EP0201815B2 - Verwendung von Tensidgemischen als Hilfsmittel für die Flotation von nichtsulfidischen Erzen - Google Patents

Verwendung von Tensidgemischen als Hilfsmittel für die Flotation von nichtsulfidischen Erzen Download PDF

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Publication number
EP0201815B2
EP0201815B2 EP86106023A EP86106023A EP0201815B2 EP 0201815 B2 EP0201815 B2 EP 0201815B2 EP 86106023 A EP86106023 A EP 86106023A EP 86106023 A EP86106023 A EP 86106023A EP 0201815 B2 EP0201815 B2 EP 0201815B2
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Prior art keywords
flotation
alkyl
mixtures
collector
component
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English (en)
French (fr)
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EP0201815A2 (de
EP0201815B1 (de
EP0201815A3 (en
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Wolfgang Dr. Von Rybinski
Rita Köster
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/012—Organic compounds containing sulfur
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/008—Organic compounds containing oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/01—Organic compounds containing nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/02—Collectors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores
    • B03D2203/04—Non-sulfide ores

Definitions

  • the invention relates to the use of mixtures of nonionic ethylene oxide / propylene oxide addition products and anionic or cationic surfactants known per se as collectors for flotation processes as auxiliaries for the flotation of non-sulfidic ores.
  • Non-sulfidic minerals include apatite, fluorite, sheelite and other salt-like minerals, cassiterite and other metal oxides, e.g. Oxides of titanium and zirconium, as well as certain silicates and aluminosilicates.
  • the ore is pre-shredded and dry, but preferably ground wet, and suspended in the water.
  • the non-sulfidic ores usually become collectors, often in connection with foaming agents and possibly other auxiliary reagents such as regulators.
  • these reagents are allowed to act on the finely ground ore for a certain time (conditioning) before air is blown into the suspension (flotation) in order to produce a foam on their surface.
  • the collector ensures that the surface of the minerals is rendered hydrophobic, so that these minerals adhere to the gas bubbles formed during the aeration.
  • the mineral components are made hydrophobic selectively in such a way that the components of the ore which are undesirable do not adhere to the gas bubbles.
  • the mineral-containing foam is stripped off and processed.
  • the aim of flotation is to extract the mineral of value from the ores in the highest possible yield, while at the same time maintaining the best possible enrichment.
  • anionic and cationic surfactants are used as collectors.
  • Known anionic collectors are, for example, saturated and unsaturated fatty acids, in particular tall oil fatty acids and oleic acid, alkyl sulfates, in particular alkyl sulfates derived from fatty alcohols or fatty alcohol mixtures, alkyl aryl sulfonates, alkyl sulfosuccinates, alkyl sulfosuccinamates and acyl lactylates.
  • Known cationic collectors are, for example, primary aliphatic amines, in particular the fatty amines derived from the fatty acids of vegetable and animal fats and oils, as well as certain alkyl-substituted and hydroxyalkyl-substituted alkylenediamines and the water-soluble acid addition salts of these amines.
  • non-ionic surfactants are hardly used as collectors in flotation.
  • combinations of ionic and nonionic surfactants are also described as collectors.
  • US-A-4,358,368 (Berol Nobel) proposes the use of selected ampholytic collectors for the flotation of apatite ores, which can be combined with a large number of water-insoluble and therefore non-surfactant co-collectors.
  • fatty alcohol polyoxyalkylene glycol ethers are also considered as possible co-collectors.
  • US-A-4,211,644 (Pennwalt) relates to the use of mercaptan and collector systems nonionic surfactants for the flotation of copper ores.
  • the object of the present invention was therefore to improve known collectors (primary collectors) for the flotation of non-sulfidic ores by suitable additives (co-collectors) in such a way that the yield of valuable minerals in the flotation process is significantly increased while the selectivity of the collectors remains practically the same Effect can also be used in such a way that (compared to the collector quantities of the prior art) reduced quantities of collector and co-collector give constant yields of valuable minerals.
  • ethylene oxide / propylene oxide addition products are known substances that can be synthesized by known methods. As a rule, they are obtained by adding the intended amounts of ethylene oxide propylene oxide to the fatty alcohols used as the starting material using known alkaline alkoxylation catalysts.
  • the addition of the alkylene oxides can be carried out either by reacting a corresponding mixture of ethylene oxide and propylene oxide with the fatty alcohol starting material or by adding one alkylene oxide first and then the other.
  • the fatty alcohol component of the ethylene oxide / propylene oxide addition products defined under a) can consist of straight-chain and branched, saturated and unsaturated compounds of this category with 12 to 18 carbon atoms, for example n-dodecanol, n-tetradecanol, n-hexadecanol, n-octadecanol, n- Eicosanol, n-docosanol, n-hexadecanol, isotridecanol and isooctadecanol.
  • the fatty alcohols mentioned can individually form the basis of the ethylene oxide / propylene oxide addition products.
  • fatty alcohol mixtures being derived from the fatty acid component of fats and oils of animal or vegetable origin.
  • fatty alcohol mixtures can be known from the native fats and oils, u. a. win over the transesterification of the triglycerides with methanol and subsequent catalytic hydrogenation of the fatty acid methyl ester.
  • Both the fatty alcohol mixtures obtained in the production process and suitable fractions with a limited chain length spectrum can serve as the basis for the addition of ethylene oxide and propylene oxide.
  • fatty alcohol mixtures obtained from natural fats and oils synthetically obtained fatty alcohol mixtures, for example the known Ziegler and oxo fatty alcohols, are also suitable as starting materials for the production of the ethylene oxide / propylene oxide addition products defined under a).
  • the polyalkylene glycol part of the adducts mentioned contains on average 1 to 10 moles of ethylene glycol units and 1 to 15 moles of propylene glycol units per mole of fatty alcohol.
  • the molar amounts are so matched that 2 to 25 moles of alkylene glycol units are present per mole of fatty alcohol and that the molar ratio between ethylene glycol and propylene glycol units is in the range from 1: 5 to 2: 1.
  • Products which contain 2 to 6 ethylene glycol units and 4 to 12 propylene glycol units per mole of fatty alcohol and in which the molar ratio between ethylene glycol units and propylene glycol units is in the range from 1: 1 to 1: 2 are preferred.
  • Anionic components come as component b). cationic and ampholytic surfactants, which are known per se as collectors for the flotation of non-sulfidic ores.
  • anionic surfactants are to be used as component b), they are made in particular from fatty acids, alkyl sulfates, alkyl sulfasuccimates, alkyl sulfosuccinamates, alkyl benzene sulfates fonaten alkyl sulfonates, petroleum sulfonates (sarcosides, taurides) and acyl lactylates selected group.
  • Suitable fatty acids are in particular the straight-chain fatty acids with 12 to 18 carbon atoms, in particular those with 16 to 18 carbon atoms, obtained from vegetable or animal fats and oils, for example by fat splitting and optionally fractionation and / or separation by the crosslinking process. Oleic acid and tall oil fatty acid are of particular importance here.
  • Suitable alkyl sulfates are the sulfuric acid half esters of fatty alcohols with 8 to 22 carbon atoms, preferably of fatty alcohols with 12 to 18 carbon atoms, which can be straight-chain or branched.
  • fatty alcohol component of the sulfuric acid half-esters the previous statements regarding the fatty alcohol component of the ethylene oxide / propylene oxide addition products defined under a) apply mutatis mutandis.
  • Suitable alkyl sulfosuccinates are sulfosuccinic acid semiesters of fatty alcohols having 8 to 22 carbon atoms, preferably fatty alcohols having 12 to 18 carbon atoms. These alkyl sulfosuccinates can be obtained, for example, by reacting appropriate fatty alcohols or fatty alcohol mixtures with maleic anhydride and subsequent addition of alkali metal sulfite or alkali metal bisulfite.
  • the information relating to the fatty alcohol component of the ethylene oxide / propylene oxide addition products defined under a) applies analogously.
  • the alkyl sulfosuccinamates considered as possible component b) correspond to the formula I, in the pure alkyl or alkenyl radical having 8 to 22 carbon atoms, preferably having 12 to 18 carbon atoms, R 'is hydrogen or an alkyl radical having 1 to 3 carbon atoms and M is a hydrogen ion, an alkali metal cation, or an ammonium ion, preferably a sodium or ammonium ion .
  • the alkylsulfosuccinamates of the formula 1 are known substances which are obtained, for example, by reacting corresponding primary or secondary amines with maleic anhydride, followed by addition of alkali metal sulfite or alkali metal bisulfite.
  • Primary amines suitable for the preparation of the alkylsulfosuccinamates are, for example, n-octylamine, n-decylamine, n-dodecylamine, n-tetradecylamine, n-hexadecylamine, n-octadecylamine, n-eicosylamine, n-docosylamine, n-hexadecenylamine and n-octadecenylamine.
  • the amines mentioned can individually form the basis of the alkylsulfosuccinamates.
  • amine mixtures are used to prepare the alkylsulfosuccinamates, the alkyl radicals of which come from the fatty acid content of fats and oils of animal or vegetable origin.
  • such amine mixtures can be obtained from the fatty acids of the native fats and oils obtained by fat cleavage via the associated nitriles by reduction with sodium and alcohols or by catalytic hydrogenation.
  • Particularly suitable secondary amines for the preparation of the alkylsulfosuccinamates of the formula are the N-methyl and N-ethyl derivatives of the above-mentioned primary amines.
  • Alkylbenzenesulfonates suitable for use as component b) correspond to formula II, in the pure straight-chain or branched alkyl radical having 4 to 16, preferably 8 to 12 carbon atoms and M represent an alkali metal cation or an ammonium ion, preferably a sodium ion.
  • Alkyl sulfonates which are suitable for use as component b) correspond to formula 111, in which R represents a straight-chain or branched alkyl radical, in particular having 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms, and M represents an alkali metal cation or an ammonium ion, preferably a sodium ion.
  • the petroleum sulfonates suitable for use as component b) were obtained from lubricating oil fractions, generally by sulfonation with sulfur trioxide or oleum.
  • Compounds in which the hydrocarbon radicals predominantly have chain lengths in the range from 8 to 22 carbon atoms are particularly suitable here.
  • the acyl lactylates also considered as possible component b) correspond to the formula IV, in which R is an aliphatic, cycloaliphatic, or alicyclic radical having 7 to 23 carbon atoms and X is a salt-forming cation.
  • R is preferably an aliphatic, linear or branched hydrocarbon radical which can be saturated, mono- or polyunsaturated and optionally substituted by hydroxyl groups.
  • cationic surfactants are to be used as component b), primary aliphatic amines and alkylenediamines substituted with a-branched alkyl radicals or hydroxyalkyl-substituted alkylenediamines and water-soluble acid addition salts of these amines are particularly suitable.
  • Particularly suitable primary aliphatic amines are the fatty amines with 8 to 22 carbon atoms derived from the fatty acids of the native fats and oils, which have already been described above in connection with the alkylsulfosuccinamates also considered as component b).
  • mixtures of fatty amines are generally used, for example tallow amines or hydrotalgamines, such as are obtainable from the tallow fatty acids or the hydrogenated tallow fatty acids via the corresponding nitriles and their hydrogenation.
  • the preparation of the compounds of formula V and their use in flotation is described in DE-A-25 47 987.
  • the aforementioned amine compounds can be used as such or in the form of their water-soluble salts.
  • the salts are optionally obtained by neutralization, which can be carried out both with equimolar amounts and with an excess or an excess of acid.
  • Suitable acids are, for example, sulfuric acid, phosphoric acid, hydrochloric acid, acetic acid and formic acid.
  • ampholytic surfactants which are used according to the invention as component b) are compounds which contain at least one anion-active and one cation-active group in the molecule, the anion-active groups preferably comprising sulfonic acid or carboxyl groups and the cation-active groups preferably comprising amino groups on secondary or tertiary amino groups.
  • Particularly suitable ampholytic surfactants are sarcosides, taurides, N-substituted aminopropionic acids and N- (1,2-dicarboxyethyl) -N-alkylsulfoccinamates.
  • N-substituted aminopropionic acids which are suitable for use as component b) correspond to formula VII in which n can be zero or a number from 1 to 4, while R denotes an alkyl or acyl radical having 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms.
  • the N-substituted aminopropionic acids mentioned are likewise known compounds which can be prepared in a known manner. With regard to their use as collectors in flotation, reference is made to H. Schubart, loc. cit. and on Int. J. Min. Proc. 9 (1982), pp. 353-384, in particular p. 380.
  • N- (1,2-dicarboxyethyl) -N-alkylsulfosuccinamates suitable for use as component b) in the collector mixtures according to the invention correspond to (VIII) in which R is an alkyl radical having 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms, and M is a hydrogen ion, an alkali metal cation or an ammonium ion, preferably a sodium ion.
  • R is an alkyl radical having 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms
  • M is a hydrogen ion, an alkali metal cation or an ammonium ion, preferably a sodium ion.
  • the N- (1,2-dicarboxyethyl) -N-alkylsulfosucinamates mentioned are known Compounds that can be prepared by known methods. The use of these compounds as collectors in flotation is also known, see H Schubert, loc. cit.
  • the weight ratio of components a): b) is in the range from 1:19 to 3: 1, preferably in the range from 1: 4 to 1: 1.
  • collector mixtures to be used according to the invention depend in each case on the type of ores to be floated and on their content of valuable minerals. As a result, the amounts required can vary within wide limits. In general, the collector mixtures according to the invention are used in amounts of 20 to 2000 g per ton of raw ore.
  • the effectiveness of the collectors of the surfactant mixtures to be used according to the invention is practically not impaired by the hardness formers of the water used to produce the slurries.
  • the mixtures of primary collectors and co-collectors to be used according to the invention are used in the known flotation processes for non-sulfidic ores instead of the known anionic, cationic and / or ampholytic collectors.
  • the customary reagents such as foaming agents, regulators, activators, deactivators, etc. are also added to the aqueous slurries of the ground ores.
  • the flotation is carried out under the conditions of the methods of the prior art.
  • the collecting mixtures to be used according to the invention can be used, for example, in the flotation of apatite-scheelite and tungsten ores, in the separation of fluorite from quartz, and in trenches quartz or alkali silicates of hematite, magnetite and chromite by inverse flotation, in the separation of cassiterite from quartz and silicates, and in the separation of oxides of iron and titanium from quartz for cleaning glass sands.
  • the material to be floated consisted of an apatite ore from the South African Phalaborawa complex, which contains the following minerals as main components:
  • the P 2 0 5 content of the ore is 6.4%.
  • the flotation task had the following grain size distribution:
  • the flotation tests were carried out in a laboratory flotation cell (model D-1 from Denver Equipment with a capacity of 1.2 liters) at approx. 20 ° C. Tap water with a hardness of 18 ° dH was used in Examples 1 to 6 to produce the slurries.
  • the slurries for Examples 4 and 6 were prepared using hard water (945 ppm Ca 2+ and 1700 ppm Mg2 +). After the ore had been slurried in the flotation cell, the magnetite was removed with a hand magnet, washed and the washing water returned to the cell.
  • the cloud density was 500 g / l. Water glass in amounts of 1000 and 2000 g / t was used as the trigger.
  • the pH of the turbidity was adjusted to 11 in each case. Flotation was carried out at a speed of rotation of the mixing device of 1500 per minute. The flotation time was 6 minutes. After the pre-flotation (rougher-flotation), the pre-concentrate was cleaned twice, in Examples 3, 4 and 7 collectors being metered in for the first cleaning flotation.
  • Column 2 of Table I below shows the collectors used and their quantities.
  • Column 3 shows the amount of water glass used as a handle.
  • Column 4 says “Magn.” for magnetite separation, "V.-F” for pre-flotation, "RF” for cleaning flotation and "conc.” for concentrate.
  • Column 5 shows the total yield of the respective flotation stage, based on the total amount of ore, in column 6 the P 2 0 5 content of the mountains in the respective process stage and in column 7 the proportion of the P 2 0 5 quantity applied in each process stage of the total amount of P 2 0 5 contained in the ore.
  • the ore to be floated consisted of an apatite ore from Brazil, which contains approx. 20% apatite, approx. 35% magnetite, limonite and hematite as well as approx. 16% calcite.
  • the P 2 0 5 content of the ore is approximately 22%.
  • the flotation task had the following grain size distribution:
  • the flotation tests were carried out under the conditions described for Examples 1 to 8 with the following deviations: Starch was used as the pusher. The pH of the turbidity was 10.5 in each case. The slurries were prepared using tap water with a hardness of 18 0 dH. The iron oxides had been removed by magnetic separation before the apatite flotation.
  • the flotation task had the following grain size distribution:
  • the comparative composition used in Example 22 contained as component a) an adduct of 5 moles of ethylene oxide with one mole of nonylphenol (co-collector D ").
  • the flotation experiments were carried out in a modified Hallimond tube (microflotation cell) according to B. Dobias. Colloid & Polymer Sci. 259 (1981). S. 775-776 at 23 ° C. The individual tests were carried out with 2 g ore each. Distilled water was used to make the slurry. Sufficient collectors and co-collectors were added to the turbidities so that a total collector quantity of 500 g / t was available. The conditioning time was 15 minutes each. During the flotation, an air stream was passed through the slurry at a flow rate of 4 ml / min. The flotation time was 2 minutes in all experiments.
  • the material to be floated consisted of a kaolinite ore from the Upper Palatinate, which contained 55.1% clay and 44.9% feldspar.
  • the flotation task had the following grain size distribution:
  • the flotation experiments were carried out using a Humbold-Wedag laboratory flotation machine from KHD Industrieanlagen AG, Humbold-Wedag, Cologne (see Seifen-Fette-Wachsen 105 (1979), p. 248) using a 1 1 flotation cell. Tap water with a hardness of 18 ° dH was used to produce the cloudiness. The cloud density was 250 g / l. Aluminum sulfate was used as the activator, in each case in an amount of 500 g / t. The pH was adjusted to 3 using sulfuric acid. The conditioning time was 10 minutes. The flotation was carried out at 23 ° C. for 15 minutes and at a rotor speed of 1200 revolutions per minute. The collector was added to the slurries in 3 or 4 aliquots as shown in Table IV below.

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  • Manufacture And Refinement Of Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Detergent Compositions (AREA)
  • Paper (AREA)
  • Physical Water Treatments (AREA)
  • Processing Of Solid Wastes (AREA)
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  • Disintegrating Or Milling (AREA)
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EP86106023A 1985-05-11 1986-05-02 Verwendung von Tensidgemischen als Hilfsmittel für die Flotation von nichtsulfidischen Erzen Expired - Lifetime EP0201815B2 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86106023T ATE65945T1 (de) 1985-05-11 1986-05-02 Verwendung von tensidgemischen als hilfsmittel fuer die flotation von nichtsulfidischen erzen.

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Application Number Priority Date Filing Date Title
DE19853517154 DE3517154A1 (de) 1985-05-11 1985-05-11 Verwendung von tensidgemischen als hilfsmittel fuer die flotation von nichtsulfidischen erzen
DE3517154 1985-05-11

Publications (4)

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EP0201815A2 EP0201815A2 (de) 1986-11-20
EP0201815A3 EP0201815A3 (en) 1989-10-18
EP0201815B1 EP0201815B1 (de) 1991-08-07
EP0201815B2 true EP0201815B2 (de) 1994-08-03

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US (1) US4789466A (tr)
EP (1) EP0201815B2 (tr)
AT (1) ATE65945T1 (tr)
AU (1) AU581512B2 (tr)
BR (1) BR8602081A (tr)
DE (2) DE3517154A1 (tr)
ES (1) ES8900152A1 (tr)
FI (1) FI79952C (tr)
MX (1) MX170350B (tr)
PT (1) PT82561B (tr)
TR (1) TR24023A (tr)
ZA (1) ZA863466B (tr)

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DE3641447A1 (de) * 1986-12-04 1988-06-09 Henkel Kgaa Tensidmischungen als sammler fuer die flotation nichtsulfidischer erze
DE3707034A1 (de) * 1987-03-05 1988-09-15 Henkel Kgaa Verwendung von derivaten des tricyclo-(5.3.1.0(pfeil hoch)2(pfeil hoch)(pfeil hoch),(pfeil hoch)(pfeil hoch)6(pfeil hoch))-decens-3 als schaeumer in der kohle- und erzflotation
EP0298392A3 (de) * 1987-07-07 1991-01-09 Henkel Kommanditgesellschaft auf Aktien Verfahren zur Gewinnung von Mineralen aus sulfidischen aus Erzen durch Flotation und Mittel zu seiner Durchführung
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EP2343131B1 (en) * 2010-01-08 2016-03-30 Université de Lorraine Flotation process for recovering feldspar from a feldspar ore
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BR112015031783A2 (pt) 2013-07-05 2017-07-25 Akzo Nobel Chemicals Int Bv composto; uso de um composto; método para flotação de espuma de minérios não sulfídicos; e polpa
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FI79952B (fi) 1989-12-29
DE3517154A1 (de) 1986-11-13
PT82561B (pt) 1988-03-03
ES8900152A1 (es) 1989-02-16
US4789466A (en) 1988-12-06
FI79952C (fi) 1990-04-10
EP0201815A2 (de) 1986-11-20
FI861953A0 (fi) 1986-05-09
MX170350B (es) 1993-08-18
EP0201815B1 (de) 1991-08-07
DE3680709D1 (de) 1991-09-12
ZA863466B (en) 1986-12-30
AU5731286A (en) 1986-11-13
AU581512B2 (en) 1989-02-23
FI861953A (fi) 1986-11-12
PT82561A (en) 1986-06-01
BR8602081A (pt) 1987-01-06
ES554819A0 (es) 1989-02-16
EP0201815A3 (en) 1989-10-18
TR24023A (tr) 1991-02-01
ATE65945T1 (de) 1991-08-15

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