EP0600923B1 - Process for producing synthetic or fuel gasses from solid or pasty residues and waste or low-grade fuels in a gasifying reactor - Google Patents
Process for producing synthetic or fuel gasses from solid or pasty residues and waste or low-grade fuels in a gasifying reactor Download PDFInfo
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- EP0600923B1 EP0600923B1 EP92916028A EP92916028A EP0600923B1 EP 0600923 B1 EP0600923 B1 EP 0600923B1 EP 92916028 A EP92916028 A EP 92916028A EP 92916028 A EP92916028 A EP 92916028A EP 0600923 B1 EP0600923 B1 EP 0600923B1
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- gas
- fraction
- gasifying reactor
- gasification
- solid
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/58—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels combined with pre-distillation of the fuel
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/58—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels combined with pre-distillation of the fuel
- C10J3/60—Processes
- C10J3/64—Processes with decomposition of the distillation products
- C10J3/66—Processes with decomposition of the distillation products by introducing them into the gasification zone
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/16—Integration of gasification processes with another plant or parts within the plant
- C10J2300/1603—Integration of gasification processes with another plant or parts within the plant with gas treatment
- C10J2300/1606—Combustion processes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/16—Integration of gasification processes with another plant or parts within the plant
- C10J2300/164—Integration of gasification processes with another plant or parts within the plant with conversion of synthesis gas
- C10J2300/1643—Conversion of synthesis gas to energy
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/18—Details of the gasification process, e.g. loops, autothermal operation
- C10J2300/1807—Recycle loops, e.g. gas, solids, heating medium, water
Definitions
- the invention relates to a method according to the preamble of patent claim 1.
- the disposal of carbon-containing waste materials of varying composition, such as domestic and industrial waste, is known from EP-A3-0 120 397.
- the aim of this process is the production of fuel gas.
- the carbon-containing waste material is smoldered in a rotary tube reactor above 200 ° C to obtain a carbonization gas and a pyrolysis coke.
- the pyrolysis coke is then gasified in a fluidized bed or fluidized bed gasifier.
- the gasification products leave the carburetor at relatively low Temperatures between 400 ° C and 1000 ° C.
- the liquid and gaseous components released from the smoldering stage and the gasification stage are subsequently burned, while the ashes that have to be disposed of have to be disposed of. -
- This process is unsatisfactory for environmentally friendly disposal of the input materials, since both the final incineration and the disposal of the ashes lead to new environmental problems.
- a process similar to that described in EP 0 120 397 A3 is also known from WO 90/02162, in which essentially the same problems as described in connection with EP 0 120 397 A3 arise.
- both the pyrolysis step and the gasification step are carried out allothermally.
- WO 90/02162 also provides for the combustion of the solid gasification residue in a gasification residue combustion chamber, the step of burning the gasification residue being an essential step for the overall process.
- the process management there aims at a particularly advantageous use of heat within the overall process, and in order to provide sufficient quantities of heat in the individual process stages, it is also intended to supply the process with coal as well as waste as a raw material.
- the object of the invention is to ensure the most environmentally compatible disposal of residues and waste materials which are difficult to handle and contain organic constituents, in particular the light shredder fraction, in the recycling of motor vehicles, and thereby to obtain a synthesis gas.
- a mechanical and thermal (drying) pretreatment of the biomass is carried out.
- a combined process of entrained flow pyrolysis takes place and entrained-flow gasification, both of which are carried out in the so-called downdraft, the entrained-flow pyrolysis taking place in an outer zone and the gasification in an inner zone of a common, concentrically constructed entrained-flow reactor in which the pyrolysis is carried out at a temperature of up to 1600 ° F, corresponding to 870 ° C is done.
- the temperature of the pyrolysis step is therefore extremely high.
- the hot carrier gas for pyrolysis also contains water vapor and CO 2 .
- GB-A-2 109 400 which describes synthesis gas production from a fibrous biomass, such as wood chips.
- a so-called slurry gasification is carried out after a pyrolytic pretreatment of the starting material.
- This type of gasification requires a relatively high liquid carrier content of approx. 40%.
- the gasification apparently takes place at relatively low process temperatures, namely below the ash softening.
- This known process is not very suitable for feedstocks of the type that are to be disposed of in accordance with the present invention.
- Gasification reactors operating according to the entrained flow principle are well known and therefore do not require any special description at this point; reference is made, for example, to DE-C2 27 21 047 and EP-B1-0 011 151. Grain bandwidths of approximately 0.001 mm to 5 mm are used for use in so-called entrained flow gasifiers.
- the particle size of the solid fraction obtained after the pyrolysis treatment stage according to the invention is adjusted after the pyrolysis treatment and before the entrained flow gasification by grinding, sieving and / or sifting, the particle size range being reduced.
- the gas fraction obtained after the pyrolysis treatment stage is preferably first subjected to a condensation step.
- the gas fraction obtained after the coding stage is then further used in the synthesis gas production process according to the invention.
- this gas fraction is fed to the gasification reactor or the pyrolysis treatment stage for introducing heat for the endothermic pyrolysis or gasification step or admixed to the product gas obtained behind the gasification reactor as part of the synthesis gas.
- the liquid fraction obtained after the condensation stage can possibly be used in another process, but is preferably used in the gasification reactor for gasification and / or supplied for the introduction of heat for the endothermic gasification process.
- the solid fraction obtained after the pyrolysis treatment stage and the liquid fraction obtained after the condensation stage are mixed and fed together to the gasification reactor, a pump or a screw machine being used, depending on the consistency of the mixture. Suitable funding bodies and procedures for this are known from DE-C2-27 21 047 and EP-B1-0 011 151 as examples.
- the gasification is generally carried out under a pressure of preferably 10 to 100 bar. Basically, higher gasification pressures are possible.
- the gasification can also be carried out at atmospheric pressure or in a slightly reduced pressure (if suction fans are used).
- Fig. 1 is a block diagram.
- FIG. 1 The block diagram shown in FIG. 1 is explained below in connection with the use of an entrained-flow gasification reactor. Alternative procedures are shown in dashed lines. Process steps that are preferably used are additionally outlined with a dashed line.
- a residual or waste material containing organic constituents hereinafter referred to as feed material
- a pyrolysis treatment stage 101 such as an indirectly heated rotary kiln (drum wall temperature up to 900 ° C.).
- the feed material is pretreated, largely without oxygen, with the addition of heat and essentially avoiding the burning of constituents of the feed material at temperatures between approximately 300 and 650 ° C.
- extraneous gas, product gas accumulating behind the gasification reactor 102 and / or pyrolysis gas accumulating behind a condensation stage 103 downstream of the pyrolysis stage, preferably accumulating in a pyrolysis gas purification stage 104 can be used.
- the intermediate product obtained in the pyrolysis treatment stage 101 from the starting material is discharged separately as steam (gas fraction) and coke (solid fraction).
- the solid fraction is adjusted, if necessary after setting the grain size range in a grinding, sieving and / or classifying stage 105, to the level which is compatible with the respective gasification reactor type (gasification reactor 102), and the gasification reactor 102, e.g. B. pneumatically supplied.
- Recyclables contained in the solid fraction, e.g. Metals can be separated in a separation stage 106, e.g. a screening device, before the solid fraction is fed to the gasification reactor 102.
- the gas fraction obtained behind the pyrolysis treatment stage 101 is either fed as vapor to the gasification reactor for the gasification and / or introduction of heat of reaction or is first passed through a condensation stage 103.
- the residual gas deposited therein, which is obtained under the condensation conditions, is fed to the pyrolysis treatment stage for introducing process heat either, preferably after passing through a pyrolysis gas purification stage 104.
- the pyrolysis gas can be supplied to the gasification reactor 102 or the product gas stream occurring behind it to introduce gasification heat. In these cases, a pyrolysis gas cleaning stage may not be necessary.
- the oil (liquid fraction) obtained behind the condensation stage 103 is recycled in other processes or, as is preferred, introduced into the gasification reactor 102. Especially when this oil is to be gasified together with the solid fraction from the pyrolysis treatment stage 101, the two fractions can first be combined and fed to the gasification reactor 102 by means of a pump or screw machine 107.
- the product gas obtained behind the gasification reactor 102 will generally be cleaned in a gas cleaning stage 108.
- the constituents removed from the product gas can be fed to the gasification reactor 102 at least as a partial stream, so that they are divided there into product gas or inorganic constituents.
- enriched harmful gas components such as sulfur, salts and heavy metals can be reused.
- the product gas obtained behind the gas purification stage 108 can, as is preferred, be fired in a power plant 109, which may be already present, or, if appropriate partially, in the pyrolysis treatment stage 101 or used as synthesis gas or other fuel gas.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Gasification And Melting Of Waste (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren gemäß dem Oberbegriff des Patentanspruchs 1.The invention relates to a method according to the preamble of patent claim 1.
Da das Deponieren fester oder pastöser Rest- und Abfallstoffe nicht weiter vertretbar ist, gewinnt die Verwertung dieser Stoffe zunehmend an Bedeutung. Zu diesen Stoffen zählen z. B. Shredder-Leichtgut von Kraftfahrzeugen, Kunststoffe, Öl-, Lack- und Lösungsmittelschlämme, teilentwässerte Klärschlämme und viele andere mehr. Diesen Stoffen ist gemeinsam, daß sie organische Bestandteile enthalten.Since the deposition of solid or pasty residues and waste materials is no longer justifiable, the recycling of these materials is becoming increasingly important. These substances include e.g. B. Shredder light goods from motor vehicles, plastics, oil, paint and solvent sludges, partially dewatered sewage sludges and many others. These substances have in common that they contain organic components.
Versuche mit sogenannten Schachtvergasern haben gezeigt, daß bei der Hochtemperaturvergasung einer Reihe von Einsatzstoffen, wie z.B. der Shredderleichtfraktion aus der Kraftfahrzeug-Verwertung erhebliche Probleme auftreten; insbesondere ist es in manchen Fällen und insbesondere bei der Shredderleichtfraktion aus der Kfz-Verwertung schwierig, dieses Chargiergut so gleichmäßig in die Vergasungszone, d.h. speziell in den Primärgasraum einzubringen, daß das Produktgas eine ausreichend gleichmäßige Qualität hat. Zur Lösung dieses Problems sind bisher nicht veröffentlichte Bemühungen unternommen worden, den Einsatzstoff zu brikettieren, um ihn dann in einer stückigen Form durch konventionelle Schleusensysteme dem Schachtvergaser aufzugeben. Die Brikettierung als solche erwies sich aber als sehr aufwendig und derzeit noch nicht ausgereift genug.Experiments with so-called shaft gasifiers have shown that in high-temperature gasification a number of feedstocks, e.g. the shredder light fraction from motor vehicle recycling encounter considerable problems; in particular, it is difficult in some cases, and in particular in the case of the light shredder fraction from motor vehicle recycling, to feed this cargo evenly into the gasification zone, i.e. to be introduced specifically into the primary gas space so that the product gas has a sufficiently uniform quality. To solve this problem, previously unpublished efforts have been made to briquette the feedstock and then to give it to the shaft gasifier in a lumpy form by conventional lock systems. The briquetting as such turned out to be very complex and not yet mature enough.
Auch ein anderer bisher nicht veröffentlichter Lösungsansatz hat nicht zum Erfolg geführt. Gemäß diesem Lösungsansatz wird der Einsatzstoff gemahlen, wie es z.B. für den Einsatz von Brennstoffen in einem Flugstromvergasungsreaktor bekannt ist. Diese Mahlung erweist sich insoweit als problematisch, als verschleißintensive Stoffe, wie Glas, Steine, Eisen und andere in dem Rest- oder Abfallstoff enthalten sein können. Außerdem ist diese Vorgehensweise sehr kostenintensiv.Another previously unpublished solution has also not led to success. According to this approach, the feed is milled, e.g. is known for the use of fuels in an entrained-flow gasification reactor. This grinding proves to be problematic insofar as wear-intensive substances such as glass, stones, iron and others can be contained in the residual or waste material. This procedure is also very expensive.
Die Entsorgung von kohlenstoffhaltigen Abfallstoffen wechselnder Zusammensetzung, wie Hausmüll und Industriemüll ist aus der EP-A3-0 120 397 bekannt. Ziel dieses Verfahrens ist die Herstellung von Brenngas. Zu diesem Zweck wird der kohlenstoffhaltige Abfallstoff in einem Drehrohrreaktor oberhalb von 200° C unter Gewinnung eines Schwelgases und eines Pyrolysekokses geschwelt. Nachfolgend wird der Pyrolysekoks in einem Fließbett oder Wirbelschichtvergaser vergast. Die Vergasungsprodukte verlassen den Vergaser bei relativ niedrigen Temperaturen zwischen 400° C und 1000° C. Die aus der Schwelstufe und der Vergasungsstufe freigesetzten flüssigen und gasförmigen Bestandteile werden nachfolgend verbrannt, während die anfallende Asche entsorgt werden muß. - Dieses Verfahren ist für eine umweltverträgliche Entsorgung der Einsatzstoffe nicht befriedigend, da sowohl die abschließende Verbrennung als auch die Entsorgung der anfallenden Asche zu neuen Umweltproblemen führt.The disposal of carbon-containing waste materials of varying composition, such as domestic and industrial waste, is known from EP-A3-0 120 397. The aim of this process is the production of fuel gas. For this purpose, the carbon-containing waste material is smoldered in a rotary tube reactor above 200 ° C to obtain a carbonization gas and a pyrolysis coke. The pyrolysis coke is then gasified in a fluidized bed or fluidized bed gasifier. The gasification products leave the carburetor at relatively low Temperatures between 400 ° C and 1000 ° C. The liquid and gaseous components released from the smoldering stage and the gasification stage are subsequently burned, while the ashes that have to be disposed of have to be disposed of. - This process is unsatisfactory for environmentally friendly disposal of the input materials, since both the final incineration and the disposal of the ashes lead to new environmental problems.
Ein ähnlicher Prozeß, wie er in der EP 0 120 397 A3 beschrieben ist, ist ferner aus der WO 90/02162 bekannt, bei dem sich im Kern die gleichen Probleme wie im Zusammenhang mit der EP 0 120 397 A3 beschrieben wurden, ergeben. Bei dem aus der WO 90/02162 bekannten Prozeß werden nämlich sowohl der Pyrolyseschritt als auch der Vergasungsschritt allotherm durchgeführt. Außerdem sieht die WO 90/02162 ein Verbrennen des festen Vergasungsreststoffes in einer Vergasungsreststoff-Brennkammer vor, wobei der Schritt der Verbrennung des Vergasungsreststoffes ein für den Gesamtprozeß wesentlicher Schritt ist. Die dortige Verfahrensführung zielt neben der Herstellung eines Synthesegases auf eine besonders vorteilhafte Wärmenutzung innerhalb des Gesamtprozesses ab, wobei zur Bereitstellung ausreichender Wärmemengen in den einzelnen Prozeßstufen es vorgesehen ist, dem Prozeß außer Müll als Einsatzstoff auch Kohle zuzuführen.A process similar to that described in EP 0 120 397 A3 is also known from WO 90/02162, in which essentially the same problems as described in connection with EP 0 120 397 A3 arise. In the process known from WO 90/02162, both the pyrolysis step and the gasification step are carried out allothermally. WO 90/02162 also provides for the combustion of the solid gasification residue in a gasification residue combustion chamber, the step of burning the gasification residue being an essential step for the overall process. In addition to the production of a synthesis gas, the process management there aims at a particularly advantageous use of heat within the overall process, and in order to provide sufficient quantities of heat in the individual process stages, it is also intended to supply the process with coal as well as waste as a raw material.
Davon ausgehend liegt der Erfindung die Aufgabe zugrunde, eine möglichst umweltverträgliche Entsorgung schwierig zu handhabender, organische Bestandteile enthaltender Rest- und Abfallstoffe insbesondere der Shredderleichtfraktion bei der Kraftfahrzeug-Verwertung zu gewährleisten und dabei ein Synthesegas zu gewinnen.Proceeding from this, the object of the invention is to ensure the most environmentally compatible disposal of residues and waste materials which are difficult to handle and contain organic constituents, in particular the light shredder fraction, in the recycling of motor vehicles, and thereby to obtain a synthesis gas.
Zur Lösung dieser Aufgabe wird das Verfahren mit den Merkmalen des Patentanspruchs 1 vorgeschlagen.To achieve this object, the method with the features of claim 1 is proposed.
Durch die Erfindung wird eine Reihe bedeutsamer Vorteile erreicht. Hierzu zählen u.a.:
- Bei dem thermischen Vorbehandlungsschritt (Pyrolysebehandlungsschritt) des Einsatzstoffes fallen die Gasfraktion und die Festfraktion, insbesondere dann, wenn es sich bei dem Einsatzstoff um eine Shredderleichtfraktion handelt, in einem Mengenverhältnis an brenn- bzw. vergasbaren Material an wie es zum Betrieb eines Flugstromvergasungsreaktors erforderlich ist (etwa 60 % Gasfraktion und etwa 40 % Festfraktion); ein Zufeuern anderer Brennstoffe in einem Primärgasbrenner ist daher so gut wie nicht erforderlich;
- die Festfraktion aus der thermischen Vorbehandlung hat Eigenschaften wie etwa ein Hüttenkoks; deshalb kann bei der Vergasung auf den Einsatz von z.B. Hüttenkoks ganz verzichtet werden, so daß das feste Chargiergut nur noch aus der Festfraktion des thermisch behandelten Einsatzstoffes besteht;
- bei der erfindungsgemäßen Vergasung der Einsatzstoffe fallen Umweltgifte wie Dioxine und Stickoxide nicht an, da die Dioxine bei der unter unterstöchiometrischen Bedingungen durchgeführten Vergasung nicht existieren können und bei den relativ hohen Vergasungstemperaturen zerstört werden; Stickoxide aus der Primärgasverbrennung werden unter den Vergasungsbedingungen reduziert; außerdem weisen etwa anfallende Metalloxide einen im Vergleich zu anderen Verwertungsverfahren geringeren Oxidationsgrad auf und sind somit weniger toxisch;
- in dem Einsatzstoff enthaltene Ballaststoffe, wie z.B. Metalle können nach dem thermischen Vorbehandlungsschritt aus der Festfraktion durch einen üblichen Trennschritt abgeschieden werden, bevor die Festfraktion dem Vergasungsreaktor als Chargiergut aufgegeben wird;
- der Eintrag des festen Chargiergutes in den Vergasungsreaktor wird wesentlich vereinfacht und vergleichmäßigt.
- In the thermal pretreatment step (pyrolysis treatment step) of the feedstock, the gas fraction and the solid fraction, in particular if the feedstock is a light shredder fraction, are obtained in a quantity ratio of combustible or gasifiable material as is required to operate an entrained-flow gasification reactor ( about 60% gas fraction and about 40% solid fraction); adding other fuels in a primary gas burner is therefore hardly necessary;
- the solid fraction from the thermal pretreatment has properties such as that of a cottage coke; Therefore, the use of, for example, smelting coke can be dispensed with entirely in the gasification, so that the solid charge only consists of the solid fraction of the thermally treated feedstock;
- In the gasification of the feedstocks according to the invention, environmental toxins such as dioxins and nitrogen oxides do not occur, since the dioxins cannot exist in the gasification carried out under substoichiometric conditions and are destroyed at the relatively high gasification temperatures; Nitrogen oxides from primary gas combustion are reduced under the gasification conditions; in addition, metal oxides that occur have a lower degree of oxidation than other recycling methods and are therefore less toxic;
- Dietary fibers contained in the feed, such as metals, can be separated from the solid fraction by a conventional separation step after the thermal pretreatment step before the solid fraction is fed to the gasification reactor as a charge;
- the entry of the solid charge in the gasification reactor is considerably simplified and evened out.
Überraschenderweise hat sich herausgestellt, daß die durch die Erfindung erreichbaren Vorteile mit den bekannten Entsorgungsverfahren, die - wie in der EP-A1-0 120 397 beschrieben - die Vergasung in der Wirbelschicht durchführen, d.h. in einem definierten stationären bis zirkulierenden Fließbett nicht erzielt werden. Bei diesen bekannten Entsorgungsverfahren entsteht ein fester Rückstand, insbesondere eine nach der Wirbelschicht abgeschiedene Zyklonasche, die zumeist höhere Anteile (z.B. 5%) an nichtreagiertem Kohlenstoff enthält und die nach den heutigen strengeren Umweltgesetzen nicht mehr deponiert werden darf. Dieser Rückstand hat den Nachteil, daß nicht vergaste feste Schadstoffe sehr leicht eluierbar sind.Surprisingly, it has been found that the advantages which can be achieved by the invention with the known disposal methods which, as described in EP-A1-0 120 397, carry out the gasification in the fluidized bed, i.e. cannot be achieved in a defined stationary to circulating fluid bed. In these known disposal methods, a solid residue is formed, in particular a cyclone ash separated after the fluidized bed, which mostly contains higher proportions (e.g. 5%) of unreacted carbon and which, according to today's stricter environmental laws, may no longer be disposed of. This residue has the disadvantage that solid gases which are not gasified can be eluted very easily.
Es hat sich auch ferner herausgestellt, daß nicht jede beliebige Kombination zwischen Pyrolysebehandlung von zu entsorgendem Material und anschließender Vergasung im Flugstrom den erheblichen Erfolg erzielt, der von der vorliegend beanspruchten Erfindung erzielt wird. Insbesondere ist der in der US-A-4,497,637 beschriebene Entsorgungsprozeß weder für derart heterogene Einsatzstoffe, wie sie gemäß der vorliegenden Erfindung entsorgt werden sollen, geeignet, noch ist es damit möglich, eine solche Entsorgung in der erwünschten umweltverträglichen Weise durchzuführen. Bei diesem bekannten Verfahren wird Synthesegas aus einer Biomasse hergestellt; hierzu zählt die US-A-4,497,637 Holzspäne, Sägemehl und ähnliches von Bäumen und anderen Landpflanzen, Algen, land- und forstwirtschaftliche Rückstände und Abfälle, den kohlehaltigen Anteil von kommunalen Abfällen und Ähnliches. Zunächst wird eine mechanische und thermische (Trocknung) Vorbehandlung der Biomasse vorgenommen. Nach der Vorbehandlung erfolgt ein kombinierter Prozeß aus Flugstrompyrolyse und Flugstromvergasung, die beide im sogenannten Fallstrom durchgeführt werden, wobei die Flugstrompyrolyse in einer äußeren Zone stattfindet und die Vergasung in einer inneren Zone eines gemeinsamen, konzentrisch aufgebauten Flugstromreaktors, in welchem die Pyrolyse bei einer Temperatur von bis zu 1600° F, entsprechend 870° C erfolgt. Damit liegt die Temperatur des Pyrolyseschritts extrem hoch. Außerdem enthält das heiße Trägergas für die Pyrolyse neben Stickstoff auch Wasserdampf und CO2. In Verbindung mit dem zwischen 1 und 5 Atmosphären liegenden Reaktionsdruck in der Flugstrom-Pyrolysekammer werden mithin Verfahrensbedingungen erreicht, bei denen bereits eine Vergasung der mechanisch und thermisch vorbehandelten Biomasse einsetzt. - Abgesehen von der aufwendigen Vorbehandlung und dem im Vergleich zur Shredderleichtfraktion aus der Kraftfahrzeug-Verwertung relativ einfach zu handhabenden Biomasse ist dieses Verfahren wegen seiner besonderen Prozeßführung in den kombinierten Pyrolyse/Vergasung-Flugstromreaktor mit dem Konzept der vorliegenden Erfindung nicht vergleichbar.It has also been found that not every combination between pyrolysis treatment of material to be disposed of and subsequent gasification in the entrained flow achieves the considerable success achieved by the presently claimed invention. In particular, the disposal process described in US Pat. No. 4,497,637 is neither suitable for such heterogeneous starting materials as are to be disposed of in accordance with the present invention, nor is it possible to carry out such disposal in the desired environmentally compatible manner. In this known method, synthesis gas is produced from a biomass; this includes US-A-4,497,637 wood shavings, sawdust and the like from trees and other land plants, algae, agricultural and forestry residues and waste, the coal-containing fraction of municipal waste and the like. First, a mechanical and thermal (drying) pretreatment of the biomass is carried out. After the pretreatment, a combined process of entrained flow pyrolysis takes place and entrained-flow gasification, both of which are carried out in the so-called downdraft, the entrained-flow pyrolysis taking place in an outer zone and the gasification in an inner zone of a common, concentrically constructed entrained-flow reactor in which the pyrolysis is carried out at a temperature of up to 1600 ° F, corresponding to 870 ° C is done. The temperature of the pyrolysis step is therefore extremely high. In addition to nitrogen, the hot carrier gas for pyrolysis also contains water vapor and CO 2 . In connection with the reaction pressure between 1 and 5 atmospheres in the entrained-flow pyrolysis chamber, process conditions are achieved in which gasification of the mechanically and thermally pretreated biomass already begins. - Apart from the complex pretreatment and the biomass which is relatively easy to handle compared to the shredder light fraction from motor vehicle recycling, this method cannot be compared with the concept of the present invention because of its special process management in the combined pyrolysis / gasification entrained flow reactor.
Ähnliches gilt für die GB-A-2 109 400, die eine Synthesegasherstellung aus einer fasrigen Biomasse, wie Holzspänen, beschreibt. Hierbei wird im Anschluß an eine pyrolytische Vorbehandlung des Einsatzstoffes eine sogenannte Slurry-Vergasung durchgeführt. Bei dieser Art von Vergasung wird ein relativ hoher flüssiger Trägeranteil von ca. 40 % benötigt. Die Vergasung läuft offenbar bei relativ geringen Prozeßtemperaturen, nämlich unterhalb der Ascheerweichung ab. Dieser bekannte Prozeß ist für Einsatzstoffe derjenigen Art, wie sie gemäß vorliegender Erfindung entsorgt werden sollen, nur wenig geeignet.The same applies to GB-
Auch andere Kombinationsverfahren zur Entsorgung kohlenstoffhaltiger Einsatzstoffe gehen von Verfahrenskonzepten aus, die den in vorliegender Erfindung gestellten Anforderungen nicht gerecht werden: So ist es aus der WO 81/00112 bekannt, bituminöse Steinkohlen, Braunkohlen, Holz, Stroh und dergleichen nach einer vorgeschalteten Drehrohrpyrolyse in einem gekoppelten Crack- und Schachtvergasungs-Prozeß unter teilweiser Verbrennung des Schwelkokses aus der Pyrolysestufe weiterzubehandeln. - Schwierige Einsatzstoffe, wie sie gemäß vorliegender Erfindung entsorgt werden sollen, können in diesem bekannten Kombinationsprozeß nicht mit dem gewünschten Ergebnis behandelt werden.Other combination processes for the disposal of carbon-containing feedstocks also start from process concepts which do not meet the requirements set out in the present invention: this is the case in WO 81/00112 known to further treat bituminous hard coal, lignite, wood, straw and the like after an upstream rotary tube pyrolysis in a coupled cracking and shaft gasification process with partial combustion of the coke from the pyrolysis stage. - Difficult feedstocks, as they should be disposed of according to the present invention, can not be treated with the desired result in this known combination process.
Nach dem Flugstromprinzip arbeitende Vergasungsreaktoren (Flugstromvergaser) sind hinreichend bekannt und bedürfen daher an dieser Stelle keiner besonderen Beschreibung; beispielhaft sei auf die DE-C2 27 21 047 und EP-B1-0 011 151 Bezug genommen. Für die Verwendung in sogenannten Flugstromvergasern werden Körnungsbandbreiten von etwa 0,001mm bis 5mm eingesetzt. Die hinter der erfindungsgemäßen Pyrolysebehandlungsstufe anfallende Festfraktion wird nach der Pyrolysebehandlung und vor der Flugstromvergasung hinsichtlich ihrer Körnungsbandbreite durch Mahlen, Sieben und/oder Sichten eingestellt, wobei die Körnungsbandbreite verringert wird.Gasification reactors operating according to the entrained flow principle (entrained flow gasifiers) are well known and therefore do not require any special description at this point; reference is made, for example, to DE-C2 27 21 047 and EP-B1-0 011 151. Grain bandwidths of approximately 0.001 mm to 5 mm are used for use in so-called entrained flow gasifiers. The particle size of the solid fraction obtained after the pyrolysis treatment stage according to the invention is adjusted after the pyrolysis treatment and before the entrained flow gasification by grinding, sieving and / or sifting, the particle size range being reduced.
Bevorzugt wird die hinter der Pyrolysebehandlungsstufe anfallende Gasfraktion zunächst einem Kondensationsschritt unterworfen. Die hinter der Kodensationsstufe anfallende Gasfraktion wird dann in dem erfindungsgemäßen Herstellungsprozeß von Synthesegasen weiterverwertet. Hierzu wird diese Gasfraktion dem Vergasungsreaktor oder der Pyrolysebehandlungsstufe zur Einbringung von Wärme für den endothermen Pyrolyse- bzw. Vergasungsschritt zugeführt oder dem hinter dem Vergasungsreaktor anfallenden Produktgas als Teil des Synthesegases beigemischt.The gas fraction obtained after the pyrolysis treatment stage is preferably first subjected to a condensation step. The gas fraction obtained after the coding stage is then further used in the synthesis gas production process according to the invention. For this purpose, this gas fraction is fed to the gasification reactor or the pyrolysis treatment stage for introducing heat for the endothermic pyrolysis or gasification step or admixed to the product gas obtained behind the gasification reactor as part of the synthesis gas.
Die hinter der Kondensationsstufe anfallende Flüssigfraktion kann ggf. in einem anderen Prozeß verwertet werden, wird aber vorzugsweise dem Vergasungsreaktor zur Vergasung und/ oder zur Einbringung von Wärme für den endothermen Vergasungsprozeß zugeführt. Hierbei werden nach einer bevorzugten Ausführungsform der Erfindung die hinter der Pyrolysebehandlungsstufe anfallende Festfraktion und die hinter der Kondensationsstufe anfallende Flüssigfraktion gemischt und dem Vergasungsreaktor gemeinsam zugeführt, wobei je nach Konsistenz des Gemisches vorzugsweise eine Pumpe oder eine Schneckenmaschine verwendet werden. Hierfür geeignete Förderorgane und Verfahrensweisen sind aus der DE-C2-27 21 047 und EP-B1-0 011 151 beispielhaft bekannt.The liquid fraction obtained after the condensation stage can possibly be used in another process, but is preferably used in the gasification reactor for gasification and / or supplied for the introduction of heat for the endothermic gasification process. According to a preferred embodiment of the invention, the solid fraction obtained after the pyrolysis treatment stage and the liquid fraction obtained after the condensation stage are mixed and fed together to the gasification reactor, a pump or a screw machine being used, depending on the consistency of the mixture. Suitable funding bodies and procedures for this are known from DE-C2-27 21 047 and EP-B1-0 011 151 as examples.
Eine besonders vorteilhafte Verwendung der erfindungsgemäß hergestellten Gase ergibt sich aus Anspruch 7.A particularly advantageous use of the gases produced according to the invention results from claim 7.
Es ist auch möglich, dem Einsatzstoff anorganische Rest- oder Abfallstoffe beizumischen, um darin enthaltene kontaminierende Substanzen in der Pyrolysebehandlungsstufe oder in der Vergasungssstufe aus dem Rest- oder Abfallstoff zu entfernen.It is also possible to add inorganic residues or waste materials to the feedstock in order to remove contaminating substances contained therein from the residue or waste material in the pyrolysis treatment stage or in the gasification stage.
Weitere im Rahmen der Erfindung liegende Verfahrensvarianten ergeben sich im Zusammenhang mit dem noch zu erläuternden Blockschaltbild (Fig. 1).Further method variants within the scope of the invention result in connection with the block diagram to be explained (FIG. 1).
Bei dem erfindungsgemäßen Herstellungsverfahren wird die Vergasung in der Regel unter Druck von vorzugsweise 10 bis 100 bar durchgeführt. Höhere Vergasungsdrücke sind - grundsätzlich - möglich. Ebenso kann die Vergasung bei Atmosphärendruck oder im leichten Unterdruck (im Falle der Verwendung von Saugzuggebläsen) durchgeführt werden.In the production process according to the invention, the gasification is generally carried out under a pressure of preferably 10 to 100 bar. Basically, higher gasification pressures are possible. The gasification can also be carried out at atmospheric pressure or in a slightly reduced pressure (if suction fans are used).
Hinsichtlich der dem Vergasungsreaktor zuzuführenden Gas- bzw. Flüssigfraktion aus der thermischen Vorbehandlung des Einsatzstoffes versteht es sich, daß diese auch feste Bestandteile in Form feinkörnigen, insbesondere staubförmigen Materials aufweisen können.With regard to the gas or liquid fraction to be fed to the gasification reactor from the thermal pretreatment of the starting material, it goes without saying that these can also have solid constituents in the form of fine-grained, in particular dust-like material.
Die vorgenannten sowie die beanspruchten und in dem nachfolgenden Ausführungsbeispiel beschriebenen, erfindungsgemäß zu verwendenden Bauteile bzw. Verfahrensschritte unterliegen in ihrer Größe, Formgestaltung, Materialauswahl und technischen Konzeption bzw. ihren Verfahrensbedingungen keinen besonderen Ausnahmebedingungen, so daß die in dem jeweiligen Anwendungsgebiet bekannten Auswahlkriterien uneingeschränkt Anwendung finden können.The size, shape, material selection, technical conception and process conditions of the above-mentioned components as well as those claimed and described in the following exemplary embodiment and to be used according to the invention are not subject to any special exceptional conditions, so that the selection criteria known in the respective field of application are used without restriction can.
Weitere Einzelheiten, Merkmale und Vorteile des Gegenstandes der Erfindung ergeben sich aus der nachfolgenden Beschreibung der zugehörigen Zeichnung. In der Zeichnung zeigt:
Fig. 1 ein Blockschaltbild.Further details, features and advantages of the subject matter of the invention result from the following description of the associated drawing. The drawing shows:
Fig. 1 is a block diagram.
Das in Fig. 1 wiedergegebene Blockschaltbild wird nachfolgend im Zusammenhang mit der Verwendung eines Flugstromvergasungsreaktors erläutert. Alternative Verfahrensführungen sind dabei gestrichelt dargestellt. Lediglich vorzugsweise zum Einsatz kommende Verfahrensstufen sind zusätzlich mit einer gestrichelten Linie umrandet.The block diagram shown in FIG. 1 is explained below in connection with the use of an entrained-flow gasification reactor. Alternative procedures are shown in dashed lines. Process steps that are preferably used are additionally outlined with a dashed line.
Gemäß Fig. 1 wird ein organische Bestandteile enthaltender Rest- oder Abfallstoff, nachfolgend als Einsatzstoff bezeichnet, einer Pyrolysebehandlungsstufe 101, wie z.B. einem indirekt beheizten Drehrohrofen (Trommelwandtemperatur bis zu 900° C), aufgegeben. In dieser wird, weitestgehend sauerstofffrei, der Einsatzstoff unter Zufuhr von Wärme und im wesentlichen unter Vermeiden eines Verbrennens von Bestandteilen des Einsatzstoffes bei Temperaturen zwischen ca. 300 und 650° C thermisch vorbehandelt. Für die Wärmezufuhr kann Fremdgas, hinter dem Vergasungsreaktor 102 anfallendes Produktgas und/oder hinter einer der Pyrolysestufe nachgeschalteten Kondensationsstufe 103 anfallendes, vorzugsweise in 5 einer Pyrolysegasreinigungsstufe 104 anfallendes Pyrolysegas eingesetzt werden.According to FIG. 1, a residual or waste material containing organic constituents, hereinafter referred to as feed material, is fed to a
Das in der Pyrolysebehandlungsstufe 101 aus dem Einsatzstoff anfallende Zwischenprodukt wird getrennt als Dampf (Gasfraktion) und Koks (Festfraktion) abgeführt. Die Festfraktion wird, ggf. nach Einstellen der Körnungsbandbreite in einer Mahl-, Sieb- und/oder Sichtstufe 105 auf das für den jeweiligen Vergasungsreaktortyp (Vergasungsreaktor 102) verträgliche Maß eingestellt und dem Vergasungsreaktor 102, z. B. pneumatisch, zugeführt. In der Festfraktion enthaltene Wertstoffe, z.B. Metalle, können in einer Trennstufe 106, z.B. einer Siebvorrichtung, entfernt werden, bevor die Festfraktion dem Vergasungsreaktor 102 zugeführt wird.The intermediate product obtained in the
Die hinter der Pyrolysebehandlungsstufe 101 anfallende Gasfraktion wird als Dampf entweder dem Vergasungsreaktor zur Vergasung und/oder Einbringung von Reaktionswärme zugeführt oder zunächst durch eine Kondensationsstufe 103 geleitet. Das darin abgeschiedene, unter den Kondensationsbedingungen anfallende Restgas wird entweder, vorzugsweise nach Durchlaufen einer Pyrolysegasreinigungsstufe 104 der Pyrolysebehandlungsstufe zur Einbringung von Prozeßwärme zugeführt. Alternativ oder ergänzend kann das Pyrolysegas zur Einbringung von Vergasungswärme dem Vergasungsreaktor 102 oder dem dahinter anfallenden Produktgasstrom zugeführt werden. In diesen Fällen kann eine Pyrolysegasreinigungsstufe ggf. entfallen.The gas fraction obtained behind the
Das hinter der Kondensationsstufe 103 anfallende Öl (Flüssigfraktion) wird in anderen Prozessen verwertet oder, wie bevorzugt, in den Vergasungsreaktor 102 eingetragen. Vor allem dann, wenn dieses Öl mit der Festfraktion aus der Pyrolysebehandlungsstufe 101 gemeinsam vergast werden soll, können die beiden Fraktionen zunächst vereinigt und mittels einer Pumpe oder Schneckenmaschine 107 dem Vergasungsreaktor 102 aufgegeben werden.The oil (liquid fraction) obtained behind the
Hinter dem Vergasungsreaktor fallen anorganische Bestandteile an, die nicht mehr deponiert werden müssen, sondern als Wertstoffe verwendbar sind. Das hinter dem Vergasungsreaktor 102 anfallende Produktgas wird in der Regel in einer Gasreinigungsstufe 108 gereinigt werden. Die aus dem Produktgas entfernten Bestandteile können zumindest als Teilstrom dem Vergasungsreaktor 102 aufgegeben werden, damit sie dort in Produktgas bzw. anorganische Bestandteile aufgeteilt werden. Im übrigen können angereicherte Schadgasbestandteile, wie Schwefel, Salze und Schwermetalle weiterverwertet werden.After the gasification reactor, there are inorganic components that no longer have to be deposited, but can be used as valuable materials. The product gas obtained behind the
Das hinter der Gasreinigungsstufe 108 anfallende Produktgas kann, wie bevorzugt, in einem, ggf. bereits vorhandenen, Kraftwerk 109 oder, ggf. teilweise, in der Pyrolysebehandlungsstufe 101 verfeuert werden oder als Synthesegas oder sonstiges Brenngas verwendet werden.The product gas obtained behind the
Claims (8)
- A process for producing synthetic gas from solid or pasty residues and waste - difficult to handle and containing organic components - in particular the shredder light fraction from vehicle utilisation with oxygen or oxygen-containing gases and, optionally, water vapour by using an entrainment gasifying reactor at temperatures of from 800°C to 1700°C and. optionally, higher, during whicha) first of all as a result of thermal pre-treatment by supplying heat and, substantially, by avoiding combustion of components of the feed (pyrolysis treatment) there is separation in a heated revolving tube into a gaseous, in particular vapour-like, fraction and a solid fraction,b) the solid fraction is fed to the entrainment gasifying reactor as a solid feed material to be gasified, optionally after separation off of valuable substances, for changing into the synthetic gas, andc) the gas fraction is utilised at least partially in the production process, in particular for introducing heat for the endothermic gasification process.
- A process according to Claim 1, characterised in that the gas fraction which is obtained during pyrolysis undergoes a condensation step before being utilised.
- A process according to Claim 2, characterised in that the gas fraction obtained after the condensation stage is combined immediately as part of the synthetic and/ or fuel gas with the product gas stream obtained downstream of the gasifying reactor, or is added to the gasifying reactor or the pyrolysis treatment stage for the purpose of introducing heat for the endothermic process.
- A process according to Claim 2 or 3, characterised in that the liquid fraction obtained after the condensation stage is utilised in another process or is added to the gasifying reactor for gasification and/or introduction of heat for the endothermic gasification process.
- A process according to any one of Claims 1 to 3, characterised in that the grain size range, obtained after the pyrolysis treatment stage, of the solid fraction is reduced before gasification in the entrainment gasifying reactor by grinding, sifting and/or classification.
- A process according to any one of Claims 1 to 4, characterised in that the solid fraction obtained after the pyrolysis treatment stage and the liquid fraction obtained after the condensation stage are mixed and, are added, preferably by means of a pump or screw machine, to the gasifying reactor.
- A process according to any one of Claims 1 to 5, characterised in that the product gas obtained downstream of the gasifying reactor and, optionally, after the condensation stage, is used, where necessary after removing for example pollutants present (pollutant gas components), as a gaseous fuel for the operation of a power station, optionally already available, in particular, a block-type thermal power station.
- A process according to any one of Claims 1 to 6, characterised in that inorganic residues or waste are added to the feed.
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DE19914123406 DE4123406C2 (en) | 1991-07-15 | 1991-07-15 | Process for the gasification of inferior solid fuels in a shaft-shaped gasification reactor |
DE4123406 | 1991-07-15 | ||
PCT/EP1992/001607 WO1993002162A1 (en) | 1991-07-15 | 1992-07-15 | Process for producing synthetic or fuel gasses from solid or pasty residues and waste or low-grade fuels in a gasifying reactor |
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EP92202501A Pending EP0523815A1 (en) | 1991-07-15 | 1992-07-15 | Process for fabrication of synthesis or fuel gases from pasty or solid refuse or waste materials or from low-grade fuels in gasification reactor |
EP92916028A Expired - Lifetime EP0600923B1 (en) | 1991-07-15 | 1992-07-15 | Process for producing synthetic or fuel gasses from solid or pasty residues and waste or low-grade fuels in a gasifying reactor |
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JP (1) | JP3203580B2 (en) |
AU (1) | AU2344492A (en) |
CA (1) | CA2113636A1 (en) |
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US4497637A (en) * | 1982-11-22 | 1985-02-05 | Georgia Tech Research Institute | Thermochemical conversion of biomass to syngas via an entrained pyrolysis/gasification process |
DE3310534A1 (en) * | 1983-03-23 | 1984-10-04 | C. Deilmann AG, 4444 Bad Bentheim | DEVICE FOR RECOVERING ENERGY FROM PYROLIZABLE, CARBONATED WASTE MATERIALS, ALTERNATING COMPOSITION |
AT382388B (en) * | 1985-03-08 | 1987-02-25 | Voest Alpine Ag | DEVICE FOR THE GASIFICATION OF FUELS |
DE3828534A1 (en) * | 1988-08-23 | 1990-03-08 | Gottfried Dipl Ing Roessle | METHOD FOR UTILIZING ENERGY-BASED MEASUREMENT, DEVICE FOR IMPLEMENTING THE METHOD AND USE OF A PRODUCT RECEIVED FROM RECYCLING |
-
1991
- 1991-07-15 DE DE19914123406 patent/DE4123406C2/en not_active Expired - Fee Related
-
1992
- 1992-07-15 AU AU23444/92A patent/AU2344492A/en not_active Abandoned
- 1992-07-15 EP EP92202501A patent/EP0523815A1/en active Pending
- 1992-07-15 WO PCT/EP1992/001607 patent/WO1993002162A1/en active IP Right Grant
- 1992-07-15 EP EP92916028A patent/EP0600923B1/en not_active Expired - Lifetime
- 1992-07-15 JP JP50258393A patent/JP3203580B2/en not_active Expired - Fee Related
- 1992-07-15 DE DE59207017T patent/DE59207017D1/en not_active Expired - Fee Related
- 1992-07-15 CA CA002113636A patent/CA2113636A1/en not_active Abandoned
-
1994
- 1994-01-14 FI FI940184A patent/FI106314B/en not_active IP Right Cessation
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0545241A1 (en) * | 1991-11-29 | 1993-06-09 | Noell Energie- und Entsorgungstechnik GmbH | Process for thermic valorisation of waste materials |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19853713A1 (en) * | 1998-11-20 | 2000-05-31 | Krc Umwelttechnik Gmbh | Slagging gasification of high calorific value, sorted, baled, diverse wastes produces useful fuel gas and leachate-free glass granules whilst avoiding typical pollutants released by incineration processes |
DE19853717A1 (en) * | 1998-11-20 | 2000-05-31 | Krc Umwelttechnik Gmbh | Slagging gasification of compacted, baled organic wastes takes place in chamber with primary and secondary oxidant supplies, producing fuel gas and useful construction material |
DE19853717C2 (en) * | 1998-11-20 | 2000-12-21 | Krc Umwelttechnik Gmbh | Methods and devices for the gasification of compact organic materials |
DE19853713C2 (en) * | 1998-11-20 | 2003-03-13 | Bbp Power Plants Gmbh | Process for the material and energetic utilization of residual and waste materials |
Also Published As
Publication number | Publication date |
---|---|
JPH07502766A (en) | 1995-03-23 |
DE59207017D1 (en) | 1996-10-02 |
DE4123406A1 (en) | 1993-01-21 |
JP3203580B2 (en) | 2001-08-27 |
FI106314B (en) | 2001-01-15 |
AU2344492A (en) | 1993-02-23 |
CA2113636A1 (en) | 1993-02-04 |
WO1993002162A1 (en) | 1993-02-04 |
FI940184A (en) | 1994-03-11 |
FI940184A0 (en) | 1994-01-14 |
EP0523815A1 (en) | 1993-01-20 |
EP0600923A1 (en) | 1994-06-15 |
DE4123406C2 (en) | 1995-02-02 |
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