EP0509200B1 - Procédé de fabrication d'explosifs désensibilisés - Google Patents
Procédé de fabrication d'explosifs désensibilisés Download PDFInfo
- Publication number
- EP0509200B1 EP0509200B1 EP92102032A EP92102032A EP0509200B1 EP 0509200 B1 EP0509200 B1 EP 0509200B1 EP 92102032 A EP92102032 A EP 92102032A EP 92102032 A EP92102032 A EP 92102032A EP 0509200 B1 EP0509200 B1 EP 0509200B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- process according
- polymer
- roller
- explosive
- aqueous dispersion
- 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
Links
- 239000002360 explosive Substances 0.000 title claims description 29
- 238000000034 method Methods 0.000 title claims description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 229920000642 polymer Polymers 0.000 claims description 21
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- 239000003380 propellant Substances 0.000 claims description 9
- 229940090898 Desensitizer Drugs 0.000 claims description 8
- 239000000028 HMX Substances 0.000 claims description 6
- UZGLIIJVICEWHF-UHFFFAOYSA-N octogen Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 UZGLIIJVICEWHF-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 4
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- AYAQUZXJSZXBNY-UHFFFAOYSA-N ethenyl propanoate prop-2-enoic acid Chemical compound C(C=C)(=O)O.C(CC)(=O)OC=C AYAQUZXJSZXBNY-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 5
- 238000000576 coating method Methods 0.000 claims 5
- 230000035945 sensitivity Effects 0.000 description 14
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 3
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000586 desensitisation Methods 0.000 description 2
- 238000005474 detonation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 2-ethylhexyl Chemical group 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000169624 Casearia sylvestris Species 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003975 dentin desensitizing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C06B23/005—Desensitisers, phlegmatisers
-
- 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
Definitions
- the invention relates to a method for producing phlegmatized, high-energy explosives, in particular hexogen (RDX) or octogen (HMX), as a component of plastic-bound explosives or propellant charge powder, in that the particulate explosive is coated with a desensitizing polymer from an aqueous phase.
- RDX hexogen
- HMX octogen
- Hexogen and octogen are characterized by a high energy or explosiveness for their use, which, however, causes considerable problems for processing.
- the high sensitivity to friction and impact leads to a correspondingly high security risk.
- This security risk is the higher, ever the grain size distribution is wider and the larger the coarse grain fraction is, since single grain detonations can then occur, for example, in propellant grains.
- Such single-grain detonations are also undesirable in use, especially when used in Lova-TLP.
- the coarse-grained fraction leads, for example, to intermittent burns in the case of TLP combustion interruptions, as a result of which the geometry of the propellant charge body changes in an uncontrolled manner and the combustion behavior and the ballistics are thus negatively influenced.
- any water moisture that may still be present is granulated in the same mixer.
- a wax is proposed as a desensitizer, which is dissolved in perchlorethylene.
- Graphite powder is also used added, which also has a desensitizing effect, in particular prevents electrostatic charges.
- a high-energy explosive produced in this way has a broad grain distribution with a high proportion of coarse grain, which not only shows the aforementioned disadvantages in processing, but is also responsible for certain technical defects.
- These explosives cannot be added to the otherwise very advantageous processing of propellant powders and explosive mixtures in extruders, in particular twin screw extruders, since the security risk is too great.
- the invention has for its object to propose a method of the type mentioned, which on the one hand does not require environmentally harmful solvents, and on the other hand leads to desensitized explosives with low sensitivity to friction.
- This object is achieved in that the particulate explosive with a particle size of up to 20 »m slurried with the polymer in aqueous dispersion, the sludges applied to a rotating, heated roller, the application dried at a temperature> 100 ° C without pressure and after Drying is scraped off the roller.
- the process according to the invention can be carried out continuously and does not require any special precautions for workplace protection or environmental protection, since work is carried out in the aqueous phase.
- a homogeneous dispersion can be achieved, which can be applied to the roller without any safety risk and which is dried without pressure by mere evaporation.
- the explosive particles are coated homogeneously with the polymer.
- the polymer used for desensitization preferably also forms the plastic binder for the finished explosive or propellant powder, the polymer being added in the amount or a part thereof required for the end product.
- polystyrene-1,3-butadiene-acrylonitrile, vinyl propionate acrylate the polymer preferably being used in a 50 to 55% strength aqueous dispersion.
- polyvinyl alcohol can also be used as the polymer, the aqueous dispersion additionally containing glycerol.
- a surface-active additive is preferably added to the aqueous dispersion.
- a surface-active additive for example, highly disperse, amorphous silicon dioxide can be used as the surface-active additive.
- the aforementioned additive prevents the formation of vapor bubbles, which in turn will cause the layer to crack open and possibly flake off. Furthermore, the flowability and the quality of the order is improved.
- Adequate desensitization is obtained when the explosive is slurried with 5 to 25% by weight of polymer in aqueous dispersion.
- the explosive is preferably used with a grain size of up to 10 .mu.m, and the grain size spectrum can also be in the range between 3 and 5 .mu.m.
- the slurry applied to the roller is preferably dried at a roller temperature between 110 ° C and 150 ° C, preferably ⁇ 140 ° C, which allows relatively short residence times to be achieved. These can be, for example, in the range of 60 s and a little more if a roller of at least 150 cm is used and the layer thickness is ⁇ 10 mm.
- An inventive desensitized RDX with a higher polymer content e.g. B. in the range of 15 to 25% can be used directly as basic granules when extruding LOVA propellant powder.
- a test series with hexogen (RDX) with a grain size of 10 »m and various polymers is shown in Table I in accordance with the annex, and the friction sensitivity and impact sensitivity determined in each case are listed.
- the desensitizers are shown in capital letters, which are explained in the footnote to the table.
- the example shows similarly good results in terms of sensitivity to friction with 75% by weight RDX and 25% by weight polymer A dispersed in water.
- the impact sensitivity in this case is 0.35 kgm.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Lubricants (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Claims (13)
- Procédé de fabrication d'explosifs hautement énergétiques, désensibilisés, tels que l'hexogène (RDX) ou l'octogène (HMX), en tant que composants d'explosifs obtenus par la combinaison de matières synthétiques ou de poudre pour charge propulsive, procédé dans lequel l'explosif, sous forme de particules, est recouvert en phase aqueuse d'un polymère désensibilisant, caractérisé en ce que l'explosif sous forme de particules, d'une granulométrie allant jusqu'à 20 »m, est mis en suspension avec le polymère dans une dispersion aqueuse, en ce que la suspension est appliquée sur un tambour chauffant en rotation et en ce que l'enduit est séché à une température supérieure à 100°C à la pression atmosphérique et raclé du tambour après séchage.
- Procédé selon la revendication 1, caractérisé en ce que le polymère est choisi dans le groupe du styrène-butadiène-1,3-acrylonitrile, vinylpropionate-acrylate.
- Procédé selon l'une quelconque des revendications 1 ou 2, caractérisé en ce que le polymère est utilisé dans une dispersion aqueuse de 50 à 55 %.
- Procédé selon la revendication 1, caractérisé en ce que le polymère utilisé est de l'alcool polyvinylique et en ce que la dispersion aqueuse contient en plus de la glycérine.
- Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que l'on ajoute à la dispersion aqueuse un additif tensioactif.
- Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que l'additif tensioactif utilisé est du dioxyde de silicium amorphe très dispersé.
- Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que le désensibilisant utilisé est un polymère servant également de liant synthétique pour l'explosif ou la poudre pour charge propulsive.
- Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que l'explosif est mis en suspension en dispersion aqueuse avec 5 à 25% en masse de polymère.
- Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce que l'on utilise des explosifs dont la granulométrie des particules peut aller jusqu'à 10 »m.
- Procédé selon l'une quelconque des revendications 1 à 9, caractérisé en ce que l'enduit sur le tambour est séché à une température comprise entre 110 et 150°C.
- Procédé selon l'une quelconque des revendications 1 à 10, caractérisé en ce que l'enduit sur le tambour est séché à une température comprise entre 110 et 140°C.
- Procédé selon l'une quelconque des revendications 1 à 11, caractérisé en ce que l'enduit est appliqué sur un tambour dont la périphérie est d'au moins 150 cm et en ce que la durée de contact de l'enduit avec le tambour est supérieure à 60 secondes.
- Procédé selon l'une quelconque des revendications 1 à 12, caractérisé en ce que l'enduit est appliqué sur le tambour en une couche d'épaisseur inférieure à 10 mm.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4111752 | 1991-04-11 | ||
DE4111752A DE4111752C1 (fr) | 1991-04-11 | 1991-04-11 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0509200A1 EP0509200A1 (fr) | 1992-10-21 |
EP0509200B1 true EP0509200B1 (fr) | 1995-07-05 |
Family
ID=6429315
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP92102032A Expired - Lifetime EP0509200B1 (fr) | 1991-04-11 | 1992-02-07 | Procédé de fabrication d'explosifs désensibilisés |
Country Status (3)
Country | Link |
---|---|
US (1) | US5547527A (fr) |
EP (1) | EP0509200B1 (fr) |
DE (2) | DE4111752C1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6893516B2 (en) | 2001-11-14 | 2005-05-17 | Diehl Munitionssysteme Gmbh & Co. Kg | Insensitive pressable explosive |
Families Citing this family (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4324739C1 (de) * | 1993-07-23 | 1994-09-08 | Deutsche Aerospace | Gegossene kunststoffgebundene Sprengladung |
FR2728562B1 (fr) * | 1994-12-22 | 1997-01-24 | Poudres & Explosifs Ste Nale | Procede de fabrication en continu de chargements pyrotechniques a liant silicone et compositions susceptibles d'etre mises en oeuvre par ce procede |
DE19605346C1 (de) * | 1996-02-14 | 1997-07-24 | Fraunhofer Ges Forschung | Phlegmatisierter Energieträger und Verfahren zur Rückgewinnung des in dem phlegmatisierten Energieträger enthaltenen Explosivstoffs |
WO1997042140A1 (fr) * | 1996-05-03 | 1997-11-13 | Eastman Chemical Company | Formulations d'explosifs |
AU3129197A (en) * | 1996-05-03 | 1997-11-26 | Eastman Chemical Company | Explosive formulations |
WO1997042138A1 (fr) * | 1996-05-03 | 1997-11-13 | Eastman Chemical Company | Compositions explosives |
US5808234A (en) * | 1996-05-06 | 1998-09-15 | Eastman Chemical Company | Explosive formulations |
CA2268768A1 (fr) * | 1996-10-15 | 1998-04-23 | Eastman Chemical Company | Formulations inflammables |
DE19907809C2 (de) * | 1999-02-24 | 2002-10-10 | Nitrochemie Gmbh | Verfahren zur Herstellung von ein-, zwei- oder dreibasigen Triebladungspulvern für Rohrwaffenmunition |
ZA200205775B (en) * | 2002-04-12 | 2003-03-28 | Diehl Munitionssysteme Gmbh | Insensitive hexogen explosive. |
FR2925488B1 (fr) * | 2007-12-19 | 2011-12-23 | Snpe Materiaux Energetiques | Desensibilisation par enrobage de cristaux de substances energetiques explosives ; cristaux de telles substances enrobes, materiaux energetiques. |
US8575074B2 (en) | 2011-06-06 | 2013-11-05 | Los Alamos National Security, Llc | Insensitive explosive composition and method of fracturing rock using an extrudable form of the composition |
CN103012299B (zh) * | 2012-12-27 | 2015-01-14 | 中国工程物理研究院化工材料研究所 | 基于dmso/h2o二元体系的hmx制备方法 |
US9850180B1 (en) * | 2015-02-12 | 2017-12-26 | The United States Of America As Represented By The Secretary Of The Army | Method for manufacture of amorphous energetics |
RU2734192C1 (ru) * | 2020-03-12 | 2020-10-13 | Акционерное общество "Взрывгеосервис" | Взрывчатый состав для изготовления зарядов кумулятивных перфораторов (варианты) |
Family Cites Families (25)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1036906A (en) * | 1912-08-27 | O Reuter | Granular explosive, especially suitable for the preparation of pressed pieces, and method of making the same. | |
DE257319C (fr) * | ||||
US1007276A (en) * | 1909-09-24 | 1911-10-31 | Du Pont Powder Co | Method of solidifying crystallizable mixtures without substantial crystallization. |
US2438281A (en) * | 1945-12-10 | 1948-03-23 | Us Sec War | Method for processing plastic sheets |
US3348986A (en) * | 1955-02-04 | 1967-10-24 | Charles W Sauer | Process of preparing plastic coated high explosive particles and articles |
US3296041A (en) * | 1964-07-08 | 1967-01-03 | Eastman Kodak Co | Granulated crystalline plastic bonded explosives |
US3266957A (en) * | 1964-09-24 | 1966-08-16 | Richard H Stresau | Booster explosive of ultrafine desensitized cyclotrimethylene-trinitramine and method of preparing same |
US3338764A (en) * | 1965-08-19 | 1967-08-29 | Du Pont | Flexible detonating compositions containing high explosives and polymeric metallocarboxylates |
US3428502A (en) * | 1966-10-25 | 1969-02-18 | Du Pont | Polyvinyl acetate binder for crystalline explosive |
US3586551A (en) * | 1968-08-27 | 1971-06-22 | Du Pont | Water-degradable cap-sensitive selfsupporting explosive |
US4163681A (en) * | 1970-04-15 | 1979-08-07 | The United States Of America As Represented By The Secretary Of The Navy | Desensitized explosives and castable thermally stable high energy explosive compositions therefrom |
FR2135534B1 (fr) * | 1971-05-06 | 1973-06-29 | Wasagchemie Ag | |
US4113811A (en) * | 1975-07-02 | 1978-09-12 | Dynamit Nobel Aktiengesellschaft | Process for the production of flexible explosive formed charges |
US4092187A (en) * | 1976-08-18 | 1978-05-30 | The United States Of America As Represented By The Secretary Of The Army | Process for coating crystalline high explosives |
NO144666C (no) * | 1980-02-29 | 1981-10-14 | Dyno Industrier As | Fremgangsmaate for fremstilling av aluminiumholdige hoeyenergisprengstoffblandinger |
DE3010052C2 (de) * | 1980-03-15 | 1982-09-09 | Friedrich-Ulf 8899 Rettenbach Deisenroth | Verfahren zur Herstellung von kunststoffgebundenen Explosivstoffen |
CA1195122A (fr) * | 1981-05-25 | 1985-10-15 | Paul Arni | Methode de preparation d'un explosif brisant; produit ainsi obtenu, et sa mise en forme |
DE3234978C1 (de) * | 1982-09-22 | 1984-01-26 | Messerschmitt-Bölkow-Blohm GmbH, 8000 München | Gegossene Sprengladung |
NO153804C (no) * | 1984-02-08 | 1986-05-28 | Dyno Indusrtrier A S Nitroglyc | Fremgangsmaate for belegning av krystallinske hoeyeksplosiver. |
DE3625412A1 (de) * | 1986-07-26 | 1988-02-04 | Messerschmitt Boelkow Blohm | Verfahren zur herstellung eines kunststoffgebundenen explosivstoffs |
DE3711995A1 (de) * | 1987-04-09 | 1988-10-20 | Messerschmitt Boelkow Blohm | Verfahren zum phlegmatisieren von spreng- und treibstoffen |
JPH07112537B2 (ja) * | 1987-11-27 | 1995-12-06 | ダイセル化学工業株式会社 | 発火または爆発性の高い物質の原料組成物の混合方法 |
US4882994A (en) * | 1988-01-28 | 1989-11-28 | Veltman Preston Leonard | Particulate fuel components for solid propellant systems |
DE3804396C1 (en) * | 1988-02-12 | 1989-05-18 | Messerschmitt-Boelkow-Blohm Gmbh, 8012 Ottobrunn, De | Process for producing plastic-bonded explosives |
DE3934368C1 (fr) * | 1989-10-14 | 1990-11-15 | Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung Ev, 8000 Muenchen, De |
-
1991
- 1991-04-11 DE DE4111752A patent/DE4111752C1/de not_active Expired - Fee Related
-
1992
- 1992-02-07 EP EP92102032A patent/EP0509200B1/fr not_active Expired - Lifetime
- 1992-02-07 DE DE59202779T patent/DE59202779D1/de not_active Expired - Fee Related
-
1993
- 1993-08-16 US US08/106,789 patent/US5547527A/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
CHEMICAL ABSTRACTS, vol. 070, no. 24, 16. Juni 1969, Columbus, Ohio, US;abstract no. 107929G, 'Solid self-supporting explosives' Seite 104; and CS-A-127 990 (J. Vacek et al.) 15.06 1968 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6893516B2 (en) | 2001-11-14 | 2005-05-17 | Diehl Munitionssysteme Gmbh & Co. Kg | Insensitive pressable explosive |
Also Published As
Publication number | Publication date |
---|---|
DE59202779D1 (de) | 1995-08-10 |
US5547527A (en) | 1996-08-20 |
DE4111752C1 (fr) | 1992-09-17 |
EP0509200A1 (fr) | 1992-10-21 |
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