EP0663896B1 - Produit precurseur de poudre - Google Patents

Produit precurseur de poudre Download PDF

Info

Publication number
EP0663896B1
EP0663896B1 EP93922517A EP93922517A EP0663896B1 EP 0663896 B1 EP0663896 B1 EP 0663896B1 EP 93922517 A EP93922517 A EP 93922517A EP 93922517 A EP93922517 A EP 93922517A EP 0663896 B1 EP0663896 B1 EP 0663896B1
Authority
EP
European Patent Office
Prior art keywords
nitrocellulose
crystalline
explosive
explosive substance
crystalline explosive
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.)
Expired - Lifetime
Application number
EP93922517A
Other languages
German (de)
English (en)
Other versions
EP0663896A1 (fr
Inventor
Gregor Fels
Gerhard Ewald
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.)
Wasagchemie Sythen GmbH
Original Assignee
Wasagchemie Sythen GmbH
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 Wasagchemie Sythen GmbH filed Critical Wasagchemie Sythen GmbH
Publication of EP0663896A1 publication Critical patent/EP0663896A1/fr
Application granted granted Critical
Publication of EP0663896B1 publication Critical patent/EP0663896B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B25/00—Compositions containing a nitrated organic compound
    • C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033—Shaping the mixture
    • C06B21/0066—Shaping the mixture by granulation, e.g. flaking
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier

Definitions

  • the invention relates to a method for producing a precursor for powder or explosive, which consists essentially of nitrocellulose and at least one crystalline explosive, in particular hexogen, and in which the crystalline explosive is combined with the nitrocellulose in the aqueous phase. Furthermore, the invention relates to a precursor for powder or explosive, which essentially consists of nitrocellulose and at least one crystalline explosive, which was combined with the nitrocellulose in the aqueous phase.
  • a powder raw mass is usually first produced, which essentially consists of nitrocellulose and an explosive oil, for example diglycol dinitrate. Hexogen is then introduced into this raw powder mass as a further working step.
  • a method for producing a rocket fuel is already known from US Pat. No. 3,702,272, in which a nitrocellulose lacquer is stirred into the aqueous suspension of a crystalline explosive, for example hexogen.
  • the crystalline explosive in the suspension should have a grain size of 0.1 to 150 ⁇ m, preferably 1 to 30 ⁇ m.
  • the nitrocellulose lacquer added to the suspension is obtained beforehand by dissolving nitrocellulose in an organic solvent.
  • the known method has been proposed primarily in terms of the safe handling of the very sensitive crystalline explosive during manufacture.
  • An explosive is also already known from US Pat. No. 3,311,513, which consists of a nitramine as crystalline component, nitrocellulose and a plasticizer for the nitrocellulose.
  • the nitramine should preferably be one Particle size between 1 and 75 microns.
  • the nitramine is first introduced into the plasticizer and then the nitrocellulose.
  • an explosive consisting of a nitramine and a highly viscous, plasticized nitrocellulose is known from US Pat. No. 401,472, in which the particle size of the crystalline component should be less than 25 ⁇ m.
  • the object of the invention is to propose a method in which the crystalline explosive is distributed particularly uniformly in the raw mass of the preliminary product.
  • the process according to the invention allows the crystalline explosive to be distributed particularly uniformly in the raw mass of the preliminary product. In addition to the very homogeneous distribution, it is also achieved that the crystalline explosive component is particularly firmly connected to the nitrocellulose and thus has a high abrasion resistance.
  • the finely crystalline explosive with the specified average particle diameter can be drawn onto the fibers of the nitrocellulose.
  • the crystalline explosive and the nitrocellulose are each stirred in the aqueous phase in a separate container.
  • the crystalline explosive can advantageously be stirred up in surfactant water (for example with a surfactant concentration of 0.1%).
  • the components that are stirred up are then brought together with stirring. As a result, particularly good mixing between the crystalline explosive and the nitrocellulose is achieved.
  • An explosive oil in particular diglycol dinitrate, can advantageously be added and preferably stirred after the nitrocellulose and crystalline explosive have been brought together. The resulting gelatinization of the nitrocellulose results in an additional binding of the crystalline explosive to the nitrocellulose.
  • an explosive oil in particular diglycol dinitrate, can be combined with the nitrocellulose and then the crystalline explosive can then be added.
  • the raw mass containing the crystalline explosive is separated from the liquid, a centrifugation method preferably being used. It has been shown that after drying the filter cake there is no increased formation of dust under mechanical stress compared to known powder raw materials which have no crystalline explosive component. This makes it clear that the crystalline explosive is particularly intimately involved.
  • a propeller stirrer can be used for stirring.
  • the method according to the invention can also be used with a crystalline explosive which has a wax additive.
  • a wax additive serve to desensitize the highly explosive crystalline explosive.
  • the nitrocellulose used advantageously has a nitrogen content of about 12.6%.
  • the stirring in water takes place with little turbulence.
  • At least one further explosive in particular nitroguanidine, can be added to the preliminary product.
  • the further explosive is again added in suspension in accordance with the primary explosive.
  • the crystalline explosive is particularly evenly distributed with respect to the nitrocellulose and firmly integrated into it.
  • the new intermediate product has very uniform properties and a particularly high abrasion resistance.
  • crystalline explosives, in particular hexogen, with a wax content can also be used.
  • the preliminary product advantageously contains an explosive oil, in particular diglycol dinitrate.
  • the process described below is intended to produce a raw material for a propellant charge powder which contains about 55% nitrocellulose, 34% diglycol dinitrate and about 11% crystalline explosive.
  • the nitrocellulose used has a nitrogen content of 12.6% and a water content of 33.3%.
  • the moist crystalline explosive is first stirred intimately in a first stirred container with a small amount of surfactant water (surfactant concentration 0.1%) and then stirred up with milk cream with the further addition of water. If the turbulence is low, the nitrocellulose is also stirred in water in a second stirred tank. In this slurry, the contents of the first stirred tank are added in portions with continued stirring. Then continue stirring for about 10 minutes. Subsequently, diglycol dinitrate is added in a thin stream with moderate stirring and stirring is continued for about 20 minutes. The raw material containing hexogen is then centrifuged off.
  • surfactant water surfactant concentration 0.15%
  • the still moist raw material of the preliminary product is obtained as a centrifugate.
  • this raw material containing the crystalline explosive cannot be distinguished from conventional raw materials which do not contain any crystalline explosive with regard to the mechanical and safety properties.
  • the powder precursor can be easily transported when moist with water and can be supplemented with the addition of another explosive component, for example nitroguanidine.
  • another explosive component for example nitroguanidine.
  • wax-containing crystalline explosives in particular wax-containing hexogen, can also be used.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Cosmetics (AREA)

Claims (11)

  1. Procédé pour la fabrication d'un produit précurseur pour poudre ou matière explosive, qui se compose essentiellement de nitrocellulose et d'au moins une matière explosive cristalline, en particulier de l'hexogène, procédé suivant lequel la matière explosive cristalline est amenée en phase aqueuse à la nitrocellulose, caractérisé en ce que la matière explosive cristalline est présente sous forme cristalline fine d'un diamètre moyen de particules d₅₀ = 2 à 8 µm, en ce que la matière explosive cristalline et la nitrocellulose sont séparées l'une de l'autre, chacune remuée en phase aqueuse, et en ce que la matière explosive cristalline et la nitrocellulose sont agitées et mélangées l'une à l'autre.
  2. Procédé selon la revendication 1,
    caractérisée en ce
    qu'une huile explosive, en particulier le dinitrate diglycole, peut être ajoutée et de préférence mélangée, après assemblage de la nitrocellulose et de la matière explosive.
  3. Produit précurseur, selon la revendication 1,
    caractérisé en ce
    qu'une huile explosive, en particulier du dinitrate diglycole, peut être amenée à la nitrocellulose et est ajoutée ensuite à la matière explosive cristalline.
  4. Procédé selon l'une des revendications 1 à 3,
    caractérisé en ce
    que la masse brute, contenant la matière explosive cristalline, est séparée du liquide, un procédé de centrifugation étant de préférence appliqué.
  5. Procédé selon l'une des revendications 1 à 4,
    caractérisé en ce
    qu'un mélange, qui se compose d'hexogène et d'une faible teneur en octogène, qui présente un diamètre moyen de particules d ₅₀ = 5 à 7 µm, est tout d'abord mélangé à une eau tensio-active diluée et est ensuite agité en une crème laiteuse par addition d'eau.
  6. Procédé selon l'une des revendications 1 à 5,
    caractérisé en ce
    que la matière explosive cristalline peut présenter un additif de cire.
  7. Procédé selon l'une des revendications 1 à 6,
    caractérisé en ce
    que la nitrocellulose présente une teneur en azote d'environ 12,6 % et est agitée dans l'eau sous faible turbulence.
  8. Procédé selon l'une des revendications 3 à 7,
    caractérisé en ce
    qu'une autre matière explosive, en particulier la nitroguanidine, est ajoutée au produit précurseur.
  9. Produit précurseur pour poudre ou explosif qui se compose essentiellement de nitrocellulose ou d'une autre matière explosive cristalline, en particulier l'hexogène, assemblée à la nitrocellulose en phase aqueuse,
    caractérisé en ce
    que la matière explosive cristalline se trouve sous forme cristalline fine, dont le diamètre de particule moyen est de d ₅₀ = 2 à 8 µm et en ce que la matière explosive cristalline et la nitrocellulose sont mélangées l'une à l'autre en phase aqueuse après agitation séparée.
  10. Produit précurseur selon la revendication 9,
    caractérisé en ce
    que la matière explosive cristalline, en particulier l'hexogène, présente une teneur en cire.
  11. Produit précurseur selon la revendication 9 ou 10,
    caractérisé en ce que
    le produit précurseur contient une huile explosive, en particulier, du dinitrate diglycole.
EP93922517A 1992-10-06 1993-10-05 Produit precurseur de poudre Expired - Lifetime EP0663896B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4233629A DE4233629C2 (de) 1992-10-06 1992-10-06 Verfahren zur Herstellung eines Pulver-Vorproduktes und Pulver-Vorprodukt
DE4233629 1992-10-06
PCT/EP1993/002722 WO1994007813A1 (fr) 1992-10-06 1993-10-05 Produit precurseur de poudre

Publications (2)

Publication Number Publication Date
EP0663896A1 EP0663896A1 (fr) 1995-07-26
EP0663896B1 true EP0663896B1 (fr) 1996-03-20

Family

ID=6469787

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93922517A Expired - Lifetime EP0663896B1 (fr) 1992-10-06 1993-10-05 Produit precurseur de poudre

Country Status (7)

Country Link
EP (1) EP0663896B1 (fr)
AT (1) ATE135674T1 (fr)
AU (1) AU5149293A (fr)
DE (1) DE4233629C2 (fr)
ES (1) ES2086966T3 (fr)
GR (1) GR3020086T3 (fr)
WO (1) WO1994007813A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100441550C (zh) * 1996-07-22 2008-12-10 大赛璐化学工业株式会社 用于气囊的产气剂
GB9913262D0 (en) * 1999-06-09 2002-08-21 Royal Ordnance Plc Desensitation of energetic materials

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1025694A (en) * 1962-02-19 1966-04-14 North American Aviation Inc Polymer coating of solid particles
US3235420A (en) * 1962-05-04 1966-02-15 Du Pont Process of making homogeneous particles comprising nitrocellulose mixtures
US3329743A (en) * 1963-05-15 1967-07-04 Olin Mathieson Lacquer process for preparing small diameter nitrocellulose particles
US3702272A (en) * 1964-01-10 1972-11-07 Olin Mathieson Spherical rocket propellant casting granules and method of preparation
US3311513A (en) * 1965-03-05 1967-03-28 Du Pont Nitramine, nitrocellulose explosive with ester plasticizer
DE2316538C3 (de) * 1973-04-03 1982-05-06 Dynamit Nobel Ag, 5210 Troisdorf Verfahren zur Herstellung von Gudol- Pulver
DE2461646C2 (de) * 1974-12-27 1984-01-05 Dynamit Nobel Ag, 5210 Troisdorf Verfahren zur Herstellung von Treibladungspulvern
US4014720A (en) * 1975-10-28 1977-03-29 The United States Of America As Represented By The Secretary Of The Army Flexible explosive composition comprising particulate RDX, HMX, or PETN and a high viscosity introcellulose binder plasticized with TEGDN
NO144666C (no) * 1980-02-29 1981-10-14 Dyno Industrier As Fremgangsmaate for fremstilling av aluminiumholdige hoeyenergisprengstoffblandinger
CH643804A5 (en) * 1980-07-24 1984-06-29 Oerlikon Buehrle Ag Explosive and process for its manufacture
DE3532525A1 (de) * 1985-09-12 1987-03-19 Fraunhofer Ges Forschung Dreibasiges treibladungspulver und verfahren zu seiner herstellung

Also Published As

Publication number Publication date
ES2086966T3 (es) 1996-07-01
DE4233629A1 (de) 1994-04-07
AU5149293A (en) 1994-04-26
EP0663896A1 (fr) 1995-07-26
GR3020086T3 (en) 1996-08-31
WO1994007813A1 (fr) 1994-04-14
DE4233629C2 (de) 1994-09-15
ATE135674T1 (de) 1996-04-15

Similar Documents

Publication Publication Date Title
DE4209878C2 (de) Gaserzeugendes Korn mit einer Beschichtung auf Wasserbasis sowie Verfahren zu dessen Herstellung
DE2820704C2 (de) Verfahren zum Herstellen einer mit Wachs desensibilisierten Sprengstoffmasse
DE60310985T2 (de) Pigmentzusammensetzungen mit metallischen aluminiumpartikeln
DE3934368C1 (fr)
DE2537529A1 (de) Gleitmittel fuer die pulvermetallurgie in form von mikrokapseln
DE2412523A1 (de) Pyrotechnische substanzen und verfahren zu ihrer herstellung
EP0509200A1 (fr) Procédé de fabrication d'explosifs désensibilisés
EP0663896B1 (fr) Produit precurseur de poudre
DE4417799A1 (de) Cermet-Sinterkörper
DE1696673B2 (de) Verfahren zum entfernen von montmorillonit aus kaolinitischen tonen
DE69315226T2 (de) Fibrillierbares ptfe in plastisch gebundenen sprengstoffen
DE3808366C2 (fr)
DE3605634C2 (fr)
DE1571179A1 (de) Verbesserung zum UEberziehen von pulverfoermigen Materialien
EP0590382A1 (fr) Procédé pour la production de granules contenant un dérivé de l'éphédrine
DE10027413B4 (de) Verfahren zum Herstellen einer Treibmittelzusammensetzung unter Anwendung eines Trockenmischverfahrens
CH643804A5 (en) Explosive and process for its manufacture
DE69918822T2 (de) Verfahren zur trocknung von melamin
DE3244444C1 (de) Zweibasige Propergolblöcke mit erhöhtem Nitramingehalt und Verfahren zu ihrer Herstellung
BE1029025B1 (de) DNT enthaltender detonierender Verbundexplosivstoff
DE4124734C2 (fr)
DE2751048B2 (de) Verstärkerkapsel mit Oktogenkristallen fur Geschosse und Verfahren zu ihrer Herstellung
DE3505278A1 (de) Verfahren zur herstellung einer suspension von feststoffen bei hoher konzentration
DE1571266B1 (de) Zündsatz
AT211207B (de) Verfahren zur Verringerung der Feuchtigkeitsempfindlichkeit von Sprengstoffen

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19950505

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DK ES FR GB GR IE IT LI LU NL PT SE

17Q First examination report despatched

Effective date: 19950814

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH DK ES FR GB GR IE IT LI LU NL PT SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 19960320

Ref country code: DK

Effective date: 19960320

Ref country code: BE

Effective date: 19960320

REF Corresponds to:

Ref document number: 135674

Country of ref document: AT

Date of ref document: 19960415

Kind code of ref document: T

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: SCHMAUDER & WANN PATENTANWALTSBUERO, INHABER KLAUS

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: 67715

ITF It: translation for a ep patent filed
ET Fr: translation filed
GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 19960430

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2086966

Country of ref document: ES

Kind code of ref document: T3

REG Reference to a national code

Ref country code: GR

Ref legal event code: FG4A

Free format text: 3020086

SC4A Pt: translation is available

Free format text: 960321 AVAILABILITY OF NATIONAL TRANSLATION

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Effective date: 19961005

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19961031

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19961107

REG Reference to a national code

Ref country code: IE

Ref legal event code: FD4D

Ref document number: 67715

Country of ref document: IE

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19990226

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: PT

Payment date: 19990305

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19990318

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19990322

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 19990325

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GR

Payment date: 19990331

Year of fee payment: 6

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19991005

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19991006

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: CH

Payment date: 19991021

Year of fee payment: 7

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: THE PATENT HAS BEEN ANNULLED BY A DECISION OF A NATIONAL AUTHORITY

Effective date: 19991030

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19991031

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000430

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 19991005

EUG Se: european patent has lapsed

Ref document number: 93922517.3

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000630

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

REG Reference to a national code

Ref country code: PT

Ref legal event code: MM4A

Free format text: LAPSE DUE TO NON-PAYMENT OF FEES

Effective date: 20000430

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20001031

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20001031

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20001113

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20051005