EP0182404A2 - Procédé de fabrication de boulettes contenant du charbon pour la gazéification - Google Patents

Procédé de fabrication de boulettes contenant du charbon pour la gazéification Download PDF

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Publication number
EP0182404A2
EP0182404A2 EP85201686A EP85201686A EP0182404A2 EP 0182404 A2 EP0182404 A2 EP 0182404A2 EP 85201686 A EP85201686 A EP 85201686A EP 85201686 A EP85201686 A EP 85201686A EP 0182404 A2 EP0182404 A2 EP 0182404A2
Authority
EP
European Patent Office
Prior art keywords
pellets
fine
weight
coal
hard coal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP85201686A
Other languages
German (de)
English (en)
Other versions
EP0182404A3 (en
EP0182404B1 (fr
Inventor
Dieter Dr. Sauter
Udo Dr. Zentner
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GEA Group AG
Original Assignee
Metallgesellschaft AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Metallgesellschaft AG filed Critical Metallgesellschaft AG
Publication of EP0182404A2 publication Critical patent/EP0182404A2/fr
Publication of EP0182404A3 publication Critical patent/EP0182404A3/de
Application granted granted Critical
Publication of EP0182404B1 publication Critical patent/EP0182404B1/fr
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L5/00—Solid fuels
    • C10L5/02—Solid fuels such as briquettes consisting mainly of carbonaceous materials of mineral or non-mineral origin
    • C10L5/06—Methods of shaping, e.g. pelletizing or briquetting
    • C10L5/10—Methods of shaping, e.g. pelletizing or briquetting with the aid of binders, e.g. pretreated binders
    • C10L5/12—Methods of shaping, e.g. pelletizing or briquetting with the aid of binders, e.g. pretreated binders with inorganic binders
    • 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
    • C10J3/02—Fixed-bed gasification of lump fuel
    • 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
    • C10J3/02—Fixed-bed gasification of lump fuel
    • C10J3/20—Apparatus; Plants
    • C10J3/30—Fuel charging devices
    • 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
    • C10J3/72—Other features
    • C10J3/78—High-pressure apparatus
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L5/00—Solid fuels
    • C10L5/02—Solid fuels such as briquettes consisting mainly of carbonaceous materials of mineral or non-mineral origin
    • C10L5/04—Raw material of mineral origin to be used; Pretreatment thereof
    • 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
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0913—Carbonaceous raw material
    • C10J2300/093—Coal
    • 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
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
    • C10J2300/0956—Air or oxygen enriched air
    • 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
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
    • C10J2300/0959—Oxygen
    • 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
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
    • C10J2300/0969—Carbon dioxide
    • 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
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
    • C10J2300/0973—Water
    • C10J2300/0976—Water as steam

Definitions

  • the invention relates to a process for producing carbon-containing pellets for gasification in a reactor in the pressure range from 5 to 150 bar with oxygen, water vapor and / or carbon dioxide as the gasifying agent, the pellets being placed in the reactor on a fixed bed which slowly moves downwards , into which the gasifying agent is introduced from below and under which the mineral components are removed as solid ash or liquid slag.
  • the invention has for its object to produce carbon-containing pellets in a simple manner, which can be gasified alone or together with granular fuel in a fixed bed. It is important that the pellets do not disintegrate during transport to the gasification reactor, even if a long transport path is necessary. Furthermore, the pellets in the reactor should have good gasification behavior and should not give rise to disruptions to the gasification operation.
  • this is achieved according to the invention in that only fine-grained hard coal with a grain size of less than 1 mm with a fine grain content with grain sizes of at most 2 mm of 3 to 10% by weight and a content of 70 to 80% by weight of a grain size of at most 63 mm is used, the fine-grained hard coal is mixed with bentonite so that the mixture has a bentonite content of 1 to 8% by weight, pellets with a water content of 15 to 25% by weight are formed from the mixture with the addition of water, and the pellets gives up the fixed bed in the moist, plastic state without drying.
  • the coals to be used for the pellets are hard coals of classes 0 to 9 according to DIN 23 003, which according to ASTM correspond to the coals of the classes "high volatile C-bituminous" to "anthracite". Fine-grained hard coal with a grain size of less than 0.35 mm is preferably used.
  • the various bentonites for example natural Na bentonites, activated Ca bentonites and also bentonite-rich raw clays are suitable as binders.
  • the bentonite binder can either placed in a grinding plant together with the coal or added to the ground hard coal in a mixer.
  • the coal and the bentonite if appropriate also together with a flux, are allowed to undergo a grinding process together, since a very homogeneous distribution of the binder is achieved in this way.
  • Fine-grain flux especially lime, can be useful if you want to lower the melting temperature of the coal ash.
  • the mixture to be pelletized contains the flux in a proportion of 2 to 15% by weight.
  • the bentonite also has the option of absorbing water and swelling it.
  • pelletizing plates water being used as the pelleting liquid.
  • a pelletizing plate for example, a rotary tube can also be used.
  • the finished pellets usually have a water content in the range from 15 to 25% by weight, this water content being primarily a function of the carbon substance and not or hardly dependent on the bentonite content.
  • these still moist pellets which usually have a plastic behavior, fully meet the requirements of a dust-free, mechanical handling during transport, handling and filling into the gasification reactor. This plastic behavior of the pellets is only achieved with bentonite as a binder and occurs with other clay-mineral coal components such as illite-containing filter sludges do not appear as binders.
  • the fine grain fraction with grain sizes up to a maximum of 4 mm is preferably 7 to 15% by weight and the fine fraction up to a maximum of 2 mm 4 to 8% by weight in the hard coal to be pelletized.
  • hard coal with an ash content of at least 10% by weight is preferably in the range from 15 to 40% by weight.
  • the moist, plastic pellets can be added to the fixed bed gasification as the sole fuel. However, it is of course also possible to mix the pellets together with granular coal with grain sizes in the range to gasify from 3 to 60 mm.
  • the filter sludge contains a grain size fraction of up to 2 mm of 7% by weight, a fraction of up to 4 mm of 12% by weight and a fraction of up to 63 mm of 78% by weight.
  • the mixture is formed into pellets of 8 to 16 mm in diameter on a pelletizing plate while spraying with water.
  • the moisture content of the pellets is 17.9% by weight, the pellets have diameters in the range from 12.5 to 16 mm and breaking strengths in the range from 25 to 32 N.
  • the pellets are subjected to the envelope test described, with less than 0.1% by weight of abrasion in the form of fine grain being less than 1 mm.
  • a non-baking, young gas coal from South Africa with 22% by weight ash and 5.3% moisture is ground to a grain size of less than 0.315 mm, the grain content up to a maximum of 2 mm 4 weight%, the proportion up to a maximum of 4 mm 10 weight% .% and the grain content up to a maximum of 63 mm is 71% by weight.
  • This ground coal is mixed with 50 g bentonite per kg coal (calculated as anhydrous) and then moistened with water. The mixture is fed to a pelletizing plate and shaped into pellets with the addition of water.
  • the pellets have a moisture content of 21.4% by weight, they have a diameter of 12.5 to 16 mm and an average strength of 35 N.
  • the pellets are subjected to the envelope test described, with only 0.9% by weight of abrasion in shape of fine grain with a grain size of less than 1 mm.
  • 50 t of the moist, not dried pellets are gasified in the gasification reactor already used for example 1 at a pressure of 25 bar.
  • the gasification runs without disturbances, the ashes can be easily removed and the results of the gasification correspond to those of granular coal.
  • the wet pellets were transported over a distance of 250 km in a railway wagon for bulk goods.
  • the pellets are unloaded into a deep bunker with clearing arm and then transported via rubber conveyor belts, screening machine, bucket elevator and scraper conveyor belt without any problems and completely dust-free.
  • the formation of fine grains of less than 3 mm is relatively low and is essentially limited to the area of the R äumarmes in deep bunker.
  • the further path of the pellets from the bunker via the weighing container, the lock and the coal distributor to the fixed bed of the gasification reactor is carried out without difficulty and without abrasion.
  • a non-baking lean coal with 25% by weight ash and 1.8% 4 moisture is ground to a grain size of less than 0.315 mm and mixed intensively with 40 g bentonite per kg coal (water-free calculated).
  • the ground coal has a grain fraction up to a maximum of 2 mm of 6% by weight, a fraction up to a maximum of 4 mm of 11% by weight and a fraction up to a maximum of 63 mm of 74% by weight.
  • the mixture is moistened and pellets of 8 to 20 mm in diameter are produced on a pelletizing plate when water is added.
  • the pellets have a moisture content of 18.7% by weight and a diameter in the range from 12.5 to 16 mm.
  • the average breaking strength of the pellets is 22 N. 400 kg of these pellets are subjected to the envelope test, which in turn produces only the smallest amounts of abrasion with grain sizes below 1 mm.
  • the pellets are first dried, with an average breaking strength of 70 N.
  • the strength values of the pellets practically do not change, so that they are fully suitable as feed for fixed bed gasification.
  • a weakly baking gas coal from Great Britain with 3.7% by weight of ash, 7.3% by weight of moisture and an expansion ratio of 1 is ground to a grain size of less than 0.315 mm.
  • the ground coal has a grain fraction namely to a maximum of 63 mm of 60 wt.%, A fraction up to at most 2 m M of only 1.7 wt.% And a fraction up to at most 4 mm of 3.9% by weight.
  • This ground coal is mixed with 6% by weight bentonite; The mixture is used to produce water-containing pellets with a moisture content of 29% by weight, as in Example 1.
  • the pellets have a strength of less than 10 N. They are not plastically deformable and behave very brittle, similar to dried pellets. Even small Z ug or shear stresses lead to the disintegration of the pellets.
  • the plastically deformable pellets are dried and coked under a pressure of 25 bar, they reach a strength of about 720 N.
  • the drying and coking of the brittle pellets described at the beginning only gives strength values in the range of 70 N.
  • a batch of 100 t of the moist , plastic pellets is easily gasified in a gasification reactor with liquid ash discharge with a mixture of water vapor and oxygen at a pressure of 25 bar. If the plastic wet pellets are produced with the addition of 3% by weight of limestone, the flow temperature of the ash in the gasification reactor is reduced by about 70 ° C.
  • the moist, plastic pellets are transported in barrels over a distance of more than 1000 km and then emptied into a bunker. This is done free of dust and abrasion. Finally, the pellets from the hopper without complications via a lock and a K ohleverteiler be added to the gasification reactor.
  • a non-baking, charcoal charcoal with 11% by weight ash and 1.8% by weight moisture is ground in a known manner.
  • the finest fractions of the ground coal are lower than usual for other, high-ash coal, because the grain fraction up to a maximum of 4 mm is 6% by weight, the grain fraction up to a maximum of 2 mm is 2.1% by weight, and the fraction up to a maximum of 63 mm amounts to 68% by weight.
  • moist pellets are produced with 4% by weight of bentonite as a binder, the pellets having a water content of 21% by weight and an average breaking strength of 17 N.
  • the pellets are not plastically deformable and break in the event of a fall from a greater height; even low tensile or shear stresses lead to disintegration; the pellets behave similarly to dried pellets.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
EP85201686A 1984-11-15 1985-10-15 Procédé de fabrication de boulettes contenant du charbon pour la gazéification Expired EP0182404B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3441757 1984-11-15
DE3441757A DE3441757A1 (de) 1984-11-15 1984-11-15 Verfahren zum herstellen kohlehaltiger pellets fuer die vergasung

Publications (3)

Publication Number Publication Date
EP0182404A2 true EP0182404A2 (fr) 1986-05-28
EP0182404A3 EP0182404A3 (en) 1987-01-21
EP0182404B1 EP0182404B1 (fr) 1989-04-19

Family

ID=6250371

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85201686A Expired EP0182404B1 (fr) 1984-11-15 1985-10-15 Procédé de fabrication de boulettes contenant du charbon pour la gazéification

Country Status (6)

Country Link
US (1) US4773919A (fr)
EP (1) EP0182404B1 (fr)
JP (1) JPS61171794A (fr)
AU (1) AU575445B2 (fr)
DE (2) DE3441757A1 (fr)
ZA (1) ZA858788B (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2343678B (en) * 1998-11-16 2002-12-11 Meirion Thomas Evans Agglomerate production
MXPA06010237A (es) * 2004-03-11 2007-04-23 Sasol Tech Pty Ltd Gasificacion de material carbonoso.
CN100360647C (zh) * 2005-11-21 2008-01-09 上海元宝能源技术有限公司 水煤气发生炉用气化型煤
CA2647954C (fr) * 2006-03-31 2014-12-23 Atlantic Combustion Technologies Inc. Augmentation du rendement de procedes de combustion
JP2008248068A (ja) * 2007-03-30 2008-10-16 Mitsui Eng & Shipbuild Co Ltd 廃棄物のガス化方法
JP5745288B2 (ja) * 2011-02-22 2015-07-08 新日鉄住金エンジニアリング株式会社 石炭ガス化装置における石炭ガス化方法
CN204111704U (zh) 2012-02-13 2015-01-21 乔治洛德方法研究和开发液化空气有限公司 用于固体燃料的固定床压力气化的装置
US9816040B2 (en) * 2012-09-10 2017-11-14 Phillips 66 Company Increasing stability of a pyrolysis product

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1445980A (fr) * 1965-08-31 1966-07-15 Bergwerksverband Gmbh Procédé pour la fabrication d'agglomérés de coke sphériques
EP0010792A1 (fr) * 1978-11-02 1980-05-14 Metallgesellschaft Ag Procédé pour gazéifier des combustibles en particules fines
EP0011887A1 (fr) * 1978-11-28 1980-06-11 Metallgesellschaft Ag Procédé pour la fabrication des briquettes du charbon collant pour la gasification
GB2061317A (en) * 1979-10-11 1981-05-13 Metallgesellschaft Ag Process for producing coal briquettes to be gasified or devolatilised

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US1913121A (en) * 1930-06-18 1933-06-06 Frederick E Kern Process of forming a fuel
US2163148A (en) * 1936-03-04 1939-06-20 Koppers Co Inc Slagging water-gas generator
DE1545461A1 (de) * 1966-05-20 1970-01-29 Metallgesellschaft Ag Verfahren zur Herstellung von ueberwiegend Kohlenmonoxyd und bzw. oder Wasserstoff enthaltenden Gasen aus festen Brennstoffen
US3692505A (en) * 1971-04-05 1972-09-19 Consolidation Coal Co Fixed bed coal gasification
US3762886A (en) * 1971-06-14 1973-10-02 Great Lakes Carbon Corp Formed carbon fuel briquets
DE2201278C2 (de) * 1972-01-12 1982-09-02 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur Erzeugung eines mit Erdgas austauschbaren Gases
GB1391034A (en) * 1973-02-05 1975-04-16 Metallgesellschaft Ag Process for the manufacture of a gas interchangeable with natural gas
DE2540166C2 (de) * 1975-09-09 1984-08-30 Steag Ag, 4300 Essen Vorrichtung zur Beschickung des Schachtes eines Kohledruckvergasers mit Briketts aus Steinkohle
GB1512677A (en) * 1975-11-27 1978-06-01 British Gas Corp Quench chambers in coal gasification plant
GB1507905A (en) * 1975-11-27 1978-04-19 British Gas Corp Removal of slag from coal gasification plant
GB1508671A (en) * 1976-12-09 1978-04-26 British Gas Corp Coal gasification plant
DE2802954A1 (de) * 1978-01-24 1979-07-26 Steag Ag Verfahren und anlage zum stueckigmachen von einsatzbrennstoff fuer die kohledruckvergasung
US4167398A (en) * 1978-03-13 1979-09-11 American Colloid Company Carbonaceous briquette and method for making same
US4239500A (en) * 1979-03-14 1980-12-16 Steag A.G. Process for the utilization of waste product tar-dust in gasification of granular fuel under pressure, especially of bituminous coal
DE3333870A1 (de) * 1983-09-20 1985-03-28 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zum betreiben eines reaktors zum vergasen fester brennstoffe

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1445980A (fr) * 1965-08-31 1966-07-15 Bergwerksverband Gmbh Procédé pour la fabrication d'agglomérés de coke sphériques
EP0010792A1 (fr) * 1978-11-02 1980-05-14 Metallgesellschaft Ag Procédé pour gazéifier des combustibles en particules fines
EP0011887A1 (fr) * 1978-11-28 1980-06-11 Metallgesellschaft Ag Procédé pour la fabrication des briquettes du charbon collant pour la gasification
GB2061317A (en) * 1979-10-11 1981-05-13 Metallgesellschaft Ag Process for producing coal briquettes to be gasified or devolatilised

Also Published As

Publication number Publication date
AU575445B2 (en) 1988-07-28
ZA858788B (en) 1987-07-29
EP0182404A3 (en) 1987-01-21
AU4992585A (en) 1986-05-22
DE3441757A1 (de) 1986-05-15
US4773919A (en) 1988-09-27
DE3569567D1 (en) 1989-05-24
EP0182404B1 (fr) 1989-04-19
JPS61171794A (ja) 1986-08-02

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