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
  • C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
  • C06B23/02—Compositions characterised by non-explosive or non-thermic constituents for neutralising poisonous gases from explosives produced during blasting
• • 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

Definitions

• the present invention relates to pyrotechnic compounds gas generators and a method for obtaining them.
• Said pyrotechnic compounds present:
• the intrinsic inflation power of a formulation is given by the product of the gaseous molar yield of said formulation (in mol / kg) by the temperature T (in K) .
• T in K
• the inflation surface flow rate is estimated by the product pxnx T x Vc, where p is the density of the material (in g / cm 3 ), n the molar gas yield of the combustion (in mole / g), T the combustion temperature (in K) and Vc the combustion rate in cm / s
• the inflation surface flow rate parameter is expressed in mol.K / cm 2 .s
• the present invention is in the technical field of pyrotechnic generation of gas. It is particularly applicable in vehicle occupant protection systems, protection by means of damping cushions (so-called "airbags”), which are inflated by the combustion gases of pyrotechnic compounds.
• airbags damping cushions
• the low temperature makes it possible to limit the thickness of the bag
• the gaseous effluents are generally of good quality vis-à-vis the acceptable toxicity standards in force in the field (USCAR).
• compositions on the other hand, have drawbacks that can penalize certain applications:
• the temperature being relatively low and the gas yield low, the inflation power is limited
• filters are necessary to reduce the emission of particles. These filters further reduce the inflation power due to the thermal losses they induce. The filters further induce an increase in the volume and cost of the generator;
• the "cold" compositions have, in almost all cases, low combustion rates. This cumulative point at low inflation power induces low inflation surface flow rates. These low inflation surface flow rates are compensated for by the use of thin pellets and small diameters which induce a strong initial surface of pyrotechnic product and a low loading density.
• the inflation power of a composition being associated with the gaseous molar yield and temperature, the compositions having a high inflation power have a high combustion temperature and a low level of particles produced during combustion.
• the low level of particles is necessary to have the maximum amount of gas emitted and so as to avoid aggression on the bags.
• Tests in airbag modules have indeed shown that the damage of the bags by the combustion products is exacerbated by the presence of particles in case of use of "hot" compositions.
• a composition with a high inflating power, a high inflating surface flow rate and no particles has many advantages with respect to the operation and miniaturization of airbag system gas generators. This miniaturization is required for reasons of cost, weight and integration inside the vehicles.
• the formulations have a high gaseous yield, a relatively high combustion temperature and a low particle level
• tests conducted in airbag modules with these compounds have shown that the operation can be good in relatively thin uncoated bag ( ⁇ 470
• the aggression on the bag is acceptable despite the high temperature due to the low level of particles produced and because of the operation induced by the monolithic block which limits aggression on the bag at the beginning of deployment.
• they are no longer used on new equipment because they do not have sufficient resistance (resistance) to aging at high temperature, such as as required by the builders automobiles.
• these compounds have an oxygen balance shifted to negative values (oxygen deficiency) which induces a carbon monoxide level well above the maximum standards in force for the application in question.
• the oxygen balance is the mass percentage of oxygen released (positive value) or absorbed (negative value) during the combustion reaction of a constituent.
• a CH 2 group the basic element of aliphatic polymers, has an oxygen balance of 343%. Indeed, it takes three oxygen atoms whose molar mass is 48 g to balance the combustion of 14 g / mole of CH 2 .
• compositions based on silicone binder were then proposed.
• Compositions based on binder "RTV" room temperature vulcanizable
• potassium perchlorate have been described in patent applications FR 2 190 776 and FR 2 213 254.
• Patent application FR 2 728 562 describes a version improved of these products, manufacturable by a process of kneading and continuous extrusion.
• the silicone binder is combined with a mixture of ammonium perchlorate and sodium nitrate; said sodium nitrate serving as a chlorine sensor.
• the compositions according to these documents exhibit an acceptable gas yield, a high combustion temperature and a high rate of combustion. The inflating surface flow rate is therefore relatively high.
• compositions based on nitrocellulose and nitroglycerine compared to compositions based on nitrocellulose and nitroglycerine, these compositions have the advantage of being very stable in temperature and can be adjusted to "oxygen balance" (balance oxygen) to meet the standards of toxicity of gaseous effluents.
• these compositions have the disadvantage of emitting a high level of particles (approximately 37% by weight of the total mass emitted during combustion), in particular sodium chloride and silica, which requires the use of a bag having a high thickness and a protective coating of the inner face of said bag.
• the patent application EP 1 216 977 describes a solvent-free extrudable composition essentially comprising a two-component oxygenated hydrocarbon binder (an elastomer (a rubber) and a plasticizer), a nitrogen-containing organic compound (nitrogen generator) and oxidizing charges.
• Said oxidizing charges consist of ammonium perchlorate and a chlorine sensor.
• Said chlorine sensor as its name indicates, is present to capture the chlorine gas emitted during the combustion of ammonium perchlorate. It intervenes, for this purpose, high content (about 15 to 20% by weight in the composition). It consists advantageously of sodium nitrate and sodium chloride (solid) is then formed.
• This composition has an inflation power and a surface flow of the same order of magnitude as the silicone bases, due to a slightly lower combustion rate and a lower particle rate.
• the gas yield, and therefore the inflation power is limited by the presence of the chlorine sensor (which thus induces the formation of a solid salt).
• the overall content of solid combustion residues of these compositions is about 14%.
• the burning rates of these compositions from about 20 to 40 mm / s at a combustion pressure of 20 MPa, remain insufficient for the intended application.
• the high pressure exponent of these compositions from about 0.63 over the pressure range 15 MPa to 35 MPa, makes it difficult to adjust the ballistic operation of said gas generator compositions.
• the combustion of these compositions at low pressure (P ⁇ 10 MPa) is also not satisfactory and can lead to extinctions.
• these compositions do not exhibit, with reference to the severe tests mentioned above, long-term aging behavior at a satisfactory high temperature.
• compositions containing, in a binder, an oxidizing charge which comprises at least one inorganic perchlorate and which does not include a chlorine sensor.
• These compositions may contain a nitrogenous organic compound, such as guanidine nitrate (NG).
• NG guanidine nitrate
• the bag can conveniently be coated with chlorine sensors.
• the absence of the oxidizing charge represented by the chlorine sensor is, within these compositions, compensated by the presence, in the composition of the binder, of a highly oxygenated hydrocarbon plasticizer having an oxygen balance greater than or equal to 230%.
• These compositions have a high swelling power, a low particle level, a high rate of combustion, from about 40 to 50 mm / s at 20 MPa, a low pressure exponent, about 0.5 over the pressure range 15 to 15 MPa. 35 MPa and good operation at low pressure.
• compositions require the use of highly oxygenated hydrocarbon plasticizers, of the diester type, more particularly of diester type plasticizers with ether functions.
• plasticizers are manufactured by trans-esterification from precursor compounds, which consist for the most part of a mixture of compounds of various molecular masses, so that the plasticizer itself consists of a mixture of compounds of various molecular masses in which are present compounds of more or less low molecular weight.
• the use of such plasticisers then require, for the applications under consideration, a purification step in order to eliminate these compounds of low molecular weight (detrimental to the thermal stability of the final product).
• compositions according to said application WO 2008/145935 do not show, either, with reference to the severe tests mentioned above, a good long-term aging behavior at high temperature.
• compositions can be free of chlorine sensor
• the skilled person is always looking for compositions with high combustion temperature, generating little particles (in order to increase the inflation capacity and the inflating surface flow rate, so as to reduce the volumes, masses and costs of gas generators for airbag system) and toxic effluents (by a balance value in oxygen close to 0), having a high combustion rate and good low-pressure combustion, a moderate pressure exponent, a satisfactory long-term aging behavior at high temperature, with reference to the severe tests mentioned above, these compositions being capable of advantageously be shaped by extrusion without solvent, which allows the realization of monolithic form facilitating loading, improving the loading density of the generator.
• the fixed improvement objective has been achieved.
• the inventors currently propose high-performance pyrotechnic compounds, with reference to the specification above, pyrotechnic compounds that perform better than the compounds of applications EP 1 216 977 and
• the pyrotechnic compounds of the invention (solid compounds) have a composition of the type of that of the compounds according to the application
• EP 1 216 977 in that it contains:
• an oxidizing charge comprising a main oxidizing charge consisting of at least one inorganic perchlorate (advantageously ammonium perchlorate) and a complementary oxidizing charge consisting of at least one nitrate chosen from alkaline and alkaline-earth nitrates (advantageously nitrate); sodium and / or nitrate potassium and / or strontium nitrate, most preferably sodium nitrate);
• a crosslinked oxygenated hydrocarbon binder obtained by crosslinking an elastomer (of the gum type according to EP 1 216 977) in the presence of at least one crosslinking agent and at least one oxygenated hydrocarbon plasticizer of said elastomer.
• the plasticizer (s) is (are) obviously perfectly miscible (s) in the elastomer, so as not to exude temperature and thus lower the glass transition temperature of said elastomer.
• said main oxidizing charge represents from 64 to 93.5%, advantageously from 72 to 82% by weight;
• said complementary oxidizing charge does not represent more than 10% by mass
• said elastomer preferably chosen from polyesters and polyacrylates, has a molecular weight greater than 200,000 and said at least one oxygenated hydrogenated plasticizer is chosen from plasticizers, whose molecular mass is greater than 350 g / mol (its tension Steam remains sufficiently low at 120 ° C (to limit or even avoid any problem of evaporation, migration ...)) and the oxygen balance equal to or greater than -280% and less than or equal to -235% , and their mixtures.
• the pyrotechnic compounds of the invention differ from the compounds according to the application EP 1 216 977 in that their composition contains a reduced level of alkaline and / or alkaline earth nitrate and does not contain any nitrogenous organic compound. Moreover, the nature of the plasticisers present is specified.
• the pyrotechnic compounds of the invention differ from the compounds according to the application WO 2008/145935 in that their composition contains a complementary oxidizing charge consisting of at least one nitrate chosen from alkaline and alkaline earth nitrates and does not contain a very high plasticizer. oxygen.
• the pyrotechnic gas-generating compounds of the invention therefore contain, in their composition, from 64 to 93.5%, preferably from 72 to 82% by weight (% by weight relative to the total weight of said compounds) of at least one inorganic perchlorate.
• the pyrotechnic gas-generating compounds of the invention thus contain, in their composition, only a low level of complementary oxidant (s) (not more than 10% by weight), a low level of at least one nitrate selected from alkaline nitrates and alkaline earth nitrates.
• the function of the said additional oxidizing agent (s) is to allow the equilibrium of the oxygen balance of the composition which does not contain a highly oxygenated plasticizer.
• Said at least one additional oxidant (nitrate) introduced into the composition of the compounds of the invention also incidentally plays the role of a chlorine sensor and makes it possible to reduce, even at a low level, the amount of chlorine gas produced by the combustion.
• the at least one nitrate chosen from alkaline nitrates and alkaline earth nitrates is generally chosen from sodium, potassium and strontium nitrates and their mixtures. It consists advantageously of sodium nitrate and / or potassium nitrate, very advantageously sodium nitrate.
• the pyrotechnic gas-generating compounds of the invention do not contain, in their composition, nitrogenous organic compound (nitrogenous organic compound present in the compositions of the application EP 1 216 977 and in those exemplified of the application WO 2008/145935, such as guanidine nitrate). This is particularly advantageous with reference to their thermal stability. Said compounds of the invention in fact support aging of 3000 hours at 110 ° C. The inventors have in fact shown the detrimental influence of guanidine nitrate on the thermal stability of the pyrotechnic compounds of the invention. This harmful influence was not expected.
• pelletized compositions based on guanidine nitrate (NG) combined with basic copper nitrate (BCN) or in combination with basic copper nitrate (BCN) and with potassium perchlorate exhibit a certain behavior. at aging in temperature quite satisfactory.
• the crosslinked oxygenated hydrocarbon binder of the compounds of the invention therefore associates with a particular elastomer at least one specific plasticizer. It is not a highly oxygenated plasticizer in the sense of the application WO 2008/145935 (it is a plasticizer which has an oxygen balance between -280% and -235%: see above) . Surprisingly, within the compounds of the invention, the presence of a highly oxygenated binder has not proved indispensable and its absence has on the other hand proved positive on the resistance to long-term aging at high temperature.
• the compounds of the invention the composition of which does not contain any nitrogenous organic compound, does not contain a highly oxygenated plasticizer (-280% ⁇ OB ⁇ -235%) and only closes a low additional oxidizing agent (s)), have proved to be very efficient.
• Said at least one oxygenated hydrocarbon plasticizer having the required molecular weight and oxygen balance, is advantageously chosen from the family of aliphatic diesters (adipates, sebacates, azelates, etc.), aromatic diesters (phthalates, etc.) and aromatic triesters (trimellitates, etc.), esters containing only ester-type oxygen functions in their formula (esters without ether function).
• Said at least one oxygenated plasticizer is very advantageously chosen from;
• DOA dioctyl adipate
• DEHA di- (2-ethylhexyl) adipate
• DINA diisononyl adipate
• DIDA diisodecyl adipate
• DOS dioctyl sebacate
• DIDP diisodecyl phthalate
• DPHP dipropylheptyl phthalate
• trimellitate of tri- (octyl, decyl): molecular mass (average) 588 g / mol, OB -261% (average value),
• the main oxidizing charge consists of at least one inorganic perchlorate. It represents from 64 to 93.5% by weight of the total mass of the compound, advantageously from 72 to 82% by weight of said total mass. It is the main constituent of the compounds of the invention.
• Said main oxidizing charge advantageously comprises ammonium perchlorate.
• Said main oxidizing charge is very advantageously ammonium perchlorate.
• Said ammonium perchlorate is advantageously used in several granulometries so as to improve its incorporation and its distribution in the elastomer and to reduce the toxicity of the gaseous effluents during combustion.
• the crosslinked oxygenated hydrocarbon binder generally represents from 6 to 20% by weight of the total mass of the compound. It advantageously represents from 8 to 16% by weight of the total mass. It comprises the crosslinked elastomer and said at least one oxygenated plasticizer.
• the elastomer in question is a high molecular weight elastomer: Mw> 200,000 g / mol. It is preferably chosen from the family of polyesters and polyacrylates.
• the polyacrylates may have reactive functionality of the chlorine / carboxyl, chlorine, hydroxyl or epoxy type.
• the polyesters may have hydroxyl-type reactive terminations. They advantageously have such hydroxyl-type reactive terminations.
• crosslinking agent Suitable crosslinking agents are known to those skilled in the art.
• a crosslinking agent for the crosslinking of a polyester-type elastomer, advantageously consists of a diisocyanate or a triisocyanate.
• said at least one elastomer and said at least one crosslinking agent represent from 3 to 10% by weight, advantageously from 4 to 9% by weight, of the total mass of the compounds of the invention; and / or, advantageously and,
• said at least one plasticizer represents from 3 to 10% by weight, advantageously from 4 to 8% by weight, of the total mass of said compounds.
• the compounds of the invention may comprise, in their composition, the following additional constituents;
• At least one ballistic catalyst (which makes it possible, among other things, to improve the rate of combustion).
• Ballistic catalyst consists of a transition metal oxide, with high specific surface area (which accelerates the decomposition of the oxidizing charge).
• a te! at least one ballistic catalyst is advantageously selected from copper oxide, iron oxide, manganese oxide, zinc oxide and cobalt oxide.
• such at least one ballistic catalyst is between 0 and 5%, advantageously between 2 and 4%, by weight within the compounds of the invention; and or
• At least one wetting agent chosen from organosilanes and titanates.
• Such at least one wetting agent is advantageously chosen from vinyltris- (2-methoxyethoxy) silane, vinyltriethoxysilane, tris- (3-trimethoxysilylpropyl) isocyanurate, ⁇ -methacryloxypropyltriethoxysilane, diethoxydiacetoxysilane, diacetoxydiethoxysilane and dibutoxyethoxymethylsilane.
• Such at least one wetting agent makes it possible to reduce the viscoelasticity and the residual porosity of the compound.
• such at least one wetting agent intervenes between 0 and 4%, advantageously between 0.2 and 3%, by weight within the compounds of the invention.
• nitrate selected from alkali and alkaline earth nitrates (additional oxidizing charge);
• the constituents (main and additional oxidizing charges + crosslinked oxygenated hydrocarbon binder + any constituents chosen from those identified above) of the composition of the compounds of the invention, listed above, represent at least 95% by weight of said compounds, generally at least 98% (or 100%) by mass of the said compounds.
• the complement, if any, is generally composed of additives, such as auxiliaries (aids) manufacturing.
• the compounds of the invention can be of different types. These are usually monolithic compounds that can be full, mono- or multi-perforated.
• Said compounds are particularly effective.
• Their composition is high-yield gas (about 34 mol / kg) with combustion temperatures around 2950 K (it is indeed so-called "hot” compositions).
• Their burning rate is fast, about 55 mm / s at a pressure of 20 MPa. Because of their composition, they generate few solid particles (at a rate of less than or equal to 6%).
• Their composition is also likely, according to advantageous variants, to have an oxygen balance value between -1% and -3%, ie they do not generate toxic gas and they are quite suitable for a application in the field of airbags.
• the inflating surface flow rates of the compositions of the compounds of the invention are very interesting. They are about 975 mol.K / cm 2 .s. Their resistance to aging at high temperature is very satisfactory.
• the compounds of the invention generally have the disadvantage of emitting hydrogen chloride, the low rate of chlorine sensor introduced into the compound does not allow to trap all of the chlorine formed by combustion. At the end of combustion, said hydrogen chloride condenses with the water formed by the combustion and can be captured by the bag.
• the level of hydrogen chloride emitted by the compounds according to the invention is approximately 0.2 g / g.
• the bag can be coated with chlorine sensors.
• the vents can be reduced so as to compensate for the deflation of the bag by cooling the gases, (taking into account the nature of the composition of the gases which contain 50 % of condensable (H 2 0) when the temperature decreases) so as to increase the capture rate by condensation of acidified water in the bag.
• the bag naturally deflates due to the drop in temperature and condensation of condensables.
• the process for obtaining the compounds of the invention is advantageously a method by analogy, as described in application WO 2008/145935. It is very advantageously a process carried out continuously, without solvent, in a twin-screw mixer-extruder.
• said method comprises:
• said mixtures and extrusions are advantageously used in a twin screw mixer-extruder.
• the twin-screw mixer-extruder includes a mixing and mixing chamber, a compression chamber and an extrusion head.
• the solid and liquid components are introduced into the mixing and kneading compartment by two different feed openings, a solids feed opening and a liquid feed opening, and then transported and kneaded.
• the homogeneous paste thus formed is degassed in the compression compartment, then extruded with the aid of an extrusion head in the form of rods, and finally, the rods thus formed are cut into loadings using an apparatus. cutting, then these charges are made to crosslink at a temperature generally between 100 ° C and 150 ° C.
• the charges thus formed find their preferential application as a pyrotechnic charge in gas generators intended to inflate a protective cushion for occupants of a motor vehicle. Indeed, the burning rate of these loadings, as well as the rate of solid residues produced and the rate of carbon monoxide and nitrogen oxides produced are particularly suitable (see above).
• FIG. 1 shows pressure curves, over time, pressure detected during combustion (after prior conditioning of the generator at 20 ° C.) of a sample of 14.5 g of compound according to (Example 1 of) the invention in a generator provided with a nozzle.
• compositions of pyrotechnic compounds have been evaluated by means of thermodynamic calculations and physical measurements.
• compositions and compounds correspond to compositions and compounds of the prior art (compositions A and B hereinafter) or to a composition and a compound of the invention.
• Composition A (prior art):
• composition with binder, contains:
• acrylic elastomer - 15% by weight of acrylic elastomer, crosslinking agent and plasticizer (dioctyl adipate).
• This composition is a composition according to patent application EP 1 216 977. It is extruded and crosslinked to generate compounds (block type). The oxygen balance of this composition is -2%. Its theoretical density is 1.7 g / cm 3 .
• the level of particles emitted is 16%.
• the burning rate of the compounds (extruded) is 38 mm / sec at 20 MPa (see Table 1 below).
• Composition B (prior art); It contains:
• DBEEEG dibutoxyethoxyethoxyethyl glutarate: highly oxygenated plasticizer
• This composition is a composition according to patent application WO 2008/145935. It is extruded and crosslinked to generate compounds (block type). The oxygen balance of this composition is -2.3%. Its theoretical density is 1.73 g / cm 3 .
• the particle content is less than 2%.
• Its pressure exponent is 0.5 between 15 MPa and 35 MPa.
• the burning rate of the compounds (extruded) is between 40 and 50 mm / s at 20 MPa (see Table 1 below).
• Composition 1 of a compound of the invention is a compound of the invention.
• composition comprises:
• plasticizer dioctyl adipate
• This composition is extruded and crosslinked to generate compounds (block type).
• the oxygen balance of this composition is -1%. Its theoretical density is 1.78 g / cm 3 .
• the particle ratio is about 5%.
• Its pressure exponent is 0.5 between 15 MPa and 35 MPa.
• the burning rate of the compounds (extruded) is between 50 and 60 mm / s at 20 MPa (see Table 1 below).
• compositions A, B and 1 and those of the corresponding compounds are given in Table 1 below.
• the pressure exponent on the pressure range between 15 MPa and 35 MPa of said compounds is about 0.44 after aging for about 0.50 before aging.
• composition of the compound of the invention has a balance in oxygen (-1%) better balanced than that of the compositions of the prior art, which is conducive to avoid the generation of toxic gases, such as carbon monoxide.
• the higher rate of combustion of the compounds of the invention compared with those of the compounds of the prior art results in a higher inflation surface flow rate.
• the characteristic dimension of the object to be burned can be doubled to ensure an equivalent operating time.
• the extruded block made from the compositions of the invention can therefore be very compact and allow the development of small generators containing a low pyrotechnic mass.
• the compounds of the invention have a low pressure exponent between 15 MPa and 35 MPa, equivalent to that of the composition B of the prior art.
• gas generators employing the compounds of the invention may be, to some extent, devoid of particulate filters. In doing so, the thermal losses of the gases are reduced.
• compositions in the form of a monolithic block with a very high combustion rate makes it possible to achieve a low flow rate ignition, and this because of the small initial combustion surface of the block.
• the monolithic geometry of the loading also allows the design of shapes to deliver a progressive or constant flow.
• a conductive gas generator containing a compound according to the invention 14 g emits 2.8 g of hydrogen chloride.
• the hydrogen chloride level is of the order of 700 ppm in a cabin of 2.8 m 3 .

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• 2010
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