GB2167397A - Process for selectively removing hydrogen sulphide from gaseous mixtures containing also carbon dioxide - Google Patents

Process for selectively removing hydrogen sulphide from gaseous mixtures containing also carbon dioxide Download PDF

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Publication number
GB2167397A
GB2167397A GB08528409A GB8528409A GB2167397A GB 2167397 A GB2167397 A GB 2167397A GB 08528409 A GB08528409 A GB 08528409A GB 8528409 A GB8528409 A GB 8528409A GB 2167397 A GB2167397 A GB 2167397A
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process according
pressure
column
regeneration
mixture
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GB2167397B (en
GB8528409D0 (en
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Luigi Gazzi
Carlo Rescalli
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SnamProgetti SpA
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SnamProgetti SpA
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    • 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
    • B01D53/14—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 by absorption
    • B01D53/1425—Regeneration of liquid absorbents
    • 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
    • B01D53/14—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 by absorption
    • B01D53/1456—Removing acid components
    • B01D53/1462—Removing mixtures of hydrogen sulfide and carbon dioxide
    • 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
    • B01D53/14—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 by absorption
    • B01D53/1493—Selection of liquid materials for use as absorbents
    • 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
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Gas Separation By Absorption (AREA)
  • Treating Waste Gases (AREA)
  • Industrial Gases (AREA)

Abstract

A process is disclosed for selectively removing hydrogen sulphide from gaseous mixtures also containing carbon dioxide, essentially comprising an absorption in a column by means of a mixture of a tertiary amine and an organic solvent with a water concentration not greater than 25% by weight, and a regeneration in a column for the distillation of the exhausted absorbent mixture, characterized in that said exhausted mixture before being regenerated in the distillation column undergoes a partial regeneration in one or more steps, the separation being obtained of a gas having a CO2/H2S ratio greater than that of the exhausted mixture leaving the absorption column. <IMAGE>

Description

SPECIFICATION Process for selectively removing hydrogen sulphide from gaseous mixtures containing also carbon dioxide The present invention relates to a process for the selective separation of hydrogen sulphide from gaseous mixtures containing also carbon dioxide, by means of a mixture of a tertiary amine and an organic solvent in aqueous solution.
It is known fron the U.K. Patent 2079307 granted on 10.5. 1984 in the same applicant's name the use as the absorption means a mixture of a tertiary amine and of an organic solvent with a water content not higher than 10% by weight.
We illustrate the process being the object of said Patent Application by means of the scheme of attached Fig. 1.
By means of the pipe 1, the gas to be processed is delivered to the absorber 2, to which the absorbent solution is supplied via the pipe 3.
From the top of the absorber 2 the processed gas is drawn via the pipe 4.
The exhausted absorbent solution is discharged from the absorber 2 by means of the pipe 5, is expanded in the valve 6, heated in the heat exchanger 7, and sent to the regeneration column 8 equipped with the reboiler 9.
From the bottom of the column 8 the regenerated solution 10 is sent to the column 2 by the pump 11, after having been colled first in 7 by the exhausted stream 5, and then in 12 by a fan.
From the head of the column 8 the acidic gases 13 containing the H2S absorbed by the solution outcome, and are cooled in 14 and separated in 15 into a liquid stream 16, which is recycled by the pump 17 to the regenerating column 8, and a gas 18 containing H2S.
By the said process the obtainment is possible of a treated gas substantially free from H2S, and of a gaseous stream mainly consisting of H2S and CO2, enriched in H2S relatively to the relative H2S and CO2 amounts in the raw gas.
Whilst for most applications the enrichment in H2S of the acidic gas stream is more than enough, some cases exist in which a higher selectivity may be desirable. Obtaining a higher selectivity is particularly advantageous when the acidic gases must be fed to a Claus plant for sulphur production, to the purpose of reducing the gas volumes fed to the Claus plant. The selectivity is also important when CO2 is to be used (as chemical product, or for alimentary use, or for the raws' assisted recovery), and has hence a value by its own, so that after the selective plant a conventional plant for CO2 recovery is installed; in this case, minimizing the CO2 amount lost together with H2S is obviously advantageous.
The increase in selectivity is usually obtained in the plants operating with aqueous tertiary amines, with a second selective treatment, i.e. by using the so-called "concentrator" plant. In such a plant, the stream of acidic gases is processed again, producing a still more concentrated H2S stream. This of course requires considerable additional investment expenses and involves greater consumptions of related utilities.
One of the reasons why the concentrator plant is particularly burdensome is the fact that the acidic gas stream is produced at a pressure slightly higher than the atmospheric pressure, so that also the reabsorption of H2S in the concentrator plant occurres at a slightly super-atmospheric pressure, and hence under particularly disadvantageous conditions. On the other hand, recompressing the whole acidic gas stream would result too expensive.
We have found a process allowing the selectivity in H2S removal from the gas mixture containing also C,02 to be increased.
The process being the object of the present invention, comprising essentially an absorption in a column by means of a tertiary amine and of an organic solvent with a water content not greater than 25% by weight and a regeneration in a distillation column of the exhausted absorbent mixture, is characterized in that said exhausted absorbent mixture is submitted, before being regenerated in the distillation column, to a partial regeneration in one or more steps, the separation being obtained of a gas having a CO2/H2S ratio greater than that of the exhausted mixture leaving the absorption column.
The gas as obtained from the partial regeneration can be recycled to the main absorption column, or to another absorption column.
The partial regeneration can be carried out by expansion or by heating or by stripping, or by means of one or more exhausting columns, or by means of a suitable combination of these treatments, and can be repeated a suitable number of times. The regeneration steps may be equal to or different from each other.
The partial regeneration by expansion consists in expanding the exhausted solution to an intermediate pressure between the absorption pressure and the regeneration pressure, and separating the gases formed.
This process may be repeated more than once, greater selectivities being obtained with a greater number of intermediate expansions.
It has been found however that the selectivity increase decreases when passing from the second to the third expansion, so that in practive providing more than three intermediate expansions in series between the absorber and the regeneration column is not suitable.
The partial regeneration by heating consists in a heating of the exhausted mixture, e.g., by using the heat of the mixture regenerated in the regeneration column, and in the separation of used gases.
The heating occurs under the pressure of the absorption column, or at an intermediate pressure between the absorption pressure and the regeneration pressure.
The partial regeneration by means of one or more exhausting columns, is carried out by operating under the same pressure as of the absorption column, or under a pressure intermediate between the absorption pressure and the regeneration pressure.
Another possible embodiment of the invention consists in allowing a slight heating between the expansion and the separation, thus a further selectivity increase being obtained.
This heating is of the order of 5-25 C, according to the selectivity increase desired, and to the number of expansion stages used. If more than one stages are used, it is generally convenient a higher heating degree before the first stage, the subsequent heatings being lower and lower.
The partial regeneration by stripping consists in stripping the exhausted mixture with a H2S-free gaseous mixture, operating under the same pressure as of the absorption pressure, or under an intermediate pressure between the absorption and the regeneration pressures.
As examples of gas streams which can be used to that purpose, we can mention fuel gas or the nitrogen available from the air fractionation unit in the plants for synthesis gas production by partial oxidation.
These gas streams may be used as well in the strippers and in the exhausting column, in addition to the heat action, in the nearby of the reboiler, or immediately above, or some trays under the same reboiler, in an additional adiabatic stripping column.
The partial regeneration may comprise also an intermediate heating inside the exhausting column and/or the stripping column.
All these systems, besides improving the selectivity of H2S relatively to CO2, have also another advantage: the heavy hydrocarbons are noticeably reduced, by being co-absorbed with H2S in the exhausted solution, if they are present in the raw gas. It is known that these heavy hydrocarbons, when present in the supply to the Claus plant, can impair the quality of sulphur, in particular the colour thereof.
According to another embodiment of the present invention, the gases obtained from the partial regeneration in the expansion stages, are compressed to the pressure of the highest partial regeneration stage and H2S is reabsorbed with a portion of the regenerated mixture. A CO2 stream substantially free from H2S becomes hence available for possible uses.
The tertiary amines which can be used either individually or as mixtures with each other are dimethylethanolamine, ethyldiethanolamine, propyldiethanolamine, dipropylethanolamine, isopropyldiethanolamine, diisopropylethanolamine, methyldiisopropanolamine, ethyldiisopropanolamine, propyldiisopropanolamine, isopropyldiisopropanolamine, N-methylmorpholine.
The solvents which may be used either individually or as mixtures with each other as components of the solution are sulpholane, Nmethylpyrrolidone, N-methyl-3-morpholone, dialkylethermonoethyleneglycols, dialkyletherpolyethyleneglycols (wherein each one of the alkyl groups contains from 1 to 4 carbon atoms), N,N-dumethylformamide, N-formylmorpholine, N,N-dimethylimidazolin-2-one and N-methylimidazole.
The invention shall be now better disclosed with the aid of the flow charts of Figs 2, 3, 4, 5, 6, 7 and 8 hereto attached, representing embodiments preferred, but which are not to be considered as limitative of the invention itself.
The flow chart of fig. 2 represents a process provided with three partial regeneration steps, constituted by an expansion in valve, under a pressure. intermediate between the absorber pressure and the regeneration column pressure, and subsequent separation of developed gases, which are recycled to the absorber.
By means of the pipe 1 the gas to be treated is sent to the absorption column 2, to which the absorption solution too is fed via the pipe 3. Within the column 2, which can be equipped with trays, or with a packing of conventional type, the gas to be processed and the absorption solution flow in countercurrent to selectively remove H2S.
From the top of the column 2 the treated gas (hydrocarbons+CO2) is drawn by the pipe 4.
The exhausted absorption solution is discharged from the column 2 through the pipe 5 and is partly regenerated in three steps, by expansion in the valves 19, 20 and 21 and separation in the separators 22, 23 and 24.
From the top of the separators 22, 23 and 24 three gas streams 25, 26 and 27 come out, with CO2/H2S ratios greater than the streams 5, and decreasing relatively to each other.
The stream 27 is compressed in 28 to the same pressure as of the stream 26, and is combined with the same; the formed mixture 29 is compressed in 30 to the pressure as of the stream 25, and is combined with it; the next mixture formed 31 is compressed in 32 to the pressure as of the absorber 2 and is recycled by 33 to the same absorber.
The liquid streams 34 and 35 leaving from the separators 22 and 23 are respectively sent into the separators 23 and 24, whilst the liquid stream 36 leaving from the separator 24 is first expanded in the valve 37, then preheated in the heat exchanger 7, and finally fed to the distillation column 8 provided with the reboiler 9 to complete the regeneration.
From the bottom of the column 8 the re generated solution 10 is sent to the column 2 by means of the pump 11, after having been first cooled in 7 with the partly regenerated stream 36 and then air-cooled by means of the fan 12.
From the head of the column 8 there come out the acidic gases 13 containing the H2S absorbed by the solution, which gases are cooled by means of the fan 14, and are sent into the separator 15 from whose botton a liquid stream 16 is drawn and recycled to the regeneration column by means of the pump 17, From the head of the separator 15 a H2Scontaining gas 18 comes out.
The flow chart of fig. 3 represents a process having three partial regeneration steps constituted each by a heating, by an expansion in valve and by a separation of the developed gases, which are recycled to the absorber.
Relatively to the flow chart of fig. 1, the additional exchangers 38, 39 and 40 are provided, which respectively heat the streams 5, 34 and 35 after having been expanded in valve.
The heat is supplied by the regenerated solution 10 before being recycled to the absorber 2.
In fig. 4 a partial regeneration step is shown, which uses an exhausting column.
The exhausted solution 5 enters the exhausting column 41 from whose bottom a stream 42 is drawn, a portion 43 of which is heated in 44 by thermal exchange, e.g., with the regenerated solution 10, whilst the remaining portion 45 is sent to a second partial regeneration stage or to the regeneration column.
From the head of the column 41 a gas stream 46 enriched in CO2 comes out.
In fig. 5 the partial regeneration step using s stripping column is used.
The exhausted solution 5 enters the stripping column 47 into the bottom of which a gas stream in fed by means of the pipe 48. From the head of the stripper a gas 49 enriched in CO2 comes out, whilst from the bottom a stream 50 is drawn and is sent to a second partial regeneration step or to the regeneration column.
The flow chart of fig. 6 represents a process provided with two regeneration stages wherein the first stage is an exhausting column, and the second one is constituted by an expansion, a heating and a separation.
The exhausted solution 5 coming out of the absorber 2 is fed, after having been expanded in 6, to the exhausting column 41, from whose bottom a solution 42 comes out, which is partly (43) recycled to the same column, after having been heated in 44 by means of the regenerated solution 10, and partly (45) is expanded in the valve 21, heated in 40 and separated in 24. From the bottom of the separator 24 a liquid stream 36 in drawn and is sent, as in preceding schemes, to the regeneration column 8; from the head of the separator a gas 27 leaves which is compressed in 28 to the pressure of the exhausting column 41 and recycled to the same column.
H2S in the column 41 is reabsorbed by a portion of the regenerated solution 10, i.e., the stream 51, so that from the head a stream 46 containing CO2 and substantially free from H2S comes out.
The flow chart of fig. 7 represents a process simplified relatively to the preceding process, having two regeneration stages, wherein the first stage is an exhausting column operating under the same pressure as of the absorption column, and the second is constituted by an expansion, a heating and a separation.
The exhausted solution 5 coming out of the absorber 2 is partly (43) recycled to the absorber 2, after having been heated in 44 by means of the regenerated solution 10, partly (45) expanded in the valve 21, heated in 40 and separated in 24. From the bottom of the separator 24 a liquid stream 36 is drawn and is sent to the regeneration column 8 similarly to the preceding schemes, whilst from the head a gas 27 comes out, which is compressed in 28 to the pressure of the column 2 and is then recycled to the same column.
The flow chart of fig. 8 represents a process with two absorption columns and with a partial regeneration stage constituted by an expansion, a heating and a separation.
The solution 5 leaving the absorber 2 after having been expanded in 6 and heated in 52 with the regenerated solution 10 is fed to a second absorber 53, from whose bottom comes out a solution 54, which is expanded in 23, heated in 40 and separated 24.
From the bottom of the separator 24 a liquid stream 36 is drawn which is sent, similarly to the preceding schemes, to the regeneration column 8; from the head of the separator 24 a gas 27 comes out, which is compressed in 28 to the pressure of the absorber 53, and recycled to the same absorber.
The H2S in the absorber 53 is reabsorbed by the stream 51, which is a portion of the regenerated solution 10, so that from the head a stream 55 of CO2 substantially free from H2S comes out.
As Example is now supplied to the purpose of better illustrating the invention, which example should not be considered as a limitation to the same invention. Said Example shall be followed by a Comparison Example.
Example 1 A natural gas, available under 56 kg/cm2, with 4.5% by volume of H2S and 64% by volume of CO2 is treated with a dimethylethanolamine solution at 40% by weight, of Nmethylpyrrolidone at 50% by weight and water (10%) by weight), according to the pro cess as schematically shown in fig. 8.
There are obtained a purified gas with less than 1 ppm of H2S, a stream of acidic gases containing 71.93% by volume of H2S, a stream of CO2 with less than 1 ppm of H2S under a pressure of 15 kg/cm3, representing 11.6% of the CO, contained in the raw gas.
(Comparison) Example 2 The same natural gas is treated according to the process as schematically shown in fig.
1 (known art), with the same type of solution, a purified gas being obtained with less than 1 ppm of H2S, and a stream of acidic gases being obtained, containing about 32.65% by volume of H2S. It can be noticed hence that, besides yielding a stream of CO, substantially free from H2S, the process claimed according to the present Patent Application yields a stream of acidic gases containing 71.93% by volume of H2S, with a decrease of the volume of gases fed to the Claus process of 2.2 times relatively to the known art.
Attention is drawn to the related application filed by us on the same day as the present application.

Claims (20)

1. A process for selectively removing hydrogen sulphide from a gaseous mixture also containing carbon dioxide, which comprises subjecting the gaseous mixture to absorption in a column by means of a mixture of a tertiary amine and of an organic solvent with a water content not greater than 25% by weight, and subjecting the exhausted absorbing mixture to regeneration in a distillation column; wherein the tertiary amine is selected from one or more of dimethylethanolamine, ethyldiethanolamine, propyldiethanolamine, dipropylethanolamine, isopropyldiethanolamine, diisopropylethanolamine, methyldiisopropanolamine, ethyldiisopropanolamine, propyldiisopropanolamine, isopropyldiisopropanolamine and N-methylmorpholine; wherein the organic solvent is selected from one or more of sulpholane, N-methylpyrrolidone, N-methyl-3-morpholone, dialkylethermonoethyleneglycols, dialkyletherpolyethyleneglycols, N,N-dimethylformamide, N-formylmorpholine, N,N-dimethylimidazolin-2-one and N-methylimidazole; and wherein the exhausted absorbing mixture is submitted, before being regenerated in the distillation column, to a partial regeneration in one or more stages thereby to obtain the separation of a gas having a Cho2: H2S ratio greater than the exhausted absorbing mixture from the absorption column.
2. A process according to claim 1, wherein the gas obtained from the partial regeneration is recycled to the absorption column.
3. A process according to claim 1 or 2, wherein the partial regeneration is effected by expansion.
4. A process according to claim 1 or 2, wherein the partial regeneration is effected by heating.
5. A process according to claim 1 or 2, wherein the partial regeneration is effected by stripping.
6. A process according to claim 1 or 2, wherein the partial regeneration is effected by the use of one or more exhausting columns.
7. A process according to claim 1 or 2, wherein the partial regeneration is effected by expansion and/or by heating and/or by stripping and/or by the use of one or more exhausting columns.
8. A process according to claim 7, wherein the number of stages of partial regeneration is from 1 to 3.
9. A process according to claim 3, wherein the partial regeneration by expansion consists in expanding in a valve the exhausted mixture to a pressure intermediate the absorption pressure and the regeneration pressure, and in separating the gas formed.
10. A process according to claim 4, wherein the partial regeneration by heating consists in heating the exhausted mixture and in separating the resulting gas.
11. A process according to claim 10, wherein the heating is effected by using the heat of the regenerated mixture.
12. A process according to claim 10 or 11, wherein the heating is effected under the pressure of the absorption column, or under a pressure intermediate the absorption pressure and the regeneration pressure.
13. A process according to claim 12, wherein the exhausting column operates under the same pressure as the absorption column, or under a pressure intermediate the absorption pressure and the regeneration pressure.
14. A process according to claim 5, wherein the partial regeneration by stripping consists in stripping the exhausted mixture with a H2S-free gas stream.
15. A process according to claim 14, wherein the stripping is effected under the same pressure as the absorption column or under a pressure intermediate the absorption pressure and the regeneration pressure.
16. A process according to claim 13, wherein stripping gas is fed to the exhausting column in the vicinity of a reboiler, or immediately above the reboiler, or to one or more plates under the reboiler.
17. A process according to any of claims 1 to 16, wherein the partial regeneration stages are the same as or different from each other.
18. A process according to claim 12 and/ or claim 14, wherein the partial regeneration also comprises a heating step upstream of the exhausting column and/or of the stripping operation.
19. A process according to claim 3, wherein the gases obtained from the partial regeneration in the expansion stages are com pressed to the pressure of the highest partial regeneration stage, the H2S contained therein being then reabsorbed with a portion of the regenerated mixture.
20. A process according to claim 1, substantially as hereinbefore described with reference to any of Figs. 2 to 8 of the drawings.
GB08528409A 1984-11-26 1985-11-19 Process for selectively removing hydrogen sulphide from gaseous mixtures containing also carbon dioxide Expired GB2167397B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
IT23739/84A IT1177324B (en) 1984-11-26 1984-11-26 PROCEDURE FOR SELECTIVELY REMOVING HYDROGEN SULFUR FROM GASEOUS MIXTURES CONTAINING ALSO CARBON DIOXIDE

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GB8528409D0 GB8528409D0 (en) 1985-12-24
GB2167397A true GB2167397A (en) 1986-05-29
GB2167397B GB2167397B (en) 1988-03-30

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AU (1) AU5005185A (en)
BR (1) BR8506058A (en)
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DE (1) DE3541775A1 (en)
DK (1) DK544185A (en)
ES (1) ES8607181A1 (en)
FR (1) FR2573671A1 (en)
GB (1) GB2167397B (en)
HU (1) HUT41994A (en)
IT (1) IT1177324B (en)
NL (1) NL8503265A (en)
NO (1) NO162218C (en)
NZ (1) NZ214165A (en)
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SE (1) SE8505463L (en)

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EP0348251A1 (en) * 1988-05-24 1989-12-27 Elf Aquitaine Production Liquid absorbant of acid gases containing a tertiary alcanolamin compound and an absorption activator for CO2 and its use for the deacidification of CO2 and possibly other acid gases
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US6342091B1 (en) * 1999-01-22 2002-01-29 Krupp Uhde Gmbh Method of removing carbon dioxide, sulphur compounds, water and aromatic and higher aliphatic hydrocarbons from industrial gases
US6203599B1 (en) 1999-07-28 2001-03-20 Union Carbide Chemicals & Plastics Technology Corporation Process for the removal of gas contaminants from a product gas using polyethylene glycols
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US7674325B2 (en) 2003-09-09 2010-03-09 Fluor Technologies Corporation Solvent use and regeneration
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DK544185A (en) 1986-05-27
HUT41994A (en) 1987-06-29
NO162218B (en) 1989-08-21
NZ214165A (en) 1988-03-30
NL8503265A (en) 1986-06-16
AU5005185A (en) 1986-06-05
IT8423739A0 (en) 1984-11-26
NO162218C (en) 1989-11-29
JPS61136421A (en) 1986-06-24
DE3541775A1 (en) 1986-05-28
DD241015A5 (en) 1986-11-26
PL256454A1 (en) 1986-09-23
ES8607181A1 (en) 1986-05-16
DE3541775C2 (en) 1987-03-05
SE8505463L (en) 1986-05-27
IT1177324B (en) 1987-08-26
ES549798A0 (en) 1986-05-16
GB2167397B (en) 1988-03-30
BR8506058A (en) 1986-08-19
NO854680L (en) 1986-05-27
DK544185D0 (en) 1985-11-25
FR2573671A1 (en) 1986-05-30
GB8528409D0 (en) 1985-12-24
SE8505463D0 (en) 1985-11-19

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