EP0953555A1 - Procédé de préparation de particules de propergols et explosifs fusibles - Google Patents

Procédé de préparation de particules de propergols et explosifs fusibles Download PDF

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Publication number
EP0953555A1
EP0953555A1 EP99105812A EP99105812A EP0953555A1 EP 0953555 A1 EP0953555 A1 EP 0953555A1 EP 99105812 A EP99105812 A EP 99105812A EP 99105812 A EP99105812 A EP 99105812A EP 0953555 A1 EP0953555 A1 EP 0953555A1
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EP
European Patent Office
Prior art keywords
matrix liquid
emulsion
melt
particles
adn
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
Application number
EP99105812A
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German (de)
English (en)
Other versions
EP0953555B1 (fr
Inventor
Ulrich Dipl.-Ing. Teipel
Horst Dr. Krause
Karlfred Leisinger
Thomas Heintz
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.)
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Filing date
Publication date
Application filed by Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Publication of EP0953555A1 publication Critical patent/EP0953555A1/fr
Application granted granted Critical
Publication of EP0953555B1 publication Critical patent/EP0953555B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033Shaping the mixture
    • C06B21/0066Shaping the mixture by granulation, e.g. flaking
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033Shaping the mixture
    • C06B21/005By a process involving melting at least part of the ingredients
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00Compositions containing an inorganic nitrogen-oxygen salt

Definitions

  • the invention relates to a method for producing essentially spherical particles of meltable, moisture-sensitive fuels and explosives and oxidizers, especially ammonium dinitramide (ADN).
  • ADN ammonium dinitramide
  • Ammonium dinitramide is an oxidizer for fuels and of great importance as an explosive. In the application are for both manufacturing and processing compactible particles desired. In the Manufacture of conventional crystalline fuels and explosives but usually arise very irregular Particle. This applies in particular to ADN.
  • the crystalline substance mostly with heating in one or dissolved in several suitable solvents and by defined cooling, the substance crystallizes out. This process can be carried out several times if necessary become. Due to the differences in solubility between Substance and impurities become unwanted accompanying substances severed because they're either a priori remain unsolved, or because if they are also in Solution because of their low concentration the matrix liquid remain when the crystals has already failed.
  • Inoculation of supersaturated solutions is also known or hypothermic melting, with traces of Solid substance in the form of germs that prevent the formation of solid phase can be added.
  • GB 2 187 726 A describes a process for the production a solid explosive mixture, so-called emulsion explosives, being a discontinuous phase in the form an oxidizer salt heated and melted and in one continuous phase serving as fuel, e.g. Paraffin oil or wax, is emulsified.
  • the emulsion additives such as emulsifiers or crystallization nuclei, added to a finely dispersed to get discontinuous phase and a confluence to prevent the disperse drops.
  • the emulsion is cooled, whereby an explosive mixture is obtained in which the oxidizer salts are finely dispersed are a spontaneous detonation, as in coarsely dispersed Prevent particles from occurring.
  • the invention has for its object a method for the production of uniform, in particular spherical Particles more meltable, more sensitive to moisture
  • ADN Ammonium dinitramide
  • the propellant or Explosive or the oxidizer converted into a melt and combined with a matrix liquid in the substance to be recrystallized is difficult or impossible is soluble.
  • the matrix liquid ensures that the moisture-sensitive fuels and explosives and oxidizers, such as the particularly hygroscopic ADN, no water during recrystallization, e.g. Humidity. It is chosen so that the molten substance can be emulsified. The later one The phase mixture is separated solely on the basis of the different melting points of the starting material and matrix fluid and not due to changes in concentration a solution.
  • the focus is to make available the melt in the matrix liquid preferably less than 50% by mass and in particular less than 60 % By mass.
  • the matrix liquid after crystallization is separated, can be reused and for example be carried out in a cycle.
  • the melt can be in the fuel or explosive or additives soluble in the oxidizer are mixed with those regarding the later product quality of the ADN particles Stability, sensitivity or fluidity can be improved.
  • a matrix liquid primarily oils, e.g. Paraffin oil or silicone oil, in Question, which have a hydrophobic character.
  • oils e.g. Paraffin oil or silicone oil, in Question, which have a hydrophobic character.
  • spherical Particles with defined particle properties, e.g. average particle size, particle size distribution, specific Preserve surface. The spherical particles not only lead to an optimal bulk and knock density, but also to a high energy density and favorable combustion behavior.
  • the emulsion is produced by introducing Energy into the fluid system. This can be done by shaking, Stirring, by introducing vibrations into the system, e.g. by means of ultrasound or by injecting the Melt into the matrix liquid or vice versa.
  • Emulsifiers and stabilizers can interfacial tension between both components and the viscosity the outer phase, and thus the manufacturing conditions and affects the stability of the emulsion become.
  • an emulsion of hygroscopic ADN in hydrophobic matrix liquid also hydrophobic emulsifier, e.g. Silicon dioxide, added the stability of the emulsion is increased and the coalescence at which the emulsified droplets flow together to form a continuous phase, reduced. Consequently, by adding a such emulsifier under otherwise the same boundary conditions an emulsion of finer droplets can be achieved. Conversely, if a stabilizer is added, otherwise the same boundary conditions are larger droplets of emulsified substance.
  • the ADN droplets as a disperse phase and one Matrix liquid existing and above the melting point emulsion tempered by ADN is in the third step of the inventive method below the melting point of Cooled down ADN, so that the disperse ADN drops to solid crystallize particles.
  • the crystallization process can, in addition to the use of a specially for the Crystallization required temperature gradients, both by entering mechanical energy, as well can be controlled by adding crystallization nuclei.
  • the entry of mechanical energy during crystallization to produce the finest possible crystalline product can be done using a stirrer or ultrasound the concentration of the disperse phase can be controlled can.
  • the inventive method can be both continuous as well as carried out in batches.
  • a discontinuous process variant in which the manufacture the emulsion and the crystallization of the disperse Drops can be carried out in a reactor e.g. various stirrers, such as blade or propeller stirrers, or discontinuous gear rim disperser for Preparation of the emulsion.
  • a reactor e.g. various stirrers, such as blade or propeller stirrers, or discontinuous gear rim disperser for Preparation of the emulsion.
  • With input of stirring energy the emulsion is then cooled, so that spherical Crystallize particles.
  • the two process steps of emulsification and recrystallization can also be carried out separately in terms of time and location be, the emulsion after its preparation is conveyed into a second reactor in which the Recrystallization, e.g. through a suitable temperature gradient, can be influenced in a targeted manner.
  • the emulsion initially using colloid mills, static mixers or continuous gear rim dispersion machines and then into the crystallization zone, e.g. in a tubular reactor or cascade crystallizer.
  • a separation unit for separating the recrystallized particles from the matrix liquid provided, the separation by sedimentation, Filtration or centrifugation can be done. After this The particles are separated with a suitable one Washed solvent and dried.
  • ADN crystalline ammonium dinitramide
  • the grain is jagged and angular. Grain size and grain shape vary widely.
  • 2 and 3 show with the inventive method from a paraffin emulsion manufactured spherical particles of ammonium dinitramide (ADN) with an average grain diameter below 500 ⁇ m in two different magnifications. The grain is almost exactly spherical and that Grain spectrum is relatively narrow.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Colloid Chemistry (AREA)
  • Silicon Compounds (AREA)
EP19990105812 1998-04-16 1999-03-23 Procédé de préparation de particules de propergols et explosifs fusibles Expired - Lifetime EP0953555B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19816853 1998-04-16
DE1998116853 DE19816853A1 (de) 1998-04-16 1998-04-16 Verfahren zur Herstellung von Partikeln schmelzfähiger Treib- und Explosivstoffe

Publications (2)

Publication Number Publication Date
EP0953555A1 true EP0953555A1 (fr) 1999-11-03
EP0953555B1 EP0953555B1 (fr) 2005-09-21

Family

ID=7864703

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19990105812 Expired - Lifetime EP0953555B1 (fr) 1998-04-16 1999-03-23 Procédé de préparation de particules de propergols et explosifs fusibles

Country Status (3)

Country Link
EP (1) EP0953555B1 (fr)
DE (2) DE19816853A1 (fr)
NO (1) NO312954B1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2884244A1 (fr) * 2005-04-12 2006-10-13 Snpe Materiaux Energetiques Sa Obtention de cristaux de dinitroamidure d'ammonium (adn); cristaux d'adn et les composites energetiques en contenant.
WO2019229385A1 (fr) * 2018-05-30 2019-12-05 Arianegroup Sas Procede d'obtention de cristaux de dinitroamidure d'ammonium (adn); cristaux d'adn et les composites energetiques en contenant
DE102020122328B3 (de) 2020-08-26 2021-08-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein Verfahren zur Herstellung von Partikeln aus Ammoniumdinitramid (ADN)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10201937B4 (de) * 2002-01-19 2005-08-04 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung von mit Additiven versetztem Ammoniumdinitramid (ADN)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2887723A (en) * 1955-02-23 1959-05-26 Stamicarbon Process for granulating material
US3468986A (en) * 1966-11-15 1969-09-23 David J Watanabe Method for producing a solid particulate material
US3522334A (en) * 1961-05-09 1970-07-28 Exxon Research Engineering Co Preparation of spherical solid oxidizer pellets from nitronium perchlorate-lithium perchlorate mixture
DE1467203A1 (de) * 1964-09-09 1972-01-27 Bundesrep Deutschland Verfahren zur Herstellung von kugeligem,nicht backendem Ammoniumnitrat mit einer mittleren Korngroesse von etwa 10 bis 300 mu
US4118797A (en) * 1977-10-25 1978-10-03 Energy And Minerals Research Co. Ultrasonic emulsifier and method
DE2924029A1 (de) * 1978-06-13 1979-12-20 Montedison Spa Verfahren zur herstellung von sphaeroidisch geformten, bei raumtemperatur festen produkten
US5071635A (en) * 1988-02-18 1991-12-10 Mitsubishi Materials Corporation Method of preparing ceramic microspheres
WO1993016415A1 (fr) * 1992-02-14 1993-08-19 Research Laboratories Of Australia Pty. Ltd. Particules spheroïdales utiles en electrostatographie
EP0759324A2 (fr) * 1995-08-18 1997-02-26 Rohm And Haas Company Un produit perlé formé à base d'eau
WO1997047571A1 (fr) * 1996-06-11 1997-12-18 United Technologies Corporation Procede de preparation de particules spheriques de composes energetiques

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2187726B (en) * 1986-03-14 1989-11-15 Ici Plc Solid explosive composition.

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2887723A (en) * 1955-02-23 1959-05-26 Stamicarbon Process for granulating material
US3522334A (en) * 1961-05-09 1970-07-28 Exxon Research Engineering Co Preparation of spherical solid oxidizer pellets from nitronium perchlorate-lithium perchlorate mixture
DE1467203A1 (de) * 1964-09-09 1972-01-27 Bundesrep Deutschland Verfahren zur Herstellung von kugeligem,nicht backendem Ammoniumnitrat mit einer mittleren Korngroesse von etwa 10 bis 300 mu
US3468986A (en) * 1966-11-15 1969-09-23 David J Watanabe Method for producing a solid particulate material
US4118797A (en) * 1977-10-25 1978-10-03 Energy And Minerals Research Co. Ultrasonic emulsifier and method
DE2924029A1 (de) * 1978-06-13 1979-12-20 Montedison Spa Verfahren zur herstellung von sphaeroidisch geformten, bei raumtemperatur festen produkten
US5071635A (en) * 1988-02-18 1991-12-10 Mitsubishi Materials Corporation Method of preparing ceramic microspheres
WO1993016415A1 (fr) * 1992-02-14 1993-08-19 Research Laboratories Of Australia Pty. Ltd. Particules spheroïdales utiles en electrostatographie
EP0759324A2 (fr) * 1995-08-18 1997-02-26 Rohm And Haas Company Un produit perlé formé à base d'eau
WO1997047571A1 (fr) * 1996-06-11 1997-12-18 United Technologies Corporation Procede de preparation de particules spheriques de composes energetiques

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2884244A1 (fr) * 2005-04-12 2006-10-13 Snpe Materiaux Energetiques Sa Obtention de cristaux de dinitroamidure d'ammonium (adn); cristaux d'adn et les composites energetiques en contenant.
WO2006108991A2 (fr) * 2005-04-12 2006-10-19 Snpe Materiaux Energetiques Obtention de cristaux de dinitroamidure d'ammonium (adn) ; cristaux d'adn et les composites energetiques en contenant
WO2006108991A3 (fr) * 2005-04-12 2007-03-22 Snpe Materiaux Energetiques Obtention de cristaux de dinitroamidure d'ammonium (adn) ; cristaux d'adn et les composites energetiques en contenant
US7789980B2 (en) 2005-04-12 2010-09-07 Snpe Materiaux Energetiques Preparation of ammonium dinitroamide (ADN) crystals, ADN crystals and energetic composites containing them
WO2019229385A1 (fr) * 2018-05-30 2019-12-05 Arianegroup Sas Procede d'obtention de cristaux de dinitroamidure d'ammonium (adn); cristaux d'adn et les composites energetiques en contenant
FR3081864A1 (fr) * 2018-05-30 2019-12-06 Arianegroup Sas Obtention de cristaux de dinitroamidure d'ammmonium (adn) ; cristaux d'adn et les composites energetiques en contenant
DE102020122328B3 (de) 2020-08-26 2021-08-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein Verfahren zur Herstellung von Partikeln aus Ammoniumdinitramid (ADN)

Also Published As

Publication number Publication date
NO991178L (no) 1999-10-18
EP0953555B1 (fr) 2005-09-21
DE59912567D1 (de) 2006-02-02
NO991178D0 (no) 1999-03-10
DE19816853A1 (de) 1999-10-21
NO312954B1 (no) 2002-07-22

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