US3653846A - Converter for high pressure synthesis - Google Patents

Converter for high pressure synthesis Download PDF

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Publication number
US3653846A
US3653846A US847665A US3653846DA US3653846A US 3653846 A US3653846 A US 3653846A US 847665 A US847665 A US 847665A US 3653846D A US3653846D A US 3653846DA US 3653846 A US3653846 A US 3653846A
Authority
US
United States
Prior art keywords
conduit
shell
segments
grating
manhole
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 - Lifetime
Application number
US847665A
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English (en)
Inventor
Jiri Kubec
Vladimir Saroch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KRALOVOPOLSKA STROJIRNA Z CHEM
KRALOVOPOLSKA STROJIRNA ZAVODY CHEMICKYCH ZARIZENI NARODNI PODNIK
Original Assignee
KRALOVOPOLSKA STROJIRNA Z CHEM
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Publication of US3653846A publication Critical patent/US3653846A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • B01J8/0285—Heating or cooling the reactor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/04—Preparation of ammonia by synthesis in the gas phase
    • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
    • C01C1/0417—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the synthesis reactor, e.g. arrangement of catalyst beds and heat exchangers in the reactor
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
    • C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
    • C07C29/152—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the reactor used
    • 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
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/00132—Tubes
    • 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
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
    • B01J2208/00398—Controlling the temperature using electric heating or cooling elements inside the reactor 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
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/0053—Controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/19—Details relating to the geometry of the reactor
    • B01J2219/194—Details relating to the geometry of the reactor round
    • B01J2219/1941—Details relating to the geometry of the reactor round circular or disk-shaped
    • B01J2219/1942—Details relating to the geometry of the reactor round circular or disk-shaped spherical
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S220/00—Receptacles
    • Y10S220/901—Liquified gas content, cryogenic

Definitions

  • No: 84 ,66 shell an upright conduit axially centered in the shell and extending from a grating in the lowermost segment close to a manhole atop the uppermost segment and barely big enough [52] CL for insertion of the conduit therethrough.
  • a body of particu- [51] [In C] Bo1j9/04 3/00 late catalyst material fills the annular space between the liner [58] Fieid s ⁇ ,289 2889l l and the conduit from the grating almost to the top end of the conduit.
  • a shell-and-tube heat exchanger is arranged in the conduit for preheating a portion of the gaseous reactants by [56] References means of the hot reaction gases.
  • the primary object of the invention is an improvement in the multiple-sphere type converter which pennits such a converter to be built at practical cost in unit sizes even larger than were possible heretofore.
  • the heat exchangers employed heretofore at the connectors between the spherical segments can be replaced by other cooling means which permit the use of an axially continuous body of particulate catalyst material extending upward from a grating in the lowermost spherical segment in at least two and preferably all the segments of the pressure resistant outer shell of the converter, and to discharge the catalyst bed through chutes in the sole grating without any need for removal of the grating.
  • This permits a substantial reduction in the size of the manhole to less than the internal cross section of the annular connectors which in turn is smaller than the cross section of the segments adjacent the converters.
  • FIGURE of the drawing shows a converter of the invention in side elevation, and partly in axial section.
  • the outer pressure shell 1 of the converter is a unitary, welded, heavy steel body. lts inner wall is lined with a thinwalled, conforming metal liner 2 whose inner face carries a coating 3 of asbestos or similar thermally resistant material chemically inert to the reactant gases and to the catalyst employed under the prevailing reaction conditions.
  • a manhole 21 at the top of the shell 1 is normally closed by a cover 4 heavy enough to withstand the operating pressure and held in place by conventional closure elements, not shown.
  • a relatively light inner cover 5 similarly closes an opening in the liner 2 aligned with the manhole in the direction of the vertical converter axis.
  • the heavy pressure-resistant shell 1 consists essentially of three approximately spherically curved segments 18a, 18b, 18c, and two, identical, heavy connector rings 19 interposed respectively between the segments 18a, 18b and 18b, 18c and forming outwardly projecting reinforcing ribs.
  • the segments and rings are joined to each other by welding into a unitary structure which is elongated and has a longitudinal, upright axis.
  • the axial height of each connector 19 is only a small fraction of the corresponding dimensions of the connected segments, and the internal cross section of each connector is smaller than the cross sections of the connected segments perpendicular to the axis adjacent the connector.
  • a cylindrical conduit 6 extends coaxially in the cavity within the liner 2 from a horizontal grating 7 in the lowermost shell segment 18c near the converter bottom almost to the cover 5 in the topmost segment 18a.
  • the annular space radially bounded by the lined shells l, 2 and the conduit 6 above the grating 7 is filled with a bed 8 of particulate catalyst material which forms a continuous body axially extending in the three segments 18a, 18b, 18c from the grating 7 practically to the top of the conduit 6.
  • the lower portion of the conduit 6 holds a heat exchanger 9 whereas the top portion is plugged by an electric heater assembly 10.
  • a horizontal partition wall 1 1 divides the converter space in the segment under the grating 7 into two chambers sealed from each other.
  • the shell 12 of the heat exchanger 9 is radially spaced from the enveloping conduit 6 and projects downwardly beyond the conduit and the grating 7 to a sealed connection with the partition 11 about an axial passage in the same.
  • tubular chutes 14 of which only one is seen in the drawing, lead downwardly and outwardly from the grating 7 through the partition wall 11 and the shell 1. They are normally capped and permit the catalyst material 8 to be drained from the shell 1 if open.
  • the tube nozzle 15 of the heat exchanger 9 passes axially outward from the segment 18c and provides the principal inlet for the mixture of gaseous reactants.
  • a discharge nipple 16 leads through the shell 1 outwardly from the lowermost chamber in the segment 18c.
  • a radial inlet duct 13 in each connector ring 19 is connected with an annular manifold pipe 20 extending along the inner, asbestos-covered face of the liner 2 in the passage of the ring 19.
  • Perforated pipes 17, of which only one is seen in the drawing, are circumferentially distributed over the inner face of the manifold pipe 20 and extend from the manifold pipe as closely to the conduit 6 as is feasible in view of the necessary clearances for thermal expansion and contraction and the need for axially withdrawing the conduit 6 from time to time for maintenance purposes.
  • the pipes 17 are spaced from each other sufficiently widely so as not to interfere with axial movement of the catalyst material when the shell 1 is charged with new catalyst or drained of spent catalyst.
  • the afore-described converter is operated as follows in the synthesis of ammonia from a gas mixture essentially consisting of nitrogen and hydrogen.
  • the gas mixture enters the converter through the tube nozzle 15 of the heat exchanger 9.
  • the heat exchanger tubes provide a channel leading upward into the heater assembly 10 where the mixture is brought up to reaction temperature during a start-up period.
  • the heated gas mixture flowing from the heater assembly at the top of the segment 18a passes downward through the catalyst bed of iron oxides and the gas-permeable grating 7 into the chamber above the partition 11, upwardly through the annular space between the wall of the conduit 6 and the heat exchanger shell 12 to the top of the latter, and ultimately through the shell 12 in heat exchanging contact with the tubes and the reactant mixture therein into the converter bottom and out of the converter shell 1 through the discharge nipple 16 for further recovery of its thermal energy in any desired manner.
  • the reaction of hydrogen with nitrogen is exothermic, and the temperature of the catalyst bed 8 is controlled by injecting a mixture of the reactants at ambient or other relatively low temperature into the reaction mixture through the perforated radial tubes 17.
  • the tubes are relatively widely spaced, the freshly introduced gases are unifonnly distributed in the reaction mixture by being released over the entire flow section of the catalyst bed and in all directions from the perforations of the pipes 17.
  • the heater assembly 10 is no longer needed, and may be deenergized.
  • the catalyst When the catalyst is spent and needs to be replaced, it is drained from the chutes 14 without requiring a man to enter the shell 1, and fresh catalyst may be supplied through the manhole 21. It is normally preferred to vary the particle size distribution of the catalyst material in such a manner as to make the effective flow section of the bed 8 approximately uniform over its axial height. Thus, coarser particles are used in the narrow catalyst bed portions within the connector rings 19 and finer particles in the widest mid-sections of the three segments 18a, 118b, 180. The variation in particle size is readily achieved by sequentially feeding suitable catalyst fractions to the manhole 21. Obviously, other variations in the composition of the several axial portions of the catalyst bed 8 may be made without installing intermediate gratings which would interrupt the axial continuity of the bed.
  • the conduit 6, heater assembly 10, and heat exchanger 9 may be withdrawn from the coverter shell 1 by means of an overhead hoist in a very simple manner if repairs should become necessary.
  • the liner 2 does not normally need to be removed, and be to removed, and damage to its thermally resistance inner coating 3 may be detected and repaired in the shell 1 since the coating is easily accessible after removal of the catalyst bed 8 and of the conduit 6 and its contents.
  • the illustrated shell segments 18a, 18b, 18c have the same radius of curvature, but shell segments differing in their radii of curvature may be employed if desired, and the radius of curvature particularly of the central segment may be chosen so that the shape of the segment closely approaches that of a cylinder. Not less than two approximately spherical segments are required for the apparatus of the invention, but more than three may be used in an obvious manner.
  • a converter for high pressure synthesis comprising, in combination:
  • a. a pressure-resistant, outer shell 1. said shell being elongated and having a longitudinal, upright axis,
  • said shell being fonned of a plurality of axially consecutive, substantially spherically curved, hollow segments having integral flanged end portions, comprising an annular connector interposed between each pair of axially consecutive segments and forming reinforcing ribs for said shell,
  • each connector being much smaller than the axial height of the connected segments, and the internal cross section of the connector being smaller than the cross sections of the connected segments transverse to said axis;
  • a conduit of substantially uniform cross section smaller than said manhole located on a longitudinal axis in said shell and extending through each of said segments from said grating to said manhole, said shell and said conduit radially bounding an axially continuous annular space from said grating to said manhole,
  • a heat exchanger axially spaced from said heater in the lower portion of said conduit and connected thereto for serial flow of fluid, said heat exchanger defining two coaxial thermally connected, separated flow channels between itself and the walls of said conduit, the radially outermost one of said channels communicating with the catalyst material;
  • feed means for feeding a gas through said heat exchanger to said heater to be reacted to
  • discharge means for withdrawing a reacted gas from the radially innermost one of said channels.
  • a converter as set forth in claim 1 further comprising cooling means for cooling the body of catalyst material, said cooling means including a plurality of circumferentially spaced, apertured distributor conduits extending towards axis within each of the connectors and the flanged end portions of each pair of segments and supply means for supplying a gas to said distributor conduits.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
US847665A 1968-06-03 1969-08-05 Converter for high pressure synthesis Expired - Lifetime US3653846A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CS407868 1968-06-03
US84766569A 1969-08-05 1969-08-05

Publications (1)

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US3653846A true US3653846A (en) 1972-04-04

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US (1) US3653846A (de)
DE (1) DE1927850A1 (de)
NL (1) NL6908412A (de)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3918918A (en) * 1972-03-15 1975-11-11 Lummus Co Catalytic reactor
US4181701A (en) * 1976-03-10 1980-01-01 Haldor Topsoe A/S Apparatus and process for the synthesis of ammonia
US4619374A (en) * 1984-05-21 1986-10-28 Ecodyne Corporation Pressure vessel with an improved sidewall structure
US4740262A (en) * 1986-01-24 1988-04-26 Ecodyne Corporation Method of manufacturing a pressure vessel with an improved sidewall structure
US4765507A (en) * 1986-01-24 1988-08-23 Ecodyne Corporation Pressure vessel with an improved sidewall structure
WO2002045836A1 (en) * 2000-12-05 2002-06-13 Texaco Development Corporation Conversion of hydrocarbon fuel to hydrogen rich gas for feeding a fuel cell
US20030057407A1 (en) * 2001-09-06 2003-03-27 Stewart David W. Hammer and hammer head having a frontal extractor
US6886711B2 (en) * 2002-08-22 2005-05-03 Samtech Corporation High-pressure tank and method for fabricating the same

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1408987A (en) * 1922-03-07 casale
US1478550A (en) * 1922-06-26 1923-12-25 Casale Ammonia Company Catalytic apparatus for the synthesis of ammonia
US1839738A (en) * 1928-04-25 1932-01-05 Maria Casale Sacchi Apparatus for effecting catalytic reactions between gases under pressure and at high temperature
US3498756A (en) * 1966-05-26 1970-03-03 Universal Oil Prod Co Multiple stage reactor suitable for high pressures

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1408987A (en) * 1922-03-07 casale
US1478550A (en) * 1922-06-26 1923-12-25 Casale Ammonia Company Catalytic apparatus for the synthesis of ammonia
US1839738A (en) * 1928-04-25 1932-01-05 Maria Casale Sacchi Apparatus for effecting catalytic reactions between gases under pressure and at high temperature
US3498756A (en) * 1966-05-26 1970-03-03 Universal Oil Prod Co Multiple stage reactor suitable for high pressures

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3918918A (en) * 1972-03-15 1975-11-11 Lummus Co Catalytic reactor
US4181701A (en) * 1976-03-10 1980-01-01 Haldor Topsoe A/S Apparatus and process for the synthesis of ammonia
US4619374A (en) * 1984-05-21 1986-10-28 Ecodyne Corporation Pressure vessel with an improved sidewall structure
US4740262A (en) * 1986-01-24 1988-04-26 Ecodyne Corporation Method of manufacturing a pressure vessel with an improved sidewall structure
US4765507A (en) * 1986-01-24 1988-08-23 Ecodyne Corporation Pressure vessel with an improved sidewall structure
US20020090334A1 (en) * 2000-12-05 2002-07-11 Stevens James F. Method for reducing the carbon monoxide content of a hydrogen rich gas
US7226490B2 (en) 2000-12-05 2007-06-05 Texaco, Inc. Fuel processor for producing a hydrogen rich gas
US20020090326A1 (en) * 2000-12-05 2002-07-11 Deshpande Vijay A. Reactor module for use in a compact fuel processor
WO2002045836A1 (en) * 2000-12-05 2002-06-13 Texaco Development Corporation Conversion of hydrocarbon fuel to hydrogen rich gas for feeding a fuel cell
US20020094310A1 (en) * 2000-12-05 2002-07-18 Krause Curtis L. Compact fuel processor for producing a hydrogen rich gas
US20020098129A1 (en) * 2000-12-05 2002-07-25 Paul Martin Apparatus and method for heating catalyst for start-up of a compact fuel processor
US7544346B2 (en) 2000-12-05 2009-06-09 Texaco Inc. Compact fuel processor for producing a hydrogen rich gas
US7455817B2 (en) 2000-12-05 2008-11-25 Texaco Inc. Compact fuel processor for producing a hydrogen rich gas
US7135154B2 (en) 2000-12-05 2006-11-14 Texaco Inc. Reactor module for use in a compact fuel processor
US20060254141A1 (en) * 2000-12-05 2006-11-16 Texaco Inc. Compact fuel processor for producing a hydrogen rich gas
US20020083646A1 (en) * 2000-12-05 2002-07-04 Deshpande Vijay A. Fuel processor for producing a hydrogen rich gas
US20070186475A1 (en) * 2000-12-05 2007-08-16 Texaco Inc. Fuel processor for producing a hydrogen rich gas
US20030057407A1 (en) * 2001-09-06 2003-03-27 Stewart David W. Hammer and hammer head having a frontal extractor
US6886711B2 (en) * 2002-08-22 2005-05-03 Samtech Corporation High-pressure tank and method for fabricating the same

Also Published As

Publication number Publication date
DE1927850A1 (de) 1969-12-04
NL6908412A (de) 1969-12-05

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