CA2017980A1 - Distillation column reactor - Google Patents
Distillation column reactorInfo
- Publication number
- CA2017980A1 CA2017980A1 CA002017980A CA2017980A CA2017980A1 CA 2017980 A1 CA2017980 A1 CA 2017980A1 CA 002017980 A CA002017980 A CA 002017980A CA 2017980 A CA2017980 A CA 2017980A CA 2017980 A1 CA2017980 A1 CA 2017980A1
- Authority
- CA
- Canada
- Prior art keywords
- catalyst
- liquid
- trays
- distillation column
- column reactor
- 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.)
- Abandoned
Links
- 238000004821 distillation Methods 0.000 title claims abstract description 40
- 239000003054 catalyst Substances 0.000 claims abstract description 113
- 239000007788 liquid Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 230000003134 recirculating effect Effects 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000004508 fractional distillation Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 abstract description 3
- 238000011069 regeneration method Methods 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 239000011949 solid catalyst Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/16—Fractionating columns in which vapour bubbles through liquid
- B01D3/18—Fractionating columns in which vapour bubbles through liquid with horizontal bubble plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S203/00—Distillation: processes, separatory
- Y10S203/06—Reactor-distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Organic Chemistry (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
A method and apparatus is provided for removing catalyst from a distillation dolumn reactor and replacing the catalyst with fresh or regenerated catalyst. More specifically a small particulate catalyst is supported by wire mesh or screen or filter medium on trays in a conventional distillation column and substantially submerged by the liquid on the trays. The vapor rising through the liquid tends to keep the catalyst in suspension in the liquid. A
draw-off is provided for each tray having catalyst supported thereon whereby liquid containing the suspended or slurried catalyst can be removed to a separator during operation. The catalyst is separated, as in a settling tank separator, from the liquid recycled to the tray until all the catalyst has been removed. The separated catalyst is removed for either regeneration or discarding. Fresh catalyst can then be added to the separator where it is slurried into the liquid again being recirculated from the tray. The trays can all be connected to the same separator/slurry mixer by the appropriate piping and manifolds.
A method and apparatus is provided for removing catalyst from a distillation dolumn reactor and replacing the catalyst with fresh or regenerated catalyst. More specifically a small particulate catalyst is supported by wire mesh or screen or filter medium on trays in a conventional distillation column and substantially submerged by the liquid on the trays. The vapor rising through the liquid tends to keep the catalyst in suspension in the liquid. A
draw-off is provided for each tray having catalyst supported thereon whereby liquid containing the suspended or slurried catalyst can be removed to a separator during operation. The catalyst is separated, as in a settling tank separator, from the liquid recycled to the tray until all the catalyst has been removed. The separated catalyst is removed for either regeneration or discarding. Fresh catalyst can then be added to the separator where it is slurried into the liquid again being recirculated from the tray. The trays can all be connected to the same separator/slurry mixer by the appropriate piping and manifolds.
Description
2i~ 7~3~
This invention relates to a dis-tillation column reactor.
The use of catalyst in a distillation column to concurrently carry out chemical reactions and separate the reaction products has been practiced for some time. This use of a catalytic distillation column reactor lends itself particularly well ~or reversible reactions in the liquid phase. See for example U.S. Patents 4,336,407 (etherification), 4,482,775 (isomerization), 4,242,530, (separation of isobutene ~rom C4 streams) and 4,551,567 (deether-i~ieation). The eombination is useful because the reactants, in the liquid phase are quickly separate~
from the reaction produets due to boiling point differences by fractional distillation. Thus the reverse reaction is suppressed.
There have been disclosed severa~ different arran~ements to achieve the desired result. For example British Patents 2,096,603 and 2,096,604 disclose placing the catalyst on conventional trays within a distillation column. A series of U.S.
patents, including those listed above eommonly assigned with the instant invention discloses using the eatalyst as part o~ the paeking :in a packed distillation eolumn. More particularly U.S. Pa~ents 4,443,559 and 4,215,011 exempli~y the later.
Where the catalyst is used as distillation packing, it is usually contained in some cloth belt or wire mesh baskets. Additionally U.S. patents 4,443,559 and 4,215,011 disclose a particu:Late resin catalyst contained in pockets on a cloth belt. The cloth belt is arranged and supported in the column by wire mesh intimately associated with the cloth pockets. U.S. patents 4,439,350 and 4,536,373 ,35 disclose apparatus for placing the cloth belts containing the catalyst on conventional ~istillation column trays.
~qi~
It is generally recognized that ion exchange resin catalyst must be in small particulate form.
See for example, "Catalytic reaction in Ion Exchanga Columns Whilst Displacing the Chemical Equilibrium,"
Chemiker-Zeitung/Chemische Apparatur, ~ol. 90, No.
13, 1966, and German Patent 1,075,613. The small parkiculate form necessitates the bags or wire mesh containers in order to prevent undue pressure drop and provide sufficient space for liquid/vapor 10w in the column.
While ion exchange resins have many applications as catalysts, in some applications they become deactivated quickly. Additionally, the catalyst may age at di~ferent rates up and down the column. At some point in time the catalyst, or some portion of it, must be replaced or regenerated. In all prior arrangements the distillation column must be shut down, either for regeneration in situ or for removal of the deactivated catalyst. Removal and replacement of the catalyst can be cumbersome and time consuming even though provision may be made for removing and replacing only a portion of the catalyst.
The inventor has thus seen a need for a method and apparatus for removing and replacing catalyst without stopping operation. Such a method and apparatus would make many more applications of ion exchange resin catalysts economically Eeasible.
In the broader aspect of the inven-tion there is provided a method and apparatus for removing catalyst from a distillation column reactor and replacing the catalyst with fresh or regenerated catalyst. More specifically a small particulate catalyst is supported by wire mesh or retained by cages on trays in a conventional distillation column and completely submerged by the liquid on the trays.
The vapor rising through the liquid tends to keep the catalyst in suspension in the liquid. A draw-off is 2q~
provided for each tray having catalyst supported thereon whereby liquid containing the suspended or slurried catalyst can be removed to a separator during operation. The catalyst is separated, as in a settling tank separator, from the liquid and the liquid recycled to the tray until all the catalyst has been removed. The separated catalyst is removed for either regeneration or discarding. Fresh catalyst can then be added to the separator where it is slurried into the liqùid again being recirculated from the tray. The trays can all be connected to the same separator/slurry mixer by the appropriate piping and manifolds.
More speci~ically the present distillation column reactor for concurrently carrying out chemical reactions and separating by fractional distillation the reactants and reaction products, comprising:
~a) a distillation column having a plurality of suitable liquid-vapor contact trays;
(b) catalyst loosely supported on at least a portion of said trays to the depth of the liquid on said trays;
(c) first means to withdraw the liquid on said trays carrying said catalyst from said trays;
(d) second means to separate said catalyst from said liquid and return said liquid less said catalyst to said trays;
(e) third means to replace said catalyst with a second catalyst and mix said second catalyst with said liquid and to return said liquid with said second catalyst to said trays.
Because the catalyst agitation may generate "fines" by physical attrition which can trickle down through the trays and build up in the bottom of the reactor, there is also provided a liquid withdrawal with filter in the lower end of the distillation column reactor. A draw-off is provided on the catch 9~
screen to remove these "finesl' withou-t shutting down operation thus preventing undue pressure drop in the column and unwanted reactions.
In the above manner catalyst on individual trays can be replaced to optimize operation of the distillation column reactor without shut down and loss of on stream time.
Broadly stated, the invention relates to an improved distillation column reactor having catalyst loosely supported on trays within the distillation column reactor, which comprises means to remove and replace the catalyst while continuing to operate the distillation column reactor. The invention also relates to a method for removing and replacing solid particulate catalyst supported on trays in a distillation column reactor, comprising the steps of:
(a) drawing liquid carrying the catalyst ~rom any of the trays to a separator;
(b) separating the solid particulate catalyst from the liquid as by settling and recirculating the clear liquid to the tray until all of the solid particulate catalyst has been removed from the tray;
(c) slurrying replacement catalyst in clear liquid recirculated from the tray; and (d) recirculating the slurried catalyst and liquid to the tray while with clear liquid for the slurrying of step (c) until all the catalyst has been replaced on the tray.
For a detailed description of the preferred embodiment of the present invention the reader is directed to the accompanying figures for illustration purposes.
In the drawings which illustrate the invention, ;~41~L79B~
Fig. 1 is a partial sectional view of a distillation column reactor showing trays having catalyst supported thereon;
Fig. 2 is a 1Ow diagram showing the vessels S and piping arrangement for removing catalyst from trays; and Fig. 3 is a flow diagram showing the vessels and piping arrangement for replacing the catalyst on the trays.
Referring ~irst to figure 1 there is shown a portion of a distillation column reactor 100 having conventional distillation trays 101 and 103 therein.
Each tray, either 101 or 103, include overflow wires 107 and downcomers 104. The trays 101 all have small particulate catalyst 109, such as an acid ion exchange resin, supported thereon and contained in liquid 108. Screens 105 cover the downcomer inlet to the trays 103 which contain the catalyst 109 to prevent the catalyst 109 from entering the downcomer.
The screens 105 may be extended downward to the overflow wires 107 on those trays having catalyst to prevent the catalyst 109 from overflowing into the downcomer. Additionally diagonal stilling baffles 106 are provided to prevent the catalyst 109 from clogging the overflow screen.
On those trays 103 containiny catalyst spargers 102 having screens are provided to preven-t catalyst 109 from trickling down the column through the vapor spaces on the trays. The spargers 102 also insure good vapor liquid contact and aid in keeping the catalyst suspended in the liquid on the -trays.
Each tray having catalyst supported thereon includes a catalyst slurry draw-of/return 110 at a minimum height on the tray above the floor of the tray. A
clear liquid draw-off/return 111 is also provided in the downcomer.
This invention relates to a dis-tillation column reactor.
The use of catalyst in a distillation column to concurrently carry out chemical reactions and separate the reaction products has been practiced for some time. This use of a catalytic distillation column reactor lends itself particularly well ~or reversible reactions in the liquid phase. See for example U.S. Patents 4,336,407 (etherification), 4,482,775 (isomerization), 4,242,530, (separation of isobutene ~rom C4 streams) and 4,551,567 (deether-i~ieation). The eombination is useful because the reactants, in the liquid phase are quickly separate~
from the reaction produets due to boiling point differences by fractional distillation. Thus the reverse reaction is suppressed.
There have been disclosed severa~ different arran~ements to achieve the desired result. For example British Patents 2,096,603 and 2,096,604 disclose placing the catalyst on conventional trays within a distillation column. A series of U.S.
patents, including those listed above eommonly assigned with the instant invention discloses using the eatalyst as part o~ the paeking :in a packed distillation eolumn. More particularly U.S. Pa~ents 4,443,559 and 4,215,011 exempli~y the later.
Where the catalyst is used as distillation packing, it is usually contained in some cloth belt or wire mesh baskets. Additionally U.S. patents 4,443,559 and 4,215,011 disclose a particu:Late resin catalyst contained in pockets on a cloth belt. The cloth belt is arranged and supported in the column by wire mesh intimately associated with the cloth pockets. U.S. patents 4,439,350 and 4,536,373 ,35 disclose apparatus for placing the cloth belts containing the catalyst on conventional ~istillation column trays.
~qi~
It is generally recognized that ion exchange resin catalyst must be in small particulate form.
See for example, "Catalytic reaction in Ion Exchanga Columns Whilst Displacing the Chemical Equilibrium,"
Chemiker-Zeitung/Chemische Apparatur, ~ol. 90, No.
13, 1966, and German Patent 1,075,613. The small parkiculate form necessitates the bags or wire mesh containers in order to prevent undue pressure drop and provide sufficient space for liquid/vapor 10w in the column.
While ion exchange resins have many applications as catalysts, in some applications they become deactivated quickly. Additionally, the catalyst may age at di~ferent rates up and down the column. At some point in time the catalyst, or some portion of it, must be replaced or regenerated. In all prior arrangements the distillation column must be shut down, either for regeneration in situ or for removal of the deactivated catalyst. Removal and replacement of the catalyst can be cumbersome and time consuming even though provision may be made for removing and replacing only a portion of the catalyst.
The inventor has thus seen a need for a method and apparatus for removing and replacing catalyst without stopping operation. Such a method and apparatus would make many more applications of ion exchange resin catalysts economically Eeasible.
In the broader aspect of the inven-tion there is provided a method and apparatus for removing catalyst from a distillation column reactor and replacing the catalyst with fresh or regenerated catalyst. More specifically a small particulate catalyst is supported by wire mesh or retained by cages on trays in a conventional distillation column and completely submerged by the liquid on the trays.
The vapor rising through the liquid tends to keep the catalyst in suspension in the liquid. A draw-off is 2q~
provided for each tray having catalyst supported thereon whereby liquid containing the suspended or slurried catalyst can be removed to a separator during operation. The catalyst is separated, as in a settling tank separator, from the liquid and the liquid recycled to the tray until all the catalyst has been removed. The separated catalyst is removed for either regeneration or discarding. Fresh catalyst can then be added to the separator where it is slurried into the liqùid again being recirculated from the tray. The trays can all be connected to the same separator/slurry mixer by the appropriate piping and manifolds.
More speci~ically the present distillation column reactor for concurrently carrying out chemical reactions and separating by fractional distillation the reactants and reaction products, comprising:
~a) a distillation column having a plurality of suitable liquid-vapor contact trays;
(b) catalyst loosely supported on at least a portion of said trays to the depth of the liquid on said trays;
(c) first means to withdraw the liquid on said trays carrying said catalyst from said trays;
(d) second means to separate said catalyst from said liquid and return said liquid less said catalyst to said trays;
(e) third means to replace said catalyst with a second catalyst and mix said second catalyst with said liquid and to return said liquid with said second catalyst to said trays.
Because the catalyst agitation may generate "fines" by physical attrition which can trickle down through the trays and build up in the bottom of the reactor, there is also provided a liquid withdrawal with filter in the lower end of the distillation column reactor. A draw-off is provided on the catch 9~
screen to remove these "finesl' withou-t shutting down operation thus preventing undue pressure drop in the column and unwanted reactions.
In the above manner catalyst on individual trays can be replaced to optimize operation of the distillation column reactor without shut down and loss of on stream time.
Broadly stated, the invention relates to an improved distillation column reactor having catalyst loosely supported on trays within the distillation column reactor, which comprises means to remove and replace the catalyst while continuing to operate the distillation column reactor. The invention also relates to a method for removing and replacing solid particulate catalyst supported on trays in a distillation column reactor, comprising the steps of:
(a) drawing liquid carrying the catalyst ~rom any of the trays to a separator;
(b) separating the solid particulate catalyst from the liquid as by settling and recirculating the clear liquid to the tray until all of the solid particulate catalyst has been removed from the tray;
(c) slurrying replacement catalyst in clear liquid recirculated from the tray; and (d) recirculating the slurried catalyst and liquid to the tray while with clear liquid for the slurrying of step (c) until all the catalyst has been replaced on the tray.
For a detailed description of the preferred embodiment of the present invention the reader is directed to the accompanying figures for illustration purposes.
In the drawings which illustrate the invention, ;~41~L79B~
Fig. 1 is a partial sectional view of a distillation column reactor showing trays having catalyst supported thereon;
Fig. 2 is a 1Ow diagram showing the vessels S and piping arrangement for removing catalyst from trays; and Fig. 3 is a flow diagram showing the vessels and piping arrangement for replacing the catalyst on the trays.
Referring ~irst to figure 1 there is shown a portion of a distillation column reactor 100 having conventional distillation trays 101 and 103 therein.
Each tray, either 101 or 103, include overflow wires 107 and downcomers 104. The trays 101 all have small particulate catalyst 109, such as an acid ion exchange resin, supported thereon and contained in liquid 108. Screens 105 cover the downcomer inlet to the trays 103 which contain the catalyst 109 to prevent the catalyst 109 from entering the downcomer.
The screens 105 may be extended downward to the overflow wires 107 on those trays having catalyst to prevent the catalyst 109 from overflowing into the downcomer. Additionally diagonal stilling baffles 106 are provided to prevent the catalyst 109 from clogging the overflow screen.
On those trays 103 containiny catalyst spargers 102 having screens are provided to preven-t catalyst 109 from trickling down the column through the vapor spaces on the trays. The spargers 102 also insure good vapor liquid contact and aid in keeping the catalyst suspended in the liquid on the -trays.
Each tray having catalyst supported thereon includes a catalyst slurry draw-of/return 110 at a minimum height on the tray above the floor of the tray. A
clear liquid draw-off/return 111 is also provided in the downcomer.
2~ 79~ -Included in the bottom 112 of the column is a liquid draw-off with a filter 113 for catching any catalyst "fines" which may be generated by agitation of the resin on the trays. Draw-off 114 is provided to remove these fines to prevent build up of excess pressure drop in the column. Alternatively the liquid bottoms may be removed to an external circulation pump and external filter (not shown).
Thus, the filter can be cleaned without having to go inside the column.
Referring now to figures 2 and 3 there are shown schematic flow diagrams of typical piping and vessels to achieve the removal and replacement of the catalyst on the trays. For illustration purposes only one tray is shown and individual lines for achieving the draw~off return in the separate operation. In practice manifolds and cross over piping would be provided to reduce the expense of installation.
Figure 2 shows the arrangement for removing catalyst from the tray. The catalyst slurried on the tray is removed through nozzle 110 and valve A via line 1 through sight glass 2 to separator generally depicted at 200. The separator may be of conven-tional design to allow settling o~ the solid catalyst from the liquid. Liquid is withdrawn from -the top of separator 200 via 11ne 3 to the suction side of pump 5 where it is pumped back to the clear liquid inlet through valve B via line 6. Liquid is continually recirculated to and from the tray until no more catalyst can be seen in sight glass 2 indicating that all the catalyst has been removed from the tray and settled out in separator 200.
~fter the catalyst has been removed from the tray, the hopper outlet 12 on separator 200 may be opened and the bulk of the solid catalyst removed.
The separa-tor can then be pressured up, as with nitrogen, through line 8 and valve ~ to blow the 2q~179~
remaining liquid in the separator through screen 10 and line 4 and 6 back to the tray. The screen 10 removes any remaining catalyst ~rom the liquid.
Referring now to figure 3 the arrangement for replacing the catalyst is shown. The replacement catalyst is placed into the separator 200 through fill opening ll, and the opening closed. The separator 200 is then slowly filled with clear liquid from the tray from no~zle lll through valve B via line 15 having an in line sight glasss. Liq~id is withdrawn through line 13 to the suction side of pump 5, the discharge side which is now connected to eductor 9 attached to lower end of separator 200.
The pumped liquid is slurried with catalyst in eductor 9 and returned to the tray return nozzle 110 via line 14 through sight glass 16 and valve A. When sight glass 16 is clear of catalyst the tray has been refilled. The remaining liquid in the separator 200 may be pressured back to the tray using nitrogen under pressure through line 8 through valve C.
As noted above, with the appropriate cross over piping and valves, some lines may be used in the different services for the diEferent operations of removing and replacing the catalyst.
The foregoing description of the invention has been directed to a particular preEerred embodiment of the present invention for purposes of explanation and illustration. It will be apparent to those skilled in the art that many modiEicatlons and changes in the apparatus may be made without departin~ from the scope and spirit of the invention.
It is, therefore, intended that the following claims cover all equivalent modifications and modifications as fall within the scope of the invention as defined by the claims.
Thus, the filter can be cleaned without having to go inside the column.
Referring now to figures 2 and 3 there are shown schematic flow diagrams of typical piping and vessels to achieve the removal and replacement of the catalyst on the trays. For illustration purposes only one tray is shown and individual lines for achieving the draw~off return in the separate operation. In practice manifolds and cross over piping would be provided to reduce the expense of installation.
Figure 2 shows the arrangement for removing catalyst from the tray. The catalyst slurried on the tray is removed through nozzle 110 and valve A via line 1 through sight glass 2 to separator generally depicted at 200. The separator may be of conven-tional design to allow settling o~ the solid catalyst from the liquid. Liquid is withdrawn from -the top of separator 200 via 11ne 3 to the suction side of pump 5 where it is pumped back to the clear liquid inlet through valve B via line 6. Liquid is continually recirculated to and from the tray until no more catalyst can be seen in sight glass 2 indicating that all the catalyst has been removed from the tray and settled out in separator 200.
~fter the catalyst has been removed from the tray, the hopper outlet 12 on separator 200 may be opened and the bulk of the solid catalyst removed.
The separa-tor can then be pressured up, as with nitrogen, through line 8 and valve ~ to blow the 2q~179~
remaining liquid in the separator through screen 10 and line 4 and 6 back to the tray. The screen 10 removes any remaining catalyst ~rom the liquid.
Referring now to figure 3 the arrangement for replacing the catalyst is shown. The replacement catalyst is placed into the separator 200 through fill opening ll, and the opening closed. The separator 200 is then slowly filled with clear liquid from the tray from no~zle lll through valve B via line 15 having an in line sight glasss. Liq~id is withdrawn through line 13 to the suction side of pump 5, the discharge side which is now connected to eductor 9 attached to lower end of separator 200.
The pumped liquid is slurried with catalyst in eductor 9 and returned to the tray return nozzle 110 via line 14 through sight glass 16 and valve A. When sight glass 16 is clear of catalyst the tray has been refilled. The remaining liquid in the separator 200 may be pressured back to the tray using nitrogen under pressure through line 8 through valve C.
As noted above, with the appropriate cross over piping and valves, some lines may be used in the different services for the diEferent operations of removing and replacing the catalyst.
The foregoing description of the invention has been directed to a particular preEerred embodiment of the present invention for purposes of explanation and illustration. It will be apparent to those skilled in the art that many modiEicatlons and changes in the apparatus may be made without departin~ from the scope and spirit of the invention.
It is, therefore, intended that the following claims cover all equivalent modifications and modifications as fall within the scope of the invention as defined by the claims.
Claims (12)
1. In a distillation column reactor having catalyst loosely supported on trays within the distillation column reactor, the improvement comprising a means to remove and replace said catalyst while continuing to operate said distilla-tion column reactor.
2. The distillation column reactor of claim 1, wherein the improvement further comprises means to remove and replace catalyst on individual trays within said distillation column reactor indepen-dently.
3. A distillation column reactor for concur-rently carrying out chemical reactions and separating by fractional distillation the reactants and reaction products, comprising:
(a) a distillation column having a plurality of suitable liquid-vapor contact trays;
(b) catalyst loosely supported on at least a portion of said trays to approximately the depth of the liquid on said trays;
(c) first means to withdraw the liquid on said trays carrying said catalyst from said trays;
(d) second means to separate said catalyst from said liquid and return said liquid less said catalyst to said trays;
(e) third means to replace said catalyst with a second catalyst and mix said second catalyst with said liquid and to return said liquid with said second catalyst to said trays.
(a) a distillation column having a plurality of suitable liquid-vapor contact trays;
(b) catalyst loosely supported on at least a portion of said trays to approximately the depth of the liquid on said trays;
(c) first means to withdraw the liquid on said trays carrying said catalyst from said trays;
(d) second means to separate said catalyst from said liquid and return said liquid less said catalyst to said trays;
(e) third means to replace said catalyst with a second catalyst and mix said second catalyst with said liquid and to return said liquid with said second catalyst to said trays.
4. The distillation column reactor of claim 3, wherein each tray supporting said catalyst is provided with means to independently withdraw and replace said catalyst.
5. The distillation column reactor of claim 3, wherein said first means comprises a first conduit connecting each of said trays supporting said catalyst to said second means.
6. The distillation column reactor of claim 3, wherein said second means comprises a settling tank separator to allow said catalyst to settle out of said liquid, a second conduit connecting said settling tank separator to the suction side of a pump, and a third conduit connecting the discharge side of said pump to said trays, said liquid less said catalyst being returned to said trays.
7. The distillation column reactor of claim 6, wherein said settling tank separator further comprises means to remove the bulk of said catalyst from the bottom of said settling tank separator and means to filter the remainder of said catalyst in said liquid prior to returning said liquid to said trays.
8. The distillation column reactor of claim 6, wherein said third means comprises said settling tank separator, a fourth conduit connecting said trays to said settling tank separator, eductor means at the lower means at the lower end of said settling tank separator connected by a fifth conduit to the discharge side of said pump to mix said second catalyst with said liquid, and a sixth conduit connecting said eductor means with said trays to carry said liquid with said second catalyst to said trays.
9. The distillation column reactor of claim 3, wherein means is provided to retain said catalyst on a tray.
10. The distillation column reactor of claim 9, further comprising a screen on each of said trays supporting said catalyst to retain said catalyst on said trays.
11. The distillation column reactor of claim 3, further comprising a draw stream near the bottom of said distillation column reactor associated with a screen to catch any catalyst entrained in the liquid.
12. A method for removing and replacing solid particulate catalyst supported on trays in a distillation column reactor, comprising the steps of:
(a) drawing liquid carrying the catalyst from any of the trays to a separator;
(b) separating the solid particulate catalyst from the liquid as by settling and recirculating the clear liquid to the tray until all of the solid particulate catalyst has been removed from the tray;
(c) slurrying replacement catalyst in clear liquid recirculated from the tray; and (d) recirculating the slurried catalyst and liquid to the tray while with clear liquid for the slurrying of step (c) until all the catalyst has been replaced on the tray.
(a) drawing liquid carrying the catalyst from any of the trays to a separator;
(b) separating the solid particulate catalyst from the liquid as by settling and recirculating the clear liquid to the tray until all of the solid particulate catalyst has been removed from the tray;
(c) slurrying replacement catalyst in clear liquid recirculated from the tray; and (d) recirculating the slurried catalyst and liquid to the tray while with clear liquid for the slurrying of step (c) until all the catalyst has been replaced on the tray.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US362,494 | 1989-06-07 | ||
US07/362,494 US5133942A (en) | 1989-06-07 | 1989-06-07 | Distillation column reactor with catalyst replacement apparatus |
Publications (1)
Publication Number | Publication Date |
---|---|
CA2017980A1 true CA2017980A1 (en) | 1990-12-07 |
Family
ID=23426341
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA002017980A Abandoned CA2017980A1 (en) | 1989-06-07 | 1990-05-31 | Distillation column reactor |
Country Status (8)
Country | Link |
---|---|
US (1) | US5133942A (en) |
EP (1) | EP0402019B1 (en) |
JP (1) | JP2935536B2 (en) |
KR (1) | KR0154531B1 (en) |
CA (1) | CA2017980A1 (en) |
DE (1) | DE69020435T2 (en) |
MX (1) | MX172022B (en) |
MY (1) | MY105976A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016020374A1 (en) * | 2014-08-05 | 2016-02-11 | Basf Se | Column for the thermal treatment of a fluid, having a return line |
Families Citing this family (22)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5948211A (en) * | 1990-02-06 | 1999-09-07 | Koch-Glitsch, Inc. | Distillation column downcomer having liquid permeable wall |
US5855741A (en) * | 1990-02-06 | 1999-01-05 | Koch Engineering Company, Inc. | Apparatus for concurrent reaction with distillation |
US5593548A (en) * | 1990-02-06 | 1997-01-14 | Koch Engineering Company, Inc. | Method for concurrent reaction with distillation |
US5454913A (en) * | 1990-02-06 | 1995-10-03 | Koch Engineering Company, Inc. | Internals for distillation columns including those for use in catalytic reactions |
US5447609A (en) * | 1990-02-06 | 1995-09-05 | Koch Engineering Company, Inc. | Catalytic reaction and mass transfer process |
US5108550A (en) * | 1990-02-06 | 1992-04-28 | Koch Engineering Company, Inc. | Catalyst system for distillation reactor |
US5130102A (en) * | 1990-06-11 | 1992-07-14 | Chemical Research & Licensing Company | Catalytic distillation reactor |
ES2057965T3 (en) * | 1991-03-08 | 1994-10-16 | Inst Francais Du Petrole | DISTILLATION-REACTION DEVICE AND ITS USE. |
US5338517A (en) * | 1992-05-18 | 1994-08-16 | Chemical Research & Licensing Company | Catalytic distillation column reactor and tray |
WO1994019079A1 (en) * | 1993-02-17 | 1994-09-01 | China Petro-Chemical Corporation | A multiple stage suspended reactive stripping process and apparatus |
CN1080914A (en) * | 1993-02-17 | 1994-01-19 | 中国石油化工总公司 | A kind of 2, the manufacture method of 2-two (4-hydroxy phenyl) propane |
US5449501A (en) * | 1994-03-29 | 1995-09-12 | Uop | Apparatus and process for catalytic distillation |
AU692960B2 (en) * | 1994-12-23 | 1998-06-18 | Marschall Acoustics Pty Ltd | Hydrophone |
US5856606A (en) * | 1996-09-27 | 1999-01-05 | Uop Llc | Turbulent bed solid catalyst hydrocarbon alkylation process |
FR2759302B1 (en) * | 1997-02-12 | 1999-03-19 | Inst Francais Du Petrole | METHOD OF LOADING AND UNLOADING A CATALYST WITHOUT STOPPING THE OPERATION OF AN OPERATION |
US6565816B1 (en) | 1997-06-25 | 2003-05-20 | Koch-Glitsch, Inc. | Saddle structure for reactive distillation |
US7718137B2 (en) * | 2005-10-28 | 2010-05-18 | Eastman Chemical Company | Reactor with optimized internal tray design |
US20070095725A1 (en) * | 2005-10-31 | 2007-05-03 | Catalytic Distillation Technologies | Processing of FCC naphtha |
WO2009011603A1 (en) * | 2007-07-16 | 2009-01-22 | Fde Process Systems Limited | Improvements in a method of distillation and/or a distillation column |
US20090183981A1 (en) * | 2008-01-23 | 2009-07-23 | Catalytic Distillation Technologies | Integrated pyrolysis gasoline treatment process |
GB201116382D0 (en) | 2011-09-22 | 2011-11-02 | Davy Process Techn Ltd | Apparatus and method |
JP6895986B2 (en) * | 2016-11-09 | 2021-06-30 | ホーコス株式会社 | Wet dust collector |
Family Cites Families (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1075613B (en) * | 1957-12-21 | 1960-02-18 | Badische Anilin &. Soda Fabrik Aktiengesellschaft, Lud« igshaf en/Rhem | Column for carrying out organic chemical reactions in the presence of fine-grain catalysts |
GB1073727A (en) * | 1964-07-15 | 1967-06-28 | Hydrocarbon Research Inc | Method of reacting a gas and a liquid |
FR1599004A (en) * | 1968-10-17 | 1970-07-15 | ||
DE2053115C3 (en) * | 1970-10-29 | 1978-08-31 | Hoechst Ag, 6000 Frankfurt | Process for the continuous implementation of heterogeneous catalytic reactions in the liquid phase in a fluidized bed |
US4046516A (en) * | 1975-12-29 | 1977-09-06 | Uop Inc. | Hydrogen fluoride-catalyzed alkylation apparatus |
BE864590A (en) * | 1977-03-10 | 1978-09-06 | Inst Francais Du Petrole | METHOD AND APPARATUS FOR CARRYING OUT THREE-PHASE CATALYTIC REACTIONS |
US4215011A (en) * | 1979-02-21 | 1980-07-29 | Chemical Research And Licensing Company | Catalyst system for separating isobutene from C4 streams |
US4242530A (en) * | 1978-07-27 | 1980-12-30 | Chemical Research & Licensing Company | Process for separating isobutene from C4 streams |
US4336407A (en) * | 1980-02-25 | 1982-06-22 | Chemical Research & Licensing Company | Catalytic distillation process |
IT1137527B (en) * | 1981-04-10 | 1986-09-10 | Anic Spa | PROCEDURE FOR THE PREPARATION OF TERTIARY ALCHYL ETHERS |
NZ200039A (en) * | 1981-04-10 | 1984-07-06 | Snam Progetti | Decomposition of alkyl t-alkyl ethers to produce olefins and alcohols |
US4443559A (en) * | 1981-09-30 | 1984-04-17 | Chemical Research & Licensing Company | Catalytic distillation structure |
US4536373A (en) * | 1982-06-21 | 1985-08-20 | Chemical Research & Licensing Company | Contact structure for use in catalytic distillation |
US4439350A (en) * | 1982-06-21 | 1984-03-27 | Chemical Research & Licensing Company | Contact structure for use in catalytic distillation |
US4551567A (en) * | 1983-07-25 | 1985-11-05 | Chemical Research & Licensing Company | Deetherification process |
US4774364A (en) * | 1987-10-07 | 1988-09-27 | Mobil Oil Corporation | Integrated alkylation/alkyl tertiary-alkyl ether synthesis process |
US4847430A (en) * | 1988-03-21 | 1989-07-11 | Institut Francais Du Petrole | Process for manufacturing a tertiary alkyl ether by reactive distillation |
-
1989
- 1989-06-07 US US07/362,494 patent/US5133942A/en not_active Expired - Lifetime
-
1990
- 1990-05-16 MY MYPI90000781A patent/MY105976A/en unknown
- 1990-05-21 MX MX020811A patent/MX172022B/en unknown
- 1990-05-23 KR KR1019900007431A patent/KR0154531B1/en not_active IP Right Cessation
- 1990-05-25 EP EP90305737A patent/EP0402019B1/en not_active Expired - Lifetime
- 1990-05-25 DE DE69020435T patent/DE69020435T2/en not_active Expired - Fee Related
- 1990-05-29 JP JP2139552A patent/JP2935536B2/en not_active Expired - Lifetime
- 1990-05-31 CA CA002017980A patent/CA2017980A1/en not_active Abandoned
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016020374A1 (en) * | 2014-08-05 | 2016-02-11 | Basf Se | Column for the thermal treatment of a fluid, having a return line |
CN106794387A (en) * | 2014-08-05 | 2017-05-31 | 巴斯夫欧洲公司 | For the tower with reflux pipeline of fluid heat treatment |
CN106794387B (en) * | 2014-08-05 | 2019-11-29 | 巴斯夫欧洲公司 | The tower with reflux pipeline for fluid heat treatment |
Also Published As
Publication number | Publication date |
---|---|
MX172022B (en) | 1993-11-29 |
KR0154531B1 (en) | 1998-11-16 |
EP0402019A2 (en) | 1990-12-12 |
EP0402019B1 (en) | 1995-06-28 |
EP0402019A3 (en) | 1992-11-19 |
MY105976A (en) | 1995-02-28 |
JP2935536B2 (en) | 1999-08-16 |
KR910000204A (en) | 1991-01-29 |
US5133942A (en) | 1992-07-28 |
JPH0332737A (en) | 1991-02-13 |
DE69020435D1 (en) | 1995-08-03 |
DE69020435T2 (en) | 1996-02-01 |
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EEER | Examination request | ||
FZDE | Discontinued |