EP0705808A1 - Propergol à base de nitrate d'ammonium nitrate à phase stabilisée - Google Patents

Propergol à base de nitrate d'ammonium nitrate à phase stabilisée Download PDF

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Publication number
EP0705808A1
EP0705808A1 EP95112989A EP95112989A EP0705808A1 EP 0705808 A1 EP0705808 A1 EP 0705808A1 EP 95112989 A EP95112989 A EP 95112989A EP 95112989 A EP95112989 A EP 95112989A EP 0705808 A1 EP0705808 A1 EP 0705808A1
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EP
European Patent Office
Prior art keywords
mass
solid fuel
fuel according
combustion
solid
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.)
Granted
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EP95112989A
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German (de)
English (en)
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EP0705808B1 (fr
Inventor
Klaus Dr. Menke
Jutta Dr. Böhnlein-Mauss
Helmut Schmid
Klaus Martin Dr. Bucerius
Walther Dr. Engel
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Publication of EP0705808A1 publication Critical patent/EP0705808A1/fr
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    • 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
    • C06B23/007—Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
    • C06B31/28—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate
    • C06B31/30—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate with vegetable matter; with resin; with rubber

Definitions

  • the invention relates to a solid fuel for rocket engines or gas generators, which contains phase-stabilized ammonium nitrate as an oxidizer.
  • Solid fuels of the type mentioned generally have a low burning rate and a high pressure exponent.
  • the burning rate can be increased by adding solid energetic substances, such as octogen (HMX) or hexogen (RDX), or metals with high heat of combustion, such as aluminum or boron.
  • Combinations with high-energy binders serve the same goal. These include isocyanate-bound glycidyl azidopolymer (GAP), polymers containing nitrate esters, such as polyglycidyl nitrate and polynitratomethylethyloxetane, or nitroamino-substituted polymers. Even if this can increase the rate of combustion, the pressure exponent and the temperature coefficient are not or only slightly reduced. Additions of ammonium perchlorate, which increase the Burning rate lead to lower the pressure exponent at higher doses, but lead to the formation of hydrochloric acid in the exhaust gas and thus to strong smoke formation at high air humidity.
  • the burning behavior can be influenced favorably by adding lead and copper salts or oxides in combination with soot, but these additives can only be used to a limited extent with fuels containing ammonium nitrate.
  • the invention has for its object to improve the combustion behavior of solid fuels based on phase-stabilized ammonium nitrate.
  • such a solid fuel consists of 35 to 80% by mass ammonium nitrate (AN) with an average grain size of 5 to 200 ⁇ m, which is phase-stabilized by chemical reaction with CuO or ZnO (PSAN), 15 to 50% by mass of a binder system made of a binder polymer and an energy-rich plasticizer and 0.2 to 5.0 mass% of a combustion moderator made of vanadium / molybdenum oxide as an oxide mixture or mixed oxide.
  • AN ammonium nitrate
  • PSAN phase-stabilized by chemical reaction with CuO or ZnO
  • Solid fuels of this formulation show a very favorable burning behavior. Depending on the composition, burning rates of over 8mm / s at normal temperature and a combustion chamber pressure of 10 MPa are achieved. The pressure exponent in the range from 4 to 25 MPa, possibly 7 to 25 MPa, reaches values of n 3 ⁇ 4 0.6, in the best case n 3 ⁇ 4 0.5. This combustion behavior makes the solid fuel composed according to the invention particularly suitable for use in missiles for tactical or strategic missile defense.
  • the solid propellants according to the invention are initially characterized by the phase-stabilized ammonium nitrate reacted with copper oxide or zinc oxide as the oxidizer, the metal oxides preferably being used in a quantity of 1 to 7% by mass. They stabilize the crystal phases of the AN and suppress larger volume changes in the grain in the temperature range from -40 to + 70 ° C.
  • the incorporation into the crystal matrix of the AN takes place via a chemical reaction of copper or zinc oxide with the melt of the pure ammonium nitrate with elimination of water .
  • the most favorable particle shape for the production of the fuel can then be obtained by spraying the melt and rapid cooling in a cold, cyclone-like air flow.
  • the combustion behavior is significantly influenced by the grain size of the phase-stabilized ammonium nitrate.
  • a finely crystalline form with an average grain size of 5 to 200 ⁇ m with a proportion of 35 to 80 mass% in the fuel is preferred.
  • Particularly favorable burn-up values result when the AN fraction is predominantly in a smaller grain size of 5 to 80 ⁇ m and less in an average grain size of 100 to 160 ⁇ m.
  • the solid propellant according to the invention may also contain high-energy substances, in particular nitramines, such as hexogen (RDX) or octogen (HMX) with an average grain size of 2 to 20 ⁇ m with a proportion of 1 to 20% by mass.
  • nitramines such as hexogen (RDX) or octogen (HMX) with an average grain size of 2 to 20 ⁇ m with a proportion of 1 to 20% by mass.
  • metals such as aluminum, magnesium or boron can be part of the fuel with 0.5 to 20% by mass.
  • a grain size of 0.1 to 50 ⁇ m is recommended.
  • stabilizers which act as nitrogen oxide and acid scavengers.
  • These are preferably diphenylamine, 2-nitrodiphenylamine, N-methylnitroaniline, which are used alone or in combination with one another in concentrations of 0.4 to 2% by mass. These can be combined, in particular in the case of fuels containing nitric acid, with small amounts in the range of 0.5% by mass of the magnesium oxide acting in the same sense.
  • the combustion moderators are preferably used as mixed oxides, in which molybdenum of the oxidation level + VI and vanadium of the oxidation level + IV and + V are present.
  • exemplary compositions of the mixed oxides are V6Mo4O25 and V6Mo15O60.
  • the combustion moderators can also have Crom III or Titan IV oxides as the carrier material.
  • combustion moderators used according to the invention with 0.2 to 5.0 mass% are advantageously added to the fraction of the combustion moderator with carbon black or graphite in a proportion of 5 to 50 mass%.
  • binder system consisting of a binder polymer and an energy-rich plasticizer.
  • the binder polymer itself can be inert, preferably isocyanate-curing, bi- or trifunctional Hydroxy-substituted polyester or polyether prepolymers.
  • high-energy polymers preferably isocyanate-curing, di- or trifunctional hydroxy-substituted glycidyl azidopolymer, can also be used.
  • the high-energy plasticizers are preferably selected from the group of chemically stable nitrate esters, nitro, nitroamino or azido plasticizers.
  • TMETN Trimethylolethane trinitrate
  • BTTN butanetriol trinitrate
  • DEGDN diethylene glycol dinitrate
  • a 1: 1 mixture of bisdinitropropyl formal / acetal may be mentioned as an example of a nitro softener, while a 1: 1 mixture of N-ethyl and N-methylnitratoethylnitroamine (EtNENA or MeNENA) or Nn-butyl- N-nitratoethylnitroamine (BuNENA) or N, N'-dinitratoethylnitroamine (DINA) is suitable.
  • EtNENA or MeNENA N-methylnitratoethylnitroamine
  • BuNENA N-butyl- N-nitratoethylnitroamine
  • DINA N, N'-dinitratoethylnitroamine
  • GAP-A bisazido-terminated GAP oligomers
  • DANPE 5-diazido-3-nitroaminopentane
  • the polymer / plasticizer ratio is 1: 3 to 20: 1 mass%.
  • the binder polymers can of course also be used in pure form.
  • 0.1 to 1% by mass of its anti-caking agent fraction for example ultrafine (grain size about 0.02 ⁇ m) silica gel, sodium lauryl sulfonate, tricalcium phosphate or other surfactants are preferably added to the phase-stabilized ammonium nitrate.
  • the vanadium / molybdenum oxide combustion moderators can be ideally combined with copper salts, oxides or complexes, which brings about a further increase in the combustion rate, especially in the low pressure range, combined with a further reduction in the pressure exponent.
  • ammonium nitrate stabilized with copper oxide in combination with vanadium / molybdenum oxides therefore has a particularly favorable effect on the combustion behavior.
  • the addition of 2 to 7% by mass of the phase-stabilizing CuO provided according to the invention results in significantly higher burn-up rates and low pressure exponents. This favorable combustion behavior can be seen above all in solid fuels whose binders contain up to 50% azido compounds in the form of energetic polymers and / or plasticizers.
  • the combustion moderators have a grain size in the range from 1 to 60 ⁇ m, preferably 1 to 10 ⁇ m, and a high internal surface area of 5 to 100 m2 / g, preferably 20 to 60 m2 / g.
  • Metal-free solid fuels of the type described are suitable for use in rocket engines due to their energy content, their low-smoke, hydrochloric acid-free combustion and their comparatively low, mechanical and detonative sensitivity, while lower-energy formulations with a higher proportion of binder are suitable for use as gas generator propellants.
  • high-melting metal carbides or nitrates preferably silicon and / or zirconium carbide, with a concentration of 0.1 to 1 mass% are advantageously added as further additives.
  • these additives suppress unstable oscillations in the combustion behavior.
  • Table 1 shows five different formulations of ammonium nitrate, which is phase-stabilized with copper oxide or zinc oxide (PSAN).
  • the burning rate r (mm / s) at 20 ° C and at three different combustion chamber pressures is given in the lower part of the table for the individual formulations. Below this is the pressure exponent n for various pressure ranges given in brackets.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Air Bags (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Inorganic Insulating Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
EP95112989A 1994-10-05 1995-08-18 Propergol à base de nitrate d'ammonium nitrate à phase stabilisée Expired - Lifetime EP0705808B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4435523A DE4435523C1 (de) 1994-10-05 1994-10-05 Festtreibstoff auf der Basis von phasenstabilisiertem Ammoniumnitrat
DE4435523 1994-10-05

Publications (2)

Publication Number Publication Date
EP0705808A1 true EP0705808A1 (fr) 1996-04-10
EP0705808B1 EP0705808B1 (fr) 1997-10-29

Family

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Family Applications (1)

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EP95112989A Expired - Lifetime EP0705808B1 (fr) 1994-10-05 1995-08-18 Propergol à base de nitrate d'ammonium nitrate à phase stabilisée

Country Status (5)

Country Link
US (1) US5589661A (fr)
EP (1) EP0705808B1 (fr)
DE (2) DE4435523C1 (fr)
ES (1) ES2110285T3 (fr)
NO (1) NO303983B1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998042639A1 (fr) * 1997-03-26 1998-10-01 Basf Aktiengesellschaft Moderateurs de combustion pour melanges generateurs de gaz
CN103191748A (zh) * 2013-04-11 2013-07-10 北京科技大学 一种剑麻状CuO-ZnO复合氧化物的制备方法

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Publication number Priority date Publication date Assignee Title
WO1996019422A1 (fr) 1994-12-21 1996-06-27 Daicel Chemical Industries, Ltd. Composition generatrice de gaz
DE19742203A1 (de) * 1997-09-24 1999-03-25 Trw Airbag Sys Gmbh Partikelfreies gaserzeugendes Gemisch
US6019861A (en) * 1997-10-07 2000-02-01 Breed Automotive Technology, Inc. Gas generating compositions containing phase stabilized ammonium nitrate
US6143103A (en) * 1998-01-27 2000-11-07 Trw Inc. Gas generating material for vehicle occupant protection device
WO1999038725A2 (fr) * 1998-02-03 1999-08-05 Talley Defense Systems, Inc. Dispositif de gonflage tres mince; procede de fabrication et d'utilisation de ce dernier
US6143104A (en) * 1998-02-20 2000-11-07 Trw Inc. Cool burning gas generating composition
US6231702B1 (en) * 1998-02-20 2001-05-15 Trw Inc. Cool burning ammonium nitrate based gas generating composition
US6136113A (en) * 1998-08-07 2000-10-24 Atlantic Research Corporation Gas generating composition
US6066213A (en) * 1998-09-18 2000-05-23 Atlantic Research Corporation Minimum smoke propellant composition
US6126763A (en) * 1998-12-01 2000-10-03 Atlantic Research Corporation Minimum smoke propellant composition
US6103030A (en) * 1998-12-28 2000-08-15 Autoliv Asp, Inc. Burn rate-enhanced high gas yield non-azide gas generants
US6592691B2 (en) * 1999-05-06 2003-07-15 Autoliv Asp, Inc. Gas generant compositions containing copper ethylenediamine dinitrate
US6149746A (en) * 1999-08-06 2000-11-21 Trw Inc. Ammonium nitrate gas generating composition
EP1142853B1 (fr) * 1999-10-06 2011-03-02 Nof Corporation Composition generatrice de gaz
US6136112A (en) * 1999-10-26 2000-10-24 Trw Inc. Smokeless gas generating composition for an inflatable vehicle occupant protection device
US6156137A (en) * 1999-11-05 2000-12-05 Atlantic Research Corporation Gas generative compositions
US6224697B1 (en) 1999-12-03 2001-05-01 Autoliv Development Ab Gas generant manufacture
US6372191B1 (en) 1999-12-03 2002-04-16 Autoliv Asp, Inc. Phase stabilized ammonium nitrate and method of making the same
US6802533B1 (en) * 2000-04-19 2004-10-12 Trw Inc. Gas generating material for vehicle occupant protection device
US6436211B1 (en) 2000-07-18 2002-08-20 Autoliv Asp, Inc. Gas generant manufacture
US6652682B1 (en) * 2001-10-17 2003-11-25 The United States Of America As Represented By The Secretary Of The Navy Propellant composition comprising nano-sized boron particles
DE10224859A1 (de) * 2002-06-05 2003-12-24 Fraunhofer Ges Forschung Verfahren zur Herstellung von rieselfähigem Perchlorat und Zusammensetzung mit solchem Perchlorat
US6872265B2 (en) 2003-01-30 2005-03-29 Autoliv Asp, Inc. Phase-stabilized ammonium nitrate
CN101468935B (zh) * 2007-12-24 2012-05-09 南京理工大学 聚合物改性相稳定硝酸铵的制备方法
CN101642709B (zh) * 2008-08-04 2011-07-20 深圳大学 一种CuO-PbO/碳纳米管复合粉体及其制备方法
RU2580735C2 (ru) * 2014-09-09 2016-04-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный технический университет им. И.И. Ползунова" (АлтГТУ) Твердотопливная металлизированная композиция на основе нитрата аммония
US10415938B2 (en) 2017-01-16 2019-09-17 Spectre Enterprises, Inc. Propellant
US11112222B2 (en) 2019-01-21 2021-09-07 Spectre Materials Sciences, Inc. Propellant with pattern-controlled burn rate
CN114539012A (zh) * 2020-11-25 2022-05-27 北京理工大学 一种适用于gap基浇注***及推进剂的复合含能增塑剂及其制法和应用
IL305237A (en) 2021-02-16 2023-10-01 Spectre Mat Sciences Inc Primer for firearms and other weapons
CN113376208B (zh) * 2021-06-09 2023-04-25 四川弘博新材科技股份有限公司 钼在提升含硼的含能材料反应性能中的应用

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DE3642850C1 (de) * 1986-12-16 1988-02-18 Fraunhofer Ges Forschung Verfahren zur Herstellung von partikelfoermigem Ammoniumnitrat fuer feste Treib- oder Explosivstoffe
GB2200903A (en) * 1987-02-12 1988-08-17 Bayern Chemie Gmbh Flugchemie A composite solid propellant
US5074938A (en) * 1990-05-25 1991-12-24 Thiokol Corporation Low pressure exponent propellants containing boron
US5076868A (en) * 1990-06-01 1991-12-31 Thiokol Corporation High performance, low cost solid propellant compositions producing halogen free exhaust
EP0553476A1 (fr) * 1991-12-27 1993-08-04 Hercules Incorporated Propergol composite sans chlore pour fusée
EP0576326A1 (fr) * 1992-06-12 1993-12-29 S.N.C. Livbag Composition pyrotechnique génératrice de gaz chauds non toxiques et son utilisation dans un système de protection des occupants d'un véhicule automobile

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EP0584899A3 (fr) * 1992-08-05 1995-08-02 Morton Int Inc Approche par incorporation d'additifs en compositions génératrices de gaz à base d'azoture pour ajuster le point de fusion des scories et la vitesse de combustion.
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Publication number Priority date Publication date Assignee Title
GB862289A (en) * 1956-03-26 1961-03-08 Phillips Petroleum Co Solid propellants
US2949352A (en) * 1956-10-01 1960-08-16 North American Aviation Inc Propellant composition
US3027282A (en) * 1958-12-29 1962-03-27 Phillips Petroleum Co Composite propellants containing modifying agents
US4158583A (en) * 1977-12-16 1979-06-19 Nasa High performance ammonium nitrate propellant
DE3642850C1 (de) * 1986-12-16 1988-02-18 Fraunhofer Ges Forschung Verfahren zur Herstellung von partikelfoermigem Ammoniumnitrat fuer feste Treib- oder Explosivstoffe
GB2200903A (en) * 1987-02-12 1988-08-17 Bayern Chemie Gmbh Flugchemie A composite solid propellant
US5074938A (en) * 1990-05-25 1991-12-24 Thiokol Corporation Low pressure exponent propellants containing boron
US5076868A (en) * 1990-06-01 1991-12-31 Thiokol Corporation High performance, low cost solid propellant compositions producing halogen free exhaust
EP0553476A1 (fr) * 1991-12-27 1993-08-04 Hercules Incorporated Propergol composite sans chlore pour fusée
EP0576326A1 (fr) * 1992-06-12 1993-12-29 S.N.C. Livbag Composition pyrotechnique génératrice de gaz chauds non toxiques et son utilisation dans un système de protection des occupants d'un véhicule automobile

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998042639A1 (fr) * 1997-03-26 1998-10-01 Basf Aktiengesellschaft Moderateurs de combustion pour melanges generateurs de gaz
CN103191748A (zh) * 2013-04-11 2013-07-10 北京科技大学 一种剑麻状CuO-ZnO复合氧化物的制备方法
CN103191748B (zh) * 2013-04-11 2014-10-15 北京科技大学 一种剑麻状CuO-ZnO复合氧化物的制备方法

Also Published As

Publication number Publication date
NO953922L (no) 1996-04-09
EP0705808B1 (fr) 1997-10-29
NO953922D0 (no) 1995-10-03
ES2110285T3 (es) 1998-02-01
NO303983B1 (no) 1998-10-05
DE4435523C1 (de) 1996-06-05
US5589661A (en) 1996-12-31
DE59500909D1 (de) 1997-12-04

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