EP1345685A1 - Agencement simplifie de reacteur de canaux a plateaux - Google Patents

Agencement simplifie de reacteur de canaux a plateaux

Info

Publication number
EP1345685A1
EP1345685A1 EP00988286A EP00988286A EP1345685A1 EP 1345685 A1 EP1345685 A1 EP 1345685A1 EP 00988286 A EP00988286 A EP 00988286A EP 00988286 A EP00988286 A EP 00988286A EP 1345685 A1 EP1345685 A1 EP 1345685A1
Authority
EP
European Patent Office
Prior art keywords
channels
fluid
plates
perforations
heat exchange
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.)
Withdrawn
Application number
EP00988286A
Other languages
German (de)
English (en)
Inventor
Jacques J. L. Romatier
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.)
Honeywell UOP LLC
Original Assignee
UOP LLC
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
Application filed by UOP LLC filed Critical UOP LLC
Publication of EP1345685A1 publication Critical patent/EP1345685A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F3/00—Plate-like or laminated elements; Assemblies of plate-like or laminated elements
    • F28F3/02—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations
    • F28F3/04—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element
    • F28F3/042—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element in the form of local deformations of the element
    • F28F3/046—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element in the form of local deformations of the element the deformations being linear, e.g. corrugations
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/249—Plate-type reactors
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
    • 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
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/002—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor with a moving instrument
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D21/00—Heat-exchange apparatus not covered by any of the groups F28D1/00 - F28D20/00
    • F28D21/0015—Heat and mass exchangers, e.g. with permeable walls
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D9/00—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D9/0031—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other
    • F28D9/0037—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other the conduits for the other heat-exchange medium also being formed by paired plates touching each 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
    • 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
    • B01J2208/00309—Controlling the temperature by indirect heat exchange with two or more reactions in heat exchange with each other, such as an endothermic reaction in heat exchange with an exothermic reaction
    • 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
    • B01J2208/022—Plate-type reactors filled with granular catalyst
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2451—Geometry of the reactor
    • B01J2219/2453—Plates arranged in parallel
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2451—Geometry of the reactor
    • B01J2219/2456—Geometry of the plates
    • B01J2219/2459—Corrugated plates
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2451—Geometry of the reactor
    • B01J2219/2456—Geometry of the plates
    • B01J2219/246—Perforated plates
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2461—Heat exchange aspects
    • B01J2219/2462—Heat exchange aspects the reactants being in indirect heat exchange with a non reacting heat exchange medium
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2461—Heat exchange aspects
    • B01J2219/2465—Two reactions in indirect heat exchange with each 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2469—Feeding means
    • B01J2219/2471—Feeding means for the catalyst
    • B01J2219/2472—Feeding means for the catalyst the catalyst being exchangeable on inserts other than plates, e.g. in bags
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2476—Construction materials
    • B01J2219/2477—Construction materials of the catalysts
    • B01J2219/2479—Catalysts coated on the surface of plates or inserts
    • 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
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2476—Construction materials
    • B01J2219/2477—Construction materials of the catalysts
    • B01J2219/2481—Catalysts in granular from between plates
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/3221—Corrugated sheets
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32213—Plurality of essentially parallel sheets
    • B01J2219/32217—Plurality of essentially parallel sheets with sheets having corrugations which intersect at an angle of 90 degrees
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32224—Sheets characterised by the orientation of the sheet
    • B01J2219/32227—Vertical orientation
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32237—Sheets comprising apertures or perforations
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32255—Other details of the sheets
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/324—Composition or microstructure of the elements
    • B01J2219/32466—Composition or microstructure of the elements comprising catalytically active material
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/324—Composition or microstructure of the elements
    • B01J2219/32466—Composition or microstructure of the elements comprising catalytically active material
    • B01J2219/32475—Composition or microstructure of the elements comprising catalytically active material involving heat exchange
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F2215/00—Fins
    • F28F2215/04—Assemblies of fins having different features, e.g. with different fin densities
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F2250/00—Arrangements for modifying the flow of the heat exchange media, e.g. flow guiding means; Particular flow patterns
    • F28F2250/10—Particular pattern of flow of the heat exchange media
    • F28F2250/104—Particular pattern of flow of the heat exchange media with parallel flow

Definitions

  • This invention relates generally to plate type exchanger arrangements for containing a reaction zone and indirectly heating the reaction zone with a heat exchange fluid.
  • reaction fluids In many industries, like the petrochemical and chemical industries, contact of reaction fluids with a catalyst in a reactor under suitable temperature and pressure conditions effects a reaction between the components of one or more reactants in the fluids. Most of these reactions generate or absorb heat to various extents and are, therefore, exothermic or endothermic.
  • the heating or chilling effects associated with exothermic or endothermic reactions can positively or negatively affect the operation of the reaction zone.
  • the negative effects can include among other things: poor product production, deactivation of the catalyst, production of unwanted by-products and, in extreme cases, damage to the reaction vessel and associated piping. More typically, the undesired effects associated with temperature changes will reduce the selectivity or yield of products from the reaction zone.
  • Exothermic reaction processes encompass a wide variety of feedstocks and products. Moderately exothermic processes include methanol synthesis, ammonia synthesis, and the conversion of methanol to olefins.
  • Phthalic anhydride manufacture by naphthalene or orthoxylene oxidation, acrylonitrile production from propane or propylene, acrylic acid synthesis from acrolein, conversion of n-butane to maleic anhydride, the production of acetic acid by methanol carbonylation and methanol conversion to formaldehyde represent another class of generally highly exothermic reactions. Oxidation reactions in particular are usually highly exothermic. The exothermic nature of these reactions has led to many systems for these reactions incorporating cooling equipment into their design.
  • Other process applications accomplish indirect heat exchange with thin plates that define channels.
  • the channels alternately retain catalyst and reactants in one set of channels and a heat transfer fluid in adjacent channels for indirectly heating or cooling the reactants and catalysts.
  • Heat exchange plates in these indirect heat exchange reactors can be flat or curved and may have surface variations such as corrugations to increase heat transfer between the heat transfer fluids and the reactants and catalysts.
  • Many hydrocarbon conversion processes will operate more advantageously by maintaining a temperature profile that differs from that created by the heat of reaction. In many reactions, the most beneficial temperature profile will be obtained by maintaining substantially isothermal conditions. In some cases, a temperature profile directionally opposite to the temperature changes associated with the heat of reaction will provide the most beneficial conditions.
  • This invention provides sections of perforations in plates defining channels for the indirect heat exchange between fluids in a plate reactor arrangement.
  • the sections of perforations extend over only portions of the plates defining the channels to allow communication of fluid between adjacent channels while maintaining a substantial channel length over which reactants or heat exchange fluids may pass on their way through the reactor.
  • the partial sections of perforations located at one end of the perforated plates allow any number of channel passes to be made by a single fluid stream through the plate channel reactor. Pressure drop and heat exchange requirements pose the only practical limitation on the number of passes any one fluid may make through the channel reactor arrangement of this invention.
  • Suitable channel arrangements will exchange heat directly across a common heat exchange surface.
  • the arrangements may use an isolated heat exchange stream to provide heat or cooling to reaction channels or may use a heat exchange fluid or reactant from one channel as the reactant or heat exchange fluid in an adjacent channel
  • the feed or reacted stream from the reaction channels may provide fuel for combustion and in situ heat generation in adjacent channels.
  • the heat exchange channels may also serve as combustion channels and receive fuel for combustion in isolation from the fluid in the reaction channels.
  • Useful arrangements may also use different portions of common channels for different functions. Such functions include passing an intermediate fluid through adjacent channels to transfer heat out of a reaction channel at one location and transfer heat back into the heated channels at a downstream channel location.
  • the intermediate channels and the reaction channel may lie in a parallel arrangement between heated channels to adjust the temperature in the reaction channels through the heated channels.
  • this invention is a reaction apparatus for contacting reactants with a catalyst in a reaction zone while indirectly heating or cooling the reactants in the reaction zone by indirect heat exchange with a heat exchange fluid.
  • the apparatus comprises a plurality of spaced apart plates defining a first plurality of channels having a fluid inlet at one end and a second plurality of channels having a fluid outlet at one end. At least one section of perforations communicates fluid between the first and second plurality of channels. At least a portion of the spaced apart plates define the perforation at one of their ends with each section of perforations extending over only a portion of the plate that defines the perforations.
  • the catalyst loading within the reaction channels and the addition of catalyst for supplementary exothermic or endothermic reactions may satisfy different processing objectives.
  • short loading of catalyst in reaction channels can provide a space above or below the reaction zone for additional feed preheat or effluent cooling.
  • extending heating channels can provide additional surface area for open channel heat exchange against the exiting reaction zone effluent or the incoming reactants.
  • this invention has particular advantages.
  • the simplification or elimination of manifolds for distribution or collection of heat exchange and reactants affords space to permit the unloading of catalyst.
  • the apparatus will utilize a distribution manifold at the top of the reaction apparatus that distributes and collects fluid from the fluid inlets and fluid outlets at the top of the channels. Locating the manifold at the top makes it possible for the channels to define particle outlets at their bottoms and incorporate the catalyst unloading device. Thus, the area below the channels may be kept free from manifolds for withdrawing catalyst. The absence of any need to provide screens or other permeable surfaces at the bottom of the channels allows a simple catalyst retaining device to control retention of catalyst in the channels.
  • the device will occlude the particle outlets when in a catalyst retention position and open the particle outlets when in an unloading position. Therefore, the channels may remain completely open for catalyst withdrawal when doors or other suitable closures are removed from the bottom of the channels. It is also possible by the simplification of this arrangement to continue fluid flow through the channels while allowing on stream removal and replacement of catalyst particles.
  • the perforated plate section will dictate the direction of fluid flow. Adjacent channels connected by the perforated plate sections will always have relative countercurrent flow between channels. Nevertheless by isolating heat exchange fluids and reactants, cocurrent flow arrangements are also possible.
  • the plates defining the channels for containing the reactions and heat exchange gases may have any configuration that produces narrow channels.
  • a preferred form of the heat exchange elements is relatively flat plates having corrugations defined therein. The corrugations serve to maintain spacing between the plates while also supporting the plates to provide a well supported system of narrow channels. Additional details on the arrangement of such plate systems are shown in US-A- 5,525,311.
  • the invention is useful in heat producing reactions or heat absorbing reactions.
  • One process that can advantageously use the arrangement of this invention is the production of ethylene oxide.
  • a particularly beneficial process application for this invention is in the production of phthalic anhydride (PA) by the oxidation of orthoxylene.
  • PA phthalic anhydride
  • the reaction apparatus feeds the orthoxylene feed to a distribution manifold that injects a controlled amount of oxygen in admixture with the orthoxylene. Injection of the oxidation compound into the manifold prevents the presence of the orthoxylene and oxygen in explosive proportions.
  • the plate arrangement of the heat exchange reactor quickly dissipates the high heat of reaction associated with the synthesis of the PA.
  • the enhanced temperature control improves product selectivity while also permitting increased throughput.
  • Another object of this invention is to move reactants or heat exchange fluid in multiple passes through a channel reactor arrangement with a reduced number of manifolds.
  • Figure 1 is a schematic illustration of a reactor arrangement of this invention.
  • Figure 2 is a section of Figure 1 taken at line 2-2.
  • Figure 3 is a cross-section of a perforated plate of this invention.
  • Figure 4 is a three dimensional view of a corrugated plate section used in this invention.
  • Figure 5 is a view of single corrugated sheet containing a section of perforations.
  • Figure 6 is a cross-sectional view schematically showing a reactor arranged in accordance with this invention.
  • Figure 7 is a section of Figure 6 taken at line 7-7.
  • Figure 8 is a cross-section showing a schematic arrangement for an alternative embodiment of the reactor of this invention.
  • Figure 9 is a section of Figure 8 taken at line 9-9.
  • Figures 10 and 11 are graphs showing the temperature profile and conversion parameters along the path length of tubes in a tubular arrangement for PA production by orthoxylene oxidation.
  • Figures 12 through 17 are graphs showing the temperature profile and conversion parameters along the path length of channels in plate heat exchange reactor arrangements for producing PA by orthoxylene oxidation.
  • This invention may be useful in any endothermic or exothermic process where a reactant or a portion of a reactant provides a heat source for heating an endothermic reaction or a heat sink for cooling an exothermic reaction in an arrangement of plate exchanger elements. Additional requirements for the compatibility of any process with a plate exchanger arrangement are typically relatively low differential temperature ( ⁇ T) and differential pressure ( ⁇ P) between any heat exchange zone and reaction zone. Differential temperatures of 200 °C or less are preferred for this invention. Differential pressures will remain low and typically reflect pressure drop requirements through the catalyst bed. Ordinarily the differential pressure across plate elements will not exceed .5 MPa.
  • At least the reaction channels will usually contain a catalyst for promoting the reaction. Suitable catalysts for the previously mentioned processes as well as other process applications are well known to those skilled in the art. Catalyst in a particulate form may fill the reaction channels as necessary for reaction time and any pre-reaction heating or post-reaction cooling in the reaction channels. As an alternate to a particulate catalyst, the catalyst may also be coated on the surface of the plates in the various reforming zones. It may be particularly advantageous to coat the reaction catalyst onto the plates to provide an upper catalytic section and a lower catalyst-free section that is maintained in heat exchange relationship across the channel defining plates with a secondary catalytic zone.
  • the heat exchange fluid used in the process or apparatus of this invention may be any type of fluid that can provide the necessary cooling or heating capacity.
  • a wide variety of heat exchange fluids may satisfy the requirement for heating or cooling.
  • Such fluids will include integral process streams as well as auxiliary fluids.
  • the fluid may absorb or release heat by sensible, latent or reactive means.
  • molten salts or metals may be particularly useful as a heat exchange medium.
  • catalysts for promoting complimentary exothermic and endothermic reactions may advantageously reside in the heat exchange channels to provide reactive cooling as well as cooling from the sensible or latent heat of the reactants.
  • An example of such an endothermic and exothermic catalyst combination is autothermal reforming of a light hydrocarbon, typically methane, to the provide what is generally referred to as "synthesis gas" or "syn-gas".
  • Synthesis gas substantially consists of hydrogen and carbon monoxide, lesser amounts of carbon dioxide, unconverted hydrocarbons, and other components which may include nitrogen and other inert components.
  • the strongly endothermic reforming reaction is efficiently balanced against a strongly exothermic oxidation reaction that may be effected by partial catalytic or thermal oxidation of the hydrocarbons. Varying the mols of hydrocarbon in either the reforming or oxidation reaction serves to balance the heat released and the heat absorbed.
  • Such an arrangement is particularly suited for incorporation into a multiple pass channel arrangement that interconnects only two pairs of adjacent channels and places an exothermic reaction channel between alternate heating channel and endothermic reaction channels.
  • a configuration providing a three pass arrangement the relatively cold reactants flow into the heating channels where indirect heat exchange with the reaction channels provides the respective heating and cooling.
  • Flowing the reacted stream from the exothermic reaction channels into the endothermic reaction channels provides additional cooling to the reaction channels across the shared plates that define the endothermic reaction channels as well as the adjacent exothermic reaction channels.
  • FIGS 1 and 2 illustrates a basic reactor arrangement for this invention.
  • a reactor 11 contains a single group of channel pairs 12. Imperforate plates 19 separate the pairs of heat exchange channels into downflow channels 15 and upflow channels 18.
  • a manifold 13 delivers the entering fluid into inlets 14 of downflow channels 15.
  • Perforated sections 16 defined in the bottom of the perforated plates 17 deliver the fluid to upflow channels 18.
  • Manifold 13 contains inlet chambers 20 and outlet chambers 21 as shown in Figure
  • Partition plates 22 segregate the volume of inlet chamber 20 and outlet chamber 21. As indicated by the ® symbol, incoming fluids flow from line 23, along inlet chamber 20 down inlets 14 into channels 15. Blankoff sections 24 of upflow channels 18 prevent fluid carried by inlet chamber 20 from flowing into the upflow channels 18. Similarly, outlet chambers 21 collect the fluid from the upflow channels 18 as indicated by the ⁇ symbols for withdrawal by outlet streams 25 while blankoff sections 26 prevent outflow of fluid from the channels 15 into outlet chamber 21.
  • Channels 15 and 18 may serve a number of different functions. Channels 15 may provide cooling by preheating reactants for an endothermic reaction that takes place in channels 18. Conversely, channels 15 may receive a heated reactant stream that provides additional heat input for an endothermic reaction that takes place in channels 18. Alternately, channels 15 may contain an oxidation catalyst for combustive heating of reactants that enter channels 18.
  • FIG. 1 shows one catalyst loading arrangement for an exothermic reaction.
  • the cold incoming reactants enter via line 23 and pass downwardly into channels 15.
  • the upper part of channels 18 serve as a heat exchange zone to preheat the entering feed against the exiting reactants.
  • the exiting reactants have been heated by the exothermic reaction that takes place in the lower portion of channels 18.
  • the reactants pass into the lower portion of channels 15, they receive further heating directly opposite the exothermic reaction taking place in the lower portions of channel 18.
  • the heated reactants pass through the perforated section 16 at the bottom of perforated plate 17, they pass into catalyst particles 27 that partially fill the bottoms of channels 18.
  • the perforations on partition 16 are sized to block the passage of catalyst particles from channels 18 into channels 15 while permitting flow of reactant fluids from channels 15 into channels 18.
  • FIG. 1 The arrangement of Figure 1 is particularly suited for changing out catalyst in channels 15, 18, or both.
  • catalyst 27 only resides in the channels 18 that are used for the exothermic reaction.
  • a catalyst unloading device shown generally at 28, will permit unloading of the catalyst from channels 18.
  • the unloading device can consist of a single set of doors 29 that at least block the bottoms 30 of channels 18 to prevent catalyst from dropping out of the channels when the doors 29 are in a closed position - as shown by the solid lines. Moving doors 29 to the open position - as shown by the dashed lines - opens bottoms 30 of channels 18 for discharge of catalyst particles.
  • Unloading device 28 may further incorporate a secondary set of doors for selectively retaining and unloading catalyst from channels 15.
  • the second set of doors 31 is shown in an open catalyst unloading position.
  • Secondary doors 31 have slots 32 separating sealing fingers 33. When door 31 is swung upward across the bottoms 34 of channels 15, sealing fingers 33 block bottoms 34 of channels 15 to prevent any catalyst discharge. Slots 32 allow catalyst in channels 18 to flow around second doors 31 for complete unloading prior to unloading catalyst from channels 15 by moving doors 31 to the open position as shown in Figure 1. Once catalyst has been emptied from channels 18 opening doors 31 permits catalyst to flow out channels 18 without any intermixing of the different catalyst particles. Catalyst is readily loaded into channels 18 and, optionally, channels 15 from the top of reactor 11.
  • manifold 13 can be removed from the top of the channels to expose the open areas of the channels and inlet and outlet chambers 20 and 21, respectively.
  • fixed screens may cover inlets 14 of the channels 15 to prevent particles from flowing therein.
  • an appropriate slotted plate may be incorporated and placed over the tops of channels 15 and 18 to selectively block the channels not receiving catalyst during a particular cycle in the loading operation.
  • the inlet and outlet chambers 20 and 21 may provide a distribution space for dispersion of catalyst over the tops of the channels that remain open in each particular chamber.
  • a chamber or series of chambers may replace the doors 29 and 31 to provide an unloading device in the form of collection chambers for receiving particulate material.
  • Suitable collection chambers may have an arrangement similar to that shown in Figure 2 for gathering catalyst from selected channels. Regulated withdrawal and addition of catalyst from the top and bottom of reactor 11 can provide any desired catalyst level within the reactor.
  • the invention relies on relatively narrow channels to provide efficient heat exchange across the thin plates.
  • the channel width should be less than one inch on average with an average width of less than V2 inch preferred.
  • Suitable plates for this invention will comprise any plates that allow a high heat transfer rate.
  • Thin plates are preferred and usually have a thickness of from 1 to 2mm.
  • the plates are typically composed of ferrous or non-ferrous alloys such as stainless steel. Preferred alloys for the plates will withstand extreme temperatures and contain high proportions of nickel and chrome.
  • the plates may be formed into curves or other configurations, but flat plates are generally preferred for stacking purposes.
  • the flat plates may have channels formed by machining, chemical etching or other methods. Again each plate may be smooth and additional elements such as spacers or punched tabs may provide fluid turbulence in the channels.
  • each plate has corrugations that are inclined to the flow of reactants and heat exchange fluid.
  • the corrugations maintain a varied channel width defined by the height of the corrugations.
  • the average channel width is most practically defined as the volume of the channels per the cross-sectional area parallel to the primary plane of the plates.
  • corrugated plates with essentially straight sloping side walls will have an average width that equals half of the maximum width across the channels.
  • Figure 3 shows the preferred corrugation arrangement for the plates 17 that divide channels 15 and channels 18.
  • the corrugation pattern can serve at least two functions. One function is to structurally support adjacent plates. The other function is to promote turbulence for enhancing heat exchange efficiency in the narrow reaction channel.
  • Figure 3 shows corrugations defined by ridges 37 and valleys 38.
  • the frequency or pitch of the corrugations may be varied as desired to promote any varying degree of turbulence. Therefore, more shallow corrugations, with respect to the fluid flow direction, as shown by ridges 37 and valleys 38 will produce less turbulence, whereas a greater corrugation pitch with respect to the direction of fluid flow, as shown by ridges 39 and valleys 40, provide increased turbulence where desired.
  • the pitch of the corrugations and the frequency may also be varied over a single heat exchange channel to vary the heat transfer factor in different portions of the channel.
  • the channels may contain a flat portion 41 about their periphery to facilitate closure of the channels about the sides and tops where desired.
  • plates 19 are essentially the same as plates 17 and preferably contain corrugations and may vary the pitch of the corrugations to vary turbulence and flow factors for heat exchange and other purposes as desired.
  • Perforation section 16 extends across plate 17. Perforations 42 normally have a relatively small diameter that permits the fluid flow across the perforated section but prevents catalyst migration through the perforated section. The perforations will usually vary in size from about 1.5 mm to about 10 mm. Perforation section 16 could be located in an intermediate portion of a plate to provide fluid bypassing in particular process applications, but will normally have a position at one end of the plates. Positioning the corrugation at one end of the plates maximizes the fluid flow path through the channels. The flow area provided by the perforated section will usually at least equal the net flow area along the channel flow path. When one of the channels contains particulate catalyst material, the net flow area would consist of the average open area between the catalyst particles across the transverse section of the channels 18.
  • FIG 4 shows a typical cross-section of a corrugated plate arrangement wherein the corrugations of plates 44 extend in an opposite direction to the corrugations of plates 46 thereby defining alternate channels 47 and 48. Holes 49 provide the perforations of this invention through plates 44.
  • Figure 4 illustrates the preferred arrangement of corrugated plates where the herringbone pattern on the faces of opposing corrugated plates extends in opposite directions and the opposing plate faces contact each other to form the flow channels and provide structural support to the plate sections.
  • Figure 5 further illustrates another possible plate configuration.
  • each reaction channel be alternated with a heat exchange channel.
  • Possible configurations of the reaction section may place two or more heat exchange channels between each reaction channel to reduce the pressure drop on the heat exchange medium side.
  • Double channel arrangements may be defined by a perforated plate that separates adjacent heat exchange channels and that contains perforations over its entire surface. The use of packing or perforated plates can enhance heat transfer with the reaction channels while providing good circulation over the entire cross-section of the heated channel.
  • Figures 6 and 7 show an arrangement where two independent groups of channel pairs circulate different fluids in isolation from opposite ends of a reactor arrangement 50.
  • An inlet stream 51 supplies fluid to a manifold arrangement 52 having upper inlet chambers 53 and upper outlet chambers 54.
  • Inlet chamber 53 distributes upper inlet stream 51 to channel pairs 55 as shown by the ® symbol.
  • Upper outlet stream 56 collects fluid from the first group of channel pairs 55 through upper outlet chambers 54 in the channel openings indicated by the ⁇ symbol.
  • a perforated section 57 connects the two channels in the first group of channel pairs 55.
  • a lower input stream 58 is distributed to a second group of channel pairs 59 via a manifold arrangement 60.
  • An upper perforated section 61 in the second group of channel pairs 59 communicates the channels for withdrawal of a lower outlet stream 62 via manifold 60.
  • the first group of channel pairs can define heat exchange channels for circulating a heat exchange fluid and the second group of channel pairs can define reaction channels for receiving a reactant stream and delivering » a reacted stream.
  • Figures 8 and 9 show an arrangement of reaction channels that uses an odd number of passes to provide a simplified inlet and outlet manifold arrangement.
  • an inlet stream 65 enters an inlet manifold 66 having a single chamber. Fluid entering inlet manifold 66 flows downwardly into inlet channels 68 of a series of three pass channel arrangements 67. Perforated sections 78 at the bottom of plate 69 pass the fluid from inlet channel 68 to middle channel 70 and an upper perforated section 74 continues the communication of fluid from middle channel 70 into outlet channel 71.
  • a manifold 72 again comprising a single open chamber, collects the effluent from outlet channel 71 for withdrawal by an outlet stream 73.
  • Figure 8 positions the perforated sections at alternate ends of the plates defining the channels to define a flow path that delivers the fluid at one end of the channels and collects the fluid from an opposite end of the channels.
  • Figure shows a further modification of the arrangement of Figure 8 wherein side manifolds 75 extend between multiple banks 76 of heat exchange channels. Single fluids or multiple fluids may be delivered to the heat exchange channels by the manifold arrangements depicted in Figures 6 through 8.
  • Side channel 75 can distribute or collect liquid from the sides 77 of one or more of the channels as defined by the spaced apart plates.
  • Figures 8 and 9 show openings 79 in the sides of channels 70 for delivery of an intermediate stream 80.
  • Openings 79 may extend across the entire length of the channel that communicates with the side manifolds or only a portion, as shown in Figure 8, by holes 79'. From a practical construction standpoint, the openings in the sides of the channels may be more conveniently provided by intermittent welding on the sides of the channels rather than defining open holes.
  • the example established the performance of the tubular reactor base case and produced similar results to current industrial tubular reactor performance.
  • a feedstock of air containing an orthoxylene concentration of 75 g/Nm 3 feed passes through a three meter long tube having a diameter of 25mm at a mass flux rate of 10,000 kg/m /hr which produces a .3 bar pressure drop along the tube.
  • the tubular reactor model uses a ring shaped particle having an outer diameter of 9mm with typically a 5mm diameter perforation. Circulation of a salt bath at a temperature of 698 °K around the shell side of the tubes provides cooling.
  • the feed enters the tubular reactor at a temperature of about 700 °K.
  • the final phthalide content in the PA product was below 1000 ppm.
  • Figure 10 graphically depicts the temperature profile over the length of a representative tube.
  • the tube achieves a peak temperature of about 835 °K within the first 50 cm of its path length.
  • Figure 11 illustrates an essentially complete conversion of orthoxylene with about the first 100 cm of tube length. As also presented by Figure 11, continued conversion in the tubes reduces the concentration of orthotolualdehyde and phthalide to levels of less than 1000 ppm while raising the PA selectivity to about 83%.
  • the plate heat exchanger type reactor operates at the same orthoxylene inlet concentration and mass flux through the heat exchange channels as the tubular reactor.
  • the channel arrangement contains a 2mm spherical catalyst in a 6 mm gap between channels in one of the channel pairs.
  • the process flux in the plate reactor arrangement drops to 7500 kg/m /hr. Nevertheless, the sizing of the plate exchange reactor maintains the same ratio of heat transfer surface area to catalyst surface area on a per reactor volume basis as in the tubular reactor arrangement.
  • the process inlet temperature in the plate exchanger reactor increases 15 °C above the tubular reactor case or to a temperature of about 713 °K to maintain the same phthalide level in the PA product.
  • Figure 12 shows the peak temperature in the channels decreasing to about 815 °C, representing about a 20 °C temperature drop relative to the tubular reactor case.
  • Figure 13 shows a rapid conversion of orthoxylene along the path length of the plate exchange reactor with about the same selectivity to PA and orthotolualdehyde and phthalide to levels below 1000 ppm.
  • the temperature reduction of this example demonstrates that the plate heat exchange reactor has about a 30% overall greater heat transfer ability than the tubular reactor.
  • Example 3 evaluates increases in the concentration of the orthoxylene in the air to the plate exchange reactor over the range of from 75 g/Nm to 110 g/Nm to determine the concentration that produces the same peak temperature in the plate heat exchange reactor as in the tubular reactor.
  • Heat from the additional orthoxylene oxidation requires increasing the circulating salt temperature from the 713 °K in Example 2 to about 717 °K to keep the phthalide concentration below 1000 ppm in the PA product.
  • the peak temperature of the plate reactor approaches the maximum temperatures of the tubular reactor arrangement.
  • the maximum orthoxylene concentration can increase significantly over the tubular case reactor by use of the plate exchanger while still maintaining the PA selectivity of about 83 mol%.
  • Example 4 demonstrates the effect on temperature and conversion of staging the injection of orthoxylene at an intermediate point in the channels to reestablish a maximum concentration of 75 g/Nm 3 .
  • Staged injection of feed in this case would use the side distribution channels of Figures 8 and 9 in combination with one of the groups of channel pairs as shown in Figures 6 and 7.
  • This example decreases initial injection of feed to reduce the process flux at the inlet of the plate reactor to 5525 kg/m 2 /hr for the first stage of orthoxylene injection.
  • the arrangement injects additional orthoxylene at 30 cm along the path length of the heat exchange reactor in a middle section of one of the channels in each pair of the upflow and downflow channel groups.
  • the temperature of the circulating salt bath drops to 700 °K, the equivalent of the tubular reactor inlet temperature.
  • the path length of the channels in this example increases to a total of 130 cm that provides an additional 30 cm for the first stage, while maintaining the same 100 cm of second stage that was used in Examples 2 and 3.
  • the additional length decreases the phthalide content below 1000 ppm in the PA product. Nevertheless, even with the increased length, total pressure drop remains below the .3 bar value of the tubular reactor example.
  • Figure 15 displays a maximum peak temperature of below 810 °K in the first stage.
  • Figure 16 shows an essentially complete orthoxylene conversion within the first 30 cm of the injection point.
  • Figure 17 demonstrates continued PA selectivity at over 83 %.

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  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
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Abstract

L'invention concerne un procédé et un appareil permettant d'échanger indirectement de la chaleur au moyen de canaux étroits dans une zone de réaction de canal de type à échange de chaleur mettant en oeuvre des plateaux (17) renfermant des sections partiellement perforées (16), de manière à simplifier ou éliminer l'utilisation de collecteurs pour distribuer et rassembler plusieurs fluides vers différents canaux. Le procédé et le système selon l'invention permettent de simplifier le fonctionnement par communication directe des canaux adjacents à travers des sections de perforations situées au niveau d'une extrémité ou de l'autre des canaux. L'agencement selon l'invention présente un caractère avantageux ce qu'il s'agit d'agencements de réacteur d'échange de chaleur plus compacts. L'agencement selon l'invention permet également de simplifier l'utilisation d'un agencement unique de collecteur au niveau d'une extrémité des canaux, de manière à faciliter un déchargement et un remplacement de catalyseur dans des canaux de réaction.
EP00988286A 2000-12-22 2000-12-22 Agencement simplifie de reacteur de canaux a plateaux Withdrawn EP1345685A1 (fr)

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GB0503908D0 (en) * 2005-02-25 2005-04-06 Accentus Plc Catalytic reactor
CN100435926C (zh) * 2006-11-03 2008-11-26 厦门大学 一种多分子接触催化反应装置及反应方法
WO2009061416A2 (fr) * 2007-11-05 2009-05-14 Velocys Inc. Chargement ou déchargement de particules dans ou hors de réacteurs à microcanaux
DE102008017342A1 (de) * 2008-04-04 2009-10-08 Linde Aktiengesellschaft Kompaktreaktor
US8263006B2 (en) * 2009-05-31 2012-09-11 Corning Incorporated Reactor with upper and lower manifold structures
BR112013013597A2 (pt) * 2010-12-01 2016-09-13 Meggitt Uk Ltd aparelho para utilização na produção de ácido nítrico
FR2974739B1 (fr) * 2011-05-03 2016-03-11 Commissariat Energie Atomique Module de reacteur solide / gaz caloporteur comprenant des diffuseurs de gaz a risques d'obturation reduits
TW201510461A (zh) 2013-06-11 2015-03-16 漢洛克半導體公司 熱交換器
ITUB20152869A1 (it) * 2015-08-05 2017-02-05 Baretti Mefe S R L Impaccamento strutturato ad ?alta capacita' ed efficienza? o ?ad alte prestazioni? per colonne di distillazione.
GB2551134B (en) * 2016-06-06 2019-05-15 Energy Tech Institute Llp Heat exchanger
US10563932B2 (en) * 2017-12-21 2020-02-18 Uop Llc Process and apparatus for cooling catalyst
PL3657114T3 (pl) * 2018-11-26 2021-11-02 Alfa Laval Corporate Ab Płyta wymiennika ciepła
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CN1527742A (zh) 2004-09-08
AU2001224509B2 (en) 2006-07-27
EA005643B1 (ru) 2005-04-28
NO20032865L (no) 2003-08-19
MXPA03005732A (es) 2003-10-06
NO20032865D0 (no) 2003-06-20
KR20030072575A (ko) 2003-09-15
CA2432082A1 (fr) 2002-07-04
CA2432082C (fr) 2009-04-28
KR100807164B1 (ko) 2008-02-27
EA200300719A1 (ru) 2004-06-24
WO2002051538A1 (fr) 2002-07-04

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