US3323903A - Method and apparatus for decomposing metal compounds - Google Patents

Method and apparatus for decomposing metal compounds Download PDF

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Publication number
US3323903A
US3323903A US416045A US41604564A US3323903A US 3323903 A US3323903 A US 3323903A US 416045 A US416045 A US 416045A US 41604564 A US41604564 A US 41604564A US 3323903 A US3323903 A US 3323903A
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Prior art keywords
metal
powder
carbonyl
stream
decomposing
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US416045A
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English (en)
Inventor
Charles E O'neill
Michael D Head
Charles B Goodrich
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Huntington Alloys Corp
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International Nickel Co Inc
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Filing date
Publication date
Application filed by International Nickel Co Inc filed Critical International Nickel Co Inc
Priority to US416045A priority Critical patent/US3323903A/en
Priority to DE19651483147 priority patent/DE1483147A1/de
Priority to FR40573A priority patent/FR1468968A/fr
Priority to NO160735A priority patent/NO116340B/no
Priority to BE673235D priority patent/BE673235A/xx
Priority to NL6515753A priority patent/NL6515753A/xx
Priority to GB51727/65A priority patent/GB1056809A/en
Priority to US646783A priority patent/US3409281A/en
Application granted granted Critical
Publication of US3323903A publication Critical patent/US3323903A/en
Priority to NO461168A priority patent/NO120092B/no
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/20—Dry methods smelting of sulfides or formation of mattes from metal carbonyls
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B15/00—Other processes for the manufacture of iron from iron compounds
    • C21B15/04—Other processes for the manufacture of iron from iron compounds from iron carbonyl

Definitions

  • the present invention is directed to a method and apparatus for decomposing metal carbonyls and, more particularly, to a method for decomposing vapors of metal carbonyls at high production rates.
  • the decomposition of metal carbonyls in the vapor phase to produce powders from the corresponding metals has long been known.
  • the method which has been widely used for many years has involved a stationary decomposer wherein the metal carbonyl vapor, e.g., iron carbonyl or nickel carbonyl, is introduced into the top of a cylindrical chamber and wherein all the requisite heat to effect the decomposition of the carbonyl is introduced through the side walls of the chamber such that decomposition of the metal carbonyl to carbon monoxide and the corresponding metal takes place during passage of the vapor downwardly through the decomposing chamber.
  • the product of such decomposition comprises a metal powder of high purity.
  • the process is attended by a relatively low production rate and a high investment in plant would be needed to provide the multiplicity of units required to support a large tonnage operation.
  • the powders produced tend to be quite fine and angular and such powders normally do not have the flow characteristics which are desired in some powder metallurgy and other applications involving the use of metal powder.
  • the present invention contemplates a method for decomposing a metal carbonyl, of such elements as nickel, iron, cobalt, chromium, tungsten and molybdenum, on a substantially continuous basis at a high production rate of decomposed metal
  • a metal carbonyl decomposing zone and a powder heating zone
  • circulating a stream of hot powdered material suspended in a gas between and through said heating zone and said decomposing zone introducing a stream of metal carbonyl to be decomposed into said decomposing zone concurrently with the hot suspended powdered material from said heating zone such that heat contained in said hot suspended powder stream entering said decomposing zone decomposes metal carbonyl in said decomposing zone.
  • product powder and carbon monoxide advantageously are removed from said circulating stream at a rate substantially equal on a weight basis to the rate of introduction of metal carbonyl.
  • the invention also contemplates an apparatus for decomposing metal carbonyl at a high production rate cc-m-' prising a decomposing chamber, a heating chamber, conduit means connecting said heating chamber and said decomposing chamber, circulating means located in said conduit means for circulating a stream of powdered material suspended in a gas between said decomposing chamber and said heating chamber and mixing means for mixing a stream of metal carbonyl and a stream of powdered material suspended in gas adjacent the points of entry of said streams into said decomposing chamber.
  • the cross-sectional area of the decomposer may be enlarged as compared to the cross-sectional area of the circulating stream of powder-laden gas such that the arrangement of the nozzles employed to introduce materials into the decomposer is facilitated and the velocity of gas through the decomposer is reduced.
  • an increase in cross section of the decomposer chamber itself may be unnecessary.
  • the heat required to eflect decomposition of metal carbonyl in the decomposer is primarily imparted by heat exchanger means, external to the decomposer, to the circulating stream of powdered material suspended in gas.
  • the heat required for decomposing the metal carbonyl in the decomposer is interchanged between the heated particles and the carbonyl in the decomposer.
  • suspended particles which may be metallic powder or nonmetallic powder having a melting point exceeding the temperature in the powder heating zone, greatly increases the heat capacity of the gas stream as compared to a similar stream of gas without the suspended particles.
  • Satisfactory metal powders include nickel, iron, chromium, copper, aluminum, magnesium, silicon, etc.
  • satisfactory non-metallic powders include alumina, magnesia, silica, thoria, graphite, refractory carbides, nitrides, silicides, borides, etc.
  • the particulate or powdered material employed in the circulating gas stream has a range of particle sizes such that it is suspendable in, and conveyable by, the gas stream.
  • the particles in the circulating gas stream may have particle sizes in the range from submicron sizes up to about 50 microns, e.g., about 0.01 micron to about microns, and advantageously about 0.1 to 10 microns.
  • Particle loadings in the circulating gas stream can be quite high, e.g., up to about :1 on a weight basis depending upon practical operating conditions, including particle density, particle size, gas velocity in the circuit outside the decomposer, etc.
  • the powder loading in the circulating carbon monoxide stream in the case of nickel or iron powder having a particle size of about 1 to about 10 microns is maintained at a Weight ratio of powder to gas of at least about 1:1 up to about 40:1 or
  • decomposition of the metal carbonyl is effected substantially completely in the decomposer.
  • the stream of powder-laden gas which is removed from the decomposer can be carried through the heat exchanger under conditions such that no plating of the heat exchanger and associated apparatus results.
  • the production rate is dependent upon the heat supplied to the decomposer through the medium of the heated metal particles or metal-coated particles borne in the circulating gas stream.
  • the rate of supply of metal carbonyl to be decomposed is coordinated with the heat content of the particleladen gas stream which is mixed with the metal carbonyl in the decomposer.
  • reference character 11 depicts a decomposing chamber and reference character 12 depicts a heat exchanger which may be, for example, made of a bundle of tubes so as to provide a high heat exchange area.
  • Decomposer chamber and heat exchanger are connected by means of ducts 14 and 15 for circulating powderladen gas therebetween.
  • a fan 13 is located in duct 14 to pull a stream of powder-laden gas, e.g., carbon monoxide, from the bottom end of decomposer 11 and force the powder-laden stream upwardly through heat exchanger 12 and thence to the upper end of decomposer 11.
  • powder-laden gas e.g., carbon monoxide
  • Means 16 are located in duct 14, advantageously between fan 13 and the inlet for heat exchanger 12,.for classifying the circulating powder and for separating product powder and excess carbon monoxide gas from the circulating system. Such classifying means may be located elsewhere in the circuit as desired in particular operations.
  • the classifier means 16 can be operated to provide a cut of the coarser particles in the system such that particles are removed only when they are built up to a predetermined size. Alternatively, a powder product cu t comprising a controlled mixture of particle sizes including the coarser particles can be taken.
  • a distributor 17 is provided at the top of decomposer 11 to divide the incoming stream of powder-laden gas advantageously into a plurality of substantially equal streams which are led by ducts 18 to the top of decomposer 11.
  • Metal carbonyl is introduced through port 19, which advantageously is water cooled to prevent decomposition of metal carbonyl prior to its entry into the decomposer 11, and mixing of the heated metal powder and the introduced stream of carbonyl is effected in the upper region of decomposer 11.
  • Heat exchanger 12 is provided with a heating fluid inlet at 20 and a heating fluid outlet 21 for inlet and exhaust of heating fluid such as steam, mineral oil, diphenyl, mixtures of diphenyl and diphenyl oxide, a molten salt mixture, hot gas (such as flue gas), etc.
  • the decomposer 11 has a cross-sectional area which is about 250 times as great as the cross-sectional area of the heat exchanger 12.
  • a circulating charge of nickel powder having an average particle size of about five microns suspended in carbon monoxide is established in the system to provide a circulating rate of about 27,000 pounds per hour of nickel powder.
  • the suspended stream is heated from a temperature of about 400 F. to 600 F. in the heat exchanger.
  • Nickel carbonyl vapor is introduced to the decomposer at 19 and is mixed with the distributed streams of hot gas-suspended nickel powder introduced concurrently therewith to efiect substantially complete decomposition of the carbonyl during its downward passage through the decomposer.
  • the operation is conducted on a substantially continuous basis with a production from classifier means 16 of about 500 pounds per hour of nickel powder. In this way, a circulating rate of nickel powder about 50 times as great as the nickel powder product rate is maintained.
  • a nickel powder loading on a weight basis of about 18:1 is maintained in the gas stream and a gas velocity of at least about 60 feet per second, e.g., about feet per second, is maintained in the circuit outside the decomposer.
  • the minimum gas velocity in the system outside the decomposer is maintained at a value sufficient to maintain at least a major portion of the particles in suspension.
  • a lower gas velocity can be employed than is necessary when the powder load comprises heavier particles.
  • a stream of metal carbonyl to be decomposed is introduced to the top of the decomposer and heat for the decomposition of the metal ca-rbonyl is concurrently brought into the decomposer by means of a stream of heated particle-laden gas, e.g., carbon monoxide, which is lead to the decomposer from the heat exchanger.
  • a stream of heated particle-laden gas e.g., carbon monoxide
  • the metal carbonyl introduced through port 19 is nickel carbonyl or iron carbonyl
  • the carbonyl stream can be introduced through port 19 in the vapor form.
  • a boiler not shown in the drawing is employed.
  • the introduction port advantageously is cooled, e.g., by water cooling.
  • the metal carbonyl can be introduced in liquid form through the introduction port 19 and heat for vaporization and decomposition of the metal carbonyl can be provided from the stream of particleladen carbon monoxide introduced concurrently therewith into the decomposer.
  • This technique also provides an advantageous means for effecting the simultaneous decomposition of metal carbonyls including metalcarbonyls which themselves occur in the solid state under ordinary conditions of temperature and pressure.
  • crystalline metal carbonyls such as the carbonyls of cobalt, tungsten, molybdenum and chromium are highly soluble in liquid carbonyls such as nickel carbonyl or iron pentacarbonyl and liquid mixtures of such carbonyls can be introduced into the top of the decomposer.
  • the method and apparatus described hereinbefore can be operated on a substantially continuous basis or batch-Wise.
  • batch-wise operation can be advantageous since the particles comprising the circulating powder load can be built up with chromiumtungstenor molybdenum-containing metal and when the desired amount of such metal has been deposited upon the particles within the circulating powder load the metal carbonyl feed can be changed from a feed containing the carbonyls of chromium, tungsten or molybdenum to a feed consisting only of the carbonyls of iron and/ or nickel to provide a final coating or plating upon the circulating powder such that the powder is protected from oxidation of more oxidizable constituents after removal thereof from the apparatus.
  • the gas employed in the circulating powder-laden stream is generally carbon monoxide.
  • other gases or gas mixtures which are essentially non-oxidizing to the metal product of decomposition, e.g., ammonia, nitrogen, hydrogen, a mixture of carbon dioxide and carbon monoxide, a mixture of hydrogen and water vapor, etc., can be employed.
  • Another technique for introducing solid metal carbonyls into the decomposer in accordance with the invention comprises introducing such carbonyls, e.g., the carbonyls of cobalt, chromium, tungsten and molydenum, iron enneacarbonyl [Fe (CO) iron tetracarbonyl [Fe(CO) cobalt ammonia cobalt carbonyl suspended as a fluidized stream in a non-oxidizing gas such as carbon monoxide.
  • carbonyls e.g., the carbonyls of cobalt, chromium, tungsten and molydenum, iron enneacarbonyl [Fe (CO) iron tetracarbonyl [Fe(CO) cobalt ammonia cobalt carbonyl suspended as a fluidized stream in a non-oxidizing gas such as carbon monoxide.
  • metal carbonyl employed herein includes substituted carbonyls decomposable to metal on heating, e.g., cobalt (II) hexammine bis tetracarbonyl cobaltate (I) [Co(NH [Co(CO') nickel (II) hexammine bis tetracarbonyl hydrogen ferrate (II) a)s] [F )4 ]2 iron (II) hexammine octacarbonyl dife-rrate (I)
  • Other com-pounds decomposable to metal by heat which may be treated in accordance with the invention include nickel formate, copper formate, chromium bis benzene, etc. If desired, a plurality of introduction .ports may be employed for the purpose of introducing a plurality of metal carbonyls, or mixtures thereof, into the decomposer.
  • the compounds to be decomposed in accordance with the invention may be introduced into the decomposer as such or diluted with other materials such as carbon monoxide.
  • materials such as carbon monoxide.
  • iron carbonyl and nickel carbonyl when iron carbonyl and nickel carbonyl are to be decomposed, they may be vaporized in the presence of carbon monoxide and introduced as a stream of vapor in concentrations of at least about 200 grams of metal as carbonyl per cubic meter of gas. The heat losses encountered in operating with lower concentrations of metal carbonyl may become so great that the process becomes uneconomic.
  • the decomposer is operated in the temperature range of about 300 F. to 1000 F. in accordance with the invention. It is advantageous to introduce the metal carbonyl to be decomposed in the center of the decomposer top and to divide the heated particle-laden gas stream into a plurality of streams which are introduced through nozzles into the decomposer at points located advantageously substantially radially and equidistantly about the metal carbonyl introduction port or nozzle. In this manner, good mixing of metal carbonyl and heated particles is efiected and decomposition takes place at a high rate without plating of the decomposer Walls being encountered. Suitable deflection vanes adapted to direct the inlet powder streams and/ or metal carbonyl vapor stream or streams toward each other may be associated with the nozzles employed to introduce the heated powder-laden gas streams into the decomposer.
  • the problem of supplying heat is separated from the operation of the decomposing chamber itself. Furthermore, heat supply at an entirely superior level of magnitude is attained. In addition, great flexibility in operating conditions is achieved. Thus, the powder loading in the circulating gas system, and its heat capacity, can be varied over Wide limits in response to operating requirements. The capability for supplying heat at high input rates to the system is thus provided and a metal production rate of a new order of magnitude can be achieved. In addition, undesirable plating of metal upon the unheated walls of the decomposer chamber is obviated.
  • decomposition of metal carbonyl at a high rate is achieved which is attributable to the intimate mixing of heated powder, e.g., metal powder or metal-coated powder, With the metal carbonyl to be decomposed.
  • heated powder e.g., metal powder or metal-coated powder
  • a minor amount of heat sufficient to offset radiation losses can be introduced directly through the decomposer walls in accordance with the invention.
  • metal powder products produced have greatly superior flow properties as compared to the flow properties of conventional grades of metal powder derived from the decomposition of metal carbonyl.
  • nickel powder produced by means of the circulating system employing nickel powder-laden carbon monoxide as the heat exchange medium flowed readily through a funnel having an opening 0.22 inch in diameter and had an apparent density of about 3.5 grams per cubic centimeter.
  • a conventional grade of carbonyl nickel powder would pass through a funnel having an opening of 0.5 inch only by means of tapping and had an apparent density of about 2.2 grams per cubic centimeter.
  • the advantage of high purity associated with carbonyl nickel powder was still retained in the new powder.
  • the present invention makes possible the production of metal powder and metal-coated powder derived from the decomposition of metal carbonyl on a tonnage basis and makes possible the production of pure metal powders, alloyed powders, and metal-coated powders having controlled compositions and having improved physical properties for use in powder metallurgy and other industries.
  • a vertical-decomposer having an enlarged cross-section as compared to the cross-section of the heat exchanger and connecting conduits has been described herein by way of example, it isto be understood that the decomposer chamber or vessel may take other forms in which, for example, the cross-section of the decomposer is not enlarged as compared to the other passages in the circuit and in which materials pass horizontally therethrough.
  • the decomposer may take the form of a series of tubes each of which is supplied with suspended heated particles and with metal carbonyl to be decomposed.
  • the method for decomposing nickel carbonyl which comprises suspending a quantity of nickel powder in carbon monoxide, heating said suspended nickel powder in a heating zone, mixing a stream of said heated nickel powder with a stream of nickel carbonyl in a decomposing zone to etfect interchange of heat between the heated nickel powder and the nickel carbonyl and to decompose said nickel carbonyl to nickel powder and carbon monoxide, circulating at least a portion of the nickel powder from said decomposing zone to said heating zone to reheat said nickel powder, and circulating at least a portion of said reheated nickel powder to said decomposing zone.
  • the method for decomposing iron carbonyl which comprises suspending a quantity of iron powder in carbon monoxide, heating said suspended iron powder in a heating zone, mixing a stream of said heated iron powder with a stream of iron carbonyl in a decomposing zone to effect interchange of heat between the heated iron powder and the iron carbonyl and to decompose said iron carbonyl to iron powder and carbon monoxide, circulating at least a portion of the iron powder from said decomposing zone to said heating zone to reheat said iron powder, and circulating at least a portion of said reheated iron powder to said decomposing zone.
  • the method for decomposing nickel carbonyl on a substantially continuous basis at a high production rate of decomposed nickel which comprises establishing a nickel carbonyl decomposing zone and a nickel powder heating zone, circulating a stream of nickel powder suspended in a gas which is non-oxidizing to nickel between and through said heating zone and said decomposing zone, introducing a stream of nickel carbonyl to be decomposed into said decomposing zone concurrently with the stream of heated nickel powder from said heating Zone such that heat contained in said nickel powder stream entering said decomposing zone decomposes nickel carbonyl therein and removing nickel powder and carbon monoxide from said circulating stream of suspended nickel powder at a rate substantially equal to the rate of introduction of nickel carbonyl such that the weight of nickel powder in said circulating stream is maintained at a controlled level.
  • the method for decomposing iron carbonyl on a substantially continuous basis at a high production rate of decomposed iron which comprises establishing an iron carbonyl decomposing zone and an iron powder heating zone, circulating a stream of iron powder suspended in a gas non-oxidizing to iron between and through said heating zone and said decomposing zone, introducing a stream of iron carbonyl to be decomposed into said decomposing zone concurrently with the stream of heated iron powder from said heating zone such that heat contained in said iron powder stream entering said decomposing Zone de composes iron carbonyl therein and removing iron powder and carbon monoxide from said circulating streamof suspended iron powder at a rate substantially equalto the rate of introduction of iron carbonyl such that the Weight of iron powder in said circulating stream is maintained at a controlled level.
  • V Y 7 5.
  • the method for decomposing a metal compound which is heat decomposable to yield metal which com prises suspending a quantity of particulate material in a gas which' is non-oxidizing to said metal, heating said suspension of particulate material in a heating zone, mixing a stream of said heated particulate material with a stream of said heat decomposable metal compound in a decomposing zone to effect interchange of heat between said heated particulate material and said heat decomposable metal compound to decompose said compound to 'metal in said decomposing Zone and circulating a gas stream containing particulate material from asid decomposing zone to said heating zone.
  • the method for decomposing a metal compound heat decomposable to metal which comprises establishing a decomposing zone and a heating zone for heating particulate material suspended in a gas stream, circulating a stream of gas laden with particulate material from said heating zone to said decomposing zone, introducing a stream of said metal compound concurrently with said heated particulate material stream into said decomposing zone to substantially decompose said metal compound to metal therein, and circulating a gas stream containing particulate material from said decomposing Zone to said heating zone.
  • the method for decomposing a metal carbonyl from the group consisting of the carbonyls of nickel, iron, cobalt, chromium, tungsten and molybdenum at a high metal powder production rate which comprises suspending a metal powder in a gas which is non-oxidizing to said metal powder, heating the powder-laden gas in a heating zone, circulating the resulting heated powderladen gas to a decomposing zone, introducing a stream of metal carbonyl concurrently with said heated powderladen gas into said decomposing zone to cause mixing of said heated powder-laden gas with said metal carbonyl and to cause substantially complete decomposition of said metal carbonyl to metal powder in said decomposing zone, and circulating a stream of metal powder suspended in gas to said heating zone.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Catalysts (AREA)
US416045A 1964-12-04 1964-12-04 Method and apparatus for decomposing metal compounds Expired - Lifetime US3323903A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US416045A US3323903A (en) 1964-12-04 1964-12-04 Method and apparatus for decomposing metal compounds
DE19651483147 DE1483147A1 (de) 1964-12-04 1965-12-01 Verfahren und Vorrichtung zur Zersetzung von Metallverbindungen
NO160735A NO116340B (de) 1964-12-04 1965-12-02
FR40573A FR1468968A (fr) 1964-12-04 1965-12-02 Procédé de décomposition de composés métalliques et installation pour sa mise en oeuvre
BE673235D BE673235A (de) 1964-12-04 1965-12-03
NL6515753A NL6515753A (de) 1964-12-04 1965-12-03
GB51727/65A GB1056809A (en) 1964-12-04 1965-12-06 Method and apparatus for decomposing metal compounds
US646783A US3409281A (en) 1964-12-04 1967-04-10 Apparatus for decomposing metal compounds
NO461168A NO120092B (de) 1964-12-04 1968-11-20

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Application Number Priority Date Filing Date Title
US416045A US3323903A (en) 1964-12-04 1964-12-04 Method and apparatus for decomposing metal compounds

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US3323903A true US3323903A (en) 1967-06-06

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US416045A Expired - Lifetime US3323903A (en) 1964-12-04 1964-12-04 Method and apparatus for decomposing metal compounds

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US (1) US3323903A (de)
BE (1) BE673235A (de)
DE (1) DE1483147A1 (de)
FR (1) FR1468968A (de)
GB (1) GB1056809A (de)
NL (1) NL6515753A (de)
NO (1) NO116340B (de)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4205979A (en) * 1978-10-10 1980-06-03 Hazen Research, Inc. Process for beneficiating oxide ores
US4239529A (en) * 1979-10-22 1980-12-16 Hazen Research, Inc. Process for beneficiating sulfide ores
US4257881A (en) * 1978-01-10 1981-03-24 Hazen Research, Inc. Process for beneficiating oxide ores
US4276081A (en) * 1978-10-10 1981-06-30 Hazen Research, Inc. Process for beneficiating ores
US4289528A (en) * 1978-07-03 1981-09-15 Hazen Research, Inc. Process for beneficiating sulfide ores
US4289529A (en) * 1978-10-10 1981-09-15 Hazen Research, Inc. Process for beneficiating sulfide ores

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63174798A (ja) * 1987-01-14 1988-07-19 Toyota Motor Corp 肉盛溶接用耐食合金

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4257881A (en) * 1978-01-10 1981-03-24 Hazen Research, Inc. Process for beneficiating oxide ores
US4289528A (en) * 1978-07-03 1981-09-15 Hazen Research, Inc. Process for beneficiating sulfide ores
US4205979A (en) * 1978-10-10 1980-06-03 Hazen Research, Inc. Process for beneficiating oxide ores
US4276081A (en) * 1978-10-10 1981-06-30 Hazen Research, Inc. Process for beneficiating ores
US4289529A (en) * 1978-10-10 1981-09-15 Hazen Research, Inc. Process for beneficiating sulfide ores
US4239529A (en) * 1979-10-22 1980-12-16 Hazen Research, Inc. Process for beneficiating sulfide ores

Also Published As

Publication number Publication date
GB1056809A (en) 1967-02-01
FR1468968A (fr) 1967-02-10
NO116340B (de) 1969-03-10
BE673235A (de) 1966-06-03
DE1483147A1 (de) 1969-05-14
NL6515753A (de) 1966-06-06

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