US3533766A - Process for reforming hydrocarbons under high pressure - Google Patents

Process for reforming hydrocarbons under high pressure Download PDF

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Publication number
US3533766A
US3533766A US635837A US3533766DA US3533766A US 3533766 A US3533766 A US 3533766A US 635837 A US635837 A US 635837A US 3533766D A US3533766D A US 3533766DA US 3533766 A US3533766 A US 3533766A
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Prior art keywords
reforming
bars
gas
catalyst
pressure
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US635837A
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English (en)
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Jean P Gignier
Pierre L Honore
Jacques Quibel
Michel Senes
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Azote et Produits Chimiques SA
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Azote et Produits Chimiques SA
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Priority claimed from FR61061A external-priority patent/FR1492926A/fr
Priority claimed from FR102684A external-priority patent/FR92171E/fr
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/02—Production of hydrogen; Production of gaseous mixtures containing hydrogen
    • C01B3/32—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air
    • C01B3/34—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air by reaction of hydrocarbons with gasifying agents
    • C01B3/38—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air by reaction of hydrocarbons with gasifying agents using catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/02—Production of hydrogen; Production of gaseous mixtures containing hydrogen
    • C01B3/32—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air
    • C01B3/34—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air by reaction of hydrocarbons with gasifying agents
    • C01B3/38—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air by reaction of hydrocarbons with gasifying agents using catalysts
    • C01B3/384—Production of hydrogen; Production of gaseous mixtures containing hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide or air by reaction of hydrocarbons with gasifying agents using catalysts with external heating of the catalyst
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • C01B2203/1047—Group VIII metal catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • C01B2203/1047—Group VIII metal catalysts
    • C01B2203/1052—Nickel or cobalt catalysts

Definitions

  • This invention relates to the catalytic reforming of gaseous and liquid hydrocarbons, particularly methane, propane, butane, residual gases from refining, light and heavy petroleum fractions and fuels, having a final boiling point not greater than 350 C.
  • Hydrocarbons can be converted to fuel and synthesis gas, for example, by cracking, partial combustion or reforming. In reforming the hydrocarbons are reacted with steam, usually in the presence of a catalyst, at relatively high temperatures. The reformed gas can be used as town gas, for the production of hydrogen, for the synthesis of ammonia or methanol or in oxo synthesis reactions.
  • the reaction with the steam is carried out under effective pressures which usually do not exceed 30-40 bars in order to preserve the mechanical stability of the catalyst being used, to obviate the danger of coking and to take into account the mechanical resistance of the reforming tubes and the desired methane content of the reformed gas which normally increases 'with pressure.
  • a process for the catalytic reforming with steam of gaseous and liquid hydrocarbons having a boiling point not greater than 350 C. wherein the process is carried out under an eflective pressure in the range of from 70 to 200 bars.
  • the process of the invention in particular makes it possible to avoid, or appreciably to reduce, all compression of the reformed gas before it is subsequently used in, for example, the low-pressure synthesis of ammonia or as town gas.
  • the process of the invention also makes it possible to use a gas which has been compressed, before the reforming thereof, to a volume smaller than that of the reformed gas or to use a liquid hydrocarbon.
  • the process is applicable to gaseous and liquid hydrocarbons, particularly to the light petroleum fractions, the hydrocarbons being saturated or unsaturated.
  • these hydrocarbons contain from 4 to 12 carbon atoms and, preferably, comprise up to 30% of aromatic hydrocarbons.
  • the reforming reaction is preferably carried out under an effective pressure of the order of 100 bars.
  • the reaction of hydrocarbons with steam is of the free-radical type and, in accordance with a development of the present invention, catalysts have been found which are sufficiently active and selective to lead to the production of reformed gas having a methane content which is between 10 and 15% using steam/carbon mol ratios which are in the range of from 3 to 5; these catalysts are described hereinafter.
  • a reformed gas with a high proportion of methane for example a gas which can be used as a substitute for natural gas, it is possible to operate at steam/ carbon mol ratios of from 1.5 to 3, preferably in the region of 2. It has moreover been confirmed that the catalysts of the present invention do not coke the hydrocarbons in the presence of a steam/carbon mol ratio higher than 1.5 even when operating under high pressures in accordance with the process of the present invention.
  • FIG. 2 of the accompanying drawings The influence of the pressure on the methane content of the reformed gas for a given volumetric velocity, in this case 1, can be seen from FIG. 2 of the accompanying drawings in which figure the pressures (P) expressed in bars, are plotted as abscissae and the methane contents of the reformed gases, expressed as a percentage (CH percent), are plotted as ordinates.
  • the internal diameter of the reforming tubes is advantageously in the range of from 10 to 100 mm. when, in accordance with the present invention, the reforming process is carried out at a pressure in the range of from 70 to 200 bars.
  • the internal diameter of the reforming tubes lies in the range of from 70 to 100 mm.
  • the reforming tubes when working under a pressure of 100 bars, the reforming tubes have an internal diameter which is in the range of from 20 to 60 mm., and when working under a pressure of 200 bars, the internal diameter of the reforming tubes is in the range of from 10 to 50 mm.
  • the effective length of the reforming tubes is in the range of from 6 to 15 metres.
  • tube there is meant not only unitary members but also any tube made up from similar separate units which are Welded or otherwise joined directly together.
  • two tubes connected by a part not containing catalyst and two tubes which although joined together have different diameters and not considered as being a single reforming tube in the present invention but are considered to be two tubes.
  • the influence of the volumetric velocity on the methane content of the reformed gas is small. A threefold increase in the volumetric velocity affects the methane content by less than 30% depending on whether the process is for the reforming of one hydrocarbon or a mixture of hydrocarbons.
  • the volumetric velocity of a liquid hydrocarbon is preferably chosen to be in the range of from 1 to 30 litres per litre of catalyst. The influence of the volumetric velocity on the methane content of the reformed gas can be seen more clearly in FIG. 3 of the pressure do not suffer from mechanical degradation due to the chemical action of the reactants.
  • These catalysts contain, as stabilisers, at least one of potassium oxide, chromium trioxide, sodium oxide and barium oxide in an amount which does not exceed 15% and is preferably accompanying drawing in which figure the volumetric D from 1 to 5% by weight of the catalyst composition.
  • Sevvelocity v, in litres, is plotted as abscissae and the methane eral examples of these new catalyst compositions are content of the reformed gas, expressed as a percentage given in the examples below. (CH percent), is plotted as ordinates for a given pres-
  • the reforming process of the invention offers a further sure, in this case 100 bars. advantage, viz.
  • the mixture to be reformed is introduced tion of different gases at the inlet to the reforming tubes. to the catalyst at a temperature which is in the range of For those hydrocarbons which can be desulphurised by from 300 to 700 C., preferably 500 to 600 C.
  • the temperature of the much carbon with respect to hydrogen, hydrogen recycled reformed gas is in the range of from 500 to 9 0 C, in a suitable proportion is introduced into the reforming preferably 800 to 900 C. tubes.
  • the reformed gas is intended for the prepara- In 4 0f the accompanying drawings there is tion of town gas, air or nitrogen are possibly introduced.
  • 5 th points C C C C represent points in the Obtain, at 100 bars, a g Which is little different from 40 reforming tube at which the temperature is measured by that which is obtained when operating at pressures in the means of thermocouples each situated in a sheath of exegi n f 2 i0 30 bars Under te p a re C n i ternal diameter 9 mm.
  • the reforming tube contained such that it is possible industrially to provide reforming 170 1, of a reforming atalyst having the following tubes at a cost which is of the same order as that of recomposition and designated type A: forming tubes adapted for use at lower pressures, this Nio 9 3 being due to a decrease in the diameter of the reforming M20 tubes and an increase in efiiciency of the catalyst.
  • Z r
  • Su1table catalysts comprise nickel, as the catalytlcally SiO 0 3 active component, on supports comprising refractory c2102 oxides.
  • the catalytically active metal content of these catu alyst compositions is in the range of from 8 to 30% by A series of tests was carried out under an effective presby weight, calculated as nickel oxide. The refractory sure of 100 bars.
  • the rates of flow of hydrocarbon, steam oxides on which the nickel catalyst is supported are one and hydrogen, the proportions of steam used, the temperor more of magnesium oxide, calcium oxide, zirconium tures recorded at the different points C C C and C dioxide, aluminium oxide and silicon dioxide.
  • Advantaand the composition of the reformed gas are set out in geously, the catalyst compositions contain from 0 to 45% the following Table I:
  • present invention also provides catalysts which satisfy the above conditions and which when under a very high lion Chromatographic analyses confirmed that the reformed gas did not contain any C hydrocarbons.
  • Catalysts of type A do not have sufficient mechanical strength to make them suitable for use in industrial opera- EXAMPLE 2
  • the tests carried out in Example 1 were repeated, using a light petroleum fraction of empirical formula C H in a reforming tube identical to that described in Example 1 but containing 170 ml. of a reforming catalyst having the following composition and designated type B:
  • At% 011 Analysis of reformed gas of leaving Catalyst Volumetric At catalyst the type velocity H2O/C CO; 00 Hz CH4 inlet length catalyst Catalysts of type B, like those of type A, do not have sufiicient mechanical strength to enable them to be used in industrial operations in which a long effective life of the catalyst is required.
  • FIG. 6 of the accompanying drawings there is shown curves A and B, which were obtained by plotting the ratio H O/C, in mols, as abscissae against the percentage methane contents (CH percent) of the reformed gas as ordinates, for the case of the catalyst E, the reforming process being carried out at pressures of 100 bars ulated by thermocouples placed in the reforming tube and 30 bars, respectively.
  • the hydrocarbon to be reformed was a light petroleum fraction having a boiling point of 40-140 C.
  • the rate of fiow of this hydrocarbon was 48 litres per hour.
  • the steam ratio, H O/C, was 3 and 0.1 mol of hydrogen per mol of hydrocarbon was recycled.
  • the temperature of the mixture to be reformed on entering the catalyst was 500 C. and that of the mixture leaving the catalyst was 950 C. Under these working conditions, the gas mixture produced had the following composition (based on dry gas):
  • FIG. 7 of the accompanying drawings there are shown diagrammatically embodiments of this installation adapted for different uses of the reformed gas.
  • FIG. 7A of the accompanying drawings is one which can be used for the separation of hydrogen or synthesis gas.
  • the primary reforming combustion is conventional and is carried out at atmospheric pressure.
  • the mixture to be treated arrives by way of the conduit 1 at a primary reforming reactor 2 under a pressure of to 200 bars and the reformed gases leaving at 3 at about 700 to 800 C. contain 10 to 25% of methane.
  • peroxidised air is used if the mixture is intended for the synthesis of ammonia or oxygen is used if it is desired to obtain a nitrogen-free gas.
  • the peroxidised air or the oxygen, which is produced at 4 is united by way of the conduit 5 with the gas which has undergone a primary reforming and these gases are sent by way of the conduit 6 into a secondary reforming reactor 7, where TABLE V Temperatures At rd Analysis of reformed gas of cat- On leav- Volumetric At alyst ing the Test N0. velocity 1120/0 CO2 00 Hz 0H4 inlet length catalyst EXAMPLE 6 their temperature is raised on leaving to 1000 to 1100 C.
  • the methane content of the gases leaving the reactor 7 and flowing through conduit 8 is between 0.1 and 1%.
  • the gases then undergo a high and low temperature conversion at 9 and then a decarbonation at 10.
  • the gases leaving at 12 contain 0.3 to 1% internal diameter of 60 mm., a thickness of 36 mm. and of methane and 0 to 25% of nitrogen, under a pressure of 9 60 to 140 bars, and can be used for obtaining hydrogen or for the preparation of the synthesis gas.
  • the diagram of the installation shows the advantage of a high degree of compactness, due to the reduction in quantities of catalysts for the primary and secondary reforming steps, and for the conversion and methanisation, which are much more active at the working pressure of the installation than at 20 to 30 bars.
  • the result is a saving in investment costs and the possibility of large productions being treated in a single line, i.e., the gas necessary for 1000 to 2000 tons per day of ammonia.
  • FIG. 7B of the accompanying drawings is one which can be used for the preparation of synthesis gas.
  • the gases treated in this installation are light fracitons of petroleum, of natural gas or of refinery gas. These gases, under a pressure of 70 to 200 bars, are introduced through an inlet 13 to a primary reforming reactor 14 and, on leaving the latter at 15, they have a temperature of 700 to 800 C. and contain 10 to 25 of methane.
  • a secondary reforming is carried out at reactor 18 in air, which is introduced by way of conduit 16 into conduit 17 containing the gases which are to be subjected to the secondary reforming.
  • the gases leave the reactor 18 at a temperature of 800 to 900 C. and contain to 15% of methane.
  • FIG. 8C of the accompanying drawings there is shown an installation for the preparation of hydrogen or synthesis gas.
  • the combustion of the primary reforming is effected under pressure, and the vapours are expanded in a turbine.
  • the pressure in reforming tubes 26 is from 70 to 200 bars and, in jacket 27, it is from 50 to 200 bars.
  • the fuel is introduced into jacket 27 at from 50 to 200 bars by way of conduit 28, as is the combustion supporter introduced through conduit 29.
  • the vapours leaving the jacket 27 are expanded from 40 to 140 bars to atmospheric pressure at 30.
  • the gases which have undergone the primary reforming in the reforming tubes 26 have a methane content of 0.5 to and are at a temperature of 850 to 1050 C.
  • the secondary reforming is carried out in air, oxygen or peroxidised air which is introduced by way of the conduit 31.
  • the gases originating from the primary reforming step and the air, oxygen or peroxidised gas are conveyed to the secondary reforming reactor 33 through conduit 32. After the double reforming, the gases leave at a temperature between 950 and 1100" C. and contain from 0.1 to 2% of methane.
  • FIG. SD of the accompanying drawings there is shown an installation in which, for the purpose of limiting the thickness of the tubes and making this installation even more compact, the primary and secondary reforming steps are carried out in the same chamber, the combustion supporter being peroxidised air or oxygen.
  • This installation is intended for the preparation of synthesis gas or oxygen.
  • the combustion supporter being either peroxidised air or oxygen, is produced in 35 and introduced under a pressure of 70 to 150 bars and through pipe 36 into jacket 37.
  • the primary reforming of the gases introduced under a pressure of 70 to 150 bars, takes place in reforming tubes 38.
  • the treated gases are introduced bymeans of the tube 39 into the secondary reforming chamber 37, and the gas leaving at 40 is at a temperature of 950 to 1100 C. and its methane content is from 0.5 to 1%.
  • the catalytic reactions are carried out both inside and outside the tubes.
  • catalyst support comprises up to 25% by weight of calcium oxide based on the total weight of catalyst composition.
  • said catalyst composition further comprises at least one stabilizer selected from the group consisting of potassium oxide, chromium trioxide, sodium oxide and barium oxide, said stabilizer being present in an amount not exceeding 15% by weight of the catalyst composition.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Hydrogen, Water And Hydrids (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US635837A 1966-05-11 1967-05-03 Process for reforming hydrocarbons under high pressure Expired - Lifetime US3533766A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR61061A FR1492926A (fr) 1966-05-11 1966-05-11 Procédé de reformage sous haute pression des hydrocarbures
FR102684A FR92171E (fr) 1967-04-14 1967-04-14 Procédé de reformage sous haute pression des hydrocarbures

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BE (1) BE698289A (ref)
DE (1) DE1645861A1 (ref)
ES (1) ES340242A1 (ref)
GB (1) GB1189001A (ref)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4005031A (en) * 1973-04-11 1977-01-25 Hoffmann-La Roche Inc. Nickel peroxide oxidizing agent
US4451578A (en) * 1982-04-26 1984-05-29 United Technologies Corporation Iron oxide catalyst for steam reforming
US4452915A (en) * 1977-12-22 1984-06-05 General Electric Company Nickel oxide catalyst supported on magnesium for the selective ortho-alkylation of phenolic compounds with an alkane
RU2553457C1 (ru) * 2013-11-08 2015-06-20 Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) Катализатор паровой конверсии углеводородов и способ его получения
US20220009773A1 (en) * 2020-07-07 2022-01-13 Proteum Energy, Llc Method and system for converting non-methane hydrocarbons to recover hydrogen gas and/or methane gas therefrom

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3501460A1 (de) * 1985-01-17 1986-07-17 Linde Ag, 6200 Wiesbaden Verfahren zur erzeugung von h(pfeil abwaerts)2(pfeil abwaerts)/co-synthesegas
GB2188061B (en) * 1986-03-21 1989-11-15 British Gas Plc Production of methane-containing gases

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2028326A (en) * 1931-01-23 1936-01-21 Standard Oil Dev Co Apparatus for the production of hydrogen
GB772787A (en) * 1952-02-19 1957-04-17 Azote Office Nat Ind Improvements in or relating to processes for the manufacture of gases containing hydrogen by a conversion of hydrocarbons
US3119667A (en) * 1961-01-31 1964-01-28 Pullman Inc Process for hydrogen production
US3132010A (en) * 1962-11-08 1964-05-05 Pullman Inc Reforming of gaseous hydrocarbons
US3186797A (en) * 1961-08-16 1965-06-01 Ici Ltd Process for catalytically steam reforming hydrocarbons
US3201214A (en) * 1963-02-01 1965-08-17 Pullman Inc Production of domestic heating gas
US3278268A (en) * 1962-08-15 1966-10-11 Engelhard Ind Inc Method for hydrogen production
US3285713A (en) * 1962-12-18 1966-11-15 Basf Ag Tube reactors
US3385670A (en) * 1964-12-29 1968-05-28 Pullman Inc Steam reforming of hydrocarbons and catalyst therefor containing a cobalt component on a zirconia support
US3394086A (en) * 1964-05-04 1968-07-23 Exxon Research Engineering Co Selective partial conversion of naphtha hydrocarbons to hydrogen
US3420643A (en) * 1965-08-24 1969-01-07 Azote & Prod Chim Method for reforming light petrol fractions under pressure

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2028326A (en) * 1931-01-23 1936-01-21 Standard Oil Dev Co Apparatus for the production of hydrogen
GB772787A (en) * 1952-02-19 1957-04-17 Azote Office Nat Ind Improvements in or relating to processes for the manufacture of gases containing hydrogen by a conversion of hydrocarbons
US3119667A (en) * 1961-01-31 1964-01-28 Pullman Inc Process for hydrogen production
US3186797A (en) * 1961-08-16 1965-06-01 Ici Ltd Process for catalytically steam reforming hydrocarbons
US3278268A (en) * 1962-08-15 1966-10-11 Engelhard Ind Inc Method for hydrogen production
US3132010A (en) * 1962-11-08 1964-05-05 Pullman Inc Reforming of gaseous hydrocarbons
US3285713A (en) * 1962-12-18 1966-11-15 Basf Ag Tube reactors
US3201214A (en) * 1963-02-01 1965-08-17 Pullman Inc Production of domestic heating gas
US3394086A (en) * 1964-05-04 1968-07-23 Exxon Research Engineering Co Selective partial conversion of naphtha hydrocarbons to hydrogen
US3385670A (en) * 1964-12-29 1968-05-28 Pullman Inc Steam reforming of hydrocarbons and catalyst therefor containing a cobalt component on a zirconia support
US3420643A (en) * 1965-08-24 1969-01-07 Azote & Prod Chim Method for reforming light petrol fractions under pressure

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4005031A (en) * 1973-04-11 1977-01-25 Hoffmann-La Roche Inc. Nickel peroxide oxidizing agent
US4452915A (en) * 1977-12-22 1984-06-05 General Electric Company Nickel oxide catalyst supported on magnesium for the selective ortho-alkylation of phenolic compounds with an alkane
US4451578A (en) * 1982-04-26 1984-05-29 United Technologies Corporation Iron oxide catalyst for steam reforming
RU2553457C1 (ru) * 2013-11-08 2015-06-20 Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) Катализатор паровой конверсии углеводородов и способ его получения
US20220009773A1 (en) * 2020-07-07 2022-01-13 Proteum Energy, Llc Method and system for converting non-methane hydrocarbons to recover hydrogen gas and/or methane gas therefrom
US12024429B2 (en) * 2020-07-07 2024-07-02 Proteum Energy, Llc Method and system for converting non-methane hydrocarbons to recover hydrogen gas and/or methane gas therefrom
US12371320B2 (en) 2020-07-07 2025-07-29 Proteum Energy, Llc Method and system for converting non-methane hydrocarbons to recover hydrogen gas and/or methane gas therefrom

Also Published As

Publication number Publication date
GB1189001A (en) 1970-04-22
ES340242A1 (es) 1968-06-01
BE698289A (ref) 1967-11-10
DE1645861A1 (de) 1970-07-09

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