WO1997038142A1 - Desulphurising calcium carbide blend - Google Patents

Desulphurising calcium carbide blend Download PDF

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Publication number
WO1997038142A1
WO1997038142A1 PCT/FR1997/000592 FR9700592W WO9738142A1 WO 1997038142 A1 WO1997038142 A1 WO 1997038142A1 FR 9700592 W FR9700592 W FR 9700592W WO 9738142 A1 WO9738142 A1 WO 9738142A1
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Prior art keywords
particle size
calcium carbide
pulverulent
powder
magnesium
Prior art date
Application number
PCT/FR1997/000592
Other languages
French (fr)
Inventor
Gilles Nussbaum
Original Assignee
Pechiney Electrometallurgie
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 Pechiney Electrometallurgie filed Critical Pechiney Electrometallurgie
Priority to CZ19983147A priority Critical patent/CZ293175B6/en
Priority to HU9902168A priority patent/HU222767B1/en
Priority to DE69700665T priority patent/DE69700665T2/en
Priority to RO98-01446A priority patent/RO117712B1/en
Priority to UA98115805A priority patent/UA49014C2/en
Priority to PL97329220A priority patent/PL183768B1/en
Priority to AU23928/97A priority patent/AU2392897A/en
Priority to SK1379-98A priority patent/SK283419B6/en
Priority to EP97919467A priority patent/EP0891431B1/en
Publication of WO1997038142A1 publication Critical patent/WO1997038142A1/en
Priority to BG102700A priority patent/BG63215B1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C1/00—Refining of pig-iron; Cast iron
    • C21C1/02—Dephosphorising or desulfurising
    • C21C1/025—Agents used for dephosphorising or desulfurising

Definitions

  • the invention relates to a desulfurizing mixture based on calcium carbide intended to be injected using a lance into the liquid cast iron obtained at the blast furnace before passing it to the converter.
  • the Applicant has found that a desulfurizing mixture based on micronized powder of calcium carbide and containing both magnesium powder and aluminum powder, the latter in a well defined concentration range, allows a significant reduction iron losses during desulfurization.
  • the subject of the invention is therefore a desulfurizing mixture of refining pig iron consisting of at least 50% (by weight) of powdered calcium carbide with a particle size ⁇ 0.2 mm, from 1 to 20% of powdered magnesium with a particle size ⁇ 0.8 mm and from 5 to 15% of aluminum powder with a particle size ⁇ 0.8 mm, with optionally other powder additives such as lime, calcium carbonate, carbonaceous products and / or coating agents in a total amount of at most 30%.
  • the mixture according to the invention is based on technical calcium carbide, which generally contains around 80% by weight of C 2 Ca, the rest being lime, ground to a particle size less than 0.2 mm, with less than 25% of particles in the particle size range 0.1 - 0.2 mm
  • This carbide can be added with lime in addition to that resulting from the manufacture of technical carbide, calcium carbonate, carbon products such as carbon black , graphite or anthracite, or other products intended to improve the flowability of the mixture or to release gases allowing a good distribution of the desulfurizer in the hot melt. It is also possible to add up to 2% of a binder for coating the grains, for example hydrogenated castor oil as described in patent EP 0511121 of the applicant.
  • the magnesium is added to the mixture in the form of a powder or granules of pure metal or of a magnesium-based alloy with a particle size ⁇ 0.8 mm.
  • the grains can also be coated, like those of calcium carbide, with an organic product, for example based on saturated aliphatic acids or their esters as described in patent EP 0485309 of the applicant.
  • the mixing of the powders or granules is advantageously carried out in a mixer operating under neutral gas, for example nitrogen.
  • the mixtures according to the invention have a desulfurization efficiency at least equal to that of mixtures where aluminum is replaced in equal quantity by magnesium and therefore do not cause any overconsumption of product, which is quite unexpected since aluminum, unlike magnesium, is not by itself a desulfurizer.
  • a slag is formed which is more fluid, easier to clean and whose cleaning leads to much lower iron losses.
  • dross does not contain any products harmful to the environment such as sodium oxide.
  • the tests were carried out on pockets of 300 t of cast iron.
  • the initial sulfur content was close to 250 ppm, while the final content was around 55 ppm.
  • the effectiveness of a desulfurizer is defined by the ratio of the number of moles removed from the cast iron to the number of moles of desulfurizer injected, that is to say, in the present case, moles of C 2 Ca and Mg, raluminium not being in itself a desulfurizing product.
  • the iron loss is defined by the ratio of the mass of pig iron contained in dross to the mass of pig iron contained in the desulfurization pocket. The following results were obtained for the 3 mixtures, which are the average of 20 tests carried out under conditions as close as possible.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)

Abstract

A desulphurising blend for basic pig iron comprises at least 50 wt. % of pulverulent calcium carbide with a particle size of < 0.2 mm, 1-20 wt. % of pulverulent or granular magnesium with a particle size of < 0.8 mm and 5-15 wt. % of pulverulent or granular aluminium with a particle size of < 0.8 mm, and optionally other pulverulent additives such as lime, calcium carbonate, carbon products and/or grain coating agents, wherein the total amount of additives is 30 % or less, said blend reducing iron loss during desulphurisation.

Description

Mélange désulfurant à base de carbure de calcium Desulfurizing mixture based on calcium carbide
Domaine de l'inventionField of the invention
L'invention concerne un mélange désulfurant à base de carbure de calcium destiné à être injecté à l'aide d'une lance dans la fonte liquide obtenue au haut -fourneau avant son passage au convertisseur.The invention relates to a desulfurizing mixture based on calcium carbide intended to be injected using a lance into the liquid cast iron obtained at the blast furnace before passing it to the converter.
Etat de la techniqueState of the art
Bien que la fonte et le laitier soient coulés séparément du haut-fourneau, il subsiste une quantité appréciable de laitier dans la poche, de l'ordre de 5 kg/t. Par ailleurs, l'utilisation d'un produit désulfurant crée des crasses riches en soufre qu'il faut séparer du métal partant pour le convertisseur. A ce stade, le décrassage est fait mécaniquement, ce qui occasionne des pertes métal par entraînement. H est connu que l'obtention d'un laitier de désulfuration fluide permet de diminuer de manière significative les pertes métal lors du décrassage des poches. Pour ce faire, on ajoute dans la poche de métal, avant décrassage, du carbonate de sodium, qui se décompose en oxyde de sodium dont le point de fusion est 1132°C. Les crasses obtenues contiennent alors du sodium nuisible à l'environnement, d'où la recherche d'autres solutions pour réduire les pertes métal.Although the pig iron and the slag are poured separately from the blast furnace, there remains an appreciable quantity of slag in the ladle, of the order of 5 kg / t. In addition, the use of a desulfurizing product creates sulfur-rich dross which must be separated from the leaving metal for the converter. At this stage, the scouring is done mechanically, which causes metal losses by entrainment. It is known that obtaining a fluid desulphurization slag makes it possible to significantly reduce the metal losses during the cleaning of the pockets. To do this, sodium carbonate, which decomposes into sodium oxide, the melting point of which is 1132 ° C., is added to the metal ladle before descaling. The dross obtained then contains sodium harmful to the environment, hence the search for other solutions to reduce metal losses.
Par ailleurs, l'addition aux désulfurants de métaux réducteurs, tels que l'aluminium ou le magnésium, pour accélérer la désulfuration grâce à l'élimination de l'oxygène dissous dans la fonte, est également connue depuis longtemps, par exemple par le brevet FR 1168646 déposé par l'IRSID en 1957. Le brevet FR 2317361 de KLOCKNER-WERKE décrit un désulfurant à base de poudre de carbure de calcium, de cyanamide calcique ou de chaux auquel on ajoute de 0,5 à 3,5% de poudre d'aluminium ou de magnésium de même granulométrie. On connaît également, par le brevet EP 0398674 d'ELKEM METALS, l'addition au carbure de calcium d'aluminate de calcium à bas point de fusion pour obtenir une désailfuration plus complète des bains à quantité de mélange injectée constante. Objet de l'inventionFurthermore, the addition to desulfurizers of reducing metals, such as aluminum or magnesium, to accelerate desulfurization by eliminating the oxygen dissolved in the cast iron, has also been known for a long time, for example by patent FR 1168646 filed by IRSID in 1957. Patent FR 2317361 by KLOCKNER-WERKE describes a desulfurizer based on calcium carbide, calcium cyanamide or lime powder to which 0.5 to 3.5% of powder is added. of aluminum or magnesium of the same particle size. Also known, from patent EP 0398674 by ELKEM METALS, the addition to calcium carbide of calcium aluminate with low melting point in order to obtain a more complete desailfuration of the baths with constant quantity of mixture injected. Subject of the invention
La demanderesse a trouvé qu'un mélange désulfurant à base de poudre micronisée de carbure de calcium et contenant à la fois de la poudre de magnésium et de la poudre d'aluminium, cette dernière dans un intervalle de concentration bien délimité, permettait une réduction significative des pertes en fer au cours de la désulfuration. L'invention a ainsi pour objet un mélange désulfurant de la fonte d'affinage constitué d'au moins 50% (en poids) de carbure de calcium en poudre de granulométrie < 0,2 mm, de 1 à 20% de magnésium en poudre de granulométrie < 0,8 mm et de 5 à 15% d'aluminium en poudre de granulométrie < 0,8 mm, avec éventuellement d'autres additifs en poudre tels que la chaux, le carbonate de calcium, des produits carbonés et/ou des agents d'enrobage en quantité totale d'au plus 30%.The Applicant has found that a desulfurizing mixture based on micronized powder of calcium carbide and containing both magnesium powder and aluminum powder, the latter in a well defined concentration range, allows a significant reduction iron losses during desulfurization. The subject of the invention is therefore a desulfurizing mixture of refining pig iron consisting of at least 50% (by weight) of powdered calcium carbide with a particle size <0.2 mm, from 1 to 20% of powdered magnesium with a particle size <0.8 mm and from 5 to 15% of aluminum powder with a particle size <0.8 mm, with optionally other powder additives such as lime, calcium carbonate, carbonaceous products and / or coating agents in a total amount of at most 30%.
Description de l'inventionDescription of the invention
Le mélange selon l'invention est à base de carbure de calcium technique, qui contient généralement autour de 80% en poids de C2Ca, le reste étant de la chaux, broyé à une granulométrie inférieure à 0,2 mm, avec moins de 25% des particules dans le domaine de granulométrie 0,1 - 0,2 mm Ce carbure peut être additionné de chaux en supplément à celle qui résulte de la fabrication du carbure technique, de carbonate de calcium, de produits carbonés comme le noir de carbone , le graphite ou l'anthracite, ou d'autres produits destinés à améliorer la coulabilité du mélange ou à dégager des gaz permettant une bonne répartition du désulfurant dans la fonte hquide. On peut également ajouter jusqu'à 2% d'un liant d'enrobage des grains, par exemple de l'huile de ricin hydrogénée comme décrit dans le brevet EP 0511121 de la demanderesse.The mixture according to the invention is based on technical calcium carbide, which generally contains around 80% by weight of C 2 Ca, the rest being lime, ground to a particle size less than 0.2 mm, with less than 25% of particles in the particle size range 0.1 - 0.2 mm This carbide can be added with lime in addition to that resulting from the manufacture of technical carbide, calcium carbonate, carbon products such as carbon black , graphite or anthracite, or other products intended to improve the flowability of the mixture or to release gases allowing a good distribution of the desulfurizer in the hot melt. It is also possible to add up to 2% of a binder for coating the grains, for example hydrogenated castor oil as described in patent EP 0511121 of the applicant.
Le magnésium est apporté au mélange sous forme de poudre ou de granules de métal pur ou d'alliage à base magnésium de granulométrie < 0,8 mm. Les grains peuvent également être enrobés, comme ceux de carbure de calcium, d'un produit organique, par exemple à base d'acides aliphatiques saturés ou de leurs esters comme décrit au brevet EP 0485309 de la demanderesse.The magnesium is added to the mixture in the form of a powder or granules of pure metal or of a magnesium-based alloy with a particle size <0.8 mm. The grains can also be coated, like those of calcium carbide, with an organic product, for example based on saturated aliphatic acids or their esters as described in patent EP 0485309 of the applicant.
On ajoute enfin au mélange de 5 à 15% de poudre ou granules d'aluminium ou d'alliage à base aluminium pouvant également être enrobés d'un produit identique à celui utilisé pour le magnésium. _ „„„„, ., PCT7FR97/00592 O 97/38142Finally, 5 to 15% of powder or granules of aluminum or aluminum-based alloy is added to the mixture, which can also be coated with a product identical to that used for magnesium. _ „„ „„,., PCT7FR97 / 00592 O 97/38142
33
Le mélange des poudres ou granules se fait avantageusement dans un mélangeur fonctionnant sous gaz neutre, par exemple de l'azote.The mixing of the powders or granules is advantageously carried out in a mixer operating under neutral gas, for example nitrogen.
Les mélanges selon l'invention ont une efficacité de désulfuration au moins égale à celle des mélanges où l'aluminium est remplacé en quantité égale par du magnésium et n'entraînent donc aucune surconsommation de produit, ce qui est assez inattendu puisque l'aluminium, contrairement au magnésium, n'est pas par lui-même un désulfurant. D'autre part, on forme un laitier plus fluide, plus facile à décrasser et dont le décrassage conduit à des pertes en fer très inférieures. Enfin, les crasses ne contiennent aucun produit nocif pour l'environnement tel que l'oxyde de sodium.The mixtures according to the invention have a desulfurization efficiency at least equal to that of mixtures where aluminum is replaced in equal quantity by magnesium and therefore do not cause any overconsumption of product, which is quite unexpected since aluminum, unlike magnesium, is not by itself a desulfurizer. On the other hand, a slag is formed which is more fluid, easier to clean and whose cleaning leads to much lower iron losses. Finally, dross does not contain any products harmful to the environment such as sodium oxide.
ExempleExample
On a comparé l'efficacité de désulfuration et les pertes en fer de 2 mélanges désulfurants de l'art antérieur à base de carbure de calcium technique, le premier contenant 20% (en poids) de granules de magnésium, le second 20% de poudre d'aluminate de chaux, à un troisième mélange, conforme à l'invention, contenant 10% de granules de magnésium et 10% de granules d'aluminium.We compared the desulfurization efficiency and the iron losses of 2 desulfurizing mixtures of the prior art based on technical calcium carbide, the first containing 20% (by weight) of magnesium granules, the second 20% of powder. of lime aluminate, to a third mixture, in accordance with the invention, containing 10% of magnesium granules and 10% of aluminum granules.
Les essais ont été réalisés sur des poches de 300 t de fonte. La teneur initiale en soufre était voisine de 250 ppm, alors que la teneur finale était d'environ 55 ppm. L'efficacité d'un désulfurant est définie par le rapport du nombre de moles éliminées de la fonte au nombre de moles de désulfurant injecté, c'est à dire, dans le cas présent, des moles de C2Ca et de Mg, raluminium n'étant pas en soi un produit désulfurant. La perte en fer est définie par le rapport de la masse de fonte contenue dans les crasses à la masse de fonte contenue dans la poche de désulfuration. On a obtenu, pour les 3 mélanges, les résultats suivants, qui sont la moyenne de 20 essais réalisés dans des conditions aussi voisines que possible.The tests were carried out on pockets of 300 t of cast iron. The initial sulfur content was close to 250 ppm, while the final content was around 55 ppm. The effectiveness of a desulfurizer is defined by the ratio of the number of moles removed from the cast iron to the number of moles of desulfurizer injected, that is to say, in the present case, moles of C 2 Ca and Mg, raluminium not being in itself a desulfurizing product. The iron loss is defined by the ratio of the mass of pig iron contained in dross to the mass of pig iron contained in the desulfurization pocket. The following results were obtained for the 3 mixtures, which are the average of 20 tests carried out under conditions as close as possible.
Figure imgf000005_0001
En comparant les mélanges 1 et 3, on constate que leur efficacité en désulfuration est très voisine, mais que l'utilisation du mélange 3 conduit à diviser la perte en fer d'un facteur 3,7.
Figure imgf000005_0001
By comparing mixtures 1 and 3, it can be seen that their desulphurization efficiency is very similar, but that the use of mixture 3 leads to dividing the iron loss by a factor of 3.7.
En comparant les mélanges 2 et 3, on constate d'une manière surprenante que l'aluminium conduit à une désulfuration nettement plus efficace et une division de la perte fer par 3, alors qu'on aurait pu s'attendre à des résultats semblables, puisque l'aluminate introduit de l'alumine dans le laitier et que l'aluminium s'oxyde dans la fonte pour former de l'alumine qui se dissout dans le laitier. By comparing mixtures 2 and 3, it is surprisingly found that aluminum leads to a much more effective desulfurization and a division of the iron loss by 3, whereas one would have expected similar results, since the aluminate introduces alumina into the slag and the aluminum oxidizes in the pig iron to form alumina which dissolves in the slag.

Claims

REVENDICATIONS
1. Mélange désulfurant pour injection dans la fonte d'affinage liquide, constitué d'au moins 50% (en poids) de carbure de calcium en poudre de granulométrie < 0,2 mm, de 1 à 20% de magnésium en poudre ou granules de granulométrie < 0,8 mm et de 5 à 15% d'aluminium en poudre ou granules de gτanulométrie < 0,8 mm, avec éventuellement d'autres additifs en poudre tels que la chaux, le carbonate de calcium, des produits carbonés et/ou des agents d'enrobage des grains, la quantité totale d'additifs étant d'au plus 30%.1. Desulfurizing mixture for injection into liquid refining pig iron, consisting of at least 50% (by weight) of calcium carbide in powder with a particle size <0.2 mm, from 1 to 20% of magnesium in powder or granules with a grain size <0.8 mm and from 5 to 15% of aluminum powder or granules with a grain size <0.8 mm, with possibly other powdered additives such as lime, calcium carbonate, carbon products and / or grain coating agents, the total amount of additives being at most 30%.
2. Mélange selon la revendication 1 dans lequel moins de 25% des grains de carbure de calcium ont une granulométrie comprise entre 0, 1 et 0,2 mm. 2. Mixture according to claim 1 in which less than 25% of the calcium carbide grains have a particle size of between 0.1 and 0.2 mm.
PCT/FR1997/000592 1996-04-04 1997-04-02 Desulphurising calcium carbide blend WO1997038142A1 (en)

Priority Applications (10)

Application Number Priority Date Filing Date Title
CZ19983147A CZ293175B6 (en) 1996-04-04 1997-04-02 Desulfurizing calcium carbide blend
HU9902168A HU222767B1 (en) 1996-04-04 1997-04-02 Desulphurising calcium carbide blend
DE69700665T DE69700665T2 (en) 1996-04-04 1997-04-02 DESulphurizing calcium-carbide mixture
RO98-01446A RO117712B1 (en) 1996-04-04 1997-04-02 Desulphurizing blend based on calcium carbide
UA98115805A UA49014C2 (en) 1996-04-04 1997-04-02 desulfurizing blend on calcium carbide base
PL97329220A PL183768B1 (en) 1996-04-04 1997-04-02 Desulphurising calcium carbide mixture
AU23928/97A AU2392897A (en) 1996-04-04 1997-04-02 Desulphurising calcium carbide blend
SK1379-98A SK283419B6 (en) 1996-04-04 1997-04-02 Desulphurising calcium carbide blend
EP97919467A EP0891431B1 (en) 1996-04-04 1997-04-02 Desulphurising calcium carbide blend
BG102700A BG63215B1 (en) 1996-04-04 1998-08-19 Desulphurization mixture based on calcium carbide

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR96/04493 1996-04-04
FR9604493A FR2747132B1 (en) 1996-04-04 1996-04-04 CALCIUM CARBIDE DESULFURING MIXTURE

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WO1997038142A1 true WO1997038142A1 (en) 1997-10-16

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EP (1) EP0891431B1 (en)
AU (1) AU2392897A (en)
BG (1) BG63215B1 (en)
CZ (1) CZ293175B6 (en)
DE (1) DE69700665T2 (en)
ES (1) ES2140232T3 (en)
FR (1) FR2747132B1 (en)
HU (1) HU222767B1 (en)
PL (1) PL183768B1 (en)
RO (1) RO117712B1 (en)
RU (1) RU2166548C2 (en)
SK (1) SK283419B6 (en)
UA (1) UA49014C2 (en)
WO (1) WO1997038142A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016004493A1 (en) * 2014-07-11 2016-01-14 Tecnosulfur Sistema De Tratamiento De Metais Liquidos S/A. Desulphurising composition and method for producing the same, packaging method and method of use in small pots for the production of iron melts

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19857733A1 (en) * 1998-12-15 2000-06-21 Almamet Gmbh Desulfurizing agent
FR2789697B1 (en) * 1999-02-12 2001-04-06 Pechiney Electrometallurgie DESULFURIZING MIXTURE BASED ON CALCIUM CARBIDE AND / OR LIME
CN101367025B (en) * 2008-08-13 2011-07-27 陈宏� Calcium based composite catalysis dry desulfurizing agent for circulating fluidized bed boiler and preparation method thereof
CN107245549B (en) * 2017-06-15 2018-12-18 王强 A kind of the efficient of electrolytic aluminium factory aluminium ash utilizes technique

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE418074C (en) * 1922-03-12 1925-08-25 Wilhelm Kroll Dr Desulphurizer for iron and steel baths
DE2447918A1 (en) * 1974-10-08 1976-04-29 Gammal Tarek Prof Dr Ing El Refining of steel - by using an alloy of calcium, aluminium and magnesium free of oxide
FR2317361A1 (en) * 1975-07-11 1977-02-04 Kloeckner Werke Ag PROCESS FOR DESULFURING CRUDE IRON
DE2709062A1 (en) * 1977-03-02 1978-09-07 Sueddeutsche Kalkstickstoff MEANS AND METHODS FOR DESULFURIZING METAL IRON
JPS54136516A (en) * 1978-04-14 1979-10-23 Kobe Steel Ltd Hot iron desulfurizing agent

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE418074C (en) * 1922-03-12 1925-08-25 Wilhelm Kroll Dr Desulphurizer for iron and steel baths
DE2447918A1 (en) * 1974-10-08 1976-04-29 Gammal Tarek Prof Dr Ing El Refining of steel - by using an alloy of calcium, aluminium and magnesium free of oxide
FR2317361A1 (en) * 1975-07-11 1977-02-04 Kloeckner Werke Ag PROCESS FOR DESULFURING CRUDE IRON
DE2709062A1 (en) * 1977-03-02 1978-09-07 Sueddeutsche Kalkstickstoff MEANS AND METHODS FOR DESULFURIZING METAL IRON
JPS54136516A (en) * 1978-04-14 1979-10-23 Kobe Steel Ltd Hot iron desulfurizing agent

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 004, no. 002 (C - 069) 9 January 1980 (1980-01-09) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016004493A1 (en) * 2014-07-11 2016-01-14 Tecnosulfur Sistema De Tratamiento De Metais Liquidos S/A. Desulphurising composition and method for producing the same, packaging method and method of use in small pots for the production of iron melts

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HU222767B1 (en) 2003-10-28
EP0891431A1 (en) 1999-01-20
FR2747132A1 (en) 1997-10-10
SK283419B6 (en) 2003-07-01
HUP9902168A2 (en) 1999-11-29
HUP9902168A3 (en) 2001-11-28
BG102700A (en) 1999-03-31
BG63215B1 (en) 2001-06-29
CZ293175B6 (en) 2004-02-18
RU2166548C2 (en) 2001-05-10
EP0891431B1 (en) 1999-10-20
AU2392897A (en) 1997-10-29
DE69700665D1 (en) 1999-11-25
PL329220A1 (en) 1999-03-15
SK137998A3 (en) 1999-05-07
PL183768B1 (en) 2002-07-31
ES2140232T3 (en) 2000-02-16
RO117712B1 (en) 2002-06-28
DE69700665T2 (en) 2000-05-11
UA49014C2 (en) 2002-09-16
CZ314798A3 (en) 1999-08-11
FR2747132B1 (en) 1998-06-19

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