US20030145923A1 - Propellant for gas generators - Google Patents

Propellant for gas generators Download PDF

Info

Publication number
US20030145923A1
US20030145923A1 US10/323,929 US32392902A US2003145923A1 US 20030145923 A1 US20030145923 A1 US 20030145923A1 US 32392902 A US32392902 A US 32392902A US 2003145923 A1 US2003145923 A1 US 2003145923A1
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US
United States
Prior art keywords
group
residue
nitrate
carbon atoms
tetrazole
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.)
Abandoned
Application number
US10/323,929
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English (en)
Inventor
Klaus Redecker
Waldemar Weuter
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Individual
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Individual
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
Application filed by Individual filed Critical Individual
Priority to US10/323,929 priority Critical patent/US20030145923A1/en
Publication of US20030145923A1 publication Critical patent/US20030145923A1/en
Priority to US10/749,504 priority patent/US20040226639A1/en
Abandoned 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
    • C06B43/00—Compositions characterised by explosive or thermic constituents not provided for in groups C06B25/00 - C06B41/00

Definitions

  • DE-A-2,142,578 describes a press-molded propellant charge for the rapid inflation of a hollow body by the reaction of tetrazylazene with oxygen carriers.
  • DE-A-1,806,550 proposes a propellant charge which generates pressure gas, yielding cool gases, based on ammonium nitrate, activated carbon, and a compound that is subject to endothermal decomposition or sublimation.
  • this system produces a large proportion of steam, representing a drawback since water leads to a strong increase in temperature due to its high heat of condensation.
  • DE-A-1,222,418 discloses mixtures generating pressurized gas, based on inorganic perchlorate oxidizers, polymeric fuel binders, and a coolant. Preparations having high proportions of chlorate or perchlorate, however, lead to chlorine components in the reaction gases. Thus, EP-A-372,733 likewise yields an unsatisfactory mixture inasmuch as the propellant charge for the proposed airbag contains about 40% ammonium perchlorate. Even nitrocellulose and nitroglycerin compositions can be found in the literature. Such suggestions cannot be considered for use in lifesaving systems. Nitrocellulose and nitroglycerin mixtures, or also other energetic compounds rich in carbon must be eliminated on account of carbon monoxide formation.
  • the invention is based on the object of making available gas compositions, the manufacture and processing and/or handling of which are harmless and the reaction products of which are nontoxic.
  • R 2 and R 2 or R 3 can be identical or different (but either R 2 or R 3 is present) and can be: hydrogen, hydroxy, amino, carboxy, an alkyl residue of 1-7 carbon atoms, an alkenyl residue of 2-7 carbon atoms, an alkylamino residue of 1-10 carbon atoms, an aryl residue optionally substituted by one or several substituents which can be identical or different, selected from the amino group, the nitro group, the alkyl residues of 1-4 carbon atoms, or an arylamino residue wherein the aryl residue can be optionally substituted, or their sodium, potassium, and guanidinium salts, or containing, as the nitrogenous compounds,
  • the nitrogen-containing compounds to be used according to this invention are those forming, in a mixture with oxidizing agents, during their thermal-chemical reaction, primarily CO 2 , N 2 and H 2 O, but not releasing any gases, such as CO or NO X in health-endangering concentrations.
  • An especially significant feature resides in that the addition of binders is not absolutely necessary.
  • R 1 preferably is hydrogen, amino, hydroxy, carboxy, a methyl, ethyl, propyl or isopropyl, butyl, isobutyl or tert-butyl, n-pentyl, n-hexyl or n-heptyl residue, a methylamino, ethylamino, dimethylamino, n-heptylamino, n-octylamino or n-decylamino residue, a phenylamino residue, or a phenyl or aminophenyl residue.
  • R 2 or R 3 is preferably hydrogen, a methyl or ethyl residue, or a phenyl or aminophenyl residue.
  • Cyanic acid derivatives used with preference are sodium cyanate, cyanuric acid, 1-cyanoguanidine and/or disodium cyanamide; triazine derivatives used with preference are 1,3,5-triazine, cyanuric acid esters and/or cyanuric acid amide (melamine); and urea derivatives used with preference are biuret, guanidine, nitroguanidine, guanidine nitrate, aminoguanidine, aminoguanidine nitrate, triaminoguanidine nitrate, aminoguanidine hydrogen carbonate, azodicarboxylic acid diamide, dicyandiamidine nitrate, dicyandiamidine sulfate, tetrazene and/or semicarbazide nitrate.
  • the mixtures according to this invention exhibit a high thermal and weather stability, which is a prerequisite for perfect action even after long-term storage.
  • Suitable oxidizing agents are nitrates of ammonium, sodium, potassium, magnesium, calcium or iron, preferably sodium nitrate, or peroxides of zinc, calcium, strontium or magnesium.
  • the peroxides are used with an oxygen value as obtainable from stable compounds. For zinc peroxide, this value is about 11 to 14% by weight.
  • the corresponding molar ratio of nitrogen-containing compound to peroxide is in a range from 1:2 to 5.5.
  • Calcium peroxide can exhibit an active oxygen value of, for example, 18.26% by weight, and grain sizes of 15.5 ⁇ m and is advantageously utilized in a molar ratio of nitrogen-containing compound/peroxide of 1:3.
  • the aforementioned peroxides can be used in a molar ratio of nitrogen-containing compound to peroxide in a range of 1:1 to 20.
  • Calcium peroxide and/or zinc peroxide is used with preference. It is also possible to employ mixtures of the peroxides with one another or mixtures with other oxidizing agents.
  • Other oxidizing agents are, for example, the above-mentioned nitrates of ammonium, sodium, potassium, magnesium, calcium or iron, preferably sodium nitrate.
  • the alkaline-acting hydrolysis products may evoke reactions with the other components of the mixture.
  • coating of the peroxides with inorganic or organic materials in accordance with conventional methods is suitable. Such a coating offers, moreover, the advantage of improved handling ability since the thus-treated propellant will no longer be dusty.
  • the mixtures to be utilized according to this invention of the tetrazole and/or its derivatives with the compounds from groups (A), (B) and/or (C) permit a finely graded staggering of the propellants with regard to their reaction rate and the thus-formed vapors and gases. This is a staggering needed for providing a maximum variety of uses for the propellant charges of this invention.
  • the propellant charges of this invention must be blended in a controlled fashion. Only in this way is it possible to attain an effect that is at an optimum in each case.
  • the degree of efficiency of the propellant charges according to this invention is, after all, affected not only by the composition, but furthermore by the ignition, and also by the tamping resulting from the construction, and by the flow-off behavior of the thus-evolving vapors and gases. Evaluation of the degree of efficiency can be accomplished, for example, by determination of the gas pressure rise gradient of the respective mixture in the given external environment in each case dependent on the structure, and the type of ignition selected.
  • the gas temperature can be kept low in a controlled fashion by addition of diammonium oxalate, oxalic acid diamide, dicyandiamide, or carbonates and, respectively, bicarbonates. If thermal stability is not a factor, and smoke formation upon addition of inorganic carbonates or bicarbonates is to be avoided, it is possible to use aminoguanidine bicarbonate as the organic bicarbonate.
  • Other additives can be constituted by oxalic acid or urea, generally added in an amount of up to 5% by weight, based on the mixture.
  • Suitable reducing agents are metal powders of iron, magnesium, zirconium or titanium which, in contrast to the nonmetallic compound boron, have no strong effect on the deflagration velocity, but in case of the latter do have an influence on the heat production of the reaction and on the reaction products.
  • the proportion of the reducing agents can amount to up to 5% by weight.
  • Suitable catalysts for a mixture of such heterogeneous composition are compounds having an effect on the decomposition of peroxides, such as, for example, metals or their oxides, e.g. manganese dioxide. Additions of vanadium pentoxide or cerium dioxide lead to an increase in the reaction velocity. When adding up to 5% by weight of molybdenum(VI) oxide, the velocity is only slightly changed, and this also applies in the presence of cerium(III) nitrate hexahydrate. These additives are effective in amounts of up to a few percent by weight. Further catalysts are metal complexes, of which ferrocene can here be cited as an example; the addition of this compound with up to about 3% by weight markedly raises the reaction velocity.
  • the gas compositions described in accordance with this invention are manufactured by mixing the components according to conventional methods, optionally with the preparation of a harmless premix to which additional components are added.
  • This mixture can already be utilized in powdered form. Unmixing on account of varying densities of the components can be counteracted by granulation of the mixture.
  • the mixture will be formed by press-molding or similar measures.
  • press-molding aids can be added to the mixture. Suitable as such are graphite, molybdenum disulfide, “Teflon”, talc, zinc stearate or boron nitride. These agents have an effect even in minimum quantities and affect the properties and deflagration behavior either not at all or only to a minor extent.
  • a method resides in admixing additives, such as salts, to the mixture prior to the actual shaping step; these additives can be removed again after molding by extraction with water or solvents.
  • Another method resides in adding materials of low thermal resistance which decompose when the molded item is heated. The surface of the mixture can also be enlarged by adding to the mixture, prior to press-molding, hollow microspheres of glass or synthetic resins.
  • the density of the press-molded article that can be attained thereby can deviate by approximately up to 20% from that of the untreated press-molded article; in this connection, this value is to be merely a roughly governing value and does not represent a limitation. This treatment leads to an extreme acceleration of the deflagration process.
  • a further treatment of the molded articles can consist in surface coating.
  • Such a measure can also be suitable for increasing the strength of the molded item.
  • the use of suitable fibers for stabilization purposes would have to be additionally provided for.
  • a side effect of the coating procedure is a decreased abrasion of the items during transport stresses.
  • the thus-treated molded articles can be introduced in loose bulk or in oriented fashion into appropriate pressure-proof containers. They are ignited according to conventional methods with the aid of initiator charges or thermal charges wherein the thus-formed gases, optionally after flowing through a suitable filter, lead to inflation of the lifesaving system within fractions of a second.
  • the propellants of this invention are especially suited for so-called airbags, impact bags which are utilized in automotive vehicles or airplanes for occupants' protection. In case of vehicle impact, the airbag must fill up within a minimum time period with gas quantities of about 50 to 300 liters, depending on system and automobile size.
  • the propellants of this invention are likewise suitable for use in belt-tightening devices.
  • Lifesaving systems containing the propellants of this invention likewise form the subject matter of the present invention.
  • 167 g of 5-aminotetrazole (5-ATZ) (produced from aminoguanidine sulfate, sodium nitrite and nitric acid) is recrystallized from about 600 ml of water under continuous agitation, dried at 110° C. after filtration, ground up, and separated from coarse proportions with a 250 gm screen (5-ATZ specification: mp/decomp.: >203° C., average grain size 80 ⁇ m and H 2 O proportion ⁇ 0.05%). From ZnSO 4 ⁇ 7H 2 O and hydrogen peroxide in aqueous ammonia, ZnO 2 is produced, washed with dilute acetic acid as well as water, and dried at 60° C. (specification of ZnO 2 : 13.47% by weight of active oxygen, average grain size 20.3 ⁇ m).
  • the gas charge mixtures described in Examples 1-24 can also be utilized in press-molded form.
  • the deflagration behavior of the press-molded items, as tested in correspondence with Example 1, is slower than that of the bulk material and requires 0.1 g of B/KNO 3 or Ti/ZnO 2 as initiating mixture.
  • the reaction velocity rises with a drop in the pressing force and drops with the size of the pressed material.
  • the residue from the reactions remains extensively preserved in the form of the pressed items.
  • Example 1 As described in Example 1, further mixtures were prepared from gas-generating components and oxygen-yielding compounds, such as zinc peroxide, with an active oxygen proportion of 13.07% by weight and an average grain size of 11.8 ⁇ m or, in case of sodium nitrate, with an average grain size of ⁇ 45 ⁇ m.
  • oxygen-yielding compounds such as zinc peroxide
  • Table 5 shows the values for the maximum pressure (bar) and the time in ms up to maximum pressure, ranging within regions as described in Example 1 for a gas charge of 5-aminotetrazole and zinc peroxide. In addition, the time between 40 and 60% of maximum pressure was determined. TABLE 5 Max. Time (ms) Example Pressure to Max. to 40-60% of No. (bar) Pressure Max. Pressure 26 359 30 1.2 27 217 123 13.1 28 352 29 1.5 29 473 39 1.3 30 549 14 0.5 31 917 7 0.2 32 148 220 20.1
  • the components are suitable for the production of gas charges on account of their miscibility, processability, press-molding ability for shaping, as well as compatibility with one another and with other additives, as well as due to their characteristic safety data.
  • the mixtures of Examples 33-44 were produced from zinc peroxide (active oxygen proportion 12.0% by weight, average grain size 4.8 ⁇ m), aminotetrazole (average grain size ⁇ 125 ⁇ m), sodium nitrate (grain size ⁇ 45 ⁇ m), and the listed components with a grain size of ⁇ 125 ⁇ m.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Air Bags (AREA)
  • Catalysts (AREA)
US10/323,929 1991-06-21 2002-12-20 Propellant for gas generators Abandoned US20030145923A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US10/323,929 US20030145923A1 (en) 1991-06-21 2002-12-20 Propellant for gas generators
US10/749,504 US20040226639A1 (en) 1991-06-21 2004-01-02 Propellant for gas generators

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
DE4120599 1991-06-21
DEP4120599.5 1991-06-21
US90169892A 1992-06-22 1992-06-22
US35474594A 1994-12-08 1994-12-08
US52456300A 2000-03-13 2000-03-13
US10/323,929 US20030145923A1 (en) 1991-06-21 2002-12-20 Propellant for gas generators

Related Parent Applications (1)

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US52456300A Continuation 1991-06-21 2000-03-13

Related Child Applications (1)

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US10/749,504 Continuation US20040226639A1 (en) 1991-06-21 2004-01-02 Propellant for gas generators

Publications (1)

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US20030145923A1 true US20030145923A1 (en) 2003-08-07

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US10/323,929 Abandoned US20030145923A1 (en) 1991-06-21 2002-12-20 Propellant for gas generators
US10/749,504 Abandoned US20040226639A1 (en) 1991-06-21 2004-01-02 Propellant for gas generators

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Country Status (4)

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US (2) US20030145923A1 (cs)
EP (1) EP0519485A1 (cs)
CZ (1) CZ291570B6 (cs)
DE (1) DE4220019A1 (cs)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080110536A1 (en) * 2006-05-05 2008-05-15 Ganta Sudhakar R Gas generant compositions
US20090008002A1 (en) * 2006-09-30 2009-01-08 Ganta Sudhakar R Gas generant compositions
US20100258221A1 (en) * 2006-05-05 2010-10-14 Ganta Sudhakar R Gas generant compositions
JP2014080310A (ja) * 2012-10-15 2014-05-08 Sekisui Chem Co Ltd ガス発生材及びマイクロポンプ
US10731062B2 (en) 2012-10-15 2020-08-04 Sekisui Chemical Co., Ltd. Gas-generating material and micropump
WO2020188931A1 (ja) * 2019-03-15 2020-09-24 永和化成工業株式会社 ガス発生剤、発泡用組成物、発泡体、及び発泡体の製造方法

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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
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US7914632B2 (en) 2006-05-05 2011-03-29 Tk Holdings, Inc. Gas generant compositions
US7692024B2 (en) 2006-05-05 2010-04-06 Tk Holdings, Inc. Gas generant compositions
US20100258221A1 (en) * 2006-05-05 2010-10-14 Ganta Sudhakar R Gas generant compositions
US20100258220A1 (en) * 2006-05-05 2010-10-14 Ganta Sudhakar R Gas generant compositions
US7847102B2 (en) 2006-05-05 2010-12-07 Tk Holdings, Inc. Gas generant compositions
US20080110536A1 (en) * 2006-05-05 2008-05-15 Ganta Sudhakar R Gas generant compositions
US8088235B2 (en) 2006-05-05 2012-01-03 Tk Holdings, Inc. Gas generant compositions
US20090008002A1 (en) * 2006-09-30 2009-01-08 Ganta Sudhakar R Gas generant compositions
US8002915B2 (en) 2006-09-30 2011-08-23 Tk Holdings, Inc. Gas generant compositions
JP2014080310A (ja) * 2012-10-15 2014-05-08 Sekisui Chem Co Ltd ガス発生材及びマイクロポンプ
US10731062B2 (en) 2012-10-15 2020-08-04 Sekisui Chemical Co., Ltd. Gas-generating material and micropump
WO2020188931A1 (ja) * 2019-03-15 2020-09-24 永和化成工業株式会社 ガス発生剤、発泡用組成物、発泡体、及び発泡体の製造方法
JPWO2020188931A1 (cs) * 2019-03-15 2020-09-24

Also Published As

Publication number Publication date
US20040226639A1 (en) 2004-11-18
EP0519485A1 (de) 1992-12-23
DE4220019A1 (de) 1992-12-24
CZ189792A3 (en) 1993-01-13
CZ291570B6 (cs) 2003-04-16

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