EP0103528B1 - Verfahren zur Behandlung von Rohöl vor dessen atmosphärischer Destillation - Google Patents

Verfahren zur Behandlung von Rohöl vor dessen atmosphärischer Destillation Download PDF

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Publication number
EP0103528B1
EP0103528B1 EP19830401798 EP83401798A EP0103528B1 EP 0103528 B1 EP0103528 B1 EP 0103528B1 EP 19830401798 EP19830401798 EP 19830401798 EP 83401798 A EP83401798 A EP 83401798A EP 0103528 B1 EP0103528 B1 EP 0103528B1
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Prior art keywords
crude oil
process according
solvent
water
carbon atoms
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Expired
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EP19830401798
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English (en)
French (fr)
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EP0103528A1 (de
Inventor
Claude Scherrer
Michel Laborde
Claude Baumann
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Compagnie Francaise de Raffinage SA
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Compagnie Francaise de Raffinage SA
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step

Definitions

  • the present invention relates to a process for treating a crude oil prior to its distillation at atmospheric pressure.
  • crude oil is understood to mean both oil coming directly from a deposit and dilute heavy crude oil, or synthetic crude oil, that is to say reconstituted from fractions of hydrocarbons, obtained from hydrocarbon products that may have undergone treatments (crude oil, heavy oils, bituminous shales, coal).
  • the invention relates in particular to a process for treating a crude oil whose density at 15.6 ° C, expressed in API degrees, is between 20 and 40, which corresponds to a density at 15 ° C between approximately 0.934 g / ml and 0.825 g / ml.
  • the upper limit of this 40 ° API range corresponds to a light crude oil, in which asphaltenes are generally scarce, while the lower limit of 20 ° API corresponds to the density of the heaviest crude oils generally treated in conventional refinery desalters.
  • the invention also relates to a method for treating a crude oil whose density at 15.6 ° C is less than 20 ° API.
  • the treatment according to the invention is applied to said crude oil after addition of a diluent such as a light gasoline, also called "fluxing agent", the proportion of which can be between 0 and 50% of the volume of the oil. gross depending on the case.
  • crude oil received by refineries, contains many impurities consisting of water, salts dissolved in water, as well as solid particles, which it is necessary to remove, to avoid as much corrosion of material and dirt deposits (solids or sludge) in storage tanks and refinery processing units as possible.
  • the salts contained in crude oil thus pass into solution in water.
  • the emulsion is then conducted to a desalter, where the water and crude oil separate.
  • a high voltage electrostatic field can be created in the desalter, to accelerate the coalescence of the water droplets.
  • This desalting operation leads to the production of a "water phase”, that is to say an aqueous layer, containing in particular salts in solution, which separates at the bottom of the desalter, and a “Crude phase” means a layer of crude oil that forms at the top of the desalter.
  • a stable emulsion can also form, under certain conditions, at the interface of the water phase and the raw phase.
  • This stable emulsion constitutes a phase separated from the water phase and the crude phase; it cannot be resolved under the temperature conditions prevailing in a desalter without specific provisions.
  • This stable emulsion can contain approximately 49 to 19% by weight of crude oil, 50 to 80% by weight of water, and 1% by weight of insoluble products.
  • These insoluble products consist of approximately 50 to 70% by weight of mineral compounds, and in particular of iron compounds (oxides, sulfides), and 50 to 30% of organic compounds (asphaltenes, carbenes).
  • Asphaltenes and carbenes are bituminous compounds soluble in carbon sulphide, the carbenes being insoluble in hot benzene, while the asphaltenes are soluble there. Asphaltenes are, depending on the temperature, partially soluble in crude oil, while carbenes are insoluble in it.
  • the “stable emulsion” is of the “water in oil” type, the water droplets being dispersed in crude oil.
  • the insoluble products are concentrated on the periphery and inside the water droplets and it is important that these droplets are not entrained by the desalted crude oil, because otherwise the insoluble products would deposit in the preheating exchangers of the desalinated crude oil preceding the furnace through which the desalinated crude oil passes before its distillation. This would result in rapid fouling of the exchangers, with the consequence of the need for frequent maintenance operations and an increase in the consumption of the fuel necessary to heat the crude oil in the furnace.
  • the crude oil coming from desalting is in fact generally subjected, then, to a distillation at atmospheric pressure, which leads to the production of a gas phase, various distillates and an atmospheric residue.
  • crude oil still contains sodium chloride, calcium chloride and magnesium chloride.
  • sodium chloride which is stable
  • calcium chloride and magnesium chloride are hydrolyzed sés by steam at a temperature above about 120 ° C and thus give rise to hydrochloric acid, which is concentrated in the overhead vapors, then in the condensing water.
  • Crude oil, after stabilization, contains practically no hydrogen sulphide in the dissolved state; on the other hand, the cracking of sulfur derivatives, which occurs during distillation, gives rise to hydrogen sulphide, which also concentrates in the head vapors of the column.
  • a neutralizing agent such as ammonia in the gaseous phase or in aqueous solution is therefore usually injected into the condensation line of the water which joins the head of the column. in the condenser, or in a reflux circulating at the top of the distillation column. This injection is intended to maintain the pH of the condensation water at a determined value or, more precisely, to maintain the variations in pH within a determined range.
  • vacuum distillation The residue from atmospheric distillation is then itself subjected to distillation under reduced pressure, called vacuum distillation, which makes it possible to separate a heavy diesel fuel, various cuts of distillates, which can serve as raw materials, for example, for lubricating oils. and cracking methods, and a vacuum residue.
  • This vacuum residue which can be used to prepare lubricants, contains asphalt in varying concentrations. It can therefore be subjected to a deasphalting operation by adding an appropriate solvent, such as propane, which precipitates the asphalt or pitch, while the deasphalted oil is recovered, the solvent being finally separated as well. deasphalted oil only from recovered pitch.
  • an appropriate solvent such as propane
  • the mechanism of this fouling is complex and varied; it can be caused by accumulations of oxidation products, deposits of asphaltenes, salts, or by scaling phenomena.
  • the deposits are made up for 50 to 70% by weight of mineral compounds, in particular iron compounds (oxides, sulfides) and for 50 to 30% of organic compounds (asphaltenes, carbenes). They can also be organic compounds which polymerize under the action of heat, oxides or oxygen dissolved in crude oil.
  • anti-fouling agents partially remedies this drawback.
  • the antifouling agent is a chemical which is added to the load at very low concentrations, of the order of a few parts per million by volume.
  • Many types of antifouling agents have already been proposed, such as, for example, agents based on phosphorus esters or else based on sulfosuccinates (see, for example, French patent No. 2421958, the holder of which is joint holder).
  • This deasphalting operation using superheated steam also causes the formation of a stable and difficult to resolve emulsion, and generally leads to the presence of large amounts of water in the effluent charge, which can be harmful during subsequent treatments. Finally, this operation must often be supplemented by an additional deasphalting treatment with solvent, which is also expensive.
  • the present invention aims to overcome these drawbacks using a process for treating a crude oil, characterized in that, prior to its atmospheric distillation, said crude oil is successively subjected to at least one desalting operation. in the liquid phase, then in at least one deasphalting operation, by treatment of the desalted crude oil using an appropriate deasphalting solvent.
  • the licensee has in fact established that the desalting operation in the liquid phase, prior to that of deasphalting, can be carried out economically at temperatures below 160 ° C., and makes it possible to remove not only the salts present in the charge to be treated, but also the quantities of water contained in the crude to be treated, thus avoiding the formation of a third liquid phase during of the subsequent deasphalting operation and to further improve the recovery of deasphalting pitches, since most of the mineral salts have been removed from the batch to be treated during the desalting operation.
  • the present invention further aims to limit the fouling of equipment in petroleum refineries and, in particular, heat exchangers and thus to increase their efficiency in considerable proportions.
  • the invention also aims to reduce the corrosion of the preheating exchangers and of the condensation devices and zones at the top of the atmospheric distillation columns, by limiting the risk of acid compounds being formed during the treatment of the charge.
  • the invention aims to obtain better quality atmospheric distillation residues, by elimination, before distillation, of most of the metals present in the feed.
  • the desalting operation can be carried out in a manner known per se, for example as described in the aforementioned French patent No. 2388037, by first adding to the crude oil a first demulsifier, for example based on oxide copolymer of ethylene and propylene, then adding a quantity of water representing 2 to 10% by volume of crude oil. This mixture is then introduced into an electrostatic desalter where the temperature is maintained below about 160 ° C. and preferably 135 ° C., in order to avoid too great an electrical conductivity due to the oxygenated and nitrogenous products present in the charge.
  • a first demulsifier for example based on oxide copolymer of ethylene and propylene
  • the desalting operation can be brought to a slightly higher temperature, without however exceeding 160 ° C., when the API viscosity of the crude decreases.
  • the pressure in the desalter can be between 1 and 20 bar.
  • a second demulsifying agent such as di-2 ethylhexyl sodium sulfosuccinate, is injected into the desalter.
  • a water phase is removed from this desalter, containing most of the sodium chloride, as well as other salts such as calcium and magnesium salts, and a desalinated crude oil phase is recovered, containing a small amount of water and salts, mainly sodium chloride, as well as asphaltenes, a fraction of which is in suspension.
  • a deasphalting solvent consisting, for example, of a cut of hydrocarbons with 3 and 4 carbon atoms or a gas condensate from a crude oil or gas production field, is introduced into the crude oil. i.e. a section obtained directly by condensation on the production field and which may contain, in variable quantities, hydrocarbons having between 3 and 7 carbon atoms or more), in an amount representing from 100 to 500% by volume and, preferably, from 100 to 250%, compared to crude oil.
  • the deasphalting solvent will be devoid of water.
  • the water which is suspended in the crude oil after desalting will largely dissolve in the solvent, which will result in an increase in the salt concentration of the undissolved water.
  • the specific mass of the water droplets present in crude oil will therefore increase, which, as will be explained in more detail in the remainder of this description, will favor the elimination with the pitch of the salt remaining in the charge, at the outcome of deasphalting, resulting in better desalination of crude oil.
  • this mixture After mixing the deasphalting solvent and the crude oil, this mixture will be introduced into a deasphalting installation, in which the pitch precipitates and separates from the crude. There is thus recovered, by usual techniques, a mixture of pitch and solvent, which are then separated in a conventional manner, and a mixture of deasphalted crude oil and solvent, also separated by known techniques.
  • an anti-fouling agent such as di-2. sodium ethylhexyl sulfosuccinate, as described in French patent No. 2421958. Indeed, while with such an anti-fouling agent, the fouling speed of the exchangers is usually reduced by approximately 50%, the treatment in accordance with invention further reduces this fouling rate due to the elimination of asphaltenes and salts prior to atmospheric distillation.
  • the atmospheric distillation residue has reduced Conradson carbon (Conradson carbon is measured according to AFNOR NFT 60-116 standard) and reduced heavy metals (vanadium, nickel, etc.) and contains practically no more alkali metals. and alkaline earth.
  • Conradson carbon is measured according to AFNOR NFT 60-116 standard
  • reduced heavy metals vanadium, nickel, etc.
  • This atmospheric distillation residue can therefore be subjected directly to a catalytic cracking, due to an acceptable content of contaminants.
  • the treatment according to the invention can be applied to a crude oil with density, expressed in API degrees, between 20 and 40. It is also possible to apply it also to heavier oils by adding a diluent such as a light gasoline also called "fluxing", representing from 0 to 50% of the volume of the crude oil, before the desalting operation and, more precisely, before the incorporation of the first demulsifying agent.
  • a diluent such as a light gasoline also called "fluxing” representing from 0 to 50% of the volume of the crude oil, before the desalting operation and, more precisely, before the incorporation of the first demulsifying agent.
  • the crude oil to be treated is first subjected to a desalting phase in an electrostatic desalter 1, which is supplied by a line 2 equipped with a pump 3.
  • Water intended to dissolve the salts present in the crude oil, is introduced via line 5 into line 2, in an amount representing from 2 to 10% by volume of the crude oil.
  • Preliminary is injected into line 2, through line 4, a first demulsifier, for example based on a copolymer of ethylene and propylene oxides, intended to promote the resolution of the unstable emulsion of petroleum and water which is introduced into the desalter.
  • the pump 3 continuously introduces into the desalter 1 the mixture of crude oil, water and first demulsifier. This mixture remains in the desalter between 20 min and 1 h, at a temperature below 160 ° C and preferably at 135 ° C.
  • the unstable emulsion is resolved there into a “water phase” 6 and a “raw phase” 7 which are drawn off continuously, respectively by lines 8 and 9.
  • An intermediate phase constituted by a stable emulsion of water in crude oil, can however form at the interface of phases 6 and 7 and, to resolve this stable emulsion, we inject into the desalter, via line 2 ', above the level of the interface of phases 6 and 7, a second demulsifying agent such as di-2 ethylhexyl sodium sulfosuccinate.
  • the desalted crude oil which is removed from the desalter by line 9 contains, in total, 0.4 to 0.7% by volume of water, of which 0.3 to 0.6% in suspension. It also contains 3 to 50 p.p.m. of various salts, most of which consists of sodium chloride. Finally, asphaltenes which have already precipitated are present there in suspension at a content of approximately 100 to 500 p.p.m.
  • a deasphalting solvent in an amount representing from 100 to 500% by volume of the crude oil and, preferably, from 100 to 250%, and the resulting mixture is introduced into a static mixer 11 .
  • the deasphalting solvent can consist of a cut of hydrocarbons with 4 carbon atoms, of a cut of hydrocarbons with 3 and 4 carbon atoms or alternatively of condensates obtained during the production of gas on production fields. of crude oil or gas, these condensates generally containing from 20 to 30% by volume of hydrocarbons with 3 carbon atoms, 20 to 30% of hydrocarbons with 4 carbon atoms, the remainder consisting mainly of 5 carbon atoms.
  • the deasphalting solvent should preferably be dry, in order to promote additional desalting of the crude oil during the deasphalting operation.
  • the mixture of crude oil and deasphalting solvent leaving the mixer 11 is evacuated by a line 12 to a deasphalting installation 13, where it remains for 15 to 30 min, at a temperature between 80 and 135 ° C and at a pressure between 30 and 50 bar, when operating with sections of hydrocarbons with 3 carbon atoms, or of hydrocarbons with 3 and 4 carbon atoms.
  • this temperature can be from 100 to 250 ° C and the pressure between 30 and 50 bar insofar as the condensate contains significant proportions of hydrocarbons at 5 carbon atoms or more.
  • a phase 14 is separated, consisting of pitch and solvent, which is discharged by line 15 and separated into 16 into solvent and pitch, discharged respectively by lines 17 and 18
  • a mixture 20 of deasphalted crude oil and of solvent is also recovered via line 19, which can be separated into 21 into solvent, discharged via line 22, and into deasphalted crude oil, discharged through line 23.
  • the mixture can be sent directly to line 23.
  • Fig. 2 illustrates in more detail the deasphalting operation, in the case where the solvent consists of a cut of hydrocarbons with 4 carbon atoms (part A of the diagram in FIG. 1).
  • the mixture of desalted crude oil and solvent arriving via line 112 is separated in the deasphalting installation 113 into a phase 114, consisting of pitch soaked in solvent, which is discharged through line 115, and into a phase 116, constituted of deasphalted crude oil and solvent, which is evacuated via line 117.
  • the mixture of pitch and solvent is heated in an oven 118 and a "flash" distillation then makes it possible, in 119, to separate the pitch, which is recovers via line 120, and the solvent, which uses line 121.
  • the mixture of deasphalted crude oil and of solvent is separated at 122 and the deasphalted crude oil is recovered by line 123 and, by line 124, to which line 21 is connected, coming from “flash” distillation 119 , solvent.
  • This one is subjected, in 125, to a new distillation, and one recovers, by line 126, a cut of hydrocarbons with 4 carbon atoms, dry, recycled on line 10 (cf. fig. 1) , and via line 127, hydrocarbons with 3 and less than 3 carbon atoms, which can be brought to line 28 of column 27, after condensation.
  • the amount of Conradson carbon removed with pitch can reach 90% of the total weight of Conradson carbon present in petroleum before deasphalting. Likewise, most of the metals present, the presence of which is particularly harmful to conversion catalysts, such as catalytic cracking catalysts, is eliminated with pitch.
  • the deasphalting operation results in more complete desalting of the crude oil.
  • the solubility of water in hydrocarbons with 4 carbon atoms, at 130 ° C, being 0.7% by weight part of the water will pass into the dry deasphalting solvent.
  • the concentration of the salts in the remaining water will therefore increase, resulting in a higher specific mass of this water, and the droplets of this heavier water will be eliminated with pitch during the deasphalting.
  • These drops of water will be all the more easily removed as it is well known that they tend to surround themselves with a film of asphaltenes.
  • the residue from the atmospheric distillation (line 30 in Fig. 1) of the desalted and deasphalted crude oil obtained by the process according to the invention is particularly suitable as feedstock for a catalytic cracking unit, because of the small amount of contaminants that 'it contains.
  • the flow of line 30 can be mixed everywhere or part of the flow of lines 29c and 29b.
  • the process which has just been described can be applied to a crude oil of 20 to 40 API. It can also be optionally applied to heavier petroleum, that is to say API degree less than 20, by incorporating it through line 31 (fig. 1), prior to any other treatment, that is that is, upstream of the injection of the first demulsifier, a light diluting essence, which can represent up to 50% by volume of crude oil.
  • a first demulsifier 10 p.p.m. of a first demulsifier is injected continuously into the charge, based on a copolymer of ethylene and propylene oxides, and 8% by volume of water based on crude oil.
  • the desalter temperature is 130 ° C and the residence time of the crude oil is 20 min.
  • Desalinated crude oil now contains only 40 mg / I of salts (expressed as sodium chloride), but contains 0.6% by volume of water.
  • the desalting rate, after deasphalting, is therefore 97% and the rate of removal of heavy metals (vanadium, nickel) is greater than 97%.
  • Desalting is carried out under the following conditions: 7 ppm of a first demulsifier is continuously injected into the feed, based on a copolymer of ethylene and propylene oxides, and 7% by volume of water based on crude oil .
  • the desalter temperature is 130 ° C and the residence time of the crude oil is 20 min.
  • the desalting rate, after deasphalting, is therefore 98% and the rate of removal of heavy metals (vanadium, nickel) is greater than 90%.
  • the yield of pitch recovered is 10%. This pitch has a softening point of 130 ° C.
  • Example 2 The same operations are repeated as in Example 2, on the same charge and under the same conditions, but varying the level of the deasphalting solvent.
  • the results obtained for various levels of solvent appear in the following table:
  • This table shows that by varying the rate of deasphalting solvent, it is possible to adjust the content of various contaminants of the treated oil and the pitch yield as desired.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Claims (10)

1. Verfahren zur Behandlung eines Rohöls, dadurch gekennzeichnet, dass das Rohöl vor seiner Destillation bei Atmosphärendruck aufeinanderfolgend mindestens einer Entsalzung in flüssiger Phase und anschliessend mindestens einer Entasphaltierung durch Behandlung des entsalzten Rohöls mittels eines geeigneten Entasphaltierungslösungsmittels unterworfen wird.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Entsalzung in flüssiger Phase in einem elektrostatischen Entsalzer durchgeführt wird, welcher auf einer Temperatur niedriger als 160° C und auf einem Druck zwischen 1 und 20 bar gehalten wird.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Entsalzung in Gegenwart eines Entemulgiermittels durchgeführt wird.
4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass es sich beim Entemulgiermittel um Di-(2-äthyl-hexyl)-natriumsulfosuccinat handelt.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass ein wasserarmes Entasphaltierungslösungsmittel verwendet wird.
6. Verfahren nach Anspruch 1 oder 5, dadurch gekennzeichnet, dass das Entasphaltierungslösungsmittel im wesentlichen aus einer Fraktion von Kohlenwasserstoffen mit 4 Kohlenstoffatomen oder einer Fraktion von Kohlenwasserstoffen mit 3 und 4 Kohlenstoffatomen oder Kondensaten der Gase von Rohöl- oder Gasproduktionsfeldern besteht.
7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass die Entasphaltierung in einer Anlage bei einer Temperatur zwischen 80° C und 135° C, wenn es sich beim Lösungsmittel um eine Fraktion von Kohlenwasserstoffen mit 3 Kohlenstoffatomen oder mit 3 oder 4 Kohlenstoffatomen handelt, bzw. bei einer Temperatur zwischen 100° C und 250° C, wenn es sich beim Lösungsmittel um ein Kondensat eines Gases von Feldern handelt, und unter einem Druck zwischen 30 und 50 bar mit einer Verweilzeit zwischen 15 und 30 Minuten durchgeführt wird.
8. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass dem Rohöl vor jeglicher Behandlung ein Verdünnungsleichtbenzin zugesetzt wird, wenn das Rohöl einen API-Grad kleiner als 20 aufweist.
9. Verfahren nach Anspruch 8, dadurch gekennzeichnet, dass das Verdünnungsbenzin 0 bis 50 Vol.-% vom Rohöl ausmacht.
10. Anwendung des Verfahrens nach einem der Ansprüche 1 bis 9 zur Herstellung einer Charge für das katalytische Cracken.
EP19830401798 1982-09-14 1983-09-14 Verfahren zur Behandlung von Rohöl vor dessen atmosphärischer Destillation Expired EP0103528B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8215501 1982-09-14
FR8215501A FR2532946A1 (fr) 1982-09-14 1982-09-14 Procede de traitement d'un petrole brut prealablement a sa distillation a pression atmospherique

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EP0103528A1 EP0103528A1 (de) 1984-03-21
EP0103528B1 true EP0103528B1 (de) 1985-07-24

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EP (1) EP0103528B1 (de)
JP (1) JPS5974185A (de)
DE (2) DE103528T1 (de)
FR (1) FR2532946A1 (de)

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Publication number Priority date Publication date Assignee Title
JP2576006B2 (ja) * 1992-10-26 1997-01-29 三菱重工業株式会社 発電方法
US5948242A (en) * 1997-10-15 1999-09-07 Unipure Corporation Process for upgrading heavy crude oil production
US20140317998A1 (en) * 2013-04-30 2014-10-30 Pall Corporation Methods and systems for processing crude oil
US8981174B2 (en) * 2013-04-30 2015-03-17 Pall Corporation Methods and systems for processing crude oil using cross-flow filtration

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE342766A (de) *
NL7214542A (de) * 1971-11-10 1973-05-14
FR2388037A1 (fr) * 1977-04-20 1978-11-17 Raffinage Cie Francaise Procede perfectionne de dessalage du petrole brut et dispositifs de mise en oeuvre dudit procede
FR2489835B1 (fr) * 1980-09-08 1986-03-14 Elf France Pretraitement de bruts lourds par viscoreduction directe

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FR2532946A1 (fr) 1984-03-16
JPS5974185A (ja) 1984-04-26
DE103528T1 (de) 1984-09-27
DE3360440D1 (en) 1985-08-29
EP0103528A1 (de) 1984-03-21

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