EP0400712A1 - Rahmen für Elektrolyseure der Filterpressenbauart und Elektrolyseure der Filterpressenbauart - Google Patents

Rahmen für Elektrolyseure der Filterpressenbauart und Elektrolyseure der Filterpressenbauart Download PDF

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Publication number
EP0400712A1
EP0400712A1 EP90201266A EP90201266A EP0400712A1 EP 0400712 A1 EP0400712 A1 EP 0400712A1 EP 90201266 A EP90201266 A EP 90201266A EP 90201266 A EP90201266 A EP 90201266A EP 0400712 A1 EP0400712 A1 EP 0400712A1
Authority
EP
European Patent Office
Prior art keywords
sheet
chassis
electrolyser
uprights
metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP90201266A
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English (en)
French (fr)
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EP0400712B1 (de
Inventor
Emile Cabaraux
Eric Paulus
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.)
Solvay SA
Original Assignee
Solvay SA
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 Solvay SA filed Critical Solvay SA
Priority to AT90201266T priority Critical patent/ATE96854T1/de
Publication of EP0400712A1 publication Critical patent/EP0400712A1/de
Application granted granted Critical
Publication of EP0400712B1 publication Critical patent/EP0400712B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/70—Assemblies comprising two or more cells
    • C25B9/73—Assemblies comprising two or more cells of the filter-press type

Definitions

  • the invention relates to electrolysers of the filter press type and more particularly to chassis used in the construction of these electrolysers.
  • Electrolysers of the filter press type are generally formed by a stack of vertical frames which delimit electrolysis chambers in which electrodes are arranged vertically. Selectively permeable membranes or electrolyte permeable diaphragms can be inserted between the frames to separate the electrolysis chambers.
  • the frames are frames formed from an assembly of tubes which are used for the circulation of electrolytes and of products of electrolysis.
  • the electrodes are perforated metal plates, which are fixed to the frames, along their periphery.
  • the tubes forming the frames must be made of a material which withstands the chemical and thermal conditions prevailing in the electrolyser; they are generally made of titanium or nickel, depending on whether they are in an anode chamber or in a cathode chamber of a membrane cell used for the electrolysis of aqueous solutions of sodium chloride. Titanium and nickel have the disadvantage of having a high electrical resistivity, compared to materials such as steel, copper or aluminum, so that these electrolysers have poor energy yields.
  • electrolysers of the filter press type are described, in which the frames include a vertical sheet and a peripheral frame, the whole being lined with a stamped metal sheet.
  • the sheet is used to convey the electric current to the electrodes and is therefore generally made of steel, copper or aluminum.
  • the stamped sheet is used to isolate the sheet and the frame from the aggressive chemical medium present in the electrolyser; it is made of titanium or nickel, depending on whether it is in an anode chamber or in a cathode chamber of a membrane cell for the electrolysis of aqueous solutions of sodium chloride.
  • the chassis have a low resistance to the conduction of electric current, which constitutes an advantage.
  • These frames have the disadvantage, however, that their frame is unusable for the circulation of electrolytes and electrolysis products, because it is entirely covered by the stamped metal sheet.
  • the invention aims to provide a chassis for an electrolyser of the filter press type, which combines the respective advantages of the known electrolysers described above, while avoiding their drawbacks. It more particularly aims to provide a chassis having a low overall resistance to the conduction of electric current, and in which a part of the frame can be used for the circulation of electrolytes and electrolysis products.
  • the invention relates to a chassis for an electrolyser of the filter press type, comprising a vertical metal sheet jacketed with a metal sheet and a peripheral frame formed by two vertical uprights and two horizontal beams; according to the invention, the two uprights are secured to the sheet and are covered with the metal sheet, and the two side members are made of the same material as the sheet, are inserted between the uprights and are secured to the sheet.
  • the frame has the function of delimiting an electrolysis chamber of the electrolyser, the latter having to contain a vertical electrode.
  • the sheet has the function of stiffening the chassis, support the frame and conduct the electric current through the electrolyser.
  • the sheet metal material is not critical, provided it is electrically conductive. However, it is especially recommended to make it from a metal or metal alloy which is a good conductor of electricity; steel, copper and aluminum are preferred.
  • the material used for the side uprights of the frame is not critical.
  • the function of the metal sheet is to isolate the metal sheet and the uprights of the frame from the aggressive chemical medium present in the electrolyser. It must therefore be made of a material which is impermeable to the aggressive constituents of this medium and inert towards them.
  • a material selected from titanium, tantalum, niobium, zirconium, tungsten and the alloys of these metals when the chassis is intended to form an anode chamber of the electrolyser; when the chassis is intended to form a cathode chamber of the electrolyser, the material of the metal sheet is advantageously chosen from nickel and nickel alloys.
  • the metal sheet must also be shaped so that it rests on the sheet, between the uprights and overlaps the uprights.
  • the profile to be given to the sheet therefore depends on the dimensions and the shape of the side members and can be obtained by a stamping or folding operation.
  • the thickness of the sheet must be sufficient for it to withstand the mechanical stresses to which it is subjected during the operation of the electrolyser. Notwithstanding this condition, it is advantageous to use the thinnest possible sheet, so that its electrical resistance, transversely to its surface, is as low as possible. The optimum thickness can be easily determined as soon as its other dimensions have been fixed, the material constituting it and the operating conditions of the electrolyser.
  • the horizontal frame rails must be made in a material which resists the aggressive chemical medium present in the electrolyser. We prefer to make them in the same material as the metal foil. They must also be secured to the metal foil in a sufficiently watertight manner to isolate the sheet and the uprights of the chassis from the aggressive medium present in the electrolyser.
  • the joining of the side members to the metal sheet is usually obtained by welding.
  • the chassis according to the invention is intended to be attached to similar chassis to form an electrolyser of the filter press type.
  • the chassis according to the invention serves to delimit an electrolysis chamber containing a vertical electrode.
  • the electrode is generally made of metal and can be connected to the metal foil by means of electrically conductive junction elements. These can for example be studs or metal profiles welded to the electrode and to the metal sheet. It is recommended that the metal foil is welded to the sheet metal, under the joining elements, to reduce the electrical resistance of the assembly.
  • the chassis comprises, on the one hand, a metal sheet and a peripheral frame on each face of the sheet and, on the other hand, two vertical electrodes arranged respectively on the side and on the 'other of the sheet and respectively connected to the metal sheets by electrically conductive junction elements.
  • the two electrodes are two anodes or two cathodes; the two metal sheets can then be made of the same material and the metal sheet must be extended by a metal strip extending outside the frame, to be connected to a source of electric current.
  • one electrode is an anode and the other electrode is a cathode
  • the metal sheet then serving for the transfer of the electric current from the cathode to the anode when the electrolyser is in operation.
  • the uprights and the frame members may have any cross section compatible with the construction of the electrolyser. We prefer to give them a polygonal cross section, generally square, rectangular or trapezoidal.
  • the longitudinal members are profiled so as to form, along the sheet, two longitudinal channels which are pierced with openings on their respective walls which face each other; one of the channels is also connected to an electrolyte intake conduit, the other channel being connected to a conduit for discharging the products of electrolysis.
  • the channels of the side members serve to distribute the electrolyte in the electrolysis chamber delimited by the frame and to evacuate the products thereof resulting from the electrolysis.
  • the chassis according to the invention can be adapted to the construction of monopolar electrolysers or bipolar electrolysers.
  • the invention therefore also relates to monopolar electrolysers of the filter press type and bipolar electrolysers of the filter press type, formed from a stack of chassis in accordance with the invention, said chassis delimiting electrolysis chambers which contain electrodes. .
  • the invention applies especially to electrolysers of this type, in which the electrolysis chambers are separated by separators which are permeable to ions.
  • the separators are sheets interposed between the successive frames of the stack and made of a material capable of being traversed by an ion current during the operation of the electrolyser. They can be either diaphragms permeable to aqueous electrolytes or membranes with selective permeability.
  • diaphragms which can be used in electrolysers according to the invention are asbestos diaphragms, such as those described in patent US-A-1855497 (STUART) and in patents FR-A-2400569, EP-A-1644 and EP -A-18034 (SOLVAY & Cie) and diaphragms in organic polymers, such as those described in patents FR-A-2170247 (IMPERIAL CHEMICAL INDUSTRIES PLC) and in patents EP-A-7674 and EP-A-37140 (SOLVAY & Cie).
  • asbestos diaphragms such as those described in patent US-A-1855497 (STUART) and in patents FR-A-2400569, EP-A-1644 and EP -A-18034 (SOLVAY & Cie)
  • diaphragms in organic polymers such as those described in patents FR-A-2170247 (IMPERIAL CHEMICAL INDUSTRIES PLC) and
  • membranes with selective permeability is understood to mean thin, non-porous membranes comprising an ion-exchange material.
  • the choice of the material constituting the membranes and of the ion exchange material will depend on the nature of the electrolytes subjected to the electrolysis and on the products which it is sought to obtain.
  • the material of the membranes is chosen from those which are capable of withstanding the thermal and chemical conditions normally prevailing in the electrolyser during electrolysis, the ion-exchange material being chosen from anion-exchange materials or cation exchange materials, depending on the electrolysis operations for which the electrolyser is intended.
  • membranes which are well suited are cationic membranes in fluorinated polymer, preferably perfluorinated, containing cationic functional groups derived from sulfonic acids, carboxylic acids or phosphonic acids or mixtures of such functional groups.
  • membranes of this type are those described in patents GB-A-1497748 and GB-A-1497749 (ASAHI KASEI KOGYO KK), GB-A-1518387, GB-A-1522877 and US-A-4126588 (ASAHI GLASS COMPANY LTD) and GB-A-1402920 (DIAMOND SHAMROCK CORP.).
  • Membranes particularly suitable for this application of the cell according to the invention are those known under the names "NAFION” (DU PONT DE NEMORS & Co) and "FLEMION” (ASAHI GLASS COMPANY LTD).
  • the electrolysers according to the invention find a particularly advantageous application for the production of chlorine and aqueous solutions of sodium hydroxide by electrolysis of aqueous solutions of sodium chloride.
  • the invention is specifically applied to electrolysers of the cationic membrane filter press type, for the production of chlorine and aqueous sodium hydroxide solutions by electrolysis of aqueous sodium chloride solutions.
  • the chassis according to the invention is designed to form two anode chambers paired with a monopolar electrolyser. It comprises a vertical sheet 1 of copper and two peripheral frames respectively disposed on either side of the sheet 1.
  • the frames have a rectangular cross section. They each include two vertical uprights 2 and 3 of copper or steel, welded to the sheet 1 and two longitudinal members 4 and 5 of titanium.
  • the sheet is lined in two titanium sheets 6 folded in the shape of an ⁇ , so that they are applied to the sheet 1 under the side members 4 and 5 and overlap the uprights 2 and 3.
  • the titanium sheets 6 are welded to the side members 4 and 5 by means of continuous weld beads, so as to form a sealed assembly.
  • Two vertical anodes 7 are disposed respectively inside the frames. Each of them consists of an openwork vertical titanium plate, carrying a conductive coating with low overvoltage for the electrochemical oxidation of chloride ions. Such coatings are well known in the art of electrolysis.
  • Each plate 7 is fixed to the sheet 6 by means of vertical titanium profiles 8.
  • the sheet 1 is extended outside the frames in the form of a marginal strip 9 intended to be connected to the positive terminal of a source direct current.
  • the electrical connection between the current source (not shown) and the anode plates 7 is made via the marginal strip 9, the sheet 1, the titanium sheets 6 and the profiles 8.
  • the electrical connection between the sheet 1 and the sheets 6 can be obtained under the action of the hydrostatic pressure of the electrolyte during the operation of the electrolyser; as a variant, it is possible to provide welding points for the sheets 6 to the sheet 1, under the profiles 8.
  • the tubular beams 4 and 5 are tubes of rectangular section thus delimiting four longitudinal channels 23. Their ends are hermetically welded to the sheets 6. They are moreover pierced with openings 10 regularly distributed on their walls which face each other.
  • the lower tubular beams 5 are provided with a tube 11 for the admission into their respective channels 23, of an aqueous solution of sodium chloride to be electrolyzed; similarly, the upper beams 4 are provided with a tube 12 for the evacuation of the electrolysis products, in this case chlorine and a dilute solution of sodium chloride.
  • the side members 4 and 5 are each formed of a titanium plate folded in a U and welded to the titanium sheet 6 so as to delimit the channel 23.
  • the horizontal beams 4 and 5, the sheets 6, the profiles 8 and the plates 7 (forming cathodes) are made of nickel.
  • the nickel plates 7 can advantageously carry a conductive coating with low overvoltage of electrochemical reduction of the protons; such coatings are well known in the art of electrolysis.
  • the chassis according to the invention is designed to form two twin chambers, respectively anode 13 and cathode 14, of a bipolar electrolyser.
  • it has the same spatial configuration as the chassis of FIGS. 1 to 3 and it also comprises a vertical sheet 1 of copper and, on each face of the latter, two vertical uprights 2 and 3 of copper or steel, welded to the sheet 1.
  • the anode chamber 13 is arranged like each of the twin anode chambers of the chassis of FIGS. 1 to 3.
  • the sheet 6 covers the sheet 1 and the two uprights 2 and 3, two titanium beams 4 and 5 pierced with a row of openings on their opposite walls, facing the titanium sheet 6 and a titanium anode (carrying an active coating for the electrochemical oxidation of chloride ions) fixed to the sheet 6 by titanium profiles 8.
  • the sheet 1 and the two vertical uprights 2 and 3 are covered with a nickel sheet 6 ′.
  • the two tubular beams 4 ′ and 5 ′ (pierced with a row of openings 10 ′ in their facing walls), the plate 7 ′ and the profiles 8 ′ are made of nickel.
  • the nickel cathode plate 7 ′ is preferably provided with an active coating for the electrochemical reduction of the protons.
  • the tubing 11 ′ is used for the admission of water or a dilute aqueous solution of sodium hydroxide into the channel 23 ′ defined by the lower beam 5 ′ and the tubing 12 ′ is used for the evacuation of the products of the electrolysis (in this case hydrogen and a concentrated aqueous solution of sodium hydroxide) outside the channel 23 ′ defined in the upper tubular beam 4 ′.
  • the products of the electrolysis in this case hydrogen and a concentrated aqueous solution of sodium hydroxide
  • the electrolyser shown in FIG. 7 is of the monopolar type. It is made up of a stack of vertical frames, alternately anodic 15 and cathodic 15 ′.
  • the anode frames 15 are similar to those described above, with reference to FIGS. 1 to 3.
  • the cathode frames 15 ′ are analogous to the anode frames 15, in which the constituent elements in titanium have been replaced by similar elements in nickel.
  • These nickel elements of chassis 15 ′ have the same reference numbers as their respective counterparts of chassis 15, but are assigned a prime index (′).
  • the electrolyser is terminated by a 15 ′ cathode half-frame.
  • the chassis 15 and 15 ′ are separated by cationic membranes 16, which thus delimit alternately anodic and cathodic electrolysis chambers.
  • the stack of frames 15 and 15 ′ and membranes 16 is retained between end plates 17 and 18, connected by tie rods not shown.
  • Sheets 24 of an electrically non-conductive material provide electrical insulation between the flanges 17 and 18 and the end half-frames 15 ′ of the electrolyser.
  • the marginal bands 9 (FIG. 2) of the sheets 1 of the anode frames 15 are connected to a common bus bar, connected to the positive terminal of a direct current source, the marginal bands 9, the bus bar and the current source n 'not being visible in Figure 7.
  • the marginal strips of the sheets 1 of the cathode frames 15' are connected to a common bus bar, connected to the negative terminal of the DC source.
  • the pipes 11 and 12 of the anode frames 15 open respectively into a common manifold 19 for admitting an aqueous solution of sodium chloride and into a manifold 20 serving for the evacuation of a chlorine emulsion in a solution. dilute aqueous sodium chloride.
  • the tubes 11 ′ and 12 ′ of the cathode frames 15 ′ open respectively into two general collectors 19 ′ and 20 ′, the manifold 19 ′ serving for the admission of water or a dilute solution of sodium hydroxide in the cathode chambers and the collector 20 ′ serving for the evacuation of the hydrogen produced during the electrolysis and of a concentrated solution of sodium hydroxide.
  • the electrolyser shown in FIG. 8 is of the bipolar type. It is formed by a stack of chassis conforming to that shown in FIGS. 5 and 6 and by cationic membranes 16, so as to delimit alternately anodic 13 and cathodic 14 electrolysis chambers. At its ends, the electrolyser is terminated by two half-frames, respectively anode 21 and cathode 22.
  • the sheet 1 of the anode half 21 is connected to the positive terminal of a direct current source, not shown and the sheet 1 of the cathode half frame 22 is connected to the negative terminal of the current source.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Selective Calling Equipment (AREA)
  • Control Of Motors That Do Not Use Commutators (AREA)
  • Treatment Of Sludge (AREA)
  • Measuring Fluid Pressure (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Body Structure For Vehicles (AREA)
EP90201266A 1989-05-29 1990-05-18 Rahmen für Elektrolyseure der Filterpressenbauart und Elektrolyseure der Filterpressenbauart Expired - Lifetime EP0400712B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT90201266T ATE96854T1 (de) 1989-05-29 1990-05-18 Rahmen fuer elektrolyseure der filterpressenbauart und elektrolyseure der filterpressenbauart.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8907142 1989-05-29
FR8907142A FR2647468B1 (fr) 1989-05-29 1989-05-29 Chassis pour electrolyseur du type filtre-presse et electrolyseurs du type filtre-presse

Publications (2)

Publication Number Publication Date
EP0400712A1 true EP0400712A1 (de) 1990-12-05
EP0400712B1 EP0400712B1 (de) 1993-11-03

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ID=9382195

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EP90201266A Expired - Lifetime EP0400712B1 (de) 1989-05-29 1990-05-18 Rahmen für Elektrolyseure der Filterpressenbauart und Elektrolyseure der Filterpressenbauart

Country Status (11)

Country Link
US (1) US5141618A (de)
EP (1) EP0400712B1 (de)
JP (1) JPH0324287A (de)
AT (1) ATE96854T1 (de)
BR (1) BR9002507A (de)
CA (1) CA2017496A1 (de)
DE (1) DE69004338T2 (de)
ES (1) ES2047823T3 (de)
FR (1) FR2647468B1 (de)
NO (1) NO303232B1 (de)
PT (1) PT94116B (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0505899A1 (de) * 1991-03-18 1992-09-30 Asahi Kasei Kogyo Kabushiki Kaisha Bipolare filterpressenartige Elektrolysezelle
EP0521386A2 (de) * 1991-06-26 1993-01-07 CHLORINE ENGINEERS CORP., Ltd. Elektrolyseur und Herstellung davon
CN1054403C (zh) * 1993-04-30 2000-07-12 氯工程公司 压滤式电解槽

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1048041C (zh) * 1995-07-27 2000-01-05 北京化工机械厂 单极式离子膜电解装置
US6080290A (en) * 1997-01-03 2000-06-27 Stuart Energy Systems Corporation Mono-polar electrochemical system with a double electrode plate
US6576096B1 (en) * 1998-01-05 2003-06-10 Lynntech International, Ltd. Generation and delivery device for ozone gas and ozone dissolved in water
US6964739B2 (en) 2000-12-12 2005-11-15 Tersano Inc. Device and method for generating and applying ozonated water
KR101083987B1 (ko) * 2007-06-26 2011-11-16 가부시키 가이샤 타케우치 기쥬쯔 켄큐쇼 커넥터의 제조방법

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0020887A1 (de) * 1979-04-12 1981-01-07 Hoechst Aktiengesellschaft Elektrolyseapparat zur Herstellung von Chlor aus wässerigen Alkalichloridlösungen
EP0172495A2 (de) * 1984-08-07 1986-02-26 Asahi Kasei Kogyo Kabushiki Kaisha Mehrzelliger Elektrolyser
EP0220659A1 (de) * 1985-10-23 1987-05-06 Asahi Kasei Kogyo Kabushiki Kaisha Bipolare Elektrolysevorrichtung und Einheitszelle für diese
EP0282614A1 (de) * 1987-03-17 1988-09-21 The Dow Chemical Company Baurahmen für eine elektrochemische Zelle

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS51119681A (en) * 1975-04-15 1976-10-20 Asahi Glass Co Ltd A cell frame for an electrolizer
US4654136A (en) * 1984-12-17 1987-03-31 The Dow Chemical Company Monopolar or bipolar electrochemical terminal unit having a novel electric current transmission element
US4666580A (en) * 1985-12-16 1987-05-19 The Dow Chemical Company Structural frame for an electrochemical cell

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0020887A1 (de) * 1979-04-12 1981-01-07 Hoechst Aktiengesellschaft Elektrolyseapparat zur Herstellung von Chlor aus wässerigen Alkalichloridlösungen
EP0172495A2 (de) * 1984-08-07 1986-02-26 Asahi Kasei Kogyo Kabushiki Kaisha Mehrzelliger Elektrolyser
EP0220659A1 (de) * 1985-10-23 1987-05-06 Asahi Kasei Kogyo Kabushiki Kaisha Bipolare Elektrolysevorrichtung und Einheitszelle für diese
EP0282614A1 (de) * 1987-03-17 1988-09-21 The Dow Chemical Company Baurahmen für eine elektrochemische Zelle

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0505899A1 (de) * 1991-03-18 1992-09-30 Asahi Kasei Kogyo Kabushiki Kaisha Bipolare filterpressenartige Elektrolysezelle
US5225060A (en) * 1991-03-18 1993-07-06 Asahi Kasei Kogyo Kabushiki Kaisha Bipolar, filter press type electrolytic cell
EP0521386A2 (de) * 1991-06-26 1993-01-07 CHLORINE ENGINEERS CORP., Ltd. Elektrolyseur und Herstellung davon
EP0521386A3 (en) * 1991-06-26 1993-03-24 Chlorine Engineers Corp., Ltd. Electrolyzer and its production
CN1054403C (zh) * 1993-04-30 2000-07-12 氯工程公司 压滤式电解槽

Also Published As

Publication number Publication date
NO303232B1 (no) 1998-06-15
JPH0324287A (ja) 1991-02-01
EP0400712B1 (de) 1993-11-03
NO902350D0 (no) 1990-05-28
FR2647468A1 (fr) 1990-11-30
BR9002507A (pt) 1991-08-13
PT94116B (pt) 1996-09-30
CA2017496A1 (fr) 1990-11-29
DE69004338D1 (de) 1993-12-09
NO902350L (no) 1990-11-30
DE69004338T2 (de) 1994-05-19
FR2647468B1 (fr) 1992-03-13
ATE96854T1 (de) 1993-11-15
US5141618A (en) 1992-08-25
PT94116A (pt) 1991-01-08
ES2047823T3 (es) 1994-03-01

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