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WO1983001612A1 - Chloruration d'un materiau alumineux - Google Patents

Chloruration d'un materiau alumineux Download PDF

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Publication number
WO1983001612A1
WO1983001612A1 PCT/GB1982/000306 GB8200306W WO8301612A1 WO 1983001612 A1 WO1983001612 A1 WO 1983001612A1 GB 8200306 W GB8200306 W GB 8200306W WO 8301612 A1 WO8301612 A1 WO 8301612A1
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WIPO (PCT)
Prior art keywords
stage
chloride
aluminium
chlorine
carbon monoxide
Prior art date
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Ceased
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PCT/GB1982/000306
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English (en)
Inventor
Process Licensing Corporation Bv Mineral
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Mineral Process Licensing Corp BV
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Mineral Process Licensing Corp BV
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Filing date
Publication date
Application filed by Mineral Process Licensing Corp BV filed Critical Mineral Process Licensing Corp BV
Priority to AU90536/82A priority Critical patent/AU9053682A/en
Publication of WO1983001612A1 publication Critical patent/WO1983001612A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/02—Halides of titanium
    • C01G23/022—Titanium tetrachloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/48—Halides, with or without other cations besides aluminium
    • C01F7/56—Chlorides
    • C01F7/58—Preparation of anhydrous aluminium chloride
    • C01F7/60—Preparation of anhydrous aluminium chloride from oxygen-containing aluminium compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/06—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide [Fe2O3]

Definitions

  • TITLE Chlorination of an aluminous material
  • This invention relates to a process for the chlorination of an aluminous material, particularly bauxite. More specifically this invention relates to a process for the chlorination of an aluminous material such as bauxite to give aluminium chloride of sufficient purity for it to be suitable for use as the cell feed for the electrolysis of aluminium chloride to give aluminium metal. According to another aspect the invention provides a process whereby by-products of the primary production of aluminium chloride from an aluminous material such as bauxite may be easily recovered and, if desired, converted into valuable components for recycling.
  • Carbochlorination of bauxite to produce aluminium chloride has been fairly widely used industrially over the past 60 years or so.
  • the best known examples are the processes employing the treatment of bauxite with chlorine and carbon, or with mixtures of chlorine and carbon monoxide or phosgene. These processes, however, relied on sources of bauxite with a very low content of iron oxide.
  • pure gibbsite was used when supplies of bauxite low in iron oxide were no longer available. This would not be economically acceptable for the production of aluminium chloride for use as electrolytic cell-feed.
  • a disadvantage of an earlier proposal is the lack of any satisfactory step either for the separation of iron chlorides from aluminium chloride, or for the recovery of chloride values from the iron chloride in conjunction with the conversion of the iron residue to an environmentally acceptable or saleable form.
  • One suggested method for the removal of iron chloride from the aluminium chloride has involved the use of metallic aluminium to reduce ferric chloride, FeCl_ , to ferrous
  • the present invention thus provides a multi ⁇ stage process for the production of aluminium chloride which comprises
  • the selective reduction in stage (C) whereby aluminium chloride is separated from ferric chloride may be accomplished using carbon monoxide as the reducing agent or metallic iron.
  • the process according to the invention is particularly economical in that reactants required for one stage of the multi-stage process can be generated from another stage.
  • carbon monoxide which is preferably employed in the first stage (A) for the chlorination of the aluminous material is obtained in a further reaction stage (E) by reaction of the carbon dioxide off-gas from the condensation stage with a suitable source of carbon at _an elevated temperature.
  • the carbon monoxide obtained from the carbon dioxide off-gas in stage ( ⁇ ) may also be used in a subsequent reaction stage, (C) according to one embodiment, where the aluminium and ferric chlorides are separated by reduction with carbon monoxide.
  • the ferrous chloride resulting from the separation of the aluminium chloride is subjected to a further reaction stage (D) where the ferrous chloride is oxidised with oxygen or an oxygen-containing gas at an ' elevated temperature preferably in the presence of at least one salt of an alkali metal or alkaline earth metal.
  • This oxidation reaction produces iron oxide and chlorine which is recycled to the initial chlorination stage (A) .
  • the oxidation reaction of stage (D) may be operated under conditions such that the iron oxide produced is in the form of an industrially useful form of iron oxide suitable, for example, for pigmentary application or for use as a filler.
  • the iron oxide, or a part thereof, obtained in stage (D) , by dechlorination of ferrous chloride may be subjected to further reduction in stage (F) , for example using carbon monoxide, to give the metal which may be recycled to stage (C) when the separation of the ferric and aluminium chloride (C) is accomplished using metallic iron.
  • stage (F) for example using carbon monoxide
  • the carbon monoxide required for this reaction may be obtained from the carbon monoxide generation stage (E) as previously described.
  • the present invention not only provides a process for the production of aluminium chloride suitable for use as feed for an electrolysis cell but also provides a process whereby chlorine values can be recovered from iron chloride by-product and used in the initial chlorination stage of the invention.
  • the invention moreover provides a multi-stage process whereby reactants -such as carbon monoxide, phosgene and metallic iron can be generated from one process stage and recycled for use in another stage.
  • reactants -such as carbon monoxide, phosgene and metallic iron can be generated from one process stage and recycled for use in another stage.
  • the invention also lends itself to the production of a potentially valuable by-product, iron oxide.
  • the process comprises the following reaction stages:- Stage A
  • bauxite (identified as BX . in the flowsheets) is chlorinated using chlorination reagents which comprise chlorine together with carbon monoxide, or phosgene (C0C1-) , or mixtures of chlorine, carbon. onoxide and phosgene. Chlorin ⁇ ation of the alumina content of the bauxite then occurs according to the following chemical equations:
  • the Fe ⁇ O.., TiO- and SiO- contents of the bauxite are similarly chlorinated to give FeCl,, TiCl 4 and SiCl. respectively.
  • the chlorination reaction may be carried out in either a fixed-bed type of reactor, as has been de ⁇ scribed in the literature for example by Wurster (Zeitschrift fur Angewandte Chemie 1930, 43, 877-880) and Hille and Durrwachter (Angewandte Chemie, I960, pp. 73-79) , or it may be performed in a fluid-bed reactor.
  • the bauxite is ' preferably calcined prior to the chlorination
  • the temperature chosen for calcination will depend to some extent on the increase in reactivity and decrease in water content desired, but is likely to be in the temperature range 600 - 1100°C.
  • the temperature employed for chlorination will depend on the reaction rate obtainable, compared with the service life of containment refractories, but will generally fall within the range 550°C-1100°C..
  • the chlorination reaction may be carried out batchwise or continuously.
  • a second stage (B) some of the chlorides by-produced in the first stage (A) , and particularly titanium and silicon tetrachlorides (ii) , are removed by condensation.
  • the product gases leaving the chlorination reactor (Stage A) comprise a mixture of carbon dioxide, aluminium chloride (AlCl,) , ferric chloride (FeCl 3 ) , titanium tetrachloride (TiCl.) , and silicon tetrachloride (SiCl.) .
  • Stage (B) is a two- stage condenser, the operating principle of which is based on the difference in volatilities between FeCl, (boiling-point 315°C) , AlCl., (Sublimation temperature 177.8°C), TiCl 4 (boiling-point 136.4°C) and SiCl 4 (boiling-point 57.6°C). Due to the well-known vapour-phase association between FeCl., and AlCl., to give FeAlCl fi , it is not possible to separate these two species by a simple condensation step.
  • the first stage of the condenser is maintained at a temperature below 177.8°C (the sublimation temperature of AlCl,) , but substantially above the boiling-point of TiCl. (136.4°C).
  • the first stage of the condenser may take any suitable form.
  • a preferred form of condenser particularly suitable for the continuous deposition in solid form of FeCl,- and AlCl,-containing species from the vapour-phase comprises a fluidised- bed of a suitable inert material, maintained at a suitable temperature to ensure substantially complete removal of the FeCl, and AlCl,-containing species from the vapour-phase.
  • a fluidised- bed of a suitable inert material maintained at a suitable temperature to ensure substantially complete removal of the FeCl, and AlCl,-containing species from the vapour-phase.
  • continuous removal of the product can be achieved by maintaining a continous bed overflow.
  • the second stage of the condenser may again take any suitable form, and is maintained at a temperature low enough to ensure substantially complete removal of the remaining chlorides, TiCl. and SiCl ⁇ ,, from the vapour-phase. Condensation of TiCl 4 and SiCl.
  • separation of TiCl. and SiCl d may be provided for by operating the second stage of the condenser at a temperature within the range between the boiling-points fo SiCl. and iCl ⁇ (57.6°C and 136.4°C respectively) with a number of fractionating stages.
  • the output from Stage (B) therefore comprises three distinct product streams, viz. (i) a solid mixture of AlCl, and FeCl., from the first stage, (ii) liquid TiCl. and SiCl ⁇ from the second stage, and (iii) carbon dioxide gas from the second stage.
  • Stage C a solid mixture of AlCl, and FeCl.
  • ferric chloride is separated from the desired aluminium chloride. Separation of the FeCl, from the AlCl, is accomplished by chemical reduction of the FeCl, to F Cl 2 , which has a much lower volatility than FeCl, and therefore can be separated by deposition as a solid
  • the reducing agent used is carbon monoxide.
  • the reduction step is represented by the following chemical equation:
  • the reaction may be carried out in the vapour-phase, at a temperature. above the boiling-point of FeCl, (315°C) but below the melting-point of eCl 2 (673°C) . Within this temperature range, reduction of FeCl, to FeCl- according to equation (3) results in the deposition of FeCl- in solid form from the vapour-phase, leaving substantially iron-free AlCl 3 in the vapour-phase, suitable for feeding to the electrolytic cell.
  • silica envelope 4 and side-arm 6 were heated by means of electrically-powered heating tape
  • AlCl, for reaction (3) may be obtained by the vaporisation of the mixed condensed FeCl, - AlCl, solids from Stage (B) , and feeding the resulting vapour
  • the desired reactor configuration may take several possible forms.
  • a particularly suitable form is a cyclone reactor, into which the carbon monoxide gas and mixed FeCl- - AlCl, vapours
  • This reactor configuration provides for continuous operation, with good mixing of the reacting gases and a relatively long residence time per unit of reaction volume, and facilitates the discharge of the solid FeCl- from the bottom of the
  • Reaction 3 may also be performed by contacting carbon ,_ monoxide gas with the solid FeCl., -AlCl,, followed by
  • Equation (3) It may be preferable to initiate the reaction exemplified in Equation (3) , whether performed as a vapour-solid reaction or as a homogeneous vapour-phase reaction, by the presence of sulphur or a sulphur chloride, as described in U.S. Patent 4,140,746.
  • the separation of FeCl, from A1C1 3 according to this invention based on Equation (3) has the advantage, not found with other methods of * separating FeCl, from AlCl,, of providing phosgene, C0C1 2 , as a useful by-product for recycle to the bauxite chlorination reactor (Stage A).
  • Stage (E) the requirement of a source of carbon monoxide for use as the reducing agent is met, as will be described later under Stage (E) , by the passage of carbon dioxide (obtained from Stage (A) and after passing through the two-stage condenser (Stage B) over heated carbon.
  • the method of separating FeCl, from AlCl, according to this embodiment of the invention is therefore eminently suitable when seen in the context of the overall process, the aim of which is to provide AlCl, of eletroclytic cell-feed purity, starting with the chlorination of an " aluminous material such as bauxite.
  • Stage (D) chlorine values are recovered from the ferrous chloride produced in Stage (C) , and, recycled to the chlorination Stage (A) .
  • the fourth Stage (D) may also be used to by-produce an industrially useful form of iron oxide.
  • the ferrous chloride by-product from Stage (C) is subjected in Stage (D) to oxidation with oxygen or an oxygen-containing -gas at an elevated temperature in the presence of at least one salt of an alkali metal or alkaline earth metal.
  • the preferred salts are those with which ferrous chloride forms melts which are most suitable to meet the particular requirements of the oxidation process
  • Sodium chloride is one of the preferred salts and is used to exemplify, in the following reaction equations, the nature of the oxidation reaction.
  • other salts may also be used to satisfy the specific requirements of the process according to the invention and to achieve the specific properties which may be required of the iron oxide produced as a co- product.
  • suitable salts include sodium sulphate, sodium carbonate, sodium metaborate, sodium tetraborate, sodium chlorate, potassium chloride, potassium carbonate, lithium chloride, magnesium chloride, magnesium sulphate, calcium carbonate and calcium chloride and mixtures thereof.
  • the oxidation reaction according to the present invention is postulated in the following equations using, as example, sodium chloride as the salt.
  • the apparatus comprises a gas-tight silica envelope 1 having a silica crucible base 2 and being
  • _CHH provided with a tube 3 for input of oxidising gas (0 2 or air) , a sheathed thermocouple 4 and outlet 5 for the C1-/0- off-gases.
  • the apparatus is adapted to be heated by means of a resistance-wound tube furnace 6.
  • a mixed charge of FeCl- and an alkali (or alkaline) earth metal salt 7 was melted and brought up to the desired reaction temperature under nitrogen in the gas-tight silica envelope 1, which was heated by the resistance-wound tube-furnace 6.
  • the melt temperature was measured by means of the sheathed thermocouple 4 immersed in the melt 7.
  • Oxidation was then commenced by bubbling oxygen or air through the melt via tube 3 at a measured flow-rate for a timed period, the off-gas 5 being scrubbed with sodium hydroxide solution.
  • the reactor and contents were allowed to cool under nitrogen, followed by water leaching and chemical analysis of the reaction products.
  • the results of a batch oxidation run performed in the apparatus shown in Fig. 4 using a melt of molar composition 0.5 FeCl-, 0.52 NaCl, 0.48 N 2 S0. are shown in the following Table 1.
  • the results show the excellent chlorine recovery (91%) attained.
  • the melt composition selected for this run is particularly suitable for batch operation in a simple sparged fused salt-bath reactor, since the added alkali-metal salts (NaCl and Na-SO d ) are present in the ratio corresponding to the NaCl-Na-SO, eutectic composition (eutectic temperature 625°C) .
  • the iron oxide co-product of the oxidation reaction was separated off by a simple water-leaching procedure, followed by filtration, water-washing and drying. If desired, the soluble salts can be recovered for re-cycling. Further water-washing of the iron oxide is needed to remove traces of absorbed chloride-. This can be achieved by elutriation with water which can be used to classify the product into fractions varying in particle size and suitable for different pigmentary applications or, for example, for use as a filler.
  • the present invention not only provides a method of recovering chlorine from iron chloride which chlorine can be recycled to the bauxite chlorination Stage (A) , but also provides a method of producing a potentially industrially useful iron oxide.
  • a by-product which has to date caused considerable problems of disposal is transformed into a readily available starting material for two valuable industrial products.
  • the optimum reaction conditions for Stage (D) of the process depend, among other things on the particular salt which is employed.
  • the oxidation reaction may be effected in the melt or on the particul ⁇ ate solids.
  • a suitable source of carbon is coke or coal char.
  • the carbon monoxide-forming reaction as represented by equation (8) is endothermic.
  • Various methods are availalbe for supplying the necessary heat, for example the coke or coal char bed, which may be either a fixed-bed or a fluidised-bed, may be heated directly by inserting electrodes into the charge and passing on electric current through the charge, as has been described, for example, for a fluidised-bed reactor in U.S. Patent No. 2,921,840, and for a fixed-bed reactor in U.K. Patent No. 001,657.
  • An alternative method of supplying process heat is to admit a mixture of oxygen and carbon dioxide to the carbon monoxide generator, the oxygen reacting exothermically with the coke or coal char according to the equations:
  • Stages (A) chlorination of bauxite), B (condensation of titanium and silicon tetracr.lorides) , D (dechlorination of ferrous chloride) and ⁇ (generation of carbon monoxide from carbon dioxide and carbon) are as described in the first embodiment of the invention described with reference to Figure 1.
  • Stage (C) is affected using metallic iron to separate hs aluminium and iron chlorides and an additional stage (Stage F) is employed in which ferric oxide is reduced with carbon monoxide to give metallic iron.
  • Stage F Stage F
  • 5zis embodiment may advantageously be employed whe for any reason it is preferred not to recycle phosgene
  • Stage (C) of this embodiment and the addition Stage (F) are as described below.
  • Stage F
  • ferric oxide is reduced with carbon monoxide to give metallic iron.
  • the underlying chemical principle of this stage is the well-known ability of carbon monoxide to reduce ferric oxide to metallic iron according to the chemical equation:
  • Equation (11) which forms the basis of the production of iron from iron ore in a blast furnace, is given in Mellor's Comprehensive Treatise on Inorganic and Theoretical Chemistry, Volume XIII (Part 2) r p. 813.
  • a reaction temperature of ca. 905°C essentially complete reduction of ferric oxide to metallic iron occurs.
  • part of the ferric oxide from Stage (D) (dechlorination of ferrous chloride) is fed to a reduction reactor which may take any suitable form e.g. a fixed- or fluidised-bed, where reaction occurs according to Equation (11) with carbon monoxide provided from Stage (E) (generation of carbon monoxide from carbon dioxide and carbon) .
  • a fluidised-bed reactor it is possible to provide for a continuous feed of ferric oxide and a continuous bed overflow of metallic iron.
  • the metallic iron which is produced in extremely reactive form, is fed to Stage (C) in which FeCl, and AlCl 3 are separated using metallic iron as described hereinafter.
  • the by-product carbon dioxide may be recycled to Stage (E) but is preferably put to stack .
  • Stage G is preferably put to stack .
  • the reducing agent used is metallic iron from Stage (F) (reduction of ferric oxide with CO to give metallic iron) .
  • the reduction step is represented by the following chemical equation:
  • the reaction is advantageously carried out at a temperature above the boiling-point of eCl 3 (315°C) but below the melting-point of FeCl- (673°C) .
  • eCl 3 315°C
  • FeCl- 673°C
  • Equation (12) reduction of FeCl, to FeCl- according to Equation (12) results in the deposition of FeCl- in solid form from the vapour-phase, leaving a substantially iron-free AlCl, vapour which is fed to the electrolytic cell for the production of aluminium metal.
  • the required feed of gaseous FeCl, andAlCl, for the reaction represented by Equation (12) may be obtained by the vaporisation of the mixed condensed FeCl 3 - AlCl, solids from Stage (B) , and feeding the resulting vapour stream into a suitable reactor where the vapour comes into contact with, and is reduced by, the metallic iron from Stage (F) .
  • the desired reactor configuration may again take several possible forms, e.g. a fixed- or fluidised-bed. De- position of ferrous chloride in solid form may occur
  • this invention comprises a most skilful synthesis from several process stages to give an overall process particularly applicable to the production of electrolytic cell-feed aluminium chloride from the c.hlorination of bauxite.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Procédé multi-étapes de production d'un chlorure d'aluminium par chloruration d'un matériau alumineux, par exemple de bauxite, de préférence en utilisant du chlore et de l'oxyde de carbone ou phosgène, consistant à condenser le produit gazeux, à séparer un mélange d'aluminium et de chlorures ferriques des chlorures d'autres éléments présents dans le matériau alumineux et de l'anhydride carbonique, à séparer le chlorure d'aluminium du chlorure ferrique au moyen d'une réduction sélective, à séparer le chlorure ferreux solide et à récupérer du chlorure d'aluminium sensiblement exempt de fer dans la phase de vapeur permettant d'alimenter une cellule électrolytique, et à oxyder le chlorure ferreux pour produire de l'oxyde de fer et du chlore pouvant être exploités industriellement, le chlorure étant recyclé vers l'étape de chloruration.
PCT/GB1982/000306 1981-10-28 1982-10-27 Chloruration d'un materiau alumineux Ceased WO1983001612A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU90536/82A AU9053682A (en) 1981-10-28 1982-10-27 Chlorination of an aluminous material

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB8132456811028 1981-10-28
GB8132456 1981-10-28

Publications (1)

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WO1983001612A1 true WO1983001612A1 (fr) 1983-05-11

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EP (1) EP0092562A1 (fr)
IT (1) IT1158027B (fr)
WO (1) WO1983001612A1 (fr)
ZA (1) ZA827753B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0120572A1 (fr) * 1983-02-24 1984-10-03 Cookson Laminox Limited Procédé pour la production d'un oxyde de fer
WO2013114391A3 (fr) * 2012-01-04 2013-11-07 Keki Hormusji Gharda Procédé de fabrication d'aluminium à partir du bauxite ou de son résidu
NO20190144A1 (en) * 2019-01-31 2020-08-03 Norsk Hydro As A process for production of aluminium

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1875105A (en) * 1926-08-07 1932-08-30 Niagara Smelting Corp Method of and apparatus for mineral chlorination
GB2020643A (en) * 1978-05-10 1979-11-21 Mineral Process Licennsing Cor Recovery of chlorine

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1875105A (en) * 1926-08-07 1932-08-30 Niagara Smelting Corp Method of and apparatus for mineral chlorination
GB2020643A (en) * 1978-05-10 1979-11-21 Mineral Process Licennsing Cor Recovery of chlorine

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0120572A1 (fr) * 1983-02-24 1984-10-03 Cookson Laminox Limited Procédé pour la production d'un oxyde de fer
EP0307486A3 (en) * 1983-02-24 1989-05-17 Cookson Laminox Limited Process for preparing an iron oxide
WO2013114391A3 (fr) * 2012-01-04 2013-11-07 Keki Hormusji Gharda Procédé de fabrication d'aluminium à partir du bauxite ou de son résidu
CN104254494A (zh) * 2012-01-04 2014-12-31 克基·霍尔穆斯吉·阿加尔达 一种从铝土矿或其残渣中生产铝的工艺
EP2800726A4 (fr) * 2012-01-04 2015-08-05 Keki Hormusji Gharda Procédé de fabrication d'aluminium à partir du bauxite ou de son résidu
CN104254494B (zh) * 2012-01-04 2016-11-16 克基·霍尔穆斯吉·阿加尔达 一种从铝土矿或其残渣中生产铝的工艺
RU2626695C2 (ru) * 2012-01-04 2017-07-31 Кеки Хормусджи ГХАРДА Способ получения алюминия из боксита или его шлама
US9896775B2 (en) 2012-01-04 2018-02-20 Keki Hormusji Gharda Process for manufacturing aluminum from bauxite or its residue
NO20190144A1 (en) * 2019-01-31 2020-08-03 Norsk Hydro As A process for production of aluminium

Also Published As

Publication number Publication date
IT8249375A0 (it) 1982-10-27
IT1158027B (it) 1987-02-18
ZA827753B (en) 1983-06-29
EP0092562A1 (fr) 1983-11-02

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