EP0705809B1 - Propergol à base de nitrate d'ammonium à phase stabilisée - Google Patents

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

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Publication number
EP0705809B1
EP0705809B1 EP95112990A EP95112990A EP0705809B1 EP 0705809 B1 EP0705809 B1 EP 0705809B1 EP 95112990 A EP95112990 A EP 95112990A EP 95112990 A EP95112990 A EP 95112990A EP 0705809 B1 EP0705809 B1 EP 0705809B1
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Prior art keywords
solid propellant
propellant according
mass
combustion
oxide
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Expired - Lifetime
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EP95112990A
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German (de)
English (en)
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EP0705809A1 (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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    • 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
    • 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

Definitions

  • the invention relates to a solid fuel for rocket engines or gas generators, which contains ammonium nitrate (AN) in pure or phase-stabilized form (PSAN) as an oxidizer.
  • AN ammonium nitrate
  • PSAN phase-stabilized form
  • 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.
  • the combustion 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 object of the invention is to improve the combustion behavior of solid fuels on the basis of pure and phase-stabilized ammonium nitrate.
  • such a solid fuel consists of 35 to 80% by mass ammonium nitrate (AN) in pure form or phase-stabilized form (PSAN) with nickel oxide, potassium or cesium nitrate with an average grain size of 5 to 200 ⁇ m, 15 to 50% by mass of a binder system from one Binder polymer and a high-energy plasticizer as well as 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 form
  • 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 favorable 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 distinguished by the fact that they contain pure AN as the oxidizer or phase-stabilized ammonium nitrate reacted with nickel oxide, potassium or cesium nitrate as the oxidizer, the nickel oxides preferably containing 1 to 7% by mass, potassium or cesium nitrate containing 3 to 15 % By mass are used. 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 the additives with the melt of the pure ammonium nitrate with elimination of water.
  • AN is preferably used in pure form with a water content below 0.2% by mass or NiO-stabilized PSAN, while PSAN stabilized with potassium or cesium nitrate brings with it somewhat higher smoke proportions.
  • the combustion behavior is significantly influenced by the grain size of the AN or PSAN.
  • 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 or PSAN fraction predominantly in smaller ones Grain size from 10 to 80 ⁇ m and less in average grain size from 100 to 160 ⁇ m is available.
  • the solid propellant according to the invention can also contain high-energy substances, in particular nitramines, such as hexogen (RDX) or octogen (HMX) with an average particle size of 2 to 200 ⁇ m with a proportion of 1 to 4% by mass.
  • nitramines such as hexogen (RDX) or octogen (HMX) with an average particle size of 2 to 200 ⁇ m with a proportion of 1 to 4% 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 ester, with small amounts in the range of 0.5% by mass of the magnesium oxide acting in the same sense.
  • combustion moderators made from vanadium / molybdenum oxide as oxide mixture or mixed oxide used according to the invention with 0.2 to 5.0 mass% are advantageously added with carbon black or graphite in a fraction of 5 to 20 mass% of the fraction of the combustion moderator.
  • binder system consisting of a binder polymer and a high-energy plasticizer.
  • the binder polymer itself can be inert, it preferably being an isocyanate-curing, bifunctional or trifunctionally hydroxyl-substituted polyester or polyether prepolymer.
  • 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
  • nitro plasticizer is a 1: 1 mixture of bisdinitropropyl formal / acetal (BDNPF / A), while a nitro amino plasticizer is a 1: 1 mixture of N-ethyl and N-methylnitratoethylnitroamine (EtNENA, MeNENA) or Nn-butyl-N -nitratoethylnitroamine (BuNENA) or N, N'-dinitratoethylnitroamine (DINA) is suitable.
  • EtNENA N-ethyl and N-methylnitratoethylnitroamine
  • BuNENA Nn-butyl-N -nitratoethylnitroamine
  • DINA N, N'-dinitratoethylnitroamine
  • GAP-A bisazido-terminated GAP oligomers
  • DANPE 5-diazido-3-nitroaminopentane
  • the ratio polymer / plasticizer is 1: 3 to 20: 1 mass%.
  • the binder polymers can of course also be used in pure form.
  • the purer or phase stabilized ammonium nitrate is preferably 0.1 to 1% by mass of its anti-caking agent fraction, e.g. ultra-fine (grain size about 0.02 ⁇ m) silica gel, sodium lauryl sulfonate, tricalcium phosphate or other surfactants are added.
  • its anti-caking agent fraction e.g. ultra-fine (grain size about 0.02 ⁇ m) silica gel, sodium lauryl sulfonate, tricalcium phosphate or other surfactants are added.
  • the vanadium / molybdenum oxide combustion moderators can be ideally combined with nickel and copper salts, oxides or complexes, which leads to a further increase in the combustion rate.
  • the combustion moderators preferably consist of mixed oxides in which molybdenum is present in the + VI and + V oxidation states and vanadium in the + IV and + V oxidation states.
  • Exemplary compositions of the mixed oxides are V 6 Mo 4 O 25 and V 6 Mo 15 O 60 .
  • the mixed oxides can furthermore contain chromium (III) and titanium (IV) oxides as the inactive carrier material or one which also participates in the reaction.
  • 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 m 2 / g, preferably 20 to 60 m 2 / g.
  • the burning rate in the low pressure range can be increased further compared to coarser grain and the pressure exponent can be further reduced.
  • the solid propellants according to the invention experience an advantageous further development in that high-melting Metal carbides or nitrides, preferably silicon and zirconium carbide in the concentration range from 0.1 to 1 mass% are added. Above all, this suppresses an unstable, oscillating combustion behavior when used in rocket engines. This is particularly important for low-smoke burning fuels without the addition of metal.
  • Solid fuels of the type described in particular with oxidizers in the form of pure AN or Ni-PSAN, are suitable due to their energy content, their low-smoke, hydrochloric acid-free combustion and their comparatively low, mechanical and detonative sensitivity for use in rocket engines, while lower-energy formulations with a higher binder content are suitable for use as gas generator propellants.
  • Table 1 shows nine different formulations with pure ammonium nitrate and a PSAN phase-stabilized with 3% nickel oxide.
  • 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.
  • AN3 to AN8 Due to the high plasticizer content, AN3 to AN8 have high specific impulses of 234s for AN6 and AN8 and 237s for AN3, AN4 and AN5 with a relaxation ratio of 70: 1.
  • the synergistic effect of copper compounds and V / Mo oxide combustion moderators has proven to be particularly favorable. Copper phthalocyanate has proven to be the most favorable in the combination of increase in the rate of combustion, reduction in the pressure exponent and acceptable stability properties.
  • the burning behavior of the formulation AN9 shows that the nickel diaminodinitrate as phase stabilizer in the AN also has a favorable effect on the burning behavior. This is also observed with the addition of nickel phthalocyanate in the AN8 formulation. The addition of RDX also increases the burning rate without, however, positively influencing the pressure exponent.
  • Table 2 shows with the examples AN10, AN11 and AN12 AN / GAP fuel formulations in which the combustion moderator is contained in different grain sizes and grain distributions with otherwise the same composition.
  • the lower part of the table clearly shows the increase in the burn-off rate achieved with the grain becoming smaller, while at the same time lowering the pressure exponent.
  • AN13 shows the burning behavior when formulated with an azido softener
  • AN14 is a formulation with the addition of zirconium carbide, with the help of which combustion oscillations are suppressed when the fuel is used in rocket engines.
  • Figure 3 shows effective combustion control even with a high nitrate ester content in the fuel without RDX addition. This is due to the synergistic effect of Cu and Ni complexes with the V / Mo oxide combustion moderators.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Claims (25)

  1. Propergol pour propulsion des fusées ou générateurs à gaz qui consiste en une quantité de 35 à 80 % en masse, de nitrate d'ammonium (AN) sous forme pure ou sous forme à phase stabilisée avec de l'oxyde de nickel, du nitrate de potassium ou de césium (PSAN) ayant une taille moyenne de grains de 5 à 200 µm, 15 à 50 % en masse d'un système d'agents liants à base d'un polymère d'agent liant et d'un agent plastifiant à haute énergie ainsi que 0,2 à 5 % en masse d'un modérateur de combustion à base d'oxyde de vanadium/oxyde de molybdène comme mélange d'oxydes ou d'oxyde mixte.
  2. Propergol selon la revendication 1,
    avec une quantité supplémentaire de 1 à 40 % en masse d'une nitramine à haute énergie choisie parmi l'hexogène ou l'octogène, ayant une taille moyenne de grains de 2 à 200 µm.
  3. Propergol selon la revendication 1 ou la revendication 2,
    ayant une quantité supplémentaire allant de 0,5 à 20 % en masse de métaux choisis parmi l'aluminium, le magnésium et le bore, ayant une taille de grains allant de 0,1 à 50 µm.
  4. Propergol selon l'une des revendications 1 à 3, ayant une quantité supplémentaire de 0,4 à 2 % en masse d'un agent stabilisant à action comme capteur d'oxyde d'azote et d'acides à base de diphénylamine de 2-nitrodiphénylamine ou de N-méthylnitroaniline ou d'une combinaison de ceux-ci.
  5. Propergol selon l'une des revendications 1 à 4, ayant un ajout de noir de fumée ou de graphite avec de 5 à 50 % en masse de la fraction du modérateur de combustion.
  6. Propergol selon l'une des revendications 1 à 5, dans lequel le polymère d'agent liant est un prépolymère du type polyester ou du type polyéther substitué par un hydroxy bi- ou trifonctionnel, qui durcit avec un isocyanate.
  7. Propergol selon l'une des revendications 1 à 5, dans lequel le polymère d'agent liant est un polymère à énergie élevée.
  8. Propergol selon la revendication 7,
    dans lequel le polymère à énergie élevée est un polymère du type glycidylazido (GAP) substitué par un hydroxyle, bi ou trifonctionnel, durcissant avec un isocyanate.
  9. Propergol selon l'une des revendications 1 à 8, dans lequel le plastifiant à énergie élevée est choisi dans le groupe des esters d'acide nitrique stables chimiquement, des agents plastifiants du type nitro, nitroamino ou azido.
  10. Propergol selon la revendication 9,
    dans lequel l'ester d'acide nitrique est un trinitrate de triméthyloléthane (TMETN), le trinitrate de butanetriol (BTTN) ou le dinitrate de diéthylèneglycol (DEGDN).
  11. Propergol selon la revendication 9,
    dans lequel l'agent plastifiant du type nitro est un mélange 1:1 de bis dinitropropylformal/bis dinitropropylacétal (BDNPF/BDNPA).
  12. Propergol selon la revendication 9,
    dans lequel l'agent plastifiant du type nitroamino est un mélange 1:1 de N-éthyl et de N-méthylnitratoéthylnitroamine (EtNENA et MeNENA) ou de N-n-butyl-N-nitratoéthylnitramine (BuNENA) ou la N,N'-dinitratoéthylnitramine (DINA).
  13. Propergol selon la revendication 9,
    dans lequel l'agent plastifiant du type azido est formé d'oligomères GAP à chaîne courte (GAP-A) ayant des groupes terminaux bisazido ou de 1,5-diazido-3-nitroaminopentane (DANPE).
  14. Propergol selon l'une des revendications 1 à 13,
    caractérisé en ce que
    les polymères d'agent liant et les agents plastifiants sont présents en fonction du type de la compatibilité et de la teneur en énergie dans le système d'agents liants, dans un rapport de 1:3 à 20:1 % en masse.
  15. Propergol selon l'une des revendications 1 à 14, dans lequel le nitrate d'ammonium pur possède une teneur en eau en dessous de 0,2 % en masse.
  16. Propergol selon l'une des revendications 1 à 14, dans lequel on met en oeuvre le nitrate d'ammonium qui est à phase stabilisée par réaction avec 1 à 7 % en masse d'oxyde de nickel ou avec 3 à 15 % en masse de nitrate de potassium ou de césium.
  17. Propergol selon la revendication 16,
    dans lequel le nitrate d'ammonium à phase stabilisée (PSAN) est accessible par incorporation par mélange des additifs dans le produit de fusion du nitrate d'ammonium pur (AN) et pulvérisation du produit de fusion tout en refroidissant en même temps.
  18. Propergol selon l'une des revendications 15 à 17,
    dans lequel on ajoute au nitrate d'ammonium de 0,1 à 1 % en masse de sa fraction en silicagel ultra fin (taille de grains environ 0,02 µm), de laurylsulfonate de sodium, de phosphate tricalcique et d'autres agents tensioactifs comme agent anti-agrégation.
  19. Propergol selon l'une des revendications 1 à 18,
    dans lequel le nitrate d'ammonium se présente avec une taille de grain de 10 à 80 µm.
  20. Propergol selon l'une des revendications 1 à 19, dans lequel les modérateurs de combustion en oxyde de vanadium/oxyde de molybdène sont mis en oeuvre en liaison avec des sels, des oxydes ou des complexes de Cu et de Ni.
  21. Propergol selon l'une des revendications 1 à 20,
    dans lequel les modérateurs de combustion renferment des oxydes mixtes de molybdène du degré d'oxydation +VI et de vanadium des degrés d'oxydation +V et +IV.
  22. Propergol selon l'une des revendications 1 à 21, dans lequel les modérateurs de combustion possèdent comme matériau support des oxydes de chrome (III) ou de titane (IV).
  23. Propergol selon l'une des revendications 1 à 22,
    caractérisé en ce que
    les modérateurs de combustion possèdent une taille de grain dans la zone allant de 1 à 60 µm, de préférence de 1 à 10 µm, et une grande surface interne allant de 5 à 100 m2/g, de préférence de 20 à 66 m2/g.
  24. Propergol selon l'une des revendications 1 à 23,
    caractérisé en ce que
    celui-ci renferme pour l'utilisation dans des moteurs de fusée, de 0,1 à 1 % en masse de carbure ou de nitrure métallique à point de fusion élevé comme additif pour supprimer un comportement à la combustion instable oscillant.
  25. Propergol selon la revendication 22,
    caractérisé en ce que
    les additifs sont le carbure de silicium et/ou de zirconium.
EP95112990A 1994-10-05 1995-08-18 Propergol à base de nitrate d'ammonium à phase stabilisée Expired - Lifetime EP0705809B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4435524A DE4435524C2 (de) 1994-10-05 1994-10-05 Festtreibstoff auf der Basis von reinem oder phasenstabilisiertem Ammoniumnitrat
DE4435524 1994-10-05

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EP0705809A1 EP0705809A1 (fr) 1996-04-10
EP0705809B1 true EP0705809B1 (fr) 1997-07-02

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US (1) US5596168A (fr)
EP (1) EP0705809B1 (fr)
DE (2) DE4435524C2 (fr)
ES (1) ES2105826T3 (fr)
NO (1) NO303909B1 (fr)

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Publication number Publication date
DE4435524A1 (de) 1996-04-11
EP0705809A1 (fr) 1996-04-10
NO953923D0 (no) 1995-10-03
DE59500344D1 (de) 1997-08-07
ES2105826T3 (es) 1997-10-16
NO303909B1 (no) 1998-09-21
NO953923L (no) 1996-04-09
DE4435524C2 (de) 1996-08-22
US5596168A (en) 1997-01-21

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