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US20010018400A1 - Completely metallic oxidation catalyst - Google Patents

Completely metallic oxidation catalyst Download PDF

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Publication number
US20010018400A1
US20010018400A1 US09/230,466 US23046699A US2001018400A1 US 20010018400 A1 US20010018400 A1 US 20010018400A1 US 23046699 A US23046699 A US 23046699A US 2001018400 A1 US2001018400 A1 US 2001018400A1
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alloy
aqueous solution
thermal treatment
emulsion
treatment
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US6274532B1 (en
Inventor
Wilfried Herda
Ulrich Heubner
Jurgen Koppe
Hartmus Lausch
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8898—Manganese, technetium or rhenium containing also molybdenum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/12—Oxidising
    • B01J37/14—Oxidising with gases containing free oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/864—Removing carbon monoxide or hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/944—Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8892—Manganese
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Definitions

  • the invention relates to a completely-metallic catalyst for the oxidation of mixtures containing carbon monoxide and/or hydrocarbons and/or soot in the gaseous phase, as defined in the preamble to claim 1 .
  • DE 44 16 469 C1 discloses a completely-metallic oxidation catalyst that contains nickel, manganese, chromium and iron and is used in the total oxidation of hydrocarbons into carbon dioxide and water.
  • This catalyst is produced from an alloy, which contains (in mass percent) 10 to 50% nickel, up to 50% copper, up to 10% manganese, 10 to 30% chromium and up to 50% iron, through thermal treatment in an oxygen-containing atmosphere for a period of 0.25 to 10 hours at temperatures of 400 to 1000° C. A reduction with a hydrocarbon-containing mixture can follow this oxidizing thermal treatment.
  • a disadvantage of this and other known oxidation catalysts is that they do not oxidize the organic components in gas flows below 400° C., and soot particles in particular are not oxidized in the temperature range below 500° C.
  • soot particles in the presence of soot particles, the danger exists that the catalyst surface will be covered by soot particles at relatively-low working temperatures below 500° C. such that they no longer have a catalytic effect. This is inevitably the case when an exhaust-gas catalyst is not used in the optimum working and temperature range, for example during the startup phase of motor-vehicle diesel catalysts.
  • the catalyst it is preferable for the catalyst to already have a catalytic effect in the relatively “cold” phase, i.e., at temperatures of up to 300° C.
  • the catalyst can be used in wire or chip form, or any other form having a sufficiently-large specific surface.
  • the catalyst of the invention makes use of a layer that adheres well and has a high degree of catalytic effectiveness, and has a high catalytic activity and a high thermal conductivity.
  • sugar, starch, latex, polyacrylate and/or polyvinyl alcohol and another modification with at least one of the following elements: boron, aluminum, indium, germanium, tin, lead, scandium, yttrium, lanthanum, titanium, zirconium, vanadium, niobium, chromium, molybdenum, tungsten, manganese, technetium, rhenium, iron, cobalt, nickel, copper, cerium, praseodymium and neodymium in the above-described manner.
  • Example 2 An alloy comprising 71.8% Mn, 350 100 benzene 17.55% Cu, 10.4% Ni, 0.1% Fe, 0.04% Si, 0.009% S and 0.017% C was annealed for 1.5 hrs at 650° C. in an air-containing environment.
  • Example 3 An alloy comprising 71.8% Mn, 300 92 n-hexane 17.55% Cu, 10.4% Ni, 0.1% Fe, 0.04% Si, 0.009% S and 0.017% C was annealed for 1.5 hrs at 650° C. in an air-containing environment.
  • Example 4 An alloy comprising 53.72% Fe, 350 100 toluene 24.2% Cr, 17.7% Ni, 6.14% Mn, 4.34% Mo, 0.53% Cu, 0.17% Nb, 0.12% Al, 0.46% N, 0.004% S, 0.012% C and 0.017% P was annealed for 2 hrs at 900° C. with air.
  • Example 5 An alloy comprising 50.85% Co, 325 100 n-hexane 19.95% Cr, 14.8% W, 2.28% Fe, 1.53% Mn, 0.096% C, 0.004% S and 0.006% p was annealed for 0.45 hr at 1000° C. with air.
  • Example 6 An alloy comprising 68.01% Cu, 385 94 n-hexane 30.6% Ni, 0.70% Fe, 0.67% Mn, 0.008% C, 0.010% Zn, 0.004% S and 0.002% P was annealed for 1.2 hrs at 875° C. with air.
  • Example 7 An alloy comprising 37.3% Ni, 315 96 n-hexane 35.73% Fe, 19.45% Cr, 3.2% Cu, 2.33% Mo, 1.51% Mn, 0.2% Nb, 0.26% Si, 0.015% P, 0.006% C and 0.003% S was annealed for 2 hrs at 910° C. with air.
  • Example 8 An alloy comprising 61.05% Ni, 375 85 n-hexane 22.5% Cr, 15.3% Mo, 0.68% Fe, 0.26% Al, 0.14% Mn, 0.03% Co, 0.006% C, 0.004% P and 0.002% S was annealed for 1 hr at 880° C. with air.
  • Example 9 An alloy comprising 45.64% Fe, 370 80 n-hexane 24.7% Ni, 20.9% Cr, 6.43% Mo, 0.90% Cu, 0.89% Mn, 0.192% N, 0.017% P, 0.006% C and 0.003% S was annealed for 0.5 hr at 1010° C. with air.
  • Example 10 An alloy comprising 32.08% Fe, 385 95 n-hexane 31.3% Ni, 26.85% Cr, 1.54% Mn, 1.34% Cu, 0.202% N, 0.015% P, 0.01% C and 0.003% S was annealed for 2 hrs at 825° C. with air.
  • the alloy was placed in 10 ml of a solution containing 1.5% polyvinyl alcohol, 60 g/l Cu 2+ ions and 10 g/l Ni 2+ ions for 2 min., removed and annealed again for 0.5 hr in air.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Combustion & Propulsion (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

A completely metallic catalyst for the oxidation of mixtures in the gaseous phase which contain carbon monoxide, hydrocarbons and/or soot, has a surface doped with a metallic element and is subjected to a second thermal treatment in an oxygen-containing atmosphere.

Description

  • The invention relates to a completely-metallic catalyst for the oxidation of mixtures containing carbon monoxide and/or hydrocarbons and/or soot in the gaseous phase, as defined in the preamble to claim [0001] 1.
  • DE 44 16 469 C1 discloses a completely-metallic oxidation catalyst that contains nickel, manganese, chromium and iron and is used in the total oxidation of hydrocarbons into carbon dioxide and water. This catalyst is produced from an alloy, which contains (in mass percent) 10 to 50% nickel, up to 50% copper, up to 10% manganese, 10 to 30% chromium and up to 50% iron, through thermal treatment in an oxygen-containing atmosphere for a period of 0.25 to 10 hours at temperatures of 400 to 1000° C. A reduction with a hydrocarbon-containing mixture can follow this oxidizing thermal treatment. [0002]
  • A disadvantage of this and other known oxidation catalysts is that they do not oxidize the organic components in gas flows below 400° C., and soot particles in particular are not oxidized in the temperature range below 500° C. [0003]
  • Thus, in the presence of soot particles, the danger exists that the catalyst surface will be covered by soot particles at relatively-low working temperatures below 500° C. such that they no longer have a catalytic effect. This is inevitably the case when an exhaust-gas catalyst is not used in the optimum working and temperature range, for example during the startup phase of motor-vehicle diesel catalysts. For these and numerous other applications, it is preferable for the catalyst to already have a catalytic effect in the relatively “cold” phase, i.e., at temperatures of up to 300° C. [0004]
  • It is the object of the invention to provide an effective catalyst for the total oxidation of gas mixtures containing hydrocarbons and/or soot, the catalyst being simple to produce and easy to dispose of, already having a catalytic effect in a low temperature range, being regenerable with little effort, and simultaneously possessing a high thermal conductivity. [0005]
  • This object is accomplished by the features in the characterizing portion of claim [0006] 1.
  • Advantageous embodiments of the invention are characterized in the dependent claims. [0007]
  • The catalyst can be used in wire or chip form, or any other form having a sufficiently-large specific surface. [0008]
  • The catalyst of the invention makes use of a layer that adheres well and has a high degree of catalytic effectiveness, and has a high catalytic activity and a high thermal conductivity. [0009]
  • In the catalysts of the invention, a possible drop in the catalytic activity—possibly following a mechanical, chemical or physical-chemical cleaning of the surface—can be eliminated through a repeated thermal treatment followed by another treatment with an aqueous solution containing oxidizable, organic substances, e.g. sugar, starch, latex, polyacrylate and/or polyvinyl alcohol, and another modification with at least one of the following elements: boron, aluminum, indium, germanium, tin, lead, scandium, yttrium, lanthanum, titanium, zirconium, vanadium, niobium, chromium, molybdenum, tungsten, manganese, technetium, rhenium, iron, cobalt, nickel, copper, cerium, praseodymium and neodymium in the above-described manner. [0010]
  • The consumed, and no longer regenerable, catalyst is melted and processed again into the catalyst of the invention. [0011]
  • The invention is explained by the following examples (all values in mass percent). [0012]
    • EXAMPLES
  • Respectively 2.0 g catalyst in wire form having a diameter of 0.25 mm were placed in a tubular reactor. The experiments were performed at different temperatures and with a pressure of 1 bar under the following loads: 10 Nl/h air with 5,000 ppm of one of the following hydrocarbons. [0013]
    Conv.
    to CO2
    T and H2O
    Hydrocarbon Catalyst [° C.] [%]
    Example 1: An alloy comprising 56.6% Fe, 16.5% 350 100
    n-hexane Cr, 24.2% Mn, 1.0% Mo, 0.8% Cu,
    0.40% N, remainder Ni, Ti, Nb, Al,
    C, P, was annealed for 1 hr at 875°
    C. with air. After cooling, the
    alloy was placed in 10 ml of an
    aqueous solution containing 1.5%
    polyvinyl alcohol, 50 g/l Cu2+ ions
    and 10 mg/l Mn2+ ions for 15 min.,
    removed and annealed again for 1 hr
    at 450° C. in air.
    Example 2: An alloy comprising 71.8% Mn, 350 100
    benzene 17.55% Cu, 10.4% Ni, 0.1% Fe, 0.04%
    Si, 0.009% S and 0.017% C was
    annealed for 1.5 hrs at 650° C. in
    an air-containing environment.
    After cooling, the alloy was placed
    in an aqueous solution containing
    2% starch and 200 g/l Cu2+ ions for
    15 min., removed and annealed again
    for 1 hr at 500° C. in air.
    Example 3: An alloy comprising 71.8% Mn, 300 92
    n-hexane 17.55% Cu, 10.4% Ni, 0.1% Fe, 0.04%
    Si, 0.009% S and 0.017% C was
    annealed for 1.5 hrs at 650° C. in
    an air-containing environment.
    After cooling, the alloy was placed
    in an aqueous solution containing 2
    g/l Cu2+ ions for 10 min., then in
    a 2% polyvinyl-alcohol solution,
    removed and annealed again for 1 hr
    at 500° C. in air.
    Example 4: An alloy comprising 53.72% Fe, 350 100
    toluene 24.2% Cr, 17.7% Ni, 6.14% Mn, 4.34%
    Mo, 0.53% Cu, 0.17% Nb, 0.12% Al,
    0.46% N, 0.004% S, 0.012% C and
    0.017% P was annealed for 2 hrs at
    900° C. with air. After cooling,
    the alloy was placed in 10 ml of an
    aqueous solution containing 1%
    polyvinyl alcohol, 100 g/l Fe3+
    ions, 100 g/l Cu2+ ions and 2 g/l
    Mo6+ ions for 10 min., removed and
    annealed again for 1 hr at 700° C.
    in air.
    Example 5: An alloy comprising 50.85% Co, 325 100
    n-hexane 19.95% Cr, 14.8% W, 2.28% Fe, 1.53%
    Mn, 0.096% C, 0.004% S and 0.006% p
    was annealed for 0.45 hr at 1000° C.
    with air. After cooling, the alloy
    was placed in 10 ml of a 5% aqueous
    crystallized-sugar solution for 3
    min., then placed in a solution
    containing 150 g/l Cu2+ ions, 5 g/l
    W6+ ions and 25 g/l Co2+ ions,
    removed and annealed again for 1 hr
    at 725° C. in air.
    Example 6: An alloy comprising 68.01% Cu, 385 94
    n-hexane 30.6% Ni, 0.70% Fe, 0.67% Mn,
    0.008% C, 0.010% Zn, 0.004% S and
    0.002% P was annealed for 1.2 hrs
    at 875° C. with air. After cooling,
    the alloy was placed in 10 ml of an
    aqueous solution containing 5%
    crystallized sugar, 0.5% polyvinyl
    and 20 g/l Cu2+ ions for 2 minutes,
    removed and annealed again for 1 hr
    at 725° C. in air.
    Example 7: An alloy comprising 37.3% Ni, 315 96
    n-hexane 35.73% Fe, 19.45% Cr, 3.2% Cu,
    2.33% Mo, 1.51% Mn, 0.2% Nb,
    0.26% Si, 0.015% P, 0.006% C and
    0.003% S was annealed for 2 hrs at
    910° C. with air. After cooling, the
    alloy was placed in a 1% aqueous
    polyvinyl-alcohol solution for 2.5
    min., then placed in a solution
    containing 150 gIl Cu2+ ions,
    removed and annealed again for 1 hr
    at 880° C. in air.
    Example 8: An alloy comprising 61.05% Ni, 375 85
    n-hexane 22.5% Cr, 15.3% Mo, 0.68% Fe, 0.26%
    Al, 0.14% Mn, 0.03% Co, 0.006% C,
    0.004% P and 0.002% S was annealed
    for 1 hr at 880° C. with air. After
    cooling, the alloy was placed in a
    solution containing 1.3% polyvinyl
    alcohol, 100 g/l Cu2+ ions and 5
    g/l V4+ ions for 4 min., removed
    and annealed again for 1 hr at 450°
    C. in air.
    Example 9: An alloy comprising 45.64% Fe, 370 80
    n-hexane 24.7% Ni, 20.9% Cr, 6.43% Mo, 0.90%
    Cu, 0.89% Mn, 0.192% N, 0.017% P,
    0.006% C and 0.003% S was annealed
    for 0.5 hr at 1010° C. with air.
    After cooling, the alloy was placed
    in an aqueous solution containing
    1.5% starch and 0.2% polyvinyl
    alcohol for 3 min., then in a
    solution containing 10 g/l Cu2+
    ions, 1 g/l W6+ ions, 1 g/l Al ions
    and 1 g/l Mn2+ ions, removed and
    annealed again for 1.5 hrs at 460°
    C. in air.
    Example 10: An alloy comprising 32.08% Fe, 385 95
    n-hexane 31.3% Ni, 26.85% Cr, 1.54% Mn,
    1.34% Cu, 0.202% N, 0.015% P, 0.01%
    C and 0.003% S was annealed for 2
    hrs at 825° C. with air. After
    cooling, the alloy was placed in 10
    ml of a solution containing 1.5%
    polyvinyl alcohol, 60 g/l Cu2+ ions
    and 10 g/l Ni2+ ions for 2 min.,
    removed and annealed again for 0.5
    hr in air.

Claims (3)

1. A completely-metallic catalyst for the oxidization of mixtures containing carbon monoxide and/or hydrocarbons and/or soot in the gaseous phase, the catalyst being obtainable through an oxidizing thermal treatment of an alloy that may contain manganese, nickel, copper, chromium and iron in an oxygen-containing atmosphere at a temperature of 250 to 1250° C. for 0.05 to 5 hours, and a subsequent treatment with an oxidizable, organic substance, characterized in that an alloy containing at least three of the following elements: manganese, nickel, copper, cobalt, chromium, molybdenum, tungsten, titanium, zirconium, vanadium, niobium, aluminum and iron with a total content of at least 95 mass percent, and up to 5 mass percent of P, N, Si and S and other typical contaminations, the alloy being subjected to an oxidizing thermal treatment in an oxygen-containing atmosphere; after cooling, the alloy is treated with an aqueous solution or emulsion containing an oxidizable, organic substance, with the surface and/or regions near the surface of the alloy being doped with one of the following elements: boron, aluminum, indium, germanium, tin, lead, scandium, yttrium, lanthanum, titanium, zirconium, vanadium, niobium, chromium, molybdenum, tungsten, manganese, technetium, rhenium, iron, cobalt, nickel, copper, cerium, praseodymium or neodymium; and the alloy is subsequently subjected to a second thermal treatment in an oxygen-containing atmosphere over a period of 5 min. to 3 hrs at a temperature of 250 to 1250° C.
2. The completely-metallic catalyst according to
claim 1
, characterized in that the elements of the aqueous solution or emulsion used to dope the surface and/or the regions near the surface of the alloy are added in a concentration that corresponds at the maximum to the saturation concentration of the metallic compound.
3. The completely-metallic catalyst according to
claim 1
, characterized in that the elements used to dope the surface and/or the regions near the surface of the alloy are applied prior to the treatment with the aqueous solution or emulsion, or after the treatment with the aqueous solution or emulsion, in an intermediate thermal treatment in a temperature range of 30 to 1250° C.
US09/230,466 1996-07-26 1997-07-23 Method of making a completely-metallic oxidation catalyst Expired - Lifetime US6274532B1 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE19630250.1 1996-07-26
DE19630250 1996-07-26
DE19630250A DE19630250C1 (en) 1996-07-26 1996-07-26 Metal alloy catalyst for the total oxidation carbon mon:oxide, soot and/or hydrocarbon
PCT/EP1997/003976 WO1998004347A1 (en) 1996-07-26 1997-07-23 Completely metallic oxidation catalyst

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US6274532B1 US6274532B1 (en) 2001-08-14
US20010018400A1 true US20010018400A1 (en) 2001-08-30

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US (1) US6274532B1 (en)
EP (1) EP0914207B1 (en)
JP (1) JP2000515805A (en)
KR (1) KR20000029572A (en)
CN (1) CN1103247C (en)
AT (1) ATE200744T1 (en)
AU (2) AU720058B2 (en)
CA (1) CA2262883A1 (en)
DE (2) DE19630250C1 (en)
WO (1) WO1998004347A1 (en)

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EP0753345A3 (en) * 1995-07-12 1997-09-03 Krupp Vdm Gmbh Entirely metallic manganese-containing oxidation catalyst
DE19646131C1 (en) * 1996-11-08 1998-08-06 Krupp Vdm Gmbh Process for producing an all-metal catalyst
DE19651807C2 (en) * 1996-12-13 1999-02-25 Krupp Vdm Gmbh Use of a catalyst for reductive NO¶x¶ removal from exhaust gases

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CN1226190A (en) 1999-08-18
AU1741699A (en) 1999-05-24
US6274532B1 (en) 2001-08-14
AU4115697A (en) 1998-02-20
KR20000029572A (en) 2000-05-25
JP2000515805A (en) 2000-11-28
CN1103247C (en) 2003-03-19
CA2262883A1 (en) 1998-02-05
ATE200744T1 (en) 2001-05-15
EP0914207B1 (en) 2001-04-25
DE19630250C1 (en) 1997-08-28
AU720058B2 (en) 2000-05-25
EP0914207A1 (en) 1999-05-12
WO1998004347A1 (en) 1998-02-05
DE59703442D1 (en) 2001-05-31

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