EP0036151B1 - Procédé de décokage de refroidisseurs de gaz craqués - Google Patents

Procédé de décokage de refroidisseurs de gaz craqués Download PDF

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Publication number
EP0036151B1
EP0036151B1 EP81101665A EP81101665A EP0036151B1 EP 0036151 B1 EP0036151 B1 EP 0036151B1 EP 81101665 A EP81101665 A EP 81101665A EP 81101665 A EP81101665 A EP 81101665A EP 0036151 B1 EP0036151 B1 EP 0036151B1
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EP
European Patent Office
Prior art keywords
cracked gas
air
gas cooler
cracking
cracked
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.)
Expired
Application number
EP81101665A
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German (de)
English (en)
Other versions
EP0036151A1 (fr
EP0036151B2 (fr
Inventor
Artur Dr. Sliwka
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BASF SE
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BASF SE
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Filing date
Publication date
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Application filed by BASF SE filed Critical BASF SE
Priority to AT81101665T priority Critical patent/ATE5891T1/de
Publication of EP0036151A1 publication Critical patent/EP0036151A1/fr
Publication of EP0036151B1 publication Critical patent/EP0036151B1/fr
Application granted granted Critical
Publication of EP0036151B2 publication Critical patent/EP0036151B2/fr
Expired legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
    • B08B9/027—Cleaning the internal surfaces; Removal of blockages
    • B08B9/032—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing
    • 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
    • C10G9/00—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G9/14—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils in pipes or coils with or without auxiliary means, e.g. digesters, soaking drums, expansion means
    • C10G9/16—Preventing or removing incrustation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B2230/00—Other cleaning aspects applicable to all B08B range
    • B08B2230/01—Cleaning with steam

Definitions

  • the present invention relates to a method for thermal decoking of cracked gas coolers for indirect cooling by means of water of ethylene-containing cracked gases which are obtained by thermal cracking of hydrocarbons in the presence of steam in an indirectly heated tubular cracking furnace.
  • the thermal cracking of hydrocarbons in the presence of water vapor in an indirectly heated tube cracking furnace is widely used in ethylene plants (steam crackers), in which, in addition to ethylene, there are other valuable unsaturated compounds such as propylene and butadiene as well as pyrolysis gasoline with a high proportion of aromatic hydrocarbons such as benzene , Toluene and xylene can be obtained.
  • steam crackers in which, in addition to ethylene, there are other valuable unsaturated compounds such as propylene and butadiene as well as pyrolysis gasoline with a high proportion of aromatic hydrocarbons such as benzene , Toluene and xylene can be obtained.
  • dwell times for the hydrocarbons in the cracked tubes of the tubular cracking furnace of 0.1 to 0.5 seconds and exit temperatures of the cracked gases from the cracked tubes of more than 750 ° C., generally between 800 and 900 ° C., are preferably observed .
  • the cracked gas must be cooled immediately after leaving the tubular cracking furnace in order to prevent undesirable side reactions which lead to a reduction in the yield of valuable products. This can be done directly by injecting liquid hydrocarbons or water into the hot cracked gas.
  • direct cooling has the disadvantage that when the heat is recovered in the form of water vapor, the water vapor obtained has only a low pressure level.
  • High-pressure steam is generated at a pressure of up to 150 bar, preferably up to 130 bar. This high-pressure steam contributes to the economics of the process, since it supplies the major part of the drive energy for the raw gas and refrigeration compressors of the ethylene plants.
  • the process has a considerable disadvantage, namely the deposition of coke on the inner walls of both the canned tubes in the tube furnace and the inlet hood and the cooling tubes in the downstream cracked gas cooler. Due to the insulating effect of the coke, the tube wall temperature of the canned tubes of the tubular cracking furnace increases and the pressure loss increases. In the downstream cracked gas cooler, the heat transfer is deteriorated by the coke deposit, so that the temperature of the cracked gas rises in the outlet of the cracked gas cooler. Once the coke deposits have reached a certain strength, the tube cracking furnace must be switched off together with the downstream cracking gas cooler and the coke removed.
  • the canned tubes are usually with a water vapor / air mixture or only with water vapor or with a mixture of water vapor and hydrogen (see. DE-A-19 48 635) at temperatures from 700 ° C to 1000 ° C from Free coke.
  • the cracked gas cooler is cleaned mechanically.
  • This method is very complex and requires a longer shutdown time of the tube cracking furnace and therefore a corresponding loss of production in the ethylene plant.
  • the tube cracking furnace is usually cooled.
  • the cracked gas cooler is opened, and the individual pipes of the cracked gas cooler, for example with more than 50 pipes, are used for mechanical cleaning, e.g. B. with a high pressure water device, at a water pressure of usually 300 to 700 bar or in very hard coke deposits by means of water / sandblasting from the coke.
  • a major disadvantage of this method is that the material of the furnace is subjected to excessive stress as a result of the frequent cooling and subsequent heating, and damage often occurs as a result.
  • the method described above is modified in such a way that the tube cracking furnace is first cooled to 200 ° C. to 400 ° C., then the cracking gas cooler is separated from the tube cracking furnace and the mechanical cleaning of the completely cooled cracking gas cooler is carried out, while at the same time performing the cracking tubes the cracked gas cooler with a water vapor / air mixture. But here too, only a small amount of time is saved, especially since the change in temperature and the stress on the canned tubes of the tubular cracking furnace can release coke from the inside of the canned tubes and thus create additional problems.
  • the coke in the cracked gas cooler is only removed to a small extent due to the lower temperatures that occur in the on-line decoking in the cracked gas cooler.
  • the disadvantage that the temperature at which the cracking gas emerges from the cracking gas cooler does not drop to the value of a mechanically cleaned cooler, but is only slightly lower than before the shutdown, so that a correspondingly smaller amount of high pressure steam is generated in the cracked gas cooler.
  • mechanical cleaning of the cracked gas cooler with all the disadvantages described is necessary.
  • French Patent 15 32 127 discloses a process for decoking in the thermal cracking of hydrocarbons without the addition of water vapor, in which the cracked gas outlet temperatures are between 600 and 700 ° C.
  • the cracked gas outlet temperatures of 600 to 700 ° C. correspond to those of the conventional ethylene processes
  • the process of the present application with cracked gas outlet temperatures above 750 ° C. relates to the high severity ethylene process, in which completely different extremely low-hydrogen coke deposits arise, the removal of which has raised completely new problems compared to the conventional ethylene processes.
  • French Patent 1532127 it is described that only steam is used for decoking, to which increasing amounts of air are then fed, the amount of air being increased by up to 100%.
  • the object of the invention was therefore to provide a method for thermal decoking of cracked gas coolers which does not have the disadvantages of the known methods.
  • the cracked gas coolers can be decoked thermally without the need for additional mechanical cleaning of the cracked gas cooler and the associated cooling of the upstream tube cracking furnaces.
  • the known methods e.g. B. in the on-line decoking described above, only annual runtimes of the tube cracking furnaces of 85 to 95% are achieved, annual runtimes of more than 97% and thus a correspondingly higher ethylene production are obtained by reducing the downtimes.
  • fewer replacement tube cracking furnaces are required in the ethylene plant due to the increased operating time, which reduces the investment costs for the ethylene plant.
  • cracked gas coolers are thermally decoked, which are used for indirect cooling by means of water of ethylene-containing cracked gases, the cracked gases being obtained by thermal cracking of hydrocarbons in the presence of steam in an indirectly heated tubular cracking furnace at gas outlet temperatures above 750 ° C.
  • Suitable starting hydrocarbons for thermal cracking are ethane, propane, butane, LPG, gasoline fractions such as light petrol, e.g. B. light petrol with the boiling range of about 30 to 150 ° C, gasoline (full-range naphtha), for. B. gasoline with the boiling range of about 30 to 180 ° C, heavy fuel, z.
  • B. heavy gasoline with the boiling range of about 150 to 220 ° C, kerosene, z.
  • the process is preferably used for cracked gas coolers for cooling cracked gases obtained from gasoline fractions, kerosene and / or gas oils.
  • the outlet temperatures of the cracked gas from the tube cracking furnace are more than 750 ° C., preferably 780 to 900 ° C., in particular 800 to 900 ° C.
  • the residence times in the tube cracking furnaces are generally 0.05 to 1 sec., Preferably 0.1 to 0.6 sec., In particular 0.1 to 0.5 sec.
  • the thermal loads on the can in the tube cracking furnaces are expediently 40,000 to 80,000 kcal / m 2 ⁇ h, preferably 50,000 to 70,000 kcal / m 2 ⁇ h.
  • the weight ratio of water vapor to the hydrocarbon used is generally 0.1: 1, preferably 0.2: 0.8, in particular 0.3: 0.7 during thermal cracking.
  • heated air or a heated mixture of air and oxygen is passed through the cracked gas cooler to be decoked for thermal decoking of the cracked gas cooler.
  • the volume ratio of air to oxygen is generally 100: 1 to 1: 100, preferably 100: 1 to 1:50, in particular 100: 1 to 1:10 however, because of the easy availability, use heated air alone without additional oxygen for decoking.
  • the cracked gas cooler inlet temperature for the heated air or the air / oxygen mixture is generally 600 to 1100 ° C., preferably 700 to 1050 ° C., in particular 800 to 1000 ° C.
  • the decoking can be done while maintaining a slightly reduced pressure in the cracked gas cooler, e.g. B. in the range of 0.5 to 1 bar.
  • atmospheric pressure or increased pressure are used in the cracked gas cooler.
  • the pressures are expediently 1 to 50 bar, preferably 1 to 20 bar, in particular 1 to 10 bar.
  • elevated pressures of 2 to 50 bar, preferably 5 to 40 bar.
  • a steam pressure of at least 80 bar expediently from 80 to 160 bar, preferably 90 to 150 bar, in particular 100 to 130 bar, is maintained in the cracked gas cooler on the boiling water side.
  • the ratio of the amount of heated air or the heated air / oxygen mixture passed through per hour during the thermal decoking to the amount of hydrocarbon passed through per hour during the thermal cracking is 0.05 to 5, preferably 0.1 to 3 , in particular 0.1 to 2.
  • the cracked gas cooler is decoked to such an extent that the exit temperature of the cracked gas from the cracked gas cooler corresponds to the initial value of the exit temperature of the cracked gas cooler from the cracked gas cooler at the start of the first start-up of the cracked gas cooler or after mechanical cleaning of the cracked gas cooler.
  • the cracked gas cooler is completely freed of the coke after about 20 to 30 hours and then has the above-mentioned initial value of the starting temperature of the cracked gas after restarting.
  • the course and completion of the decoking process can be followed in a simple manner by determining the carbon dioxide concentration in the gas mixture introduced into the cracked gas cooler and the gas mixture emerging from the spa gas cooler.
  • the air or the air / oxygen mixture can be heated to the cracked gas cooler inlet temperatures in a separate oven, bypassing the cracking furnace or tubes belonging to the cracked gas cooler, and passed through the cracked gas cooler.
  • the air or the air / oxygen mixture in the associated tubular cracking furnaces is preferably heated to the inlet temperature for the cracked gas cooler and passed through the downstream cracked gas cooler.
  • the cracked tubes of the upstream tube cracking furnace are first decoked. This is expediently carried out in such a way that, after the addition of the hydrocarbon to be split has been prevented, a water vapor / air mixture is passed through the indirectly heated cracking tubes of the tube cracking furnace and at the same time through the downstream cracking gas cooler, and after the decoking of the cracking tubes of the tube cracking furnace has ended, the water vapor supply is prevented and only air or the air / oxygen mixture are passed through the indirectly heated gap tube of the tubular furnace and the downstream gap gas cooler.
  • outlet temperatures for the gas mixture leaving the tube cracking furnace are generally used, between 600 and 1 100 ° C, preferably between 700 to 1 050 ° C, in particular between 700 and 900 ° C.
  • the water vapor / air mixture used expediently has a weight ratio of water vapor to air of 100: 1 to 2: 8, preferably 9: 1 to 3: 7, expediently using a water vapor / air mixture with a very low air content , e.g. B. less than 10 wt.% Air, or water vapor alone begins and then admixing increasing amounts of air, for. B. up to a content of air in the water vapor / air mixture of 70 wt.%.
  • a mixture of 2.2 t / h of a gasoline fraction (naphtha) with a boiling range of 40 to 180 ° C and 1.05 t / h of water vapor is passed through in a tube gap furnace, which contains four canned tubes, and at an oven outlet temperature of 850 ° C split.
  • the cracked gas from 2 cracked tubes is cooled in a downstream cracked gas cooler.
  • the cooler outlet temperature is 350 ° C.
  • This cracked gas cooler outlet temperature finally increases after several months of operation to 450 ° C, the highest outlet temperature permitted for the cracked gas cooler.
  • the hydrocarbon flow through the tube cracking furnace is interrupted and the cracked tubes and the cracked gas cooler are decoked in a conventional manner by passing a water vapor / air mixture through the cracked tubes and the downstream cracked gas cooler.
  • 1.0 t / h of water vapor and 0.08 t / h of air are initially passed through each can.
  • the air throughput is slowly increased and the water vapor throughput is reduced until finally a water vapor / air mixture with 70 vol.% Air is passed through each can. This state is maintained for a further 6 hours, so that the entire decoking process takes 16 hours.
  • the tubular cracking furnace is operated as described in the first paragraph of the comparative example, initially to produce the cracked gas with the addition of naphtha and water vapor and, after reaching the maximum permissible cracked gas cooler outlet temperature of 450 ° C., is subjected to the decoking of 16 hours described in the first paragraph of the comparative example.
  • the water vapor throughput is then completely prevented and only air in an amount of 1.3 t / h per can is passed through. This corresponds to a weight ratio of 0.59 of the amount of air passed per hour per can to the amount of hydrocarbon passed per hour during the thermal cracking.
  • a furnace outlet temperature of 850 ° C is maintained.
  • a cracked gas cooler outlet temperature of 335 ° C is reached.
  • High pressure steam of 125 bar continues to be generated during these 30 hours.
  • the tube cracking furnace without cooling down, is again passed through by passing 2.2 t / h of naphtha and 1.05 t / h of steam each Canned tube put into operation.
  • 2.2 t / h of gas oil and 1.7 t / h of water vapor are split in a tube cracking furnace at a furnace exit temperature of 830 ° C.
  • the cracked gas cooler outlet temperature in the clean state is 550 ° C with a steam pressure on the water side of 125 bar.
  • the cracked gas cooler outlet temperature rises to 650 ° C, the highest outlet temperature permitted for the cracked gas cooler.
  • the hydrocarbon stream is interrupted and, as described in the example and in the comparative example, first a mixture of water vapor and air with a slowly increasing air content (until a water vapor / air mixture with 70 vol.% Air is reached) through the can and the downstream Split gas cooler directed.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Claims (4)

1. Procédé pour le décokage thermique de réfrigérants de gaz de craquage, utilisés pour le refroidissement indirect, au moyen d'eau, de gaz de craquage contenant de l'éthylène qui sont obtenus par craquage thermique d'hydrocarbures, en présence de vapeur d'eau, dans un four tubulaire de craquage à chauffage indirect, à des températures de sortie des gaz de craquage de plus de 750 °C, caractérisé en ce que de l'air chauffé ou un mélange chauffé d'air et d'oxygène est envoyé à travers les tubes à décoker du réfrigérant des gaz de craquage et, dans ces conditions, une pression de vapeur d'au moins 80 bars est maintenue dans le réfrigérant des gaz de craquage, du côté de l'eau bouillante.
2. Procédé selon la revendication 1, caractérisé en ce que le réfrigérant des gaz de craquage est décoké dans une mesure suffisante pour que la température du gaz de craquage à la sortie du réfrigérant des gaz de craquage corresponde à la valeur initiale de la température du gaz de craquage à la sortie du réfrigérant des gaz de craquage au début de la première mise en service du réfrigérant des gaz de craquage ou à la suite d'un nettoyage mécanique du réfrigérant des gaz de craquage.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que le rapport de la quantité pondérale d'air chauffé ou du mélange d'air/oxygène chauffé, passée par heure pendant le décokage thermique, à la quantité d'hydrocarbure passée par heure pendant le craquage thermique est compris entre 0,05 et 5.
4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce qu'avant le décokage thermique du réfrigérant des gaz de craquage, les tubes de craquage du four tubulaire de craquage placé en amont subissent tout d'abord un décokage consistant en ce qu'après l'interruption de l'arrivée de l'hydrocarbure à craquer, un mélange de vapeur d'eau/air est envoyé à travers les tubes de craquage à chauffage indirect du four tubulaire de craquage et à travers le réfrigérant des gaz de craquage placé en aval, et, après l'achèvement du décokage des tubes de craquage du four tubulaire de craquage, l'arrivée de vapeur d'eau est interrompue et il n'est plus envoyé que de l'air ou un mélange d'air/oxygène à travers les tubes de craquage à chauffage indirect du four tubulaire de craquage et à travers le réfrigérant des gaz de craquage placé en aval.
EP81101665A 1980-03-15 1981-03-07 Procédé de décokage de refroidisseurs de gaz craqués Expired EP0036151B2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81101665T ATE5891T1 (de) 1980-03-15 1981-03-07 Verfahren zur thermischen entkokung von spaltgaskuehlern.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3010000 1980-03-15
DE19803010000 DE3010000A1 (de) 1980-03-15 1980-03-15 Verfahren zur thermischen entkokung von spaltgaskuehlern

Publications (3)

Publication Number Publication Date
EP0036151A1 EP0036151A1 (fr) 1981-09-23
EP0036151B1 true EP0036151B1 (fr) 1984-01-18
EP0036151B2 EP0036151B2 (fr) 1987-05-13

Family

ID=6097306

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81101665A Expired EP0036151B2 (fr) 1980-03-15 1981-03-07 Procédé de décokage de refroidisseurs de gaz craqués

Country Status (7)

Country Link
US (1) US4420343A (fr)
EP (1) EP0036151B2 (fr)
JP (1) JPS56142217A (fr)
AT (1) ATE5891T1 (fr)
AU (1) AU540068B2 (fr)
CA (1) CA1164385A (fr)
DE (2) DE3010000A1 (fr)

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DE4102862A1 (de) * 1991-01-31 1992-08-06 Linde Ag Verfahren zur entkokung von spaltoefen
KR940009317A (ko) * 1992-10-05 1994-05-20 알버트 어네스트 가레드 공기 펄스를 이용한 코크스제거 방법
DE4335711C1 (de) * 1993-10-20 1994-11-24 Schmidt Sche Heissdampf Verfahren zur thermischen Entkokung eines Spaltofens und des nachgeschalteten Spaltgaskühlers
FR2728578A1 (fr) * 1994-12-26 1996-06-28 Inst Francais Du Petrole Procede de vapocraquage flexible et installation de vapocraquage correspondante
FR2750140B1 (fr) * 1996-06-25 1998-08-07 Inst Francais Du Petrole Installation de vapocraquage avec moyens de protection contre l'erosion
US6113774A (en) * 1998-05-22 2000-09-05 Phillips Petroleum Company Antifoulant control process
FR2837273B1 (fr) * 2002-03-15 2004-10-22 Inst Francais Du Petrole Procede d'elimination au moins partielle de depots carbones dans un echangeur de chaleur
US7763162B2 (en) * 2005-07-08 2010-07-27 Exxonmobil Chemical Patents Inc. Method for processing hydrocarbon pyrolysis effluent
US7465388B2 (en) * 2005-07-08 2008-12-16 Exxonmobil Chemical Patents Inc. Method for processing hydrocarbon pyrolysis effluent
US8524070B2 (en) * 2005-07-08 2013-09-03 Exxonmobil Chemical Patents Inc. Method for processing hydrocarbon pyrolysis effluent
US7780843B2 (en) * 2005-07-08 2010-08-24 ExxonMobil Chemical Company Patents Inc. Method for processing hydrocarbon pyrolysis effluent
US7749372B2 (en) * 2005-07-08 2010-07-06 Exxonmobil Chemical Patents Inc. Method for processing hydrocarbon pyrolysis effluent
CN100425940C (zh) * 2005-10-21 2008-10-15 中国石油化工股份有限公司 一种大型管壳类换热设备管束的高温裂解除垢设备及除垢方法
DE102007048984A1 (de) 2007-10-12 2009-04-16 Linde Aktiengesellschaft Verfahren zur Entkokung von Spaltöfen
FR3011556B1 (fr) * 2013-10-09 2015-12-25 Commissariat Energie Atomique Procede de purification d'un gaz de synthese brut issu d'une pyrolyse et/ou gazeification d'une charge de matiere carbonee par destruction de goudrons contenus dans le gaz
CN104327904A (zh) * 2014-10-30 2015-02-04 北京晟辉兴业科技有限公司 一种液态锅炉结焦抑制剂
WO2024089443A1 (fr) * 2022-10-25 2024-05-02 Dow Global Technologies Llc Procédé de décokage d'un four de craquage

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US2057441A (en) * 1935-05-15 1936-10-13 Texas Co Method of burning coke from heater tubes
US2289350A (en) * 1937-12-29 1942-07-14 Texas Co Method of reconditioning furnace tubes
US2289351A (en) * 1939-04-06 1942-07-14 Texas Co Method of cleaning heater tubes
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FR1532127A (fr) * 1966-07-25 1968-07-05 Idemitsu Petrochemical Co Procédé perfectionné pour enlever les dépôts de carbone des appareils de craquage thermique
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US3764634A (en) * 1969-04-23 1973-10-09 Mitsui Shipbuilding Eng Process and apparatus for preparing lower olefins
EP0021167B1 (fr) * 1979-06-08 1982-03-03 Linde Aktiengesellschaft Procédé et dispositif pour le décokage thermique d'un réacteur de craquage thermique d'hydrocarbures, le reacteur comportant une zone de craquage et un refroidisseur pour le gaz de craquage

Also Published As

Publication number Publication date
ATE5891T1 (de) 1984-02-15
DE3010000A1 (de) 1981-09-24
AU6835381A (en) 1981-09-24
JPH0113515B2 (fr) 1989-03-07
EP0036151A1 (fr) 1981-09-23
JPS56142217A (en) 1981-11-06
DE3161916D1 (en) 1984-02-23
CA1164385A (fr) 1984-03-27
EP0036151B2 (fr) 1987-05-13
US4420343A (en) 1983-12-13
AU540068B2 (en) 1984-11-01

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