CA1229059A - Downwardly-directed fluid flow distribution system for ebullated bed reactor - Google Patents
Downwardly-directed fluid flow distribution system for ebullated bed reactorInfo
- Publication number
- CA1229059A CA1229059A CA000436283A CA436283A CA1229059A CA 1229059 A CA1229059 A CA 1229059A CA 000436283 A CA000436283 A CA 000436283A CA 436283 A CA436283 A CA 436283A CA 1229059 A CA1229059 A CA 1229059A
- Authority
- CA
- Canada
- Prior art keywords
- plenum
- flow
- conduit
- reactor
- flow distribution
- 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
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
-
- 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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
Abstract
ABSTRACT OF THE DISCLOSURE
An improved flow distribution system for a cata-lytic reactor plenum chamber for a gas-liquid-solids ebullated bed reactor. The flow distribution system includes a downwardly directed conduit and a flow distri-butor device such as a baffled nozzle attached to the inner end of the conduit, said nozzle containing at least two substantially parallel baffle plates usually oriented substantially normal to the nozzle inlet flow direction for providing initially downward flow and good mixing and radial flow dispersion of gas-liquid materials in the lower portion of the plenum. The initially downward flow is then deflected generally upwardly by the curved lower head of the reactor plenum chamber and passes uniformly upwardly through a flow distribution grid into the ebullated catalyst bed. A sparger can be provided in the plenum above the flow distributor device for feeding additional gas-liquid mixture into the reactor.
Alternatively, the flow distribution system can include a oonical-shaped flow deflector device having its base rigidly attached to the plenum lower wall and having its apex oriented toward and substantially aligned with the centerline of the inner end of the conduit. The flow distribution system provides substantially uniform flow dispersion of the gas-liquid mixture into the ebullated bed, and minimizes stagnant zones in the plenum and thereby provides fouling-free operation of the reactor.
An improved flow distribution system for a cata-lytic reactor plenum chamber for a gas-liquid-solids ebullated bed reactor. The flow distribution system includes a downwardly directed conduit and a flow distri-butor device such as a baffled nozzle attached to the inner end of the conduit, said nozzle containing at least two substantially parallel baffle plates usually oriented substantially normal to the nozzle inlet flow direction for providing initially downward flow and good mixing and radial flow dispersion of gas-liquid materials in the lower portion of the plenum. The initially downward flow is then deflected generally upwardly by the curved lower head of the reactor plenum chamber and passes uniformly upwardly through a flow distribution grid into the ebullated catalyst bed. A sparger can be provided in the plenum above the flow distributor device for feeding additional gas-liquid mixture into the reactor.
Alternatively, the flow distribution system can include a oonical-shaped flow deflector device having its base rigidly attached to the plenum lower wall and having its apex oriented toward and substantially aligned with the centerline of the inner end of the conduit. The flow distribution system provides substantially uniform flow dispersion of the gas-liquid mixture into the ebullated bed, and minimizes stagnant zones in the plenum and thereby provides fouling-free operation of the reactor.
Description
DOWNW~RDLY-DIRECTED FLUID FLOW DISTRIBUTION SYSTEM FOR
EBULLATED BED REACTOR
. .
BACKGROUND OF INVENTION
This invention pertains to a fluid flow distributor device and system for intxoducing feed and recycle fluid streams uniformly into a plenum and an ebullated catalyst bed of a reactor. It pertains particularly to such a flow distribution system for - handling petroleum and coal-oil slurry and gas streams in which the flow is initially directed downwardly for substantially uniform mixing and flow distribution into an ebullated catalyst bed.
Experience in operating pilot plant and commercial reactors used in H-Oil~ and H-Coal M processes has shown that improper design of the inlet flow distribution in the reactor plenum can cause operational difficulties, such as ~ coke formation in the plenum, flow maldistribution in the ; ~ catalyst bed, localized catalyst bed slumping, and formation of coke in the bed. These problems have reduced catalyst utilization, and resulted in frequent reactor shutdowns and shortened periods of operation.
The prior art has apparently not provided an adequate solution to this flow distribution problem in fluidized bed catalytic reactors. For example, U.S. Patent 25 No. 3,197,288 to Johanson shows a catalytic reactor configuration using simple conduits for introducing the inlet feed and recycle liquid into the reactor plenum chamber, and U.S. Patent 3,202,603 to Keith et al, shows use of dual spargers in the lower end of a reactor. Also, 30 U.S. Patent 3,540,995 to Woik et al generally discloses operation of a coal hydrogenation process using an ebullated catalyst bed reactor in which feed and recycle ; liquid streams are introduced into the reac~or lower end plenum below a flow distribution grid means. ~owever~
introducing such gas and liquid streams into a reactor plenum at hi~h velocity requires more specific arrangements :;
i I
~J~
~.~2~5~
for the streams to achieve adequate mixing and uniform flow distribution. For this reason, improved designs of flow distribu~or devices to provide desirably uniform flow patterns in the reactor plenum have now been developed.
SUMMARY OF INVENTION
The present invention provides a fluid flow distributor device and flow distribution system for feeding hydrocarbon liquid or slurry and a gas uniformly into a plenum chamber and upwardly into an ebullated catalyst bed of a reactor. The invention comprises a flow distributor device for providing uniform flow distribution of a gas/liquid mixture into an ebullated bed of a reactor, the flow distributor device being located in a plenum of the reactor, said plenum being formed by a distribution grid and the lower end and lower walls of the reactor below the grid, the flow distributor device compris-ing a conduit extending into said plenum from outside the reactor with the conduit inner end being directed downwardly in the plenum and a baffled nozzle positioned at the inner end of the conduit within the plenum and downward-ly directed toward the lower walls of the reactor for recycling a hydrocarbon fluid at least partially derived from a reaction within the ebullated bed, said baffled nozzle having at least two substantially parallel baffles spaced apart from each other and rigidly attached to the inner end of said conduit, the innermost or downstream baffle consisting of a solid plate, and at least one other upstream baffle having a central opening and located upstream of the solid plate downstream baffle, whereby said baffled nozzle mixes a gas and a liquid material fed through said conduit downwardly into said plenum and is arranged in combination with said distribution cJrid to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture upwardly into said ebullated bed of the xeactor.
The invention also comprises a fluid flow distribution system for providing a uniform flow distribution of a fluid material into an ebullated catalyst bed of a reactor, the distribution system comprising a plenum provided in the lower part of the reactor and formed by the lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor; a conduit extending into the plenum for carrying a flowable fluid material initially downwardly into the plenum; and a flow distributor device located in the lower end of the plenum and associated in flow relationship with the conduit, whereby the distributor device mixes a gas and a liquid material fed through said conduit downwardly into said plenum and is so arranged in combination with the distribution grid as to effect a substantially uniform mixing and flow lS distribution of the gas/liquid mixture upwardly into the ebullated bed of the reactor.
In another embodiment of the invention, the flow distribution system comprises a plenum provided in the lower part of the reactor and formed by the reactor lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor; a conduit extending into said plenum for carrying a flowable fluid material initally downwardly into the plenum; and comprises a conical-shaped f 1QW deflector device located in the lower end of the plenum, said deflector having its base rigidly attached to the plenum lower end and having its apex oriented toward the inner end of the conduit, the centerline of the conical-shaped deflector being substantially aligned with the centerline of the inner end of the conduit, whereby said conical deflector mixes a gas and a liquid material fed through said conduit into said plenum and is arranged in combination with the distribution grid to effect a substantially uniform mixing and flow distribution of the gas~liquid mixture uniformly upwardly into said ebullated bed of the reactor.
This invention is particularly useful for handling hydrocarbon eedstreams such as petroleum and coal ., , o~
slurries for uniform distribution together with hydrogen gas into an ebullated catalyst bed reactor, partlcularly when the superficial velocity in the feed conduit exceeds about 8 ft./sec. Accordingly, the texm gas/liquid mixture is understood to include also a gas/liquid slurry mixture containing fine particulate solids.
BRIEE' DESCRIPTION OF DRAWINGS
FIG. 1 is a vertical cross-sectional view of the lower portion of an ebullated bed reactor utilizing the invention and including a plenum and flow distributor device.
FIG. 2 is a vertical cross-sectional detail vie~7 of a baffled nozæle flow distributor device used in the invention.
FIG. 3 shows a vertical cross-sectional view of an alternative embodiment of the invention in which feed and recycle streams are introduced into the plenum through separate flow devices.
FIG. 4 shows another embodiment of the invention similar to FIG. 3 but utilizing a centrally located conical shaped deflector device.
DESCRIPTION OF INVENTION
In the present invention, the fluid feed stream such as a mixture of coal-derived liquid slurry and hydrogen at 650-950F temperature and 500-3000 psig pressure 25 conditions is passed through a conduit and a distributor device such as a disc-donut type baffled nozzle into a plenum located at the lower end of a reactor~ The inner end of the conduit is downwardly-directed and the plenum distributor device is positioned at the inner end of the conduit within the plenum and is also downwardly directed toward the lower wall of the reactor. The distributor device usually contains a series of substantially parallel spaced apart baffle plates located at an angle of 45-90 to the centerline of conduit inner end, which device provides lateral or radially outward flow deflection within the plen~m. The inlet flow distributor device for the reactor plenum of gas-liquid-solids fluidized bed ~:Z90~5~
reactors provides a fouling-free distributor device for dispersion of the kinetic energy in the flowing fluids fed into the plenum chamber~ The distributor device prevents "jetting" of the recycle liquid and gas stream in the plenum, and disperses the liquid flow uniformly in the plenum.
Depending on the reactor operating conditions and the space available in the plenum, the flow distributor device can have various configurations. The liquid flow distributor device can consist of at least two preferably circular baffle plates located at the outlet of the recycle liquid conduit. For a central vertical baffled nozzle location within the plenum, these baffle plates are usually e~ually spaced from each other. The distributor device bottom plate is solid, and deflects the inlet flow laterally to prevent direct impingement of liquid on the bottom of the plenum. The other baffle or dispersion plates in the device have central openings sized to intercept and deflect portions of the liquid flow laterally or radially outwardly into the plenum. The flow paths of these lateral streams are directed to sweep the plenum bottom to eliminate stagnation æones and provide good mixing of gas/liquid (or gas/liquid slurry) and substantially uniform flow distribution upwardly through openings in the flow distribution grid into the ebullated bed.
The percent o~ total material flowing radially outwardly from the spac~ between each baffle plate can be varied by selecting the dimensions of the distributor device, but usually a greater percentage of the flow is emitted from the lowest space~ In a typical deflector device design, about 40-45% of the inlet liquid flow is deflected by the first plate, 25-35% i5 deflected by the middle plate, and the remaining flow is deflected radially outwardly by the bottom innermost plate. For a nozzle configuration entering the plenum from one ~ide and not located on the pl~num cen~-erline, the baf~le plates are oriented a~ an angle varying from about 0 ~o about 10 s~
with the adj~cent baffle to provide a uniform disper~ion of the gas/liquid flow within the plenum.
For small diameter reactors having inside diameters less than about 5 feet, it is usually more convenient to mix the feed liquid and gas streams with the reactor recycle liquid external to the reactor prior to uniformly distributing the combined mixture in the reactor plenum, utilizing the distributor device of FIG. 1 as described below. For reactors having diameters larger than about 6 ft., it is usually desirable to introduce the feed liquid and gas mixture into the reactor plenum through separate distributor devices. For example, a circular perforated sparger ring is usually located in the plenum upper portion and can be used to distribute the gas-liquid feed mixture uniformly across the reactor plenum. Uniform flow of small bubbles and liquid feed is produced by providing a pressure drop across the sparger and directing the mixed gas-liquid streams from the sparger downwardly to substantially dissipate the stream kinetic energy in the liquid. This kinetic energy is utilized to increase the intensity of liquid backmixing in the plenum. Pressure drops across the sparger ring openings usually range from 1-15 psi for typical heavy petroleum crude upgrading and coal liquefaction processes.
In an alternative embodiment of the invention, the flow distributor device consists of a conduit and a conical-shaped deflector having its base rigidly attached to the plenum lower wall and having its apex oriented toward and substantially aligned with the centerline of the inner 3Q end of the conduit.
This lnlet flow distributor device is used upstream and in combination with the reactor flow distribution grid to provide an improved flow distribution system for an ebullated bed catalyst reactor. The pres~ure drop across the baffled nozzle distribu~or device at rated flow is usually 5-25% of the total pressure drop across bo~h the distributor device and the distribution grid.
Al-though the distributi.on grid can consist of a perfordted plate, it preferably contains multiple vertical tubes each provided with a cap over the tube upper end. This distribution system provides improved gas-liquid contacting and gas mixing in the reactor plen~, eliminates undesired direct impingement of the fluid streams on the distribution grid, and minimizes coke formation in the plenum and in the catalyst bed support above the grirl.
The invention will be further described with reference to FIG. 1, which shows an inlet conduit 10 inserted into a plenum chamber 12 of reactor 14. The conduit has a baffled nozzle or disc donut type flow distributor device 16 oriented generally downwardly in the plenum for feeding a liquid and gas mixture into the plenum, then passing the mixtu.re uniformly upwardly through openings 19 in flow distribution grid 18 into ebullated catalyst bed 20.
Reactor liquid is withdrawn from above the catalyst bed downward through central conduit 24 to a recycle pump (not shown3, from which the liquid is recycled together with fresh liquid and gas feed through inlet conduit 10 to flow distributor 16. The plenum 12 preferably has a height equal to S-10 times the inner diameter conduit 10, and distribution grid 18 preferably has a diameter equal to 4-12 times the inner diameter of conduit 10 As shown in greater detail in FI~ 2, flow distributor device 16 comprises at least one annular-shaped plate 30 having central opening 31 located upstream of bottom circular solid plate 32, and all retained toget~er by three circumferentially equally-spaced structural rods 33, which are preferably located at the baffle plate outer edges. Usually an additional annular-shaped plate 34, having progressively smallex central opening 35, can be located intermediate plates 30 and 32 to provide a preferred baffled nozzle confi~uration for further radial distribution of the flow from conduit 10. The greater percentage of flow should preferably be emitted from the lowest or downstream space, because of the greater ()5~
distance of fluid travel in plenum 12 before reaching dis-tribution qrid 18. For a flow distributor device 16 having three pla-tes, the plate dimensions are preferably selected such that about 40-45 volume percent of the fluid flow is deflected radially outwardly by bottom solid or downstream baffle 32, about 25-35 volume percent is deflected outwardly by the second or intermediate baffle 34, and the remaining flow radially deflected by top or upstream baffle plate 30. If desired, at least one 10w straightening vane 36 can be centrally oriented longitudinally inside conduit 10, so that the flow pattern reaching the distributor device 16 is substantially unidirectional. Such flow straightening vane is particularly useful when the angle of deflection for the flowing fluid in conduit 10 exceed about 30.
FIG. 3 shows an alternative configuration of the fluid flow distribution system of this invention, wherein the flow distributor device 16 is centrally located on the longitudinal center line of the plenum and downwardly oriented in the bottom part of plenum chamber 12 below distribution grid 18, and is located above the bottom of the reactor plenum by a distance equal to 1.0-2.0 times the inside diameter of the inlet conduit. The flow distribution grid 18 preierably contains multiple vertical tubes 26 having an inner diameter of 0.75-1.5 inches and which extend below the grid ~y a distance equal to 4 10 times tne tube inner diameter. Tubes 26 extend above the grid by a distance equal to about 1.5-4 times the tube inner diameter. ~bove the upper end of each tube 26, a cylindrical-shaped cap 28 is provided, which is spaced away from the tube and is rigidly supported from the tube by suitable structural m~mbers ~not shown). Cap 28 is oriented 50 as to prevent en~ry of ca~alyst solid particles 22 from the ebullated bed into tubes 26 whenever there is no upward fluid 10w through the tube, such as may occur during operationai upsets or occurs at process shutdowll.
A circular annular-shaped sparger ring 40 havinq ~l2~.~V5S~
uniformly spaced openings ~1 on its lower side is provided above flow distributor device 16 to uniformly distribute gas and liquid flow in the upper portion 12a of the plenum chamber. The sparger ring 40 encircles downcomer conduit 24 and is particularly useful for large diameter reactors, such as exceeding about 8 feet inside diameter. Multiple spaced openings 41 in the sparger ring 40 are sized to provide a uniform pressure drop and are located to direct the flow downwardly so as to substantially dissipate its kinetic energy and increase the back-mixing action of gas and liquid in the plenum 12.
In another embodiment of the invention as shown by FIG. 4, the flow distributor device consists of a conduit and a conical-shaped deflector 46 which is centrally-located within the bottom portion of the plenum 12, and hasits base rigidly attached to the plenum bottom wall 49. The apex 48 of the deflector 46 is centrally aligned with downwardly oriented end 11 of inlet conduit 10, so that the flow from conduit 10 is deflected substantially uniformly radially outwardly against the lower walls 49 of th~ plenum 12. The conical surface of deflector 46 can be made straight, or curved outwardly at the lower end to facilitate a gradual outward deflection of the flow of the gas/liquid mixture in the plenum. Thus, flow deflector device 46 operates similarly as for distribu~or device 16, whereby the total flow passes radially outwardly and against the walls of the plenum. Circular sparger 40 is provided in plenum chamber 12 centrally located above flow distribution device 46, simmlarly as for the FIG. 3 configuration. The conduit 10 contains at least one flow straightening vane.
The effectiveness of using the inlet flow distributor device configuration is illustrated by ~he following examples, which should not be regarded as limiting the scope of the invention.
EXAMPLES
In a coal hydrogenation plant using the "~-Coal"~
Process for coal liquefaction and having an ebullated bed _,~
s~3 catalyst reactor with 5 ft. inside diameter, (200 tons/day Catlettsburg "H~Coal"TM Pilot Plant Reactor), the feed coal slurry and gas is mixed with the recycle ebullation liquid flow external to the reactor. The total combined stream is then distributed through a side-entering downwardly directed baffled nozzle equipped with three inclined baffle plates, as generally described in the F`IG. 1 embodiment of this invention. Following installation of the flow distributor nozzle in the plenum, coking in the reactor ebullated catalyst bed due to flow maldistribution therein is substantially eliminated.
In a commercial "H-Coal" (18,000 tons/day) Plant reactor design having an 11 ft. inside diameter, the inlet flow distribution system in the plenum contains a side-entering downwardly directed baffled nozzle e~uipped with three inclined baffle plates for dispersion of the recycle liquid slurry flow and a circular sparger ring located above the nozzle for distributing the feed liquid slurry and gas. In a commercial H-Oil~ ~35,000 bbl/day~
Plant reactor design, having 10 ft~ inside diameter, the inlet flow distribution system in the reactor plenum consists of a centrally located vertically oriented baffled nozzle equipped with three horizontal plates for dispersion of ~he recycle ebullating liquid flow, and a sparger ring located above ~he nozzle for uniform flow distribution of the feedstream liquid and gas.
Althouyh this invention has been described broadly and in terms of various specific embodiments, it will be understood that modification~ and variations can be made and some elements used without o~hers all within the spirit and ~cope of the invention, which is defined b~ the following claims,
EBULLATED BED REACTOR
. .
BACKGROUND OF INVENTION
This invention pertains to a fluid flow distributor device and system for intxoducing feed and recycle fluid streams uniformly into a plenum and an ebullated catalyst bed of a reactor. It pertains particularly to such a flow distribution system for - handling petroleum and coal-oil slurry and gas streams in which the flow is initially directed downwardly for substantially uniform mixing and flow distribution into an ebullated catalyst bed.
Experience in operating pilot plant and commercial reactors used in H-Oil~ and H-Coal M processes has shown that improper design of the inlet flow distribution in the reactor plenum can cause operational difficulties, such as ~ coke formation in the plenum, flow maldistribution in the ; ~ catalyst bed, localized catalyst bed slumping, and formation of coke in the bed. These problems have reduced catalyst utilization, and resulted in frequent reactor shutdowns and shortened periods of operation.
The prior art has apparently not provided an adequate solution to this flow distribution problem in fluidized bed catalytic reactors. For example, U.S. Patent 25 No. 3,197,288 to Johanson shows a catalytic reactor configuration using simple conduits for introducing the inlet feed and recycle liquid into the reactor plenum chamber, and U.S. Patent 3,202,603 to Keith et al, shows use of dual spargers in the lower end of a reactor. Also, 30 U.S. Patent 3,540,995 to Woik et al generally discloses operation of a coal hydrogenation process using an ebullated catalyst bed reactor in which feed and recycle ; liquid streams are introduced into the reac~or lower end plenum below a flow distribution grid means. ~owever~
introducing such gas and liquid streams into a reactor plenum at hi~h velocity requires more specific arrangements :;
i I
~J~
~.~2~5~
for the streams to achieve adequate mixing and uniform flow distribution. For this reason, improved designs of flow distribu~or devices to provide desirably uniform flow patterns in the reactor plenum have now been developed.
SUMMARY OF INVENTION
The present invention provides a fluid flow distributor device and flow distribution system for feeding hydrocarbon liquid or slurry and a gas uniformly into a plenum chamber and upwardly into an ebullated catalyst bed of a reactor. The invention comprises a flow distributor device for providing uniform flow distribution of a gas/liquid mixture into an ebullated bed of a reactor, the flow distributor device being located in a plenum of the reactor, said plenum being formed by a distribution grid and the lower end and lower walls of the reactor below the grid, the flow distributor device compris-ing a conduit extending into said plenum from outside the reactor with the conduit inner end being directed downwardly in the plenum and a baffled nozzle positioned at the inner end of the conduit within the plenum and downward-ly directed toward the lower walls of the reactor for recycling a hydrocarbon fluid at least partially derived from a reaction within the ebullated bed, said baffled nozzle having at least two substantially parallel baffles spaced apart from each other and rigidly attached to the inner end of said conduit, the innermost or downstream baffle consisting of a solid plate, and at least one other upstream baffle having a central opening and located upstream of the solid plate downstream baffle, whereby said baffled nozzle mixes a gas and a liquid material fed through said conduit downwardly into said plenum and is arranged in combination with said distribution cJrid to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture upwardly into said ebullated bed of the xeactor.
The invention also comprises a fluid flow distribution system for providing a uniform flow distribution of a fluid material into an ebullated catalyst bed of a reactor, the distribution system comprising a plenum provided in the lower part of the reactor and formed by the lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor; a conduit extending into the plenum for carrying a flowable fluid material initially downwardly into the plenum; and a flow distributor device located in the lower end of the plenum and associated in flow relationship with the conduit, whereby the distributor device mixes a gas and a liquid material fed through said conduit downwardly into said plenum and is so arranged in combination with the distribution grid as to effect a substantially uniform mixing and flow lS distribution of the gas/liquid mixture upwardly into the ebullated bed of the reactor.
In another embodiment of the invention, the flow distribution system comprises a plenum provided in the lower part of the reactor and formed by the reactor lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor; a conduit extending into said plenum for carrying a flowable fluid material initally downwardly into the plenum; and comprises a conical-shaped f 1QW deflector device located in the lower end of the plenum, said deflector having its base rigidly attached to the plenum lower end and having its apex oriented toward the inner end of the conduit, the centerline of the conical-shaped deflector being substantially aligned with the centerline of the inner end of the conduit, whereby said conical deflector mixes a gas and a liquid material fed through said conduit into said plenum and is arranged in combination with the distribution grid to effect a substantially uniform mixing and flow distribution of the gas~liquid mixture uniformly upwardly into said ebullated bed of the reactor.
This invention is particularly useful for handling hydrocarbon eedstreams such as petroleum and coal ., , o~
slurries for uniform distribution together with hydrogen gas into an ebullated catalyst bed reactor, partlcularly when the superficial velocity in the feed conduit exceeds about 8 ft./sec. Accordingly, the texm gas/liquid mixture is understood to include also a gas/liquid slurry mixture containing fine particulate solids.
BRIEE' DESCRIPTION OF DRAWINGS
FIG. 1 is a vertical cross-sectional view of the lower portion of an ebullated bed reactor utilizing the invention and including a plenum and flow distributor device.
FIG. 2 is a vertical cross-sectional detail vie~7 of a baffled nozæle flow distributor device used in the invention.
FIG. 3 shows a vertical cross-sectional view of an alternative embodiment of the invention in which feed and recycle streams are introduced into the plenum through separate flow devices.
FIG. 4 shows another embodiment of the invention similar to FIG. 3 but utilizing a centrally located conical shaped deflector device.
DESCRIPTION OF INVENTION
In the present invention, the fluid feed stream such as a mixture of coal-derived liquid slurry and hydrogen at 650-950F temperature and 500-3000 psig pressure 25 conditions is passed through a conduit and a distributor device such as a disc-donut type baffled nozzle into a plenum located at the lower end of a reactor~ The inner end of the conduit is downwardly-directed and the plenum distributor device is positioned at the inner end of the conduit within the plenum and is also downwardly directed toward the lower wall of the reactor. The distributor device usually contains a series of substantially parallel spaced apart baffle plates located at an angle of 45-90 to the centerline of conduit inner end, which device provides lateral or radially outward flow deflection within the plen~m. The inlet flow distributor device for the reactor plenum of gas-liquid-solids fluidized bed ~:Z90~5~
reactors provides a fouling-free distributor device for dispersion of the kinetic energy in the flowing fluids fed into the plenum chamber~ The distributor device prevents "jetting" of the recycle liquid and gas stream in the plenum, and disperses the liquid flow uniformly in the plenum.
Depending on the reactor operating conditions and the space available in the plenum, the flow distributor device can have various configurations. The liquid flow distributor device can consist of at least two preferably circular baffle plates located at the outlet of the recycle liquid conduit. For a central vertical baffled nozzle location within the plenum, these baffle plates are usually e~ually spaced from each other. The distributor device bottom plate is solid, and deflects the inlet flow laterally to prevent direct impingement of liquid on the bottom of the plenum. The other baffle or dispersion plates in the device have central openings sized to intercept and deflect portions of the liquid flow laterally or radially outwardly into the plenum. The flow paths of these lateral streams are directed to sweep the plenum bottom to eliminate stagnation æones and provide good mixing of gas/liquid (or gas/liquid slurry) and substantially uniform flow distribution upwardly through openings in the flow distribution grid into the ebullated bed.
The percent o~ total material flowing radially outwardly from the spac~ between each baffle plate can be varied by selecting the dimensions of the distributor device, but usually a greater percentage of the flow is emitted from the lowest space~ In a typical deflector device design, about 40-45% of the inlet liquid flow is deflected by the first plate, 25-35% i5 deflected by the middle plate, and the remaining flow is deflected radially outwardly by the bottom innermost plate. For a nozzle configuration entering the plenum from one ~ide and not located on the pl~num cen~-erline, the baf~le plates are oriented a~ an angle varying from about 0 ~o about 10 s~
with the adj~cent baffle to provide a uniform disper~ion of the gas/liquid flow within the plenum.
For small diameter reactors having inside diameters less than about 5 feet, it is usually more convenient to mix the feed liquid and gas streams with the reactor recycle liquid external to the reactor prior to uniformly distributing the combined mixture in the reactor plenum, utilizing the distributor device of FIG. 1 as described below. For reactors having diameters larger than about 6 ft., it is usually desirable to introduce the feed liquid and gas mixture into the reactor plenum through separate distributor devices. For example, a circular perforated sparger ring is usually located in the plenum upper portion and can be used to distribute the gas-liquid feed mixture uniformly across the reactor plenum. Uniform flow of small bubbles and liquid feed is produced by providing a pressure drop across the sparger and directing the mixed gas-liquid streams from the sparger downwardly to substantially dissipate the stream kinetic energy in the liquid. This kinetic energy is utilized to increase the intensity of liquid backmixing in the plenum. Pressure drops across the sparger ring openings usually range from 1-15 psi for typical heavy petroleum crude upgrading and coal liquefaction processes.
In an alternative embodiment of the invention, the flow distributor device consists of a conduit and a conical-shaped deflector having its base rigidly attached to the plenum lower wall and having its apex oriented toward and substantially aligned with the centerline of the inner 3Q end of the conduit.
This lnlet flow distributor device is used upstream and in combination with the reactor flow distribution grid to provide an improved flow distribution system for an ebullated bed catalyst reactor. The pres~ure drop across the baffled nozzle distribu~or device at rated flow is usually 5-25% of the total pressure drop across bo~h the distributor device and the distribution grid.
Al-though the distributi.on grid can consist of a perfordted plate, it preferably contains multiple vertical tubes each provided with a cap over the tube upper end. This distribution system provides improved gas-liquid contacting and gas mixing in the reactor plen~, eliminates undesired direct impingement of the fluid streams on the distribution grid, and minimizes coke formation in the plenum and in the catalyst bed support above the grirl.
The invention will be further described with reference to FIG. 1, which shows an inlet conduit 10 inserted into a plenum chamber 12 of reactor 14. The conduit has a baffled nozzle or disc donut type flow distributor device 16 oriented generally downwardly in the plenum for feeding a liquid and gas mixture into the plenum, then passing the mixtu.re uniformly upwardly through openings 19 in flow distribution grid 18 into ebullated catalyst bed 20.
Reactor liquid is withdrawn from above the catalyst bed downward through central conduit 24 to a recycle pump (not shown3, from which the liquid is recycled together with fresh liquid and gas feed through inlet conduit 10 to flow distributor 16. The plenum 12 preferably has a height equal to S-10 times the inner diameter conduit 10, and distribution grid 18 preferably has a diameter equal to 4-12 times the inner diameter of conduit 10 As shown in greater detail in FI~ 2, flow distributor device 16 comprises at least one annular-shaped plate 30 having central opening 31 located upstream of bottom circular solid plate 32, and all retained toget~er by three circumferentially equally-spaced structural rods 33, which are preferably located at the baffle plate outer edges. Usually an additional annular-shaped plate 34, having progressively smallex central opening 35, can be located intermediate plates 30 and 32 to provide a preferred baffled nozzle confi~uration for further radial distribution of the flow from conduit 10. The greater percentage of flow should preferably be emitted from the lowest or downstream space, because of the greater ()5~
distance of fluid travel in plenum 12 before reaching dis-tribution qrid 18. For a flow distributor device 16 having three pla-tes, the plate dimensions are preferably selected such that about 40-45 volume percent of the fluid flow is deflected radially outwardly by bottom solid or downstream baffle 32, about 25-35 volume percent is deflected outwardly by the second or intermediate baffle 34, and the remaining flow radially deflected by top or upstream baffle plate 30. If desired, at least one 10w straightening vane 36 can be centrally oriented longitudinally inside conduit 10, so that the flow pattern reaching the distributor device 16 is substantially unidirectional. Such flow straightening vane is particularly useful when the angle of deflection for the flowing fluid in conduit 10 exceed about 30.
FIG. 3 shows an alternative configuration of the fluid flow distribution system of this invention, wherein the flow distributor device 16 is centrally located on the longitudinal center line of the plenum and downwardly oriented in the bottom part of plenum chamber 12 below distribution grid 18, and is located above the bottom of the reactor plenum by a distance equal to 1.0-2.0 times the inside diameter of the inlet conduit. The flow distribution grid 18 preierably contains multiple vertical tubes 26 having an inner diameter of 0.75-1.5 inches and which extend below the grid ~y a distance equal to 4 10 times tne tube inner diameter. Tubes 26 extend above the grid by a distance equal to about 1.5-4 times the tube inner diameter. ~bove the upper end of each tube 26, a cylindrical-shaped cap 28 is provided, which is spaced away from the tube and is rigidly supported from the tube by suitable structural m~mbers ~not shown). Cap 28 is oriented 50 as to prevent en~ry of ca~alyst solid particles 22 from the ebullated bed into tubes 26 whenever there is no upward fluid 10w through the tube, such as may occur during operationai upsets or occurs at process shutdowll.
A circular annular-shaped sparger ring 40 havinq ~l2~.~V5S~
uniformly spaced openings ~1 on its lower side is provided above flow distributor device 16 to uniformly distribute gas and liquid flow in the upper portion 12a of the plenum chamber. The sparger ring 40 encircles downcomer conduit 24 and is particularly useful for large diameter reactors, such as exceeding about 8 feet inside diameter. Multiple spaced openings 41 in the sparger ring 40 are sized to provide a uniform pressure drop and are located to direct the flow downwardly so as to substantially dissipate its kinetic energy and increase the back-mixing action of gas and liquid in the plenum 12.
In another embodiment of the invention as shown by FIG. 4, the flow distributor device consists of a conduit and a conical-shaped deflector 46 which is centrally-located within the bottom portion of the plenum 12, and hasits base rigidly attached to the plenum bottom wall 49. The apex 48 of the deflector 46 is centrally aligned with downwardly oriented end 11 of inlet conduit 10, so that the flow from conduit 10 is deflected substantially uniformly radially outwardly against the lower walls 49 of th~ plenum 12. The conical surface of deflector 46 can be made straight, or curved outwardly at the lower end to facilitate a gradual outward deflection of the flow of the gas/liquid mixture in the plenum. Thus, flow deflector device 46 operates similarly as for distribu~or device 16, whereby the total flow passes radially outwardly and against the walls of the plenum. Circular sparger 40 is provided in plenum chamber 12 centrally located above flow distribution device 46, simmlarly as for the FIG. 3 configuration. The conduit 10 contains at least one flow straightening vane.
The effectiveness of using the inlet flow distributor device configuration is illustrated by ~he following examples, which should not be regarded as limiting the scope of the invention.
EXAMPLES
In a coal hydrogenation plant using the "~-Coal"~
Process for coal liquefaction and having an ebullated bed _,~
s~3 catalyst reactor with 5 ft. inside diameter, (200 tons/day Catlettsburg "H~Coal"TM Pilot Plant Reactor), the feed coal slurry and gas is mixed with the recycle ebullation liquid flow external to the reactor. The total combined stream is then distributed through a side-entering downwardly directed baffled nozzle equipped with three inclined baffle plates, as generally described in the F`IG. 1 embodiment of this invention. Following installation of the flow distributor nozzle in the plenum, coking in the reactor ebullated catalyst bed due to flow maldistribution therein is substantially eliminated.
In a commercial "H-Coal" (18,000 tons/day) Plant reactor design having an 11 ft. inside diameter, the inlet flow distribution system in the plenum contains a side-entering downwardly directed baffled nozzle e~uipped with three inclined baffle plates for dispersion of the recycle liquid slurry flow and a circular sparger ring located above the nozzle for distributing the feed liquid slurry and gas. In a commercial H-Oil~ ~35,000 bbl/day~
Plant reactor design, having 10 ft~ inside diameter, the inlet flow distribution system in the reactor plenum consists of a centrally located vertically oriented baffled nozzle equipped with three horizontal plates for dispersion of ~he recycle ebullating liquid flow, and a sparger ring located above ~he nozzle for uniform flow distribution of the feedstream liquid and gas.
Althouyh this invention has been described broadly and in terms of various specific embodiments, it will be understood that modification~ and variations can be made and some elements used without o~hers all within the spirit and ~cope of the invention, which is defined b~ the following claims,
Claims (21)
1. A flow distributor device for providing a uniform flow distribution of a gas/liquid mixture into an ebullated bed of a reactor, said flow distributor device being located in a plenum of said reactor, said plenum being formed by a distribution grid and the lower end and lower walls of said reactor below said grid, said flow distributor device comprising:
(a) a conduit extending into said plenum from outside the reactor with the conduit inner end being directed downwardly in the plenum;
and (b) a baffled nozzle positioned at the inner end of said conduit within said plenum and downwardly directed toward the lower walls of the reactor for recylcing a hydrocarbon fluid at least partially derived from a reaction within said ebullated bed; said baffled nozzle having at least two substantially parallel baffles spaced apart from each other and rigidly attached to the inner end of said conduit, the innermost or downstream baffle consisting of a solid plate, and at least one other upstream baffle having a central opening and located upstream of the solid plate downstream baffle, whereby said baffled nozzle mixes a gas and a liquid material fed through said conduit downstream into said plenum and is arranged in combination with said distribution grid to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture upwardly into said ebullated bed.
(a) a conduit extending into said plenum from outside the reactor with the conduit inner end being directed downwardly in the plenum;
and (b) a baffled nozzle positioned at the inner end of said conduit within said plenum and downwardly directed toward the lower walls of the reactor for recylcing a hydrocarbon fluid at least partially derived from a reaction within said ebullated bed; said baffled nozzle having at least two substantially parallel baffles spaced apart from each other and rigidly attached to the inner end of said conduit, the innermost or downstream baffle consisting of a solid plate, and at least one other upstream baffle having a central opening and located upstream of the solid plate downstream baffle, whereby said baffled nozzle mixes a gas and a liquid material fed through said conduit downstream into said plenum and is arranged in combination with said distribution grid to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture upwardly into said ebullated bed.
2. The flow distributor device of claim 1, wherein said conduit has at least one flow straightening vane located upstream of said nozzle.
3. The flow distributor device of claim 1, wherein said spaced-apart baffles are oriented at an angle of 45°-90° with the centerline of the inner end of said conduit.
4. The flow distributor device of claim 1, wherein the baffled nozzle device is centrally located on the longitudinal centerline of said plenum with the centerline of said conduit entering the plenum being at an angle of 45-90° with the vertical centerline of said plenum and reactor.
5. The flow distributor device of claim 1, wherein said device consists of three circular baffle plates, the upper first plate having a central opening, the intermediate second plate having a central opening smaller than that in said upper first plate, and the lower third plate being solid.
6. The flow distributor device of claim 5, wherein said upper first plate central opening has a diameter 0.6-0.75 times the conduit inner diameter, and said intermediate plate central opening has a diameter 004-0.5 times the conduit inner diameter.
7. The flow distributor device of claim 1, wherein said baffle plates are spaced apart by a distance equal to 0.3-0.5 times the conduit inner diameter.
8. The flow distributor device of claim 1, wherein the fluid pressure drop across the distributor device is 5-25% of the total fluid pressure drop across the device and said distribution grid.
9. A fluid flow distribution system for providing a uniform flow distribution of a fluid material into an ebullated catalyst bed of a reactor, said distribu-tion system comprising:
(a) a plenum provided in the lower part of the reactor and formed by the lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor;
(b) a conduit extending into said plenum for carrying a flowable fluid material initially downwardly into the plenum; and (c) a flow distributor device located in the lower end of said plenum and associated in flow relationship with said conduit, whereby said distributor device mixes a gas and a liquid material fed through said conduit downwardly into said plenum and is so arranged in combination with said distribution grid as to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture upwardly into said ebullated bed.
(a) a plenum provided in the lower part of the reactor and formed by the lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor;
(b) a conduit extending into said plenum for carrying a flowable fluid material initially downwardly into the plenum; and (c) a flow distributor device located in the lower end of said plenum and associated in flow relationship with said conduit, whereby said distributor device mixes a gas and a liquid material fed through said conduit downwardly into said plenum and is so arranged in combination with said distribution grid as to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture upwardly into said ebullated bed.
10. The flow distribution system of claim 9, wherein said conduit has at least one flow straightening vane located upstream of said flow distribution device.
11. The flow distribution system of claim 9, wherein said distribution grid comprises multiple vertical tubes each covered by a cap over the tube upper end.
12. The flow distribution system of claim 9, wherein an annulus-shaped sparger is provided in said plenum below said distribution grid and above said flow distribution device.
13. A flow distribution system for providing a uniform flow distribution of a fluid material into an ebullated bed of a reactor, said distribution system comprising:
(a) a plenum provided in the lower part of the reactor and formed by the reactor lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor;
(b) a conduit extending into said plenum for carrying a flowable fluid material initially downwardly into the plenum; and (c) a baffled nozzle rigidly attached to the inner end of said conduit, said baffled nozzle having at least two substantially parallel baffles spaced apart from each other, the innermost or downstream baffle con-sisting of a solid plate, and at least one other upstream baffle having a central opening and located upstream of the solid plate downstream baffle, whereby said baffled nozzle mixes a gas and a liquid material fed through said conduit downstream into said plenum and is arranged in combination with said distribution grid, to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture uniformly upwardly into said ebullated bed.
(a) a plenum provided in the lower part of the reactor and formed by the reactor lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor;
(b) a conduit extending into said plenum for carrying a flowable fluid material initially downwardly into the plenum; and (c) a baffled nozzle rigidly attached to the inner end of said conduit, said baffled nozzle having at least two substantially parallel baffles spaced apart from each other, the innermost or downstream baffle con-sisting of a solid plate, and at least one other upstream baffle having a central opening and located upstream of the solid plate downstream baffle, whereby said baffled nozzle mixes a gas and a liquid material fed through said conduit downstream into said plenum and is arranged in combination with said distribution grid, to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture uniformly upwardly into said ebullated bed.
14. The flow distribution system of claim 13, wherein the spaced-apart baffles are oriented at an angle of 45-90° with the axis of the inner end of said conduit.
15. The flow distribution system of claim 13, wherein said baffled nozzle is centrally located in said plenum with the axis of said conduit entering into said plenum being at an angle of 45-90° with the vertical centerline of said plenum and reactor.
16. The flow distribution system of claim 13, wherein said nozzle consists of three circular baffle plates, the upper first plate having a central opening, the intermediate second plate having a central opening smaller than that in said upper first plate, and the lowest third plate being solid.
17. The flow distribution system of claim 13, wherein said upper first plate central opening has a diameter 0.6-0.75 times the conduit inner diameter, and said intermediate plate central opening has a diameter 0.4-0.5 times the conduit inner diameter.
18. The flow distribution system of claim 13, wherein said baffle plates are spaced apart by a distance equal to 0.3-0.5 times the conduit inner diameter.
19. The flow distribution system of claim 13, wherein an annulus-shaped sparger is provided in said plenum below said distribution grid and above said baffled nozzle.
20. A flow distribution system for providing a uniform flow distribution of a fluid material into an ebullated bed of a reactor, said distribution system comprising:
(a) a plenum provided in the lower part of the reactor and formed by the reactor lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor;
(b) a conduit extending into said plenum for carrying a flowable fluid material initially downwardly into the plenum; and (c) a conical-shaped flow deflector device located in the lower end of said plenum, said deflector having its base rigidly attached to the plenum lower end and having its apex oriented toward the inner end of said conduit and having the centerline of said deflector substantially aligned with the centerline of the inner end of said conduit, whereby said conical deflector mixes a gas and a liquid material fed through said conduit into said plenum and is arranged in combination with said distribution grid to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture uniformly upwardly into said ebullated bed.
(a) a plenum provided in the lower part of the reactor and formed by the reactor lower end and side walls and also by a distribution grid located below the ebullated bed in the reactor;
(b) a conduit extending into said plenum for carrying a flowable fluid material initially downwardly into the plenum; and (c) a conical-shaped flow deflector device located in the lower end of said plenum, said deflector having its base rigidly attached to the plenum lower end and having its apex oriented toward the inner end of said conduit and having the centerline of said deflector substantially aligned with the centerline of the inner end of said conduit, whereby said conical deflector mixes a gas and a liquid material fed through said conduit into said plenum and is arranged in combination with said distribution grid to effect a substantially uniform mixing and flow distribution of the gas/liquid mixture uniformly upwardly into said ebullated bed.
21. The flow distribution system of claim 20, wherein said conduit contains at least one flow straightening vane located upstream of said flow deflector.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US41642982A | 1982-09-09 | 1982-09-09 | |
| US416,429 | 1982-09-09 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1229059A true CA1229059A (en) | 1987-11-10 |
Family
ID=23649944
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000436283A Expired CA1229059A (en) | 1982-09-09 | 1983-09-08 | Downwardly-directed fluid flow distribution system for ebullated bed reactor |
Country Status (10)
| Country | Link |
|---|---|
| AU (1) | AU562212B2 (en) |
| CA (1) | CA1229059A (en) |
| DE (1) | DE3329682A1 (en) |
| FI (1) | FI833190A (en) |
| FR (1) | FR2532859B1 (en) |
| GB (1) | GB2126494B (en) |
| IT (1) | IT1170469B (en) |
| MX (1) | MX159052A (en) |
| SE (1) | SE8304854L (en) |
| ZA (1) | ZA835490B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824017A (en) * | 2017-03-14 | 2017-06-13 | 四川泸州巨宏化工有限责任公司 | Auxiliary reactor for producing methyl butynol |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB845655A (en) * | 1957-04-18 | 1960-08-24 | Atomic Energy Commission | Multistage fluidized bed reactor |
| GB919359A (en) * | 1959-04-13 | 1963-02-27 | Svenska Skifferolje Ab | Fluidized bed reactor |
| DE1208736B (en) * | 1963-05-31 | 1966-01-13 | Basf Ag | Vortex reactor |
| US3552033A (en) * | 1968-09-03 | 1971-01-05 | Dorr Oliver Inc | Diffusion nozzle for solids fluidizing apparatus |
| GB1265770A (en) * | 1969-07-01 | 1972-03-08 | ||
| GB1402543A (en) * | 1971-06-21 | 1975-08-13 | Boland K M V | Methods for passing gases through discrete solids and through liquids |
| GB1558969A (en) * | 1977-06-10 | 1980-01-09 | Apollo Heat Ltd | Fluidised beds |
| US4184438A (en) * | 1978-01-05 | 1980-01-22 | Foster Wheeler Development Corporation | Fluidized bed start-up apparatus |
| US4282172A (en) * | 1980-09-11 | 1981-08-04 | Howe-Baker Engineers, Inc. | Gas to liquid diffuser |
-
1983
- 1983-07-27 ZA ZA835490A patent/ZA835490B/en unknown
- 1983-07-27 AU AU17351/83A patent/AU562212B2/en not_active Ceased
- 1983-08-08 GB GB08321321A patent/GB2126494B/en not_active Expired
- 1983-08-17 DE DE3329682A patent/DE3329682A1/en not_active Withdrawn
- 1983-09-06 IT IT48933/83A patent/IT1170469B/en active
- 1983-09-06 MX MX198622A patent/MX159052A/en unknown
- 1983-09-07 FI FI833190A patent/FI833190A/en not_active Application Discontinuation
- 1983-09-08 CA CA000436283A patent/CA1229059A/en not_active Expired
- 1983-09-09 SE SE8304854A patent/SE8304854L/en unknown
- 1983-09-09 FR FR838314429A patent/FR2532859B1/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| FR2532859B1 (en) | 1992-08-07 |
| FI833190A (en) | 1984-03-10 |
| ZA835490B (en) | 1984-04-25 |
| GB8321321D0 (en) | 1983-09-07 |
| IT8348933A0 (en) | 1983-09-06 |
| SE8304854D0 (en) | 1983-09-09 |
| GB2126494A (en) | 1984-03-28 |
| DE3329682A1 (en) | 1984-07-12 |
| SE8304854L (en) | 1984-03-10 |
| FR2532859A1 (en) | 1984-03-16 |
| AU562212B2 (en) | 1987-06-04 |
| MX159052A (en) | 1989-04-13 |
| GB2126494B (en) | 1986-06-25 |
| IT1170469B (en) | 1987-06-03 |
| FI833190A0 (en) | 1983-09-07 |
| AU1735183A (en) | 1984-03-15 |
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