2004-09-01
ATE300508T1 (de) 2005-08-15
BR0106250B1 (pt) 2010-11-16
DE60112231D1 (de) 2005-09-01

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