US3433609A - Process for the production of gases containing methane from hydrocarbons - Google Patents

Process for the production of gases containing methane from hydrocarbons Download PDF

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US3433609A
US3433609A US353381A US3433609DA US3433609A US 3433609 A US3433609 A US 3433609A US 353381 A US353381 A US 353381A US 3433609D A US3433609D A US 3433609DA US 3433609 A US3433609 A US 3433609A
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catalyst
bed
nickel
mixture
steam
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US353381A
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English (en)
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George Percival
Thomas Alan Yarwood
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Gas Council
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Gas Council
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
    • B01J8/0446—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical
    • B01J8/0476—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more otherwise shaped beds
    • B01J8/048—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more otherwise shaped beds the beds being superimposed one above the other
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0005—Catalytic processes under superatmospheric pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0207—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly horizontal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
    • B01J8/0257—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical in a cylindrical annular shaped bed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/02—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles
    • B01J2208/021—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles comprising a plurality of beds with flow of reactants in parallel

Definitions

  • This invention is directed to a process for the production of gases containing methane by preparing a mixture of paraftinic hydrocarbons containing an average of 4-15 carbon atoms and steam, preheating the mixture to at least 350 C.
  • the catalyst may contain an oxide, hydroxide or carbonate of an alkali metal or alkaline earth metal or of magnesium.
  • the pressure may be up to 50 atmospheres, but may be higher, if desired. Convenient pressures are within the range of to 25 atmospheres.
  • the proportion of steam relatively to hydrocarbons shall be greater than that which enters into reaction.
  • the excess of steam required for this purpose depends on the average molecular weight of the hydrocarbons used and increases with an increase in molecular weight. However, the excess is not great and 2 parts by weight of steam to 1 part by weight of hydrocarbons can be used with all mixtures of hydrocarbons containing an average of 4 to 10 carbon atoms; a larger proportion, up to 5 parts by weight of steam to 1 part by weight of hydrocarbons may be used if desired. With hydrocarbon mixtures containing an average of 4 to 7 carbon ⁇ atoms the proportion of steam may be as low as 1.5 parts by weight.
  • the gas produced, after the removal of carbon dioxide and water vapour therefrom, will generally contain at least 50 percent by volume of methane, and the concentration of methane may exceed percent under a relatively higher pressure, such as 50 atmospheres.
  • The-catalyst is a coarsely particulate, -for example, granulated or pelleted, nickel alumina catalyst that has for example been prepared by coprecipitating nickel and aluminum compounds by treating an aqueous solution of water-soluble salts, for example, the nitrates, of nickel and aluminum with an alkali, such as sodium carbonate, and reducing the nickel compound in the precipitate to metallic nickel.
  • an alkali such as sodium carbonate
  • the present invention provides a process for the production of gases containing methane from mix-tures of predominantly paraflinic hydrocarbons containing an average 4of 4 to l5 carbon atoms, wherein a mixture of the vapour of the hydrocarbons and steam, at a temperature of at least 350 C. is passed under atmosphereic or superatmospheric pressure at a linear velocity not exceeding 0.3 foot per second (as hereinbefore defined) and a space velocity of at least 400 volumes per volume per hour through a bed of a particulate nickel alumina cat-aylst, whereby the bed is maintained at temperatures of from 400 C. to 600 C. or 575 C. or 550 C., when substantially no carbon deposition takes place on the catalyst. Under normal operating conditions no carbon deposition takes place on the catalyst.
  • the linear velocity is advantageously within the range of 0.01 to 0.3 foot per second.
  • linear velocity is used herein to denote a velocity calculated by measuring the volume of the mixture entering the bed in unit time and the volume of the mixture leaving the bed in unit time, correcting the volumes for the dierence in temperature between the ingoing and outgoing mixtures, taking the mean of these volumes, and calculating the linear velocity from the mean volume (regarding the vessel containing the catalyst as being empty for this calculation).
  • space velocity is used herein to denote the total volume of reactants, adjusted to standard temperature and pressure conditions, passed per hour into the catalyst bed per unit of reactor volume that is packed with catalyst.
  • the average number of carbon atoms in the hydrocarbon mixtures referred to herein is determined by ⁇ determining the average molecular weight of the mixture of hydrocarbons by measuring the depression in the freezing point of pure benzene caused by dissolving a given quantity of the mixture therein, and estimating the number of carbon atoms present in the average hydrocarbon molecule by analysing the mixture by powder chromatography to determine the relative proportions by volume of the parafnic olelinic and aromatic hydrocarbons present in the mixture.
  • An improvement in the process of specification No. 820,257 consists in using a nickel-alumina catalyst of the kind described above, but which contains an addition of an oxide, hydroxide or carbonate of an alkali metal or alkaline earth metal or of magnesium preferably from 0.75 to 8.6 percent calculated as metal on the combined weight of the nickel and alumina. Especially advantageous is an addition of potassium carbonate.
  • the effect of the addition of such alkaline compound is to increase the life of the catalyst.
  • the process of the present invention may be carried out with such a catalyst or with a nickel-alumina catalyst containing no addition of an alkaline compound as aforesaid.
  • the catalyst bed may take the form of a plurality of beds through which the gaseous mixture is passed in parallel.
  • the catalyst bed may be of an elongated, tubular form through which the gaseous mixture is passed in a radial direction from the inner periphery of the bed to the outer periphery thereof or in the reverse direction. If desired, a plurality of such tubular beds may be used through which the gaseous mixture is passed in parallel.
  • the catalyst in the form of particles having a size within the range of 150 to 1,000 microns, which is considerably smaller than the size generally used with the usual linear velocities, for example, particles of 1A to 1/6 inch at linear velocities of 1 to 2 feet per second.
  • the effect of using catalyst particles of the aforesaid small size is to increase the life of the catalyst, as indicated by the period from the initial introduction of the hydrocarbon-steam mixture into the catalyst bed to the time at which undecomposed hydrocarbon is lirst detected in the issuing gases, as compared with the use of larger particles at velocities not exceeding 0.3 feet per second and at the usual high velocities.
  • the preferred proportion of metallic nickel in the catalyst was within the range of 28 to 75 percent calculated on the combined weight of metallic nickel and alumina.
  • Nickel-alumina catalysts having nickel contents higher than 75 percent are of somewhat lower mechanical strength, so that at the usual linear velocities there is a risk of disintegration of the particles and dust formation and a consequent increase in the resistance of the bed to the flow of gases therethrough. This applies not only to the nickel-alumina catalysts containing an addition of an alkaline compound, but also to nickel-alumina catalysts having no such addition.
  • nickel-alumina catalysts which have been prepared by coprecipitation followed by reduction of the nickel compound as referred to above, and which contain a proportion of metallic nickel higher than 75 and not more than 90 percent calculatd on the combined weight of the nickel and alumina.
  • These catalysts may or may not contain an addition of an alkaline compound as described above.
  • the proportion of nickel is preferably within the range of 80 to 85 percent calculated on the above basis.
  • Catalysts having the aforesaid higher nickel contents also have the advantage that the cost of recovering the nickel from such catalysts, when they have to be replaced or for any other reason, is lower than for catalysts having lower nickel contents.
  • FIGURE l shows in longitudinal section a pressure vessel having a plurality of catalyst beds through which the gaseous mixture is passed in parallel, and
  • FIGURE 2 shows in longitudinal section a pressure vessel containing a catalyst bed of tubular form through which the gaseous mixture is passed in a radial direction from the interior to the exterior of the bed.
  • a pressure vessel 1 is provided with a centrally arranged tube 2, which is open at the top and closed at the bottom, and is surrounded by a casing 3.
  • a plurality of catalyst units 4 each of which consists of a perforated tray 5 and a partition 6 above, and a partition 7 below the tray, the partitions being joined to the tube 2 and casing 3 in a gas-tight manner.
  • the partition 6 constitutes the top of the casing 3.
  • Each tray 5 supports a catalyst bed 8 of a convenient depth.
  • the preheated mixture of hydrocarbon vapour and steam is introduced into the tube 2 at 9, and is divided into parallel streams that pass through ports 10 in the tube 2 into the spaces above the catalyst in the units 4.
  • Each gaseous stream passes downwardly through a catalyst bed into the space beneath the latter and emerges through ports 11 in the casing 3 into an annular space 12, where the streams unite and nally issue from the pressure vessel through its outlet 13.
  • the partitions 6 and 7 ensure the flow of the gas along the required path. Instead of providing two partitions between each pair of adjacent units 4, a single partition may be used to serve both as an upper and a lower partition.
  • the tube 2 may be open at the bottom and closed at the top, so that the mixture of hydrocarbon vapour and steam is introduced into the bottom of the tube.
  • the product gases may issue from the top or the bottom of the pressure vessel.
  • a pressure vessel 20 is provided with a centrally arranged catalyst carrier 21 which is formed by two coaxial Iperforated tubular members 22 and 23, which may be right cylinders or frustra of cones.
  • the inner member 22 communicates at its upper end with a gas inlet 24 at the top of the pressure vessel, and is closed at the lower end.
  • the annular space 25 bounded by the members 22 and 23 is closed at the bottom, so that gas 'is constrained to flow radially outwards therethrough.
  • the pressure vessel 20 is provided at its lower end with a gas outlet 26.
  • the annular space 25 is filled with catalyst, and the preheated mixture of hydrocarbon vapour and steam is introduced through the inlet 24.
  • the mixture passes radially outwards through the catalyst bed into an outer annular space 27 within the pressure vessel, and issues from the latter through the outlet 26.
  • the pressure vessel may be arranged vertically as shown in FIGURE 2, or it may be arranged horizontally or in any other convenient posi- EXAMPLE 1
  • a granulated nickel-alumina catalyst was used that had been prepared in the manner described in Example 2 without the addition of potassium carbonate.
  • the catalyst had the following composition:
  • a light petroleum distillate having an average number of carbon atoms of 5.8, a boiling range of 40 C. to 97 C., and specific gravity of ⁇ 0.67 at 20 C. was used.
  • a mixture of 1 part by weight of the vapour of the distillate and 2 parts by Weight of steam was preheated to 450 C. and passed under 25 atmospheres pressure through a bed of the aforesaid catalyst having a depth of 6 inches. The mixture was passed through the bed at a space velocity of 4,000 volumes per Volume per hour and a linear velocity of 0.075 foot per second.
  • the precipitate is partially dried by suction, and the resulting paste thoroughly mixed with an aqueous solution of 106 grams per litre of potassium carbonate.
  • the mixture is then dried in an oven at 110 C., granulated to the required particle size and then heated in a stream of hydrogen to reduce the nickel compounds to metallic nickel.
  • the catalyst had the following composition, the quantities being by weight:
  • the granulated catalyst was sieved to the particle size given below.
  • the granulated catalysts were sieved to a size range of 500-850 microns.
  • a process as claimed in claim 1 wherein the pressure is from 10 to 25 atmospheres.
  • a process as claimed in claim 4 wherein the catalyst beds circumscribe a central supply duct at intervals along its length and are themselves surrounded by an annular exhaust duct, and communication mea-ns being provided between said central supply duct and each of said catalyst beds and between said annular exhaust duct and each of said catalyst beds and said mixture of hydrocarbon vapor and steam passes ⁇ from the supply duct through each catalyst bed into the exfhaust duct.
  • thc nickelalumina catalyst contains an addition of a compound selected from the group consisting of oxide, hydroxide and carbonate of a metal selected from the group consisting of alkali metals and alkaline earth metals.
  • a process as claimed in claim 1 wherein the nickelalumina catalyst has a particle size within the range of about 150 microns to about 1,000 microns.
  • nickelalum'ina catalyst contains vfrom 75 to 90 percent by weight of nickel based on the combined weight of nickel and alumina.
  • a pressure of from 1 to 50 atmospheres pressure at a linear velocity of not more than about 0.15 foot per second and a space velocity of at least 400 volumes per volume per hour through a bed of a nickel-alumina catalyst prepared by coprecipitation followed by reduction of the nickel compounds in the coprecipitate to metallic nickel having a composition of from about 75 to about 90 percent of nickel, from about 25 to about 10 percent of alumina and from 0 to albout 1.1615 percent of potassium, said percentages being by weight, and a particle size of from about 210 microns to about 850 microns, said bed being maintained at temperatures of from 400 C. to 550 C. whereby substantially no carbon deposition takes place on the catalyst.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US353381A 1964-03-13 1964-03-20 Process for the production of gases containing methane from hydrocarbons Expired - Lifetime US3433609A (en)

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NL6402670A NL6402670A (fr) 1964-03-13 1964-03-13
US35338164A 1964-03-20 1964-03-20

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3778239A (en) * 1971-03-10 1973-12-11 Ford Bacon & Davis Inc Production of gaseous and liquid fuels from crude oil
US3882636A (en) * 1971-10-07 1975-05-13 Japan Gasoline Two-stage steam reforming process of hydrocarbons
US3926584A (en) * 1973-04-30 1975-12-16 Ici Ltd Catalyst and catalytic process
US3996014A (en) * 1974-06-07 1976-12-07 Metallgesellschaft Aktiengesellschaft Methanation reactor
US4205044A (en) * 1976-09-24 1980-05-27 Tecnimont S.P.A. Reactor for catalyzed exothermic reactions
EP0026057A1 (fr) * 1979-09-14 1981-04-01 Imperial Chemical Industries Plc Réacteur de synthèse et procédés
US4340501A (en) * 1979-09-06 1982-07-20 Imperial Chemical Industries Limited Fluid flow
US4417905A (en) * 1975-09-29 1983-11-29 British Gas Corporation Gas making

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2338346A (en) * 1940-02-26 1944-01-04 Universal Oil Prod Co Apparatus for catalytic conversion reactions
US2634194A (en) * 1951-10-31 1953-04-07 Universal Oil Prod Co Lined reactor
US2816942A (en) * 1954-03-29 1957-12-17 Union Oil Co Production of acetylene
GB820257A (en) * 1958-03-06 1959-09-16 Gas Council Process for the production of gases containing methane from 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
US3186957A (en) * 1960-04-14 1965-06-01 Du Pont Method of preparing a nickel oxidealumina catalyst composition and the product thereof
US3201214A (en) * 1963-02-01 1965-08-17 Pullman Inc Production of domestic heating gas
US3271325A (en) * 1961-09-11 1966-09-06 Ici Ltd Catalytic compositions for use in steam reforming of hydrocarbons

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2338346A (en) * 1940-02-26 1944-01-04 Universal Oil Prod Co Apparatus for catalytic conversion reactions
US2634194A (en) * 1951-10-31 1953-04-07 Universal Oil Prod Co Lined reactor
US2816942A (en) * 1954-03-29 1957-12-17 Union Oil Co Production of acetylene
GB820257A (en) * 1958-03-06 1959-09-16 Gas Council Process for the production of gases containing methane from hydrocarbons
US3186957A (en) * 1960-04-14 1965-06-01 Du Pont Method of preparing a nickel oxidealumina catalyst composition and the product thereof
US3119667A (en) * 1961-01-31 1964-01-28 Pullman Inc Process for hydrogen production
US3271325A (en) * 1961-09-11 1966-09-06 Ici Ltd Catalytic compositions for use in steam reforming of hydrocarbons
US3132010A (en) * 1962-11-08 1964-05-05 Pullman Inc Reforming of gaseous hydrocarbons
US3201214A (en) * 1963-02-01 1965-08-17 Pullman Inc Production of domestic heating gas

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3778239A (en) * 1971-03-10 1973-12-11 Ford Bacon & Davis Inc Production of gaseous and liquid fuels from crude oil
US3882636A (en) * 1971-10-07 1975-05-13 Japan Gasoline Two-stage steam reforming process of hydrocarbons
US3926584A (en) * 1973-04-30 1975-12-16 Ici Ltd Catalyst and catalytic process
US3996014A (en) * 1974-06-07 1976-12-07 Metallgesellschaft Aktiengesellschaft Methanation reactor
US4417905A (en) * 1975-09-29 1983-11-29 British Gas Corporation Gas making
US4205044A (en) * 1976-09-24 1980-05-27 Tecnimont S.P.A. Reactor for catalyzed exothermic reactions
US4340501A (en) * 1979-09-06 1982-07-20 Imperial Chemical Industries Limited Fluid flow
EP0026057A1 (fr) * 1979-09-14 1981-04-01 Imperial Chemical Industries Plc Réacteur de synthèse et procédés
US4311671A (en) * 1979-09-14 1982-01-19 Imperial Chemical Industries Limited Synthesis reactor
US4411877A (en) * 1979-09-14 1983-10-25 Imperial Chemical Industries Plc Synthesis processes

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